CN210796304U - Continuous production device for preparing polycarbonate dihydric alcohol - Google Patents

Continuous production device for preparing polycarbonate dihydric alcohol Download PDF

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Publication number
CN210796304U
CN210796304U CN201921284814.7U CN201921284814U CN210796304U CN 210796304 U CN210796304 U CN 210796304U CN 201921284814 U CN201921284814 U CN 201921284814U CN 210796304 U CN210796304 U CN 210796304U
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tower
storage tank
plate
reaction
continuous production
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刘修华
李义田
高伟
李培花
刘金玲
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Shandong Yuanli Technology Co ltd
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Shandong Yuanli Technology Co ltd
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Abstract

The utility model discloses a continuous production device for preparing polycarbonate dihydric alcohol, which comprises a reaction tower and a rectifying tower, wherein the reaction tower is connected with a first raw material storage tank, a second raw material storage tank, a first condenser and an intermediate product storage tank; the first condenser is connected with the first byproduct storage tank; the first byproduct storage tank is connected with the rectifying tower; the intermediate product storage tank is connected with the polymerization reaction kettle; the polymerization reaction kettle is connected with a vacuum buffer tank; the vacuum buffer tank is connected with the rectifying tower; the rectifying tower is connected with the second raw material storage tank; the rectifying tower comprises a tower body, and a plurality of first tower plates and second tower plates are arranged in the tower body in an up-down staggered manner; the utility model accelerates the moving-out speed of the byproduct alcohol, and improves the reaction conversion rate and the reaction rate; the aperture ratio of the tower plate of the rectifying tower is improved, the space utilization rate of the tower plate is improved, the gas-liquid contact area in the rectifying tower is increased, the gas-liquid contact time is prolonged, the mass transfer efficiency is improved, the recovery utilization rate of raw materials in the reaction process is improved, and the consumption of raw materials and energy is reduced.

Description

Continuous production device for preparing polycarbonate dihydric alcohol
Technical Field
The utility model relates to a preparation polycarbonate dihydric alcohol continuous production's device belongs to chemical industry equipment technical field.
Background
Polycarbonate diol (PCDL) is a polymer which contains a plurality of carbonate groups in a molecule and has hydroxyl groups at two ends of the molecule, is a novel multi-component compound, can be used for synthesizing polyurethane with excellent performance, and has excellent mechanical property, hydrolysis resistance, heat resistance, oxidation resistance and light resistance compared with the polyurethane synthesized by the traditional polyester polyol and polyether polyol. Therefore, polycarbonate diol (PCDL) is considered to be a polyol having the best performance at present, and is widely used for preparing various polyurethane materials with excellent quality and excellent performance.
The existing production technology of polycarbonate diol mainly adopts a kettle type reactor, raw materials of diol, micromolecular carbonate and a catalyst are added into a reaction kettle together for ester exchange method production, and after the reaction is finished, vacuum pumping is carried out for polycondensation to finally obtain a target product. The relatively advanced production mode is that one raw material and a catalyst are added into a reaction kettle, and then another raw material is dripped into the reaction kettle, so that the energy consumption is reduced, and the conversion rate of the raw material is improved.
The prior known technical data mostly explain the technology from the aspects of polycarbonate diol product modification, different types of products and catalyst modification. Chinese utility model CN205061943U discloses a process and apparatus for producing polycarbonate diol through dripping jar dropwise add raw and other materials, connect the rectifying column in the reation kettle top, carry out the mode of initial gross separation through the rectifying column with accessory substance methyl alcohol and raw and other materials dimethyl carbonate, make dimethyl carbonate backward flow to continue to participate in the reaction in reation kettle to reach the purpose that improves raw and other materials reaction conversion rate, reduce energy resource consumption, improve product quality.
The production technology of the polycarbonate diol described in the above patent is carried out under the improvement of the traditional batch kettle type reaction, on one hand, the process has the advantages of small gas-liquid contact time and contact area, low mass transfer efficiency and poor separation effect when the distillation tower carries out distillation; the aperture ratio of the tower plate is low, and the space utilization rate of the tower plate is low, so that the problems of large raw material consumption and low raw material recovery utilization rate in the reaction process exist; on the other hand, the reaction time period is long, and the energy consumption is relatively high, so that a larger promotion space exists in the production of the product field.
In view of the above, the prior art is obviously inconvenient and disadvantageous in practical use, and needs to be improved.
Disclosure of Invention
The utility model aims to solve the problems that the device for preparing the polycarbonate diol continuous production is provided, which can accelerate the moving-out speed of the byproduct alcohol and improve the reaction conversion rate and the reaction rate; the aperture ratio of the tower plate of the rectifying tower can be improved, the space utilization rate of the tower plate is improved, the gas-liquid contact area in the rectifying tower can be increased, the gas-liquid contact time is prolonged, the mass transfer efficiency is improved, the recovery utilization rate of raw materials in the reaction process is improved, and the consumption of raw materials and energy is greatly reduced.
In order to solve the problem, the utility model adopts the following technical scheme: a continuous production device for preparing polycarbonate dihydric alcohol comprises a reaction tower and a rectifying tower, wherein the upper part and the lower part of the reaction tower are respectively connected with a first raw material storage tank and a second raw material storage tank; the upper part of the reaction tower is also connected with a first condenser, the first condenser is connected with a first byproduct storage tank, and the first byproduct storage tank is connected with the rectifying tower; the lower part of the reaction tower is also connected with an intermediate product storage tank; the intermediate product storage tank is connected with the polymerization reaction kettle; the polymerization reaction kettle is also connected with a vacuum buffer tank; the vacuum buffer tank is connected with the rectifying tower; the vacuum buffer tank is also connected with a vacuum pump; the upper part of the rectifying tower is connected with a third condenser; the third condenser is connected with a storage tank for storing final byproducts; the bottom of the rectifying tower is connected with a second raw material storage tank;
the rectifying tower comprises a tower body, and a plurality of first tower plates and second tower plates are arranged in the tower body in an up-down staggered manner; the first tower plate and the second tower plate are both composed of a plurality of folded plates; the section of the folded plate is in an inverted V shape; the side edges of two adjacent folded plates are connected.
Furthermore, the plurality of folded plates form a circle around the axis of the tower body along the horizontal circumference to form a circle; a liquid flow channel is formed between every two adjacent folded plates; a plurality of air lifting holes are formed in the folded plate, and the air lifting holes are circular; the center distance between two adjacent air lifting holes is the same.
Furthermore, a baffle plate is arranged at one end, close to the center of the tower body, of each folded plate in the first tower plate, and the bottom end of each baffle plate is fixedly welded with the first blocking plate; the first blocking plate is welded and fixed with the first tower plate; a central downcomer is arranged above the first blocking plate; the lower end of the central downcomer is spaced from the upper surface of the first blocking plate by a certain distance; the lower end of the central downcomer is lower than the uppermost end of the first tray.
Furthermore, a plurality of first overflow weirs are arranged on the peripheral surface of the first tower plate fixed with the inner wall of the tower body; the height of the first overflow weir is equal to the highest point of the first tower plate.
Further, the lower part of the first overflow weir is communicated with an edge downcomer; the lower end of the edge downcomer extends to the upper part of the liquid flow channel of the second tower plate, and a certain distance is arranged between the lower end surface of the edge downcomer and the second tower plate.
Furthermore, a first control valve is arranged on a pipeline between the reaction tower and the first raw material storage tank.
Furthermore, a second overflow weir is fixedly arranged at the position, close to the center of the tower body, of the second tower plate, and the lower end of the second overflow weir is fixedly welded with the second blocking plate; the second blocking plate is of a disc-shaped structure with a central hole; the central hole of the second blocking plate is communicated with the upper end of the central downcomer.
Further, the height of the second overflow weir is equal to the highest point of the second tower plate; the second overflow weir is provided with an opening at the upper end.
Further, a reboiler is arranged between the reaction tower and the second raw material storage tank.
The utility model adopts the above technical scheme, compare with prior art, have following technological effect:
the utility model aims to solve the problems that the moving-out speed of the byproduct alcohol can be accelerated, the reaction conversion rate and the reaction rate are improved, and the reaction time is shortened; the aperture ratio of the tower plate of the rectifying tower can be improved, the space utilization rate of the tower plate is improved, the gas-liquid contact area in the rectifying tower can be increased, the gas-liquid contact time is prolonged, the mass transfer efficiency is improved, the recovery utilization rate of raw materials in the reaction process is improved, and the consumption of raw materials and energy is greatly reduced.
The present invention will be described in detail with reference to the accompanying drawings and examples.
Drawings
FIG. 1 is a schematic structural diagram of the present invention;
FIG. 2 is a schematic structural diagram of a column plate in the rectifying tower of the utility model;
in the figure:
1-a first raw material storage tank, 2-a second raw material storage tank, 3-an intermediate product storage tank, 4-a vacuum buffer tank, 5-a first byproduct storage tank, 6-a storage tank, 7-a reaction tower, 8-a rectification tower, 81-a tower body, 82-a first tower plate, 83-a central downcomer, 84-a first overflow weir, 85-an edge downcomer, 86-a second tower plate, 87-a second overflow weir, 88-a first blocking plate, 89-a baffle, 810-an air lifting hole, 811-a second blocking plate, 9-a polymerization reaction kettle, 10-a reboiler, 11-a first condenser, 12-a vacuum pump, 13-a second condenser, 14-a third condenser, 15-a first control valve, 16-a second control valve and 17-a third control valve, 18-fourth control valve, 19-fifth control valve, 20-feeding pipe, 21-folded plate.
Detailed Description
EXAMPLE 1A continuous production apparatus for producing polycarbonate diol
As shown in fig. 1, the utility model provides a continuous production device for preparing polycarbonate diol, which comprises a reaction tower 7, wherein the reaction tower 7 is used for a first step reaction, the first step reaction is specifically an ester exchange reaction, two raw materials react to generate an intermediate product and a first byproduct, and the first byproduct is a gaseous byproduct alcohol; the upper part and the lower part of the reaction tower 7 are respectively provided with a feeding hole; the upper part of the reaction tower 7 is also provided with a gas phase outlet; the lower part of the reaction tower 7 is also provided with a discharge hole;
a feed inlet at the upper part of the reaction tower 7 is connected with a first raw material storage tank 1 through a pipeline, and a first control valve 15 is arranged on the pipeline between the reaction tower 7 and the first raw material storage tank 1; a gas phase outlet at the upper part of the reaction tower 7 is connected with a first condenser 11, the discharge end of the first condenser 11 is connected with a first byproduct storage tank 5, and the discharge end of the first byproduct storage tank 5 is connected with a rectifying tower 8 through a pipeline; and a fifth control valve 19 is arranged on a pipeline between the first byproduct storage tank 5 and the rectifying tower 8.
The rectifying tower 8 is a variable pressure rectifying tower, a gas discharge port is formed in the upper part of the rectifying tower 8, and a liquid discharge port is formed in the bottom of the rectifying tower 8; the middle part of the rectifying tower 8 is provided with two byproduct feeding ports.
A gas discharge port at the upper part of the rectifying tower 8 is connected with a third condenser 13; the discharge hole of the third condenser 13 is connected with the storage tank 6; the storage tank 6 is used for storing a final byproduct, which is methanol in this embodiment;
a return pipe is also arranged on the third condenser 13 and is used for returning the condensate in the third condenser 13 to the rectifying tower 8;
a feed inlet at the lower part of the reaction tower 7 is connected with a reboiler 10; the feed end of the reboiler 10 is connected with the second raw material storage tank 2 through a pipeline; a second control valve 16 is provided on a pipe between the reboiler 10 and the second raw material storage tank 2.
The second raw material storage tank 2 is also connected with a liquid discharge hole at the bottom of the rectifying tower 8, and the high-purity second raw material separated by azeotropic separation in the rectifying tower 8 enters the second raw material storage tank 2 to be continuously used, so that the recovery rate of raw materials in the reaction process is improved, and the consumption of raw materials and energy is greatly reduced.
A discharge hole at the lower part of the reaction tower 7 is connected with a feed end of the intermediate product storage tank 3; the discharge end of the intermediate product storage tank 3 is connected with the polymerization reaction kettle 9 through a pipeline; a third control valve 17 is arranged on a pipeline between the intermediate product tank 3 and the polymerization reaction kettle 9; the polymerization reaction kettle 9 is used for the second step reaction, and the second step reaction is specifically that the intermediate product is subjected to polymerization reaction to generate a product and a second byproduct;
a feeding pipe 20 is connected to the upper part of the polymerization reaction kettle 9, and the feeding end of the feeding pipe 20 is communicated with a pipeline between the reboiler 10 and the second control valve 16;
a stirrer is arranged in the polymerization reaction kettle 9; the polymerization reaction kettle 9 is also connected with the vacuum buffer tank 4 through a pipeline; the discharge end of the vacuum buffer tank 4 is connected with a rectifying tower 8; a fourth control valve 18 is arranged between the vacuum buffer tank 4 and the rectifying tower 8;
the vacuum buffer tank 4 is also connected with a vacuum pump 12; the vacuum pump 12 is used for adjusting the degree of vacuum in the polymerization reaction vessel 9.
As shown in fig. 2, the rectifying column 8 includes a column body 81, a first tray 82, and a second tray 86; the first tower plate 82 and the second tower plate 86 are both arranged in the tower body 81; the number of the first tower plate 82 and the second tower plate 86 is multiple and the number of the first tower plates and the number of the second tower plates are the same;
the tower body 81 is of a cylindrical structure; the upper and lower ends of the tower body 81 are provided with end sockets.
The first tower plate 82 and the second tower plate 86 are both circular in plan view; the outer peripheral surfaces of the first tower plate 82 and the second tower plate 86 are welded and fixed with the inner wall of the tower body 81; the first tray 82 and the second tray 86 are each comprised of a plurality of flaps 21; the section of the folded plate 21 is in an inverted V shape; the side edges of two adjacent folded plates 21 are connected; the plurality of folded plates 21 form a circle around the axis of the tower body 81 along the horizontal circumference to form a circle; a liquid flow channel is formed between two adjacent folded plates 21; a plurality of air lifting holes 810 are formed in the folded plate 21, and the air lifting holes 810 are circular; the center-to-center distances between adjacent two of the lift holes 810 are the same.
A baffle 89 is arranged at one end of each folded plate 21 in the first tower plate 82, which is close to the center of the tower body, and the baffle 89 is triangular; the bottom end of the baffle 89 is welded and fixed with the first blocking plate 88; the first closure plate 88 is of a disc-shaped configuration; the upper surface of the first blocking plate 88 is fixedly welded with the first tower plate 82; the baffle 89 and the first blocking plate 88 are arranged to enable the liquid to flow along the liquid flow channel between two adjacent folded plates 21; a central downcomer 83 is arranged above the first blocking plate 88, and the central downcomer 83 is a circular pipe; the lower end of the central downcomer 83 is spaced a distance from the upper surface of the first blocking plate 88 and the lower end of the central downcomer 83 is lower than the uppermost end of the first tray 82.
A plurality of first overflow weirs 84 are arranged on the peripheral surface of the first tower plate 82 fixed with the inner wall of the tower body 81; the height of the first weir 84 is equal to the highest point of the first tray 82; the first overflow weir 84 is arranged on the liquid flow channel between two adjacent folded plates 21; the lower part of the first overflow weir 84 is communicated with a side downcomer 85; the edge downcomer 85 and the tower wall of the tower body 81 form a downcomer channel; the lower end of the edge downcomer 85 extends to the upper part of the liquid flow channel of the second tower plate 86, and a certain distance is arranged between the lower end surface of the edge downcomer 85 and the second tower plate 86, so that the liquid can smoothly flow into the liquid flow channel of the second tower plate 86;
a second overflow weir 87 is fixedly arranged at the position, close to the center of the tower body 81, of the second tower plate 86, and the height of the second overflow weir 87 is equal to the highest point of the second tower plate 86; the second overflow weir 87 is open at the upper end; the lower end of the second overflow weir 87 is welded and fixed with a second blocking plate 811; the second blocking plate 811 has a disc-shaped structure with a central hole; the second blocking plate 811 is welded and fixed with the second tower plate 86; the central hole of the second blocking plate 811 is communicated with the upper end of the central downcomer 83; the central downcomer 83 is welded and fixed below the second blanking plate 811.
The number of the first tower plate 82 and the second tower plate 86 is multiple; the first tray 82 and the second tray 86 are arranged in a vertically staggered manner, so that the liquid flows from the center of the column body 81 through the first tray 82 to the column wall of the column body 81, then flows through the side downcomer 85 to the second tray 86, flows from the second tray 86 to the center of the column body 81, and circulates in order to flow in the radial direction of the liquid.
The working principle of the utility model is as follows:
when the method is used, a first raw material enters the reaction tower 7 from the first raw material storage tank 1, a second raw material enters the reboiler 10 from the second raw material storage tank 2 to be vaporized and then enters the reaction tower 7 to perform sufficient ester exchange reaction with the first raw material, and an intermediate product and a gas-phase byproduct alcohol are generated; the degree of the transesterification reaction is controlled by controlling the feeding rate of the first raw material through the first control valve 15, thereby increasing the reaction conversion rate and the removal rate of the byproduct alcohol; the gaseous by-product alcohol and the gaseous second raw material enter a first condenser 11 for condensation, then enter a first by-product storage tank 5, and then enter a rectifying tower 8 through a second control valve 14; the intermediate product enters an intermediate product storage tank 3 from the bottom of the reaction tower 7; the intermediate product enters a polymerization reaction kettle 9 from an intermediate product storage tank 3 for polymerization reaction to generate a product and a second byproduct; the polymerization reactor 9 is adjusted in vacuum degree by a vacuum pump 12. The second by-product in the polymerization reaction kettle 9 enters a vacuum buffer tank 4, and then the vacuum buffer tank 4 enters a rectifying tower 8 to carry out azeotropic separation with the first by-product and the gas-phase raw material 2; the separated gas-phase by-product methanol is condensed by a second condenser 13 and then enters a storage tank 6 for storage, and the separated high-purity second raw material is condensed by a third condenser 14 and then enters a second raw material storage tank 2 for continuous use.
The utility model discloses the setting of well rectifying column plate structure improves the percent opening of rectifying column plate, improves the space utilization of column plate, can increase gas-liquid area of contact among the rectifying column, makes gas-liquid contact time increase, improves mass transfer efficiency, improves the recycle rate of raw materials in the reaction process, the consumption of greatly reduced raw materials and energy.
In a word, the utility model discloses can accelerate the speed of shifting out of accessory substance alcohol, improve reaction conversion rate and reaction rate, shorten reaction time.
The foregoing is illustrative of the best mode of the invention, and details not described herein are within the common general knowledge of a person of ordinary skill in the art. The protection scope of the present invention is subject to the content of the claims, and any equivalent transformation based on the technical teaching of the present invention is also within the protection scope of the present invention.

Claims (9)

1. A continuous production device for preparing polycarbonate dihydric alcohol is characterized in that: the device comprises a reaction tower (7) and a rectifying tower (8), wherein the upper part and the lower part of the reaction tower (7) are respectively connected with a first raw material storage tank (1) and a second raw material storage tank (2); the upper part of the reaction tower (7) is also connected with a first condenser (11), the first condenser (11) is connected with a first byproduct storage tank (5), and the first byproduct storage tank (5) is connected with a rectifying tower (8); the lower part of the reaction tower (7) is also connected with an intermediate product storage tank (3); the intermediate product storage tank (3) is connected with the polymerization reaction kettle (9); the polymerization reaction kettle (9) is also connected with the vacuum buffer tank (4); the vacuum buffer tank (4) is connected with the rectifying tower (8); the vacuum buffer tank (4) is also connected with a vacuum pump (12); the upper part of the rectifying tower (8) is connected with a third condenser (13); the third condenser (13) is connected with a storage tank (6) for storing final byproducts; the bottom of the rectifying tower (8) is connected with a second raw material storage tank (2); the rectifying tower (8) comprises a tower body (81), and a plurality of first tower plates (82) and second tower plates (86) are arranged in the tower body (81) in an up-down staggered manner; the first tray (82) and the second tray (86) are both composed of a plurality of folded plates (21); the section of the folded plate (21) is in an inverted V shape; the side edges of two adjacent folded plates (21) are connected.
2. The continuous production apparatus for producing polycarbonate diol according to claim 1, wherein: the plurality of folded plates (21) form a circle around the axis of the tower body (81) along the horizontal circumference to form a circle; a liquid flow channel is formed between two adjacent folded plates (21); a plurality of air lifting holes (810) are formed in the folded plate (21), and the air lifting holes (810) are circular; the center distance between two adjacent air lifting holes (810) is the same.
3. The continuous production apparatus for producing polycarbonate diol according to claim 1, wherein: a baffle (89) is arranged at one end of each folded plate (21) in the first tower plate (82) close to the center of the tower body, and the bottom end of the baffle (89) is welded and fixed with the first blocking plate (88); the first blocking plate (88) is fixedly welded with the first tower plate (82); a central downcomer (83) is arranged above the first blocking plate (88); the lower end of the central downcomer (83) is spaced a distance from the upper surface of the first closure plate (88); the lower end of the central downcomer (83) is lower than the uppermost end of the first tray (82).
4. The continuous production apparatus for producing polycarbonate diol according to claim 1, wherein: a plurality of first overflow weirs (84) are arranged on the peripheral surface of the first tower plate (82) fixed with the inner wall of the tower body (81); the height of the first overflow weir (84) is equal to the highest point of the first tray (82).
5. The continuous production apparatus for producing polycarbonate diol according to claim 4, wherein: the lower part of the first overflow weir (84) is communicated with an edge downcomer (85); the lower end of the edge downcomer (85) extends to the upper part of the liquid flow passage of the second tower plate (86), and a certain distance is arranged between the lower end surface of the edge downcomer (85) and the second tower plate (86).
6. The continuous production apparatus for producing polycarbonate diol according to claim 1, wherein: and a first control valve (15) is arranged on a pipeline between the reaction tower (7) and the first raw material storage tank (1).
7. The continuous production apparatus for producing polycarbonate diol according to claim 3, wherein: a second overflow weir (87) is fixedly arranged at the position, close to the center of the tower body (81), of the second tower plate (86), and the lower end of the second overflow weir (87) is fixedly welded with a second blocking plate (811); the second blocking plate (811) is of a disc-shaped structure with a central hole; the central hole of the second blocking plate (811) is communicated with the upper end of the central downcomer (83).
8. The continuous production apparatus for producing polycarbonate diol according to claim 7, wherein: the height of the second overflow weir (87) is equal to the highest point of the second tray (86); the second overflow weir (87) is open at the upper end.
9. The continuous production apparatus for producing polycarbonate diol according to claim 1, wherein: a reboiler (10) is arranged between the reaction tower (7) and the second raw material storage tank (2).
CN201921284814.7U 2019-08-09 2019-08-09 Continuous production device for preparing polycarbonate dihydric alcohol Active CN210796304U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117327260A (en) * 2023-11-30 2024-01-02 中国科学院宁波材料技术与工程研究所 Polyester oligomer, preparation method thereof, copolyester and application thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117327260A (en) * 2023-11-30 2024-01-02 中国科学院宁波材料技术与工程研究所 Polyester oligomer, preparation method thereof, copolyester and application thereof

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