Preparation method of soluble polyimide precipitated fiber

A technology of polyimide and precipitating fiber is applied in the field of preparation of soluble and fusible polyimide precipitating fiber, which can solve the problem that it is difficult to prepare high-performance and high-temperature resistant polyimide paper, and it is difficult to prepare short polyimide paper. Cut fibers are closely combined, affecting the strength of polyimide paper, etc., to achieve continuous and large-scale stable production, controllable shape and beating degree, and good filament separation.

Active Publication Date: 2021-03-09
CHANGZHOU SUNCHEM HIGH FORMANCE POLYMER
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the thermal imidization of polyamic acid fibrids, moisture will be generated, which will lead to agglomeration of fibrids, which will greatly affect the performance of polyimide paper made by wet papermaking
[0005] In addition, the existing polyimide fibrids are basically not melted, so they cannot be tightly combined with polyimide chopped fibers during hot pressing, thus affecting the strength of the prepared polyimide paper and making it difficult to prepare Lithium battery separator paper, capacitor paper, insulating paper, honeycomb paper and other high-performance high-temperature resistant polyimide paper

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1）

[0022] The preparation method of the soluble polyimide precipitated fiber of the present embodiment has the following steps:

[0023] ①Precipitation agent preparation: mix calcium chloride, N,N-dimethylacetamide [hereafter expressed as DMAc] and water according to the weight percentage of 3%, 80% and 17% and stir evenly.

[0024] ②Preparation of polyimide stock solution: Stir and react equimolar diamine monomers and dianhydride monomers and an appropriate amount of solvent DMAc at a temperature of 0°C and under nitrogen protection for 15 hours to obtain a polyamic acid solution, and then undergo a chemical cycle dehydration to obtain a polyimide solution (mass concentration of 20%), and finally dilute the polyimide solution to a mass concentration of 7% with N,N-dimethylacetamide to obtain a polyimide stock solution. The intrinsic viscosity of this polyimide stock solution was 3.8 dl / g.

[0025] The diamine monomers used in this example are equimolar 4,4'-diaminodiphenyl ethe...

Embodiment 2～ Embodiment 4）

[0030] The preparation method of the soluble polyimide fibrids of each embodiment is basically the same as that of Example 1, and the differences are shown in Table 1.

[0031] Table 1

[0032] Example 1 Example 2 Example 3 Example 4 calcium chloride 3% 5% 8% 10% DMAC 80% 85% 80% 80% water 17% 10% 12% 10% Diamine monomer 4,4'-ODA and APABI BAPS and APABI 4,4'-ODA and APABI BAPS and APABI Dianhydride monomer HQDPA and 6FDA HQDPA and 6FDA HQDPA and 6FDA HQDPA and 6FDA Intrinsic viscosity of polyimide stock solution 3.8dl / g 2.8dl / g 3.8dl / g 2.8dl / g Polyimide Stock Solution Concentration 7% 6% 7% 6% Precipitating agent flow 500kg / h 400kg / h 600kg / h 400kg / h Polyimide stock solution flow rate 50kg / h 40kg / h 40kg / h 30kg / h Sedimentation machine speed 3000rpm 4000rpm 4000rpm 4500rpm beating degree 31°SR 35°SR 33°SR 41°SR fiber weight average le...

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Abstract

The invention discloses a preparation method of soluble and meltable polyimide precipitated fiber, which comprises the following steps: ① mixing calcium chloride, N,N-dimethylacetamide and water in proportion and stirring evenly to obtain Precipitating agent; ②React diamine monomer and dianhydride monomer in an aprotic polar solvent to form a polyamic acid solution, then undergo chemical cyclodehydration to obtain a polyimide solution, and finally dilute to obtain a polyimide Stock solution; ③Inject the precipitating agent and the polyimide stock solution into the precipitator respectively, stir and shear at a high speed in the precipitator to obtain a suspension, and then filter and wash with water to obtain a soluble polyimide precipitator fiber. The polyimide fibrids prepared by the present invention can not only meet the requirements of wet papermaking well, but also can be melted, so that they can be closely combined with polyimide chopped fibers during hot pressing, and finally can be applied to the preparation of High-strength lithium battery separator paper, capacitor paper, insulating paper, honeycomb paper and other high-performance and high-temperature resistant paper products.

Description

technical field [0001] The invention belongs to the technical field of polyimide, and in particular relates to a preparation method of soluble and meltable polyimide precipitated fibers. Background technique [0002] Polyimide is a polymer material with high heat resistance in industrial applications. It has excellent heat resistance, low temperature resistance, insulation, flame retardancy, corrosion resistance, radiation resistance, stable size, stable chemical properties, high strength, High modulus, strong creep resistance, excellent friction performance, non-toxic and other excellent properties, widely used in aviation, aerospace, electrical appliances, machinery, chemicals, microelectronics and other high-tech fields. At present, the technology and production capacity of the United States and Japan are still in the leading position in the world. [0003] Due to the characteristics of imide groups, polyimide has better heat resistance and chemical stability than aramid...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F6/88D01F1/10D21H13/26C08G73/10
CPCC08G73/1042C08G73/1057C08G73/1078D01F1/10D01F6/88D21H13/26
Inventor 胡国宜胡锦平易泽雄蒋志强奚小金
Owner CHANGZHOU SUNCHEM HIGH FORMANCE POLYMER
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