WO2020191789A1 - Plateau de distillation à écoulement piston et procédé de préparation d'isophorine par condensation en phase liquide de l'acétone - Google Patents

Plateau de distillation à écoulement piston et procédé de préparation d'isophorine par condensation en phase liquide de l'acétone Download PDF

Info

Publication number
WO2020191789A1
WO2020191789A1 PCT/CN2019/080512 CN2019080512W WO2020191789A1 WO 2020191789 A1 WO2020191789 A1 WO 2020191789A1 CN 2019080512 W CN2019080512 W CN 2019080512W WO 2020191789 A1 WO2020191789 A1 WO 2020191789A1
Authority
WO
WIPO (PCT)
Prior art keywords
tray
liquid
downcomer
phase
weir
Prior art date
Application number
PCT/CN2019/080512
Other languages
English (en)
Chinese (zh)
Inventor
何岩
黎源
田博
边路路
周锐
员玫
李金明
孙媛媛
Original Assignee
万华化学集团股份有限公司
万华化学（宁波）有限公司
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 万华化学集团股份有限公司, 万华化学（宁波）有限公司 filed Critical 万华化学集团股份有限公司
Publication of WO2020191789A1 publication Critical patent/WO2020191789A1/fr

Links

Images

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14—Fractional distillation or use of a fractionation or rectification column
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
    • C07C45/61—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups
    • C07C45/67—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups by isomerisation; by change of size of the carbon skeleton
    • C07C45/68—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups by isomerisation; by change of size of the carbon skeleton by increase in the number of carbon atoms
    • C07C45/72—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups by isomerisation; by change of size of the carbon skeleton by increase in the number of carbon atoms by reaction of compounds containing >C = O groups with the same or other compounds containing >C = O groups
    • C07C45/74—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups by isomerisation; by change of size of the carbon skeleton by increase in the number of carbon atoms by reaction of compounds containing >C = O groups with the same or other compounds containing >C = O groups combined with dehydration
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
    • C07C45/78—Separation; Purification; Stabilisation; Use of additives
    • C07C45/81—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
    • C07C45/82—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C2601/00—Systems containing only non-condensed rings
    • C07C2601/12—Systems containing only non-condensed rings with a six-membered ring
    • C07C2601/16—Systems containing only non-condensed rings with a six-membered ring the ring being unsaturated
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency

Definitions

  • the invention relates to a reactive distillation tray and a process for preparing isophorone by using the reactive distillation tray.
  • Isophorone is one of the important products of acetone deep processing, chemical name: 3,5,5-trimethyl-2-cyclohexen-1-one, English name: Isophorone (abbreviated as IP), molecular formula is C 9 H 14 O. Isophorone has a wide range of uses, with strong dissolving ability, good dispersibility, and good leveling. It is an excellent high boiling point green solvent.
  • IPN isophorone nitrile
  • IPDA isophorone diamine
  • IPDI isophorone diisocyanate
  • KIP oxoisophorone
  • isophorone is mainly prepared by acetone condensation.
  • acetone condensation According to the contact state of the reactants, there are two methods for preparing isophorone by condensation of acetone: one is the pressurized liquid phase condensation in an alkaline solution; the other is the gas phase of gaseous acetone on the surface of the solid catalyst. Catalytic condensation method.
  • the liquid phase process is the mainstream industrial production method in the world.
  • the difficulty of the liquid-phase process is that the reaction is a typical series and parallel complex reaction network, which produces more by-products, resulting in lower selectivity of the target product isophorone, and greatly restricts the single-pass conversion of acetone in industry. rate.
  • the reaction under the reaction conditions, there are two liquid phases in the system, which puts forward high requirements for the mixing of the reaction liquid, the control of the flow field and the control of the product yield.
  • BP company discloses a method for preparing isophorone by reactive distillation in DE2520681, US2399976 and US3981918.
  • the reaction and rectification are integrated into a pressurized reaction rectification tower, and the disturbance of the gas phase is used to play a strong stirring effect.
  • the acetone and the catalyst are fully contacted to react in the reaction section, and the resulting product immediately enters the separation section to recover unreacted acetone.
  • some high boilers produced by the condensation of acetone will decompose into acetone and isophorone, which improves the product yield.
  • the traditional reactive distillation reactor used still has many problems: such as large liquid holding capacity, uneven liquid phase flow, many side reactions, and low distillation efficiency ,
  • the tray pressure drop is large (the pressure drop of the conventional technology single plate can exceed 2kPa), and the energy consumption is high.
  • the downcomer "pulsation" the liquid-liquid flow is not flowing
  • the traditional tray is limited by technology and needs to be met by increasing the number of plates, which increases the difficulty of equipment manufacturing and the amount of investment.
  • the gas phase has to pass through the liquid phase, for a reactive distillation tray with a large liquid holdup, the energy consumption caused by the total pressure drop of the tower and the increase in the temperature of the bottom of the tower are generally unacceptable.
  • the reaction system of acetone has a particularly important value: the reaction network for the preparation of IP by condensation of acetone contains a large number of series of reactions. Excessive temperature will significantly reduce the selectivity of IP products, and significantly increase the difficulty of post-processing and IP refining and purification procedures.
  • IP and lye system is a strong and easy foaming system, and a very serious foaming phenomenon will occur under the traditional rectification tower, which greatly reduces the rectification efficiency and even brings safety hazards.
  • traditional distillation trays such as sieve trays, bubble caps and valve tray technology are used; the above-mentioned trays are essentially bubble distillation towers.
  • the operation form of bubbling determines that the film pulling and bubbling effect on the liquid is inevitable during the process of bubbles passing through the liquid layer and gradually merging and growing. It is inevitable for the fine foaming system similar to IP/lye.
  • the invention provides a flat-plug flow rectification tray.
  • a pressurized reaction rectification tower containing the flat-plug flow rectification tray of the present invention is used for easy foaming
  • IP isophorone
  • the post-treatment of IP (isophorone)/lye system can make the liquid phase more evenly distributed and flow, which is beneficial to improve the reaction effect.
  • One aspect of the present invention provides a flat-plug flow rectification tray, which is particularly suitable for the process of preparing isophorone by liquid-phase condensation of acetone.
  • the flat-plug flow rectification tray provided by the present invention includes a tray and one or more sets of flat-plug flow components arranged on the tray.
  • the flat-plug flow components include a downcomer, a grading overflow weir, and light and heavy phases. Diversion element, receiving plate I and flow guiding element;
  • the downcomer is connected to the tray, the upper part of the downcomer is provided with an inlet, the grading overflow weir is provided on the inlet of the downcomer, and the downcomer is provided with a vertical flow channel
  • the light and heavy phase splitting element is arranged in the downcomer and located below the grading overflow weir, and is used to receive the material liquid overflowing from the tray through the overflow weir to the vertical flow channel of the downcomer, and Separate the light phase material liquid and the heavy phase material liquid from the material liquid and drain the two through different channels to the bottom of the downcomer;
  • the liquid receiving tray I is connected to the tray, and is located on the opposite side of the side where the downcomer is connected to the tray;
  • the flow guide element is arranged above the connection between the liquid receiving tray I and the tray, and the flow guide element is provided to enable the material liquid on the liquid receiving tray I to be divided into multiple streams to guide the tower Multiple diversion channels of the disc.
  • an outlet weir is formed at the junction of the receiving tray I and the tray, and the flow guiding element is located above the outlet weir.
  • the outlets at the bottom of the light phase channel and the heavy phase channel respectively include a plurality of discontinuous channel outlets, that is, a plurality of independent channel outlets, so as to play a role similar to a liquid distributor, with liquid (or liquid) Distribution function.
  • the downcomer includes a downcomer plate and a back plate, the downcomer plate is connected to the tray, the back plate and the downcomer plate are enclosed to form the vertical flow channel, and the back plate Higher than the grading overflow weir.
  • the number of stages of the grading overflow weir is ⁇ 1, wherein the first-stage overflow weir is provided on the downcomer plate, and it is further preferred that the first-stage overflow weir is provided with a plurality of different heights.
  • the overflow hole preferably the number of stages of the grading overflow weir ⁇ 2, when the number of stages of the grading overflow weir ⁇ 2, from the downcomer plate to gradually away from the downcomer plate and toward the direction of the downcomer cavity ,
  • the overflow weirs at all levels are arranged at intervals and their heights increase sequentially, and the height difference between the adjacent two overflow weirs is 50-150mm.
  • the guide element includes a set of guide vanes arranged above the outlet weir; the outlet weir includes a first edge of the outlet weir connected to the liquid receiving tray I and an outlet weir connected to the tray Second edge
  • the set of guide vanes are arranged at intervals along the first edge of the outlet weir above the outlet weir.
  • the guide channels are formed between adjacent guide vanes, and each guide channel is directed from the liquid receiving plate I to the tower. The direction of the disk goes through;
  • each guide vane and the vertical line of the first edge of the outlet weir is ⁇ 0° and ⁇ 90°, and the vertical line refers to the plane located on the tray connected to the outlet weir.
  • a vertical line perpendicular to the first edge of the outlet weir; the angle between the adjacent guide vanes and the vertical line of the first edge of the outlet weir is the same or different.
  • each guide vane is arranged obliquely from one end of the first edge of the outlet weir close to the middle of the tray toward the end of the first edge of the outlet weir close to the tower wall; preferably the guide vanes closer to the first edge of the outlet weir The greater the angle with the perpendicular.
  • the outlet weir is arranged obliquely, and the bottom of the outlet weir is connected to the receiving tray I through the first edge of the outlet weir, and the top of the outlet weir is connected to the tray I through the second edge of the outlet weir.
  • the angle between the outlet weir and the receiving tray I is an obtuse angle; the outlet weir has the function of making the material liquid flow from the receiving tray I to the tray in an oblique upward direction.
  • the light-heavy-phase flow dividing element includes a liquid-receiving pan II, a split weir, a heavy phase channel, and a light-phase channel.
  • the split weir is arranged on the liquid-receiving pan II and the liquid-receiving pan II It is divided into a heavy phase receiving area and a light phase receiving area; the heavy phase receiving area is located on the same side of the grading overflow weir in the downcomer and is located below the grading overflow weir, so that the grading overflow The material flow overflowing from the weir into the downcomer tends to flow into the heavy phase receiving area;
  • the heavy phase channel is used to divert the heavy phase material liquid deposited at the bottom or bottom of the heavy phase liquid receiving zone to below the downcomer;
  • the light-phase liquid receiving area is used to receive the light-phase material liquid from the upper part of the heavy-phase liquid-receiving area overflowed by the divided weir, and the light-phase channel is used to divert the light-phase material liquid from the light-phase liquid receiving area to Below the downcomer;
  • the heavy phase channel is provided with a partition plate, the partition plate is provided with drainage ports, the inlet and the outlet of the heavy phase channel are respectively located on both sides of the partition plate, and the drainage port
  • the lower edge of is higher than the upper edge of the entrance of the heavy phase channel, preferably the height difference between the two is 20-100mm;
  • a baffle plate is also provided in the downcomer, and the baffle plate is arranged in the space between the grading overflow weir and the light-heavy phase dividing element, and is located in the downcomer with a grading overflow.
  • the opposite side of one side of the weir so that the material flow overflowing into the downcomer through the staged overflow weir tends to flow to the heavy phase receiving area.
  • the flat-plug flow assembly further includes a riser pipe and a spray hood.
  • the riser pipe is provided on the tray and is located in the area between the staged overflow weir and the liquid receiving tray I.
  • the riser pipe is provided with There are gas-phase channels used to guide the gas-phase upwards under the tray;
  • the spray hood is arranged on the riser pipe, and a gap used as a lower suction hole is left between the bottom of the spray hood and the tray; the lower part of the spray hood is provided above the lower suction hole.
  • the upper liquid suction hole of the spray cover is provided with a spray hole, and the position of the spray hole is higher than the outlet of the gas phase passage of the gas riser;
  • a gas guide vane is installed on the outside of the jet hood to guide the jet stream ejected from the jet hole to reduce the collision between the jet stream jets ejected from each jet hole; preferably the gas guide The flow sheet is arranged beside the jet hole;
  • a foam breaking plate is further provided outside the spray hood, and the foam breaking plate corresponds to the position of the spray hole; preferably, the distance between the foam breaking plate and the spray hole is 1-200 mm, more preferably 10-200 mm. 100mm; the surface of the foam breaking plate is smooth or rough, preferably a rough surface, more preferably the foam breaking plate has spikes;
  • the part of the spray cover provided with the upper liquid suction hole is formed with a constricted structure that is recessed into the spray cover.
  • the height of the highest-level overflow weir of the staged overflow weir is between 30-1000m; the height of the lift pipe is 10-50mm, preferably 20-40mm, lower than the highest-level overflow weir.
  • the cross-section of the riser pipe is circular or rectangular, and the cross-sectional shape of the jet hood is correspondingly circular or rectangular;
  • the shape of the upper liquid suction hole is rectangular, trapezoidal, circular or elliptical, or a trapezoidal, rectangular, circular or elliptical shape with teeth gaps;
  • the ratio of the open area of the upper liquid suction hole to the lower liquid suction hole is 10-1:1;
  • the diameter of the spray hood at the necking structure is 50%-99% of the diameter of other parts of the spray hood;
  • the width of the spray hood at the necking structure is 50%-99% of the width of the rest of the spray hood;
  • the shape of the injection hole is circular, rectangular, triangular or oblong, preferably the injection hole is a rectangular hole or an oblong hole, and the length ratio of the long and short sides of the injection hole is 1-20:1, preferably 1.5-10:1;
  • the angle between the gas deflector and the tangential direction of the injection hole surface is 1-90°, preferably 1-45°; the gas deflector is provided next to each injection hole,
  • the included angles between the adjacent gas guide vanes and the tangential direction of the corresponding injection hole surface are the same or different, and the same angle is preferably used.
  • the second aspect of the present invention provides a pressurized reactive rectification tower, which is provided with multiple layers of the above-mentioned flat plug flow rectification trays arranged up and down at intervals.
  • one of the receiving trays I on the flat-plug flow distillation tray of the next layer corresponds to the flat-plug flow distillation tray of the upper layer.
  • the receiving tray I is used to receive the light and heavy phase splitting elements in the downcomer (from the upper level of the flat plug flow distillation tray) directly above it Light phase material liquid and heavy phase material liquid separated from
  • the area between the connection between the receiving tray I and the tray and the bottom of the downcomer of the upper layer of the flat push-flow rectification tray is provided with the material liquid outlet of the receiving tray I, and the material liquid on the receiving tray I passes through The material liquid outlet can flow to the tray;
  • an outlet weir is formed at the junction of the receiving tray I and the tray; the guide element is located on the material and liquid outlet of the receiving tray I, and is located above and above the outlet weir. Below the downcomer of the flat push-flow distillation tray.
  • a set of plug flow components are provided on the flat plug flow rectification tray of the upper layer, and a set of plug flow components corresponding to it are provided on the flat plug flow rectification tray of the next layer.
  • Components, and the downcomers of the corresponding plug flow components from the adjacent plug flow rectification trays are arranged in a staggered arrangement;
  • the length of the flow passages for the liquid-phase material flow from the material liquid outlet of the liquid receiving tray I of the flat-plug flow assembly to the staged overflow weir are all equal.
  • the present invention also provides a method for preparing isophorone by liquid phase condensation of acetone, which is further improved on the basis of the technology disclosed in CN201110325830 and CN201110325843.
  • the method for preparing isophorone by liquid phase condensation of acetone includes the following steps:
  • step 2) The liquid-phase stream containing the reaction product obtained in step 1) enters the hydrolysis reaction section, and the by-products (ie, high-molecular-weight by-products in the condensation reaction product) contained in the liquid-phase stream containing carbon atoms ⁇ 12 and water Contact and hydrolyze to recover part of the valuable components;
  • the hydrolysis reaction section is carried out in a pressurized reactive distillation tower equipped with a flat plug flow distillation tray;
  • the pressurized reactive distillation tower is the above The pressurized reactive distillation tower;
  • the raw material acetone can be condensed to produce isophorone products with higher yield, reducing by-products, and significantly reducing downstream separation energy consumption and production costs.
  • the high boilers with carbon atoms ⁇ 12 obtained by the deep condensation of acetone are hydrolyzed in a pressurized reactive distillation tower, and unreacted light components are obtained at the top of the tower, which are condensed into a liquid state by a condenser and then recycled Continue to participate in the reaction in the upstream process section.
  • the product obtained at the bottom of the tower contains condensation products and catalyst solution.
  • the oil phase is mainly isophorone and by-product organics
  • the water phase is mainly water and catalyst solution.
  • the liquid phase stream containing the reaction product obtained in step 1) is mainly composed of water and valuable organic matter.
  • the valuable organic matter includes IP generated by the liquid-phase condensation reaction of acetone and high-boiling matter (such as xylose). Xylitone and Isoxylitone, etc.), and contains a small amount of acetone, diacetone alcohol, mesityl oxide, mesitylene, etc.
  • the condensation reaction section includes two or more condensation reaction sections connected in series, that is, the acetone aldol condensation reaction is carried out in at least two reaction process sections; preferably, the temperature of the aldol condensation reaction of each condensation reaction section is 190-280°C, preferably the temperature of the aldol condensation reaction in the first condensation reaction stage is 200-280°C.
  • the step 1) includes a first condensation reaction section and a second condensation reaction section, and through the first condensation reaction section, an acetone conversion rate of ⁇ 10%, preferably acetone conversion rate of ⁇ 8% is obtained. ; In the second condensation reaction section, acetone continues to react to obtain more IP (isophorone) products.
  • IP isophorone
  • the first condensation reaction stage can be carried out in the upper tray of the reactive distillation column, or can be carried out in a separate reactor, which is not particularly limited.
  • it can be carried out in a tubular reactor with a static mixer or a micro-channel mixer arranged in series before the reactive distillation column, or directly in a reactive distillation column reactor; more preferably a static mixer or a micro-channel mixer Tubular reactor with channel mixer.
  • the second condensation reaction stage can be carried out in a conventional reactive distillation tower, or in a pressurized reactive distillation tower reactor provided with a flat plug flow distillation tray (referred to as pressurized Reactive distillation tower).
  • the second condensation reaction section and the hydrolysis reaction section in step 2) are carried out in the same pressurized reactive distillation tower.
  • the pressurized reactive distillation tower the upper part is the condensation reaction section and the lower part It is the hydrolysis reaction section.
  • the trays provided in the pressurized reactive rectification tower can all be the flat plug flow rectification tray provided by the present invention, or part of the conventional trays available in the art (such as the pressure reactive rectification tower The upper part adopts this conventional tray), while part of it is the flat plug flow distillation tray provided by the present invention (for example, the lower part of the pressurized reactive distillation tower adopts the present invention tray), and the former is preferred.
  • the reaction temperature of the first condensation reaction section is operated at least 10°C higher than the second condensation reaction section.
  • the mass ratio (or mass flow ratio) of acetone and water in the first condensation reaction section is preferably 4-10:1; the mass ratio of acetone and water (or mass flow ratio) in the second condensation reaction section is preferably 4:1 -1:4, more preferably 4:1-1:2.
  • the second condensation reaction stage adopts a pressurized reactive distillation tower reactor at a temperature of 190-260°C and 20-60 Bar(A); preferably the temperature is 200-240°C, The pressure is 25-40 Bar (A); the second condensation reaction section in the pressurized reaction rectification tower preferably adopts a plate tower with a liquid residence time of 30-180 min, preferably 60-120 min.
  • the catalyst solution may be an aqueous solution containing KOH or NaOH, and the amount of the catalyst accounts for 0.001 to 1% of the total mass flow of the reactants, preferably 0.01 to 0.1%.
  • the present invention further optimizes the process for preparing isophorone by liquid-phase condensation of acetone.
  • a new type of flat plug flow distillation tray is provided.
  • the use of the tray in a pressurized reaction rectification tower facilitates the uniform distribution and flow of the liquid phase, which is close to the flat plug flow flow; at the same time, it is beneficial to solve the existing reactive distillation
  • the traditional reactive distillation trays have problems such as low rectification efficiency, serious foaming, liquid-liquid phase separation, uneven liquid flow, and large pressure drop on the trays.
  • the process of preparing isophorone by liquid-phase condensation of acetone can realize the defoaming of IP/lye streams without additional chemical additives. , Uniform flow and efficient operation; thereby providing a strong foundation for improving reaction efficiency, reducing product color numbers, reducing tray pressure drop, and simplifying production processes.
  • Figure 1 is a schematic diagram of the cylindrical spray hood and riser in an example
  • Figure 2 is a schematic diagram of the structure of the spray hood and the foam breaker when the cylindrical spray hood in an example is viewed from above;
  • Figure 3 is a schematic diagram of the rectangular jet hood and riser structure in an example
  • Figure 4 is a partial schematic top view of the arrangement of the rectangular spray hood and the foam plate on the tray in an example
  • Figure 5 is a schematic diagram of the reaction process for preparing IP by liquid phase condensation of acetone.
  • Figure 6a is a schematic diagram of the positional relationship between the downcomer and the liquid receiving tray of the adjacent-layer flat plug flow distillation tray;
  • Fig. 6b is a partial schematic diagram illustrating the structure of the flow guiding element in the top view of Fig. 6a;
  • Figure 7a Schematic diagram of the downcomer arrangement with multiple downcomers on the flat plug flow distillation tower plate
  • Figure 7b a schematic diagram of the arrangement of multiple downcomers provided on the flat plug flow rectification tower plate adjacent to the lower layer of Figure 7a;
  • Figure 8 In an example, the structure diagram of the adjacent upper and lower horizontal plug flow rectification trays arranged in the rectification tower.
  • the present invention provides a flat plug flow distillation tray.
  • Figure 8 shows a partial schematic diagram of a pressurized reactive distillation tower, which shows a schematic diagram of the upper and lower two layers of flat plug flow distillation trays 1 and 2 ; The figure does not fully show the structure of the plug flow distillation trays of other layers.
  • the flat plug flow distillation tray of the present invention will be described.
  • the flat plug flow distillation tray 1 includes tray 3 and flat plug flow assembly 48.
  • the flat plug flow assembly 48 includes downcomer 5, graded overflow weir 9, and light and heavy phase splitting elements. 13.
  • the liquid receiving pan I 6 and the guide element 20 is a partial schematic diagram of a pressurized reactive distillation tower, which shows a schematic diagram of the upper and lower two layers of flat plug flow distillation trays 1 and 2 ; The figure does not fully show the structure of the plug flow distillation trays of other layers.
  • the flat plug flow distillation tray of the present invention will be described.
  • the flat plug flow distillation tray 1 includes tray 3 and
  • the downcomer 5 is connected to the tray 3, and the downcomer 5 is provided with an inlet, which is located on the upper part of the downcomer.
  • the graded overflow weir 9 is arranged on the inlet of the downcomer 5, and a vertical flow channel is formed in the downcomer 5.
  • the material liquid on the tray 3 can overflow into the vertical flow channel of the downcomer 5 by the staged overflow weir 9.
  • the light-heavy phase splitting element 13 is arranged in the downcomer 5 and located below the graded overflow weir 9; the light-heavy phase splitting element 13 is used to receive the vertical overflow from the tray 3 through the overflow weir 9 to the downcomer 5
  • the material liquid in the flow channel, and separate the light phase material liquid and the heavy phase material liquid from these material liquids, the light and heavy phase splitting element 13 is also used to divert the light phase material liquid and the heavy phase material liquid to the down liquid through different channels Below tube 5.
  • the liquid receiving tray I 6 is connected to the tray 3, and the connection position with the tray 3 is the opposite side of the side where the downcomer 5 and the tray 3 are connected.
  • a guide element 20 Above the connection between the liquid receiving tray I 6 and the tray 3 is provided a guide element 20, and the guide element 20 is provided with a plurality of streams for diverting the liquid on the liquid receiving tray I6 to the tray 3 in multiple streams. A diversion channel.
  • An outlet weir 34 is preferably formed at the connection between the liquid receiving tray I and the tray, and the flow guiding element 20 is located above the outlet weir 34.
  • the outlet weir 34 is arranged obliquely, and the whole is in a slope shape.
  • the bottom of the outlet weir 34 is connected to the tray I7 through the first edge of the outlet weir 341
  • the top of the outlet weir 34 is connected to the tray 4 through the second edge of the outlet weir 342
  • the outlet weir 34 is connected to the receiving tray.
  • An obtuse angle is formed between I7, so that the outlet weir 34 forms an inclined upward ramp between the liquid receiving tray I7 and the tray 4.
  • the outlet weir is arranged in a slope shape, so that when the material liquid overflows from the liquid receiving pan I to the tray via the outlet weir, it is guided upward by the outlet weir, which facilitates the uniform distribution of light and heavy liquids.
  • the light-heavy phase diversion element 13 specifically includes a liquid receiving pan II 49, a dividing weir 41, a heavy phase channel 40, and a light phase channel 39.
  • the dividing weir 41 is arranged on the liquid receiving pan II49, and the liquid receiving pan II 49 is divided into a heavy phase liquid receiving area 38 and a light phase liquid receiving area 37.
  • the heavy-phase liquid receiving area 38 is located in the downcomer 5 and below the graded overflow weir 9, and is located on the same side as the graded overflow weir 9, so that the material flow in the downcomer 5 overflows from the graded overflow weir 9 Will preferentially flow into the heavy phase receiving area 38, that is, tend to flow into the heavy phase receiving area 38, so that the material can be deposited in the heavy phase receiving area 38, and then the heavy phase material liquid forming the lower layer and the light phase material of the upper layer can be separated Liquid, which plays a role in liquid phase separation.
  • the heavy phase channel 40 is used to divert the heavy phase material liquid deposited at the bottom or bottom of the heavy phase liquid receiving zone 38 to below the downcomer 5.
  • the light-phase liquid receiving area 37 is used to receive the light-phase material liquid from the upper part of the heavy-phase liquid-receiving area 38 overflowed by the dividing weir 41, and the light phase channel 39 is used to divert the light-phase material liquid in the light-phase liquid receiving area 37 To the bottom of the downcomer 5.
  • the heavy phase channel 40 and the light phase channel 39 the light phase material liquid and the heavy phase material liquid can respectively flow to the space below the downcomer 5 through separate channels.
  • a partition plate 42 is provided in the heavy phase channel 40, and a drainage port 43 is provided on the partition plate 42.
  • the inlet 45 and the outlet 46 of the heavy phase channel 40 are located on both sides of the partition plate 42 rather than on the same side with respect to the partition plate 42.
  • the heavy-phase channel 40 is specifically configured to form a channel by enclosing the heavy-phase drainage plate 44 and the dividing weir 41.
  • the lower edge of the heavy-phase drainage plate 44 and the bottom of the heavy-phase liquid receiving area 38 are left The spacing is used as the entrance 45 of the heavy phase channel; and the partition plate 42 is vertically arranged in the heavy phase channel 40 and connected to the receiving plate II 49; on the receiving plate II in the area between the partition plate 42 and the dividing weir 41 An opening 46 is provided as the outlet of the heavy phase channel.
  • the lower edge of the drainage port 43 is higher than the lower edge of the heavy phase drainage plate 44 (that is, the upper edge of the inlet 45 of the heavy phase channel), and the height difference between the two is preferably 20-100mm, which can also be called the liquid seal height ( See Figure 6a), the height difference can play a role of liquid seal.
  • the vertical distance between the lower edge of the heavy phase guide plate 44 and the bottom 36 of the heavy phase liquid receiving area 38 is preferably 20-200 mm.
  • the light phase channel 39 is formed by a member with an internal pipe provided in the light phase receiving area 37.
  • the internal pipe inlet of the member is a vertical distance from the bottom of the light phase receiving area.
  • the internal pipe outlet of the component leads to the area under the downcomer.
  • outlets of the light phase channel 39 and the heavy phase channel 40 are not particularly limited. For example, they can be elongated, round, square, etc., and can also be composed of multiple channel outlets distributed at intervals.
  • the outlets at the bottom of the phase channel 40 are respectively arranged to include a plurality of mutually discontinuous channel outlets, that is, each outlet is independently arranged and discontinuous to each other. Play a role similar to a liquid distributor.
  • the light phase channel is provided with a long strip-shaped outlet or the heavy phase channel is provided with a plurality of spaced outlets. This is only an example and is not limited to these forms. .
  • each guide channel 201 in the guide element 20 penetrates from the liquid receiving tray I7 to the direction of the tray 4.
  • the guide element 20 includes a set of guide vanes arranged above the outlet weir, and a group of guide vanes specifically includes a plurality of guide vanes.
  • Flow fins 202, a plurality of guide fins 202 are sequentially spaced above the outlet weir 34 along the first edge 341 of the outlet weir.
  • Diversion channels 201 are formed between adjacent guide fins 202, and each guide channel is formed by a liquid receiving plate. I penetrates in the direction of the tray.
  • each guide vane and the vertical line of the first edge 341 of the outlet weir is ⁇ 0° and ⁇ 90°, and the vertical line is located on the plane of the tray 4 connected to the outlet weir, And a perpendicular line perpendicular to the first edge 341 of the outlet weir.
  • the angles between adjacent guide vanes and the vertical line of the first edge of the outlet weir are the same or different.
  • each guide vane is arranged obliquely from an end of the first edge of the outlet weir close to the middle of the tray (or a position close to the middle of the tray) to the direction of the first edge of the outlet weir close to the end of the tower wall.
  • the angle between the guide vanes at both ends of the first edge of the outlet weir and the perpendicular is larger.
  • the gap between the guide vane closest to the tower wall and the tower wall also forms a channel, and its function is the same as that of the guide channel, which can also make the material liquid flow from the liquid receiving tray I to the tray.
  • the baffle can be fixed by welding, for example, fixed on the receiving tray, outlet weir and/or tray.
  • a baffle 14 is also provided in the downcomer 5, and the baffle 14 is provided in the space between the graded overflow weir 9 and the light-heavy-phase dividing element 13, and Located in the downcomer 5 on the side opposite to the side where the overflow weir 9 is provided, in FIG. 8, the baffle 14 is located directly above the light phase liquid receiving area 37.
  • the downcomer 5 specifically includes a downcomer plate 16 and a backing plate 15.
  • the downcomer plate 16 is connected to the tray 3, for example, the downcomer plate 16 is vertically installed on the tray 3; the backing plate 15 and the downcomer plate 16 is enclosed to form a vertical flow channel.
  • the specific shape of the downcomer 5 is not particularly limited, for example, it is a bow-shaped, rectangular or polygonal box-type downcomer.
  • the back plate 15 is higher than the grading overflow weir 9, so as to prevent the material from overflowing from the back plate.
  • the baffle 14 and the back plate 15 are connected, and the liquid receiving plate II49 is connected between the downcomer plate 16 and the back plate 15.
  • the number of stages of the graded overflow weir 9 is greater than or equal to 1, for example, there are overflow weirs of 1, 2, or 3 or more.
  • the meaning of the number of stages refers to the number of overflow weirs of different heights.
  • Fig. 8 shows a specific example with a three-stage overflow weir.
  • the one-stage overflow weir 12 is arranged on the downcomer plate 16, specifically formed by the downcomer plate 16 extending upward, higher than the tray 3
  • a flat surface forms an overflow weir; a plurality of overflow holes 47 of different heights are preferably opened on the first-level overflow weir 12 to ensure that the upper, middle and lower liquid layers on the tray 3 can overflow.
  • the number of stages of the staged overflow weir 9 is ⁇ 2.
  • the stage number of the staged overflow weir 9 is ⁇ 2, from the downcomer plate 16 to the direction gradually away from the downcomer plate 16 and towards the inner cavity of the downcomer 5,
  • the overflow weirs 9 are arranged at intervals and increase in height.
  • the second-stage overflow weir 11 is higher than the first-stage overflow weir 12, and the third-stage overflow weir 10 is higher than the second-stage overflow weir 11.
  • overflow weirs of different heights can ensure the uniformity of the liquid phase flow at different heights on the tray; more than two overflow channels are formed between the overflow weirs to facilitate the horizontal push of the liquid phase in the vertical direction
  • the design of the overflow weir with more than two stages can also effectively suppress the foam in the downcomer for the easy-foaming IP/lye system, and significantly reduce the impact of system foaming on the downcomer.
  • the height difference between two adjacent overflow weirs is 50-150mm, which is beneficial to the uniformity of liquid phase flow at different heights.
  • the flat push flow assembly 48 also preferably includes a riser tube 19 and a jet hood 17.
  • the riser tube and the jet hood are only schematically shown in Figure 8.
  • the specific structure of the two can be seen in Figures 1-4; 1 is a schematic diagram of the spray hood 17 (or called a cylindrical spray hood) with a circular cross-section;
  • Figure 2 is a schematic diagram of the structure of the cylindrical spray hood and the foam breaking plate when viewed from above;
  • Figure 3 is the spray hood with a rectangular cross-section 27 (or called a strip spray hood or a rectangular spray hood) schematic diagram,
  • FIG. 4 is a schematic diagram of the distribution of the strip spray hood 27 and the froth breaker plate on the tray in an example.
  • the riser pipe 19 is provided on the tray 3 and is located in the area between the staged overflow weir 9 and the liquid receiving tray I 6.
  • the riser pipe 19 is provided with a gas phase channel so that the gas phase below the tray can flow upward through the gas phase channel .
  • the spray hoods 17, 27 are set on the riser pipe 19, for example, a vertical hood is set on the riser pipe 19; a gap for the lower suction hole 25 is left between the bottom of the spray hoods 17, 27 and the tray 3;
  • the lower part of the covers 17 and 27 is provided with an upper liquid suction hole 26 located above the lower liquid suction hole 25, and the upper part of the spray covers 17 and 27 is provided with a spray hole 21, and the position of the spray hole 21 is higher than the gas phase passage outlet of the gas riser 19.
  • the spray hoods 17, 27 can be specifically fixed on the tray 3, for example, fixed on the tray 3 by screws or brackets.
  • the jet hoods 17, 27 are equipped with gas guide vanes 22 to guide the jet streams ejected from the jet holes 21 to reduce the collision between the jet streams ejected from the jet holes and reduce the generation of foam ;
  • the gas deflector 22 can be specifically arranged next to the injection hole 21.
  • the angle ⁇ between the gas deflector 22 and the tangential direction of the injection hole 21 surface is preferably 1-90°, more preferably 1-45°; each injection hole 21 is provided with a corresponding gas deflector 22, adjacent gas deflectors
  • the angle between the sheet 22 and the tangential direction of the surface of the corresponding injection hole 21 is the same or different, and the same angle is preferably used.
  • the spray hoods 17 and 27 are also provided with a foam breaking plate 23.
  • the position of the foam breaking plate 23 corresponds to the position of the spray hole 21.
  • the foam breaking plate 23 can be connected to the gas deflector 22 and opposite to the position of the spray hole 21; or, referring to FIG. 4, a foam breaking plate is provided at least between adjacent spray hoods 27.
  • the distance between the foam breaker 23 and the spray hole 21 is 1-200mm, preferably 10-100mm; the surface of the foam breaker 23 is smooth or rough, preferably a rough surface, and more preferably the foam breaker 23 has spikes, such as sharp Barbed nail board.
  • the spray hood 17, 27 or the tray 3 is provided with a foam breaker 23, which uses the solid surface to further eliminate foam and mist. The rough surface and the nail plate can strengthen the foam and defoam effect.
  • parts of the spray hoods 27 and 17 provided with the upper liquid suction holes 26 are formed with a necking structure 26 recessed into the spray hood.
  • the diameter of the spray hood at the necking structure is preferably 50%-99% of the diameter of other parts of the spray hood; when the cross section of the spray hood is rectangular, the spray hood is shrinking.
  • the width of the neck structure is preferably 50%-99% of the width of the rest of the spray hood.
  • the design of the necking structure reduces the cross-sectional area of the jet hood from the upper suction hole, increases the gas velocity, and causes the Bernoulli effect, that is, the increase in velocity and the decrease in pressure, which promote the effect of liquid absorption into the recess.
  • the height of the highest level overflow weir 10 of the graded overflow weir 9 is preferably between 30-1000m; the height of the riser pipe 19 is lower than the highest level overflow weir 10, preferably 10-50mm lower, more preferably 20-40mm lower .
  • the tray in the present invention can ensure extremely high liquid holding capacity: the design of a higher overflow weir, riser pipe and spray hood can ensure the holding time of the tray and the residence time required for the reaction.
  • the reactive distillation process is particularly suitable.
  • the cross-section of the riser pipe 19 may be circular or rectangular
  • the cross-sectional shape of the spray hoods 17, 27 are correspondingly circular or rectangular
  • the corresponding spray hood may be called a cylindrical spray hood or a bar-shaped spray hood.
  • the shape of the upper liquid suction hole 26 may be a rectangle, a trapezoid, a circle, or an ellipse, or a trapezoid, a rectangle, a circle, or an ellipse with slits.
  • the ratio of the open area of the upper liquid suction hole 26 to the lower liquid suction hole 25 is preferably 10-1:1.
  • the design of the upper and lower liquid suction holes and the optimization of the open area can ensure the upper liquid with a higher concentration of organic phase in the liquid phase.
  • the first phase enters the jet hood for mass transfer, which is of great significance for demulsification and improvement of IP recovery.
  • the shape of the spray holes can be round, rectangular, triangular or oblong, preferably rectangular holes or oblong holes, and the length ratio of the long and short sides of the spray holes is 1-20:1, preferably 1.5-10:1;
  • the present invention also provides a pressurized reactive distillation tower provided with the above-mentioned plug flow rectification trays.
  • the pressurized reactive distillation tower is provided with multiple horizontal plug flow arranged at intervals. Distillation tray. Refer to the above description for the specific structure description of the plug flow distillation tray.
  • the pressurized reaction rectification tower provided by the present invention is mainly based on the existing rectification tower, and its trays are improved.
  • Figure 8 illustrates the relative position of the upper and lower two-layer plug flow distillation trays 1 and 2 in a pressurized reactive distillation tower. Take this as an example to illustrate the pressure reactive distillation
  • the structure of the plug flow rectification trays in the adjacent layers of the tower is not shown in the figure one by one for the plug flow distillation trays of the remaining layers.
  • a liquid receiving tray I 7 on the flat plug flow distillation tray 2 of the next layer corresponds to the flat plug flow distillation tray I 7 of the upper layer.
  • the receiving tray I7 is used to receive the light phase material and the heavy phase separated from the light and heavy phase splitting element 13 of the upper level plug flow distillation tray 1.
  • Phase material liquid is provided.
  • the area between the junction of the receiving tray I7 and the tray 4 and the bottom of the downcomer 5 of the upper level plug flow rectification tray 1 is provided with the material liquid outlet 35 of the receiving tray I7, and on the receiving tray I7 The material liquid can flow to the tray 4 through the material liquid outlet 35.
  • An outlet weir 34 is formed at the junction of the liquid receiving tray I7 and the tray 4.
  • the outlet weir 34 is preferably arranged in an inclined manner, and the whole is inclined.
  • the bottom of the outlet weir 34 is connected to the tray I7 through the first edge of the outlet weir 341, the top of the outlet weir 34 is connected to the tray 4 through the second edge of the outlet weir 342, and the outlet weir 34 is connected to the receiver.
  • An obtuse angle is formed between the trays I7, so that the outlet weir 34 forms an inclined upward ramp between the liquid receiving tray I7 and the tray 4.
  • the outlet weir is arranged in a slope shape, so that when the material liquid overflows from the liquid receiving pan I to the tray via the outlet weir, it is guided upward by the outlet weir, which facilitates the uniform distribution of light and heavy liquids.
  • the guide element 20 is located on the material liquid outlet 35 of the liquid receiving tray I and above the outlet weir, that is, the transition area between the receiving tray I and the tray.
  • the guiding element 20 is formed with a plurality of guiding channels 201 spaced apart on the material and liquid outlet of the liquid receiving tray I, and each guiding channel penetrates from the receiving tray I7 to the direction of the tray 4, thereby making the receiving.
  • the material liquid on the tray I7 can be divided into a plurality of streams to flow toward the tray 4 more evenly; specifically, a plurality of guide vanes 202 can be distributed at intervals to form the guide element 20, and a self-receiving element 20 is formed between adjacent guide vanes.
  • the diversion channel 201 through which the liquid tray penetrates the direction of the tray for details, please refer to FIG. 6b.
  • Fig. 6b is a schematic view of the flow guiding element in Fig. 6a when viewed from above.
  • Fig. 6b is mainly to reflect the distribution of the flow guiding channels of the flow guiding element, and other components are not shown one by one.
  • the guide element 20 includes a set of guide vanes arranged above the outlet weir, and a group of guide vanes specifically includes a plurality of guide vanes 202,
  • the guide vanes 202 are arranged at intervals along the first edge 341 of the outlet weir 34 above the outlet weir 34.
  • Diversion channels 201 are formed between the adjacent guide vanes 202, and each guide channel extends from the liquid receiving tray I to the direction of the tray. Run through.
  • the angle between each guide vane and the vertical line of the first edge 341 of the outlet weir is ⁇ 0° and ⁇ 90°, and the vertical line is located on the plane of the tray 4 connected to the outlet weir, And a perpendicular line perpendicular to the first edge 341 of the outlet weir.
  • the angles between adjacent guide vanes and the vertical line of the first edge of the outlet weir are the same or different.
  • the present invention designs light and heavy phase splitting elements on the tray, which can play the role of light and heavy phase splitting and distribution, can effectively avoid the pulsation when the light and heavy two phases are mixed, and at the same time facilitate the even "distribution" of the light and heavy phases at the downcomer outlet
  • the light and heavy liquid in conjunction with the ramp design of the outlet weir and the design of the diversion element, can be more evenly distributed in the horizontal direction to achieve a flow close to the horizontal plug flow.
  • the specific shapes of the outlets of the light phase channel 39 and the heavy phase channel 40 are not particularly limited. For example, they can be elongated, circular, square, etc., and they can also be composed of multiple channel outlets distributed at intervals; preferably the light phase
  • the outlets at the bottom of the channel 39 and the heavy phase channel 40 are respectively arranged to include a plurality of mutually discontinuous channel outlets.
  • the outlets of the light phase channel 39 and the heavy phase channel 40 are preferably arranged as liquid distribution ports with a liquid distribution function, which play a similar liquid distribution function.
  • the function of the filter is to make the light phase material liquid and the heavy phase material liquid evenly distributed to the liquid receiving plate I7 directly below the light phase channel 39 and the heavy phase channel 40.
  • the light phase channel is provided with a long strip-shaped outlet or the heavy phase channel is provided with a plurality of spaced outlets. This is only an example and is not limited to these forms. .
  • one or more sets of flat plug flow assemblies 48 may be provided, for example, two or more sets of flat plug flow assemblies 48 are provided.
  • a set of plug flow components 48 is provided on the flat plug flow rectification tray 1 of the upper layer, and a set of plug flow components 48 are provided on the flat plug flow rectification tray 2 of the next layer.
  • the downcomers 5 of the corresponding plug-flow components from the adjacent-layer plug-flow rectification trays are arranged in a staggered arrangement; see Figure 8 for details.
  • Fig. 8 is a schematic diagram when only one set of flat plug flow components 48 is provided on each flat plug flow rectification tower plate. At this time, the back plate 15 is the tower wall of the pressure reaction rectification tower.
  • Each layer of plug flow rectification trays can also be provided with more than two sets of plug flow components 48.
  • Figures 7a and 7b show an example of the upper layer of plug flow distillation trays and the next layer.
  • Figure 7a An example arrangement of the guide vanes of the guide element located under the downcomer is also shown.
  • the liquid phase flows from the material liquid outlet (or outlet weir) of the liquid receiving tray I6 of the plug flow assembly 48 )
  • the lengths of the channels flowing to the staged overflow weir 9 are all equal.
  • the pressure reaction rectification tower with the flat plug flow rectification tray of the present invention in which the design of the light and heavy phase splitting element 13 can ensure that the light and heavy phases in the downcomer 5 can pass through their respective channels ( For example, the light phase channel and the heavy phase channel) flow to the next stage of the tray, combined with the design of the outlet weir 34 and the multi-stage overflow weir, to ensure that the fluid leaves the downcomer 5 and enters the next level of flat push-flow distillation tray
  • the flow on the tray 4 in the vertical direction can be close to the flow of the flat push flow; combined with the design of the guide element 20 above the outlet weir 34, it is ensured that the fluid leaves the downcomer 5 and enters the tray of the next layer of trays.
  • the horizontal flow on 4 is relatively uniform, which is close to the flow of flat push flow.
  • the use of the pressurized reactive distillation tower of the present invention can effectively overcome the pulsation phenomenon in the prior art without dividing the channel design, and effectively reduce the possible intermittent flow-no-flow-flow problems of the light and heavy phases, thereby improving the liquid phase Flow uniformity and reaction effect.
  • the downcomers of the upper and lower trays are arranged staggered so that the liquid phase flows out from the downcomer, and the flow channels from the material liquid outlet of the liquid tray I6 to the overflow weir 9 are equal, which can ensure that the liquid phase on the trays of the same stage flows close to each other.
  • Flat push
  • the overflow weir is a graded overflow weir, and the number of stages is ⁇ 1, preferably ⁇ 2, each stage of overflow weir is higher than the previous one, and the height difference is 50-150mm, so as to ensure the liquid phase flow at different heights on the tray The uniformity.
  • the first-level overflow weir of the staged overflow weir is equipped with overflow holes of different heights to ensure that the upper, middle and lower liquid layers can overflow, and the design of two or more overflow channels formed by the staged overflow weir, Ensure the horizontal plug flow of the liquid phase in the vertical direction; at the same time, the setting of the multi-stage overflow weir, for the easy-foaming IP/lye system, can also effectively inhibit the foam in the downcomer and significantly reduce the system The effect of foaming on the downcomer.
  • the liquid phase can flow close to the horizontal and vertical direction on the tray, and the light and heavy phases in the downcomer can also flow more uniformly, which can obtain a higher reaction yield for the series of reaction intermediate products. Provides a strong foundation.
  • the present invention also provides a method for preparing isophorone by liquid-phase condensation of acetone, which mainly includes the following steps:
  • step 2) The liquid phase stream containing the reaction product obtained in step 1) enters the hydrolysis reaction section, and the by-products with carbon atoms ⁇ 12 contained in the liquid phase stream are in contact with water and hydrolyzed; the hydrolysis reaction section is equipped with a horizontal push
  • the pressure reaction rectification tower used in the hydrolysis reaction section is the pressure reaction rectification tower provided by the present invention as described above; some valuable components are recovered by hydrolysis. Minute;
  • the condensation reaction section preferably includes two or more condensation reaction sections in series; preferably, the aldol condensation reaction temperature of each condensation reaction section is 190-280°C, preferably the aldol condensation reaction temperature of the first condensation reaction section It is 200-280°C.
  • Each condensation reaction stage can be carried out in a reactor well known in the art.
  • step 1) includes a first condensation reaction section and a second condensation reaction section, and through the first condensation reaction section, an acetone conversion rate ⁇ 10%, preferably acetone conversion rate ⁇ 8% is obtained, for example 5%-10%, 5%-8%, etc., of course, can also be lower; in the second condensation reaction stage, acetone continues to react to obtain more IP (isophorone) products.
  • IP isophorone
  • the reactor used in the first condensation reaction stage can be carried out in the upper tray of the reactive distillation tower, or in other reactors separately installed, such as a static mixer or a static mixer installed in series before the reactive distillation tower A tubular reactor with a microchannel mixer, or a reactive distillation tower reactor; more preferably a static mixer (such as the SMV static mixer of Sulzer, Switzerland) or a microchannel mixer (such as the German Eppen Germany’s Miprowa type microchannel reactor) tubular reactor.
  • the second condensation reaction stage can be carried out in a conventional reactive distillation tower, such as a sieve plate, a float valve, a bubble-cap type plate-type reactive distillation tower; preferably, it is carried out in the pressurized reactive distillation tower provided by the present invention.
  • the second condensation reaction section and the hydrolysis reaction section described in step 2) are preferably carried out in the same pressurized reactive distillation tower provided by the present invention, and the upper tray of the pressurized reactive distillation tower is the second condensation reaction section , The lower tray is the hydrolysis reaction section.
  • the reaction temperature of the first condensation reaction section is operated at least 10°C higher than that of the second condensation reaction section, for example, 10°C higher than that of the second condensation reaction section.
  • -50°C preferably 10-20°C higher;
  • the acetone-water mass ratio in the first condensation reaction stage is preferably 4-10:1;
  • the acetone-water ratio in the second condensation reaction stage is preferably 4:1-1:4, More preferably 4:1-1:2.
  • the second condensation reaction stage preferably adopts a pressurized reactive distillation tower reactor at a temperature of 190 ⁇ 260°C and 20 ⁇ 60Bar(A); the preferred temperature is 200 ⁇ 240°C, pressure 25-40Bar(A); the liquid phase residence time in the pressure reaction rectification tower of the second condensation reaction section is 30-180min, preferably 60-120min.
  • the catalyst solution may specifically be an aqueous solution containing KOH or NaOH, and the amount of the catalyst accounts for 0.001 to 1% of the total mass flow of the reactants, preferably 0.01 to 0.1%.
  • the high boilers such as Xylitone and Isoxylitone, etc.
  • carbon atoms ⁇ 12 obtained by the deep condensation of acetone are hydrolyzed in a pressurized reactive distillation tower.
  • the unreacted light components mainly acetone, but also a small amount of diacetone alcohol DAA, mesityl oxide MO, ⁇ -isophorone, trimethylbenzene, etc.
  • DAA diacetone alcohol
  • ME mesityl oxide MO
  • ⁇ -isophorone trimethylbenzene, etc.
  • the product obtained at the bottom of the tower contains condensation products and catalyst solution.
  • After passing through an oil-water separator it is divided into two phases of oil and water.
  • the oil phase is mainly isophorone and by-product organics
  • the water phase is mainly water and catalyst solution.
  • step 2) the liquid phase stream from step 1) is mainly composed of water and valuable organic matter.
  • the valuable organic matter includes IP generated by the liquid-phase condensation reaction of acetone and high boilers (such as xylose). Xylitone and Isoxylitone, etc.), and contains a small amount of acetone, diacetone alcohol, mesityl oxide, mesitylene, etc.
  • the tray has a large liquid holding capacity.
  • the pressure drop loss increases sharply, the foaming is serious, and the liquid
  • the liquid phase separation causes uneven mixing and uneven flow of the liquid phase.
  • step 2 is carried out in a pressurized reactive distillation tower equipped with such trays, so that the liquid phase is close to the flow of the flat plug flow on the tray.
  • the light and heavy phase splitting element makes the light and heavy phases in the downcomer flow evenly in the vertical direction to the receiving tray I of the lower tray according to different channels, avoiding the pulsation when the two phases are mixed, and then through the flow guiding element, so that The light and heavy phases are evenly distributed, combined with the oblique upward diversion function of the outlet weir, the light and heavy phases flow evenly in the horizontal direction to the tray of the next layer of trays.
  • the design of the staged overflow weirs with more than two stages can ensure the uniformity of the liquid phase flow at different heights on the tray.
  • Two or more overflow channels are formed between the overflow weirs, which is conducive to the leveling of the liquid phase in the vertical direction. Push flow.
  • the new flat-plug flow distillation tray of the present application is used to carry out the hydrolysis process for recovering valuable components in the by-products, without the need to add additional chemical additives (in the prior art, for example, CN201110140108, it is necessary to add at least one defoamer Isophorone can be prepared under the conditions of the agent, which can realize the defoaming of the IP/lye stream, uniform flow and efficient operation.
  • the rectification operation without additional additives can be carried out smoothly and efficiently.
  • the key is the innovative design of the internal components of the tower.
  • Traditional distillation towers such as bubble tower, valve tower, and sieve tray all belong to the category of bubbling distillation towers, and the operation mode fundamentally limits their applicability to easy-foaming systems.
  • the innovative tray internal component form (combined design of spray hood and riser tube) proposed by the present invention makes the gas phase need not be bubbled through the liquid layer, and the problem is solved by changing the mass transfer form.
  • the basic operation mode of the combined structure of the spray hood and the riser is:
  • the gas phase enters the spray hood through the riser.
  • the upper liquid phase and the lower liquid phase in the tray enter the spray hood through the upper suction hole at the necking structure of the spray hood and the lower suction hole near the tray.
  • the rising gas of the riser is torn into smaller droplets.
  • the gas phase is used as the continuous phase and the liquid phase is used as the dispersed phase in the spray hood and sprayed into the space outside the spray hood through the spray hole of the spray hood.
  • Contact and heat transfer, mass transfer; the liquid phase that falls back on the tray after the liquid phase is sprayed can strengthen the disturbance and mixing of the liquid phase on the tray in the vertical direction.
  • the adoption of a new-type tray structure can not only ensure the large liquid holding capacity required for the IP synthesis reaction, but also effectively solve the problem of large pressure drop, easy foaming, difficulty in liquid-liquid phase separation, and distillation efficiency in the IP synthesis reaction system. Low-level issues.
  • Step 2 The treated product is cooled and separated into two phases: oil and water, the oil phase is mainly organic products containing IP, and the water phase is mainly water and homogeneous base catalyst.
  • the treated organic phase is washed, flashed, distilled, rectified and other purification and purification methods, and finally obtained high-yield, low-color, and economically competitive qualified IP products.
  • the measurement method of the product color number in the embodiment is implemented in accordance with the regulations of GB/T 3143.
  • the organic phase composition of the IP reaction liquid was analyzed by gas chromatography (GC) analysis method, and the gas chromatography analysis conditions were as follows:
  • the analytical instrument used is: Shimadzu GC-2010PLUS;
  • Vaporization chamber temperature 180°C;
  • Program temperature rise conditions initial temperature 40°C, keep for 3 minutes, 15°C/min to 280°C, keep for 11 minutes;
  • Carrier gas high-purity nitrogen (purity 99.999%),
  • the plug flow distillation tray 1 includes a tray 3 and a plug flow assembly 48 arranged on the tray 3.
  • the plug flow assembly 48 includes a staged overflow weir 9, a downcomer plate 16, a light and heavy phase splitting element 13, and The liquid pan I6 and the guide element 20.
  • the plug flow rectification tray of this embodiment is a single overflow, that is, in the rectification tower, a downcomer 5 and a liquid receiver are installed on the trays of each layer of the flat plug flow rectification tray installed at intervals.
  • Disk I6, that is, a set of flat plug flow components 48 is installed.
  • the downcomers 5 of the plug flow assembly 48 of the upper and lower plug flow rectification trays are arranged in a staggered manner.
  • the liquid receiving trays I6 and 7 in the upper and lower layers are also arranged in a staggered manner.
  • Each liquid receiving tray I6 and 7 is correspondingly located on the upper Just below the downcomer 5 of a layer of flat push-flow distillation tray.
  • the diameter of the plug flow rectification tray is 800 mm. In this example, it is the distance between the downcomer back plates of the upper and lower plug flow distillation trays in FIG. 8.
  • the graded overflow weir 9 in each downcomer has 3 stages, namely, the first-stage overflow weir 12, the second-stage overflow weir 11, and the third-stage overflow weir 10, and the heights are 100, 150, and 100 respectively. 200mm.
  • the first-level overflow weir 12 has 60 overflow holes 47 with a diameter of 6 mm, and the overflow holes 47 are distributed at different heights.
  • the height of the lowest overflow hole 47 from the tray 3 is 50 mm.
  • the cross-sectional area of the downcomer accounts for 24% of the projected area of the tray in the vertical direction, and the back plate 15 of the downcomer 5 is 290 mm high. Since in this embodiment, a downcomer is installed on the tray of each horizontal plug flow rectification tray, the back plate 15 is the part of the tower wall corresponding to the rectification tower wall.
  • the horizontal distance between the primary overflow weir 12 and the secondary overflow weir 11 is 6 mm, and the horizontal distance between the secondary overflow weir 11 and the tertiary overflow weir 10 is 10 mm.
  • the light-heavy-phase flow dividing element 13 includes a liquid-receiving plate II 49, a dividing weir 41, a light-phase liquid-receiving area 37 and a heavy-phase liquid-receiving area 38, a light-phase channel 39 and a heavy-phase channel 40.
  • the specific structure is shown in Figure 8, Figure 6a-6b and The corresponding description in the previous section will not be repeated here.
  • the lower edge of the drainage hole 43 on the partition plate 42 of the heavy phase channel 40 is 50 mm higher than the lower edge of the gravity phase deflector 44, which corresponds to the "liquid seal height" in FIG. 6a.
  • the liquid-phase material flow flows from the material liquid outlet 35 (or the position corresponding to the outlet weir) of the liquid-receiving plate I6 of the flat-plug flow assembly to the flow channel of the graded overflow weir 9 Are equal.
  • the area between the connection between the receiving tray I6 and the tray 3 and the downcomer of the upper layer of the flat push-flow distillation tray is provided with the material liquid outlet 35 of the receiving tray I, and the receiving tray I
  • An outlet weir 34 is formed at the junction with the tray; the material and liquid outlet of the liquid receiving tray I is provided with a flow guiding element 20 and is located above the outlet weir 34.
  • the guide element 20 is provided with a plurality of guide channels 201 spaced apart on the material and liquid outlet of the liquid receiving tray I, and each guide channel penetrates from the liquid receiving tray to the direction of the tray, so that the The material liquid can be divided into relatively uniform multiple streams to flow toward the tray.
  • the structure of the guide element 20 can be seen in Figures 6a and 6b, and the specific structure description can be referred to the foregoing, and will not be repeated.
  • the spray hood 17 provided on the flat plug flow rectification tower plate of this embodiment is a cylindrical spray hood with a circular cross section.
  • the cylindrical spray hood 17 is provided on the tray 3, and there is a gap between the bottom of the spray hood and the tray, and the gap is used as the lower suction hole 25; the lower part of the spray hood 17 is provided There is an upper liquid suction hole 26, which is located above the lower liquid suction hole 25; the gas lift pipe 19 is installed on the tray 3, and the spray cover 17 is arranged on the gas lift pipe 19.
  • the riser tube 19 is cylindrical as a whole, with a circular cross section and a diameter of 30 mm.
  • the riser tube 19 is 160 mm higher than the tray 3.
  • the upper liquid suction hole 26 of the spray hood 17 is higher than the top outlet of the riser pipe 19, and the whole spray hood is also cylindrical.
  • the spray hood 17 has a necking structure 24 recessed toward the inside of the spray hood at the upper liquid suction hole 26.
  • the upper part of the spray hood is provided with spray holes 21.
  • the spray holes 21 are specifically rectangular gas spray holes arranged vertically and parallel to each other.
  • the total height of the spray hood is 300mm, and the upper diameter of the spray hood is 60mm.
  • the center of the upper suction hole 26 (that is, the middle part of the upper suction hole) is 100mm from the tray 3, and the diameter of the necking structure 24 is 45mm (this diameter does not include the transition area between the necking structure and the other parts of the spray cover diameter).
  • the upper and lower suction holes 26 and 26 are both rectangular in cross section (the specific structure of the lower suction holes is not shown in Figure 1), the width of the upper and lower suction holes is the same, and the heights of the upper and lower suction holes are 20mm and 10mm, respectively.
  • the opening area ratio is 2:1.
  • the spray holes 21 on the spray hood 17 are specifically 10 rows of 5*50 mm rectangular holes that are parallel in the vertical direction and arranged uniformly.
  • a guide vane 22 is provided next to the jet hole 21, and the tangential angle to the surface of the jet hole 21 is 45°.
  • a nail plate with sharp protrusions is provided next to the guide vane 22 as the foam breaking plate 23.
  • the foam breaker 23 is processed into an arc shape to prevent the gas and liquid between adjacent spray hoods and adjacent spray holes of the same spray hood from colliding with each other, resulting in additional foam.
  • the outer diameter of the foam breaker is 120mm (the outer diameter of the foam breaker is the diameter of the circle formed by each foam breaker).
  • This embodiment is basically the same as Example 1, except that the spray hood used in the flat plug flow distillation tray is a strip spray hood with a rectangular cross section (or called a rectangular spray hood):
  • the strip-shaped spray hood 27 is provided on the tray 3.
  • the same structural parts of the strip-shaped spray hood 27 and the cylindrical spray hood 17 of the first embodiment will not be repeated here.
  • Embodiment 1 the main differences are described as follows: the cross section of the riser tube 19 is rectangular, the length and width are 240mm and 20mm respectively, the longer side of the rectangle is installed on the tray 3 along the direction of liquid flow, the riser tube 19 160mm higher than tray 3.
  • the total height of the spray hood 27 is 200 mm.
  • the spray hood 27 is arranged on the riser 19, and the overall cross-sectional shape of the spray hood 27 is also rectangular.
  • the spray hood 27 is provided with a necking structure 24 recessed toward the inside of the spray hood at the upper suction hole 26, the upper part of the spray hood 27 has a width of 60mm, and the center of the upper suction hole 26 is 100mm higher than the tray; the upper suction hole has a necking structure.
  • the width is 50mm (this width does not include the width of the transition area between the necking structure and other parts of the spray cover).
  • the upper and lower suction holes 26 and 25 are rectangular in cross section (the specific structure of the lower suction holes is not shown in Fig. 3), the width of the upper and lower suction holes is the same, and the heights of the upper and lower suction holes are 15mm and 15mm, respectively.
  • the opening area is 1:1.
  • the upper part of the spray hood 27 is specifically provided with 14 rows of 8*100mm rectangular spray holes 21 arranged vertically, parallel to each other, and evenly arranged.
  • a gas deflector 22 is provided next to the spray cover.
  • the tangential direction of the gas deflector 22 and the spray hole (in this embodiment can be understood as the angle ⁇ ° with the surface of the spray hole) is an angle of 30° , To prevent the jet streams from adjacent jet holes of the same jet cover from colliding with each other, resulting in extra foam.
  • the foam breaker 23 is arranged on the tray 3, and is arranged parallel to the longer side of the spray hood 27, and can be positioned opposite to the spray hole 21 provided on the spray hood 27.
  • the foam breaker is 60 mm from the long side of the spray hood.
  • the foam breaker is a nail plate with rough surface or with nail-like protrusions to avoid the collision of gas and liquid between adjacent spray covers to cause extra foam.
  • the strip spray hoods are arranged in parallel on the tray at intervals, and foam breakers are installed between adjacent strip spray hoods.
  • the following examples illustrate the application of acetone liquid phase condensation to produce isophorone using a rectifying tower provided with a flat-plug flow rectifying tray of the present invention.
  • the measurement method of the product color number in the embodiment is implemented in accordance with the regulations of GB/T 3143.
  • FIG. 5 The schematic diagram of the process for preparing isophorone (or IP for short) by liquid-phase condensation of acetone is shown in FIG. 5, the acetone and NaOH aqueous solution are preheated by the preheater 28 and the mixer 29 (this embodiment specifically adopts the Swiss Sulzer Company
  • the SMV static mixer is fully mixed and then enters the first condensation reactor 30 (the reactor 30 used in this example is a tubular fixed-bed reactor), the reaction temperature is 210°C, the pressure is 3.5 MPa (G), and the acetone processing capacity It is 600kg/h, the mass ratio of acetone and water is 5:1, the catalyst is NaOH, and based on the total flow of the reaction liquid, the mass concentration of NaOH is 0.1%.
  • the acetone conversion rate corresponding to the outlet of the first condensation reactor 30 is 10%, and the reaction liquid (that is, the liquid phase stream) then enters the pressure reaction rectification tower 31.
  • the pressure reaction rectification tower 31 is at 3.0MPa and the temperature is 200°C. Operation, the mass ratio of acetone to water is 3:1.
  • the pressure reaction rectification tower 31 has a diameter of 800 mm and includes 50 trays of the present invention, of which the residence time of the second condensation reaction section is 30 min.
  • the trays used in this example are specifically the plug flow rectification tower in Example 1.
  • the arrangement of each tray in the rectification tower is also the same as in Example 1.
  • the cylindrical spray hood adopts the design of the cylindrical spray hood of the first embodiment.
  • the distance between the trays of the upper and lower flat push-flow distillation trays is 800mm, and the pressure drop of the single plate is 650Pa; the distance between the bottom of the tower and the bottom tray is 2.0m, and the upper limit of the liquid level of the tower is 1.2m.
  • the reactor liquid in the reaction rectification tower is cooled by the cooler 32, and is divided into two phases of oil and water by the water separator 33.
  • the content of IP (isophorone) in the obtained organic phase is 90%, the others are mainly high boiling point 9.5%, acetone 0.01%, and a small amount of intermediate components.
  • the color number of the IP product is less than No. 10, and the device and product quality are stable.
  • the single board pressure drop is small; the device has been running continuously for 1 year, and the product index is stable.
  • the schematic diagram of the process for preparing isophorone by liquid-phase condensation of acetone is shown in FIG. 5.
  • the acetone and KOH aqueous solution are preheated by the preheater 28 and the mixer 29 (this embodiment specifically adopts the SMV static mixer of Sulzer, Switzerland).
  • the first condensation reactor 30 the reactor used in this example is a tubular fixed-bed reactor
  • the reaction temperature is 250 °C
  • the pressure is 6 MPa (G)
  • the acetone processing capacity is 720 kg/h
  • acetone and The water ratio is 4:1
  • the catalyst is KOH
  • the mass concentration of KOH is 0.04% based on the total flow of the reaction liquid.
  • the acetone conversion rate corresponding to the outlet of the first condensation reactor 30 is 8%, and the reaction liquid (that is, the liquid phase stream) immediately enters the pressure reaction rectification tower 31, and the pressure reaction rectification tower is at a pressure of 5.0 MPa and a temperature of 240°C. Operation, the ratio of acetone to water is 4:1.
  • the pressure reaction rectification tower has a diameter of 800mm and includes 50 trays of the present invention, of which the residence time of the second condensation reaction section is 30min.
  • the trays used in this embodiment are specifically the plug flow rectification trays in Example 2.
  • the arrangement of the trays in the rectification tower is also the same as in Example 2.
  • the distance between the upper and lower flat push-flow distillation trays is 800mm, and the pressure drop of the single plate is 600Pa; the distance between the bottom of the tower and the bottom tray is 2.0m, and the upper limit of the liquid level of the tower is 1.2m.
  • the reactor liquid in the reaction rectification tower is cooled by the cooler 32, and is divided into two phases of oil and water by the water separator 33.
  • the IP content in the obtained organic phase is 92%, the others are mainly high boilers 7.5%, acetone 0.01%, and a small amount of intermediate components.
  • the color number of the IP product can be less than No. 10 and the device and product quality are running Stable, small single board pressure drop; the device has been running continuously for 1 year, and the product index is stable.
  • FIG. 5 The schematic diagram of the process for preparing isophorone (or IP for short) by liquid-phase condensation of acetone is shown in FIG. 5, the acetone and NaOH aqueous solution are preheated by the preheater 28 and the mixer 29 (this embodiment specifically adopts the Swiss Sulzer Company
  • the SMV static mixer is fully mixed and then enters the first condensation reactor 30 (the reactor 30 used in this example is a tubular fixed-bed reactor), the reaction temperature is 210°C, the pressure is 3.5 MPa (G), and the acetone processing capacity It is 450 kg/h, the mass ratio of acetone and water is 5:1, the catalyst is NaOH, and the total flow rate of the reaction liquid is used as a reference, and the mass concentration of NaOH is 0.1%.
  • the acetone conversion rate corresponding to the outlet of the first condensation reactor 30 is 10%, and the reaction liquid (that is, the liquid phase stream) then enters the pressure reaction rectification tower 31.
  • the pressure reaction rectification tower 31 is at 3.0 MPa and the temperature is 205-235. Operate at °C.
  • the pressure reaction rectification tower 31 has a diameter of 800mm and includes 50 traditional bubble-cap trays.
  • the residence time of the second condensation reaction section is 45min. It uses a single overflow downcomer.
  • the area of the downcomer is 24 of the cross-sectional area of the tower.
  • the height of the overflow weir is 200mm
  • 28 traditional cylindrical bubble caps are set on each tray
  • the riser is cylindrical
  • the inner diameter is 30mm
  • the height is 160mm, the same as in Example 1.
  • the distance between the trays of the upper and lower flat push-flow distillation trays is 800mm
  • the single-plate pressure drop is 1700Pa
  • the distance between the bottom of the tower and the bottom tray is 2.0m
  • the upper limit of the liquid level of the tower is 1.2m.
  • the reactor liquid in the reaction rectification tower is cooled by the cooler 32, and is divided into two phases of oil and water by the water separator 33.
  • the IP content in the obtained organic phase is 86.3%, and the others are mainly 13.4% of high boilers, 0.05% of acetone, and a small amount of intermediate components.
  • the color number of the IP product obtained according to the above embodiment is No. 25, with a light yellow color.
  • the inventor tried to increase the rectification load and then the acetone processing load, but the rectification tower was stopped due to flooding.
  • the upper limit of acetone processing is about 450 kg/h.
  • traditional tray technology such as the bubble cap tray used in this comparative example
  • IP synthesis a system that requires large liquid holding capacity and is easy to foam
  • the upper limit of the gas phase load of the rectification column is significantly reduced, and the rectification efficiency is significantly lower than the corresponding process of the novel tray disclosed in the present invention, resulting in a reduction in the load of the reactive rectification column and poor rectification effect.
  • the hydrolysis effect of high boilers will affect the color number and yield of IP products.
  • the pressurized reactive distillation tower based on the new flat plug flow distillation tray designed in the present invention can be used in the process of preparing isophorone by the liquid phase condensation of acetone, which can improve the reaction effect and promote the uniform flow of the liquid phase. And distribution is beneficial to improve production efficiency, improve product color number, and reduce tray pressure drop; and no additional chemical additives are needed to achieve defoaming of IP/lye streams; the device can operate stably and efficiently.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

La présente invention concerne un plateau de distillation à écoulement piston et un procédé de préparation d'isophorone par condensation en phase liquide de l'acétone. Le plateau de distillation à écoulement piston selon la présente invention comprend un plateau et un ensemble à écoulement piston disposé sur le plateau, l'ensemble à écoulement piston comprenant un trop-plein, un déversoir de trop-plein, un élément de division d'écoulement de phase lourde de lumière, un plateau de réception de liquide I et un élément de guidage d'écoulement ; le trop-plein est relié au plateau, et le déversoir de trop-plein est disposé sur une entrée du trop-plein ; l'élément de division de flux de phase légère-lourde est disposé dans le trop-plein et est situé au-dessous du déversoir de trop-plein arasé ; le plateau de réception de liquide I est relié au plateau, et est situé sur un côté opposé au côté où le trop-plein est relié au plateau ; l'élément de guidage d'écoulement est disposé au-dessus de la jonction du plateau de réception de liquide I et du plateau, et l'élément de guidage d'écoulement est pourvu d'une pluralité de passages de guidage d'écoulement. Une colonne de distillation réactive sous pression comprenant le plateau de distillation à écoulement piston de la présente invention peut être utilisée pour effectuer un post-traitement d'une IP (isophorone)/liquide alcalin qui est facile à mousser, de sorte que la phase liquide puisse être distribuée et s'écouler de façon relativement uniforme, ce qui facilite l'amélioration de l'effet de réaction.
PCT/CN2019/080512 2019-03-27 2019-03-29 Plateau de distillation à écoulement piston et procédé de préparation d'isophorine par condensation en phase liquide de l'acétone WO2020191789A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN201910237769.8 2019-03-27
CN201910237769.8A CN110038317B (zh) 2019-03-27 2019-03-27 平推流精馏塔板及丙酮液相缩合制备异佛尔酮的方法

Publications (1)

Publication Number Publication Date
WO2020191789A1 true WO2020191789A1 (fr) 2020-10-01

Family

ID=67275398

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/CN2019/080512 WO2020191789A1 (fr) 2019-03-27 2019-03-29 Plateau de distillation à écoulement piston et procédé de préparation d'isophorine par condensation en phase liquide de l'acétone

Country Status (2)

Country Link
CN (1) CN110038317B (fr)
WO (1) WO2020191789A1 (fr)

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110038317B (zh) * 2019-03-27 2020-04-10 万华化学集团股份有限公司 平推流精馏塔板及丙酮液相缩合制备异佛尔酮的方法
CN112441896B (zh) * 2019-09-03 2023-07-14 万华化学集团股份有限公司 一种丙酮液相缩合制备异佛尔酮的反应工艺
CN111888873A (zh) * 2020-08-13 2020-11-06 绿水青山环保科技（大连）有限公司 一种湿法全组分废气净化塔、净化系统及净化方法
CN113429290A (zh) * 2021-07-16 2021-09-24 南京延长反应技术研究院有限公司 一种dmc的制备系统及制备方法
CN114702089B (zh) * 2022-04-12 2023-03-31 中国神华煤制油化工有限公司 污水汽提塔的降液管溢流堰扰动装置及污水汽提塔
CN115845685B (zh) * 2022-12-29 2024-05-10 大连理工大学 一种逆流射流环隙微混合器

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102367223A (zh) * 2011-10-18 2012-03-07 烟台万华聚氨酯股份有限公司 一种异佛尔酮的合成方法
CN102516051A (zh) * 2011-10-18 2012-06-27 烟台万华聚氨酯股份有限公司 一种丙酮在碱性催化剂下液相缩合制备异佛尔酮的方法
CN102531866A (zh) * 2010-12-08 2012-07-04 赢创德固赛有限责任公司 异佛尔酮的制备方法
CN110038317A (zh) * 2019-03-27 2019-07-23 万华化学集团股份有限公司 平推流精馏塔板及丙酮液相缩合制备异佛尔酮的方法

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3700216A (en) * 1970-12-21 1972-10-24 Universal Oil Prod Co Vapor-liquid contacting device
AU8404298A (en) * 1997-07-18 1999-02-10 Koch-Glitsch, Inc. Tray-to-tray transfer device for chemical process tower
US20020175427A1 (en) * 2000-12-21 2002-11-28 Fluor Corporation Methods and apparatus for mixing fluids
CN100398174C (zh) * 2006-04-11 2008-07-02 西安石油大学 带消能器降液管的塔盘
CN201618434U (zh) * 2010-04-02 2010-11-03 天津市北方博隆塔器技术开发有限公司 一种板式塔的塔内件

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102531866A (zh) * 2010-12-08 2012-07-04 赢创德固赛有限责任公司 异佛尔酮的制备方法
CN102367223A (zh) * 2011-10-18 2012-03-07 烟台万华聚氨酯股份有限公司 一种异佛尔酮的合成方法
CN102516051A (zh) * 2011-10-18 2012-06-27 烟台万华聚氨酯股份有限公司 一种丙酮在碱性催化剂下液相缩合制备异佛尔酮的方法
CN110038317A (zh) * 2019-03-27 2019-07-23 万华化学集团股份有限公司 平推流精馏塔板及丙酮液相缩合制备异佛尔酮的方法

Also Published As

Publication number Publication date
CN110038317B (zh) 2020-04-10
CN110038317A (zh) 2019-07-23

Similar Documents

Publication Publication Date Title
WO2020191789A1 (fr) Plateau de distillation à écoulement piston et procédé de préparation d'isophorine par condensation en phase liquide de l'acétone
CN102188831B (zh) 反应蒸馏的方法
US11919845B2 (en) Reaction system and method for preparing butyraldehyde by propylene carbonylation
CN107735391A (zh) 蒸馏装置
CN108635889B (zh) 一种苯加氢系统中的轻苯蒸发塔及其工作方法
CN101613248B (zh) 一种热解聚双环戊二烯制环戊二烯的方法
CN109761940B (zh) 粗顺酐连续精馏装置及工艺方法
CN100465147C (zh) 一种分离3-羟基丙醛溶液中丙烯醛的精馏塔
CN101456807B (zh) 一种生产(甲基)丙烯酸的方法
CN104225955B (zh) 醚后碳四脱甲醇工艺
US11247958B2 (en) Method and apparatus for decomposing phenolic by-product
CN111377806B (zh) 一种丙酮液相缩合法制异佛尔酮的后处理工艺
CN110526823B (zh) 高纯度三正丁胺生产方法及所用装置
CN112920031A (zh) 一种制备1,3-丙二醇过程中丙烯醛分离回用的方法
CN111377807B (zh) 一种低色号、低酸值的异佛尔酮制备方法
US20130055896A1 (en) Microreactor device having an essentially vertical or inclined upper portion comprising means for collection and removal of gas formed in situ during a liquid-medium reaction and method
WO2023284024A1 (fr) Système de renforcement de micro-interface pour préparer de l'octénal par condensation de n-butyraldéhyde, et procédé de préparation
CN111018021B (zh) 基于侧线与塔釜回流比控制的硫化氢酸性水净化方法
KR102627301B1 (ko) 고순도 메탄올 생성을 위한 분리 벽 기술의 사용
CN112500269B (zh) 一种cdol脱氢制备cdon混合物冷却的装置系统和方法
CN205252611U (zh) 一种气液分离器
CN114618418B (zh) 一种用于Saucy-Marbet反应的装置和烯酮的制备方法
US20240174585A1 (en) Method for preparing isopropyl alcohol
CN204121807U (zh) 萃取塔
CN216093693U (zh) 一种生产α异佛尔酮的反应精馏塔

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 19921747

Country of ref document: EP

Kind code of ref document: A1

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 19921747

Country of ref document: EP

Kind code of ref document: A1