CN204058323U

CN204058323U - Effluent mixed cell

Info

Publication number: CN204058323U
Application number: CN201420173445.5U
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 Technologies SARL Switzerland
Current assignee: Invista North America LLC
Priority date: 2013-05-01
Filing date: 2014-04-10
Publication date: 2014-12-31
Anticipated expiration: 2024-04-10
Also published as: TWM502033U

Abstract

The application relates to a kind of effluent mixed cell, and described effluent mixed cell comprises: at least one upstream entrance, at least one mixing section and at least one lower exit; Wherein each upstream entrance is configured to the main polymeric amide stream pipeline of the polymeric amide be substantially polymerized from described continuous polymeric amide production system to shunt; At least one mixing section wherein said is configured to additive to mix with the polymeric amide be substantially polymerized shunted by least one in described upstream entrance; And wherein each described lower exit is placed in the upstream of polymeric amide forcing machine or polyamide thread material forming unit.

Description

Effluent mixed cell

The cross reference of related application

This application claims the benefit of priority of the U.S. Provisional Patent Application numbers 61/818,217 submitted on May 1st, 2013, it is open is combined in this with its full content by reference.

Technical field

The application relates to the effluent being mixed for polymeric amide synthesis.

Background technology

It is problematic for adding to the additive in polymeric amide in continuous methods for production of polyamides.If additive mixes with reaction-ure mixture by the course of the polymerization process early stage, treatment facility can become the degraded product dirtization being added agent and additive.If mixed with the polymeric amide be substantially polymerized by additive, it is difficult for mixing, because polymeric amide is very sticky.In addition, additive solvent can upset polyreaction, such as, especially, if solvent is water.Water is the product of polyreaction.A large amount of water can drive polyreaction in the opposite direction or cause side reaction.

Impurity can or be introduced in polymeric amide by additive agent mixture or as the result of the reaction between the component of polyblend and additive or its solvent.Polymerization reaction mixture is melting form.When introducing additive, heating can promote that by product is formed.Polyblend experiences decompression usually to contribute to driving polyreaction forward.The viscosity of polyblend makes to need pumping or other power to pass through production system with mobile polymkeric substance usually.Pressure difference between additive solution and polyblend can cause (blow back) fouling to additive entrance neutralization additive feeding unit that refluxes.

Can by additive and polymer support (also referred to as thinner) pre-mixing.Additive and the polymkeric substance of this pre-mixing are commonly called " masterbatch ".Although the use of masterbatch can overcome comparatively early introduce some adjoint problems of additive in the method, inject carrier polymer self and can bring problem (if it is not identical with the reaction product of carried out polyreaction).If carrier polymer is different from reaction product, so carrier polymer becomes impurity in the product.Even if carrier polymer has the chemical formula substantially similar to product, carrier polymer can be upper different in the polymerization degree (as reflected by molecular weight).Therefore a kind of method and apparatus for the mode that undesirable impurity is introduced in product stream not to be introduced additive to utilize the mixing benefit of master batch operations is completely provided by needing.

Summary of the invention

This document describes the system and method in order to be mixed to by additive in polymerizing polyamide logistics, it can solve insufficient mixing, pollutent is introduced, by product is formed and the problem of equipment scaling.

In one aspect of the invention, provide a kind of effluent mixed cell, described effluent mixed cell comprises:

At least one upstream entrance, at least one mixing section and at least one lower exit;

Wherein each upstream entrance is configured to the main polymeric amide stream pipeline of the polymeric amide be substantially polymerized from described continuous polymeric amide production system to shunt;

At least one mixing section wherein said is configured to additive to mix with the polymeric amide be substantially polymerized shunted by least one in described upstream entrance; And

Wherein each described lower exit is placed in the upstream of polymeric amide forcing machine or polyamide thread material forming unit.

An example of this system is a kind of polymeric amide production system continuously, and described system comprises:

Effluent mixed cell, described effluent mixed cell has at least one upstream entrance, at least one mixing section and at least one lower exit;

Wherein effluent unit is parallel to the main polymeric amide stream pipeline arrangement of continuous polymeric amide production system;

Effluent mixed cell also can comprise at least one additive reservoir, at least one pump, at least one impeller, at least one mixing tank, at least one under meter, one or more discharge outlet (vent), or their combination.

Continuous polymeric amide production system can comprise reactant reservoir, vaporizer, polymerization reactor, batch reactor flasher, finisher (finisher), polyamide thread material forming unit, forcing machine, and their combination.

What also describe herein is use the method with this system of this effluent mixed cell.Such as, a kind of for by additive, the method be mixed in polymerizing polyamide logistics comprises:

Substantially a the polymeric amide be polymerized is shunted from the upstream line continuous polymeric amide production system to produce polymeric amide effluent by ();

B additive is mixed in polymeric amide effluent to produce polymeric amide-additive side mixture by (); With

C () makes polymeric amide-additive side mixture be back to downstream line in system to produce polymeric amide-additive main flow;

Wherein, when shunting, the polymeric amide be substantially polymerized from upstream line has the water-content of about 0.1%-3 % by weight.

Accompanying drawing explanation

Fig. 1 is the schematic diagram of the example feature that can comprise in example effluent mixed cell described herein, and it is a part for continuous polymeric amide production system.

Embodiment

As described herein, additive can be problematic to adding of polymerizing polyamide mixture, adds pollutent and side product can be caused to be formed because this, and equipment scaling.When polymerizing polyamide mixture becomes sticky, additive is problematic to the Homogeneous phase mixing in mixture.Do not have the required polymeric amide the mixed equably-additive product of impurity, by product and gel (the Disordered solid material of oxidation or thermal degradation products such as, can be comprised) can obtain by using method described herein and effluent mixed cell.Polymeric amide can be the polymeric amide of any appropriate, as nylon 6, nylon 7, nylon 11, nylon 12, nylon 6,6, nylon 6,9; Nylon 6,10, nylon 6,12, or their multipolymer.

Effluent mixed cell described herein can be configured in the position of being substantially polymerized by polymeric amide in continuous polymeric amide production system.Such as, the polymeric amide be substantially polymerized branched in effluent mixed cell can have and is less than 5 % by weight, or is less than 2 % by weight, or is less than the water-content of 1.5 % by weight.Can the main flow of the amount of any appropriate be branched in effluent mixed cell, according to appointment 0.01 % by weight to about 99.9 % by weight, about 1 % by weight to about 80 % by weight, about 1 % by weight to about 30 % by weight, about 0.01 % by weight or less, 0.1 % by weight, 1,2,3,4,5,10,15,20,25,30,35,40,45,50,55,60,65,70,75,80,85,90,95,96,97,98,99,99.9 % by weight or about 99.99 % by weight or more.The flow velocity of any appropriate can be had from its main flow of taking out shunting stream, 1L/ minute to about 1 according to appointment, 000,000L/ minute, or about 10L/ minute to about 100,000L/ minutes, or about 1L/ minute or lower, 10L/ minute, 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.

The fouling (such as, by additive, pollutent and additive-polymeric by-products fouling) of the equipment adopted in the early process of polymerization process is avoided in this arrangement.Therefore, in order to reduce the equipment of the water-content of reactant as vaporizer, in order to promote the reactor of the polymerization of reactant, and to remain in order to the flasher unit of the molecular weight increasing polymkeric substance and there is no pollutent, additive and byproducts build-up, this can be produced by the early stage introducing of additive to polymerization process.Pollutent, additive and by product can be accumulated on equipment, such as, on heating surface, at the irregular place of equipment surface, and in the flowing of polyblend, occur the position of vortex.This gathering can cause other problematic materials as the formation of gel and accumulation.

Effluent mixed cell described herein is configured in continuous polymeric amide production system in the position that polymeric amide is polymerized substantially.But the position of effluent mixed cell described herein also before the extruding of polyamide products of polymerization is configured in continuous polymeric amide production system.In extrusion, adding of additive can introduce solvent and other material, and it adversely can affect the quality of polyamide products.The effluent mixed cell that position before the extruding of polyamide products of polymerization is configured in production system allows the further process of additive solvent, mixes and remove.

Such as, in continuous polymeric amide production system, effluent mixed cell can be placed in finisher unit right on or finisher unit right astern.

This point in production system, polyblend is polymerized substantially.Compare with the polyblend of the commitment in system, the water-content of mixture significantly reduces.Such as, the water-content of the polymeric amide be substantially polymerized when branching in effluent mixed cell can be less than about 2 % by weight.Water-content can be low to moderate about 1 % by weight or even lowly reach about 0.1 % by weight.Such as, the water-content of the polymeric amide be substantially polymerized when branching in effluent mixed cell can be less than 0.9%, be less than 0.7%, be less than 0.6%, be less than 0.5%, be less than 0.4%, be less than 0.3% or be less than 0.2%.

Substantially the polymeric amide be polymerized, when branching in effluent mixed cell, is viscosity.Such as, the polymeric amide be substantially polymerized can have about 2.3 to 100, or 9-20, or the relative viscosity of 30-100, as measured by method described herein.The relative viscosity of the polymeric amide be substantially polymerized can than the relative viscosity of the original stock of subelement before the polymerization at least about 0.4.

Usually, effluent mixed cell is configured to receive the polymeric amide that is substantially polymerized to produce polymeric amide effluent from the upstream line of continuous polymeric amide production system.Additive is mixed produce polymeric amide-additive side mixture with polymeric amide effluent after effluent mixed cell, and downstream line polymeric amide-additive side mixture being back to continuous polymeric amide production system is to produce polymeric amide-additive main flow.Can by polymeric amide-additive main flow mixing to produce uniform polymeric amide-additive product substantially.This mixing of polymeric amide-additive main flow can appear in downstream line or in the separate chamber of continuous polymeric amide production system.

Additive can be the additive of any appropriate.Such as, additive can be polymerizing catalyst, end-capping reagent (such as, to stop polymerization), thermo-stabilizer (such as, contributing to the thermoinducible oxidation reducing or prevent polymkeric substance), photostabilizer (such as, contributing to the photoxidation reducing or prevent polymkeric substance), lubricant (such as, reduces viscosity, increase workability), biocide, tinting material, toughener (such as, polymkeric substance being gained in strength or hardness), weighting agent (cost such as, reducing polymkeric substance or the character improving polymkeric substance are as intensity or hardness), fire retardant, fluoropolymer (such as, malleableize, compatibilized, promote to adhere to or increase snappiness), ANTIMONY TRIOXIDE SB 203 99.8 PCT (such as, fire retardant), polycaprolactone (such as, increasing the shock-resistance of handlability or raising resulting polymer), matting agent, titanium dioxide (such as, anatase octahedrite or rutile-type, the matting agent of 0.0001 % by weight to about 0.05 % by weight or about 0.01 % by weight, about 0.05 % by weight to about 5 % by weight or about 0.1 % by weight to about 1 % by weight or about 0.1 % by weight to about 0.3 % by weight brighten tinting material), zinc sulphide (such as, matting agent), or their combination.Additive can be dyestuff, pigment, glass fibre, fibrous magnesium silicate, carbon fiber, Kevlar, gypsum fiber, Calucium Silicate powder, kaolin, calcined kaolin, wollastonite, talcum, chalk, phosphoric acid ester, phosphoric acid, phosphorous acid ester, phosphinate, phosphorous acid ester, organo-phosphine oxide, sodium hypophosphite, acetic acid, propionic acid, phenylformic acid, succsinic acid, vinylidene fluoride, R 1216, chlorotrifluoroethylene, tetrafluoroethylene, perfluoralkyl perfluorovinyl ether or their combination.Additive can occur with the concentration of any appropriate in the polymer, as 0.000, 001g/L or lower, 0.000, 005g/L, 0.000, 01, 0.000, 05, 0.000, 1, 0.000, 5, 0.001, 0.005, 0.01, 0.05, 0.1, 0.5, 1, 2, 3, 4, 5, 10, 15, 20, 30, 35, 40, 45, 50, 75 or about 100g/L or higher, or about 0.000, 001 % by weight or lower, or about 0.000, 005 % by weight, 0.000, 01, 0.000, 05, 0.000, 1, 0.000, 5, 0.001, 0.005, 0.01, 0.05, 0.1, 0.5, 1, 2, 3, 4, 5, 10, 15, or about 20 % by weight or higher.Additive can be added to main flow in pure form, or be diluted in suitable solid support material, as solvent (such as, water or organic solvent) or as polymer support, as having the polymer support of the composition substantially the same with host polymer stream.Additive can be added to main flow with following ratio: 0.000, 001g additive/L carrier current or lower, or 0.000, 005g/L, 0.000, 01, 0.000, 05, 0.000, 1, 0.000, 5, 0.001, 0.005, 0.01, 0.05, 0.1, 0.5, 1, 2, 3, 4, 5, 10, 15, 20, 25, 30, 35, 40, 45, 50, 75, 100, 150, 200, 250, 300, 350, 400, 450g/L, or about 500g/L or higher, or about 0.001-20 % by weight, or about 0.01-15 % by weight, or about 0.01-10 % by weight, or about 0.1-10 % by weight, or about 0.1-9 % by weight, or about 0.01-8 % by weight, or about 0.01-7 % by weight, or about 0.01-6 % by weight, or about 0.01-5 % by weight, or about 0.1-3 % by weight.

Effluent mixed cell can comprise feature or the parts of certain number.Such as, effluent mixed cell can comprise at least one additive reservoir, at least one mixing section, one or more mixing tank, one or more heating unit, one or more cooling unit, one or more pump, one or more valve, one or more detector, one or more discharge outlet, and one or more connection line, it is for promoting that material is at least one additive reservoir, at least one mixing section, and the movement continuously between polymeric amide production system.

Effluent mixed cell can comprise a mixing section, or more than one mixing section.When there is more than one mixing section, mixing section can serial or parallel connection configuration.Such as, the mixing section of configured in series can allow the polymeric amide be substantially polymerized of increasing amount or additive to be sequentially introduced in a series of rooms of the ratio containing different polymeric amide and additive.Room can receive or containing the selected ratio of molten polyamide with additive, and after by polymeric amide and additive mixing, this mixture can be moved to the second Room, wherein by more polymeric amide of being substantially polymerized or additive introducing.After blending, polymeric amide-additive agent mixture can move to the 3rd Room, wherein introduces the more polymeric amide or additive etc. that are substantially polymerized.Thisly add the generation that can promote even polymeric amide-additive side mixture gradually, it has the additive of optimization and the ratio of polymeric amide, avoid being not only polymeric amide-additive side mixture, the side reaction also in final polymeric amide-additive product, polymer degradation, gel formation and the qualitative discordance of physics and chemistry simultaneously.

Therefore, effluent mixed cell can comprise, and method described herein can comprise, the mixing section of the certain number that series connection keeps, such as, and a series of 2-10 mixing section.Additive reservoir can may be operably coupled to the first mixing section in this string.Alternatively, each mixing section can be connected to masterbatch additive reservoir independently or be connected to separation, independent additive reservoir.The structure of effluent mixed cell also can change to make some mixing sections may be operably coupled to one or more additive reservoir, and other mixing section does not connect.

Effluent mixed cell can also comprise more than one mixing section, wherein mixing section parallel connection configuration.Such as, different mixing sections can may be operably coupled to different additive reservoirs individually.After dissimilar additive to the adding and mix of each mixing section, the inclusion of different mixing sections can be emptied into the different downstream position of main polymeric amide stream pipeline in continuous polymeric amide production system independently.Alternatively, the inclusion of the different mixing section be arranged in parallel can be emptied in larger masterbatch mixing section, be emptied to afterwards in the downstream position of main polymeric amide stream pipeline in continuous polymeric amide production system.This handiness allowed on the different position of the main flow different additives being incorporated into polymerizing polyamide reaction that is arranged in parallel of mixing section.Such as, additive that can be interact with each other under conc forms separately can be processed and is incorporated in main polymeric amide stream with rarer form afterwards.

Therefore effluent mixed cell can comprise, and method described herein can comprise, the mixing section of the certain number kept in parallel, such as, and the about 2-10 mixing section be arranged in parallel.One or more mixing sections of configuration in parallel can may be operably coupled at least one additive reservoir.

One or more mixing section can have at least one mixing tank separately.Multiple mixing tank can be adopted as arm mixer, ribbon-type blender, mixing screw, dual-shaft mixer, orbital shaker, double planetary mixer, high speed disperser, kneader, two kneaders etc.

One or more mixing section can have discharge outlet to allow volatile component (such as, water or additive solvent) to remove.This discharge outlet can also exist in one or more additive reservoir.

One or more mixing section can also be configured to mixture to keep under reduced pressure.

Effluent mixed cell can may be operably coupled to main polymeric amide stream pipeline in continuous polymeric amide production system to receive the polymeric amide be substantially polymerized from the upstream position in system and the downstream position be back to by polymeric amide-additive side mixture in system.

Effluent mixed cell can may be operably coupled to the main polymeric amide stream pipeline in continuous polymeric amide production system via stream pipeline and valve.At least one inlet valve can be placed in upstream position in main polymeric amide stream pipeline with the polymeric amide controlling substantially to be polymerized to the shunting in effluent mixed cell.This one or more inlet valve can be mounted to close to the junction between the main flow pipeline of polymeric amide production system and the shunting stream pipeline emptying the mixing section injecting effluent mixed cell.This structure can reduce the flow turbulence in main flow pipeline and avoid the foundation of the stagnation side pocket of polymeric amide (its can gelling block other part of inlet valve or unit or system).

In multiple embodiment, effluent mixed cell can have the inside of polishing, to contribute to preventing gel formation wherein or adhesion.By the partially polished degree to any appropriate of effluent mixed cell and be connected transmission pipeline and the inner any appropriate of valve, can reduce with the inside of the one or more parts making gel formation or adhere to effluent mixed cell.Term " mean roughness " (R _a) be the surperficial peak at those irregular places and the average value measured of paddy, and express with micron (μm) with microinch (μ in).Surface texturisation measurement is well known by persons skilled in the art and adopts surface topography device.Known surface topography device can derive from TAYLOR-HOBSON, company AMETEK, INC., 1100Cassatt Road, P.O.Box 1764, Berwyn, Pennsylvania, 19312 USA.In some instances, the glazed surface of the inside of side water vapour mixed cell can be the average surface roughness of any appropriate, as being not more than about 6.00 μm, about 1.00 μm to about 6.00 μm, about 0.90 μm to about 1.50 μm, about 0.60 μm to about 1.00 μm, be not more than about 0.5 μm, be not more than about 0.10 μm, about 0.10 μm to about 0.80 μm, or the average surface roughness of about 0.90 μm to about 1.50 μm.

Other inlet valve can be placed in the ingress of one or more mixing sections of effluent mixed cell to control or to regulate the stream of polymeric amide to one or more room be substantially polymerized.

One or more outlet valve can be placed in downstream position in main polymeric amide stream pipeline to control the emptying of one or more mixing section and polymeric amide-additive side mixture to entering in the main flow pipeline of polymeric amide production system.At least one outlet valve can be mounted to close to the junction between the downstream position of the main flow pipeline of polymeric amide production system and the stream pipeline of the mixing section of emptying effluent mixed cell.This outlet valve can be configured to the flow turbulence that reduces in main flow pipeline and avoid the foundation (its can gelling the part of clog downstream system) of the stagnation side pocket of polymeric amide.

Entrance and exit valve can may be operably coupled to one or more detector.Such as, entrance or outlet valve can may be operably coupled to flow detector with the monitoring of the volume or amount that allow to flow through the material of valve.Therefore, such as, detector can may be operably coupled to inlet valve with the volume making detector can monitor or regulate the polymeric amide be substantially polymerized being flowed through valve when branching in effluent mixed cell.When unit comprises this flow detector-inlet valve, valve program can turn to and cut out when the polymeric amide be substantially polymerized of selected volume is branched to effluent mixed cell.

Inlet valve alternately or dividually can may be operably coupled to the detector in one or more mixing section.Such as, this mixing section detector can detect the additive that when there is selected amount or volume in mixing section.When this mixing section detector may be operably coupled to inlet valve, inlet valve can be activated to open by detector and be branched in mixing section by the polymeric amide be substantially polymerized.Alternatively, mixing section detector can detect in mixing section the polymeric amide be substantially polymerized that when there is selected amount or volume.When this mixing section detector may be operably coupled to inlet valve, mixing section detector can activate inlet valve and cuts out to make it possible to the polymeric amide be substantially polymerized of selected volume to remain in mixing section and mix with additive.Therefore the combination of detector can be used to control when open and close one or more inlet valve.

One or more outlet valve can be placed in one or more pipelines that leave of drawing from the one or more mixing sections of effluent mixed cell to regulate the emptying of one or more mixing section.Similarly, outlet valve can be placed in the joint between the stream pipeline of the downstream position of the main flow pipeline of polymeric amide production system and the mixing section of emptying effluent mixed cell.

Outlet valve can may be operably coupled to one or more detector.Such as, detector can be placed in mixing section to monitor the temperature of material in mixing section, pressure or composition.In another example, detector can be placed in the joint left in pipeline or between the stream pipeline and the main flow pipeline of polymeric amide production system of emptying mixing section from mixing section.Detector in mixing section is passable, such as, the polymeric amide mixing detecting when additive and be substantially polymerized, or when in mixing section the composition of material there is selected composition, temperature or pressure.Mixing section detector can may be operably coupled to one or more outlet valve.One or more outlet valve can work as to be detected by the detector in mixing section selected to form, water-content, composition homogeneity, open when temperature or pressure.If the composition of material, temperature or pressure depart from selected composition, water-content, composition homogeneity, temperature or pressure in mixing section, mixing section detector also can may be operably coupled to one or more outlet valve to cut out this valve.

One or more flow monitoring detector also can be placed in leaving pipeline from mixing section extraction, or empties the joint of the stream pipeline of mixing section and the main flow pipeline of polymeric amide production system.This flow monitoring detector can may be operably coupled to one or more outlet valve to regulate polymeric amide-additive side mixture to the stream in the downstream line of polymeric amide production system.Such as, this flow monitoring detector can activate one or more outlet valve to reduce or to be increased to the volume of the polymeric amide-additive side mixture in the downstream line of polymeric amide production system.The adjustment of outlet valve can thus by detect polymeric amide-additive side mixture volume, form, the detector of temperature or pressure mediates.

One or more supplement valve can be placed between the mixing section of additive reservoir and effluent mixed cell.This supplement valve can opening and close to allow additive to flow in selected mixing section.One or more detector can may be operably coupled to one or more supplement valve.Such as, the detector that may be operably coupled to one or more supplement valve can detect the volume of additive, composition, temperature or pressure and activate the opening and closing of one or more supplement valve.Therefore, such as, when suitable additive volumetric flow is to mixing section, flow detector can activate the closedown of one or more supplement valve.When the temperature of additive, composition or pressure are in selected scope or when measuring parameter leap threshold value, supplement valve can open to be released in mixing section by additive.Similarly, when the temperature of additive, composition or pressure are outside selected scope, supplement valve can close or keep to close.

One or more supplement valve also can may be operably coupled to the one or more detectors in mixing section.Detector in mixing section can detect the composition of material in mixing section, temperature or pressure, as explained above.When mixing section detector detect select composition, temperature or pressure range time, mixing section detector can drive one or more supplement valve open and release additives in mixing section.If the composition of material, temperature or pressure depart from selected composition, temperature or pressure in mixing section, one or more mixing section detector can also may be operably coupled to one or more supplement valve with shut-off valve.

Effluent mixed cell can be configured to time durations material being mixed in mixing section any appropriate, to make to occur that enough mixing are to produce the substantially uniform mixture that preparation is back to main flow pipeline.Such as, substantially the mean time that the polymeric amide be polymerized spent before being back to downstream line in mixing section can be about 0.000,1s to about 1h, or about 0.001s was to about 30 minutes, or about 0.01s was to about 20 minutes, or about 0.000,1s or less, or about 0.001s, 0.01s, 0.1s, 0.5s, 1s, 2s, 3s, 4s, 5s, 10s, 15s, 20s, 30s, 40s, 50s, 1 minute, 1.5 minutes, 2 minutes, 3 minutes, 4 minutes, 5 minutes, 10 minutes, 15 minutes, 20 minutes, 25 minutes, 30 minutes, 40 minutes, 50 minutes or about 1h or more.

One or more heating unit can be configured to the temperature keeping material in effluent mixed cell.Such as, whole effluent mixed cell can enclose the indoor of thermal conditioning.Alternatively, the temperature of multiple pipelines of one or more additive reservoir, one or more mixing section, one or more valve and effluent mixed cell can be regulated respectively by independent heating unit.

The separate regulation of the temperature of the different parts of effluent mixed cell has some benefits.Such as, mixing section can be heated above additive reservoir and be in molten state to keep the polymeric amide be substantially polymerized in mixing section, avoid the thermolysis of heat sensitive additive simultaneously.If additive is heat sensitive, such as, it can be remained on lesser temps until before just entering in mixing section.Such as, by being heated in the pipeline extending to mixing section from additive reservoir by additive, additive can be heated to selected temperature.Also mixing section can be heated above or lower than the temperature of additive reservoir with the mixing promoting material in these parts of unit or reaction.

Therefore, effluent mixed cell can comprise one or more stream pipeline heating unit, one or more mixing section heating unit, one or more additive reservoir heating unit, and one or more valve heating unit.

Heating unit can may be operably coupled to thermostatted or other device respectively, and it can start or stop thermal output to regulate the temperature of parts in effluent mixed cell (such as, flowing pipeline, mixing section, additive reservoir or valve).

One or more cooling unit also can may be operably coupled to the parts of effluent mixed cell.This cooling unit can also may be operably coupled to thermostatted to start or to stop the cooling of parts of effluent mixed cell.Such as, cooling unit can be configured to cooling additive reservoir, or promotes the adjustment of temperature in additive reservoir.Although mixing section, valve and stream pipeline only may need cooling once in a while, cooling unit can may be operably coupled to these parts too, such as, to make the temperature of each parts remain in stated limit.

One or more mixing tank can be arranged in mixing section or additive reservoir with mixing material wherein.Mixing tank can promote that material mixing is to even.Mixing tank can be regulated by one or more detector thus with selected velocity or the mixing starting material in selected time durations.Such as, if additive water-content is significantly different from the water-content of the polymeric amide be substantially polymerized, detector mixing tank can be actuated to start the more tacky polymeric amide be substantially polymerized with the mixing of suitable speed and speed can introduce along with more additive and change.

One or more pump can be integrated in other parts of multiple stream pipeline and effluent mixed cell.Such as, one or more pump operationally can be integrated into and to draw from the upstream line continuous polymeric amide production system and to enter in the one or more stream pipelines in one or more mixing section.One or more pump can also operationally be integrated into draw from additive reservoir and to enter in the one or more stream pipelines one or more mixing section.Similarly, one or more pump operationally can be integrated into and to draw from one or more mixing section and to enter in the one or more stream pipelines in the downstream line continuous polymeric amide production system.One or more pump can also operationally be placed between mixing section.

Therefore, effluent mixed cell can comprise the parts of certain number, comprise at least one additive reservoir, at least one mixing section, one or more mixing tank, one or more heating unit, one or more cooling unit, one or more pump, one or more valve, one or more detector, one or more discharge outlet and one or more connection line, it is for promoting that material is at least one additive reservoir, at least one mixing section and the movement continuously between polymeric amide production system.

Downstream line in continuous polymeric amide production system can also have one or more mixing tank as one or more static mixer (online), arm mixer, ribbon-type blender, kneader, mixing screw, dual-shaft mixer, orbital shaker, double planetary mixer, high or low Rate Dispersion device, two kneaders etc.See, such as, the Chemical Engineering Handbook of Perry, the 5th edition, 19-22 page.Downstream line in continuous polymeric amide production system can also have one or more independent mixing section to promote to contain polymeric blends (' masterbatch ') and polymkeric substance the mixing in downstream line of additive.This mixed downstream room can also have one or more mixing tank, any one as described herein in those, or the available any mixing tank of those skilled in the art.

The method of effluent mixed cell and this unit of use provides uniform additive to mix, and decreasing pollution thing is introduced, and avoids by product to be formed, and does not cause equipment scaling.Avoid gel formation.Gel can stagnation bag-like region and irregular place or by the vortex in the polymer flow of system in formed.Effluent mixed cell, and the method using this unit, promote that stream and additive are mixed in polymeric amide.Effluent mixed cell can also reduce or avoid the gel formation in production system.

Example effluent mixed cell

Fig. 1 is the schematic diagram of an example of example effluent mixed cell.Such as, by being connected to shunting stream pipeline 20 and the outlet flow pipeline 50 of the main polymeric amide stream pipeline in continuous polymeric amide production system, effluent mixed cell may be operably coupled to continuous polymeric amide production system.Effluent mixed cell can in parts 10 downstream of continuous polymeric amide production system.Such as, parts 10 can be flash evaporation unit or the aftercondensated unit of continuous polymeric amide production system.Thus can branch to not having the polymeric amide be substantially polymerized of additive 60 in effluent mixed cell, and the polymeric amide be substantially polymerized with additive 70 can be removed from effluent mixed cell or flow out.Valve such as valve 15,25,35 and 45 can regulate material (such as, additive or the polymeric amide that is substantially polymerized) from a region of effluent mixed cell or parts to another flowing.Such as, the polymeric amide be substantially polymerized can be branched in mixing section 30 by shunting stream pipeline 20.Additive also can flow to the mixing section 30 that wherein can occur mixing from additive reservoir 40.Therefore effluent mixed cell can produce the polymeric amide be substantially polymerized with additive 70.

Polymeric amide is produced

Term " polymeric amide " means the polymkeric substance containing multiple amido linkage.Polymeric amide, such as, is also referred to as nylon at the aliphatic polyamide repeating to have between amide units at least 85% aliphatic key.Term " straight chain " means polymeric amide can derive from Bifunctionalized reactant, and wherein structural unit connects with chain like manner tail with tail.Like this, this term is intended to get rid of and derives from triamine or derive from the three dimensional polymeric structure that may exist in the polymkeric substance of triprotic acid.

Aliphatic polyamide can derive from di-carboxylic acid and other di-carboxylic acid acid amides when reacting with uncle or secondary amine forms derivative as acid anhydrides, acid amides, carboxylic acid halides, half ester and diester.Substantially all aliphatic polyamide polymers can be completed by the reaction of the acid amides of uncle or secondary diamine (having the diamines that at least one is connected to the hydrogen of each nitrogen) and dicarboxylic acid or di-carboxylic acid-formed derivative from being formed of the monomer be made up of dicarboxylic acid and diamines.

HOOC-R-COOH+H ₂N-R'-NH ₂→-[NH-R’-NH-CO-R-CO] _m-+nH ₂O

Wherein R and R ' represents bivalent hydrocarbon radical.

The product produced is formed by from the long-chain set up by the series of identical unit of following Structure composing:

-NH-R'-NH-CO-R-CO-

Wherein water is unique by product of polymer formation.

Carothers introduces the UNC for diamines and diacid polymeric amide, and it is adopted.As a result, " structural unit " of the polymkeric substance of the diacid and diamines that derive from each a part is named with the number of carbon atom in respective radicals R and R '.The polymeric amide called after " nylon 6,6 " (polyhexamethylene adipamide) that will be provided by hexa-methylene-1,6-diamines and hexanodioic acid is the result of this convention.

Business method for the preparation of polymeric amide can comprise makes the aqueous solution of diamines-dicarboxylate under superatmospheric pressure continually by continuous reaction zone.See, such as, the U.S. Patent number 2,361,717 of Taylor; The U.S. Patent number 2,689,839 of Heckert.

Polymeric amide can by adding hot preparation by the derivative of the diamines of equimolar amount and the formation acid amides of dicarboxylic acid or di-carboxylic acid substantially under polycondensation condition.This polycondensation condition generally comprises the temperature of about 180 DEG C to 300 DEG C.

Such as, at nylon 6, in 6 methods, can to the aqueous solution of continuous polymerization reactor charging hexa-methylene two ammonium adipate (nylon 6,6 salt), it has the concentration in the scope of 35 to 65 % by weight.The concentration of hexa-methylene two ammonium adipate is adjustable in the optional vaporizer of reactor upstream.Effluent from flasher level (also referred to as secondary reactor) comprises polyamide prepolymer polymkeric substance, and it typically has the relative viscosity of about 9-20.This stream is fed in aftercondensated (finishing) device.Controlled variable in aftercondensated device can comprise temperature, pressure and staying volume.These controlled variable are adjustable with the final polymkeric substance of relative viscosity needed for making to obtain typically in the scope of 30 to 100.Temperature in aftercondensated device is remained in the scope of 270 ° to 290 DEG C.Pressure is remained on 250 to 640 millibars.Staying volume is about 20 to 40 minutes.

When obtaining enough high molecular, product has fibroblast character.Such as, when polymeric amide have as measure in m-cresol solution about 0.5 and 2.0 scope in intrinsic viscosity time, this fibroblast occurs.

When obtain needed for the polymerization degree time be polymerized.The polymerization degree is with polymer viscosity indirect expression.The polymerization degree, measuring usually used as relative viscosity or RV, is to viscosity and and then the alternative measurement of molecular weight.

At high temperature, the polymerization degree is the function of the amount of existing water and is limited by it.At polymkeric substance on the one hand and between water, and on the other hand, and there is running balance between the polymkeric substance of depolymerization (or even reactant).It is normally more suitable than the polymeric amide by balancing the significantly higher RV of obtainable RV at normal atmosphere and water vapour to have.

The character of given polymeric amide can change, especially along with the change of molecular weight of polymeric amide.Polymeric amide character is also subject to the characteristics influence of its end group, itself so that depend on which kind of reactant excessive use, diamines or diacid.

The molecular-weight average of polymeric amide can be difficult to determine, but for most of object, the precise knowledge of molecular-weight average is generally unessential.It is believed that general two stages or the degree that there is polymerization: its molecular weight is probably placed in the oligopolymer near 1000 to 4000, and its molecular weight probably higher than about at least 7000 fibre-forming polyamide.Difference between oligopolymer and superpolymer or " superpolymer " be the former viscosity is relatively low upon melting.Superpolymer glues very much, even if in 25 DEG C of temperature higher than their fusing point.

Contrary with oligopolymer, the superpolymer of polymeric amide easily spins as strong, continuous print, pliable and tough, permanent directed fiber.Such as, but oligopolymer, has those of element length being less than about 9, superpolymer can be converted into by successive polymerization reaction.

Fibre-forming polyamide generally has high-melting-point and low solubility.Derive from simpler type amine and acid those be generally opaque solid, it is in the temperature melting quite determined or become transparent.Lower than their fusing point, fibre-forming polyamide generally represents sharp-pointed X-ray crystal powder diffraction pattern, and this is the evidence of their crystalline structure.The density of these polymeric amide is generally placed between 1.0 to 1.2.Nylon 6, the density of 6 is considered to 1.14 grams/cc usually.

Polymeric amide can have the independent unit of analog structure.To the mean sizes of these independent unit, the molecular-weight average of polymkeric substance, controls cautiously in specific scope.Polyreaction is carried out further, and molecular-weight average (and intrinsic viscosity) will be higher.If use reactant with accurately equimolar amount in the course of the polymerization process, and heating continues for a long time under the condition of effusion allowing volatile matter product, obtains the polymeric amide of very high molecular.But if any one reactant of excessive use, polymerization can proceed to specified point and substantially stop afterwards.The point that polymerization stops depends on the diamines of excessive use or the amount of diprotic acid (or derivative).

The facilitated method preparing polymeric amide can comprise by the diamines of amount equal for approximately chemistry and dicarboxylic acid are mixed with salt in a liquid.Liquid can be the poor solvent of obtained salt.Salt from liquid separation can be purified afterwards, if needed, by from suitable solvent crystallization.These diamines-dicarboxylates are crystal and have the fusing point determined.They are solvable and can from specific alcohol and alcohol-water mixture crystallization in water.

Fibre-forming polyamide can be carried out with several means by the preparation of diamines-dicarboxylate.Salt can be heated to temperature of reaction (180 DEG C-300 DEG C) when there is not solvent or thinner under the condition removed of the water allowing to be formed in the reaction.

Polymerizing polyamide reaction can experience decompression, such as, equals the absolute pressure of 50 to 300mm mercury column (67 to 400 millibars) to promote substantially to complete polymerization.Such as, the reaction vessel wherein preparing polymeric amide can be vacuumized, allow polymer cure afterwards.

Usually, do not need to add catalyzer in the method formed at above-described polymeric amide.But specific phosphorated material can play catalysis to a certain degree.Phosphorated material can comprise metal phosphinate hydrochlorate.The use of additional catalyst can promote the production of high molecular weight material.

Testing method

Thermal destruction index (TDI) is measures relevant to the thermal history of polymkeric substance.Lower TDI refers to temperature history more inviolent in process of production.The available TDI measuring method of those skilled in the art measures the absorbancy of polymkeric substance 1% (by weight) solution in 90% formic acid at the wavelength of 292nm.

Oxidative degradation index (ODI) in its high temperature production process, is exposed to relevant the measuring of oxidizing condition to polymkeric substance.Lower ODI refers to degraded more not serious in process of production.It is determined in the absorbancy of the wavelength of 260nm by measuring polymkeric substance 1% (by weight) solution in 90% formic acid.

Relative viscosity (RV) refers to the ratio at 25 DEG C of solution measured and solvent viscosity in capillary viscosimeter.The RV measured by ASTM D789-06 be the basis of this test procedure and 8.4 % by weight solution being polymeric amide in the 90% formic acid water of 10 % by weight (90 % by weight formic acid and) at viscosity (in centipoise) and 90% formic acid of 25 DEG C from the ratio in the viscosity (in centipoise) of 25 DEG C.

Definition

As used herein term " about " can certain variable pitch of permissible value or scope, such as, in 10% of described value or described range limit, in 5%, or in 1%.

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

As used herein term " solvent " refers to can the liquid of dissolved solids, liquid or gas.The limiting examples of solvent is siloxanes, organic compound, water, alcohol, ionic liquid and supercutical fluid.

As used herein term " air " refers to the mixture of the gas with the composition approximately identical with the natural composition of the gas usually obtained from air at ground level.In some instances, air takes from surrounding environment.Air has and comprises about 78% nitrogen, 21% oxygen, 1% argon and 0.04% carbonic acid gas, and the composition of other gas in a small amount.

The value expressed with range format should explain with flexi mode the numerical value clearly described using the boundary not only comprised as scope, and comprises all independent numerical value or subrange that comprise within the scope of this, as stated the same by each numerical value clearly with subrange.Such as, the scope of " about 0.1% to about 5% " or " about 0.1% to 5% " should be interpreted as not only comprising about 0.1% to about 5%, and comprise independent value in pointed scope (such as, 1%, 2%, 3% and 4%) and subrange (such as, 0.1% to 0.5%, 1.1% to 2.2%, 3.3% to 4.4%).Unless otherwise noted, state that " about X to Y " has the implication identical with " about X to about Y ".Equally, unless otherwise noted, state that " about X, Y or about Z " has the implication identical with " about X, about Y or about Z ".

In this article, unless context is clearly pointed out in addition, use term " ", " one " or " described " to comprise one or more than one.Unless otherwise noted, term "or" is used to refer to the "or" of non-exclusive.In addition, it is to be appreciated that adopt herein and the wording differently do not defined or term only for illustration of object and be nonrestrictive.The use of any paragraph heading is contemplated to and helps the understanding of article and be not interpreted as limiting; The information relevant to paragraph heading can within special paragraph or outside occur.

By following examples example polymeric amide effluent unit and the method using this unit style for polymeric amide, its intention is purely example and does not limit the present invention.

embodiment

continuous polymerization method.carry out following methods in an embodiment.In continuous nylon 6,6 production method, hexanodioic acid and hexamethylene-diamine are blended in water with about equimolar ratio in salt pond, to be formed containing nylon 6,6 salt, there is the aqueous mixture of about 50 % by weight water.Salt brine solution is passed to vaporizer.Salt brine solution is heated to about 125-135 DEG C (130 DEG C) and is removed by the salt brine solution of water from heating by vaporizer, makes water concentration be increased to about 30 % by weight.The salt mixture of the evaporation with the relative viscosity of about 1.4-1.9 (1.6) is passed to reactor.The temperature of the salt mixture of evaporation reaches about 218-250 DEG C (235 DEG C) by reactor, allow reactor by water from the salt mixture of evaporation of heating to remove further, water concentration is reached to about 10 % by weight, and salt is polymerized further.The mixture of reaction is passed to flasher.The mixture of reaction is heated to about 270-290 DEG C (280 DEG C) by flasher, allows flasher to remove water further from reaction mixture, makes water concentration reach about 0.5 % by weight, and the mixture reacted is polymerized further.The mixture of flash distillation of the relative viscosity with about 9 to 20 (13) is passed to finisher.Finisher makes polyblend stand vacuum to remove water further, makes water concentration reach about 0.1 % by weight, with the polymerization degree making polymeric amide obtain suitable final scope, afterwards the polyblend that aftercondensated is crossed is passed to forcing machine and tablets press.

Embodiment 1a: additive adds to the nylon be partly polymerized

10% aqeous suspension of the titanium dioxide Detitanium-ore-type additive being preheated to 130 DEG C is pumped to the polyamide solution partly formed leaving vaporizer, is not more than 30 seconds from the timed interval being heated to inject.The polymeric amide stream leaving vaporizer has the flow velocity of about 75L/ minute, and 10% additive stream (steam) has the flow velocity of about 1.7L/ minute.These streams merged flow in reactor.With the polymkeric substance leaving finisher for 59L/ minute have 0.9 intrinsic viscosity and containing 0.3 % by weight additive.

By system closing after operation 12 weeks.Significant additive deposition is observed in flasher and other components downstream.Titanium dioxide reagent is coated in heat transfer surface, has the mean thickness of about 0.2mm, reduces the efficiency of heat trnasfer in the method.

Embodiment 1b: additive adding to the nylon that is partly polymerized in an extruder

Effluent additive unit is placed in flasher downstream.Inlet valve is opened branched to the mixing section of effluent additive unit from the main flow of nylon by the polymerization nylon substantially of about 5 % by weight.Mixing section is heated to equably the temperature (about 280 DEG C) equal with the nylon be substantially polymerized in main flow.Titanium dioxide Detitanium-ore-type additive and the shunted nylon be substantially polymerized are mixed the uniform additive stream of the temperature to form water-content and about 280 DEG C with about 0.1-0.2 % by weight by mixing section.Polymeric blends flows through mixing section with about 3L/ minute, has the average total residence time in mixing section of about 10 minutes, and obtains the titanium dioxide concentration of about 6 % by weight.Uniform nylon-additive stream is by outlet valve to rejoin the main flow in polymeric amide forcing machine, and polymeric amide is extruded as line material by described polymeric amide forcing machine.The pressure entering the material of mixing section by the pressure influence of material leaving flasher, and leaves the pressure influence of pressure by material in forcing machine of the material of mixing section.Change little on pressure between material the material left from flasher and forcing machine causes the pressure change in mixing section, makes the flow forward being difficult to keep additive from additive chamber consistently.Occur that polymeric blends is to the adverse current in additive entrance, makes additive feeding unit because of polymeric blends fouling, this requires that additive system off-line is for clean.Final product has the mean concns of the titanium dioxide of about 0.3 % by weight; But be added to the proximity of extrusion owing to additive, in main flow, the mixing of additive is not thorough and consistent, provides the pellet of the vicissitudinous additive concentration of tool, and correspondingly reduces product qualities.

Embodiment 1c: additive adds to the nylon be partly polymerized, uses prefabricated nylon 6,6 carrier current

Effluent additive unit is placed in flasher downstream.Titanium dioxide Detitanium-ore-type additive and prefabricated nylon 6,6 polymer support stream are mixed for being added to main flow by additive unit.The mixing section of additive unit is heated to equably the temperature (about 280 DEG C) equal with the nylon be substantially polymerized in main flow.Mixing section produces the uniform additive stream with the water-content of about 0.1-0.2 % by weight and the temperature of about 280 DEG C.Polymeric blends in mixing section has the titanium dioxide concentration of about 6 % by weight.Polymeric blends leaves additive unit from mixing section flowing, and enters with about 3L/ minute in the main flow of forcing machine upstream.Polymeric blends has the average total residence time of about 10 minutes in mixing section.Final product has the concentration of the titanium dioxide of about 0.3 % by weight.Nylon 6, the polymerization degree of 6 carrier currents is not the polymerization degree Perfect Matchings of nylon 6,6 in all time and main flow.Additive is added to main flow in prefabricated nylon 6,6 carrier current and causes nylon 6, the change in the polymerization degree of 6 products, reduce product qualities.

Embodiment 1d: additive adds to the nylon be partly polymerized, uses nylon 6 carrier current

Effluent additive unit is placed in flasher downstream.Titanium dioxide Detitanium-ore-type additive and prefabricated nylon 6/poly compound carrier current are mixed for being added to main flow by additive unit.The mixing section of additive unit is heated equably with the temperature (about 280 DEG C) equal with the nylon be substantially polymerized in main flow.Mixing section produces the uniform additive stream with the water-content of about 0.1-0.2 % by weight and the temperature of about 280 DEG C.Mixing section have about 10 minutes the average total residence time in mixing section and have about 6 % by weight titanium dioxide concentration.Polymeric blends leaves additive unit from mixing section flowing, and enters to about 3L/ minute in the main flow of forcing machine upstream.Final product has the concentration of the titanium dioxide of about 0.3 % by weight.Nylon 6 carrier current is and nylon 6, the polymkeric substance that 6 main flows are different.Additive is added in nylon 6 main flow and nylon 6 impurity is added to nylon 6,6 products, reduce product qualities.

Embodiment 2: for additive to the method for the improvement added of nylon be substantially polymerized

Effluent additive unit is placed in flasher downstream.Inlet valve is opened branched to the mixing section of effluent additive unit from the main flow of nylon by the polymerization nylon substantially of about 5 % by weight.Mixing section is heated to equably the temperature (about 280 DEG C) equal with the nylon be substantially polymerized in main flow.Mixing section comprises for titanium dioxide is mixed the device of the even nylon-additive stream of the temperature to form water-content and about 280 DEG C with about 0.1-0.2 % by weight with polymerization nylon substantially.Polymeric blends flows through mixing section with about 3L/ minute, has the average total residence time in mixing section of about 10 minutes, and obtains the titanium dioxide concentration of about 6 % by weight.Even nylon-additive stream by outlet valve with the upstream recombine at forcing machine to main flow.Final product has the concentration of the titanium dioxide of about 0.3 % by weight.

After operation 12 weeks, by system closing.Additive deposition is not observed in forcing machine upstream.Heat transfer surface does not have additive and in the method described in embodiment 1a, less gel formation is observed in the position of additive accumulation.Between the entrance and the outlet of mixing section of mixing section, occur little pressure change, additive is easily kept to the flow forward in mixing section, avoid polymer reflow in additive entrance, this and embodiment 1b are formed and contrast.Because the carrier current for additive takes from main nylon 6,6 stream, polymerization degree accurate match, does not cause the reduction on product qualities, and this and embodiment 1c and 1d are formed and contrast.

All patents quoted herein or mention and be openly the instruction of level of theme one of ordinary skill in the art of the present invention, and each this quoted patent or open being therefore bonded to particularly by reference all to combine with it with individually through quoting or to provide the identical degree of its full content herein.Applicant retains and is bonded to right in this specification sheets by from any this patent of quoting or disclosed any and all materials and information physical.

Concrete method described herein, device and composition are the representative of preferred embodiment and are example and the restriction do not expected as the scope to theme of the present invention.Consider those skilled in the art after this specification sheets can expect other object, in and embodiment, and included by theme of the present invention.What one skilled in the art will readily appreciate that is to carry out multiple replacement and change to the present invention disclosed herein and not depart from the scope of the present invention and spirit.

The theme of the present invention schematically described herein can be there are not any one or more key elements aptly, or implements when one or more restriction, and it is necessary not open particularly herein.The Method and Process schematically described herein can be implemented with the order of different steps aptly, and Method and Process is not necessarily limited to the order of the step pointed out in this paper or claim.

Under any circumstance this patent all cannot be interpreted as being defined in herein disclosed specific examples or embodiment or method particularly.Any statement that under any circumstance this patent all cannot be interpreted as being made by any other official of any auditor or patent and trademark office or employee limits, unless in the written reply of applicant particularly and adopt this statement clearly without restriction or preserve.

The term adopted and express illustratively term use and be not restrictive; and do not wish in the use of this term and expression, get rid of feature that is given and that describe any Equivalent or its part; but it should be understood that; in the scope of the present invention for required protection, multiple amendment is possible.Therefore, will understand is that, although the present invention is disclosed particularly by preferred embodiment and optional feature, the modifications and variations of concept disclosed herein can be taked by those skilled in the art, and this modifications and variations are considered to be in by appended claim of the present invention and state in the scope of the present invention that limits.

Herein broadly and generally describe the present invention.Drop on generally open interior each narrower species and subclass group and also form a part of the present invention.This comprises the general remark of the present invention having and remove the restriction of any theme or reverse side restriction from a class, and with whether point out that herein got rid of material has nothing to do particularly.In addition, when with the term description of Ma Kushi group feature of the present invention or in, it will be apparent to one skilled in the art that the present invention thus also with the term description of the member independent arbitrarily of the member of Ma Kushi group or subgroup.

Statement:

1., for additive being mixed to the method in polymerizing polyamide logistics, described method comprises:

B additive is mixed in described polymeric amide effluent to produce polymeric amide-additive side mixture by (); With

C described polymeric amide-additive side mixture is back to downstream line in described system to produce polymeric amide-additive main flow by ();

Wherein, when shunting, there is from the polymeric amide be substantially polymerized described in upstream line the water-content of about 0.1%-3 % by weight.

2. the method for statement described in 1, wherein when shunting, the described polymeric amide be substantially polymerized in described upstream line has the water-content of about 0.1-2 % by weight.

3. the method for statement described in 1 or 2, wherein when shunting, the described polymeric amide be substantially polymerized in described upstream line has the water-content of about 0.1-1 % by weight.

4. state the method described in any one in 1-3, wherein said additive contains solvent, and is substantially removed from described polymeric amide-additive side mixture by described solvent before being back to described downstream line.

5. state the method described in any one in 1-4, wherein before being back to described downstream line, water is removed from described polymeric amide-additive side mixture.

6. state the method described in any one in 1-5, wherein said polymeric amide-additive side mixture returns to downstream when it has the water-content of 0.9-1.1 times of the polymeric amide water-content in downstream line.

7. state the method described in any one in 1-6, % by weight additive in wherein said polymeric amide-additive side mixture is about 0.001-20 % by weight, or about 0.01-15 % by weight, or about 0.01-10 % by weight, or about 0.1-10 % by weight, or about 0.1-9 % by weight, or about 0.01-8 % by weight, or about 0.01-7 % by weight, or about 0.01-6 % by weight, or about 0.01-5 % by weight, or about 0.1-3 % by weight.

8. state the method described in any one in 1-7, % by weight additive in wherein said polymeric amide-additive main flow is about 1-5 % by weight.

9. state the method described in any one in 1-8, wherein said continuous polymeric amide production system comprises reactant reservoir, vaporizer, polymerization reactor, batch reactor flasher, finisher, polyamide thread material forming unit, forcing machine, and their combination.

10. state the method described in any one in 1-9, wherein from the shunting of described upstream line after polymerizing polyamide reaction mixture is by the flasher described system.

The method described in any one in 11. statement 1-10, returns to downstream after wherein said polymeric amide-additive side mixture flasher in the system.

The method described in any one in 12. statement 1-11, wherein from the shunting of described upstream line after polymerizing polyamide reaction mixture is by the finisher described system.

The method described in any one in 13. statement 1-12, wherein said polymeric amide-additive side mixture returns to downstream after polymerizing polyamide reaction is by finisher.

The method described in any one in 14. statement 1-13, is back to described main polymeric amide stream pipeline before wherein said polymeric amide-additive side mixture polyamide thread material forming unit in the system.

The method described in any one in 15. statement 1-14, wherein said polymeric amide-additive side mixture is back to described main polymeric amide stream pipeline at polymeric amide by before the extruding of forcing machine.

The method described in any one in 16. statement 1-15, by described polymeric amide-additive main flow mixing after described method is also included in and described polymeric amide-additive side mixture is back to described downstream line.

The method described in any one in 17. statement 1-16, described polymeric amide-additive main flow mixes after being also included in and described polymeric amide-additive side mixture being back to described downstream line by described method.

The method described in any one in 18. statement 1-17, wherein after described polymeric amide-additive side mixture is back to the described downstream line of described system, mixes described polymeric amide-additive main flow in the mixed cell of described system.

The method described in any one in 19. statement 1-18, wherein said additive is polymerizing catalyst, end-capping reagent, thermo-stabilizer, photostabilizer, lubricant, biocide, tinting material, toughener, weighting agent, fire retardant, fluoropolymer, ANTIMONY TRIOXIDE SB 203 99.8 PCT, polycaprolactone, zinc sulphide, matting agent, titanium dioxide, or their combination.

The method described in any one in 20. statement 1-19, wherein said additive is dyestuff, pigment, glass fibre, fibrous magnesium silicate, carbon fiber, Kevlar, gypsum fiber, Calucium Silicate powder, kaolin, calcined kaolin, wollastonite, talcum, chalk, phosphoric acid ester, phosphoric acid, phosphorous acid ester, phosphinate, phosphorous acid ester, organo-phosphine oxide, sodium hypophosphite, acetic acid, propionic acid, phenylformic acid, succsinic acid, vinylidene fluoride, R 1216, chlorotrifluoroethylene, tetrafluoroethylene, perfluoralkyl perfluorovinyl ether or their combination.

The method described in any one in 21. statement 1-20, wherein heated described additive before mixing with described polymeric amide effluent.

22. 1 kinds of continuous polymeric amide production systems, described system comprises

Wherein said effluent mixed cell is settled or is configured to parallel with the main polymeric amide stream pipeline of described continuous polymeric amide production system;

At least one mixing section wherein said is configured to additive to mix with the polymeric amide be substantially polymerized shunted by least one in described upstream entrance; With

The system of 23. statements described in 22, wherein each described upstream entrance is configured to flasher unit in the system and is shunted from described main polymeric amide stream pipeline by the polymeric amide be substantially polymerized with the position in the described main polymeric amide stream pipeline between described polymeric amide forcing machine unit or polyamide thread material forming unit.

The system of 24. statements described in 22 or 23, wherein each described upstream entrance is configured to finisher unit in the system and is shunted from described main polymeric amide stream pipeline by the polymeric amide be substantially polymerized with the position in the described main polymeric amide stream pipeline between described polymeric amide forcing machine unit or described polyamide thread material forming unit.

The system described in any one in 25. statement 22-24, at least one in wherein said upstream entrance comprises detector, its for detect branch to described effluent mixed cell described mixing section in described in the amount of polymeric amide of being substantially polymerized or volume.

The system described in any one in 26. statement 22-25, at least one in wherein said upstream entrance may be operably coupled to detector, when at least one mixing section polymeric amide be substantially polymerized described in selected amount or volume being branched to described effluent mixed cell, described detector close described in the upstream entrance that is operably connected.

The system described in any one in 27. statement 22-26, at least one in wherein said upstream entrance may be operably coupled to detector, and this detector detects the water-content of the polymeric amide be substantially polymerized in described main polymeric amide stream pipeline.

The system described in any one in 28. statement 22-27, at least one in wherein said upstream entrance may be operably coupled to detector, this detector detects the water-content of the polymeric amide be substantially polymerized in described main polymeric amide stream pipeline, and wherein when the water-content of the selected polymeric amide be substantially polymerized being detected, at least one in described upstream entrance opened by described detector.

The system described in any one in 29. statement 22-28, at least one in wherein said mixing section comprises mixing tank, and this mixer configuration is described additive and the described polymeric amide be substantially polymerized are mixed to evenly.

The system described in any one in 30. statement 22-29, at least one in wherein said mixing section comprises the mixing tank that may be operably coupled to detector, and described detector configurations is the degree of uniformity detected described additive and the described polymeric amide mixing be substantially polymerized.

The system described in any one in 31. statement 22-30, wherein said lower exit may be operably coupled to detector, and this detector configurations is open described lower exit when described additive and the described polymeric amide be substantially polymerized being mixed equably.

The system described in any one in 32. statement 22-31, wherein said effluent mixed cell comprises well heater, and this heater configuration is at least one in mixing section described in even underground heat.

The system described in any one in 33. statement 22-32, wherein said effluent mixed cell comprises well heater, this heater configuration for heat equably in described mixing section at least one and in heated mixing section, additive and the mixture of polymeric amide that is substantially polymerized are remained on molten state.

The system described in any one in 34. statement 22-33, wherein said effluent mixed cell comprises well heater, and this heater configuration is that at least one heating equably in described mixing section also promotes that the polymeric amide be substantially polymerized is polymerized further when it mixes with described additive.

The system described in any one in 35. statement 22-34, wherein said effluent mixed cell comprises at least one additive reservoir.

The system described in any one in 36. statement 22-35, wherein said effluent mixed cell comprises well heater, and this heater configuration is heated described additive equably before being mixed with the polymeric amide be substantially polymerized by described additive.

The system described in any one in 37. statement 22-36, wherein said effluent mixed cell comprises the well heater with thermostatted, and this thermostatted is configured to regulate the temperature of the material at least one or at least one the additive reservoir in described mixing section.

The system described in any one in 38. statement 22-37, wherein said effluent mixed cell also comprises detector, this detector for monitor in mixing section comprise described in the water-content of the mixture of polymeric amide that is substantially polymerized.

The system described in any one in 39. statement 22-38, at least one in wherein said lower exit may be operably coupled to water-content detector, when the water-content of selected described mixture being detected, described water-content detector additive for activating and the mixture of polymeric amide that is substantially polymerized are by described outlet and the release entered in the main polymeric amide stream pipeline of described system.

The system described in any one in 40. statement 22-39, wherein said effluent also comprises pump, impeller, under meter, one or more discharge outlet, or their combination.

The system described in any one in 41. statement 22-40, at least one in wherein said upstream entrance may be operably coupled to detector, the water-content of the polymeric amide be substantially polymerized described in this detector detects.

The system described in any one in 42. statement 22-41, wherein when the described polymeric amide be substantially polymerized has the water-content of about 0.1%-3 % by weight, by the described polymeric amide be substantially polymerized by least one shunting in described upstream entrance.

The system described in any one in 43. statement 22-42, wherein when the described polymeric amide be substantially polymerized has the water-content of about 0.1-2 % by weight, by the described polymeric amide be substantially polymerized by least one shunting in described upstream entrance.

The system described in any one in 44. statement 22-43, wherein when the described polymeric amide be substantially polymerized has the water-content of about 0.1-1 % by weight, by the described polymeric amide be substantially polymerized by least one shunting in described upstream entrance.

The system described in any one in 45. statement 22-44, wherein at least one mixing section has discharge outlet.

The system described in any one in 46. statement 22-45, at least one in wherein said mixing section has the discharge outlet that additive solvent, water or their combination can be passed through from it.

The system described in any one in 47. statement 22-46, at least one in wherein said lower exit may be operably coupled to detector, and this detector detects the water-content of the mixture in mixing section.

The system described in any one in 48. statement 22-47, wherein said polymeric amide-additive side mixture returns to downstream when having the water-content of 0.9-1.1 times of water-content of polymeric amide in described downstream line.

The system described in any one in 49. statement 22-48, wherein said continuous polymeric amide production system comprises reactant reservoir, vaporizer, polymerization reactor, batch reactor flasher, finisher, polyamide thread material forming unit, forcing machine, or their combination.

The system described in any one in 50. statement 22-49, wherein said main polymeric amide stream pipeline comprises: be placed in the mixing tank in the described main polymeric amide stream pipeline after described lower exit.

The system described in any one in 51. statement 22-50, wherein said continuous polymeric amide production system also comprises the mixed cell be placed in described lower exit described main polymeric amide stream pipeline below.

The system described in any one in 52. statement 22-51, wherein said additive is polymerizing catalyst, end-capping reagent, thermo-stabilizer, photostabilizer, lubricant, biocide, tinting material, toughener, weighting agent, fire retardant, fluoropolymer, ANTIMONY TRIOXIDE SB 203 99.8 PCT, polycaprolactone, zinc sulphide, matting agent, titanium dioxide, or their combination.

The system described in any one in 53. statement 22-52, wherein said additive is dyestuff, pigment, glass fibre, fibrous magnesium silicate, carbon fiber, Kevlar, gypsum fiber, Calucium Silicate powder, kaolin, calcined kaolin, wollastonite, talcum, chalk, phosphoric acid ester, phosphoric acid, phosphorous acid ester, phosphinate, phosphorous acid ester, organo-phosphine oxide, sodium hypophosphite, acetic acid, propionic acid, phenylformic acid, succsinic acid, vinylidene fluoride, R 1216, chlorotrifluoroethylene, tetrafluoroethylene, perfluoralkyl perfluorovinyl ether or their combination.

The system described in any one in 54. statement 22-53, % by weight additive in wherein said polymeric amide-additive side mixture is about 0.001-20 % by weight, or about 0.01-15 % by weight, or about 0.01-10 % by weight, or about 0.1-10 % by weight, or about 0.1-9 % by weight, or about 0.01-8 % by weight, or about 0.01-7 % by weight, or about 0.01-6 % by weight, or about 0.01-5 % by weight, or about 0.1-3 % by weight.

Following claim sums up the feature of system and method described herein.

Claims

1. an effluent mixed cell, described effluent mixed cell comprises:

2. effluent mixed cell according to claim 1, wherein each described upstream entrance is configured to flasher unit in the system and is shunted from described main polymeric amide stream pipeline by the polymeric amide be substantially polymerized with the position in the described main polymeric amide stream pipeline between polyamide thread material forming unit or forcing machine unit.

3. effluent mixed cell according to claim 1 and 2, wherein each described upstream entrance is configured to finisher unit in the system and is shunted from described main polymeric amide stream pipeline by the polymeric amide be substantially polymerized with the position in the described main polymeric amide stream pipeline between polyamide thread material forming unit or forcing machine unit.

4. the effluent mixed cell according to any one in claim 1-3, at least one in wherein said upstream entrance comprises detector, this detector for detect branch to described effluent mixed cell at least one mixing section in the amount of the described polymeric amide be substantially polymerized or volume.

5. the effluent mixed cell according to any one in claim 1-4, at least one in wherein said upstream entrance may be operably coupled to detector, and this detector is for detecting the water-content of the polymeric amide be substantially polymerized described in described main polymeric amide stream pipeline.

6. the effluent mixed cell according to any one in claim 1-5, at least one in wherein said mixing section comprises mixing tank, and this mixer configuration is by described additive and the described polymeric amide mixing be substantially polymerized.

7. the effluent mixed cell according to any one in claim 1-6, wherein said lower exit may be operably coupled to detector, and this detector configurations is open described lower exit when described additive and the described polymeric amide be substantially polymerized being mixed equably.

8. the effluent mixed cell according to any one in claim 1-7, wherein said effluent mixed cell comprises: be configured at least one well heater heated equably in described mixing section.

9. the effluent mixed cell according to any one in claim 1-8, wherein said effluent mixed cell comprises at least one additive reservoir.

10. the effluent mixed cell according to any one in claim 1-9, wherein said effluent mixed cell comprises: be configured to the well heater heated equably by described additive before being mixed with the polymeric amide be substantially polymerized by described additive.

11. effluent mixed cells according to any one in claim 1-10, wherein said effluent mixed cell comprises: the well heater with the thermostatted of the temperature being configured to the material regulated in described effluent mixed cell.

12. effluent mixed cells according to any one in claim 1-11, wherein said effluent mixed cell comprises: the well heater with the thermostatted of the temperature of the material at least one or at least one the additive reservoir being configured to regulate described mixing section.

13. effluent mixed cells according to any one in claim 1-12, wherein said effluent mixed cell also comprises detector, this detector for monitor in mixing section comprise described in the water-content of the mixture of polymeric amide that is substantially polymerized.

14. effluent mixed cells according to any one in claim 1-13, wherein said effluent mixed cell also comprises at least one pump, at least one impeller, at least one under meter, one or more discharge outlet, or their combination.

15. effluent mixed cells according to any one in claim 1-14, wherein when the described polymeric amide be substantially polymerized has the water-content of about 0.1%-3 % by weight, by the described polymeric amide be substantially polymerized by least one shunting in described upstream entrance.

16. effluent mixed cells according to any one in claim 1-15, wherein at least one mixing section has discharge outlet.

17. effluent mixed cells according to any one in claim 1-16, described system also comprises the detector of the water-content of the mixture detected in mixing section.

18. effluent mixed cells according to any one in claim 1-17, wherein return to described polymeric amide-additive side mixture to downstream when the 0.9-1.1 that it has a polymeric amide water-content in downstream line water-content doubly.

19. effluent mixed cells according to any one in claim 1-18, wherein said polymeric amide-additive side mixture returns to downstream when the 0.99-1.01 that it has a water-content of polymeric amide in downstream line water-content doubly.

20. effluent mixed cells according to any one in claim 1-19, wherein said continuous polymeric amide production system comprises reactant reservoir, vaporizer, polymerization reactor, batch reactor flasher, finisher, polyamide thread material forming unit, forcing machine or their combination.

21. effluent mixed cells according to any one in claim 1-20, wherein said main polymeric amide stream pipeline comprises: be placed in the mixing tank in the described main polymeric amide stream pipeline after described lower exit.

22. effluent mixed cells according to any one in claim 1-21, wherein said continuous polymeric amide production system also comprises the mixed cell be placed in described lower exit described main polymeric amide stream pipeline below.