CN113578229A - Polymerization reaction system capable of preventing violent heat release - Google Patents
Polymerization reaction system capable of preventing violent heat release Download PDFInfo
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- CN113578229A CN113578229A CN202110727626.2A CN202110727626A CN113578229A CN 113578229 A CN113578229 A CN 113578229A CN 202110727626 A CN202110727626 A CN 202110727626A CN 113578229 A CN113578229 A CN 113578229A
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- reaction kettle
- main reaction
- auxiliary container
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- port
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- 238000006116 polymerization reaction Methods 0.000 title claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 79
- 238000005086 pumping Methods 0.000 claims abstract description 32
- 239000000463 material Substances 0.000 claims abstract description 31
- 230000003068 static effect Effects 0.000 claims description 7
- 239000002826 coolant Substances 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims 2
- 239000000178 monomer Substances 0.000 abstract description 17
- 239000002002 slurry Substances 0.000 abstract description 9
- 239000006185 dispersion Substances 0.000 abstract description 3
- 229920001721 polyimide Polymers 0.000 description 10
- GTDPSWPPOUPBNX-UHFFFAOYSA-N ac1mqpva Chemical compound CC12C(=O)OC(=O)C1(C)C1(C)C2(C)C(=O)OC1=O GTDPSWPPOUPBNX-UHFFFAOYSA-N 0.000 description 9
- 238000003756 stirring Methods 0.000 description 7
- 239000004642 Polyimide Substances 0.000 description 5
- 150000004985 diamines Chemical class 0.000 description 5
- 239000000498 cooling water Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 125000005462 imide group Chemical group 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 239000002798 polar solvent Substances 0.000 description 1
- 229920005575 poly(amic acid) Polymers 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010345 tape casting Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 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
- B01J19/1862—Stationary reactors having moving elements inside placed in series
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Polymerisation Methods In General (AREA)
Abstract
The invention provides a polymerization reaction system for preventing violent heat release, which comprises: main reation kettle and inside have vice container of vice rabbling mechanism, wherein: the main reaction kettle and the auxiliary container are both provided with feed ports, and a pumping pipeline for pumping part of materials in the main reaction kettle and conveying the materials into the auxiliary container and a return pipeline for guiding the materials in the auxiliary container into the main reaction kettle are arranged between the main reaction kettle and the auxiliary container. The invention solves the problems that the powdery reaction monomer is added in the later period and directly added into a large amount of slurry to cause difficult rapid dispersion and local violent heat release.
Description
Technical Field
The invention relates to the technical field of polyimide processing equipment, in particular to a polymerization reaction system capable of preventing violent heat release.
Background
Polyimide film is one of the most demanded polyimide products, and its excellent corona resistance, radiation resistance, dielectric properties and dimensional stability make the demand for high-performance polyimide film materials continuously increasing. Due to a large number of imide rings and benzene ring structures in the polyimide main chain, strong intermolecular force exists among molecular chains, so that the polyimide molecular chain structure is compact, the characteristics of difficult dissolution and difficult dissolution are shown, the barrier of mass production and processing of polyimide is formed, and the development of polyimide film products in more application fields is influenced. In order to avoid the problem of solubility, the production of the polyimide film mainly adopts a two-step method, wherein a polyamic acid solution is synthesized, and then the polyimide film is prepared by a tape-casting film forming process of a pre-drying process and a thermal imidization treatment. The amic acid is generally prepared by reacting dianhydride and diamine in an aprotic polar solvent at a low temperature, and the specific operation mode is that the diamine is added firstly, and then the dianhydride is added in batches for multiple times, because the diamine has high solubility and the dianhydride has low solubility, and if the dianhydride is added firstly, the dianhydride and the water in the solvent are hydrolyzed; meanwhile, due to the exothermic reaction between dianhydride and diamine, severe heat release can be caused if dianhydride is put into the kettle at one time, and the excessive input amount can be caused to cause waste. Then, the viscosity of the polymerization solution in the kettle is increased along with the continuation of the reaction, and the dianhydride is powdery, so that the later input is difficult to rapidly disperse, and further, the problem of local violent heat release is easily caused.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention provides a polymerization reaction system for preventing violent heat release.
The invention provides a polymerization reaction system for preventing violent heat release, which comprises: main reation kettle with main rabbling mechanism and inside have vice container of vice rabbling mechanism, wherein:
the main reaction kettle and the auxiliary container are both provided with feed ports, and a pumping pipeline for pumping part of materials in the main reaction kettle and conveying the materials into the auxiliary container and a return pipeline for guiding the materials in the auxiliary container into the main reaction kettle are arranged between the main reaction kettle and the auxiliary container.
Preferably, the feeding end of the pumping pipeline is positioned at the central part of the bottom of the main reaction kettle.
Preferably, the feed end of the return line is higher than the discharge end thereof.
Preferably, the outer periphery of the return line is covered with a cooling water jacket for passing a cooling medium.
Preferably, the main reaction kettle is also provided with a discharge hole, a pumping hole and a feed back hole, and the auxiliary container is also provided with a feed inlet and a discharge hole; the feeding end of the pumping pipeline is connected with the material pumping port of the main reaction kettle, and the discharging end of the pumping pipeline is connected with the feeding port of the auxiliary container; the feed end of the return line is connected with the feed inlet of the auxiliary container, and the discharge end of the return line is connected with the feed back port of the main reaction kettle.
Preferably, the material pumping port of the main reaction kettle is positioned at the central part of the bottom of the main reaction kettle.
Preferably, the discharge hole of the auxiliary container is higher than the feed back hole of the main reaction kettle.
Preferably, a static mixer is installed in the return line.
Preferably, the static mixer is covered with a cooling water jacket for passing a cooling medium.
In the invention, a main reaction kettle and an auxiliary container are arranged, and the main reaction kettle and the auxiliary reaction container are both provided with feed ports, so that an auxiliary stirring mechanism is arranged in the auxiliary container; meanwhile, a pumping pipeline and a return pipeline are arranged between the main reaction kettle and the auxiliary reaction container, the pumping pipeline can extract materials from the main reaction kettle and convey the materials into the auxiliary container, the return pipeline can guide the materials in the auxiliary container into the main reaction kettle, so that when the system performs polymerization reaction, the main reaction kettle is used for performing preliminary reaction, when the preliminary reaction reaches a certain degree, and when the viscosity of slurry in the kettle reaches the certain degree, part of the slurry is extracted from the main reaction kettle into the auxiliary container, meanwhile, reaction monomers to be added are fed into the auxiliary container from a feed opening of the auxiliary container, and the auxiliary stirring mechanism is used for stirring and mixing uniformly and then guiding the slurry mixed with the reaction monomers to the main reaction kettle again. The arrangement mode solves the problems that the powdery reaction monomer is added in the later period and directly thrown into a large amount of slurry to cause difficulty in rapid dispersion and local violent heat release.
Drawings
FIG. 1 is a schematic view showing a polymerization system for preventing severe heat release according to the present invention.
Detailed Description
Referring to fig. 1, the present invention provides a polymerization reaction system for preventing severe heat release, comprising: main reation kettle 1 and inside have vice container 2 of vice rabbling mechanism, wherein: the main reaction kettle 1 and the auxiliary container 2 are both provided with a feeding port, and a pumping pipeline 3 for pumping part of materials in the main reaction kettle 1 and conveying the materials into the auxiliary container 2 and a return pipeline 4 for guiding the materials in the auxiliary container 2 into the main reaction kettle 1 are arranged between the main reaction kettle 1 and the auxiliary container 2. Specifically, the method comprises the following steps: the main reaction kettle 1 is also provided with a discharge hole, a pumping hole and a feed back hole, and the auxiliary container 2 is also provided with a feed hole and a discharge hole; the feeding end of the pumping pipeline 3 is connected with the material pumping port of the main reaction kettle 1, and the discharging end of the pumping pipeline is connected with the feeding port of the auxiliary container 2; the feed end of the return pipeline 4 is connected with the feed inlet of the auxiliary container 2, and the discharge end of the return pipeline is connected with the feed back port of the main reaction kettle 1. The polymerization reaction system has the following specific working mode:
injecting a solvent (such as dimethylacetamide (DMAc) or N-methylpyrrolidone (NMP)) and a first monomer (such as diamine) into a main reaction kettle 1 in advance, and uniformly stirring the first monomer and the solvent; then, putting a part of second monomer (such as dianhydride) into the main reaction kettle 1 so as to ensure that the second monomer is stirred by the stirrer in the kettle to fully react with the first monomer; in the reaction process, along with the rising of temperature and the increase of inside thick liquids viscosity in the cauldron, extract partial material by pumping pipeline 3 in from main reation kettle 1 again and get into in auxiliary container 2, put into the second monomer in auxiliary container 2 while stirring simultaneously, so that the second monomer is quick with auxiliary container 2 misce bene, then loopback again to main reation kettle 1 in by return circuit pipeline 4, and then avoid pulverous second monomer directly to drop into main reation kettle in 1, can't scatter, and the local violent exothermic problem of meeting.
According to the invention, the main reaction kettle 1 and the auxiliary container 2 are arranged, the main reaction kettle 1 and the auxiliary reaction container are provided with the feed ports, and the auxiliary stirring mechanism is arranged in the auxiliary container 2; meanwhile, a pumping pipeline 3 and a return pipeline 4 are arranged between the main reaction kettle 1 and the auxiliary reaction container, the pumping pipeline 3 can extract materials from the main reaction kettle 1 and convey the materials into the auxiliary reaction container 2, and the return pipeline 4 can guide the materials in the auxiliary reaction container 2 into the main reaction kettle 1, so that when the system performs polymerization reaction, the main reaction kettle 1 is used for performing preliminary reaction in advance, when the preliminary reaction reaches a certain degree, and when the viscosity of slurry in the kettle reaches a certain degree, part of the slurry is extracted from the main reaction kettle 1 into the auxiliary reaction container 2, meanwhile, the reaction monomers to be added are fed into the auxiliary reaction container 2 from a feed opening of the auxiliary reaction container 2, and the slurry mixed with the reaction monomers is guided to the main reaction kettle 1 again after being uniformly stirred and mixed by an auxiliary stirring mechanism. The arrangement mode solves the problems that the powdery reaction monomer is added in the later period and directly thrown into a large amount of slurry to cause difficulty in rapid dispersion and local violent heat release.
In addition, in this embodiment, the feeding port of the main reaction vessel 1 is located at the top thereof, and the material pumping port of the main reaction vessel 1 is located at the central portion of the bottom thereof (i.e., the feeding end of the pumping pipeline 3 is located at the central portion of the bottom of the main reaction vessel 1), so that the material pumped by the pumping pipeline 3 is a reaction product with relatively sufficient reaction.
In this embodiment, the height of the discharge port of the secondary container 2 is higher than the height of the feed back port of the main reaction vessel 1 (i.e. the feed end of the return line 4 is higher than the discharge end thereof), so that the material can automatically enter the main reaction vessel 1 from the secondary container 2 under the action of gravity.
In the present embodiment, the pumping line 3 includes a delivery line and a delivery pump installed in the delivery line.
In addition, in this embodiment, the periphery cladding of return line 4 has the cooling water jacket that is used for leading to coolant to the temperature that the guarantee got into in main reation kettle 1 is in low temperature state, and then can cool down to the interior material of main reation kettle 1 after getting into main reation kettle 1. Or a static mixer 5 is arranged in the return pipeline 4 to enhance the mixing effect between the second monomer and the extracted substance, thereby ensuring that the second monomer enters the main reaction kettle 1 to have a good dispersing effect. The static mixer 5 is coated with a cooling water jacket for leading cooling medium to cool the material in the static mixer 5, so that the material flowing out of the auxiliary container 2 enters the main reaction kettle 1 at low temperature, and the material in the main reaction kettle 1 is cooled.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (9)
1. A polymerization system protected from a severe exotherm, comprising: main reation kettle (1) and inside have vice container (2) of vice rabbling mechanism, wherein:
the main reaction kettle (1) and the auxiliary container (2) are both provided with feed inlets, a pumping pipeline (3) for pumping part of materials in the main reaction kettle (1) and conveying the materials into the auxiliary container (2) and a return pipeline (4) for guiding the materials in the auxiliary container (2) into the main reaction kettle (1) are arranged between the main reaction kettle (1) and the auxiliary container (2).
2. Polymerization system preventing severe exotherm according to claim 1, wherein the feed end of the pumping line (3) is located in the central portion of the bottom of the main reactor (1).
3. Polymerization system with protection against violent exotherms according to claim 1, characterized in that the feed end of the return line (4) is higher than its discharge end.
4. Polymerization system with protection against violent exotherms according to claim 1, characterized in that the periphery of the return line (4) is coated with a cooling jacket for the passage of a cooling medium.
5. The polymerization reaction system capable of preventing violent heat release according to claim 1, wherein the main reaction kettle (1) further has a discharge port, a pumping port and a feed back port, and the auxiliary container (2) further has a feed port and a discharge port; the feeding end of the pumping pipeline (3) is connected with the material pumping port of the main reaction kettle (1), and the discharging end of the pumping pipeline is connected with the feeding port of the auxiliary container (2); the feed end of the return pipeline (4) is connected with the feed inlet of the auxiliary container (2), and the discharge end of the return pipeline is connected with the feed back port of the main reaction kettle (1).
6. Polymerization system preventing severe exotherm according to claim 5, wherein the withdrawal port of the main reactor (1) is located at the central portion of the bottom thereof.
7. Polymerization system preventing violent heat release according to claim 5, wherein the discharge port of the secondary container (2) is located at a height higher than the feed back port of the main reactor (1).
8. Polymerization system to prevent violent exotherms according to any of claims 1 to 7, characterized in that a static mixer (5) is installed in the return line (4).
9. Polymerization system with protection against violent exotherms according to claim 8, characterized in that the static mixer (5) is covered with a cooling jacket for the passage of a cooling medium.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110727626.2A CN113578229A (en) | 2021-06-29 | 2021-06-29 | Polymerization reaction system capable of preventing violent heat release |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110727626.2A CN113578229A (en) | 2021-06-29 | 2021-06-29 | Polymerization reaction system capable of preventing violent heat release |
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| CN113578229A true CN113578229A (en) | 2021-11-02 |
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| CN202110727626.2A Pending CN113578229A (en) | 2021-06-29 | 2021-06-29 | Polymerization reaction system capable of preventing violent heat release |
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|---|---|---|---|---|
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| CN210367717U (en) * | 2019-06-20 | 2020-04-21 | 南京斯拜科生化实业有限公司 | Stirring device for producing kojic acid through biological fermentation |
| CN212284002U (en) * | 2020-04-21 | 2021-01-05 | 江苏奥神新材料股份有限公司 | Dispersing and mixing device for polymerizing polyamic acid |
| CN112844280A (en) * | 2020-12-23 | 2021-05-28 | 中国纺织科学研究院有限公司 | Horizontal reaction kettle, functional polyester production system applying same and production method |
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2021
- 2021-06-29 CN CN202110727626.2A patent/CN113578229A/en active Pending
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| JPH01259036A (en) * | 1988-04-10 | 1989-10-16 | Kanegafuchi Chem Ind Co Ltd | Production of polymer and production equipment therefor |
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| FR2827294A1 (en) * | 2001-07-10 | 2003-01-17 | Rhodianyl | Batch production of polyamide, e.g. polyamide 6,6, from diacid and diamine involves polycondensation after adjusting the stoichiometry of the reaction mixture by adding diamine at a rate determined by end-group analysis |
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Application publication date: 20211102 |