CN114797716A - Reaction device, and glycolide production system and production method - Google Patents
Reaction device, and glycolide production system and production method Download PDFInfo
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- CN114797716A CN114797716A CN202110109397.8A CN202110109397A CN114797716A CN 114797716 A CN114797716 A CN 114797716A CN 202110109397 A CN202110109397 A CN 202110109397A CN 114797716 A CN114797716 A CN 114797716A
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 191
- RKDVKSZUMVYZHH-UHFFFAOYSA-N 1,4-dioxane-2,5-dione Chemical compound O=C1COC(=O)CO1 RKDVKSZUMVYZHH-UHFFFAOYSA-N 0.000 title claims abstract description 121
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 40
- 239000007788 liquid Substances 0.000 claims abstract description 71
- 238000003756 stirring Methods 0.000 claims abstract description 49
- 239000000463 material Substances 0.000 claims abstract description 42
- 238000000034 method Methods 0.000 claims abstract description 38
- 229920000954 Polyglycolide Polymers 0.000 claims abstract description 37
- 239000004633 polyglycolic acid Substances 0.000 claims abstract description 36
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 24
- 238000005336 cracking Methods 0.000 claims abstract description 11
- 239000002893 slag Substances 0.000 claims abstract description 10
- 229920000642 polymer Polymers 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims description 27
- 238000010438 heat treatment Methods 0.000 claims description 26
- 239000002994 raw material Substances 0.000 claims description 17
- 238000004064 recycling Methods 0.000 claims description 8
- 238000005507 spraying Methods 0.000 claims description 8
- 125000004122 cyclic group Chemical group 0.000 claims description 7
- 238000004891 communication Methods 0.000 claims description 4
- 229920001577 copolymer Polymers 0.000 claims description 2
- 238000004939 coking Methods 0.000 abstract description 12
- 238000007086 side reaction Methods 0.000 abstract description 3
- 239000000047 product Substances 0.000 description 64
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Polymers OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 description 29
- 239000012071 phase Substances 0.000 description 28
- 239000003054 catalyst Substances 0.000 description 18
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- 239000007789 gas Substances 0.000 description 14
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- 238000002156 mixing Methods 0.000 description 10
- 238000003860 storage Methods 0.000 description 7
- 238000010268 HPLC based assay Methods 0.000 description 6
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- 238000004140 cleaning Methods 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
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- 239000001569 carbon dioxide Substances 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
- B01J4/002—Nozzle-type elements
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D319/00—Heterocyclic compounds containing six-membered rings having two oxygen atoms as the only ring hetero atoms
- C07D319/10—1,4-Dioxanes; Hydrogenated 1,4-dioxanes
- C07D319/12—1,4-Dioxanes; Hydrogenated 1,4-dioxanes not condensed with other rings
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Polyesters Or Polycarbonates (AREA)
Abstract
The invention provides a reaction device, a glycolide production system and a glycolide production method. The reaction device comprises a reaction kettle body, wherein the reaction kettle body comprises a reaction chamber; a vertically extending stirring shaft is arranged in the reaction chamber, and the stirring shaft comprises a hollow cavity; more than one liquid conveying branch pipe is arranged on the stirring shaft, and the liquid conveying branch pipes are communicated with the hollow cavity; the free end of the liquid conveying branch pipe is provided with a nozzle; and the reaction kettle body is provided with an exhaust pipe and a slag discharge port. The production method adopts the reaction device, and molten polyglycolic acid is introduced into the reaction device and is sprayed out from the nozzle to carry out cracking reaction, thus obtaining crude glycolide steam. The method has simple and efficient process, and the reaction materials are highly dispersed on the surface of the high-temperature reaction kettle body, so that the residence time of the reaction materials in a high-temperature area is extremely short, the side reactions such as further polymerization, coking and the like caused by the overlong residence time of the low polymers in the depolymerization kettle are effectively avoided, the product yield is improved, and the coking rate is reduced.
Description
Technical Field
The invention belongs to the technical field of chemical products, relates to the process production of glycolide, and particularly relates to a reaction device, a glycolide production system and a glycolide production method.
Background
Polyglycolic acid (PGA), also called polyglycolic acid or polyglycolide, is a polymer of glycolic acid, is gradually degraded into water and carbon dioxide in nature, exhibits good biodegradability, and is one of the most actively studied materials at present. However, the method of dehydrating and polycondensing glycolic acid as a starting material can only obtain polyglycolic acid having a low degree of polymerization. Low-polymerization-degree polyglycolic acid is insufficient in strength, melt processability, gas barrier property, and the like, and is too rapidly decomposed in the natural environment and in the living body, and when it is applied to many uses, it cannot satisfy the requirement of durability.
Glycolide is a cyclic dimer of glycolic acid, ring-opening polymerization of glycolide is a mature method for preparing polyglycolic acid, a polyglycolic acid product with high relative molecular mass can be obtained by the method, and the purity of glycolide is directly related to the performance of polyglycolic acid.
At present, glycolide is mainly prepared by high-temperature depolymerization of polyglycolic acid, the process takes low-molecular-weight polyglycolic acid as a raw material, crude glycolide is obtained after depolymerization and cooling collection at high temperature, and the crude glycolide is purified by subsequent rectification. Glycolide is highly heat-sensitive and is highly susceptible to self-polymerization, coking, and hydrolysis in the molten state. The depolymerization reaction is usually carried out in a tank reactor, and a large amount of coking and pipeline blockage are caused by long-time high-temperature boiling of raw materials, so that the yield and the product purity are greatly influenced. In addition, the crude glycolide can generate self-polymerization in a tower bottom and a reboiler through rectification and refining, so that a large amount of raw materials are lost, and related pipelines are easily blocked. In order to alleviate the problem of self-polymerization of crude glycolide and to improve the product yield, a solvent azeotropic method is currently reported as a more extensive depolymerization method.
The Chinese invention patent application (application publication No. CN107868076A, application publication No. 2018-4-3) discloses that glycolic acid crystals and a catalyst are mixed to carry out polycondensation reaction to obtain glycolic acid oligomers, polyether solvents are added into the system, high-temperature depolymerization is carried out, and the solvents and glycolide are co-distilled.
Chinese invention patent application (application publication No. CN104903306A, application publication date: 2015-9-9) discloses a method for producing glycolide, which comprises heating Glycolic Acid Oligomer (GAO) to depolymerize it, comprising: a step 1 of heating a mixture containing a polar organic solvent and GAO having a terminal carboxyl group concentration of 400eq/t or less to a depolymerization temperature of the GAO under normal pressure or reduced pressure; a step 2 of continuing heating at the temperature to depolymerize the GAO and distilling the produced GL and the solvent out of the depolymerization reaction system; and a step 3 of obtaining GL from the co-distillate; the GAO is preferably prepared by a method for producing GAO comprising a step of condensing glycolic acid and a step of dehydrating GA by continuing heating GA together with a polar organic solvent or a depolymerization reaction liquid to continue the condensation reaction of GA.
Chinese invention patent application (application publication No. CN102712617A, application publication date: 2012-10-3) discloses a method for producing glycolide, comprising the step of heating a mixture containing a glycolic acid oligomer, a high-boiling polar organic solvent having a boiling point of 230-450 ℃, and a tin compound to a temperature at which the glycolic acid oligomer is depolymerized under normal pressure or reduced pressure, thereby dissolving the glycolic acid oligomer in the high-boiling polar organic solvent; heating the solution in which the glycolic acid oligomer is dissolved to a temperature at which the glycolic acid oligomer is depolymerized under normal pressure or reduced pressure, thereby depolymerizing the glycolic acid oligomer in the solution to produce glycolide, and co-distilling the high-boiling polar organic solvent and the produced glycolide out of the depolymerization reaction system.
These patents all report that a high boiling polar solvent and a solubilizer are added and heated to form a liquid phase of glycolic acid oligomer, and many depolymerization solvents are liable to cause thermal deterioration during the reaction, and are liable to react with glycolide to lower the product yield. In addition, in order to separate the distilled glycolide from the solvent, solvent washing and solvent recovery steps are required, which causes mutual contamination of the solvents and increase in energy consumption, and therefore, the glycolide tends to be eliminated in industrial production.
In addition, the glycolide is purified by adopting a recrystallization method. The Chinese invention patent application (application publication number: CN107868075A) discloses a method for refining glycolide, which comprises the following steps: 1) adding a recrystallization solvent to the crude glycolide at room temperature; 2) heating and dissolving the mixture of crude glycolide and recrystallization solvent under the protection of inert gas, cooling the filtrate to below 25 ℃ after heat filtration to crystallize and separate out glycolide, filtering to remove liquid phase, and drying the obtained solid to obtain recrystallized glycolide; 3) mixing the recrystallized glycolide obtained in the previous step with a dried poor solvent, stirring at room temperature, and filtering; 4) repeating the step 3) for at least two times, and carrying out vacuum drying on the obtained solid to obtain the refined glycolide. The recrystallization method results in a large amount of solvent consumption and solvent residue, and environmental protection and discharge problems cause that the method cannot be widely applied in large-scale industrial processes.
Disclosure of Invention
In view of the technical problems in the prior art, the present invention aims to provide a reaction apparatus, a glycolide production system, and a glycolide production method, wherein reaction materials are highly dispersed on the surface of a high temperature reaction kettle, so that the residence time of the reaction materials in a high temperature region is extremely short, side reactions such as further polymerization and coking caused by too long residence time of oligomers in a depolymerization kettle are effectively avoided, the product yield is improved, and the coking rate is reduced.
The invention is realized by the following technical scheme:
the invention provides a reaction device in a first aspect, which comprises a reaction kettle body, wherein the reaction kettle body comprises a reaction chamber; a vertically extending stirring shaft is arranged in the reaction chamber, and the stirring shaft comprises a hollow cavity; more than one liquid conveying branch pipe is arranged on the stirring shaft, and the liquid conveying branch pipes are communicated with the hollow cavity; the free end of the liquid conveying branch pipe is provided with a nozzle; and the reaction kettle body is provided with an exhaust pipe and a slag discharge port.
Preferably, at least one of the following technical features is also included:
1) the reaction device also comprises a driving unit, and one end of the stirring shaft extends out of the reaction kettle body and is connected with the driving unit;
2) the reaction device also comprises a heating layer, and the heating layer is arranged outside the reaction kettle body;
3) the reaction device also comprises a scraper component, the scraper component comprises a scraper support and an inner wall scraper, the scraper support is arranged on the stirring shaft, and the inner wall scraper is arranged on the scraper support and is close to the inner wall of the reaction kettle body; the scraper component improves the dirt cleaning capability of the reaction device;
4) the included angle between the liquid conveying branch pipe and the stirring shaft is 10-90 degrees;
5) when the reaction device comprises a plurality of liquid conveying branch pipes, the plurality of liquid conveying branch pipes are arranged on the stirring shaft in a staggered manner;
6) the reaction device also comprises a raw material conveying pipeline, and the raw material conveying pipeline is communicated with the hollow cavity of the stirring shaft;
7) the nozzle is an atomizing nozzle;
8) the exhaust pipe is arranged at the top of the reaction kettle body;
9) the slag discharge port is arranged at the bottom of the reaction kettle body.
More preferably, at least one of the following technical characteristics is also included:
31) in the characteristic 3), the inner wall scraper is arranged along the side wall and/or the bottom wall of the reaction kettle body;
41) in the characteristic 4), the included angle between the liquid conveying branch pipe and the stirring shaft is 70-90 degrees;
51) the liquid conveying branch pipes are arranged into a plurality of liquid conveying groups along different heights of the stirring shaft, and the liquid conveying branch pipes in the adjacent liquid conveying groups are arranged in a staggered mode.
The second aspect of the invention provides a glycolide production system, which comprises the reaction device and the first condenser which are communicated in sequence.
Preferably, the reaction device further comprises a second condenser, and the reaction device, the first condenser and the second condenser are communicated in sequence.
More preferably, the first condenser and the second condenser are both tube condensers.
In a third aspect of the present invention, there is provided a method for producing glycolide, using the above reaction apparatus, wherein a molten reaction material containing polyglycolic acid is introduced into the reaction apparatus, and is ejected from the nozzle to cause a cracking reaction, thereby obtaining a crude glycolide vapor.
Liquid materials are not accumulated in the reaction device, and the reaction materials pass through in a single pass and are not returned through extracorporeal circulation.
Preferably, at least one of the following technical features is also included:
1) the method for producing glycolide further comprises the following steps: condensing the crude glycolide vapor to respectively obtain a light component and a mixture containing the heavy component and glycolide;
2) the method for producing glycolide further comprises the following steps: condensing the crude glycolide vapor to respectively obtain a mixture containing a light component and glycolide and a heavy component; condensing the mixture containing the light component and the glycolide to respectively obtain a light component and a glycolide product;
3) residue obtained by the cracking reaction is scraped by the scraper and is discharged from a residue discharge port;
4) the spraying amount is controlled to form a liquid film on the surface of the reaction kettle body after the molten reaction material is sprayed out;
5) the polyglycolic acid is a copolymer of
The molecular weight of the polymer with the characteristic structure is 1000-30000, such as 1000-3000, 3000-5000, 5000-8000, 8000-10000 or 10000-30000;
6) the reaction temperature is 190-350 ℃, such as 190-220 ℃, 220-240 ℃, 240-260 ℃, 260-280 ℃, 280-290 ℃, 290-300 ℃ or 300-350 ℃;
7) the absolute pressure of the reaction is 10Pa to 20000Pa, such as 10Pa to 100Pa, 100Pa to 500Pa, 500Pa to 1000Pa, 1000Pa to 2000Pa or 2000Pa to 20000 Pa.
More preferably, at least one of the following technical characteristics is also included:
11) in the characteristic 1), the light component is refluxed to a preorder polymerization section for cyclic utilization;
12) in feature 1), the temperature of the mixture comprising the heavy component and glycolide is from 80 ℃ to 180 ℃, e.g., from 80 ℃ to 120 ℃, from 120 ℃ to 130 ℃, or from 130 ℃ to 180 ℃;
21) in the characteristic 2), the light component and/or the heavy component are/is refluxed to a preorder polymerization section for recycling;
22) in the characteristic 2), the temperature of the heavy component is 110-180 ℃, such as 110-140 ℃, 140-150 ℃ or 150-180 ℃;
23) in the characteristic 2), the temperature of the glycolide product is 80-140 ℃, such as 80-90 ℃ or 90-140 ℃;
31) in the feature 3), the residue is intermittently or continuously removed;
41) in feature 4), the spraying amount is 1kg/m 2 .h～100kg/m 2 .h；
51) The molecular weight is 3000-10000 in the characteristic 5);
61) in the characteristic 6), the reaction temperature is 210-280 ℃;
71) the absolute pressure of the reaction in the feature 7) is 300Pa to 2000 Pa.
Even more preferably, in the feature 41), the shower amount is 10kg/m 2 .h～50kg/m 2 .h。
The invention has the beneficial effects that:
1) the method has simple and efficient process, and the reaction materials are highly dispersed on the surface of the high-temperature reaction kettle body, so that the residence time of the reaction materials in a high-temperature area is extremely short, the side reactions such as further polymerization, coking and the like caused by the overlong residence time of the low polymers in the depolymerization kettle are effectively avoided, the product yield is improved, and the coking rate is reduced.
2) The invention increases the heat transfer and mass transfer capacity of the reaction materials by using a spraying mode, leads the depolymerization reaction to be completed in a short time, improves the energy utilization rate, reduces the retention time of the raw materials in a high-temperature stage, is beneficial to reducing the degree of coking and self-polymerization, shortens the reaction time and improves the production efficiency.
3) The depolymerization-condensation integrated process reduces coking and self-polymerization in the subsequent purification and heating process of the crude glycolide, and improves the utilization rate of raw materials and the utilization rate of energy sources.
4) The condensation of the invention can run under the working condition without filler, and the pressure drop of the separation step is reduced to the maximum extent, so that the reaction device can be operated under lower pressure, thereby reducing the reaction temperature, improving the utilization rate of raw materials and reducing the coking rate.
5) The method has the advantages of no solvent pollution, high product purity, convenient continuous separation process and suitability for large-scale production.
Drawings
FIG. 1 is a schematic sectional view of a reaction apparatus according to the present invention.
FIG. 2 is a schematic top view of the reactor of the present invention.
FIG. 3 is a schematic sectional view of a reaction vessel in the reaction apparatus of the present invention.
FIG. 4 is a schematic view of the angle α between the liquid delivery branch and the stirring shaft in the reaction apparatus of the present invention.
Fig. 5 is a first diagram of a glycolide production system according to the present invention.
Fig. 6 is a second diagram of a glycolide production system according to the present invention.
Reference numerals
1 reaction apparatus
11 reaction kettle body
111 reaction chamber
112 exhaust pipe
113 slag discharge hole
12 stirring shaft
121 hollow cavity
13 liquid conveying branch pipe
14 nozzle
15 drive unit
16 heating layer
17 flight assembly
171 scraper support
172 inner wall scraper
18 raw material conveying pipeline
2 first condenser
3 second condenser
Detailed Description
The technical solution of the present invention is illustrated by specific examples below. It is to be understood that one or more method steps mentioned in the present invention do not exclude the presence of other method steps before or after the combination step or that other method steps may be inserted between the explicitly mentioned steps; it should also be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Moreover, unless otherwise indicated, the numbering of the various method steps is merely a convenient tool for identifying the various method steps, and is not intended to limit the order in which the method steps are arranged or the scope of the invention in which the invention may be practiced, and changes or modifications in the relative relationship may be made without substantially changing the technical content.
A reaction apparatus, as shown in fig. 1 to 3, comprising a reaction vessel body 11, wherein the reaction vessel body 11 comprises a reaction chamber 111; a vertically extending stirring shaft 12 is arranged in the reaction chamber 111, and the stirring shaft 12 comprises a hollow cavity 121; more than one liquid conveying branch pipe 13 is arranged on the stirring shaft 12, and the liquid conveying branch pipes 13 are communicated with the hollow cavity 121; the free end of the liquid conveying branch pipe 13 is provided with a nozzle 14; the reaction kettle body 11 is provided with an exhaust pipe 112 and a slag discharge port 113.
The invention utilizes the liquid conveying branch pipes and the nozzles to spray the reaction materials in a spraying mode, increases the heat transfer and mass transfer capacities of the reaction materials, completes the depolymerization reaction in a short time, improves the energy utilization rate, reduces the retention time of the reaction materials in a high-temperature stage, is beneficial to reducing the degree of coking and self-polymerization, shortens the reaction time and improves the production efficiency.
In a preferred embodiment, the reaction apparatus further comprises a driving unit 15, and one end of the stirring shaft 12 extends out of the reaction vessel body 11 and is connected with the driving unit 15. The driving unit 15 may be a motor.
In a preferred embodiment, the reaction apparatus further comprises a heating layer 16, and the heating layer 16 is disposed outside the reaction kettle body 11.
In a preferred embodiment, the reaction device further comprises a scraper assembly 17, the scraper assembly 17 comprises a scraper support 171 and an inner wall scraper 172, the scraper support 171 is disposed on the stirring shaft 12, and the inner wall scraper 172 is disposed on the scraper support 171 and is close to the inner wall of the reaction kettle body 11. The scraper component 17 improves the dirt cleaning capability of the reaction device and meets the requirement of industrial steady-state operation.
In a preferred embodiment, the inner wall scrapers 172 are disposed along the side wall and/or the bottom wall of the reaction vessel body 11.
In a preferred embodiment, the included angle between the liquid conveying branch pipe 13 and the stirring shaft 12 is 10 ° to 90 °, as shown in fig. 4, where α is the included angle, the included angle between the center line of the stirring shaft and the center line of the liquid conveying branch pipe, and the range indicated by the double arrow is the included angle range.
In a preferred embodiment, the included angle between the liquid conveying branch pipe 13 and the stirring shaft 12 is 70-90 degrees.
In a preferred embodiment, when the reaction device comprises a plurality of liquid conveying branch pipes 13, the plurality of liquid conveying branch pipes 13 are arranged on the stirring shaft 12 in a staggered manner.
In a preferred embodiment, the plurality of liquid conveying branch pipes 13 are arranged into a plurality of liquid conveying groups at different heights along the stirring shaft 12, and the liquid conveying branch pipes in the adjacent liquid conveying groups are arranged in a staggered manner.
In a preferred embodiment, the reaction device further comprises a raw material conveying pipe 18, and the raw material conveying pipe 18 is communicated with the hollow cavity 121 of the stirring shaft 12. The raw material sequentially passes through the raw material delivery pipe 18, the hollow chamber 121, the liquid delivery manifold 13, and the nozzle 14 to enter the reaction chamber 111.
In a preferred embodiment, the nozzle 14 is an atomizing nozzle. The reaction materials are sprayed out in a spraying mode, and the heat transfer and mass transfer capacities of the reaction materials are improved.
In a preferred embodiment, the exhaust pipe 112 is disposed at the top of the reaction vessel body 11.
In a preferred embodiment, the slag discharge port 113 is disposed at the bottom of the reaction vessel body 11.
A glycolide production system, as shown in FIG. 5, comprises the above reaction apparatus 1 and the first condenser 2, which are connected in series. By means of which a light fraction and a mixture comprising a heavy fraction and glycolide are obtained, respectively.
In a preferred embodiment, as shown in fig. 6, the production system further comprises a second condenser 3, and the reaction device 1, the first condenser 2 and the second condenser 3 are communicated in sequence. Respectively obtaining a mixture containing light components and glycolide and heavy components from the first condenser through the production system; and respectively obtaining a light component and a glycolide product from the second condenser.
In a preferred embodiment, the first condenser 2 and the second condenser 3 are both tube condensers.
The reaction apparatus (diameter 1m, height 1.8m) used in the following examples 1 to 8 comprises a reaction vessel body 11, wherein the reaction vessel body 11 comprises a reaction chamber 111 therein; a vertically extending stirring shaft 12 is arranged in the reaction chamber 111, and the stirring shaft 12 comprises a hollow cavity 121; 9 liquid conveying branch pipes 13 are arranged on the stirring shaft 12, and the liquid conveying branch pipes 13 are communicated with the hollow cavity 121; the free end of the liquid conveying branch pipe 13 is provided with a nozzle 14; the reaction kettle body 11 is provided with an exhaust pipe 112 and a slag discharge port 113. The reaction device further comprises a driving unit 15, and one end of the stirring shaft 12 extends out of the reaction kettle body 11 and then is connected with the driving unit 15. The reaction device further comprises a heating layer 16, wherein the heating layer 16 is arranged outside the reaction kettle body 11. The reaction device further comprises a scraper component 17, the scraper component 17 comprises a scraper support 171 and an inner wall scraper 172, the scraper support 171 is arranged on the stirring shaft 12, and the inner wall scraper 172 is arranged on the scraper support 171 and is close to the inner wall of the reaction kettle body 11. The inner wall scraper 172 is arranged along the side wall and the bottom wall of the reaction kettle body 11, and the liquid conveying branch pipe 13 is perpendicular to the stirring shaft 12. The 9 liquid conveying branch pipes 13 are arranged on the stirring shaft 12 in a staggered manner: the 9 liquid conveying branch pipes are divided into 3 groups of liquid conveying groups, 3 liquid conveying branch pipes in each group are arranged on the stirring shaft 12 in a Y shape, the liquid conveying branch pipes are arranged at an included angle of 120 degrees and in the same plane, and the plane is vertical to the stirring shaft; the 9 liquid conveying branch pipes 13 form 3 planes which are parallel to each other, the intervals between the planes are 50cm, and the Y-shaped branch pipes between the adjacent planes are staggered by 60 degrees. The reaction device further comprises a raw material conveying pipeline 18, and the raw material conveying pipeline 18 is communicated with the hollow cavity 121 of the stirring shaft 12. The nozzle 14 is an atomizing nozzle. The exhaust pipe 112 is arranged at the top of the reaction kettle body 11. The slag discharge port 113 is arranged at the bottom of the reaction kettle body 11.
The reaction apparatus (4L) used in comparative examples 1 to 2 below included a reaction vessel body (diameter 15cm, height 30cm) in which an anchor stirrer was disposed and a heat-conducting oil jacket was disposed outside the vessel body.
The following examples 1 to 5 use a glycolide production system shown in fig. 5, comprising the above-mentioned reaction apparatus 1 and a first condenser 2 in communication with each other, the first condenser 2 being a tubular condenser. The light fraction and the mixture comprising the heavy fraction and glycolide are obtained separately by the production system.
The following examples 6 to 8 use a glycolide production system shown in fig. 6, which comprises the above-described reaction apparatus 1, first condenser 2, and second condenser 3 in communication in this order, and the first condenser 2 and the second condenser 3 are each a tube condenser. Respectively obtaining a mixture containing light components and glycolide and heavy components from the first condenser through the production system; and respectively obtaining a light component and a glycolide product from the second condenser.
The following production system for glycolide used in comparative examples 1 to 2 comprised the above-mentioned reaction apparatus (4L) and a first condenser, which were communicated in this order.
Example 1
Polyglycolic acid (molecular weight Mw: 5000) and Sb 2 O 3 The catalyst (the addition amount is 0.2 wt% of polyglycolic acid) is uniformly mixed and heated to 220 ℃ for melting, the melted material is sprayed to a reaction kettle at the speed of 80kg/h through a hollow cavity, a liquid conveying branch pipe and a nozzle in sequence, and the cracking reaction is generatedThe temperature of the reaction kettle is controlled at 220 ℃, the reaction pressure is controlled at 2000Pa, crude glycolide vapor generated in the process enters a first condenser, the temperature of materials at the outlet of the first condenser is controlled at 120 ℃, a condensed liquid product, namely a crude glycolide product (containing a mixture of heavy components and glycolide), is obtained and can be collected in a storage tank, and a gas phase outlet material of the first condenser, namely a first condensed gas phase product (light components), is transferred to a preorder polymerization section for cyclic utilization. The crude glycolide product obtained showed 93.8% purity by HPLC assay and 83.8% yield. The slagging rate of the reaction device is 0.8 percent.
Example 2
Polyglycolic acid (molecular weight Mw 3000) and Sb 2 O 3 Uniformly mixing a catalyst (the adding amount is 0.2 wt% of the polyglycolic acid), heating to 210 ℃ to melt the catalyst, ejecting the molten material to a reaction kettle at a speed of 400kg/h through a hollow cavity, a liquid conveying branch pipe and a nozzle in sequence, controlling the temperature of the reaction kettle at 350 ℃ and the reaction pressure at 20000Pa, introducing crude glycolide vapor generated in the process into a first condenser, controlling the temperature of the material at the outlet of the first condenser at 180 ℃ to obtain a condensed liquid substance, namely a crude glycolide product (a mixture containing heavy components and glycolide), collecting the condensed liquid substance, namely a first condensed gas-phase product (light components), in a storage tank, and transferring the gas-phase outlet substance of the first condenser, namely a first condensed gas-phase product (light components) to a preorder polymerization section for recycling. The crude glycolide product obtained showed a purity of 94.3% and a yield of 76.3% by HPLC test analysis. The slagging rate of the reaction device is 0.4 percent.
Example 3
Polyglycolic acid (molecular weight Mw 30000) and Sb 2 O 3 Uniformly mixing a catalyst (the addition amount is 0.4wt percent of polyglycolic acid), heating to 230 ℃ to melt the catalyst, sequentially ejecting the melted material to a reaction kettle through a hollow cavity, a liquid conveying branch pipe and a nozzle at the speed of 120kg/h, carrying out cracking reaction, controlling the temperature of the reaction kettle at 240 ℃ and the reaction pressure at 100Pa, generating crude glycolide vapor in the process, entering a first condenser, controlling the temperature of the material at the outlet of the first condenser at 80 ℃, and obtaining a condensed liquid substance, namely a crude glycolide product (containing heavy components and polyglycolic acid products) (containing heavy components and 80℃)Mixture of glycolide) can be collected in a storage tank, and the gas phase outlet material of the first condenser, namely the first condensed gas phase product (light component), is transferred to the previous polymerization section for recycling. The crude glycolide product obtained showed a purity of 96.83% by HPLC assay, with a yield of 94.8%. The slagging rate of the reaction device is 1.8 percent.
Example 4
Polyglycolic acid (molecular weight Mw: 10000) and SnCl 2 Uniformly mixing a catalyst (the addition amount is 0.2 wt% of polyglycolic acid), heating to 210 ℃ to melt the catalyst, ejecting the molten material to a reaction kettle at a speed of 200kg/h through a hollow cavity, a liquid conveying branch pipe and a nozzle in sequence, controlling the temperature of the reaction kettle at 280 ℃ and the reaction pressure at 1000Pa under the absolute pressure, allowing crude glycolide vapor generated in the process to enter a first condenser, controlling the temperature of the material at the outlet of the first condenser at 130 ℃ to obtain a condensed liquid substance, namely a crude glycolide product (a mixture containing heavy components and glycolide), collecting the condensed liquid substance, namely a first condensed gas-phase product (light components) in a storage tank, and transferring the gas-phase outlet substance of the first condenser, namely a first condensed gas-phase product (light components) to a preorder polymerization section for recycling. The crude glycolide product obtained showed a purity of 98.83% by HPLC assay, with a yield of 95.2%. The slagging rate of the reaction device is 0.9 percent.
Example 5
Polyglycolic acid (molecular weight Mw: 10000) and SnCl 2 Uniformly mixing a catalyst (the adding amount is 0.2 wt% of the polyglycolic acid), heating to 210 ℃ to melt the catalyst, continuously pumping the molten material into a reaction kettle at the speed of 250kg/h, carrying out cracking reaction, controlling the temperature of the reaction kettle at 300 ℃, controlling the reaction pressure at 1000Pa, generating crude glycolide vapor in the process, entering a first condenser, controlling the temperature of the material at the outlet of the first condenser at 120 ℃, obtaining a condensed liquid substance, namely a crude glycolide product (a mixture containing heavy components and glycolide), collecting the condensed liquid substance in a storage tank, and transferring the gas phase outlet substance of the first condenser, namely a first condensed gas phase product (light components) to a preceding polymerization section for recycling. The crude glycolide product obtained showed a purity of 98.23% by HPLC assay, with a yield of 96.2%. The slagging rate of the reaction device is 0.3 percent.
Example 6
Polyglycolic acid (molecular weight Mw 8000) and SnCl 2 Uniformly mixing a catalyst (the addition amount is 0.2 wt% of polyglycolic acid), heating to 210 ℃ to melt the catalyst, sequentially ejecting the melted material to a reaction kettle through a hollow cavity, a liquid conveying branch pipe and a nozzle at the speed of 120kg/h, carrying out cracking reaction, controlling the temperature of the reaction kettle at 260 ℃ and the reaction pressure at 500Pa, introducing crude glycolide vapor generated in the process into a first condenser, controlling the temperature of the material at the outlet of the first condenser at 150 ℃, and respectively obtaining a first condensed liquid phase product, namely a heavy component and a first condensed gas phase product, namely a mixture containing a light component and glycolide; and then the first condensed gas-phase product is connected into a second condenser, the temperature of the material at the outlet of the second condenser is controlled to be 90 ℃, a second condensed liquid-phase product, namely a glycolide product, and a second condensed gas-phase product, namely a light component, are respectively obtained, and the second condensed gas-phase product is transferred to a preorder polymerization section for cyclic utilization. The second condensed liquid phase product obtained, i.e., the glycolide product, showed a purity of 99.43% by HPLC test analysis, and a yield of 89.2%. The slagging rate of the reaction device is 0.3 percent.
Example 7
Polyglycolic acid (molecular weight Mw: 10000) and Sb 2 O 3 Uniformly mixing a catalyst (the addition amount is 0.2 wt% of polyglycolic acid), heating to 210 ℃ to melt the catalyst, sequentially ejecting the melted material to a reaction kettle through a hollow cavity, a liquid conveying branch pipe and a nozzle at the speed of 120kg/h, and carrying out cracking reaction, wherein the temperature of the reaction kettle is controlled at 290 ℃, the reaction pressure is controlled at 100Pa, crude glycolide vapor generated in the process enters a first condenser, the temperature of the material at the outlet of the first condenser is controlled at 140 ℃, and a first condensed liquid phase product, namely a heavy component, and a first condensed gas phase product, namely a mixture containing a light component and glycolide, are respectively obtained; and then the first condensed gas-phase product is connected into a second condenser, the temperature of the material at the outlet of the second condenser is controlled to be 90 ℃, a second condensed liquid-phase product, namely a glycolide product, and a second condensed gas-phase product, namely a light component, are respectively obtained, and the second condensed gas-phase product is transferred to a preorder polymerization section for cyclic utilization. The second condensed liquid phase product, i.e. the glycolide product, is obtainedThe product was analyzed by HPLC test to show 99.5% purity and 92.2% yield. The slagging rate of the reaction device is 0.1 percent.
Example 8
Polyglycolic acid (molecular weight Mw 1000) and Sb 2 O 3 Uniformly mixing a catalyst (the addition amount is 0.2 wt% of polyglycolic acid), heating to 210 ℃ to melt the catalyst, sequentially ejecting the melted material to a reaction kettle through a hollow cavity, a liquid conveying branch pipe and a nozzle at a speed of 5kg/h, and carrying out cracking reaction, wherein the temperature of the reaction kettle is controlled at 190 ℃, the reaction pressure is controlled at 10Pa, crude glycolide vapor generated in the process enters a first condenser, the temperature of the material at the outlet of the first condenser is controlled at 140 ℃, and a first condensed liquid phase product, namely a heavy component, and a first condensed gas phase product, namely a mixture containing a light component and glycolide, are respectively obtained; and then the first condensed gas-phase product is connected into a second condenser, the temperature of the material at the outlet of the second condenser is controlled to be 90 ℃, a second condensed liquid-phase product, namely a glycolide product, and a second condensed gas-phase product, namely a light component, are respectively obtained, and the second condensed gas-phase product is transferred to a preorder polymerization section for cyclic utilization. The second condensed liquid phase product obtained, i.e. the glycolide product, showed a purity of 96.3% by HPLC test analysis, and a yield of 78.3%. The slagging rate of the reaction device is 0.1 percent.
Comparative example 1
Polyglycolic acid 2kg (molecular weight Mw: 10000) and Sb 2 O 3 Uniformly mixing a catalyst (the addition amount is 0.2wt percent of polyglycolic acid), transferring the mixture into a 4L reaction device, heating the material to 220 ℃ to melt the material, controlling the temperature of the reaction kettle to 240 ℃ under vigorous stirring, gradually vacuumizing and controlling the reaction pressure to be 2000Pa, generating crude glycolide vapor in the process, entering the crude glycolide vapor into a first condenser, controlling the temperature of the material at the outlet of the first condenser to be 140 ℃, obtaining a condensed liquid substance, namely a crude glycolide product (a mixture containing heavy components and glycolide), collecting the condensed liquid substance in a storage tank, and transferring the gas phase outlet substance of the first condenser, namely a first condensed gas phase product (light components) to a preorder polymerization section for recycling. The crude glycolide product obtained showed a purity of 59.5% by HPLC assay, and a yield of 67.2%. The slagging rate of the reaction device is 23.9 percent.
Comparative example 2
Polyglycolic acid 2kg (molecular weight Mw 20000) and Sb 2 O 3 Uniformly mixing a catalyst (the adding amount is 0.2 wt% of polyglycolic acid), transferring the mixture into a 4L reaction device, heating the material to 220 ℃ to melt the material, controlling the temperature of the reaction kettle to be 250 ℃ under vigorous stirring, gradually vacuumizing and controlling the reaction pressure to be 200Pa, generating crude glycolide vapor in the process, entering the crude glycolide vapor into a first condenser, controlling the temperature of the material at the outlet of the first condenser to be 140 ℃, obtaining a condensed liquid substance, namely a crude glycolide product (a mixture containing heavy components and glycolide), collecting the condensed liquid substance in a storage tank, and transferring the gas phase outlet substance of the first condenser, namely a first condensed gas phase product (light components) to a preorder polymerization section for recycling. The crude glycolide product obtained showed a purity of 62.5% by HPLC assay, and a yield of 56.2%. The slagging rate of the reaction device is 19.9 percent.
While the invention has been described with respect to a preferred embodiment, it will be understood by those skilled in the art that the foregoing and other changes, omissions and deviations in the form and detail thereof may be made without departing from the scope of this invention. Those skilled in the art can make various changes, modifications and equivalent arrangements, which are equivalent to the embodiments of the present invention, without departing from the spirit and scope of the present invention, and which may be made by utilizing the techniques disclosed above; meanwhile, any changes, modifications and variations of the above-described embodiments, which are equivalent to those of the technical spirit of the present invention, are within the scope of the technical solution of the present invention.
Claims (10)
1. A reaction device, which is characterized by comprising a reaction kettle body (11), wherein the reaction kettle body (11) comprises a reaction chamber (111); a vertically extending stirring shaft (12) is arranged in the reaction chamber (111), and the stirring shaft (12) comprises a hollow cavity (121); more than one liquid conveying branch pipe (13) is arranged on the stirring shaft (12), and the liquid conveying branch pipes (13) are communicated with the hollow cavity (121); the free end of the liquid conveying branch pipe (13) is provided with a nozzle (14); the reaction kettle body (11) is provided with an exhaust pipe (112) and a slag discharge port (113).
2. The reactor device according to claim 1, characterized in that it further comprises at least one of the following technical features:
1) the reaction device also comprises a driving unit (15), and one end of the stirring shaft (12) extends out of the reaction kettle body (11) and is connected with the driving unit (15);
2) the reaction device also comprises a heating layer (16), and the heating layer (16) is arranged outside the reaction kettle body (11);
3) the reaction device further comprises a scraper component (17), the scraper component (17) comprises a scraper support (171) and an inner wall scraper (172), the scraper support (171) is arranged on the stirring shaft (12), and the inner wall scraper (172) is arranged on the scraper support (171) and is close to the inner wall of the reaction kettle body (11);
4) the included angle between the liquid conveying branch pipe (13) and the stirring shaft (12) is 10-90 degrees;
5) when the reaction device comprises a plurality of liquid conveying branch pipes (13), the liquid conveying branch pipes (13) are arranged on the stirring shaft (12) in a staggered mode;
6) the reaction device also comprises a raw material conveying pipeline (18), and the raw material conveying pipeline (18) is communicated with the hollow cavity (121) of the stirring shaft (12);
7) the nozzle (14) is an atomizing nozzle;
8) the exhaust pipe (112) is arranged at the top of the reaction kettle body (11);
9) the slag discharge port (113) is arranged at the bottom of the reaction kettle body (11).
3. The reactor device according to claim 2, characterized in that it further comprises at least one of the following technical features:
31) in the characteristic 3), the inner wall scraper (172) is arranged along the side wall and/or the bottom wall of the reaction kettle body (11);
41) in the characteristic 4), the included angle between the liquid conveying branch pipe (13) and the stirring shaft (12) is 70-90 degrees;
51) in the characteristic 5), the liquid conveying branch pipes (13) are arranged into a plurality of liquid conveying groups along different heights of the stirring shaft (12), and the liquid conveying branch pipes in the adjacent liquid conveying groups are arranged in a staggered mode.
4. A glycolide production system characterized by comprising the reaction apparatus (1) according to any one of claims 1 to 3 and a first condenser (2) in communication with each other.
5. A glycolide production system according to claim 4, further comprising a second condenser (3), wherein the reaction device (1), the first condenser (2) and the second condenser (3) are in communication in this order.
6. A glycolide production system according to claim 5, characterized in that the first condenser (2) and the second condenser (3) are both tube condensers.
7. A process for the production of glycolide, characterized in that, using the reaction apparatus according to any one of claims 1 to 3, a molten reaction material containing polyglycolic acid is introduced into the reaction apparatus, ejected from the nozzle, and subjected to a cracking reaction to obtain a crude glycolide vapor.
8. The method for the production of glycolide according to claim 7, further comprising at least one of the following technical features:
1) the method for producing glycolide further comprises the following steps: condensing the crude glycolide vapor to respectively obtain a light component and a mixture containing the heavy component and glycolide;
2) the method for producing glycolide further comprises the following steps: condensing the crude glycolide vapor to respectively obtain a mixture containing a light component and glycolide and a heavy component; condensing the mixture containing the light component and the glycolide to respectively obtain a light component and a glycolide product;
3) residue obtained by the cracking reaction is scraped by the scraper and is discharged from a residue discharge port;
4) the spraying amount is controlled to form a liquid film on the surface of the reaction kettle body after the molten reaction material is sprayed out;
5) the polyglycolic acid is a copolymer of
The molecular weight of the polymer with the characteristic structure is 1000-30000;
6) the reaction temperature is 190-350 ℃;
7) the absolute pressure of the reaction is 10Pa to 20000 Pa.
9. The method for the production of glycolide according to claim 8, further comprising at least one of the following technical features:
11) in the characteristic 1), the light component is refluxed to a preorder polymerization section for cyclic utilization;
12) in the characteristic 1), the temperature of the mixture containing the heavy component and the glycolide is 80-180 ℃;
21) in the characteristic 2), the light component and/or the heavy component are/is refluxed to a preorder polymerization section for recycling;
22) in the characteristic 2), the temperature of the heavy component is 110-180 ℃;
23) in the characteristic 2), the temperature of the glycolide product is 80-140 ℃;
31) in the feature 3), the residue is intermittently or continuously removed;
41) in feature 4), the spraying amount is 1kg/m 2 .h～100kg/m 2 .h；
51) The molecular weight is 3000-10000 in the characteristic 5);
61) in the characteristic 6), the reaction temperature is 210-280 ℃;
71) the absolute pressure of the reaction in the feature 7) is 300Pa to 2000 Pa.
10. The process for producing glycolide according to claim 9, wherein the spraying amount is 10kg/m in feature 41) 2 .h～50kg/m 2 .h。
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