CN118420907A - Synthesis method of polyamide imide - Google Patents
Synthesis method of polyamide imide Download PDFInfo
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- CN118420907A CN118420907A CN202410684348.0A CN202410684348A CN118420907A CN 118420907 A CN118420907 A CN 118420907A CN 202410684348 A CN202410684348 A CN 202410684348A CN 118420907 A CN118420907 A CN 118420907A
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- imide
- polyamide
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- binding agent
- polyamideimide
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- 229920002312 polyamide-imide Polymers 0.000 title claims abstract description 56
- 239000004962 Polyamide-imide Substances 0.000 title claims abstract description 55
- 238000001308 synthesis method Methods 0.000 title claims description 8
- 238000000034 method Methods 0.000 claims abstract description 31
- 239000002253 acid Substances 0.000 claims abstract description 26
- -1 trimellitic anhydride acyl chloride Chemical class 0.000 claims abstract description 26
- 239000011230 binding agent Substances 0.000 claims abstract description 23
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 6
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 6
- 239000000178 monomer Substances 0.000 claims abstract description 5
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 20
- 229920000642 polymer Polymers 0.000 claims description 13
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 8
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 7
- 239000003960 organic solvent Substances 0.000 claims description 5
- YBRVSVVVWCFQMG-UHFFFAOYSA-N 4,4'-diaminodiphenylmethane Chemical compound C1=CC(N)=CC=C1CC1=CC=C(N)C=C1 YBRVSVVVWCFQMG-UHFFFAOYSA-N 0.000 claims description 4
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 4
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 4
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 4
- NJMOHBDCGXJLNJ-UHFFFAOYSA-N trimellitic anhydride chloride Chemical compound ClC(=O)C1=CC=C2C(=O)OC(=O)C2=C1 NJMOHBDCGXJLNJ-UHFFFAOYSA-N 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- GEYOCULIXLDCMW-UHFFFAOYSA-N 1,2-phenylenediamine Chemical compound NC1=CC=CC=C1N GEYOCULIXLDCMW-UHFFFAOYSA-N 0.000 claims description 3
- WUGQZFFCHPXWKQ-UHFFFAOYSA-N Propanolamine Chemical compound NCCCO WUGQZFFCHPXWKQ-UHFFFAOYSA-N 0.000 claims description 3
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 3
- SLINHMUFWFWBMU-UHFFFAOYSA-N Triisopropanolamine Chemical compound CC(O)CN(CC(C)O)CC(C)O SLINHMUFWFWBMU-UHFFFAOYSA-N 0.000 claims description 3
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 3
- LVTYICIALWPMFW-UHFFFAOYSA-N diisopropanolamine Chemical compound CC(O)CNCC(C)O LVTYICIALWPMFW-UHFFFAOYSA-N 0.000 claims description 3
- 229940043276 diisopropanolamine Drugs 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- WZCQRUWWHSTZEM-UHFFFAOYSA-N 1,3-phenylenediamine Chemical compound NC1=CC=CC(N)=C1 WZCQRUWWHSTZEM-UHFFFAOYSA-N 0.000 claims description 2
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 claims description 2
- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 claims description 2
- HXKKHQJGJAFBHI-UHFFFAOYSA-N 1-aminopropan-2-ol Chemical compound CC(O)CN HXKKHQJGJAFBHI-UHFFFAOYSA-N 0.000 claims description 2
- VOZKAJLKRJDJLL-UHFFFAOYSA-N 2,4-diaminotoluene Chemical compound CC1=CC=C(N)C=C1N VOZKAJLKRJDJLL-UHFFFAOYSA-N 0.000 claims description 2
- 229940075142 2,5-diaminotoluene Drugs 0.000 claims description 2
- RLYCRLGLCUXUPO-UHFFFAOYSA-N 2,6-diaminotoluene Chemical compound CC1=C(N)C=CC=C1N RLYCRLGLCUXUPO-UHFFFAOYSA-N 0.000 claims description 2
- OBCSAIDCZQSFQH-UHFFFAOYSA-N 2-methyl-1,4-phenylenediamine Chemical compound CC1=CC(N)=CC=C1N OBCSAIDCZQSFQH-UHFFFAOYSA-N 0.000 claims description 2
- PSMDTBKTSLWKRN-UHFFFAOYSA-N 4-(trifluoromethyl)cyclohexa-1,5-diene-1,4-diamine Chemical compound NC1=CCC(N)(C(F)(F)F)C=C1 PSMDTBKTSLWKRN-UHFFFAOYSA-N 0.000 claims description 2
- KZSXRDLXTFEHJM-UHFFFAOYSA-N 5-(trifluoromethyl)benzene-1,3-diamine Chemical compound NC1=CC(N)=CC(C(F)(F)F)=C1 KZSXRDLXTFEHJM-UHFFFAOYSA-N 0.000 claims description 2
- 229940102253 isopropanolamine Drugs 0.000 claims description 2
- 229940018564 m-phenylenediamine Drugs 0.000 claims description 2
- 150000002894 organic compounds Chemical class 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 2
- 238000010298 pulverizing process Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 6
- 239000002360 explosive Substances 0.000 abstract description 5
- 150000001263 acyl chlorides Chemical class 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000000843 powder Substances 0.000 description 14
- HLBLWEWZXPIGSM-UHFFFAOYSA-N 4-Aminophenyl ether Chemical compound C1=CC(N)=CC=C1OC1=CC=C(N)C=C1 HLBLWEWZXPIGSM-UHFFFAOYSA-N 0.000 description 7
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 6
- NGNBDVOYPDDBFK-UHFFFAOYSA-N 2-[2,4-di(pentan-2-yl)phenoxy]acetyl chloride Chemical compound CCCC(C)C1=CC=C(OCC(Cl)=O)C(C(C)CCC)=C1 NGNBDVOYPDDBFK-UHFFFAOYSA-N 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- 239000004642 Polyimide Substances 0.000 description 3
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 3
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 3
- 229920001721 polyimide Polymers 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 150000003949 imides Chemical group 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 125000003368 amide group Chemical group 0.000 description 1
- 150000001408 amides Chemical group 0.000 description 1
- HFACYLZERDEVSX-UHFFFAOYSA-N benzidine Chemical group C1=CC(N)=CC=C1C1=CC=C(N)C=C1 HFACYLZERDEVSX-UHFFFAOYSA-N 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 150000004985 diamines Chemical class 0.000 description 1
- 125000005442 diisocyanate group Chemical group 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000009489 vacuum treatment Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
Classifications
-
- 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
- C08G73/14—Polyamide-imides
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
Abstract
The invention relates to the technical field of polyamide-imide material synthesis, in particular to a method for synthesizing polyamide-imide. The method takes trimellitic anhydride acyl chloride and diamine compound as reaction monomers and alcohol amine organic compound as acid binding agent to prepare polyamide imide. According to the invention, the alcohol amine organic compound with lower inflammable and explosive grade is used as the acid binding agent, so that the safety risk of the traditional acid binding agent is greatly avoided, and the safety in the process of preparing polyamide imide by an acyl chloride method is improved. The acid binding agent has the advantages of easily available raw materials and easy large-scale industrialized application.
Description
Technical Field
The invention relates to the technical field of polyamide-imide material synthesis, in particular to a method for synthesizing polyamide-imide.
Background
Polyamide imide (PAI) is a high-performance polymer derived from polyimide, and has an imide structure and an amide structure on a molecular chain, and has the characteristics of solvent resistance, corrosion resistance, high temperature resistance, impact resistance and the like. In contrast to polyimide, the molecular chain contains both rigid imide rings and flexible amide groups. Therefore, the polyamide imide not only maintains the excellent heat resistance and mechanical property of polyimide, but also solves the defect of difficult processing, greatly increases the tensile property and impact resistance, and has good creep property. Therefore, the excellent performance of PAI is widely applied to the industries of coating, aerospace and the like, has wide application prospect especially in the electronic field, and is highly valued by personnel in various industries.
Researchers have now developed a variety of PAI preparation methods including acid chloride, polycondensation, and diisocyanate, among which the most common and convenient method is acid chloride. The acid chloride method adopts trimellitic anhydride acid chloride and diamine as reaction monomers, has high reaction activity and simple post-treatment, but generates hydrogen chloride waste gas in the preparation process, so that an acid binding agent is required to be added to absorb hydrogen chloride. The traditional acid binding agent mainly comprises triethylamine, epoxypropane and the like, but the triethylamine and the epoxypropane belong to inflammable and explosive agents, and the safety risks of links such as transportation, storage, use and the like are high.
Therefore, the polyamide imide synthesis method adopting the acid binding agent with lower inflammable and explosive grade is provided, and has important significance for the technical field of polyamide imide material synthesis.
Disclosure of Invention
Based on the above, the present invention provides a method for synthesizing polyamideimide. The method adopts the alcohol amine organic compound with lower inflammable and explosive grade as the acid binding agent, so that the safety risk of the traditional acid binding agent is greatly avoided.
In order to achieve the above object, the present invention provides the following solutions:
According to one of the technical schemes of the invention, the synthesis method of the polyamide imide is characterized in that trimellitic anhydride acyl chloride and diamine compounds are used as reaction monomers, and alcohol amine organic compounds are used as acid binding agents to prepare the polyamide imide.
The second technical scheme of the invention is a method for improving the safety in the synthesis process of the polyamide-imide, and the method for synthesizing the polyamide-imide is adopted.
The invention discloses the following technical effects:
according to the invention, the alcohol amine organic compound with lower inflammable and explosive grade is used as the acid binding agent, so that the safety risk of the traditional acid binding agent is greatly avoided, and the safety in the process of preparing polyamide imide by an acyl chloride method is improved.
The acid binding agent has the advantages of easily available raw materials and easy large-scale industrialized application.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a graph showing the thermogravimetric loss of the polyamideimide powders prepared in example 1, example 2, and example 3.
FIG. 2 is an infrared image of the polyamideimide powders prepared in example 1, example 2, and example 3.
Detailed Description
Various exemplary embodiments of the invention will now be described in detail, which should not be considered as limiting the invention, but rather as more detailed descriptions of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. In addition, for numerical ranges in this disclosure, it is understood that each intermediate value between the upper and lower limits of the ranges is also specifically disclosed. Every smaller range between any stated value or stated range, and any other stated value or intermediate value within the stated range, is also encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the invention described herein without departing from the scope or spirit of the invention. Other embodiments will be apparent to those skilled in the art from consideration of the specification of the present invention. The specification and examples of the present invention are exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are intended to be inclusive and mean an inclusion, but not limited to.
As used herein, the term "room temperature", unless otherwise indicated, means 20 to 30 ℃.
The first aspect of the invention provides a method for synthesizing polyamide-imide, which uses trimellitic anhydride acyl chloride and diamine compound as reaction monomers and alcohol amine organic compound as acid-binding agent to prepare the polyamide-imide.
In some embodiments of the invention, the alcohol amine-based organic compound is at least one of ethanolamine, diethanolamine, triethanolamine, propanolamine, dipropanolamine, tripropanolamine, isopropanolamine, diisopropanolamine, triisopropanolamine, n-butanolamine, di-n-butanolamine, and tri-n-butanolamine.
In some embodiments of the invention, the diamine compound is at least one of o-phenylenediamine, m-phenylenediamine, p-phenylenediamine, 2, 4-diaminotoluene, 2, 5-diaminotoluene, 2, 6-diaminotoluene, 1, 4-diaminobenzotrifluoride, 3, 5-diaminobenzotrifluoride, 4' -diaminobiphenyl, 4' -diaminodiphenyl ether, and 4,4' -diaminodiphenylmethane.
In some embodiments of the invention, the molar ratio of the trimellitic anhydride acid chloride to the diamine compound is 1:1; the mole ratio of the acid binding agent to the trimellitic anhydride acyl chloride is (1.2-2): 1.
Too little amount of acid-binding agent can lead to residual hydrogen chloride, too much amount of acid-binding agent can lead to waste and increase the difficulty of solvent recovery. The amount of the acid-binding agent used in the present invention is preferably limited to the above-mentioned ratio range.
In some embodiments of the invention, a method of synthesizing polyamideimide comprises the steps of:
adding diamine compound into organic solvent to dissolve, adding trimellitic anhydride acyl chloride to dissolve, and then adding acid binding agent to react to obtain polymer solution;
imidizing the polymer solution to obtain polyamide imide.
The synthetic method of the polyamide imide comprises the step of preparing at least one of N, N-dimethylacetamide, N-dimethylformamide, N-methylpyrrolidone, tetrahydrofuran, dioxane and dimethyl sulfoxide from the organic solvent.
The synthesis method of polyamide imide, wherein the concentration of the diamine compound in the organic solvent is 0.25-0.45mol/L; the reaction time is 1-12 hours.
The synthesis method of polyamide imide further comprises the steps of adding the polymer solution into water to obtain a filiform polymer, and crushing and drying the filiform polymer.
The reaction route of the method of the invention is as follows:
Wherein the method comprises the steps of
Ar1：
The second aspect of the present invention provides a method for improving the safety in the synthesis of polyamideimide, which adopts the above-mentioned polyamideimide synthesis method.
The invention is further illustrated by the following examples.
Example 1
Step 1, preparation of a polyamide-amic acid solution: to a reaction vessel with nitrogen inlet, water separator, temperature measuring device and stirring device, 50mmol (10.0118 g) of 4,4' -diaminodiphenyl ether and 125mL of N, N-dimethylacetamide were added and stirred until the solution was clear. To the solution, 50mmol (10.5285 g) of trimellitic anhydride acid chloride was added, and after the solution was clarified by stirring, 60mmol (3.66 g) of ethanolamine was added, and the reaction was carried out for 5 hours to obtain a polyamide-amic acid solution.
Step 2, post-treatment: pouring the polyamide-amic acid solution into deionized water to obtain a filamentous polymer, crushing and drying; the obtained polymer powder is subjected to vacuum treatment (the temperature is programmed to 200 ℃ for 1h,250 ℃ for 1h,300 ℃ for 1 h) according to a certain temperature-raising program, and the temperature-raising rate is 10-20 ℃/min, so as to obtain the polyamide-imide powder.
Example 2
The only difference from example 1 was that 125mL of N, N-dimethylacetamide was replaced with 200mL of N, N-dimethylformamide, and 60mmol (3.66 g) of ethanolamine was replaced with 60mmol (6.31 g) of diethanolamine; the rest steps and parameters are the same as those of the embodiment 1; the polyamide-imide powder is prepared.
Example 3
The only difference from example 1 is that 125mL of N, N-dimethylacetamide was replaced with 140mL of N-methylpyrrolidone, and 60mmol (3.66 g) of ethanolamine was replaced with 60mmol (8.95 g) of triethanolamine; the rest steps and parameters are the same as those of the embodiment 1; the polyamide-imide powder is prepared.
FIG. 1 is a graph showing the thermogravimetric loss of the polyamideimide powders prepared in example 1, example 2, and example 3.
FIG. 2 is an infrared image of the polyamideimide powders prepared in example 1, example 2, and example 3.
As can be seen from fig. 1 and 2, the present invention successfully synthesizes polyamideimide; the thermal weight loss curve graph and the infrared graph of the polyamide imide obtained by changing the types of the acid binding agents have the same shape and trend.
Example 4
The only difference from example 1 was that 50mmol (10.0118 g) of 4,4 '-diaminodiphenyl ether was replaced with 50mmol (9.9130 g) of 4,4' -diaminodiphenylmethane and 60mmol (3.66 g) of ethanolamine was replaced with 60mmol (4.51 g) of propanolamine; the rest steps and parameters are the same as those of the embodiment 1; the polyamide-imide powder is prepared.
Example 5
The only difference from example 1 is that 50mmol (10.0118 g) of 4,4 '-diaminodiphenyl ether was replaced with 50mmol (9.2120 g) of 4,4' -diaminodiphenyl ether and 60mmol (3.66 g) of ethanolamine was replaced with 60mmol (7.99 g) of dipropanolamine; the rest steps and parameters are the same as those of the embodiment 1; the polyamide-imide powder is prepared.
Example 6
The only difference from example 1 is that 50mmol (10.0118 g) of 4,4' -diaminodiphenyl ether was replaced with 50mmol (5.4070 g) of o-phenylenediamine and 60mmol (3.66 g) of ethanolamine was replaced with 60mmol (11.48 g) of tripropanolamine; the rest steps and parameters are the same as those of the embodiment 1; the polyamide-imide powder is prepared.
Example 7
The only difference from example 1 was that 50mmol (10.0118 g) of 4,4 '-diaminodiphenyl ether was replaced with 50mmol (9.9130 g) of 4,4' -diaminodiphenylmethane, 125mL of N, N-dimethylacetamide was replaced with 150mL of N-methylpyrrolidone, and 60mmol (3.66 g) of ethanolamine was replaced with 60mmol (7.99 g) of diisopropanolamine; the rest steps and parameters are the same as those of the embodiment 1; the polyamide-imide powder is prepared.
Example 8
The only difference from example 1 was that 50mmol (10.0118 g) of 4,4 '-diaminodiphenyl ether was replaced with 50mmol (9.2120 g) of 4,4' -diaminodiphenyl, 125mL of N, N-dimethylacetamide was replaced with 130mL of N, N-dimethylformamide, and 60mmol (3.66 g) of ethanolamine was replaced with 60mmol (11.48 g) of triisopropanolamine; the rest steps and parameters are the same as those of the embodiment 1; the polyamide-imide powder is prepared.
The thermal decomposition temperatures of 5% and 10% of the polyamide-imide powders prepared in examples 1 to 8 are shown in Table 1.
TABLE 1
The above embodiments are only illustrative of the preferred embodiments of the present invention and are not intended to limit the scope of the present invention, and various modifications and improvements made by those skilled in the art to the technical solutions of the present invention should fall within the protection scope defined by the claims of the present invention without departing from the design spirit of the present invention.
Claims (9)
1. A method for synthesizing polyamide-imide is characterized in that trimellitic anhydride acyl chloride and diamine compound are used as reaction monomers, and alcohol amine organic compound is used as acid binding agent to prepare the polyamide-imide.
2. The method for synthesizing polyamide-imide according to claim 1, wherein the alcohol amine-based organic compound is at least one of ethanolamine, diethanolamine, triethanolamine, propanolamine, dipropanolamine, tripropanolamine, isopropanolamine, diisopropanolamine, triisopropanolamine, n-butanolamine, di-n-butanolamine, and tri-n-butanolamine.
3. The method for synthesizing polyamide-imide according to claim 1, wherein the diamine compound is at least one of o-phenylenediamine, m-phenylenediamine, p-phenylenediamine, 2, 4-diaminotoluene, 2, 5-diaminotoluene, 2, 6-diaminotoluene, 1, 4-diaminobenzotrifluoride, 3, 5-diaminobenzotrifluoride, 4' -diaminobiphenyl, 4' -diaminodiphenyl ether, and 4,4' -diaminodiphenyl methane.
4. The method of synthesizing a polyamideimide according to claim 1, wherein the molar ratio of the acid-binding agent to the trimellitic anhydride acid chloride is (1.2-2): 1.
5. The method for synthesizing polyamideimide according to claim 1, comprising the steps of:
adding diamine compound into organic solvent to dissolve, adding trimellitic anhydride acyl chloride to dissolve, and then adding acid binding agent to react to obtain polymer solution;
imidizing the polymer solution to obtain polyamide imide.
6. The method for synthesizing polyamideimide according to claim 5, wherein the organic solvent is at least one of N, N-dimethylacetamide, N-dimethylformamide, N-methylpyrrolidone, tetrahydrofuran, dioxane and dimethylsulfoxide.
7. The method for synthesizing polyamideimide according to claim 5, wherein the reaction time is 1 to 12 hours.
8. The method for synthesizing polyamideimide according to claim 5, further comprising the steps of adding the polymer solution to water to obtain a filamentous polymer, and pulverizing and drying the filamentous polymer before the imidization treatment.
9. A method for improving safety in the synthesis of polyamideimide, characterized in that the polyamideimide synthesis method according to any one of claims 1to 8 is used.
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| CN103819674A (en) * | 2014-01-20 | 2014-05-28 | 江苏巨贤合成材料有限公司 | Synthesis method of direct-spinning polyamide-imide polymer |
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| JP2020097732A (en) * | 2018-12-14 | 2020-06-25 | 東レ株式会社 | Solution including aromatic polyamide or aromatic polyamideimide |
| JP2021109437A (en) * | 2020-01-08 | 2021-08-02 | 東レ株式会社 | Glass laminate |
| JP2022174847A (en) * | 2021-05-12 | 2022-11-25 | 東レ株式会社 | Film |
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| JPH1149858A (en) * | 1997-07-31 | 1999-02-23 | Toray Ind Inc | Polyamide-imide and its production |
| CN103819674A (en) * | 2014-01-20 | 2014-05-28 | 江苏巨贤合成材料有限公司 | Synthesis method of direct-spinning polyamide-imide polymer |
| CN108291005A (en) * | 2015-12-07 | 2018-07-17 | 日立化成株式会社 | Polyamide-imide resin composition and fluoro coatings |
| JP2020097732A (en) * | 2018-12-14 | 2020-06-25 | 東レ株式会社 | Solution including aromatic polyamide or aromatic polyamideimide |
| JP2021109437A (en) * | 2020-01-08 | 2021-08-02 | 東レ株式会社 | Glass laminate |
| JP2022174847A (en) * | 2021-05-12 | 2022-11-25 | 東レ株式会社 | Film |
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