CN113499596A - Esterification device and method for AA and BDO in PBAT production process - Google Patents
Esterification device and method for AA and BDO in PBAT production process Download PDFInfo
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/009—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D3/10—Vacuum distillation
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
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- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
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- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
- C08G63/82—Preparation processes characterised by the catalyst used
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Abstract
The utility model provides a device of esterifying of AA and BDO in PBAT production process, including little interface winding tubular reactor, the feed bin, the vacuum flash tank, the feed inlet of feed bin is used for linking to each other with the AA source, the BDO source, the bin outlet of feed bin is through the charge-in pump, the heater, it links to each other with the material passageway import of reactor, the material passageway export of reactor links to each other with the vacuum flash tank, the material passageway import sets up little interface generator, the bottom leakage fluid dram of vacuum flash tank is used for outside discharge BSA, the top steam exhaust mouth of vacuum flash tank links to each other with vacuum separator through the condenser, vacuum separator's noncondensable gas export all links to each other with the negative pressure source. The invention has simple structure, convenient operation and greatly improved operation efficiency, can meet the production requirement of large-scale production of PBAT with low cost, can ensure that the esterification reaction can be carried out in a forward direction without adopting a BDO excess mode, can effectively improve the esterification rate of AA and BDO to reach more than 98.5 percent, can also effectively avoid material back mixing, reduces the circulation volume of BDO by 95 percent and greatly reduces energy consumption.
Description
Technical Field
The invention relates to the field of chemical industry, in particular to an esterification device and method for AA and BDO in a PBAT production process.
Background
At present, plastics used in large quantities, such as polyvinyl chloride, polyethylene, polypropylene and the like, do not have biological self-degradability, form a large amount of white garbage and cause serious environmental pollution. The fly ash, dioxin and other harmful gases generated by incineration treatment seriously pollute the atmosphere and seriously threaten the human health.
In 16 days 1 month in 2020, the ministry of national development and improvement, in conjunction with the ecological environment, issued an opinion on further enhancement of plastics pollution control, required in 2025 to perfect a management system of links such as production, circulation, consumption and recycling of plastic products, and gradually forbid and restrict the use of non-degradable plastics. At present, a plurality of provinces issue local edition plastic forbidden orders successively. The degradable plastic has great practical significance for environmental protection and sustainable development, and the production and use of the bio-based degradable plastic are imperative.
PBAT (polybutylene adipate terephthalate) is a copolymer of PTA (terephthalic acid), BDO (1,4 butanediol) and AA (adipic acid), has good ductility, elongation at break, heat resistance and impact resistance, has excellent biodegradability, and is one of the current low-carbon, environment-friendly and biodegradable plastics. In the degradable plastics, the high-performance degradable plastics of a few tensile films, compared with the degradable plastics modified by blending the PBAT with PLA (polylactic acid) and PPC (carbon dioxide-based cyclopropyl resin), have wider application range and wider application range, such as: packaging films, agricultural mulching films, shopping bags, garbage bags, rolling bags, express bags, take-away disposable lunch boxes and the like.
Typically, the production of PBAT comprises the following six procedures:
(1) PTA/BDO esterification procedure
(2) AA/BDO esterification procedure
(3) PTA/BDO and AA/BDO ester fully-mixed esterification procedure
(4) Esterification steam separation process
(5) Polycondensation step
(6) Post-treatment Process
At present, a stirring type esterification kettle is adopted for esterification reaction aiming at the AA and BDO esterification procedure. Stirring formula esterification kettle is discontinuous reation kettle, lead to AA and BDO's esterification efficiency lower, and need add excessive BDO and guarantee that esterification reaction goes on towards the forward, lead to follow-up separation BDO's cost higher, in addition, to large-scale production PBAT's demand, kettle-type esterification kettle throughput receives agitator and heat transfer area restriction, single kettle-type esterification kettle throughput is limited, can only be through the mode of increasing stirring formula esterification kettle quantity, still lead to enterprise production PBAT's investment cost higher.
Therefore, how to develop a production device and a process of PBAT with large production capacity, low consumption, less three wastes and low investment is a problem to be solved urgently by technical personnel in the field.
Disclosure of Invention
One of the purposes of the invention is to provide an esterification device of AA and BDO in the production process of PBAT aiming at the defects of the prior art, which has simple structure, convenient operation and greatly improved operation efficiency and can meet the production requirement of large-scale production of PBAT with low cost.
The invention also aims to provide a method for esterifying AA and BDO by adopting the esterification device, which can ensure that the esterification reaction can be carried out in a forward direction without adopting a BDO excess mode, can effectively improve the esterification rate of AA and BDO to reach more than 98.5 percent, can also effectively avoid material back mixing, reduces the circulating amount of BDO by 95 percent, and greatly reduces the energy consumption required by the rectification and recovery of BDO.
The technical scheme for realizing one purpose of the invention is as follows: the utility model provides a device of esterifying of AA and BDO in PBAT production process, includes reactor, feed bin, vacuum flash tank, be equipped with the agitator in the feed bin, the feed inlet of feed bin is used for linking to each other with AA source, BDO source, and the bin outlet of feed bin is through charge-in pump, heater, and the material passageway import with the reactor links to each other, sets up little interface generator in the esterification reactor, and the esterification reactor is around tubular reactor, the material passageway export of reactor with the vacuum flash tank links to each other, the material passageway import sets up little interface generator, the bottom leakage fluid dram of vacuum flash tank is used for external discharge BSA, the top steam vent of vacuum flash tank links to each other with vacuum separator through the condenser, vacuum separator's noncondensable gas export all links to each other with the negative pressure source.
The reactor is a micro-interface winding tube type fixed bed reactor and comprises a closed shell, a material channel is arranged in a winding tube of the shell, and a medium channel is arranged in a space between the material channel and the shell.
The material channel is a pipeline, the pipeline is bent and extended in a reciprocating mode in the hollow space of the shell, the pipeline is divided into two sections, the two sections of pipelines are bent and extended in a reciprocating mode to form a first winding pipe and a second winding pipe, and the second winding pipe rotates 90 degrees relative to the first winding pipe along the circumferential direction of the shell.
The number of the material channels is one or more, and the material channels are arranged in the inner space of the shell side by side.
The medium channel uses a mixture of biphenyl and biphenyl ether as a heat medium, and the mass ratio of the biphenyl to the biphenyl ether is 1: 3.
And a liquid outlet at the bottom of the vacuum separator discharges esterified water containing BDO through a water pump, and the storage bin is formed by connecting an upper cylindrical section and a lower inverted conical section into a whole.
The second technical scheme for realizing the aim of the invention is as follows: the method for synthesizing BSA by using any one of the esterification apparatuses comprises the following steps:
1) adding BDO and AA into a storage bin, and uniformly stirring to obtain AA/BDO solid-liquid slurry, wherein the molar ratio of BDO to AA is 1.05-1.1: 1;
2) heating the AA/BDO solid-liquid slurry to 160-class 220 ℃ by a heater to obtain AA/BDO homogeneous-phase slurry, entering a material channel of a reactor after entering a reactor micro-interface generator, carrying out esterification reaction at the esterification temperature of 190-class 260 ℃ by using materials in the tube and using a heat medium between the tubes to generate BSA (bovine serum albumin) and esterification water;
3) and discharging BSA (bovine serum albumin) and esterification water to a vacuum flash tank, wherein the vacuum degree is 0.2bar (A), the esterification water is condensed into liquid state from a top steam outlet through a condenser in a steam state, the liquid state enters a vacuum separator for gas-liquid separation, and the BSA is discharged from a bottom liquid outlet of the vacuum flash tank in a liquid state.
Preferably, the molar ratio of BDO to AA in step 1) is 1.1: 1.
preferably, the temperature of the AA/BDO slurry in the step 1) is 40-60 ℃, the temperature of the AA/BDO slurry in the step 2) is raised to 180 ℃, the esterification temperature is 200 ℃, and the esterification time is 1 h.
Further, the homogeneous slurry and the catalyst in the step 2) enter a material channel of the reactor through a micro-interface generator, the adding amount of the catalyst is 0.1-0.5kg/t PBAT, and the catalyst is tetrabutyl titanate.
Adopt above-mentioned technical scheme to have following beneficial effect:
1. the reactor of the esterification device is provided with the material channel which is an esterification space of AA and BDO, can continuously carry out esterification reaction, greatly improves the esterification efficiency compared with the batch esterification reaction of the traditional stirring esterification kettle, does not have the phenomenon of material back mixing, greatly reduces the circulation volume of materials, particularly BDO by more than 95 percent, and effectively reduces the energy consumption.
2. The reactor of the esterification device is characterized in that a material channel is a pipeline and extends in a reciprocating bending manner, a micro-interface generator is arranged at an inlet of the material channel, so that homogeneous slurry entering the material channel is subjected to interface esterification reaction at a micron level, a winding pipe is arranged in the reactor, the material disturbance in a micro-interface state is enhanced, the esterification efficiency and the esterification rate of AA and BDO can be effectively improved to more than 98.5%, and the molar ratio of AA to BDO can be directly 1.1: 1 (including a small amount of BOD which is dehydrated to generate THF), the esterification reaction can be carried out in the positive direction without adopting a BDO excessive mode, the defects that the AA and the BDO in the traditional stirring esterification kettle are not esterified completely and the unesterified BDO causes the separation burden of downstream procedures due to low esterification rate are effectively overcome, and the esterification time is shortened to 1 h.
3. According to the reactor of the esterification device, the space between the material channel and the shell is the medium channel, and by increasing the number and the length of the material channels, enough heat exchange area can be provided, the heat exchange efficiency of the material channels is greatly improved, and the control requirement of enterprises on esterification reaction parameters can be effectively met.
4. The material channel of the reactor of the esterification device is a pipeline which is bent and extended in a reciprocating manner, so that the space utilization rate of the reactor is greatly improved, the requirements of different capacities can be met by adjusting the number and the length of the material channels, and the equipment investment cost and the space occupation amount are greatly reduced compared with the traditional stirring esterification kettle.
5. The heat medium used by the reactor medium channel is a mixture of biphenyl and biphenyl ether, and the mass ratio of the biphenyl to the biphenyl ether is 1:3, the vapor-liquid two-phase performance is excellent, the vapor phase enters the medium channel to supply heat to the material channel, the temperature of the esterification reaction is controlled to be 190-260 ℃ by controlling the vapor quantity of the mixture, after the heat is supplied, the mixture is liquefied into liquid, and the liquid is discharged from the medium channel and recycled after being vaporized. If the mass ratio of biphenyl to biphenyl ether is too low, the polymerization temperature is too high, resulting in a higher molecular weight of the polymer, and if the mass ratio of biphenyl to biphenyl ether is too high, the polymerization temperature is too low, resulting in a lower molecular weight of the polymer.
6. The esterification method of the invention utilizes a heater to heat AA/BDO solid-liquid slurry to 160-220 ℃ to obtain homogeneous slurry, the homogeneous slurry enters a one-way flowing material channel after being processed by a micro-interface generator to carry out typical interface reaction, meanwhile, the material channel is divided into two sections, the two sections of pipelines are respectively bent and extended to and fro to form a first winding pipe and a second winding pipe, and the second winding pipe rotates 90 degrees along the circumferential direction of the shell relative to the first winding pipe, so that the materials are continuously blended in the unidirectional flow process, fresh BDO and AA are exchanged to the surface layer of the interface, the esterified substance is continuously removed, the aim of 'promoting aging new' is achieved, the esterification rate of AA and BDO can be effectively improved to more than 98.5 percent, and then raw materials (AA and BDO) can be fed according to the theoretical value proportion (1: 1.1), so that the defect of subsequent BDO separation caused by excessive BDO in the traditional esterification method is avoided.
7. The esterification method of the invention also adds a catalyst to ensure the complete esterification of AA and BDO, and on the basis of ensuring the complete esterification, the invention avoids the problems of large CV value of the polymer, too wide molecular weight distribution, low esterification rate and un-esterified monomer existing in the materials discharged from the reactor to increase the burden of a subsequent separation system due to the fact that the catalyst is not added or the adding amount of the catalyst is too low by controlling the adding amount of 0.1-0.5kg/t PBAT.
The following further description is made with reference to the accompanying drawings and detailed description.
Drawings
FIG. 1 is a schematic connection diagram of an esterification apparatus according to the present invention.
In the attached figure, 1 is a reactor, 2 is a storage bin, 3 is a vacuum flash tank, 4 is a feeding pump, 5 is a heater, 6 is a condenser, 7 is a vacuum separator, and 8 is a water pump.
Detailed Description
In the invention, the equipment or the component which is not marked with a specific structure or model is generally conventional equipment or component in the chemical field, and the equipment or the component which is not marked with a specific connection mode is generally a conventional connection mode in the chemical field or a connection mode suggested by a manufacturer.
Example 1
Referring to fig. 1, a specific example of an apparatus for esterification of AA and BDO in a PBAT production process is shown. The esterification apparatus for AA and BDO in the production of PBAT comprises a reactor 1, a silo 2, a vacuum flash tank 3. The storage bin 2 is formed by connecting an upper cylindrical section and a lower inverted conical section into a whole, a coil pipe is further arranged in the storage bin and used for heating and insulating AA and BDO in the storage bin, a stirrer is arranged in the storage bin, a feed inlet of the storage bin 2 is used for being connected with an AA source and a BDO source, AA (adipic acid) is usually powder, and BDO (1, 4-butanediol) is usually oily liquid. The discharge outlet of the storage bin 2 is connected with the inlet of the material channel of the reactor 1 through a feed pump 4 and a heater 5, the feed pump adopts a jacket gear pump, and the heater adopts high-temperature heat conducting oil as a heat medium. The outlet of the material channel of the reactor 1 is connected with the vacuum flash tank 3, the inlet of the material channel is provided with a micro-interface generator, in the embodiment, the reactor 1 comprises a micro-interface generator, a winding tube, a closed shell, the closed shell extends along the vertical direction, the shell is characterized in that a material channel is arranged in a winding pipe of the shell, a space between the material channel and the shell is a heat medium channel, the heat medium channel uses a mixture of biphenyl and diphenyl ether as a heat medium, the mass ratio of the biphenyl to the diphenyl ether is 1:3, an inlet of the material channel is positioned at the upper part of the shell, an outlet of the material channel is positioned at the lower part of the shell, specifically, the material channel is a pipeline, the pipeline extends in a reciprocating bending mode in the hollow space of the shell, the pipeline is divided into two sections, the two sections of the pipeline respectively extend in a reciprocating bending mode to form a first winding pipe and a second winding pipe, and the second winding pipe rotates 90 degrees relative to the first winding pipe along the circumferential direction of the shell. According to the capacity requirement, the number of the material channels is one or more, the material channels are arranged in the hollow space of the shell side by side, and the length of the material channels is determined according to the esterification time. The bottom liquid discharge port of the vacuum flash tank 3 is used for discharging BSA (target product, butanediol adipate) outwards, the top steam discharge port of the vacuum flash tank 3 is connected with the vacuum separator 7 through the condenser 6, non-condensable gas outlets of the condenser 6 and the vacuum separator 7 are both connected with a negative pressure source, and specifically, the bottom liquid discharge port of the vacuum separator 7 is used for discharging esterified water containing BDO outwards through the water pump 8 and recycling the BDO in the esterified water.
Example 2 production of 30 million tons/year PBAT
A method for synthesizing BSA using the esterification apparatus of example 1, including the steps of:
1) adding BDO (60 ℃, oily liquid) and AA (30 ℃ powder) into a storage bin, stirring and uniformly mixing to ensure that the powder AA and the liquid-phase BDO are fully mixed to obtain AA/BDO solid-liquid slurry, and controlling the temperature of the solid-liquid slurry to be 40-60 ℃;
2) pumping the AA/BDO solid-liquid slurry by a feed pump, heating to 180 ℃ by a heater to obtain AA/BDO homogeneous slurry, and mixing with a catalyst (tetrabutyl titanate, the addition amount is 0.1-0.5kg/t PBAT)
Entering a material channel of the reactor through a micro-interface generator, carrying out esterification reaction at the esterification temperature of 200 ℃ for 1h, and discharging BSA and esterification water from an outlet of the material channel;
3) BSA and esterification water are discharged to a vacuum flash tank, the flow rate is 17.5t/h, the vacuum degree of the vacuum flash tank is 0.2bar (A), the esterification water is condensed into liquid from a top steam outlet through a condenser in a steam state, the liquid enters a vacuum separator for gas-liquid separation to obtain esterification water containing BDO, the flow rate is 1.93t/h, the esterification water is used for separating and recovering the BDO in the esterification water, the BSA is discharged from a bottom liquid outlet of the vacuum flash tank in a liquid state and is used as a raw material in a mixed esterification kettle process, the flow rate is 15.57t/h, and the purity is 98.5 percent
The esterification rate of AA and BDO was calculated to be 98.5%.
Claims (10)
1. An esterification device of AA and BDO in the production process of PBAT is characterized by comprising a reactor (1), a storage bin (2) and a vacuum flash tank (3),
a stirrer is arranged in the bin (2), a feed inlet of the bin (2) is used for being connected with an AA source and a BDO source, a discharge outlet of the bin (2) is connected with a material channel inlet of the reactor (1) through a feed pump (4) and a heater (5), a material channel outlet of the reactor (1) is connected with the vacuum flash tank (3), a micro-interface generator is arranged at the material channel inlet,
the bottom liquid discharge port of the vacuum flash tank (3) is used for discharging BSA outwards, the top steam discharge port of the vacuum flash tank (3) is connected with the vacuum separator (7) through the condenser (6), and the non-condensable gas outlets of the condenser (6) and the vacuum separator (7) are connected with a negative pressure source.
2. The apparatus for esterification of AA and BDO in the production of PBAT according to claim 1, characterized in that: the reactor (1) is a micro-interface winding tube type fixed bed reactor and comprises a closed shell, a material channel is arranged in a winding tube of the shell, and a space between the material channel and the shell is a medium channel.
3. The apparatus for esterification of AA and BDO in the production of PBAT according to claim 2, characterized in that: the material channel is a pipeline, the pipeline is bent and extended in a reciprocating mode in the hollow space of the shell, the pipeline is divided into two sections, the two sections of pipelines are bent and extended in a reciprocating mode to form a first winding pipe and a second winding pipe, and the second winding pipe rotates 90 degrees relative to the first winding pipe along the circumferential direction of the shell.
4. The apparatus for esterification of AA and BDO in the production of PBAT according to claim 2 or 3, characterized in that: the number of the material channels is one or more, and the material channels are arranged in the inner space of the shell side by side.
5. The apparatus for esterification of AA and BDO in the production of PBAT according to claim 2, characterized in that: the medium channel uses a mixture of biphenyl and biphenyl ether as a heat medium, and the mass ratio of the biphenyl to the biphenyl ether is 1: 3.
6. The apparatus for esterification of AA and BDO in the production of PBAT according to claim 1, characterized in that: the esterification water containing BDO is discharged from a bottom liquid outlet of the vacuum separator (7) through a water pump (8), and the storage bin (2) is formed by connecting an upper cylindrical section and a lower inverted conical section into a whole.
7. A method for synthesizing BSA using the esterification apparatus according to any of claims 1 to 6, which comprises the steps of:
1) adding BDO and AA into a storage bin, and uniformly stirring to obtain AA/BDO solid-liquid slurry, wherein the molar ratio of BDO to AA is 1.05-1.1: 1;
2) heating the AA/BDO solid-liquid slurry to 160-class 220 ℃ by a heater to obtain AA/BDO homogeneous-phase slurry, entering a material channel of a reactor by a micro-interface generator, and carrying out esterification reaction at the esterification temperature of 190-class 260 ℃ to generate BSA (bovine serum albumin) and esterification water;
3) and discharging BSA (bovine serum albumin) and esterification water to a vacuum flash tank, wherein the vacuum degree is 0.2bar (A), the esterification water is condensed into liquid state from a top steam outlet through a condenser in a steam state, the liquid state enters a vacuum separator for gas-liquid separation, and the BSA is discharged from a bottom liquid outlet of the vacuum flash tank in a liquid state.
8. The process of claim 7, wherein the molar ratio of BDO to AA in step 1) is 1.1: 1.
9. the method according to claim 7, wherein the temperature of the AA/BDO solid-liquid slurry in the step 1) is 40-60 ℃, the temperature of the AA/BDO solid-liquid slurry in the step 2) is raised to 180 ℃, the esterification temperature is 200 ℃, and the esterification time is 1 h.
10. The method of claim 7, wherein the homogeneous slurry and the catalyst in step 2) enter a material channel of the reactor through the micro-interface generator, the addition amount of the catalyst is 0.1-0.5kg/t PBAT, and the catalyst is tetrabutyl titanate.
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| CN203096014U (en) * | 2013-01-06 | 2013-07-31 | 杭州林达化工技术工程有限公司 | Device for producing natural gas from factory waste gas |
| CN109529753A (en) * | 2019-01-14 | 2019-03-29 | 扬州惠通化工科技股份有限公司 | A kind of PBT esterification system |
| CN111389314A (en) * | 2020-03-31 | 2020-07-10 | 南京延长反应技术研究院有限公司 | Built-in micro-interface unit enhanced reaction system and process for producing PTA (purified terephthalic acid) by PX (para-xylene) |
| CN111440301A (en) * | 2020-05-06 | 2020-07-24 | 扬州惠通化工科技股份有限公司 | Multifunctional polyester continuous production system |
| CN212284008U (en) * | 2020-05-06 | 2021-01-05 | 扬州惠通科技股份有限公司 | PBT production is with system of esterifying |
| CN111875724A (en) * | 2020-06-17 | 2020-11-03 | 南京延长反应技术研究院有限公司 | Micro-interface enhanced reaction system and method for preparing polyethylene by solution method |
| CN111635317A (en) * | 2020-06-29 | 2020-09-08 | 福建春达化工有限公司 | Energy-saving technology for esterification reaction of dioctyl terephthalate (DOTP) |
| CN112724388A (en) * | 2020-12-28 | 2021-04-30 | 扬州普立特科技发展有限公司 | Production device for recycling polyester to be regenerated into degradable material PBAT |
| CN113522198A (en) * | 2021-08-16 | 2021-10-22 | 华峰集团上海工程有限公司 | Esterification device and method for PTA and BDO in PBAT production process |
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