CN104128139B

CN104128139B - Tubular reactor with Curve guide impeller and its application method

Info

Publication number: CN104128139B
Application number: CN201410142795.XA
Authority: CN
Inventors: 查尔斯·R·克尔曼; 托马斯·A·米茨卡; 约翰·P·普安萨蒂; 加里·R·韦斯特
Original assignee: Invista Textiles UK Ltd
Current assignee: Invista Textiles UK Ltd
Priority date: 2013-05-01
Filing date: 2014-04-10
Publication date: 2018-11-06
Anticipated expiration: 2034-04-10
Also published as: TW201500381A; CN104128139A; WO2014179044A1

Abstract

The present invention relates to the mthods, systems and devices for preparing the polyamide at least two heat transmission mediums for transferring heat to tubular reactor.This method may include by the first flowable heat transmission medium heating, to provide heated first flowable heat transmission medium.This method may include that heat is transferred to the second flowable heat transmission medium from the first heated flowable heat transmission medium, to provide heated second flowable heat transmission medium.This method can further include that heat is transferred to the tubular reactor of polyamide synthesis system from the second heated flowable heat transmission medium.

Description

Tubular reactor with Curve guide impeller and its application method

Cross reference to related applications

This application claims the benefit of priority for the U.S. Provisional Patent Application No. 61/818,320 that on May 1st, 2013 submits, Its disclosure is incorporated herein by reference in their entirety.

Technical field

This application involves tubular reactors and its application method with Curve guide impeller.

Background technology

The durability and intensity that polyamide has useful property for example high, this allows them to make in a variety of environment With.Polyamide such as nylon, aromatic polyamides and poly- (aspartic acid) sodium are commonly used in, for example, carpet, air bag, mechanical part, clothes Decorations, rope and stocking.Nylon-6,6, a kind of soft and smooth thermoplastic and a kind of most-often used polyamide.Nylon- 6,6 long chain and compact texture makes it be qualified as advanced nylon fiber, shows high mechanical properties, rigidity and heat Stability.

Polyamide commercial synthesis in extensive manufacturing equipment.For example, nylon-6,6 can be by making hexamethylene diamine Condensation reaction is undergone with adipic acid, form amido bond and discharges water and synthesizes.Including autoclave or reactor, flash vessel and after In a series of components of condensation kettle, heat is applied to reaction mixture and gradually removes water to drive balance towards polyamides Amine, until polymer reaches required length range.Later, the nylon-6 of melting, 6 is extruded into pellet, can be spun and is Fiber is processed as other shapes.Entire manufacturing equipment needs a large amount of heating, so that condensation reaction occurs and from reaction Mixture removes water.Typically, central heating installation will be filled with the single heating circuit heating of volatility heat transmission medium With by medium vapor, the medium is recycled to all parts for needing to heat, including reactor in whole equipment later.

A type of reactor for polyamide synthesis is tubular reactor.When tubular reactor heats reaction mixing When object, vapor water (for example, vapor) is generated.Tubular reactor detaches vapor from reaction mixture at least partly to incite somebody to action Water is removed from reaction mixture and will be balanced and driven to polyamide.When tubular reactor heats reaction mixture, reacting Can occur quick thermal change in mixture, the formation phase of this and unfavorable by-product that polyamide products can be polluted It closes.Quick thermal change may further result in the formation of gel, can accumulate and multiple and different components of final block system, need The closing and cleaning of reactor and other component are wanted, and pollutes polyamide products and causes to the negative of the properties such as screw strength It influences.When forming vapor in tubular reactor, it increases the pressure in reactor and forms vapor and reaction mixing The mixture of object.The increase of pressure can cause vapor and reaction mixture to be traveling at high speeds along tubular reactor, this can be with So that the temperature of control reaction mixture is difficult, and can to complicate vapor from reaction mixture isolation.Reaction The high speed of vapor and reaction mixture can lead to the aerosolized of reaction mixture in device, this can cause vapor to be arranged It puts mouth to be blocked by reaction mixture and polyamide gels, thus reactor is needed frequently to close to be cleaned.

In polyamide synthesis, there is the relevant safety wind of use with a large amount of volatile materials as heat transmission medium Danger, including catch fire, burn and health risk, and exist such as with use single whole equipment (plant-wide) The problem of heating circuit is for the relevant loss in efficiency of multiple components of heating equipment and inconvenience etc.

Invention content

The present invention can provide a kind of method preparing polyamide.This method may include transmitting the first flowable heat to be situated between Matter heats, to provide heated first flowable heat transmission medium.This method may include can from heated first by heat Flowing heat transmission medium is transferred to the second flowable heat transmission medium, to provide heated second flowable heat transmission medium. This method can also include that heat is transferred to the tubular type of polyamide synthesis system from the second heated flowable heat transmission medium Reactor.

The present invention, which can provide, a kind of preparing nylon-6,6 method.This method may include：By including terphenyl One flowable heat transmission medium heating, to provide heated first flowable heat transmission medium.This method may include will be hot It is transferred to the second flowable heat transmission medium from the flowable heat transmission medium of heated first including diphenyl ether and biphenyl, with The flowable heat transmission medium of heated second and used first flowable heat transmission medium are provided.First flowable heat passes Passing medium, the heated first flowable heat transmission medium and used first flowable heat transmission medium can be arranged In one heating circuit.By the first flowable heat transmission medium heating and by heat from the first heated flowable heat transmission medium During being transferred to the second flowable heat transmission medium, the first flowable heat transmission medium, the heated first flowable heat Transfer medium and used first flowable heat transmission medium can be substantially liquid phase.The first flowable heat is transferred to pass The heat passed the heat of medium and transmitted from the first flowable heat transmission medium may include substantially all sensible heat.By heat from heating During the first flowable heat transmission medium crossed is transferred to the second flowable heat transmission medium, the second flowable heat, which is transmitted, to be situated between Matter substantially all can be gasified.This method may include being recycled back to the used first flowable heat transmission medium The heating of first flowable heat transmission medium.This method may include passing heat from the second heated flowable heat transmission medium It is handed to nylon-6, the tubular reactor of 6 synthesis systems.Second flowable heat transmission medium and the heated second flowable heat pass Passing medium can be arranged in the second heating circuit.Second flowable heat transmission medium and used second flowable heat are transmitted Medium can be substantially liquid phase.The second heated flowable heat transmission medium can be substantially liquid phase.It is transferred to The heat of second flowable heat transmission medium, and may include from the heat of the second flowable heat transmission medium transmission：About 70- 100% latent heat for including heat of gasification, and about 0-30% sensible heats.This method can also include the second heat transfer circuit of control Pressure is to control the saturation temperature of the second flowable heat transmission medium, wherein controlling polyamide synthesis system by controlling saturation temperature The temperature of the tubular reactor of system.This method can further include being recycled back to the used second flowable heat transmission medium In the transmission of heat from the first heated flowable heat transmission medium.Tubular reactor can be with about 75 to about 125 meters of length, about 25cm are to the internal diameter of about 60cm, and the length/diameter (L/D) of about 100 to about 500.Tubular reactor May include about 10 to about 25 floss holes along its length.

The present invention can provide a kind of method preparing polyamide.This method may include that the first flowable heat of heating is transmitted Medium, to provide heated first flowable heat transmission medium.This method may include that can flow heat from heated first Dynamic heat transmission medium is transferred to the second flowable heat transmission medium, to provide heated second flowable heat transmission medium.It should Method may include that heat is transferred to the pipe reaction of polyamide synthesis system from the second heated flowable heat transmission medium Device.Tubular reactor can be with about 75 to about 125 meters of length, the internal diameter of about 25cm to about 60cm, and about 100 to about 500 length/diameter (L/D).Tubular reactor may include about 10 to about 25 floss holes along its length.

The present invention can provide the system for being used to prepare polyamide.The system may include heater, and the heater is matched It is set to the first flowable heat transmission medium heating to provide heated first flowable heat transmission medium.The system can wrap First heat exchanger is included, the first heat exchanger is configured to transmit heat from the first heated flowable heat transmission medium to carry For the second heated flowable heat transmission medium.The system can also include second heat exchanger, the second heat exchanger It is configured to for heat to be transferred to the tubular reactor of polyamide synthesis system from the second heated flowable heat transmission medium.

The present invention can provide a kind of device being used to prepare polyamide.The device may include heater, the heating Device is configured to the first flowable heat transmission medium heating to provide heated first flowable heat transmission medium.The system can To include first heat exchanger, the first heat exchanger is configured to transmit heat from the first heated flowable heat transmission medium To provide heated second flowable heat transmission medium.The system can also include second heat exchanger, and second heat is handed over Parallel operation is configured to for heat to be transferred to the tubular reactor of polyamide synthesis system from the second heated flowable heat transmission medium.

The present invention can provide one kind and be used to prepare nylon-6,6 device.The device may include heater, described to add Hot device is configured to the first flowable heat transmission medium heating that will be including terphenyl, is passed with providing the flowable heat of heated first Pass medium.The device may include first heat exchanger, and the first heat exchanger is configured to can from heated first by heat Flowing heat transmission medium is transferred to the second flowable heat transmission medium including diphenyl ether and biphenyl, to provide heated second Flowable heat transmission medium and used first flowable heat transmission medium, and the used first flowable heat is transmitted Medium circulation is back to first heat exchanger.First flowable heat transmission medium, the heated first flowable heat transmission medium It can be arranged in the first heating circuit with the used first flowable heat transmission medium.It is situated between transmitting the first flowable heat Matter heats and by heat from during the first heated flowable heat transmission medium is transferred to the second flowable heat transmission medium, First flowable heat transmission medium, the heated first flowable heat transmission medium and used first flowable heat are transmitted and are situated between Matter can be basic liquid phase.It is transferred to the heat of the first flowable heat transmission medium and is passed from the first flowable heat transmission medium The heat passed may include substantially all sensible heat.In addition, heat is transferred to from the first heated flowable heat transmission medium During second flowable heat transmission medium, the second flowable heat transmission medium can be by substantially all gasification.The device May include second heat exchanger, the second heat exchanger is configured to：Heat is transmitted from the second heated flowable heat and is situated between Matter is transferred to the tubular reactor of polyamide synthesis system, to provide the used second flowable heat transmission medium, and Used second flowable heat transmission medium is recycled back to from the first heated flowable heat transmission medium Heat transmission in.Second flowable heat transmission medium and the heated second flowable heat transmission medium can be arranged second In heating circuit, the pressure of the second heat transfer circuit in order to control is configured to control the saturation temperature of the second flowable heat transmission medium Degree.Control saturation temperature can control the temperature of the tubular reactor of polyamide synthesis system.Second flowable heat transmission medium Can be substantially liquid phase with the used second flowable heat transmission medium, the heated second flowable heat transmission medium can To be basic liquid phase.It is situated between in addition, being transferred to the heat of the second flowable heat transmission medium and being transmitted from the second flowable heat Matter transmit heat may include：About 70-100% latent heat for including heat of gasification, and about 0-30% sensible heats.Tubular reactor It can be with the length/diameter of about 75 to about 125 meters of length, the internal diameter of about 25cm to about 60cm, and about 100 to about 500 (L/D).Tubular reactor may include about 10 to about 25 floss holes along its length.

The present invention can provide better than other be used to prepare polyamide mthods, systems and devices benefit, it is therein extremely Some are unexpected less.If the heating circuit containing volatility (for example, gaseous state) heat transmission medium has leakage, material is leaked Material can spread the space around leakage.If volatility heat transmission medium is flammable, leakage can cause to spread The explosion in the space around leaking or burning risk.In addition, steam heat transmission medium can cause far more than the most adjacent of leakage Neighbouring security risks.If leakage occurs that polymer material is made to enter level-one heating circuit, add for heating level-one Coke formation in the stove of hot loop can establish the burning risk of generation.Containing fixedness heat transmission medium (for example, liquid Body) heating circuit can be more safer than the heating circuit containing volatility heat transmission medium.If leakage occurs, non-volatile Property leakage material be generally moved to the ground around leakage, to which any burning and security risks mastery to be limited in and let out The region of leakage near and below, and there is risk of explosion more lower than volatile material.If leakage occurs so that polymer Material enters level-one heating circuit, then the burning risk of the pipe of the coking in heater can be significantly lower.

The single circuit of fixedness material, or can be with using the two level heating circuit wherein with fixedness material It is attributed to and undergoes localized hyperthermia using sensible heat heat is transferred to tubular reactor from heating circuit, this can enable control pipes The heating of formula reactor is difficult.It is relevant with the fixedness material that is used in the heating circuit for heated Tube reactor Disadvantage can be avoided by using each embodiment of the present invention：Add when using the level-one containing fixedness heat transmission medium Hot loop (for example, in used temperature and pressure, material is substantially maintained as liquid when heated and after cooling) with (include at least one pipe reaction respectively for heating in one or more two level heating circuits when heating two level heating circuit One or more components of device) in using volatile material (for example, in used temperature and pressure, material becomes when heated It obtains and substantially gasifies and condense after cooling).Secondary circuit can be used for heating mainly using latent heat (for example, heat of gasification) Tubular reactor or other arbitrary optional components are to transfer heat to component, it may be advantageous that allow easier temperature to control, together When avoid the use of a large amount of volatile material and avoid heating all components using single heating circuit.

Use primary circuit (higher volatilization of its heating for heated Tube reactor of more low volatility heat transmission medium Property heat transmission medium secondary circuit) leakage in heating circuit for tubular reactor can be made to be easier to repair (fix).For example, if for heating, to include several components around the equipment of tubular reactor have a heat of steam wherein It transmits and is leaked in the single heating circuit of material, then entire circuit must be closed to repair leakage, or extinguish by leaking Caused burning leads to the equipment off-line of most, this can be inconvenient and expensive.However, being included in by having The steam heat transfer material being specific in the secondary circuit of tubular reactor, the leakage in secondary circuit only need the dimension in the circuit It repaiies, while the remaining part of equipment can normally continue to operate.In multiple examples, by primary circuit using not waving Hair property heat transmission medium and by avoid use a large amount of volatile combustible heat transmission medium, with making for volatility heat transfer material It is reduced with relevant security risks.For example, the leakage in the big primary circuit containing liquid phase heat transfer material can be ratio Spillage risk in big circuit containing steam heat transfer material is low.

The use in the circuit of single heat transfer material, which can will can be used for heat, transmits the temperature limiting of material used and be The temperature of close limit.It can allow to hold for tubular reactor using the secondary circuit wherein with volatility heat transmission medium It changes places and controls the temperature of heat transmission medium.It can use primary circuit that the volatile material in secondary circuit is vaporized, it can To allow to be condensed to transfer heat to tubular reactor.The pressure in secondary circuit can be adjusted to control heat transmission medium Saturation temperature, to accurately control the temperature of the gasification and condensation of the volatility heat transmission medium in secondary circuit, to equipment portion The temperature of part is used to prepare the controlling extent of the mthods, systems and devices offer bigger of polyamide than others.When using respective When multiple secondary circuits containing volatility heat transmission medium, the saturation temperature of the heat transmission medium in each secondary circuit can be with It is readily controlled.

The use in the single circuit with volatility heat transfer material (steam/gas phase) may include by heat transfer material The temperature that initial heating is used to each component being suitably above by equipment.This can cause heat transfer material to be overheat (such as so that temperature is higher than the saturation temperature for given pressure).It is controlled if necessary to rigid temperature, then needs other answer Polygamy obtains temperature uniformity to remove overheat.In each embodiment, secondary circuit can allow or connect very much Heat transfer material is used in the secondary circuit of nearly saturation temperature, it is uniform to obtain high temperature with the equipment of lower complexity Property.In each embodiment, opposite superheated vapor, it can be more effective that heat, which is transmitted, using saturated vapor.If steamed Gas significantly overheats, then steam is cooled to saturation temperature before condensation occurs first.The steam of overheat has than condensing steam Much lower heat transfer coefficient.In each embodiment, passed using the heat with the overheat fewer than other method or apparatus Material is passed to transmit the more heat of given surface product permission as saturated vapor or allow smaller surface area to obtain equal amount Heat transmit.In each embodiment, the condensation in the low volatilyty liquid and secondary circuit in level-one heating circuit is steamed The use of gas can allow smaller area of heat transfer (process vessel size), such as method in the part with high heat demand In.

The possible too fast heating polyamide reaction mixture of tubular reactor, this can lead to the shape of unfavorable by-product At unfavorable by-product can pollute required polyamide products.Quick thermal change may further result in the formation of gel, can With accumulation and multiple components of final block system, it is desirable that the closing and cleaning of reactor and other component.Quick thermal change The loss of diamines bigger in vapor caused by can causing.Quick thermal change can increase the aerosol of reaction mixture Change, this can cause moisture discharge mouth to be blocked by reaction mixture and polyamide gels, thus it requires reactor is more frequent It closes to be cleaned.It can be longer in length that the present invention, which can provide, have less diameter, or the length with bigger Degree with diameter than at least one of tubular reactor can allow reaction mixture compared with other tubular reactors More slowly and leniently it is heated to target temperature.The present invention can provide the table for having bigger than other tubular reactors The tubular reactor of area and volume ratio, to the heating for allowing reaction mixture gentler.Therefore, the present invention can be provided in The tubular reactor of less unfavorable by-product is generated in polyamide building-up process, this is by less gel-forming and product It is tired, the closing and cleaning of relatively low frequency are needed, and less diamines is lost from reaction mixture.

Tubular reactor can have from the entrance of reactor to the increased diameter in outlet.If diameter is along the expansion of length The too fast appearance of rate, then the possible too fast cooling polyamide reaction mixture of reactor, leads to gelation and the solidification of reaction mixture, This may need the more frequent closing of reactor for cleaning.The present invention can provide with can be sufficiently small expansion rate to subtract Less or minimize gelation and the solidification of reaction mixture tubular reactor, therefore it is required that than with bigger expansion rate its The closing and cleaning of the relatively low frequency of his tubular reactor.The present invention can provide a kind of tubular reactor, with sufficiently large Expansion rate so that pressure is suitably reduced from the entrance of reactor to outlet to provide removal ratio of the water from reaction mixture It is more effective with other tubular reactors compared with low thermal expansion or without expansion rate.

The high speed of vapor and polyamide reaction mixture can cause the gas of reaction mixture molten in tubular reactor Gelatinization, this can cause moisture discharge mouth to be blocked by reaction mixture and polyamide gels, it is desirable that the frequent closing of reactor For cleaning.High speed in tubular reactor is it is also possible that be difficult to control the temperature of reaction mixture.The present invention can carry For with can be with greater number or more desirably along the tubular reactor of the floss hole of distribution of lengths, so that reaction mixture It can be reduced or minimized than other tubular reactors via the acceleration of the generation of vapor, this can reduce aerosolized and simple Change the temperature control of reaction mixture.The present invention can provide the method being injected into solvent, such as water in floss hole pipeline, this The formation or accumulation of gel or other materials in floss hole pipeline can be made to reduce or minimize.It is reducing or minimum The injection of aerosolized or water can be provided needs the closing of lower frequency and clean tubular type compared with other tubular reactors Reactor.

In various embodiments, tubular reactor can have the interval between certain amount floss hole and floss hole, It provides the annular flow than other tubular reactor greater proportions, leads to the heat transfer area between reaction mixture and reactor Higher is designed than other tubular reactors.For example, with relatively closely spaced and undergo with the air gas along reactor head Bubble or with along the bottom of reactor formed semicircular column reaction mixture flow pattern other tubular reactor ratios Compared with some embodiments interval with bigger between floss hole, to provide better annularly flow.For example, with more Large-spacing and the part for undergoing reaction mixture flash and other tubular reactors of piston flow pattern compare, some implementations Scheme has relatively closely spaced to provide better annularly flow between floss hole.

Description of the drawings

The attached drawing being not drawn necessarily to scale by way of example, but is not the usually example by way of restriction The present invention.

Fig. 1 examples are according to the tubular reactors of multiple embodiments.

Fig. 2 examples are according to the system or device of multiple embodiments.

Fig. 3 examples are according to the system or device of multiple embodiments.

Specific implementation mode

Now with detailed reference to certain examples of disclosed topic, show in the accompanying drawings to these instance section.Although will In conjunction with the disclosed theme of cited claim description, it should be apparent that be that exemplified theme is not expected by claim It is limited to disclosed theme.

It should be construed to include not only clearly describing as the boundary of range using flexible way with the value that range format is expressed Numerical value, and include all independent numerical value or subrange for including within the scope of this, as each numerical value and subrange is bright It really states the same.For example, the range of " about 0.1% to about 5% " or " about 0.1% to 5% " should be construed as including not only about 0.1% to about 5%, and include individual value (for example, 1%, 2%, 3% and 4%) and subrange in pointed range (for example, 0.1% to 0.5%, 1.1% to 2.2%, 3.3% to 4.4%).Unless otherwise noted, statement " about X to Y " have with " about X to about Y " identical meaning.Equally, unless otherwise noted, statement " about X, Y or about Z " has and " about X, about Y or about Z " phase Same meaning.

Herein, unless the context clearly indicates otherwise, term "one", "an" or " described " be used for include One or more than one.Unless otherwise noted, term "or" is used to refer to non-exclusive "or".In addition, it should be apparent that It is the purpose that words or terms that are using herein and defining not otherwise are merely to illustrate and is non-limiting. The use of any paragraph heading is expected to the understanding for helping article and is not interpreted to limit；With the relevant information of paragraph heading Can occur inside or outside special paragraph.In addition, all disclosure, patents, and patent literature quoted herein are logical Cross reference and this be fully incorporated in it, as individually through reference in conjunction with.This paper and that being incorporated by reference in this way In the case that use between a little documents is inconsistent, in conjunction with citation in use should be considered as benefit herein It fills；For irreconcilable contradiction, it is subject to usage herein.

In manufacturing method described herein, multiple steps can carry out the original without departing from the present invention with random order Reason, except when explicitly pointing out interim or operation order.In addition, specific step can be carried out at the same time, unless explicitly Claim language points out that they are dividually carried out.For example, the step of progress X claimed and progress claimed The step of Y, can simultaneously carry out in single operation, and obtained method will be fallen in method claimed In literal scope.

Term as used herein " about " can be with certain variable pitch on permissible level or range, for example, described In the 10% of numerical value or the scope limitation, in 5% or in 1%.

Term as used herein refers to " substantially " major part, or mainly, such as account at least about 50%, 60%, 70%, 80%, 90%, 95%, 96%, 97%, 98%, 99%, 99.5%, 99.9%, 99.99% or at least about 99.999% or more.

Term as used herein " solvent " refers to can be with the liquid of dissolved solid, liquid or gas.Solvent it is unrestricted Property example is siloxanes, organic compound, water, alcohol, ionic liquid and supercritical fluid.

Term as used herein " standard temperature and pressure (STP) " refers to 0 DEG C and 100KPa.

Term as used herein " polymer " may include copolymer.

Term as used herein " heat exchanger " refers to for heat to be transferred to another device from a medium.It is situated between Matter can be detached by solid wall.The example of heat exchanger includes shell-and-tube formula exchanger, heat-exchangers of the plate type, the friendship of shell-and-plate heat Parallel operation, adiabatic wheel heat exchangers, plate fin type heat exchanger, pillow heat-exchangers of the plate type, fluid heat exchanger, Waste Heat Recovery list Member, dynamic scraped-surface heat exchanger and phase-change heat exchanger.

Term as used herein " sensible heat " refers to the heat by object or thermokinetics systems exchange, wherein the effect exchanged Variation substantially in the temperature of object or system, and seldom mutually fade to no phase transformation.

Term as used herein " latent heat " refers to the heat by object or thermokinetics systems exchange, wherein the effect exchanged Phase transformation substantially in object or system, and seldom it is changed to no temperature change.

Term as used herein " relative viscosity " (RV) refer in capillary viscometer at 25 DEG C measure solution and The ratio of solvent viscosity.In an example, it is 90% formic acid (90 weight % formic acid and 10 weights according to the RV of ASTM D789-06 Measure % water) in 8.4 weight % polyamide solutions in 25 DEG C of viscosity (in terms of centipoise) and 90% formic acid from viscous in 25 DEG C Spend the ratio of (in terms of centipoise).

Term as used herein " saturation temperature " refers in special pressure (for example, in saturation pressure of the temperature) liquid Body boiling is that the temperature of its vapor phase and steam start the temperature for being condensed into its liquid phase.Saturation temperature of the substance in specified pressure Under, when temperature reduces or pressure increases, which will condense.Substance is under the saturation temperature of specified pressure, when temperature increases Or when pressure reduction, boiling is its vapor phase by material.

The present invention relates to being used to prepare at least two heat transmission mediums for transferring heat to tubular reactor The mthods, systems and devices of polyamide.Polyamide can be any appropriate polyamide, such as nylon 6, nylon 7, nylon 11, Buddhist nun Dragon 12, nylon 6,6, nylon 6,9；Nylon 6,10, nylon 6,12, the polyamide (for example, nylon at higher temperature) of partially aromatic or it Copolymer.

The method for making each polyamide

This method may include passing the first flowable heat transmission medium heating to provide the flowable heat of heated first Pass medium.Heating can carry out in any suitable manner.Heating can be in heat exchanger, as in any appropriate heat exchanger It carries out.First flowable heat transmission medium can be located in heating circuit.First flowable heat transmission medium can be in power house Or it is heated in the center heating region in equipment and can be used to heat from level-one heating circuit to one or more two levels Circuit transmission heat is back to power house for reheating later to whole equipment.Two level heating circuit can be used for heating equipment One or more tubular reactors.First flowable heat transmission medium can be fixedness, so that the first flowable heat Transfer medium can be substantially liquid phase before and after heating.

Level-one heating circuit and one or more two level heating circuits can have arbitrary volume suitable relative to each other. Level-one heating circuit can have the volume than two level heating circuit bigger.Level-one heating circuit can have about the same body Product has volume more smaller than two level heating circuit.Level-one heating circuit can be with the pact of the volume of two level heating circuit 0.000,1%-1,000,000% or two level heating circuit volume about 100% to 1,000,000%, or about 0.000, 1% or lower, or about 0.001%, 0.01%, 0.1%, 1%, 5%, 10%, 25%, 50%, 75%, 100%, 125%, 150%, 175%, 200%, 300%, 400%, 500%, 750%, 1000%, 1500%, 2000%, 3000%, 4000%, 5000%, 10,000%, 20,000%, 50,000%, 100,000%, about 500,000%, or about 1,000,000% or more It is high.First flowable heat transmission medium and the heated first flowable heat transmission medium can have to be passed with the second flowable heat Pass medium and any appropriate mass ratio of the heated second flowable heat transmission medium.For example, the first flowable heat is transmitted and is situated between Matter and the mass combination of the heated first flowable heat transmission medium and the second flowable heat transmission medium and heated the The ratio of the mass combination of two flowable heat transmission mediums can be about 0.000,000,1：1 to about 10,000,000：1, about 100：1 To about 100：1, about 0.000,000,1：1 or lower, or about 0.000,1：1,0.001：1,0.01：1,0.1：1,1：1,5：1, 10：1,25：1,50：1,75：1,100：1,125：1,150：1,175：1,200：1,300：1,400：1,500：1,750：1, 1000：1,1500：1,2000：1,3000：1,4000：1,5000：1,10,000：1,20,000：1,50,000：1,100,000: 1,500,000: 1, about 1,000,000：1 or about 10,000,000：1 or higher.

This method may include that heat is transferred to the second flowable heat from the first heated flowable heat transmission medium to pass Medium is passed, to provide heated second flowable heat transmission medium.Heating can carry out in any suitable manner.Heating can To be carried out in heat exchanger, such as any appropriate heat exchanger.Second flowable heat transmission medium can sufficiently be volatilized Property is so that substantially gas phase can be heated to by the first flowable heat transmission medium by it, and allow to it in heat It is condensed to basic liquid phase from the second heated flowable heat transmission medium to the transmittance process of tubular reactor.

First flowable heat transmission medium can remain liquid, while the second flowable heat by heating with hot transmission Transfer medium can become to be gasified and can be condensed when from its transmission heat when heated.In normal temperature and pressure Power, the first flowable heat transmission medium can have the vapour pressure lower than the second flowable heat transmission medium；Alternatively, first can flow Dynamic heat transmission medium can have the vapour pressure higher than the second flowable heat transmission medium.The second flowable heat can be controlled to transmit The pressure of medium is so that it is in required temperature gasification and condenses.Because the first flowable heat transmission medium can heated Liquid is remained later, and the second flowable heat transmission medium can substantially be gasified after heating, it is heated The second flowable heat transmission medium can have vapour pressure more higher than the heated first flowable heat transmission medium.

First flowable heat transmission medium and the second flowable heat transmission medium can all be combustible organic materials, or can be with It all include flammable organic component.Steam and high vapour pressure combustible organic materials are typically carried than the liquid with more low-vapor pressure The risk of catching fire and burn of flammable organic compound bigger.The second heated flowable heat transmission medium can be than heated The first flowable heat transmission medium it is at least one of more flammable and more inflammable.

This method can also include that heat is transferred to tubular reactor from the second heated flowable heat transmission medium.Heat Transmission can carry out in any suitable manner.The transmission of heat can be in heat exchanger, as in any appropriate heat exchanger It carries out.Heat can be transferred to one or more tubular reactors, Yi Jiren from the second heated flowable heat transmission medium The one or more other parts of appliance of selection of land, such as pre-heater, evaporator, polymer reactor, flash vessel, finisher and height Press at least one of kettle.Pre-heater can be any appropriate pre-heater and any appropriate portion that can be with equipment Part connects, such as the pre-heater at least one of evaporator, polymer reactor, flash vessel, finisher and autoclave. Can make the temperature of individual component by the second heated flowable heat transmission medium reach any appropriate temperature or The range of temperature.For example, enough heat can be transferred to evaporator so that the temperature of wherein reaction mixture to be increased to arbitrarily Suitable temperature, such as from about 100-230 DEG C or 100-150 DEG C, or about 100 DEG C or lower, or about 110 DEG C, 120,130,140, 150,160,170,180,190,200,210,220 DEG C or about 230 DEG C or more of temperature.For example, enough heat can be transmitted To reactor the temperature of reaction mixture therein to be increased to any appropriate temperature, such as from about 150-300 DEG C, or about 200- 250 DEG C, or about 215-245 DEG C, or about 150 DEG C or lower, or about 160 DEG C, 170,180,190,200,210,215,220, 225,230,235,240,245,250,260,270,280,290 DEG C or about 300 DEG C or more of temperature.For example, can will be enough Heat be transferred to flash vessel so that the temperature of reaction mixture therein to be increased to any appropriate temperature, such as from about 150-400 DEG C, Or about 250-350 DEG C, or about 250-310 DEG C, or about 200 DEG C or lower, or about 210 DEG C, 220,230,240,250,260, 265,270,275,280,285,290,295,300,305,310,320,330,340 DEG C, or about 350 DEG C or more of temperature.Example Such as, enough heat can be transferred to finisher so that the temperature of reaction mixture therein to be increased to any appropriate temperature Degree, such as from about 150-400 DEG C, or about 250-350 DEG C, or about 250-310 DEG C, or about 200 DEG C or lower, or about 210 DEG C, 220, 230,240,250,260,265,270,275,280,285,290,295,300,305,310,320,330,340 DEG C, or about 350 DEG C or more temperature.

It may include by pipe reaction that heat is transferred to tubular reactor from the second heated flowable heat transmission medium The temperature of device is maintained at any appropriate temperature, such as from about 100 DEG C to about 400 DEG C, 150 DEG C to 350 DEG C, 150 DEG C to 250 DEG C, and 250 DEG C to 350 DEG C, 200 DEG C to 300 DEG C, or about 210 DEG C to 260 DEG C, or about 218 DEG C to about 250 DEG C, or about 100 DEG C, 110,120, 130、140、150、160、170、180、190、200、205、210、215、220、225、230、235、240、245、250、255、 260,265,270,280,290,300,310,320,330,340,350,360,370,380,390 DEG C or about 400 DEG C or more.It will At least one component that heat is transferred to polyamide synthesis system from the second heated flowable heat transmission medium may include by The temperature of polyamide compound in reactor is maintained at any appropriate temperature, such as from about 210 DEG C to 260 DEG C, and 218 DEG C to about 250 DEG C, or about 100 DEG C or lower, or about 110 DEG C, 120,130,140,150,160,170,180,190,200,205,210, 215、220、225、230、235、240、245、250、255、260、265、270、280、290、300、310、320、330、340、 350,360,370,380,390 DEG C or about 400 DEG C or more.

Notwithstanding the heating of unit operation, but it will be appreciated by those of skill in the art that using described herein Conventional method can carry out the cooling of one of one or more unit operations.

Tubular reactor

Tubular reactor can be any appropriate tubular reactor that can heat polyamide reaction mixture.Tubular type is anti- Answer device that can have any appropriate shape and design.Tubular reactor may include having chuck to transfer heat on it The cylindrical tube of reactor.Heat transfer fluid can flow through the chuck of reactor.

The schematic diagram of suitable tubular reactor 1 is presented in Fig. 1.Tubular reactor 1 includes entrance 2 and outlet 3.Tubular type Reactor 1 includes straight portion 4 and bending section 5.Tubular reactor includes floss hole 6.

Tubular reactor can have any appropriate length, the length such as between straight portion and the entrance and outlet of bending section Degree.Tubular reactor can have about 50 to 300 meters, or about 75 to 125 meters, or about 90 to 110 meters, or about 50 meters or smaller, Or about 60 meters, 70,80,85,90,95,100,105,110,115,120,130,140,150,160,170,180,190,200, 225, the length of 250,275 or about 300 meters or bigger.

Tubular reactor can have any appropriate internal diameter such as straight portion and bending section.Internal diameter can be from the one of reactor End to other end variation or internal diameter can be constant.For example, internal diameter can be from the entrance of tubular reactor to pipe reaction The outlet of device expands.Tubular reactor can have about 10cm to 80cm, or about 25cm is to about 60cm, or about 35cm to 50cm, Or about 10cm or lower, or about 15cm, 20,25,30,35,36,37,38,39,40,41,42,43,44,45,46,47,48, 49, the internal diameter of 50,55,60,65,70,75cm or about 80cm or bigger.If tubular reactor includes chuck, chuck can be with Such as be more than 1-50cm of internal diameter with any appropriate overall diameter, or about 1 to 25cm, or be more than internal diameter about 1cm or lower, or surpasses Cross internal diameter about 2,4,6,8,10,12,14,16,18,20,22,24,26,28,30,32,34,36,38,40,42,44,46,48 or About 50cm or bigger.

Tubular reactor can expand with constant internal diameter or diameter from the entrance of reactor to outlet, such as Linear expansion or non-linear expansion.Diameter can fully expand so that when using reactor from the entrance of reactor to Outlet keeps substantial constant pressure.Diameter can expand so that pressure is reduced from entrance to outlet when using reactor. The expansion rate of tubular reactor can be sufficient to make the heat applied to reaction mixture, from reaction mixture by gasifying and discharging The amount of the water of removal, and the combination of pressure in the reaction mixture of the given position along length help to maintain reaction mixing The flowing of object orientating reaction device outlet and the generation or accumulation for reducing or minimizing gel or other impurities.The internal diameter of reactor About 2.5cm can be expanded with the length of every about 6.25m to about 750m, often the length of about 22.5m to about 550m expands about 2.5cm, often The length of 22.5m to about 110m expands about 2.5cm, or the often length of about 6m or lower, or about 8m, 10,15,20,25,30,35, 40、45、50、55、60、65、70、75、80、85、90、95、100、105、110、120、125、150、175、200、225、250、 275, the length of 300,325,350,375,400,425,450,475,500,525,550,600,650,700 or about 750m expands About 2.5cm.

Tubular reactor can have any appropriate length/diameter (L/D, for example, length divided by average diameter).Example Such as, the length/diameter (L/D) of tubular reactor can be about 50 to 2500, or about 100 to 500, or about 230 to 270, or about 50 or lower, or about 75,100,125,150,175,200,210,220,230,235,240,245,250,255,260,265, 270,280,290,300,400,500,600,700,800,900,1000,1250,1500,1750,2000,2250 or about 2500 Or higher.

Tubular reactor may include floss hole along its length.Tubular reactor may include any appropriate number and class The floss hole of type, so that can discharge vapor from floss hole.Tubular reactor may include any appropriate along its length The floss hole of number.For example, tubular reactor can have about 5 to 50 floss holes, or about 10 to 25 discharges along its length Mouthful, or about 5 or less floss holes, or along its length about 6,7,8,9,10,11,12,13,14,15,16,17,18,19,20,21, 22,23,24,25,30,35, about 45 floss holes or about 50 or more floss hole.

The range that floss hole can leave any appropriate average distance of adjacent floss hole in tubular reactor is deposited ?.For example, tubular reactor can be along often about 2 meters to about 15 meters of the length of tubular reactor, the length along tubular reactor is every About 3 meters to about 9 meters, or often about 5 to about 8 meters there are average about 1 floss hole, or often about 2 meters or less, or about 3 meters, 4,5,6, 7, there is average about 1 floss hole 8,9,10,11,12,13,14 or about 15 meters or more.

Tubular reactor can be along its length with equispaced amount any appropriate between floss hole.For example, tubular type is anti- Answer device that can be averaged about 2 meters to about 15 meters in being spaced apart for floss hole along the length of tubular reactor, or about 3 meters to about 9 meters, or Person is along about 5 to about 8 meters of length, or about 2 meters or lower, or along about 3 meters of length, 4,5,6,7,8,9,10,11,12,13,14, or It is about 15 meters or more average.

Tubular reactor can the floss hole with certain amount and distribution so that in tubular reactor vapor speed Degree is no more than any appropriate maximum value.For example, the number of floss hole and distribution can be sufficient to make the water in tubular reactor The speed of steam is no more than about 0.5m/s to about 400m/s, 1-200m/s, 2-100m/s, 4-50m/s or about 0.5m/s, or more It is low, or about 1m/s, 2,3,4,5,15,10,20,25,30,35,40,45,50,55,60,65,70,75,80,85,90,95, 100,125,150,175,200,250,300m/s, or about 400m/s or higher.

Tubular reactor can have any appropriate flow velocity by polymer material therein.For example, flow velocity can be with 1L/ minutes to about 1,000,000L/ minute, or about 10L/ minutes to about 100,000L/ minutes, or about 1L/ minutes hereinafter, 10L/ minutes, 20,30,40,50,60,70,80,90,100,125,150,175,200,225,250,275,300,350,400, 450,500,600,700,800,900,1,000,2,500,5,000,10,000,50,000,100,000,500,000 or about 1, 000,000L/ minutes or more.Paradigmatic system including tubular reactor can manufacture polymer with any appropriate rate, such as from about 1L/ minutes to about 1,000,000L/ minute, or about 10L/ minutes to about 100,000L/ minutes, or about 1L/ minutes or lower, 10L/ minutes, 20,30,40,50,60,70,80,90,100,125,150,175,200,225,250,275,300,350,400, 450,500,600,700,800,900,1,000,2,500,5,000,10,000,50,000,100,000,500,000 or about 1, 000,000L/ minute or higher.

Tubular reactor can the floss hole with certain amount and distribution so that tubular reactor with any appropriate The F factors.Floss hole can be connected to suitable floss hole pipeline.This method may include injecting water into floss hole pipeline. Water can be injected into each floss hole with any appropriate rate.

The present invention tubular reactor any appropriate time can be run between closing and cleaning with remove gel or Other pollutants.For example, this method can in the case that be not related to stopped pipe type reactor for it is clean carry out at least about 1 to 7 years, 2 to 5 years, or about 2.3 to 3 years, or about 3 years.

Tubular reactor can have the flow pattern of any appropriate reaction mixture and vapor wherein.For example, Tubular reactor can mainly have annularly flow (for example, the interior side contacts of most of liquid and reactor tube, at the same gas and Vapor mainly travels downwardly at the center of reactor tube).In some instances, tubular reactor can have piston flow (example Substantially continuous liquid column point is embroidered with substantially continuous gas and vapor column in pipe in such as pipe), and other flowings Mode (for example, the bottom that liquid rests on pipe is formed close to semicylinder, while gas and vapor rest on the top of pipe). Can occur any appropriate combination of annular flow, piston flow and other flow patterns in tubular reactor.

In multiple examples, reactor can heat reaction mixture and by water from its evaporation, and balance is advanced further towards Polyamide products.Reaction mixture can be heated to any appropriate temperature, such as from about 150-400 DEG C in reactor, or about 250-350 DEG C, or about 250-310 DEG C, or about 200 DEG C or lower, or about 210 DEG C, 220,230,240,250,260,265, 270,275,280,285,290,295,300,305,310,320,330,340 DEG C or about 350 DEG C or higher.Leave reactor Reaction mixture can be with the water of any appropriate weight percent, such as from about 0.000,1 weight % to 20 weight %, and 0.001 To 15 weight %, or about 0.01 to 15 weight %, or about 0.000,1 weight % or lower, or about 0.001 weight %, 0.01, 0.05、0.06、0.07、0.08、0.09、0.1、0.2、0.3、0.4、0.5、0.6、0.7、0.8、0.9、1.0、1.2、1.4、1.6、 1.8,2,3,4,5,6,7,8,9,10,11,12,13,14,15,16,17,18,19 weight % or about 20 weight % or higher.

It is used to prepare the system and device of polyamide

The present invention can provide the system for being used to prepare polyamide.The system can carry out method described herein Any appropriate system.The system includes heater.Heater can be any appropriate heater.Heater can be matched It is set to the first flowable heat transmission medium heating to provide heated first flowable heat transmission medium.

System may include first heat exchanger.First heat exchanger can be any appropriate heat exchanger.First heat Exchanger is configurable to transmit from the first heated flowable heat transmission medium hot flowable to provide heated second Heat transmission medium.

The system may include second heat exchanger.Second heat exchanger can be any appropriate heat exchanger.Second Heat exchanger be configurable to by heat from the second heated flowable heat transmission medium be transferred to polyamide synthesis system to A few tubular reactor.

The present invention can provide a kind of device being used to prepare polyamide.The system can be can carry out it is described herein Any appropriate device of method.The device may include heater.Heater can be any appropriate heater.Heater It is configurable to the first flowable heat transmission medium heating to provide heated first flowable heat transmission medium.

The device may include first heat exchanger.First heat exchanger can be any appropriate heat exchanger.First Heat exchanger is configurable to flow to provide heated second from the first heated flowable heat transmission medium transmission heat Dynamic heat transmission medium.

The device may include second heat exchanger.Second heat exchanger can be any appropriate heat exchanger.Second Heat exchanger be configurable to by heat from the second heated flowable heat transmission medium be transferred to polyamide synthesis system to A few tubular reactor.

The embodiment that Fig. 2 illustrates the system for being used to prepare polyamide or device 10.The system or device may include Heater 15.Heater heats the first flowable heat transmission medium 20 being arranged in level-one heating circuit 25, is added with providing The first flowable heat transmission medium 30 that heat is crossed.The system or device may include first heat exchanger 35.First heat exchanger Heat is transferred to second be arranged in two level heating circuit 45 by 35 from the first heated flowable heat transmission medium 30 to flow Dynamic heat transmission medium 40, to provide the flowable heat transmission medium of heated second 50.By the first flowable heat transmission medium 20 (for example, used first flowable heat transmission medium) transmission is back to heater 15 for reheating.System or device can be with Including second heat exchanger 55.Heat is transferred to poly- by second heat exchanger 55 from the second heated flowable heat transmission medium 50 The tubular reactor of amide synthesis system is integrated with second heat exchanger 55.By 40 (example of the second flowable heat transmission medium Such as, the used second flowable heat transmission medium) it transmits and is back to second heat exchanger 35 for reheating.System or device Can be using any appropriate mode heat transmission medium is sent to another from a position, such as pumping or convection current.

Fig. 3 examples are used to prepare the system of polyamide or the embodiment of device 21.The system or device may include adding Hot device 15.Heater 15 heats the first flowable heat transmission medium 20 being arranged in level-one heating circuit 25, is added with providing The first flowable heat transmission medium 30 that heat is crossed.The system or device may include first heat exchanger 35.First heat exchanger Heat is transferred to second be arranged in two level heating circuit 45 by 35 from the first heated flowable heat transmission medium 30 to flow Dynamic heat transmission medium 40, to provide the flowable heat transmission medium of heated second 50.The system or device may include second Heat exchanger 55.Heat is transferred to polyamide synthesis by second heat exchanger 55 from the second heated flowable heat transmission medium 50 The tubular reactor of system is integrated with second heat exchanger 55.By the second flowable heat transmission medium 40 (for example, using The second flowable heat transmission medium) transmit and be back to second heat exchanger 35 for reheating.Heated first can be flowed Dynamic heat transmission medium 30 is transferred to third heat exchanger 36.Third heat exchanger 36 passes heat from the first heated flowable heat It passs medium 30 and is transferred to the flowable heat transmission medium 41 of second be arranged in two level heating circuit 46, to provide heated Two flowable heat transmission mediums 51.The system or device may include the 4th heat exchanger 56.4th heat exchanger 56 by heat from The second heated flowable heat transmission medium 51 is transferred at least one portion for accommodating polyamide of polyamide synthesis system Part can be integrated such as salt pond (salt strike), evaporator, reactor or flash vessel with the 4th heat exchanger 56.By The transmission of two flowable heat transmission mediums 41 (for example, used second flowable heat transmission medium) is back to third heat exchanger 36 for handling.The transmission of first flowable heat transmission medium 20 (for example, used first flowable heat transmission medium) is returned Heater 15 is back to for reheating.

Although the exemplary embodiments of Fig. 3 are by first heat exchanger 35 and the series connection of third heat exchanger 36 so that third Heat exchanger 36 the first heated flowable heat transmission medium 30 transfer heat to the second flowable heat transmission medium 40 it The first heated flowable heat transmission medium 30 is received afterwards, and the invention also includes handed between level-one and two level heating circuit The heat exchanger of heat exchange is arranged in parallel.Such as in one embodiment, third heat exchanger 36 can be by heated One flowable heat transmission medium is in the first heating circuit in the used first flowable heat transmission medium from heat exchanger 35 The point of the upstream of return takes out, and transmits some heat in first heat exchanger 35 so that third heat exchanger does not take out To the first flowable heat transmission medium of the second flowable heat transmission medium 40.

First flowable heat transmission medium

In this method, system or device, the first flowable heat transmission medium can be that any appropriate flowable heat passes Pass medium.First flowable heat transmission medium may include having to constitute suitable in method described herein, system and dress Set one or more organic compounds of the feature of the middle flowable heat transmission medium of first used.First flowable heat, which is transmitted, to be situated between Matter can be, for example, water, polyethylene glycol, polypropylene glycol, mineral oil, silicone oil, diphenyl ether, biphenyl,Board At least one of heat transfer fluid and DOWTHERMTM board heat transfer fluids.First flowable heat transmission medium can be example Such as,Board heat transfer fluid, such asVLT is (for example, hexahydrotoluene, trimethyl Pentane),D-12 is (for example, C_10-13Alkane, for example, isoalkane),LT (examples Such as, diethylbenzene),XP (for example, paraffin oil (white petroleum mineral oil)),55 (for example, C14-30 alkylaryl compounds),59 (for example, ethyl two Diphenylphosphino ethane, diphenylethane, diethyl diphenylethane, ethylbenzene polymer),62 (for example, two is different Pentylbiphenyl, tri isopropyl biphenyl),VP-3 (for example, cyclohexyl benzene, dicyclohexyl),66 (for example, terphenyl (ortho-terphenyl, meta-terphenyl, para-terpheny), the terphenyl of hydrogenation, part The quaterphenyl of hydrogenation, partially hydrogenated more advanced polyphenyl),72 (for example, diphenyl ether, terphenyl, connection Benzene, phenanthrene),VP-1 (for example, diphenyl ether, biphenyl),FF is (for example, vinylation Benzene) at least one of.First flowable heat transmission medium may include, for example, trimethylpentane, C_10-13Alkane, C_10-13 Isoalkane, C_14-30Alkylaryl compounds, diethylbenzene, the benzene of vinylation, cyclohexyl benzene, C_14-30Alkylbenzene, paraffin oil, ethyl Diphenylethane, diphenylethane, diethyl diphenylethane, diphenyl ether (diphenyl ether), diphenyl ether (diphenyl Oxide), ethylbenzene polymer, biphenyl, inorganic salts, diisopropyl biphenyl, tri isopropyl biphenyl, hexahydrotoluene, dicyclohexyl, Terphenyl, the terphenyl of hydrogenation, partially hydrogenated quaterphenyl, partially hydrogenated more advanced polyphenyl, diphenyl ether and phenanthrene, diarylide Close object, tri-aryl compounds, diaryl ether, triaryl ether, alkylaryl compounds, alkylaryl compounds, alkyl diaryl Compound or combination thereof.

First flowable heat transmission medium can have any appropriate temperature.For example, the first flowable heat transmission medium Can be about 20 DEG C to 400 DEG C, or about 50 DEG C to 350 DEG C, 100 DEG C to 300 DEG C, 100 DEG C to 200 DEG C, 200 DEG C to 250 DEG C, or About 250 DEG C to 300 DEG C, or about 20 DEG C or lower, or about 30 DEG C, 40,50,60,70,80,90,100,110,120,130,140, 150、160、170、180、190、200、210、220、230、240、250、260、270、280、290、300、310、320、330、 340,350,360,370,380,390 DEG C or about 400 DEG C or more.First flowable heat transmission medium can have any appropriate Phase, such as gas phase, liquid phase or its any appropriate combination.For example, the first flowable heat transmission medium can be pact by weight 60% or lower, or about 70%, 80,85,90,95,96,97,98 or about 99% with liquid phase.First flowable heat transmission medium It can be substantially liquid phase.

The first heated flowable heat transmission medium can have any appropriate temperature.For example, heated first Flowable heat transmission medium can be about 100 DEG C to 500 DEG C, 100 DEG C to 400 DEG C, 100 DEG C to 300 DEG C, 100 DEG C to 200 DEG C, 200 DEG C to 250 DEG C, 250 DEG C to 300 DEG C, 300 DEG C to 350 DEG C, 350 DEG C to 400 DEG C, 400 DEG C to 500 DEG C, 280 DEG C to 400 DEG C or 330 DEG C to 350 DEG C, or about 100 DEG C or lower, or about 110 DEG C, 120,130,140,150,160,170,180,190, 200、210、220、230、240、250、260、270、280、290、300、310、320、330、340、350、360、370、380、 390 DEG C or about 400 DEG C or more.The first heated flowable heat transmission medium can have any appropriate phase, such as gas phase, liquid Phase or its any appropriate combination.For example, the first heated flowable heat transmission medium can be about 60% by weight Or it is lower, or about 70%, 80,85,90,95,96,97,98 or about 99% with liquid phase.The first heated flowable heat is transmitted Medium can be substantially liquid phase.

During heating the first flowable heat transmission medium, the first flowable heat transmission medium can be protected substantially It holds as liquid (for example, not occurring the gasification of the first flowable heat transmission medium substantially).In the first flowable heat transmission medium Heating during, the heat for being transferred to the first flowable heat transmission medium may include substantially all sensible heat.For example, will During first flowable heat transmission medium heating, the heat for being transferred to the first flowable heat transmission medium may include arbitrary conjunction The sensible heat of suitable percentage, such as from about 60% or lower, or about 70%, 80,85,90,95,96,97,98 or about 99% or more sensible heat, And remaining part is latent heat (for example, heat of gasification).

In the process that heat is transferred to the second flowable heat transmission medium from the first heated flowable heat transmission medium In, the heated first flowable heat transmission medium can be substantially maintained as liquid.It is passed for example, not occurring the first flowable heat Pass the freezing of medium.Heat is being transferred to the second flowable heat transmission medium from the first heated flowable heat transmission medium In the process, do not occur the condensation of the flowable heat transmission medium of heated first substantially.For example, if heated first can It is substantially liquid phase to flow heat transmission medium, is not condensed, or the only heated first flowable heat transmission medium lacks The gaseous component of amount condenses.It is situated between heat to be transferred to the second flowable heat and transmit from the first heated flowable heat transmission medium During matter, the heat transmitted from the first heated flowable heat transmission medium may include substantially all sensible heat.For example, During heat is transferred to the second flowable heat transmission medium from the first heated flowable heat transmission medium, from heating The heat that the first flowable heat transmission medium crossed transmits may include the sensible heat of any appropriate percentage, and such as from about 60% or lower, Or about 70%, 80,85,90,95,96,97,98 or about 99% or more aobvious heat, and remaining part is latent heat (for example, gasification Heat).

First flowable heat transmission medium and the heated first flowable heat transmission medium can be all disposed within first and add In hot loop.Heat is transferred to the second flowable heat transmission medium from the first heated flowable heat transmission medium to be provided Used first flowable heat transmission medium.This method may include by the used first flowable heat transmission medium cycle It is back to the heating of the first flowable heat transmission medium.First heating circuit can be by the first heat transfer material in a device The level-one recycled between center heating location and the one or more secondary circuits for accommodating the second flowable heat transmission medium is returned Road or the first heating circuit can be for for example, heating all or fewer than accommodate the second flowable heat transmission medium The primary circuit of secondary circuit.

This method may include controlling the pressure of the first flowable heat transmission medium and to control heated first flowable At least one of temperature of heat transmission medium.It controls the pressure of the first flowable heat transmission medium and controls heated first The pressure of flowable heat transmission medium may include the pressure controlled in the first heating circuit.It is arbitrary conjunction that pressure can be controlled Suitable pressure, such as from about 50KPa are to 1,000,000KPa, 100KPa to 500,000KPa or 500KPa is to 250,000KPa, or about 50KPa or lower, or about 100KPa, 500KPa, 1MPa, 2MPa, 3,4,5,6,7,8,9,10,12.5,15,17.5,20,25, 30,35,40,45,50,60,70,80,90,100,125,150,175,200MPa or about 250MPa or higher.In some examples In, it is any appropriate temperature that can control saturation temperature, and such as from about 100 DEG C to 500 DEG C, 100 DEG C to 400 DEG C, 100 DEG C are extremely 300 DEG C, 100 DEG C to 200 DEG C, 200 DEG C to 250 DEG C, 250 DEG C to 300 DEG C, 300 DEG C to 350 DEG C, 350 DEG C to 400 DEG C, 400 DEG C To 500 DEG C, 210 DEG C to 350 DEG C or 260 DEG C to 300 DEG C, or about 100 DEG C or lower, or about 110 DEG C, 120,130,140, 150、160、170、180、190、200、210、220、230、240、250、260、270、280、290、300、310、320、330、 340,350,360,370,380,390 DEG C or about 400 DEG C or higher.The highest temperature of the first heated flowable heat transmission medium Degree can be in any appropriate range of the saturation temperature of the first heated flowable heat transmission medium, such as heated About 0-100 DEG C of the saturation temperature of first flowable heat transmission medium, in the range of 0-60 DEG C, about 0-40 DEG C, or about 0 DEG C, 1,2,3,4,5,10,15,20,25,30,35,40,50,60,70,80,90, or in about 100 DEG C.In each embodiment, In the example of the gasification including the first heat transmission medium, the first flowable heat transmission medium and heated can be similarly controlled The first flowable heat transmission medium pressure to control the saturation temperature of the first flowable heat transmission medium.Control first can The temperature of heat transmission medium gasification and the temperature of the heated first flowable heat transmission medium condensation are flowed (for example, saturation temperature Degree) temperature of the flowable heat transmission medium of heated second can be controlled.

First flowable heat transmission medium and the heated first flowable heat transmission medium can independently have arbitrary Suitable vapour pressure, such as from about 50KPa to 1,000,000KPa, 100KPa to 500,000KPa or 500KPa to 250,000KPa, Or about 50KPa or lower, or about 100KPa, 500KPa, 1MPa, 2MPa, 3,4,5,6,7,8,9,10,12.5,15,17.5,20, 25,30,35,40,45,50,60,70,80,90,100,125,150,175,200MPa, or about 250MPa or higher.

First flowable heat transmission medium and the heated first flowable heat transmission medium can have any appropriate Thermal capacitance.For example, at about 100 DEG C or lower, or about 110 DEG C, 120,130,140,150,160,170,180,190,200, 210、220、230、240、250、260、270、280、290、300、310、320、330、340、350、360、370、380、390 DEG C, or can have in about 400 DEG C or higher, the first flowable heat transmission medium and the heated first flowable heat transmission medium There is about 0.2KJ/Kg DEG C to about 8.5KJ/Kg DEG C, about 1KJ/Kg DEG C to about 4KJ/Kg DEG C, about 0.2KJ/Kg DEG C or lower, or about 0.5KJ/Kg DEG C, 1,1.1,1.2,1.3,1.4,1.5,1.6,1.7,1.8,1.9,2,2.1,2.2,2.3,2.4,2.5,2.6, 2.7,2.8,2.9,3,3.1,3.2,3.5,4,4.5,5,5.5,6,6.5,7,7.5,8KJ/Kg DEG C, or about 8.5KJ/Kg DEG C or more High thermal capacitance.

First flowable heat transmission medium can be with any appropriate rate loop, such as from about 1L/ minutes to about 1, and 000, 000L/ minutes, or about 10L/ minutes to about 100,000L/ minutes, or about 1L/ minutes or lower, 10L/ minutes, 20,30,40, 50、60、70、80、90、100、125、150、175、200、225、250、275、300、350、400、450、500、600、700、 800,900,1,000,2,500,5,000,10,000,50,000,100,000,500,000 or about 1,000,000L/ minutes or Higher.

Second flowable heat transmission medium

In method, system or device, the second flowable heat transmission medium can be that any appropriate flowable heat is transmitted Medium.Second flowable heat transmission medium may include having to constitute suitable in method described herein, system and device One or more organic compounds of the feature of the middle flowable heat transmission medium of second used.Second flowable heat transmission medium It can be such as at least one of the following：Water, polyethylene glycol, polypropylene glycol, mineral oil, silicone oil, diphenyl ether, biphenyl, Terphenyl,Board heat transfer fluid and DOWTHERM^TMBoard heat transfer fluid.Second flowable heat, which is transmitted, to be situated between Matter may include, for example, DOWTHERM^TMBoard heat transfer fluid, such as at least one of the following：DOWTHERM^TM A (for example, diphenyl ether and biphenyl, for example, the eutectic mixture of diphenyl ether and biphenyl, such as 26.5 weight % diphenyl and 73.5 Weight % diphenyl ether), DOWTHERM^TMG (for example, biaryl compound, tri-aryl compounds, diaryl and triaryl ether), DOWTHERM^TMJ (for example, alkylaryl compounds), DOWTHERM^TMMX (for example, alkylaryl compounds), DOWTHERM^TM Q (for example, diphenylethane, alkylaryl compounds), DOWTHERM^TMRP (for example, diaryl alkane based compound) and DOWTHERM^TMT is (for example, C_14-30Alkylbenzene).Second flowable heat transmission medium may include, for example, trimethylpentane, C_10-13Alkane, C_10-13Isoalkane, C_14-30Alkylaryl compounds, diethylbenzene, the benzene of vinylation, cyclohexyl benzene, C_14-30Alkyl Benzene, paraffin oil, ethyl diphenyl ethane, diphenylethane, diethyl diphenylethane, diphenyl ether, dipheny oxide, ethylbenzene polymerization Object, biphenyl, inorganic salts, diisopropyl biphenyl, tri isopropyl biphenyl, hexahydrotoluene, dicyclohexyl, terphenyl, hydrogenation three Biphenyl, partially hydrogenated quaterphenyl, partially hydrogenated more advanced polyphenyl, diphenyl ether and phenanthrene, biaryl compound, triaryl chemical combination Object, diaryl ether, triaryl ether, alkylaryl compounds, alkylaryl compounds, diaryl alkane based compound or they Combination.

Second flowable heat transmission medium can have any appropriate temperature.For example, the second flowable heat transmission medium Can be about 20 DEG C to 400 DEG C, or about 50 DEG C to 350 DEG C, 100 DEG C to 300 DEG C, 100 DEG C to 200 DEG C, 200 DEG C to 250 DEG C, or About 250 DEG C to 300 DEG C, or about 20 DEG C or lower, or about 30 DEG C, 40,50,60,70,80,90,100,110,120,130,140, 150、160、170、180、190、200、210、220、230、240、250、260、270、280、290、300、310、320、330、 340,350,360,370,380,390 DEG C, or about 400 DEG C or higher.Second flowable heat transmission medium can have arbitrary conjunction Suitable phase, such as gas phase, liquid phase or their any appropriate combinations.For example, the second flowable heat transmission medium can be with weight About 60% or less of meter, or about 70%, 80,85,90,95,96,97,98 or about 99% or more gas phase.Second is flowable Heat transmission medium can be substantially gas phase.

The second heated flowable heat transmission medium can have any appropriate temperature.For example, heated second Flowable heat transmission medium can be about 100 DEG C to 500 DEG C, 100 DEG C to 400 DEG C, 100 DEG C to 300 DEG C, 100 DEG C to 200 DEG C, 200 DEG C to 250 DEG C, 250 DEG C to 300 DEG C, 300 DEG C to 350 DEG C, 350 DEG C to 400 DEG C, 400 DEG C to 500 DEG C, 210 DEG C to 350 DEG C or 260 DEG C to 300 DEG C, or about 100 DEG C or lower, or about 110 DEG C, 120,130,140,150,160,170,180,190, 200、210、220、230、240、250、260、270、280、290、300、310、320、330、340、350、360、370、380、 390 DEG C or about 400 DEG C or higher.The second heated flowable heat transmission medium can have any appropriate phase, as gas phase, Liquid phase or their any appropriate combinations.For example, the second heated flowable heat transmission medium can be pact by weight 60% or less, or about 70%, 80,85,90,95,96,97,98 or about 99% or more gas phase.Heated second can flow Dynamic heat transmission medium can be substantially gas phase.

In the process that heat is transferred to the second flowable heat transmission medium from the first heated flowable heat transmission medium In, the second flowable heat transmission medium can essentially become gas (for example, the second flowable heat transmission medium can be basic Upper all gasifications).Heat is being transferred to the second flowable heat transmission medium from the first heated flowable heat transmission medium In the process, the heat for being transferred to the second flowable heat transmission medium may include substantially all latent heat (for example, heat of gasification).Example Such as, it during heat is transferred to the second flowable heat transmission medium from the first heated flowable heat transmission medium, passes The heat for being handed to the second flowable heat transmission medium may include the latent heat of any appropriate percentage, and such as from about 60% to 100%, 70% to 100%, 80% to 100%, 90% to 100%, or about 60% or lower, or about 65%, 70,75,80,85,90, 95,96,97,98% or about 99% or higher latent heat (for example, heat of gasification), and remaining part is sensible heat.

In the tubular reactor that heat is transferred to polyamide synthesis system from the second heated flowable heat transmission medium During, the second heated flowable heat transmission medium can be substantially condensed into liquid.For example, can will be heated The second flowable heat transmission medium substantially all of vapor condensation.Heat is being transmitted from the second heated flowable heat During medium is transferred to the tubular reactor of polyamide synthesis system, the heat transmitted from the second flowable heat transmission medium can To include substantially all latent heat (for example, heat of gasification).Heat is being transferred to from the second heated flowable heat transmission medium During the tubular reactor of polyamide synthesis system, the heat transmitted from the second flowable heat transmission medium may include arbitrary The latent heat of suitable percentage, such as from about 60% to 100%, 70% to 100%, 80% to 100%, 90% to 100%, or about 60% or lower, or about 65%, 70,75,80,85,90,95,96,97,98% or about 99% or higher latent heat (for example, gasification Heat), and remaining part is sensible heat.

This method may include controlling the pressure of the second flowable heat transmission medium and to control heated second flowable The pressure of heat transmission medium is to control the temperature of the second flowable heat transmission medium gasification, and heated second flowable of control The temperature of heat transmission medium condensation.Second heat transmission medium and the second heated heat transmission medium can be arranged in the second heating In circuit.The tubular reactor that heat is transferred to polyamide synthesis system from the second heated flowable heat transmission medium can be with Used second flowable heat transmission medium is provided.This method may include by the used second flowable heat transmission medium It is recycled back in the transmission of the heat from the first heated flowable heat transmission medium.

It controls the pressure of the second flowable heat transmission medium and controls the pressure of the second heated flowable heat transmission medium Power may include the pressure controlled in the second heating circuit.It is any appropriate pressure that pressure can be controlled, and such as from about 50KPa is extremely 1,000,000KPa, 100KPa are to 500,000KPa or 500KPa to 250,000KPa, or about 50KPa or lower, or about 100KPa、500KPa、1MPa、2MPa、3、4、5、6、7、8、9、10、12.5、15、17.5、20、25、30、35、40、45、50、 60,70,80,90,100,125,150,175,200MPa or about 250MPa or higher.It in some instances, can be by saturation temperature Degree control be any appropriate temperature, such as from about 100 DEG C to 500 DEG C, 100 DEG C to 400 DEG C, 100 DEG C to 300 DEG C, 100 DEG C to 200 DEG C, 200 DEG C to 250 DEG C, 250 DEG C to 300 DEG C, 300 DEG C to 350 DEG C, 350 DEG C to 400 DEG C, 400 DEG C to 500 DEG C, 210 DEG C are extremely 350 DEG C or 260 DEG C to 300 DEG C, or about 100 DEG C or lower, or about 110 DEG C, 120,130,140,150,160,170,180, 190、200、210、220、230、240、250、260、270、280、290、300、310、320、330、340、350、360、370、 380,390 DEG C or about 400 DEG C or higher.The maximum temperature of the second heated flowable heat transmission medium can be heated In any appropriate range of the saturation temperature of second flowable heat transmission medium, such as transmits and be situated between in the second heated flowable heat About 0-100 DEG C of the saturation temperature of matter, in the range of 0-60 DEG C, about 0-40 DEG C, or about 0 DEG C, 1,2,3,4,5,10,15,20, 25, in the range of 30,35,40,50,60,70,80,90, or about 100 DEG C.In each embodiment, passed including the first heat In the example for passing the gasification of medium, the first flowable heat transmission medium and the heated first flowable heat can be similarly controlled The pressure of transfer medium is to control the saturation temperature of the first flowable heat transmission medium.

Control temperature and the heated second flowable heat transmission medium condensation of the second flowable heat transmission medium gasification Temperature (for example, saturation temperature) can control polyamide synthesis system tubular reactor temperature.By control pressure, and It, can be by the temperature of the tubular reactor of polyamide synthesis system and to the saturation temperature of the second flowable heat transmission medium of control Degree control be any appropriate temperature, such as from about 100 DEG C to 500 DEG C, 100 DEG C to 400 DEG C, 100 DEG C to 300 DEG C, 100 DEG C to 200 DEG C, 200 DEG C to 250 DEG C, 250 DEG C to 300 DEG C, 300 DEG C to 350 DEG C, 350 DEG C to 400 DEG C, 400 DEG C to 500 DEG C, 210 DEG C are extremely 350 DEG C or 260 DEG C to 300 DEG C, or about 100 DEG C or lower, or about 110 DEG C, 120,130,140,150,160,170,180, 190、200、210、220、230、240、250、260、270、280、290、300、310、320、330、340、350、360、370、 380,390 DEG C or about 400 DEG C or higher.

Second flowable heat transmission medium and the heated second flowable heat transmission medium can independently have arbitrary Suitable vapour pressure, such as from about 50KPa to 1,000,000KPa, 100KPa to 500,000KPa or 500KPa to 250,000KPa, Or about 50KPa or lower, or about 100KPa, 500KPa, 1MPa, 2MPa, 3,4,5,6,7,8,9,10,12.5,15,17.5,20, 25,30,35,40,45,50,60,70,80,90,100,125,150,175,200MPa, or about 250MPa or higher.

Second flowable heat transmission medium and the heated second flowable heat transmission medium can have any appropriate Thermal capacitance.For example, at about 100 DEG C or lower, or about 110 DEG C, 120,130,140,150,160,170,180,190,200, 210、220、230、240、250、260、270、280、290、300、310、320、330、340、350、360、370、380、390 DEG C, or can have in about 400 DEG C or higher, the second flowable heat transmission medium and the heated second flowable heat transmission medium There is about 0.2KJ/Kg DEG C to about 8.5KJ/Kg DEG C, about 1KJ/Kg DEG C to about 4KJ/Kg DEG C, about 0.2KJ/Kg DEG C or lower, or about 0.5KJ/Kg DEG C, 1,1.1,1.2,1.3,1.4,1.5,1.6,1.7,1.8,1.9,2,2.1,2.2,2.3,2.4,2.5,2.6, 2.7,2.8,2.9,3,3.1,3.2,3.5,4,4.5,5,5.5,6,6.5,7,7.5,8KJ/Kg DEG C, or about 8.5KJ/Kg DEG C or more High thermal capacitance.

Between heated the first flowable heat transmission medium and the temperature of the heated second flowable heat transmission medium Difference can be any appropriate difference；For example, the difference can be about 0-300 DEG C, and 0-200 DEG C, 0-100 DEG C, 0-60 DEG C, about 0-40 DEG C, or about 0 DEG C, 1,2,3,4,5,10,15,20,25,30,35,40,50,60,70,80,90,100,110, 120,130,140,150,160,170,180,190,200,210,220,230,240,250,260,270,280,290 DEG C or about 300 DEG C or higher.Difference between first flowable heat transmission medium and the temperature of the heated first flowable heat transmission medium It not and the difference between the second flowable heat transmission medium and the temperature of the heated second flowable heat transmission medium, can To be any appropriate difference；For example, the difference can be independently about 0-300 DEG C, and 0-200 DEG C, 0-100 DEG C, 0-60 DEG C, About 0-40 DEG C, or about 0 DEG C, 1,2,3,4,5,10,15,20,25,30,35,40,50,60,70,80,90,100,110,120, 130,140,150,160,170,180,190,200,210,220,230,240,250,260,270,280,290 DEG C or about 300 DEG C or higher.

Second flowable heat transmission medium can be with any appropriate rate loop, such as from about 1L/ minutes to about 1, and 000, 000L/ minutes, or about 10L/ minutes to about 100,000L/ minutes, or about 1L/ minutes or lower, 10L/ minutes, 20,30,40, 50、60、70、80、90、100、125、150、175、200、225、250、275、300、350、400、450、500、600、700、 800,900,1,000,2,500,5,000,10,000,50,000,100,000,500,000 or about 1,000,000L/ minutes or Higher.

Other flowable heat transmission mediums

In this method, system or device, can future the first flowable heat transmission medium that self-heating is crossed heat transmit To one or more than one the second flowable heat transmission medium.For example, the first heating containing the first flowable heat transmission medium Circuit can be used for heating respectively multiple other heating circuits containing the second flowable heat transmission medium.In another example In, the first heating circuit containing the first flowable heat transmission medium, which can be used for heating, respectively to be transmitted containing the second flowable heat The second heating circuit of one or more of medium, and one or more thirds respectively containing the flowable heat transmission medium of third Heating circuit.

Heat is transferred to the second flowable heat transmission medium from the first heated flowable heat transmission medium to be provided Used first flowable heat transmission medium.This method may include by heat from the used first flowable heat transmission medium It (for example, arranged in series) or is transferred to third from the first heated flowable heat transmission medium (for example, arranged in parallel) and can flow Dynamic heat transmission medium, to provide heated third flowable heat transmission medium.This method may include by heat from heated The flowable heat transmission medium of third is transferred at least one component for accommodating polyamide of polyamide synthesis system.Third can flow Dynamic heat transmission medium can be any appropriate heat transmission medium described herein.The flowable heat transmission medium of third can be with Second heat transmission medium is same or different.The polyamide that heat is transferred to from the heated flowable heat transmission medium of third At least one component of synthesis system can be and the polyamides that is transferred to heat from the second heated flowable heat transmission medium At least one component of amine synthesis system is same or different.

Polyamide

The polyamide prepared by the method, system or device can be any appropriate polyamide.Polyamide can be with It is synthesized by the dicarboxylic acids of straight chain and the diamines of straight chain or the oligomer by being formed from the dicarboxylic acids of straight chain and the diamines of straight chain synthesizes. Polyamide can be nylon-6,6.

Dicarboxylic acids can be any appropriate dicarboxylic acids.Dicarboxylic acids can have structure HO C (O)-R¹- C (O) OH, wherein R¹ It is C₁-C₁₅Alkylidene, such as methylene, ethylidene, propylidene, butylidene, pentylidene, hexylidene, heptamethylene, octamethylene, sub- nonyl Base or decylene.Dicarboxylic acids can be adipic acid (for example, R¹=butylidene).

Diamines can be any appropriate diamines.Diamines can have structure H₂N—R²-NH₂, wherein R²It is C₁-C₁₅Alkylene Base, such as methylene, ethylidene, propylidene, butylidene, pentylidene, hexylidene, heptamethylene, octamethylene, nonylene or decylene. Diamines can be hexamethylene diamine, (for example, R²=butylidene).

Embodiment

By reference to the following instance provided by way of example, the present invention may be better understood.The present invention is unlimited In example given herein.

Conventional method for determining gel fraction.Each gel fraction described in embodiment is by taking two methods to be determined Gel fraction average value and determine.In first method, while reaction mixture is still heat, liquid reactions are mixed Object is discharged from system, and system is cooled down, and dismantles, and visual inspection is to estimate the volume of gel therein.In the second approach, While reaction mixture is still heat, liquid reaction mixture is discharged from system, it is cooling, water is filled, and water is discharged. The volume for the water being discharged from system is subtracted to determine the volume of the gel in system by the system bulk of not gel.For determination Gel fraction in the specific component of one or more of equipment or specific position downstream, only by the specific component or specific position of equipment The system water in downstream is filled.In two methods, the density of gel is it is estimated that be 0.9g/cm³。

Liquid phase heat transmission medium in embodiment 1a. comparative example level-one heating circuits

It will66 are heated to about 340 DEG C and cycle through nylon-6, and the level-one in 6 manufacturing equipments adds Hot loop.Level-one heating circuit will66 with suitable flow velocity power house and evaporator, reactor and It recycles between heat exchanger on finisher, later will66 transmission are back to power house for adding again Heat.Use about 10,000,000L's in level-one heating circuit66。66 Liquid is remained in entire technique.

In continuous nylon-6,6 manufacturing methods, adipic acid and hexamethylene diamine are mixed in water with about equimolar ratio It closes to be formed containing nylon-6, the aqueous mixtures of 6 salt, and the aqueous mixtures have about 50 weight % water.By saline solution with It is transferred to evaporator within about 105L/ minutes.By heat from level-one heating circuit66 are transferred to steaming Device is sent out, to which saline solution is heated to about 125-135 DEG C (130 DEG C) by evaporator and moves water from heated saline solution It removes so that water concentration reaches about 30 weight %.Salt mixture after evaporation was transferred to tubular reactor with about 75L/ minutes. Tubular reactor has the length of about 40m, the mean inside diameter of about 89cm, often in the slave entrance to outlet of 5m length about 2.5cm Diameter expansion rate, about 45 L/D ratios, and 3 floss holes along distribution of lengths.In level-one heating circuit by heat from66 are transferred to reactor so that the temperature of the salt mixture after evaporation reaches about 218-250 DEG C (235 DEG C), so that reactor is further removed water from the salt mixture after heated evaporation so that water concentration reaches about 10 weights % is measured, and salt is further polymerize.The mixture of reaction was transferred to flash vessel with about 60L/ minutes.It is heated in level-one In circuit by heat from66 are transferred to flash vessel, and the mixture of reaction is heated to about 270-290 DEG C (280 DEG C), make flash vessel further remove water from reaction mixture, so that water concentration reaches about 0.5 weight %, and make The mixture that must be reacted further polymerize.Mixture after flash distillation was transferred to finisher with about 54L/ minutes so that poly- It closes mixture and undergoes vacuum further to remove water so that water concentration reaches about 0.1 weight %, so that polyamide obtains properly Final polymerization scope, the polyblend that aftercondensated is crossed is transferred to extruder and comminutor later.

Liquid66 need big pump to be recycled in entire level-one heating circuit to provide material All unit operation is simultaneously back to power house for reheating.Material is transmitted with the heat for undergoing phase transformation in heat transfer process is used The other methods of material compare, per KgThe 66 every KJ heat transmitted66 temperature Total change is bigger on degree；Use the surface area of higher cycle rate and bigger in heat exchanger transmitted for heat It is transmitted with completing the desired amount of heat.In addition, the accurate temperature of each unit operation is kept to be difficult, because heat transmission medium Temperature only can be integrally-regulated and individual unit cannot be adjusted.

The part flash distillation for leading to the high pressure bag and liquid of vapor along three floss holes of 40m reactors distribution, causes to live Flow pattern is filled in, reduces the ratio of annular flow, and generate uncontrollable pressure.Piston flow and flash distillation lead to reaction mixture It is uneven by the flow velocity of reactor.The rapid expansion of diameter causes increased gel in tubular reactor to generate and react mixing The solidification (for example, condensation) of object, and lead to the removal of excessive water, this causes flash vessel to undergo flow instabilities, reaction mixing The condensation of object, and vibration.

Gas phase heat transmission medium in embodiment 1b. comparative example level-one heating circuits

By DOWTHERM^TMA is steam in about 340 DEG C and about 400KPa pressure heatings and cycles through nylon-6,6 manufactures The level-one heating circuit between power house and multiple unit operations in equipment, herein it transfer heat to multiple unit operations, It transmits later and is back to power house for reheating.The DOWTHERM of about 10,000,000L is used in level-one heating circuit^TM A。DOWTHERM^TMA remains steam in entire technique, and with enough rate loops, so that material will not drop to Less than the saturation temperature in cycle.

As the description in embodiment 1a carries out continuous nylon-6,6 manufacturing process, but steam is used in entire technique DOWTHERM^TMA.Compared with the other methods for using the heat transfer material for undergoing phase transformation during heat is transmitted, per Kg DOWTHERM^TMDOWTHERM when A transmits the heat per KJ^TMTotal change is bigger in the temperature of A；Make in a heat exchanger It is transmitted with higher cycle rate and the surface area of bigger transmitted for heat with completing the desired amount of heat.In addition, keeping each The accurate temperature of unit operation such as tubular reactor is difficult because the temperature of heat transmission medium only can it is integrally-regulated and Individual unit cannot be adjusted.

Embodiment 1c. comparative examples has the volatility heat transmission medium in the level-one heating circuit of condensation

According to embodiment 1b, but use the DOWTHERM with certain cycle rate^TMA is so that more transferring heat to From DOWTHERM during a unit operation^TMA absorbs enough heat, so as to cause in level-one heating circuit DOWTHERM^TMThe partial condensation of A.By generated liquid circulation to remaining unit operation and to be back to power house, need Other equipment, including liquid knockout drum, pipe in addition and pump are so that condensate is back to power house and carries out reheating and again gas Change.The accurate temperature of each unit operation such as tubular reactor is kept to be difficult, because the temperature of heat transmission medium only can be with It is integrally-regulated and individual unit cannot be adjusted.

Volatility heat transmission mediums of the embodiment 1d. comparative examples in the level-one heating circuit of leakage

According to embodiment 1b.It is leaked in level-one heating circuit.It is attributed to the height used in level-one heating circuit Press steam, DOWTHERM^TMA steams are escaped by leaking so that the pressure reduction of entire level-one heating circuit.It is attributed to level-one The size of heating circuit, before the level of pressure reduction in systems to the reduced rate for allowing leakage the steam of large volume from Leak escapes.Around leakage position and leakage, it is included in the region fluidly connected with the airspace near leakage In, the DOWTHERM of effusion^TMThere is burning or risk of explosion in A steams.In order to stop leaking, or extinguishes and fired caused by leaking It burns, it is necessary to close the entire level-one heating circuit in equipment.

Volatility heat transmission mediums of the embodiment 1e. comparative examples in the level-one heating circuit of leakage

According to embodiment 1c.It is leaked in level-one heating circuit.It is attributed to the height used in level-one heating circuit Press steam, DOWTHERM^TMA steams are overflowed by leaking, to reduce the pressure in entire level-one heating circuit.It is attributed to The size of level-one heating circuit, before pressure reduction to the level for the reduced rate for allowing leakage in systems, large volume Steam is overflowed from leakage.Around leakage position and leakage, being included in has and leaks what neighbouring airspace fluidly connected In region, the DOWTHERM of effusion^TMThere is burning or risk of explosion in A steams.In order to stop leaking, or extinguish since leakage is drawn Combust, it is necessary to close the entire level-one heating circuit in equipment.

Embodiment 2a. is in the level-one with the evaporator, tubular reactor and the flash vessel that are heated via two level heating circuit In heating circuit 66

It will66 are heated to about 340 DEG C and cycle through nylon-6, and the level-one in 6 manufacturing equipments adds Hot loop.Level-one heating circuit will66 heat exchanger on power house and two level heating circuit, with And it is recycled between the heat exchanger in some individual unit operations.Two level heating circuit contains DOWTHERM^TMA, and be used for Heating evaporation device, reactor and flash vessel.The pressure of two level heating circuit is independently adjusted to change DOWTHERM^TMThe gasification of A And condensation temperature, to accurately control the temperature for each of being heated specific unit operation.Level-one heating circuit contains about 10,000,000L's66, and each two level heating circuit contains the DOWTHERM of about 50,000L^TM A。

In continuous nylon-6,6 manufacturing methods, by adipic acid and hexamethylene diamine with about equimolar ratio group in water It closes to be formed containing nylon-6,6 salt and the aqueous mixture with about 50 weight % water.By saline solution with about 105L/ Minute is transferred to evaporator.By heat from DOWTHERM in the two level heating circuit for evaporator^TMA is transferred to evaporator, permits Perhaps saline solution is heated to about 125-135 DEG C (130 DEG C) and removes water from heated saline solution by evaporator so that Water concentration reaches about 30 weight %.The pressure of two level heating circuit on evaporator is adjusted to about 1KPa to about 3KPa (2KPa), by DOWTHERM^TMThe saturation temperature of A is maintained at about 130 DEG C.By the salt mixture of evaporation with about 75L/ minutes It is transferred to tubular reactor.Tubular reactor has the length of about 40m, the average internal diameter of about 89cm, per 5m length about 2.5cm Slave entrance to the internal diameter expansion rate of outlet, about 45 L/D ratios, and 3 floss holes along distribution of lengths.For reacting By heat from DOWTHERM in the two level heating circuit of device^TMA is transferred to reactor so that the temperature of the salt mixture after evaporation reaches To about 218-250 DEG C (235 DEG C), reactor is allowed further to remove water from the salt mixture of heated evaporation so that water Concentration reaches about 10 weight %, and salt is further polymerize.By the pressure tune of the two level heating circuit on reactor Section is to about 28KPa to about 97KPa (80KPa), by DOWTHERM^TMThe saturation temperature of A is maintained at about 235 DEG C.By the mixed of reaction It closes object and was transferred to flash vessel with about 60L/ minutes.In the two level heating circuit for flash vessel, by heat from DOWTHERM^TMA is passed It is handed to flash vessel, the mixture of reaction is heated to about 270-290 DEG C (280 DEG C), allows flash vessel from reaction mixture into one Step removes water so that water concentration reaches about 0.5 weight %, and the mixture of reaction is further polymerize.It will be used to flash The pressure of two level heating circuit on device is adjusted to about 150KPa to about 200KPa (180KPa), by DOWTHERM^TMA's is full It is maintained at about 280 DEG C with temperature.The mixture of flash distillation was transferred to finisher with about 54L/ minutes so that polyblend passes through Vacuum is gone through further to remove water so that water concentration reaches about 0.1 weight %, to be passed in the polyblend for crossing aftercondensated It is handed to before extruder and comminutor, polyamide obtains suitable final polymerization scope.

The part flash distillation for leading to the high pressure bag and liquid of vapor along 3 floss holes of 40m reactors distribution, leads to piston Flow pattern reduces the ratio of annular flow, and generates uncontrollable pressure.Piston flow and flash distillation cause reaction mixture logical The flow velocity for crossing reactor is uneven.The rapid expansion of diameter leads to increased gel generation and reaction mixture in tubular reactor Solidification (for example, condensation), and lead to the removal of excessive water, this leads to flash vessel experience flow instabilities, reaction mixture Condensation and vibration.

Embodiment 2b. is in the level-one with the evaporator, tubular reactor and the flash vessel that are heated via two level heating circuit In heating circuit 66。

It will66 are heated to about 340 DEG C and cycle through nylon-6, and the level-one in 6 manufacturing equipments adds Hot loop.Level-one heating circuit will66 heat exchanger on power house and two level heating circuit it Between, and recycled between the heat exchanger in some individual unit operations.Two level heating circuit contains DOWTHERM^TMA, And it is used for heating evaporation device, reactor and flash vessel.The pressure of two level heating circuit is independently adjusted to change DOWTHERM^TM The gasification of A and condensation temperature, to accurately control the temperature for each of being heated specific unit operation.Level-one heating circuit Contain about 10,000,000L's66, and each two level heating circuit contains about 50,000L's DOWTHERM^TM A。

In continuous nylon-6,6 manufacturing methods, by adipic acid and hexamethylene diamine with about equimolar ratio group in water It closes to be formed containing nylon-6,6 salt and the aqueous mixture with about 50 weight % water concentrations.By saline solution with about It is transferred to evaporator within 105L/ minutes.By heat from DOWTHERMT in the two level heating circuit for evaporator^MA is transferred to evaporation Device allows evaporator that saline solution is heated to about 125-135 DEG C (130 DEG C) and removes water from heated saline solution, So that water concentration reaches about 30 weight %.The pressure of two level heating circuit on evaporator is adjusted to about 1KPa to about 3KPa (2KPa), by DOWTHERM^TMThe saturation temperature of A is maintained at about 130 DEG C.It is heated back in level-one heating circuit and two level Heat between road is transmitted, and it is mainly sensible heat that the heat between two level heating circuit and evaporator, which is transmitted, and for steaming Send out DOWTHERM in the two level heating circuit of device^TMThe temperature change of A is no more than about about 15 DEG C of 130 DEG C of saturation temperature or so. The salt mixture of evaporation was transferred to tubular reactor with about 75L/ minutes.Tubular reactor has the length of about 40m, about The average internal diameter of 89cm, slave entrance per 5m length about 2.5cm to the internal diameter expansion rate of outlet, about 45 L/D ratios, and Along 3 floss holes of distribution of lengths.By heat from DOWTHERM in the two level heating circuit for reactor^TMA is transferred to reaction Device so that the temperature of the salt mixture of evaporation reaches about 218-250 DEG C (235 DEG C), allows reactor further by water from heating The salt mixture for the evaporation crossed removes so that water concentration reaches about 10 weight %, and salt is further polymerize.It will be used for anti- The pressure of the two level heating circuit on device is answered to be adjusted to about 28KPa to about 97KPa (80KPa), by DOWTHERM^TMThe saturation of A Temperature is maintained at about 235 DEG C.Heat between level-one heating circuit and two level heating circuit is transmitted, and in two level heating circuit Heat between reactor transmits mainly sensible heat, and DOWTHERM^TMA is in the two level heating circuit medium temperature for reactor About 15 DEG C or so of the saturation temperature of no more than about 235 DEG C of variation on degree.The mixture of reaction was transmitted with about 60L/ minutes To flash vessel.By heat from DOWTHERM in the two level heating circuit for flash vessel^TMA is transferred to flash vessel, by the mixed of reaction It closes object to be heated to about 270-290 DEG C (280 DEG C), allows flash vessel further to remove water from reaction mixture so that water concentration reaches To about 0.5 weight %, and the mixture of reaction is further polymerize.By the pressure of the two level heating circuit on flash vessel Power is adjusted to about 150KPa to about 200KPa (180KPa), by DOWTHERM^TMThe saturation temperature of A is maintained at about 280 DEG C.? Heat between level-one heating circuit and two level heating circuit is transmitted, and the heat between two level heating circuit and flash vessel is transmitted Mainly sensible heat, and DOWTHERM^TMVariations of the A in the two level heating circuit for flash vessel in temperature is no more than about 280 DEG C about 15 DEG C or so of saturation temperature.The mixture of flash distillation was transferred to finisher with about 54L/ minutes so that polymerization is mixed It closes object and undergoes vacuum further to remove water so that water concentration reaches about 0.1 weight %, so that in the polymerization for crossing aftercondensated Mixture is transferred to before extruder and comminutor, and polyamide obtains suitable final polymerization scope.

The part flash distillation for leading to the high pressure bag and liquid of vapor along 3 floss holes of 40m reactors distribution, leads to piston Flow pattern reduces the ratio of annular flow, and generates uncontrollable pressure.Piston flow and flash distillation cause reaction mixture logical The flow velocity for crossing reactor is uneven.The rapid expansion of diameter leads to increased gel generation and reaction mixture in tubular reactor Solidification (for example, condensation), and lead to the removal of excessive water, this causes flash vessel to undergo flow instabilities, reaction mixture Condensation, and vibration.

In embodiment 2c. level-one heating circuits 66, have and is heated via two level heating circuit Evaporator, tubular reactor and flash vessel, have for evaporator secondary circuit in water.

It will66 are heated to about 340 DEG C and cycle through nylon-6, and the level-one in 6 manufacturing equipments adds Hot loop.Level-one heating circuit will66 heat exchanger on power house and two level heating circuit it Between, and recycled between the heat exchanger in some individual unit operations.It is heated for the two level of reactor and flash vessel Contain DOWTHERM in circuit^TMA.Two level heating circuit for evaporator contains water.It is independently adjusted the pressure of two level heating circuit Power is to change DOWTHERM^TMThe gasification of A or water and condensation temperature each of are heated specific unit and are grasped to accurately control The temperature of work.Level-one heating circuit contains about 10,000,000L's66, and each two level heats back Contain the DOWTHERM of about 50,000L in road^TMA or water.

In continuous nylon-6,6 manufacturing methods, by adipic acid and hexamethylene diamine with about equimolar ratio group in water It closes to be formed containing nylon-6,6 salt and the aqueous mixture with about 50 weight % water concentrations.By saline solution with about It is transferred to evaporator within 105L/ minutes.Heat is transferred to steaming from the DOWTHERMTM A in the two level heating circuit for evaporator Device is sent out, allow evaporator that saline solution is heated to about 125-135 DEG C (130 DEG C) and moves water from heated saline solution It removes so that water concentration reaches about 30 weight %.The pressure of two level heating circuit on evaporator is adjusted to about 270KPa The saturation temperature of water is maintained at about 130 DEG C.Heat between level-one heating circuit and two level heating circuit is transmitted, Yi Ji Heat between two level heating circuit and evaporator transmits mainly sensible heat, and the water in the two level heating circuit for evaporator Temperature on about 15 DEG C or so of saturation temperature of no more than about 130 DEG C of variation.By the salt mixture of evaporation with about 75L/ Minute is transferred to tubular reactor.Tubular reactor has the length of about 40m, and the average internal diameter of about 89cm, every 5m length is about The slave entrance of 2.5cm is to the internal diameter expansion rate of outlet, about 45 L/D ratios, and 3 floss holes along distribution of lengths.With By heat from DOWTHERM in the two level heating circuit of reactor^TMA is transferred to reactor so that the temperature of the salt mixture of evaporation Degree reaches about 218-250 DEG C (235 DEG C), allows reactor further to remove water from the salt mixture of heated evaporation, makes It obtains water concentration and reaches about 10 weight %, and salt is further polymerize.By the pressure of the two level heating circuit on reactor Power is adjusted to about 28KPa to about 97KPa (80KPa), by DOWTHERM^TMThe saturation temperature of A is maintained at about 235 DEG C.In level-one Heat between heating circuit and two level heating circuit is transmitted, and the heat between two level heating circuit and reactor is transmitted mainly It is sensible heat, and the DOWTHERM in the two level heating circuit for reactor^TMVariation in the temperature of A is no more than about 235 DEG C about 15 DEG C or so of saturation temperature.The mixture of reaction was transferred to flash vessel with about 60L/ minutes.For flash vessel Two level heating circuit in by heat from DOWTHERMT^TMA is transferred to flash vessel, and the mixture of reaction is heated to about 270-290 DEG C (280 DEG C) allow flash vessel further to remove water from reaction mixture so that water concentration reaches about 0.5 weight %, and makes The mixture that must be reacted further polymerize.The pressure of two level heating circuit on flash vessel is adjusted to about 150KPa to about 200KPa (180KPa), by DOWTHERM^TMThe saturation temperature of A is maintained at about 280 DEG C.Add with two level in level-one heating circuit Between hot loop heat transmit, and between two level heating circuit and flash vessel heat transmit be mainly sensible heat, and with The DOWTHERM in the two level heating circuit of flash vessel^TMThe pact of the saturation temperature of no more than about 280 DEG C of variation in the temperature of A 15 DEG C or so.The mixture of flash distillation was transferred to finisher with about 54L/ minutes so that polyblend undergo vacuum with into One step removes water so that water concentration reaches about 0.1 weight %, so that being transferred to extrusion in the polyblend for crossing aftercondensated Before machine and comminutor, polyamide obtains suitable final polymerization scope.

In 3. level-one heating circuit of embodiment 66, with what is heated via two level heating circuit Reactor and the evaporator and flash vessel heated via level-one heating circuit.

It will66 are heated to about 340 DEG C and cycle through nylon-6, and the level-one in 6 manufacturing equipments adds Hot loop.Level-one heating circuit will66 heat exchangers on power house and two level heating circuit and It is recycled between heat exchanger in some individual unit operations.Two level heating circuit contains DOWTHERM^TMA, and for adding Thermal reactor.The pressure of two level heating circuit is adjusted to change DOWTHERM^TMThe gasification of A and condensation temperature are to accurately control The temperature of reactor.Level-one heating circuit contains about 10,000,000L's66, and two level heats back Contain the DOWTHERM of about 50,000L in road^TM A。

In continuous nylon-6,6 manufacturing methods, by adipic acid and hexamethylene diamine with about equimolar ratio group in water It closes, contains nylon-6 to be formed, the aqueous mixture of 6 salt and the water with about 50 weight %.By saline solution with about 105L/ points Clock is transferred to evaporator.In level-one heating circuit, by heat from66 are transferred to evaporator, allow to evaporate Saline solution is heated to about 125-135 DEG C (130 DEG C) and removes water from heated saline solution by device so that water concentration Reach about 30 weight %.The salt mixture of evaporation was transferred to reactor with about 75L/ minutes.Tubular reactor has about 40m's Length, the average internal diameter of about 89cm, slave entrance per 5m length about 2.5cm to the internal diameter expansion rate of outlet, about 45 L/D ratios Example, and along 3 floss holes of distribution of lengths.By heat from DOWTHERM in two level heating circuit^TMA is transferred to reactor, makes The temperature for the salt mixture that must be evaporated reaches about 218-250 DEG C (235 DEG C), allows reactor further by water from heated steaming The salt mixture of hair removes so that water concentration reaches about 10 weight %, and salt is further polymerize.It will be used for reactor The pressure of two level heating circuit be adjusted to about 28KPa to about 97KPa (80KPa), by DOWTHERM^TMThe saturation temperature of A is protected It holds at about 235 DEG C.Between level-one heating circuit and two level heating circuit heat transmit, and two level heating circuit with react Heat between device transmits mainly sensible heat, and DOWTHERM^TMA is in the two level heating circuit for reactor in temperature About 15 DEG C or so of the saturation temperature that no more than about 235 DEG C of variation.The mixture of reaction was transferred to flash distillation with about 60L/ minutes Device.In level-one heating circuit by heat from66 are transferred to flash vessel, and the mixture of reaction is heated to About 270-290 DEG C (280 DEG C) allow flash vessel further to remove water from reaction mixture so that water concentration reaches about 0.5 weight % is measured, and the mixture of reaction is further polymerize.The mixture of flash distillation was transferred to finisher with about 54L/ minutes, So that polyblend undergoes vacuum further to remove water so that water concentration reaches about 0.1 weight %, so that by retraction The polyblend gathered is transferred to before extruder and comminutor, and polyamide obtains suitable final polymerization scope.

Embodiment 4.Tubular reactor with longer length and less diameter

According to embodiment 2a, using tubular reactor, the mean inside diameter with about 100 meters of length and about 0.41m, per 5m The slave entrance of length about 2.54cm with about 246 L/D ratios, and has along the 8 of distribution of lengths to the internal diameter expansion rate of outlet A floss hole.

Compared with embodiment 1a-e and 2a-2b, the salt mixture of tubular reactor more slowly heating evaporation, although its quilt It is heated to be its target temperature, this causes the formation of undesirable by-product less and the diamines from the vapor that reactor discharges It loses less.The slower heating of the salt of evaporation causes polymeric blends aerosolized less, this causes floss hole pipeline clear The longer time is not blocked between clean.

Embodiment 5a.Tubular reactor with longer length and less diameter

According to embodiment 2a, using tubular reactor, the mean inside diameter with about 100 meters of length and about 41cm, often The slave entrance of 550m length about 2.5cm with about 246 L/D ratios, and has along distribution of lengths to the internal diameter expansion rate of outlet 8 floss holes.

Compared with embodiment 1a-e and 2a-2b, the salt mixture of tubular reactor more slowly heating evaporation, although its quilt It is heated to be its target temperature, this causes the formation of undesirable by-product less and the diamines from the vapor that reactor discharges It loses less.The slower heating of the salt of evaporation leads to the aerosolized less of polymeric blends, this leads to floss hole pipeline not It blocks, the interval time between cleaning is longer.

Embodiment 5b.Tubular reactor with longer length and less diameter.

According to embodiment 2a, and tubular reactor is used, the tubular reactor is with about 100 meters of length and about 41cm Mean inside diameter, the internal diameter expansion rate of slave entrance per 110m length about 2.5cm to outlet, with about 246 L/D ratios, and With 8 floss holes along distribution of lengths.

Compared with embodiment 1a-e and 2a-2b, the salt mixture of tubular reactor more slowly heating evaporation, although its quilt It is heated to be its target temperature, this causes the formation of undesirable by-product less and the diamines from the vapor that reactor discharges It loses less.The slower heating of the salt of evaporation leads to the aerosolized less of polymeric blends, this leads to floss hole pipeline not It blocks, the interval time between cleaning is longer.Diameter increment rate reduces the generation and accumulation of gel and other impurities in reactor, Help to maintain the annularly flow of greater proportion in entire reactor.Diameter increment rate is provided between the entrance and outlet of reactor Pressure drop, this leads to the more effective fruit of water in reactor and removal more efficiently, while reducing or preventing from polymerizeing in reactor The solidification of object mixture.

Embodiment 5c.Tubular reactor with longer length and less diameter.

Compared with embodiment 1a-e and 2a-2b, the salt mixture of tubular reactor more slowly heating evaporation, although its quilt Be heated to be its target temperature, so as to cause undesirable by-product formation it is less and from reactor discharge vapor in diamines Loss it is less.The slower heating of the salt of evaporation causes polymeric blends aerosolized less, this leads to floss hole pipeline not It blocks, the interval time between cleaning is longer.Diameter increment rate reduces the generation and accumulation of gel and other impurities in reactor, Help to maintain the annularly flow of greater proportion in entire reactor.Diameter increment rate is provided between the entrance and outlet of reactor Pressure drop, this leads to the more effective fruit of water in reactor and removal more efficiently, while reducing or preventing from polymerizeing in reactor The solidification of object mixture.

Embodiment 5d.Tubular reactor with longer length and less diameter.

According to embodiment 2a, and tubular reactor is used, the tubular reactor is with about 100 meters of length and about 41cm Mean inside diameter, the internal diameter expansion rate of slave entrance per 1000m length about 2.5cm to outlet, with about 246 L/D ratios, and With 8 floss holes along distribution of lengths.

Compared with embodiment 1a-e and 2a-2b, the salt mixture of tubular reactor more slowly heating evaporation, although its quilt Be heated to be its target temperature, so as to cause undesirable by-product formation it is less and from reactor discharge vapor in diamines Loss it is less.The slower heating of the salt of evaporation causes polymeric blends aerosolized less, this leads to floss hole pipeline not It blocks, the interval time between cleaning is longer.

Compared with embodiment 5b and 5c, diameter increment rate provides the water in more inefficient reactor and removes, it is desirable that more Energy is to remove same amount of water.

Embodiment 6a.Tubular reactor with the floss hole for increasing number.

According to embodiment 2a, using the tubular reactor with identical size, but with 7 discharges along distribution of lengths Mouthful.

Compared with embodiment 1a-e and 2a-2b, the tubular reactor with the floss hole for increasing number is each to positioning The amount smaller for the vapor for being advanced through reaction tube is set, and the vapor in pipe is moved with lower speed.The water of reduction steams Air volume and speed cause less polymeric blends to march in floss hole pipeline, do not allow floss hole pipeline before cleaning not During blocking the ground operation longer time.The floss hole of increase number with layout pitch helps to prevent the part of liquid from dodging Steaming and piston flow pattern, provide more stable flow velocity and the annular flow of greater proportion.

Embodiment 6b.Tubular reactor with small interval between the floss hole and some floss holes for increasing number.

According to embodiment 2a, and using the tubular reactor with identical size, but there are 7 floss holes, wherein 5 Floss hole is evenly distributed, and remaining 2 floss holes are gathered near the centre of reactor and are separated by about 1m.

Compared with embodiment 1a-e and 2a-2b, the tubular reactor with the floss hole for increasing number is each to positioning The amount smaller for the vapor for being advanced through reaction tube is set, and the vapor in pipe is moved with lower speed.The water of reduction steams Air volume and speed cause less polymeric blends to march in floss hole pipeline, do not allow floss hole pipeline before cleaning not During blocking the ground operation longer time.The floss hole for increasing number additionally aids the part flash distillation for preventing liquid and piston flowing Kenel provides more stable flow velocity and the annular flow of greater proportion.However, small between the floss hole assembled among reactor It is destroyed in those of reactor region every leading to annularly flow；On the contrary, the flowing of liquid is similar to the half of the lower part of pipe The fluid of cylinder, wherein gas and vapor are in a remainder part for horizontal tube.The annular flow of reduction ratio causes relatively low The heat to the reaction mixture in pipe of efficiency is transmitted.

Embodiment 6c.Tubular reactor with an excessive number of floss hole.

According to embodiment 2a, and using the tubular reactor with identical size, but with 40 rows along distribution of lengths Put mouth.

Compared with embodiment 1a-e and 2a-2b, the tubular reactor with the floss hole for increasing number is each to positioning Setting has more a small amount of vapor for being advanced through reaction tube, and the vapor in pipe is moved with lower speed.It reduces Vapor volume and speed cause less polymeric blends to march in floss hole pipeline, allow floss hole pipeline in cleaning It is preceding run the longer time with not blocking during.

However, the closely-spaced length for causing annular flow to run through reactor between floss hole is destroyed；On the contrary, the stream of liquid The flowing of the dynamic semicylinder similar to pipe lower part, wherein gas and vapor are in a remainder part for horizontal tube.Reduce ratio The annular flow of example causes the heat of the more inefficient reaction mixture in pipe to be transmitted.

Embodiment 7.The tubular reactor of cleaning method is injected using water.

According to embodiment 2a, and using the floss hole clean method wherein injected water into floss hole pipeline to contribute to Prevent the accumulation of gel in floss hole pipeline.

Compared with embodiment 1a-e and 2a-2b, tubular reactor is not in the case where blocking floss hole in necessary cleaning Between run the longer time during.

Embodiment 8a.Tubular reactor with longer length and less diameter and the floss hole for increasing number, And inject cleaning method using water

According to embodiment 2a, but tubular reactor is used, the mean inside diameter with about 100 meters of length and about 41cm, tool There are about 246 L/D ratios, and with 17 floss holes along distribution of lengths.Using wherein injecting water into floss hole pipeline Floss hole clean method to help to prevent the accumulation of gel in floss hole pipeline.

Compared with embodiment 1a-e and 2a-2b, the salt mixture of tubular reactor more slowly heating evaporation, although its quilt Be heated to be its target temperature, so as to cause undesirable by-product formation it is less and from reactor discharge vapor in diamines Loss it is less.The slower heating of the salt of evaporation leads to less aerosolized of polymeric blends, this leads to floss hole pipeline It does not block, the interval time between cleaning is longer.Tubular reactor with the floss hole for increasing number is in each given position With more a small amount of vapor for being advanced through reaction tube, and the vapor in pipe is moved with lower speed.The water of reduction Vapor volume and speed cause less polymeric blends to march in floss hole pipeline, allow floss hole pipeline before cleaning During running the longer time with not blocking.The floss hole for increasing number additionally aids the part flash distillation for preventing liquid and piston flow Ejector half state provides more stable flow velocity and the annular flow of greater proportion.

Embodiment 8b.Tubular reactor with longer length and less diameter and the floss hole for increasing number, And inject cleaning method using water.

According to embodiment 3, but tubular reactor is used, the tubular reactor is with about 100 meters of length and about 41cm Mean inside diameter, with about 246 L/D ratios, and with along distribution of lengths 17 floss holes.Using wherein injecting water into Floss hole clean method in floss hole pipeline is to help to prevent the accumulation of gel in floss hole pipeline.

Embodiment 8c.Tubular reactor with longer length and less diameter and the floss hole for increasing number, And inject cleaning method using water.

According to embodiment 2a, but tubular reactor is used, the tubular reactor is with about 100 meters of length and about 41cm Mean inside diameter, the slave entrance per 300m length about 2.5cm with about 246 L/D ratios, and have to the internal diameter expansion rate of outlet There are 17 floss holes along distribution of lengths.Using floss hole clean method, wherein injecting water into floss hole pipeline to help In the accumulation for preventing gel in floss hole pipeline.

Compared with embodiment 1a-e and 2a-2b, the salt mixture of tubular reactor more slowly heating evaporation, although its quilt It is heated to be its target temperature, thus causes the formation of undesirable by-product less and the diamines from the vapor that reactor discharges Loss it is less.The slower heating of the salt of evaporation causes polymeric blends aerosolized less, this leads to floss hole pipeline not It blocks, the interval time between cleaning is longer.Tubular reactor with the floss hole for increasing number has in each given position There is more a small amount of vapor for being advanced through reaction tube, and the vapor in pipe is moved with lower speed.The water of reduction steams Air volume and speed cause less polymeric blends to march in floss hole pipeline, do not allow floss hole pipeline before cleaning not During blocking the ground operation longer time.The floss hole for increasing number additionally aids the part flash distillation for preventing liquid and piston flowing Kenel provides more stable flow velocity and the annular flow of greater proportion.Diameter increment rate reduces gel and other impurities in reactor Generation and accumulation, help to maintain the annularly flow of greater proportion in entire reactor.Diameter increment rate provides reactor Pressure drop between entrance and outlet, this leads to the more effective fruit of water in reactor and removal more efficiently, while reducing or anti- Only in reactor polymeric blends solidification.

In 9. level-one heating circuit of embodiment 66, with what is heated via two level heating circuit Evaporator, tubular reactor and flash vessel, and have leakage in level-one heating circuit.

According to embodiment 2a.It is leaked in level-one heating circuit.

Leave the liquid of leakage66 are in relatively low pressure, to limit total row of material It puts.Because of discharged liquidIn contrast 66 be non-volatile, so the risk of explosion is close Zero and burn risk it is low, and be comprised in closest to leakage near.

In 10. level-one heating circuit of embodiment 66, have and is heated via two level heating circuit Evaporator, reactor and flash vessel, in two level heating circuit have leakage.

According to embodiment 2a.It is leaked in the two level heating circuit for tubular reactor.

Compared with embodiment 1d and 1e, the volatility DOWTHERM of smaller volume is used in two level heating circuit^TMA, this It reduces and the relevant safety hazards of high temperature combustible vapor using pressurization.With the level-one heating circuit in embodiment 1d and 1e In comparison the amount for the discharge that the volumetric constraint of smaller two level heating circuit occurs.Most of heating system in equipment It can operate continuously, while DOWTHERM will be contained^TMThe secondary circuit of A is closed to be burnt with repairing leakage or extinguishing.

Used terms and expressions are used as illustrative, and are unrestricted, and in this terms and expressions Use in it is not expected exclude given and description arbitrarily equivalent feature or part of it, but institute is it is recognized that a variety of repair It is possible to change into the range of the claimed invention.The modifications and variations of concept disclosed herein can be by this field Technical staff uses, and this modifications and variations are considered as in the scope of the present invention as defined in the appended claims.

Other embodiments.

The present invention provides at least the following terms and states that serial number is not interpreted to provide the level of importance：

Statement 1 provides a kind of method preparing polyamide, the method includes：First flowable heat transmission medium is added Heat, to provide heated first flowable heat transmission medium；It is situated between with heat is transmitted from the first heated flowable heat Matter is transferred to the second flowable heat transmission medium, to provide heated second flowable heat transmission medium；With by heat from described The second heated flowable heat transmission medium is transferred to the tubular reactor of polyamide synthesis system.

Statement 2 provides the method described in statement 1, wherein the tubular reactor includes about 50 to about 300 meters of length.

Statement 3 provides the method described in any one of statement 1-2, wherein the tubular reactor includes about 75-125 The length of rice.

Statement 4 provides the method described in statement any one of 1-3, wherein the tubular reactor include about 10cm extremely The internal diameter of about 80cm.

Statement 5 provides the method described in statement any one of 1-4, wherein the tubular reactor includes about 25cm to about The internal diameter of 60cm.

Statement 6 provides the method described in any one of statement 1-5, wherein the length/diameter of the tubular reactor (L/D) it is about 50 to about 2500.

Statement 7 provides the method described in any one of statement 1-6, wherein the length/diameter of the tubular reactor (L/D) it is about 100 to about 500.

Statement 8 provides the method described in any one of statement 1-7, wherein the tubular reactor includes along its length Floss hole.

Statement 9 provides the method described in statement 8, wherein the tubular reactor includes about 5 to about 50 floss holes.

Statement 10 provides the method described in statement any one of 8-9, wherein the tubular reactor includes about 10 to about 25 floss holes.

Statement 11 provides the method described in any one of statement 8-10, wherein the tubular reactor includes along the pipe Average often about 3 meters to about 9 meters about 1 floss holes of the length of formula reactor.

Statement 12 provides the method described in any one of statement 8-11, wherein the tubular reactor includes along the pipe Average often about 2 meters to about 15 meters about 1 floss holes of the length of formula reactor.

Statement 13 provides the method described in any one of statement 8-12, wherein the tubular reactor includes along described About 2 meters to about 15 meters of equispaced between the floss hole of the length of tubular reactor.

Statement 14 provides the method described in any one of statement 8-13, wherein the tubular reactor includes along described About 3 meters to about 9 meters of equispaced between the floss hole of the length of tubular reactor.

Statement 15 provides the method described in any one of statement 8-14, wherein the floss hole is connected to floss hole pipe Line, the method includes injecting water into the floss hole pipeline.

Statement 16 provides the method described in any one of statement 1-15, and wherein the method is not closing the tubular type Reactor is for carrying out at least about 1 to about 5 year in the case of clean.

Statement 17 provides the method described in any one of statement 1-16, and wherein the method is not closing the tubular type Reactor is for carrying out at least about 2.5 to about 3 years in the case of clean.

Statement 18 provides the method described in any one of statement 1-17, wherein the polyamide synthesis system is by straight chain Dicarboxylic acids and straight chain diamines synthesizing polyamides or oligomer be formed by by the dicarboxylic acids of straight chain and the diamines of straight chain synthesize Polyamide.

Statement 19 provides the method described in statement 18, wherein the dicarboxylic acids has structure HO C (O)-R¹- C (O) OH, Middle R¹It is C₁-C₁₅Alkylidene.

Statement 20 provides the method described in statement 19, wherein the dicarboxylic acids is adipic acid.

Statement 21 provides the method described in any one of statement 18-20, wherein the diamines has structure H₂N—R²- NH₂, wherein R²It is C₁-C₁₅Alkylidene.

Statement 22 provides the method described in statement 21, wherein the diamines is hexamethylene diamine.

Statement 23 provides the method described in any one of statement 18-22, wherein the polyamide is nylon-6,6.

Statement 24 provides the method described in any one of statement 1-23, wherein in standard temperature and pressure (STP), described first Flowable heat transmission medium has the vapour pressure lower than the described second flowable heat transmission medium.

Statement 25 provides the method described in any one of statement 1-24, wherein the second heated flowable heat Transfer medium has the vapour pressure higher than the first heated flowable heat transmission medium.

Statement 26 provides the method described in any one of statement 1-25, wherein the second flowable heat of the heating is transmitted Medium is at least one of more flammable and more inflammable than the first heated flowable heat transmission medium.

Statement 27 provides the method described in any one of statement 1-26, wherein the first flowable heat transmission medium Including at least one of the following：Water, polyethylene glycol, polypropylene glycol, mineral oil, silicone oil, diphenyl ether and biphenyl.

Statement 28 provides the method described in any one of statement 1-27, wherein the first flowable heat transmission medium It is at least one of the following：Trimethylpentane, C_10-13Alkane, C_10-13Isoalkane, C_14-30Alkylaryl compounds, two Ethylbenzene, the benzene of vinylation, cyclohexyl benzene, C_14-30Alkylbenzene, paraffin oil, ethyl diphenyl ethane, diphenylethane, diethyl two Diphenylphosphino ethane, diphenyl ether, dipheny oxide, ethylbenzene polymer, biphenyl, inorganic salts, diisopropyl biphenyl, tri isopropyl biphenyl, first Butylcyclohexane, dicyclohexyl, terphenyl, the terphenyl of hydrogenation, partially hydrogenated quaterphenyl, partially hydrogenated more advanced polyphenyl, Diphenyl ether and phenanthrene, biaryl compound, tri-aryl compounds, diaryl ether, triaryl ether, alkylaryl compounds, alkyl virtue Based compound and diaryl alkane based compound.

Statement 29 provides the method described in any one of statement 1-28, wherein the first heated flowable heat Transfer medium is about 280 DEG C to about 400 DEG C.

Statement 30 provides the method described in any one of statement 1-29, wherein the first heated flowable heat Transfer medium is about 330 DEG C to about 350 DEG C.

Statement 31 provides the method described in any one of statement 1-30, wherein the first flowable heat transmission medium It is basic liquid phase with the first heated flowable heat transmission medium.

Statement 32 provides the method described in any one of statement 1-31, wherein being transmitted by the described first flowable heat During medium heats, the first flowable heat transmission medium is substantially maintained as liquid.

Statement 33 provides the method described in any one of statement 1-32, is situated between wherein being transmitted in the described first flowable heat In the heating process of matter, do not occur the gasification of the described first flowable heat transmission medium substantially.

Statement 34 provides the method described in any one of statement 1-33, wherein being transmitted by the described first flowable heat During medium heats, the heat for being transferred to the described first flowable heat transmission medium includes substantially all sensible heat.

Statement 35 provides the method described in statement any one of 1-34, wherein can from described heated first by heat During flowing heat transmission medium is transferred to the described second flowable heat transmission medium, the first heated flowable heat Transfer medium is substantially maintained as liquid.

Statement 36 provides the method described in statement any one of 1-35, wherein by heat from described heated first During flowable heat transmission medium is transferred to the described second flowable heat transmission medium, do not occur substantially described heated The first flowable heat transmission medium condensation.

Statement 37 provides the method described in statement any one of 1-36, wherein heat can from described heated first Flow heat transmission medium to the described second flowable heat transmission medium transmission during, can be flowed from described heated first The heat that dynamic heat transmission medium transmits includes substantially all sensible heat.

Statement 38 provides the method described in any one of statement 1-37, wherein the first flowable heat transmission medium It is arranged in the first heating circuit with the first heated flowable heat transmission medium.

Statement 39 provides the method described in statement any one of 1-38, wherein can from described heated first by heat Flowing heat transmission medium, which is transferred to the described second flowable heat transmission medium and provides the used first flowable heat and transmit, to be situated between Matter, the method further include that the used first flowable heat transmission medium is recycled back to the described first flowable heat The heating of transfer medium.

Statement 40 provides the method described in any one of statement 1-39, wherein the second flowable heat transmission medium It is at least one of the following：Water, polyethylene glycol, polypropylene glycol, mineral oil, silicone oil, diphenyl ether, biphenyl and terphenyl.

Statement 41 provides the method described in any one of statement 1-40, wherein the second flowable heat transmission medium is At least one of the following：Trimethylpentane, C_10-13 alkane, C_10-13Isoalkane, C_14-30Alkylaryl compounds, diethyl Benzene, the benzene of vinylation, cyclohexyl benzene, C_14-30Alkylbenzene, paraffin oil, ethyl diphenyl ethane, diphenylethane, diethyl hexichol Base ethane, diphenyl ether, dipheny oxide, ethylbenzene polymer, biphenyl, inorganic salts, diisopropyl biphenyl, tri isopropyl biphenyl, methyl Hexamethylene, dicyclohexyl, terphenyl, the terphenyl of hydrogenation, partially hydrogenated quaterphenyl, partially hydrogenated more advanced polyphenyl, two Phenylate and phenanthrene, biaryl compound, tri-aryl compounds, diaryl ether, triaryl ether, alkylaryl compounds, alkylaryl Compound and diaryl alkane based compound.

Statement 42 provides the method described in any one of statement 1-41, wherein the second heated flowable heat passes It is about 210 DEG C to about 350 DEG C to pass medium.

Statement 43 provides the method described in any one of statement 1-42, wherein the second heated flowable heat passes It is about 260 DEG C to about 300 DEG C to pass medium.

Statement 44 provides the method described in any one of statement 1-43, wherein the second heated flowable heat passes It is basic liquid phase to pass medium.

Statement 45 provides the method described in any one of statement 1-44, wherein the second heated flowable heat passes It is substantially gas phase to pass medium.

Statement 46 provides the method described in statement any one of 1-45, wherein can from described heated first by heat During flowing heat transmission medium is transferred to the described second flowable heat transmission medium, the second flowable heat transmission medium Essentially become gas.

Statement 47 provides the method described in statement any one of 1-46, wherein can from described heated first by heat During flowing heat transmission medium is transferred to the described second flowable heat transmission medium, the second flowable heat transmission medium It is substantially all gasification.

Statement 48 provides the method described in statement 47, and the method further includes the control second flowable heat transmission medium Pressure to control the temperature of the described second flowable heat transmission medium gasification.

Statement 49 provides the method described in statement 48, wherein second heat transmission medium and the second heated heat Transfer medium is arranged in the second heating circuit, wherein the pressure for controlling the described second flowable heat transmission medium includes control institute State the pressure in the second heating circuit.

Statement 50 provides the method described in any one of statement 48-49, wherein by controlling the second flowable heat The temperature of transfer medium gasification controls the temperature of the tubular reactor.

Statement 51 provides the method described in statement any one of 1-50, wherein by heat from described heated first During flowable heat transmission medium is transferred to the described second flowable heat transmission medium, it is transferred to the described second flowable heat The heat of transfer medium includes substantially all of latent heat, and the latent heat includes heat of gasification.

Statement 52 provides the method described in statement any one of 1-51, wherein by heat from described heated first During flowable heat transmission medium is transferred to the described second flowable heat transmission medium, it is transferred to the described second flowable heat The heat of transfer medium includes：About 70-100% latent heat for including heat of gasification, and about 0-30% sensible heats.

Statement 53 provides the method described in statement any one of 1-52, wherein can from described heated second by heat During flowing heat transmission medium is transferred to the tubular reactor of the polyamide synthesis system, described heated second can Flowing heat transmission medium is substantially condensed into liquid.

Statement 54 provides the method described in statement 53, and the method further includes the control second heated flowable heat The pressure of transfer medium undergoes the temperature at least partly condensed with the adjust the heating second flowable heat transmission medium.

Statement 55 provides the method described in statement 54, wherein being situated between by controlling the second heated flowable heat and transmitting The matter temperature that at least partly condenses of experience controls the temperature to the tubular reactor.

Statement 56 provides the method described in statement any one of 54-55, wherein second heat transmission medium and described The second heated heat transmission medium is arranged in the second heating circuit, is passed wherein controlling the second heated flowable heat The pressure for passing medium includes the pressure in control second heating circuit.

Statement 57 provides the method described in statement 56, wherein it includes control institute to control the pressure in second heating circuit State the saturation temperature of the flowable heat transmission medium of heated second.

Statement 58 provides the method described in statement 57, wherein the highest of the second heated flowable heat transmission medium Temperature is in the range of about 0-40 DEG C of the saturation temperature of the second heated flowable heat transmission medium.

Statement 59 provides the method described in statement any one of 1-58, wherein by heat from described heated second During flowable heat transmission medium is transferred to the tubular reactor, transmits and be situated between from the second heated flowable heat The heat that matter is transmitted includes substantially all of latent heat, and the latent heat includes heat of gasification.

Statement 60 provides the method described in statement any one of 1-59, wherein by heat from described heated second During flowable heat transmission medium is transferred to the tubular reactor, transmitted from the described second flowable heat transmission medium Heat includes：About 70-100% includes the latent heat of heat of gasification, and about 0-30% sensible heats.

Statement 61 provides the method described in statement any one of 1-60, wherein can from described heated second by heat Flowing heat transmission medium is transferred to the tubular reactor and provides the used second flowable heat transmission medium, the method Further include the used second flowable heat transmission medium is recycled back to it is flowable from described heated first In the transmission of the heat of heat transmission medium.

Statement 62 provides the method described in statement any one of 1-61, wherein heat can be flowed from described heated second It includes that the temperature of the tubular reactor is maintained at about 150 DEG C to about that dynamic heat transmission medium, which is transferred to the tubular reactor, 350℃。

Statement 63 provides the method described in statement any one of 1-62, wherein heat can be flowed from described heated second It includes that the temperature of the tubular reactor is maintained at about 210 DEG C to about that dynamic heat transmission medium, which is transferred to the tubular reactor, 260℃。

Statement 64 provides the method described in statement any one of 1-63, wherein can from described heated second by heat It includes being maintained at the temperature of polyamide compound in the reactor that flowing heat transmission medium, which is transferred to the tubular reactor, About 218 DEG C to about 250 DEG C.

Statement 65 provides the method described in statement any one of 1-64, wherein can from described heated first by heat Flowing heat transmission medium, which is transferred to the described second flowable heat transmission medium and provides the used first flowable heat and transmit, to be situated between Matter, the method further include by heat from the used first flowable heat transmission medium or can from described heated first Flowing heat transmission medium is transferred to the flowable heat transmission medium of third, to provide the flowable heat transmission medium of third of heating；It will Heat is transferred to described at least one of polyamide synthesis system from the flowable heat transmission medium of heated third and accommodates The component of polyamide.

Statement 66 provides the method described in statement 65, wherein by heat from the flowable heat transmission medium of heated third At least one component for the polyamide synthesis system being transferred to is different from the tubular reactor.

Statement 67 provide it is a kind of prepare nylon-6,6 method, the method includes：First including terphenyl can be flowed Dynamic heat transmission medium heating, to provide heated first flowable heat transmission medium；By heat from including diphenyl ether and biphenyl The first heated flowable heat transmission medium is transferred to the second flowable heat transmission medium, to provide heated second Flowable heat transmission medium and used first flowable heat transmission medium, wherein the first flowable heat transmission medium, The first heated flowable heat transmission medium and the used first flowable heat transmission medium are arranged first In heating circuit, passed by the described first flowable heat transmission medium heating and by heat from the first heated flowable heat Pass during medium is transferred to the described second flowable heat transmission medium, the first flowable heat transmission medium, it is described plus The the first flowable heat transmission medium and the used first flowable heat transmission medium that heat is crossed are basic liquid phases, are passed The heat for being handed to the heat of the described first flowable heat transmission medium and being transmitted from the described first flowable heat transmission medium includes basic Upper complete sensible heat, and heat is being transferred to the described second flowable heat from the first heated flowable heat transmission medium During transfer medium, the second flowable heat transmission medium is by substantially all gasification；By described used first Flowable heat transmission medium is recycled back to the heating of the described first flowable heat transmission medium；By heat from described heated Two flowable heat transmission mediums are transferred to the tubular reactor of polyamide synthesis system, provide the used second flowable heat and pass Medium is passed, wherein the second flowable heat transmission medium and the heated second flowable heat transmission medium setting are the In two heating circuits, the second flowable heat transmission medium and the used second flowable heat transmission medium are basic Liquid phase, the second heated flowable heat transmission medium is basic liquid phase, and being transferred to described second can The heat of flowing heat transmission medium and the heat transmitted from the described second flowable heat transmission medium include about 70-100% latent heat (including heat of gasification), and about 0-30% sensible heats；Controlling the pressure of second heat transfer circuit can be flowed with controlling described second The saturation temperature of dynamic heat transmission medium, wherein controlling the temperature of the tubular reactor by controlling saturation temperature；With by institute The used second flowable heat transmission medium is stated to be recycled back to from the first heated flowable heat transmission medium Heat transmission in；The wherein described tubular reactor includes about 75 to about 125 meters of length, and the tubular reactor includes about The internal diameter of 25cm to about 60cm, the tubular reactor include the length/diameter (L/D) of about 100 to about 500, and wherein institute It states tubular reactor and includes about 10 to about 25 floss holes along its length.

Statement 68 provides a kind of method preparing polyamide, the method includes：The first flowable heat transmission medium is heated, To provide heated first flowable heat transmission medium；It is passed from the first heated flowable heat transmission medium with by heat It is handed to the second flowable heat transmission medium, to provide heated second flowable heat transmission medium；With by heat from the heating The the second flowable heat transmission medium crossed is transferred to the tubular reactor of polyamide synthesis system；The wherein described tubular reactor packet About 75 to about 125 meters of length is included, the tubular reactor includes internal diameters of the about 25cm to about 60cm, the tubular reactor packet The length/diameter (L/D) of about 100 to about 500 is included, and the wherein described tubular reactor includes about 10 to about 25 along its length Floss hole.

Statement 69 provides a kind of system being used to prepare polyamide, the system comprises：Heater, the heater configuration To heat the first flowable heat transmission medium to provide heated first flowable heat transmission medium；First heat exchanger, The first heat exchanger is configured to transmit from the first heated flowable heat transmission medium hot heated to provide Second flowable heat transmission medium；And second heat exchanger, the second heat exchanger are configured to heat from described heated Second flowable heat transmission medium is transferred to the tubular reactor of polyamide synthesis system.

Statement 70 provides a kind of device being used to prepare polyamide, and described device includes：Heater, the heater configuration It is to heat the first flowable heat transmission medium to provide heated first flowable heat transmission medium；First heat exchanger, institute First heat exchanger is stated to be configured to transmit heat from the heated first flowable heat transmission medium to provide heated the Two flowable heat transmission mediums；And second heat exchanger, the second heat exchanger are configured to heat from described heated Two flowable heat transmission mediums are transferred to the tubular reactor of polyamide synthesis system.

Statement 71 provides the device described in statement 70, wherein the tubular reactor includes about 50 to about 300 meters of length.

Statement 72 provides the device described in any one of statement 70-71, wherein the tubular reactor includes about 75- 125 meters of length.

Statement 73 provides the device described in any one of statement 70-72, wherein the tubular reactor includes about 10cm To the internal diameter of about 80cm.

Statement 74 provides the device described in any one of statement 70-73, wherein the tubular reactor includes about 25cm To the internal diameter of about 60cm.

Statement 75 provides the device described in any one of statement 70-74, wherein the length/diameter of the tubular reactor (L/D) it is about 50 to about 2500.

Statement 76 provides the device described in any one of statement 70-75, wherein the length/diameter of the tubular reactor (L/D) it is about 100 to about 500.

Statement 77 provides the device described in any one of statement 70-76, wherein the tubular reactor includes along its length The floss hole of degree.

Statement 78 provides the device described in statement 77, wherein the tubular reactor includes about 5 to about 50 floss holes.

Statement 79 provides the device described in statement any one of 77-78, wherein the tubular reactor include about 10 to About 25 floss holes.

Statement 80 provides the device described in any one of statement 77-79, wherein the tubular reactor includes along described Average often about 3 meters to about 9 meters about 1 floss holes of the length of tubular reactor.

Statement 81 provides the device described in any one of statement 77-80, wherein the tubular reactor includes along described Average often about 2 meters to about 15 meters about 1 floss holes of the length of tubular reactor.

Statement 82 provides the device described in any one of statement 77-81, wherein the tubular reactor includes along described About 2 meters to about 15 meters of equispaced between the floss hole of the length of tubular reactor.

Statement 83 provides the device described in any one of statement 77-82, wherein the tubular reactor includes along described About 3 meters to about 9 meters of equispaced between the floss hole of the length of tubular reactor.

Statement 84 provides the device described in any one of statement 77-83, wherein the floss hole is connected to floss hole pipe Line, the method includes injecting water into the floss hole pipeline.

Statement 85 provides the device described in any one of statement 70-84, and wherein the method is not closing the tubular type Reactor is for carrying out at least about 1 to about 5 year in the case of clean.

Statement 86 provides the device described in any one of statement 70-85, and wherein the method is not closing the tubular type Reactor is for carrying out at least about 2.5 to about 3 years in the case of clean.

Statement 87 provides the device described in statement 70-86, wherein the device for being used to prepare polyamide is configured to by straight The dicarboxylic acids of chain and the diamines synthesizing polyamides of straight chain are formed by oligomer conjunction by the dicarboxylic acids of straight chain and the diamines of straight chain At polyamide.

Statement 88 provides the device described in statement 87, wherein the dicarboxylic acids has structure HO C (O)-R¹- C (O) OH, Middle R¹It is C₁-C₁₅Alkylidene.

Statement 89 provides the device described in statement 88, wherein the dicarboxylic acids is adipic acid.

Statement 90 provides the device described in any one of statement 87-89, wherein the diamines has structure H₂N—R²- NH₂, wherein R²It is C₁-C₁₅Alkylidene.

Statement 91 provides the device described in statement 90, wherein the diamines is hexamethylene diamine.

Statement 92 provides the device described in any one of statement 87-91, wherein the polyamide is nylon-6,6.

Statement 93 provides the device described in any one of statement 70-92, wherein in standard temperature and pressure (STP), described first Flowable heat transmission medium has the vapour pressure lower than the described second flowable heat transmission medium.

Statement 94 provides the device described in any one of statement 70-93, wherein the second heated flowable heat Transfer medium has the vapour pressure higher than the first heated flowable heat transmission medium.

Statement 95 provides the device described in any one of statement 70-94, wherein the second heated flowable heat Transfer medium is at least one of more flammable and more inflammable than the first heated flowable heat transmission medium.

Statement 96 provides the device described in any one of statement 70-95, wherein the first flowable heat transmission medium Including at least one of the following：Water, polyethylene glycol, polypropylene glycol, mineral oil, silicone oil, diphenyl ether and biphenyl.

Statement 97 provides the device described in any one of statement 70-96, wherein the first flowable heat transmission medium It is at least one of the following：Trimethylpentane, C_10-13Alkane, C_10-13Isoalkane, C_14-30Alkylaryl compounds, two Ethylbenzene, the benzene of vinylation, cyclohexyl benzene, C_14-30Alkylbenzene, paraffin oil, ethyl diphenyl ethane, diphenylethane, diethyl two Diphenylphosphino ethane, diphenyl ether, dipheny oxide, ethylbenzene polymer, biphenyl, inorganic salts, diisopropyl biphenyl, tri isopropyl biphenyl, first Butylcyclohexane, dicyclohexyl, terphenyl, the terphenyl of hydrogenation, partially hydrogenated quaterphenyl, partially hydrogenated more advanced polyphenyl, Diphenyl ether and phenanthrene, biaryl compound, tri-aryl compounds, diaryl ether, triaryl ether, alkylaryl compounds, alkyl virtue Based compound and diaryl alkane based compound.

Statement 98 provides the device described in any one of statement 70-97, wherein the first heated flowable heat Transfer medium is about 280 DEG C to about 400 DEG C.

Statement 99 provides the device described in any one of statement 70-98, wherein the first heated flowable heat Transfer medium is about 330 DEG C to about 350 DEG C.

Statement 100 provides the device described in any one of statement 70-99, wherein the first flowable heat is transmitted and is situated between Matter and the first heated flowable heat transmission medium are basic liquid phases.

Statement 101 provides the device described in any one of statement 70-100, wherein being passed by the described first flowable heat During passing medium heating, the first flowable heat transmission medium is substantially maintained as liquid.

Statement 102 provides the device described in any one of statement 70-101, wherein being passed by the described first flowable heat During passing medium heating, do not occur the gasification of the described first flowable heat transmission medium substantially.

Statement 103 provides the device described in any one of statement 70-102, wherein being passed by the described first flowable heat During passing medium heating, the heat for being transferred to the described first flowable heat transmission medium includes substantially all sensible heat.

Statement 104 provides the device described in statement any one of 70-103, wherein by heat from described heated the During one flowable heat transmission medium is transferred to the described second flowable heat transmission medium, described heated first can flow Dynamic heat transmission medium is substantially maintained as liquid.

Statement 105 provides the device described in statement any one of 70-104, wherein by heat from described heated the During one flowable heat transmission medium is transferred to the described second flowable heat transmission medium, do not occur the heating substantially The condensation for the first flowable heat transmission medium crossed.

Statement 106 provides the device described in statement any one of 70-105, wherein by heat from described heated the It, can from described heated first during one flowable heat transmission medium is transferred to the described second flowable heat transmission medium It includes substantially all sensible heat to flow the heat that heat transmission medium transmits.

Statement 107 provides the device described in any one of statement 70-106, wherein the first flowable heat is transmitted and is situated between Matter and the first heated flowable heat transmission medium are arranged in the first heating circuit.

Statement 108 provides the device described in statement any one of 70-107, wherein by heat from described heated first Flowable heat transmission medium is transferred to the described second flowable heat transmission medium and provides the used first flowable heat transmission Medium, the method further include that the used first flowable heat transmission medium is recycled back to described first is flowable The heating of heat transmission medium.

Statement 109 provides the device described in any one of statement 70-108, wherein the second flowable heat is transmitted and is situated between Matter is at least one of the following：Water, polyethylene glycol, polypropylene glycol, mineral oil, silicone oil, diphenyl ether, biphenyl and three Benzene.

Statement 110 provides the device described in any one of statement 70-109, wherein the second flowable heat is transmitted and is situated between Matter is at least one of the following：Trimethylpentane, C^10-13Alkane, C10^-13Isoalkane, C_14-30Alkylaryl compounds, Diethylbenzene, the benzene of vinylation, cyclohexyl benzene, C_14-30Alkylbenzene, paraffin oil, ethyl diphenyl ethane, diphenylethane, diethyl Diphenylethane, diphenyl ether, dipheny oxide, ethylbenzene polymer, biphenyl, inorganic salts, diisopropyl biphenyl, tri isopropyl biphenyl, It is hexahydrotoluene, dicyclohexyl, terphenyl, the terphenyl of hydrogenation, partially hydrogenated quaterphenyl, partially hydrogenated more advanced poly- Benzene, diphenyl ether and phenanthrene, biaryl compound, tri-aryl compounds, diaryl ether, triaryl ether, alkylaryl compounds, alkyl Aryl compound and diaryl alkane based compound.

Statement 111 provides the device described in statement any one of 70-110, wherein described heated second is flowable Heat transmission medium is about 210 DEG C to about 350 DEG C.

Statement 112 provides the device described in statement any one of 70-111, wherein described heated second is flowable Heat transmission medium is about 260 DEG C to about 300 DEG C.

Statement 113 provides the device described in statement any one of 70-112, wherein described heated second is flowable Heat transmission medium is basic liquid phase.

Statement 114 provides the device described in statement any one of 70-113, wherein described heated second is flowable Heat transmission medium is substantially gas phase.

Statement 115 provides the device described in statement any one of 70-114, wherein by heat from described heated the During one flowable heat transmission medium is transferred to the described second flowable heat transmission medium, the second flowable heat is transmitted Medium essentially becomes gas.

Statement 116 provides the device described in statement any one of 70-115, wherein by heat from described heated the During one flowable heat transmission medium is transferred to the described second flowable heat transmission medium, the second flowable heat is transmitted Medium is by substantially all gasification.

Statement 117 provides the device described in any one of statement 70-116, wherein second heat transmission medium and institute The second heated heat transmission medium is stated to be arranged in the second heating circuit.

Statement 118 provides the device described in statement 117, wherein second heating circuit configuration in order to control described second can The pressure for flowing heat transmission medium, to control the temperature of the described second flowable heat transmission medium gasification.

Statement 119 provides the device described in statement 118, wherein being gasified by controlling the described second flowable heat transmission medium Temperature control the temperature of the tubular reactor.

Statement 120 provides the device described in statement any one of 70-119, wherein by heat from described heated the During one flowable heat transmission medium is transferred to the described second flowable heat transmission medium, it is flowable to be transferred to described second The heat of heat transmission medium includes substantially all of latent heat, and the latent heat includes heat of gasification.

Statement 121 provides the device described in statement any one of 70-120, wherein by heat from described heated the During one flowable heat transmission medium is transferred to the described second flowable heat transmission medium, it is flowable to be transferred to described second The heat of heat transmission medium includes：About 70-100% latent heat for including heat of gasification, and about 0-30% sensible heats.

Statement 122 provides the device described in statement any one of 70-121, wherein by heat from described heated the During two flowable heat transmission mediums are transferred to the tubular reactor, the second heated flowable heat, which is transmitted, to be situated between Matter is substantially condensed into liquid.

Statement 123 provides the device described in statement 122, and described device further includes controller, and the controller is configured to control It makes the pressure of the second heated flowable heat transmission medium and is situated between with adjusting the second heated flowable heat and transmitting The temperature at least partly condensed described in matter experience.

Statement 124 provides the device described in statement 123, wherein being transmitted by controlling the second heated flowable heat The medium temperature that at least partly condenses of experience controls the temperature of the tubular reactor.

Statement 125 provides the device described in statement any one of 123-124, wherein second heat transmission medium and Heated second heat transmission medium is arranged in the second heat cycles, wherein it is flowable to control described heated second The pressure of heat transmission medium includes the pressure in control second heat cycles.

Statement 126 provides the device described in statement 125, wherein it includes control to control the pressure in second heating circuit The saturation temperature of the second heated flowable heat transmission medium.

Statement 127 provides the device described in statement 126, wherein the second heated flowable heat transmission medium is most High-temperature is in the range of about 0-40 DEG C of the saturation temperature of the second heated flowable heat transmission medium.

Statement 128 provides the device described in statement any one of 70-127, wherein by heat from described heated the During two flowable heat transmission mediums are transferred to the tubular reactor, transmitted from the second heated flowable heat The heat that medium transmits includes substantially all of latent heat, and the latent heat includes heat of gasification.

Statement 129 provides the device described in statement any one of 70-128, wherein by heat from described heated the During two flowable heat transmission mediums are transferred to the tubular reactor, transmitted from the described second flowable heat transmission medium Heat include：About 70-100% latent heat for including heat of gasification, and about 0-30% sensible heats.

Statement 130 provides the device described in statement any one of 70-129, wherein by heat from described heated second Flowable heat transmission medium is transferred to the tubular reactor of the polyamide synthesis system, and to provide used second flowable Heat transmission medium, the method further include that the used second flowable heat transmission medium is recycled back to from described In the transmission of the heat of the first heated flowable heat transmission medium.

Statement 131 provides the device described in statement any one of 70-130, wherein by heat from described heated second The tubular reactor that flowable heat transmission medium is transferred to the polyamide synthesis system includes by the polyamide synthesis system The temperature of tubular reactor be maintained at about 150 DEG C to about 350 DEG C.

Statement 132 provides the device described in statement any one of 70-131, wherein by heat from described heated second The tubular reactor that flowable heat transmission medium is transferred to the polyamide synthesis system includes by the polyamide synthesis system The temperature of tubular reactor be maintained at about 210 DEG C to about 260 DEG C.

Statement 133 provides the device described in statement any one of 70-132, wherein by heat from described heated second The tubular reactor that flowable heat transmission medium is transferred to the polyamide synthesis system includes mixing polyamide in reactor The temperature of object is maintained at about 218 DEG C to about 250 DEG C.

Statement 134 provides the device described in statement any one of 70-133, wherein by heat from described heated first Flowable heat transmission medium is transferred to the described second flowable heat transmission medium and provides the used first flowable heat transmission Medium, wherein the second heat exchanger is configured to heat from the used first flowable heat transmission medium or from described The first heated flowable heat transmission medium is transferred to the flowable heat transmission medium of third, flowable with the third for providing heating Heat transmission medium, described device further include third heat exchanger, and the third heat exchanger arrangement is by heat from described heated The flowable heat transmission medium of third be transferred at least one component for accommodating polyamide of the polyamide synthesis system, packet Include at least one of pre-heater, evaporator, polymer reactor, flash vessel, finisher and autoclave.

Statement 135 provides the device described in statement 134, is situated between wherein heat is transmitted from the flowable heat of the heated third At least one component for the polyamide synthesis system that matter is transferred to is different from the tubular reactor.

Statement 136 provide it is a kind of prepare nylon-6,6 device, described device includes：Heater, the heater configuration For that will include the first flowable heat transmission medium heating of terphenyl, to provide heated first flowable heat transmission medium； First heat exchanger, the first heat exchanger are configured to transmit heat from the first heated flowable heat transmission medium To including the second flowable heat transmission medium of diphenyl ether and biphenyl, with provide the flowable heat transmission medium of heated second with Used first flowable heat transmission medium, and the used first flowable heat transmission medium is recycled back to The first heat exchanger, wherein the first flowable heat transmission medium, the first heated flowable heat transmission medium and The used first flowable heat transmission medium is arranged in the first heating circuit, is transmitted by the described first flowable heat Medium, which heats and heat is transferred to the described second flowable heat and is transmitted from the first heated flowable heat transmission medium, to be situated between During matter, the first flowable heat transmission medium, the first heated flowable heat transmission medium and described make Used first flowable heat transmission medium is basic liquid phase, be transferred to the described first flowable heat transmission medium heat and The heat transmitted from the described first flowable heat transmission medium includes substantially all sensible heat, and by heat from described heated During first flowable heat transmission medium is transferred to the described second flowable heat transmission medium, the second flowable heat passes Medium is passed by substantially all gasification；And second heat exchanger, the second heat exchanger are configured to heat from the heating The the second flowable heat transmission medium crossed is transferred to the tubular reactor of polyamide synthesis system, to provide used second Flowable heat transmission medium, and the used second flowable heat transmission medium is recycled back to from the heating In the transmission of the heat for the first flowable heat transmission medium crossed, wherein the second flowable heat transmission medium and described heated the Two flowable heat transmission mediums are arranged in the second heating circuit, and second heat passes in order to control for the second heating circuit configuration Pull over road pressure to control the saturation temperature of the described second flowable heat transmission medium, wherein being controlled by controlling saturation temperature Make the temperature of the tubular reactor, the second flowable heat transmission medium of the second flowable heat transmission medium and the use It is basic liquid phase, the second heated flowable heat transmission medium is basic liquid phase, and is transferred to described The heat of second flowable heat transmission medium and the heat transmitted from the described second flowable heat transmission medium include about 70-100% Latent heat (latent heat includes heat of gasification), and about 0-30% sensible heat；The wherein described tubular reactor includes about 75 to about 125 meters of length, the tubular reactor include internal diameters of the about 25cm to about 60cm, the tubular reactor include about 100 to About 500 length/diameter (L/D), and the wherein described tubular reactor includes about 10 to about 25 floss holes along its length.

Statement 137 provide will state 1-136 described in either one or two of or the device or method that arbitrarily combine, described device or Method is optionally configured so that all elements or option may be used in or select.

Claims

1. a kind of method preparing polyamide, the method includes：

By the first flowable heat transmission medium heating, to provide heated first flowable heat transmission medium, wherein described the One flowable heat transmission medium and the first heated flowable heat transmission medium are basic liquid phases；With

Heat is transferred to the second flowable heat transmission medium from the first heated flowable heat transmission medium, is added with providing The second flowable heat transmission medium that heat is crossed；With

Heat is transferred to the tubular reactor of polyamide synthesis system from the second heated flowable heat transmission medium,

The wherein described tubular reactor includes the internal diameter of 50 to 300 meters of length and 10cm to 80cm.

2. method described in claim 1, wherein the tubular reactor includes 75 to 125 meters of length.

3. method described in claim 1, wherein the tubular reactor includes the internal diameter of 25cm to 60cm.

4. method described in claim 1, wherein the length/diameter (L/D) of the tubular reactor is 50 to 2500.

5. method described in claim 1, wherein the tubular reactor includes floss hole along its length.

6. the method described in claim 5, wherein the tubular reactor includes being averaged for the length along the tubular reactor Every 3 meters to 9 meters 1 floss holes.

7. the method described in claim 5, wherein the tubular reactor includes the discharge along the length of the tubular reactor 2 meters to 15 meters of equispaced between mouthful.

8. the method described in claim 5, wherein the floss hole is connected to floss hole pipeline, the method includes injecting water into To in the floss hole pipeline.

9. method described in claim 1, wherein the method are not closing the tubular reactor for clean It carries out at least 1 to 5 year.

10. method described in claim 1, wherein the polyamide is nylon-6,6.

11. method described in claim 1, wherein the first heated flowable heat transmission medium is 280 DEG C to 400 ℃。

12. method described in claim 1, wherein being transferred to institute from the first heated flowable heat transmission medium in heat During stating the second flowable heat transmission medium, the heat transmitted from the first heated flowable heat transmission medium includes Substantially all sensible heat.

13. method described in claim 1, wherein heat is transferred to institute from the first heated flowable heat transmission medium It states the second flowable heat transmission medium and provides the used first flowable heat transmission medium, the method further includes will be described Used first flowable heat transmission medium is recycled back to the heating of the described first flowable heat transmission medium.

14. method described in claim 1, wherein heat to be transferred to from the first heated flowable heat transmission medium During the second flowable heat transmission medium, the second flowable heat transmission medium substantially becomes gas.

15. method described in claim 1, wherein heat to be transferred to from the first heated flowable heat transmission medium During the second flowable heat transmission medium, the heat for being transferred to the described second flowable heat transmission medium includes： The latent heat and 0-30% sensible heats including heat of gasification of 0-100%.

16. method described in claim 1, wherein described heat to be transferred to from the second heated flowable heat transmission medium During tubular reactor, the heat transmitted from the described second flowable heat transmission medium includes：70-100%'s includes gasification The latent heat and 0-30% sensible heats of heat.

17. method described in claim 1, wherein heat is transferred to institute from the second heated flowable heat transmission medium It includes that the temperature of the tubular reactor is maintained at 150 DEG C to 350 DEG C to state tubular reactor.

18. nylon-6 is prepared a kind of, 6 method, the method includes：

By the first flowable heat transmission medium heating including terphenyl, it is situated between with providing the flowable heat of heated first and transmitting Matter；

Heat is transferred to the including diphenyl ether and biphenyl second flowable heat from the first heated flowable heat transmission medium to pass Medium is passed, to provide the flowable heat transmission medium of heated second and used first flowable heat transmission medium, wherein

The first flowable heat transmission medium, the first heated flowable heat transmission medium and described used First flowable heat transmission medium is arranged in the first heating circuit,

The described first flowable heat transmission medium heating and heat from the first heated flowable heat transmission medium to In the transmittance process of the second flowable heat transmission medium, the first flowable heat transmission medium, described heated One flowable heat transmission medium and the used first flowable heat transmission medium are substantially liquid phase,

The heat packet for being transferred to the heat of the described first flowable heat transmission medium and being transmitted from the described first flowable heat transmission medium Substantially all sensible heat is included, and

Heat is being transferred to the described second flowable heat transmission medium from the first heated flowable heat transmission medium In the process, the described second flowable heat transmission medium is substantially all is gasified；

The used first flowable heat transmission medium is recycled back to adding for the described first flowable heat transmission medium Heat；

Heat is transferred to the tubular reactor of polyamide synthesis system from the second heated flowable heat transmission medium, from And the used second flowable heat transmission medium is provided, wherein

Second flowable heat transmission medium and the second heated flowable heat transmission medium are arranged in the second heating circuit In,

Second flowable heat transmission medium and the used second flowable heat transmission medium are basic liquid phases,

The second heated flowable heat transmission medium is basic liquid phase, and

It is transferred to the heat of the described second flowable heat transmission medium, and the heat transmitted from the described second flowable heat transmission medium Including：The latent heat and 0-30% sensible heats including heat of gasification of 70-100%；

The pressure of second heating circuit is controlled to control the saturation temperature of the described second flowable heat transmission medium, wherein logical It crosses and controls the temperature that the saturation temperature controls the tubular reactor；With

The used second flowable heat transmission medium is recycled back to from the first heated flowable heat In the transmission of the heat of transfer medium；

The wherein described tubular reactor includes 75 to 125 meters of length, and the tubular reactor includes the internal diameter of 25cm to 60cm, The tubular reactor includes 100 to 500 length/diameter (L/D), and the wherein described tubular reactor includes along its length 10 to 25 floss holes.

19. a kind of system being used to prepare polyamide, the system comprises：

Tubular reactor,

Heater, the heater configuration are the first flowable heat transmission medium of heating to provide heated first flowable heat Transfer medium, wherein the first flowable heat transmission medium and the first heated flowable heat transmission medium are basic Liquid phase；

First heat exchanger, the first heat exchanger are configured to heat from the first heated flowable heat transmission medium It transmits to provide heated second flowable heat transmission medium；With

Second heat exchanger, the second heat exchanger are configured to heat from the second heated flowable heat transmission medium It is transferred to the tubular reactor,