CN113831534A - Preparation and application of organic silicon modified hyperbranched polyimide resin - Google Patents
Preparation and application of organic silicon modified hyperbranched polyimide resin Download PDFInfo
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- CN113831534A CN113831534A CN202111304398.4A CN202111304398A CN113831534A CN 113831534 A CN113831534 A CN 113831534A CN 202111304398 A CN202111304398 A CN 202111304398A CN 113831534 A CN113831534 A CN 113831534A
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- organic silicon
- silicon modified
- modified hyperbranched
- polyimide resin
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1057—Polyimides containing other atoms than carbon, hydrogen, nitrogen or oxygen in the main chain
- C08G73/106—Polyimides containing other atoms than carbon, hydrogen, nitrogen or oxygen in the main chain containing silicon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1003—Preparatory processes
- C08G73/1007—Preparatory processes from tetracarboxylic acids or derivatives and diamines
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention discloses preparation and application of an organic silicon modified hyperbranched polyimide resin, and belongs to the technical field of polyimide resins. According to the invention, the solid water absorbent is arranged to remove redundant moisture in the reaction solution, so that the reaction is more stable, the dehydrating agent can further reduce moisture, the solution has higher purity and good flocculation property, the friction resistance between liquids can be reduced, and the quality of the prepared solution is higher.
Description
Technical Field
The invention relates to the technical field of polyimide resin, in particular to preparation and application of organic silicon modified hyperbranched polyimide resin.
Background
Polyimide refers to a polymer containing imide rings on a main chain, is one of organic high polymer materials with the best comprehensive performance, can be divided into three types of aliphatic polyimide, semi-aromatic polyimide and aromatic polyimide according to the chemical structure of a repeating unit, and is widely applied to the fields of aviation, aerospace, microelectronics, nano-scale, liquid crystal, separation membranes, laser and the like as a special engineering material.
Chinese patent with patent number CN109880092A discloses a preparation and application of organosilicon modified hyperbranched polyimide resin, which is through improving the mechanical properties of hyperbranched polyimide, high temperature resistance, and simultaneously, cross-linking can be performed between siloxane, forming a stable system, making the friction block prepared by organosilicon modified hyperbranched polyimide resin not decompose at higher temperature, more durable, but dianhydride monomer is easy to hydrolyze in water in the preparation process, leading to too low polyimide molecular weight, making the solvent synthesis process not in time separate water, and leading to the reduction of reaction efficiency, and leading to the preparation process not safe enough.
Disclosure of Invention
The invention aims to: in order to solve the problems of low power factor of an asynchronous motor and insufficient safety of a circuit in the running process of the asynchronous motor, the preparation and the application of the organic silicon modified hyperbranched polyimide resin are provided.
In order to achieve the purpose, the invention adopts the technical scheme that: a preparation method of organic silicon modified hyperbranched polyimide resin comprises the following steps:
step one, adding a mixed solvent of a triamine monomer, a dianhydride monomer and methanol into a reaction apparatus one by one, carrying out polymerization reaction, stirring for 10-20 minutes at normal temperature for dissolution, then adjusting the temperature to 45-70 ℃, introducing nitrogen, stirring again for reaction for 6-12 hours, and obtaining a hyperbranched polyamic acid solution;
step two, adding a siloxane monomer into the hyperbranched polyamic acid solution obtained in the step one, and reacting for 8-12 hours at 60-80 ℃ to obtain an organic silicon modified hyperbranched polyamic acid solution;
adding the organic silicon modified hyperbranched polyamic acid solution obtained in the step two into a solid water absorbent, stirring, heating to 100-200 ℃, introducing nitrogen, continuing to react for more than 6 hours, then cooling to 70-80 ℃, separating the solid water absorbent from the reaction solution while the solid water absorbent is hot, then adding a catalyst and a dehydrating agent, reacting for 4-12 hours at the temperature of 30-120 ℃, and carrying out chemical imidization reaction to obtain an organic silicon modified hyperbranched polyimide solution;
step four, carrying out vacuum defoaming treatment on the organic silicon modified hyperbranched polyimide solution obtained in the step three, extruding the organic silicon modified hyperbranched polyimide solution by an extruder, and cooling and drying the organic silicon modified hyperbranched polyimide solution to obtain organic silicon modified hyperbranched polyimide resin;
and step five, carrying out grain cutting, component weighing and packaging on the organic silicon modified hyperbranched polyimide resin obtained in the step four.
Further, the solid water absorbent in the third step is one or more of a molecular sieve, activated alumina, anhydrous sodium sulfate and activated anhydrous copper sulfate.
Through adopting above-mentioned technical scheme, can get rid of unnecessary moisture in the reaction solution through solid water absorbent for the reaction is more stable.
Further, the catalyst in the third step is one or more of pyridine, triethylamine or N-methylpiperidine.
By adopting the technical scheme, the reaction rate among the raw materials can be accelerated through the catalyst, so that the preparation is quicker.
Further, the dehydrating agent in the third step is one or more of Polyacrylamide (PAM), acetic anhydride and propionic anhydride.
By adopting the technical scheme, the dehydrating agent can further reduce moisture, so that the solution has higher purity and good flocculation property, the friction resistance between liquids can be reduced, and the quality of the prepared solution is higher.
Further, the vacuum defoaming treatment in the fourth step is added with a fluorine-containing end-capping agent for mixing.
By adopting the technical scheme, the chemical reaction can be terminated by the fluorine-containing end-capping reagent, so that the vacuum defoaming treatment is more convenient, faster and more comprehensive.
Further, the extrusion, cooling and drying in the fourth step are carried out in the same production line, and the interval time is not more than 5 minutes.
By adopting the technical scheme, the resin preparation process is faster and more stable.
Further, the grain cutting, the weight distribution and the packaging in the step 5 are processed through a numerical control machine.
By adopting the technical scheme, the resin can be quickly molded for later application.
Further, the stirring mode adopts a solution stirrer.
Through adopting above-mentioned technical scheme, can make solution stirring more even accurate through solution stirrer.
Further, the heating mode adopts one or more of electric heating tank heating, electric heating rod heating and steam heating.
By adopting the technical scheme, the solution is heated more quickly by the cooperation of multiple heating modes, so that the preparation process is more convenient and faster.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, the solid water absorbent is arranged, so that redundant water in the reaction solution can be removed, the reaction is more stable, the dehydrating agent can further reduce water, the solution purity is higher, the flocculation property is good, the friction resistance between liquids can be reduced, the quality of the prepared solution is higher, the chemical reaction can be terminated through the fluorine-containing end capping agent, so that the vacuum defoaming treatment is more comprehensive, and the resin preparation process is more rapid and stable through subsequent extrusion, cooling and drying.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The first embodiment is as follows:
a preparation method of organic silicon modified hyperbranched polyimide resin comprises the following steps:
step one, adding 4 parts of triamine monomer, 6 parts of dianhydride monomer and 3 parts of methanol mixed solvent into a reaction apparatus one by one, carrying out polymerization reaction, stirring for 10 minutes at normal temperature for dissolution, then adjusting the temperature to 45 ℃, introducing nitrogen, stirring again for reaction for 6 hours, and obtaining hyperbranched polyamic acid solution;
step two, adding 2.5 parts of siloxane monomer into the hyperbranched polyamic acid solution obtained in the step one, and reacting for 8 hours at 60 ℃ to obtain an organic silicon modified hyperbranched polyamic acid solution;
step three, adding 5 parts of solid water absorbent into the organic silicon modified hyperbranched polyamide acid solution obtained in the step two, stirring, heating to 100 ℃, introducing nitrogen, continuing to react for more than 6 hours, then cooling to 70 ℃, separating the solid water absorbent from the reaction solution while the solution is hot, then adding 3 parts of catalyst and 3 parts of dehydrating agent, reacting for 6 hours at the temperature of 50 ℃, and carrying out chemical imidization reaction to obtain an organic silicon modified hyperbranched polyimide solution;
step four, carrying out vacuum defoaming treatment on the organic silicon modified hyperbranched polyimide solution obtained in the step three, extruding the organic silicon modified hyperbranched polyimide solution by an extruder, and cooling and drying the organic silicon modified hyperbranched polyimide solution to obtain organic silicon modified hyperbranched polyimide resin;
and step five, carrying out grain cutting, component weighing and packaging on the organic silicon modified hyperbranched polyimide resin obtained in the step four.
Example two:
a preparation method of organic silicon modified hyperbranched polyimide resin comprises the following steps:
step one, adding 8 parts of triamine monomer, 12 parts of dianhydride monomer and 6 parts of methanol mixed solvent into a reaction apparatus one by one, carrying out polymerization reaction, stirring for 15 minutes at normal temperature for dissolution, then adjusting the temperature to 55 ℃, introducing nitrogen, stirring again for reaction for 8 hours, and obtaining hyperbranched polyamic acid solution;
step two, adding 7 parts of siloxane monomer into the hyperbranched polyamic acid solution obtained in the step one, and reacting at 70 ℃ for 10 hours to obtain an organic silicon modified hyperbranched polyamic acid solution;
step three, adding 10 parts of solid water absorbent into the organic silicon modified hyperbranched polyamide acid solution obtained in the step two, stirring, heating to 150 ℃, introducing nitrogen, continuing to react for more than 6 hours, then cooling to 75 ℃, separating the solid water absorbent from the reaction solution while the solution is hot, then adding 5 parts of catalyst and 8 parts of dehydrating agent, reacting for 6 hours at the temperature of 80 ℃, and carrying out chemical imidization reaction to obtain an organic silicon modified hyperbranched polyimide solution;
step four, carrying out vacuum defoaming treatment on the organic silicon modified hyperbranched polyimide solution obtained in the step three, extruding the organic silicon modified hyperbranched polyimide solution by an extruder, and cooling and drying the organic silicon modified hyperbranched polyimide solution to obtain organic silicon modified hyperbranched polyimide resin;
and step five, carrying out grain cutting, component weighing and packaging on the organic silicon modified hyperbranched polyimide resin obtained in the step four.
Example three:
a preparation method of organic silicon modified hyperbranched polyimide resin comprises the following steps:
step one, adding 10 parts of triamine monomer, 12 parts of dianhydride monomer and 8 parts of methanol mixed solvent into a reaction apparatus one by one, carrying out polymerization reaction, stirring for 20 minutes at normal temperature for dissolution, then adjusting the temperature to 70 ℃, introducing nitrogen, and stirring again for reaction for 12 hours to obtain hyperbranched polyamic acid solution;
step two, adding 14 parts of siloxane monomer into the hyperbranched polyamic acid solution obtained in the step one, and reacting at 80 ℃ for 12 hours to obtain an organic silicon modified hyperbranched polyamic acid solution;
step three, adding 8 parts of solid water absorbent into the organic silicon modified hyperbranched polyamide acid solution obtained in the step two, stirring, heating to 200 ℃, introducing nitrogen, continuing to react for more than 6 hours, then cooling to 80 ℃, separating the solid water absorbent from the reaction solution while the solution is hot, then adding 5 parts of catalyst and 5 parts of dehydrating agent, reacting for 12 hours at the temperature of 120 ℃, and carrying out chemical imidization reaction to obtain an organic silicon modified hyperbranched polyimide solution;
step four, carrying out vacuum defoaming treatment on the organic silicon modified hyperbranched polyimide solution obtained in the step three, extruding the organic silicon modified hyperbranched polyimide solution by an extruder, and cooling and drying the organic silicon modified hyperbranched polyimide solution to obtain organic silicon modified hyperbranched polyimide resin;
and step five, carrying out grain cutting, component weighing and packaging on the organic silicon modified hyperbranched polyimide resin obtained in the step four.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (9)
1. A preparation method of organic silicon modified hyperbranched polyimide resin is characterized by comprising the following steps:
step one, adding a mixed solvent of a triamine monomer, a dianhydride monomer and methanol into a reaction apparatus one by one, carrying out polymerization reaction, stirring for 10-20 minutes at normal temperature for dissolution, then adjusting the temperature to 45-70 ℃, introducing nitrogen, stirring again for reaction for 6-12 hours, and obtaining a hyperbranched polyamic acid solution;
step two, adding a siloxane monomer into the hyperbranched polyamic acid solution obtained in the step one, and reacting for 8-12 hours at 60-80 ℃ to obtain an organic silicon modified hyperbranched polyamic acid solution;
adding the organic silicon modified hyperbranched polyamic acid solution obtained in the step two into a solid water absorbent, stirring, heating to 100-200 ℃, introducing nitrogen, continuing to react for more than 6 hours, then cooling to 70-80 ℃, separating the solid water absorbent from the reaction solution while the solid water absorbent is hot, then adding a catalyst and a dehydrating agent, reacting for 4-12 hours at the temperature of 30-120 ℃, and carrying out chemical imidization reaction to obtain an organic silicon modified hyperbranched polyimide solution;
step four, carrying out vacuum defoaming treatment on the organic silicon modified hyperbranched polyimide solution obtained in the step three, extruding the organic silicon modified hyperbranched polyimide solution by an extruder, and cooling and drying the organic silicon modified hyperbranched polyimide solution to obtain organic silicon modified hyperbranched polyimide resin;
and step five, carrying out grain cutting, component weighing and packaging on the organic silicon modified hyperbranched polyimide resin obtained in the step four.
2. The preparation method of the organic silicon modified hyperbranched polyimide resin according to claim 1, characterized in that: and the solid water absorbent in the third step is one or more of a molecular sieve, active aluminum oxide, anhydrous sodium sulfate and active anhydrous copper sulfate.
3. The preparation method of the organic silicon modified hyperbranched polyimide resin according to claim 1, characterized in that: the catalyst in the third step is one or more of pyridine, triethylamine or N-methylpiperidine.
4. The preparation method of the organic silicon modified hyperbranched polyimide resin according to claim 1, characterized in that: the dehydrating agent in the third step is one or more of Polyacrylamide (PAM), acetic anhydride and propionic anhydride.
5. The preparation method of the organic silicon modified hyperbranched polyimide resin according to claim 1, characterized in that: and adding a fluorine-containing end-capping agent for mixing in the vacuum defoaming treatment in the fourth step.
6. The preparation method of the organic silicon modified hyperbranched polyimide resin according to claim 1, characterized in that: and the extrusion, cooling and drying in the fourth step are carried out in the same production line, and the interval time is not more than 5 minutes.
7. The preparation method of the organic silicon modified hyperbranched polyimide resin according to claim 1, characterized in that: and the grain cutting, the weight and the packaging in the step 5 are processed by a numerical control machine.
8. The preparation method of the organic silicon modified hyperbranched polyimide resin according to claim 1, characterized in that: the stirring mode adopts a solution stirrer.
9. The preparation method of the organic silicon modified hyperbranched polyimide resin according to claim 1, characterized in that: the heating mode adopts one or more of electric heating tank heating, electric heating rod heating and steam heating.
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| CN202111304398.4A CN113831534A (en) | 2021-11-05 | 2021-11-05 | Preparation and application of organic silicon modified hyperbranched polyimide resin |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114805803A (en) * | 2022-04-18 | 2022-07-29 | 上海通联新材料科技股份有限公司 | Organic silicon modified polyimide resin and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109880092A (en) * | 2019-02-27 | 2019-06-14 | 济南大学 | A kind of preparation and its application of organic-silicon-modified super-branched polyimide resin |
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- 2021-11-05 CN CN202111304398.4A patent/CN113831534A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109880092A (en) * | 2019-02-27 | 2019-06-14 | 济南大学 | A kind of preparation and its application of organic-silicon-modified super-branched polyimide resin |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114805803A (en) * | 2022-04-18 | 2022-07-29 | 上海通联新材料科技股份有限公司 | Organic silicon modified polyimide resin and preparation method and application thereof |
| CN114805803B (en) * | 2022-04-18 | 2024-01-12 | 上海通联新材料科技股份有限公司 | Organosilicon modified polyimide resin and preparation method and application thereof |
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