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Preparation method of aqueous sizing agent for modified polycaprolactam carbon fibers

A technology of caprolactam carbon fiber and polyamide, which is applied in the field of synthetic polyamide derivatives, fatty alcohol, phosphoric acid ester and phosphoric acid modified polyamide, which can solve the problems of poor emulsion stability, poor water solubility, and limited application range, etc., to avoid environmental pollution Pollution, cost saving effects

Active Publication Date: 2019-06-18
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the products obtained by the above preparation methods more or less have poor emulsion stability, poor water solubility and limited scope of application. Therefore, in view of the above-mentioned problems, we have prepared a water-soluble emulsion with wide application range, good emulsion stability and water solubility. Polyamide

Method used

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  • Preparation method of aqueous sizing agent for modified polycaprolactam carbon fibers
  • Preparation method of aqueous sizing agent for modified polycaprolactam carbon fibers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] The preparation method of embodiment 1. phosphoric acid modified polyamide 6 (PA6)

[0015] Weigh 20g of PA6 and add it to the prepared three-necked flask (there is a thermometer and condenser installed on the three-necked flask), then add 50ml of acetylacetone, and slowly heat up to 120°C at a heating rate of 5°C / min, then start stirring and continue to heat up to 160°C ℃, then add 40g of phosphoric acid in portions, and continue to heat up to 180°C, stop the reaction at this temperature for 4 hours, then carry out vacuum distillation to remove acetylacetone, start to cool down and weigh the sample to measure its acid value, the product acid The value is 110 mgKOH / g, and finally neutralized with 20% KOH aqueous solution at 80° C. for 2 hours to obtain water-soluble phosphoric acid-modified polyamide 6 (PA6).

[0016] The modified polyamide was formulated into a 1.0% solution as a sizing agent to treat the carbon fiber. The surface morphology of carbon fibers before an...

Embodiment 2

[0017] The preparation method of embodiment 2.O3P modified polyamide 6 (PA6)

[0018] Weigh 20g of PA6 and add it to the prepared three-necked flask (there is a thermometer and a condenser on the three-necked flask), then add 50ml of N-methyl-2-pyrrolidone, and slowly raise the temperature to 130°C at a rate of 5°C / min, then start stirring And continue to heat up to 190°C, then add 38gO3P in portions, and continue to heat up to 200°C, stop the reaction after constant temperature at this temperature for 4h, then carry out vacuum distillation to remove N-methyl-2-pyrrolidone, start to cool down and weigh A sample was taken to measure its acid value. The acid value of the product was 160 mgKOH / g. Finally, it was neutralized with 20% KOH aqueous solution at 80° C. for 2 hours to obtain water-soluble O3P modified polyamide 6 (PA6).

[0019] The modified polyamide was formulated into a 1.0% solution as a sizing agent to treat the carbon fiber. The surface morphology of carbon fiber...

Embodiment 3

[0020] The preparation method of embodiment 3. lauryl alcohol modified polyamide 6 (PA6)

[0021] Weigh 20g of PA6 and add it to the prepared three-necked flask (there is a thermometer and a condenser on the three-necked flask), then add 50ml of N-methyl-2-pyrrolidone, and slowly raise the temperature to 125°C at a rate of 5°C / min, then start stirring And continue to heat up to 180°C, then add 41g of dodecanol in portions, and continue to heat up to 200°C, stop the reaction after constant temperature at this temperature for 4h, and then carry out vacuum distillation to remove N-methyl-2-pyrrolidone, start Cool down and weigh the sample to measure its acid value. The acid value of the product is 120mgKOH / g. Finally, neutralize it with 20% KOH aqueous solution at 80° C. for 2 hours to obtain water-soluble dodecanol-modified polyamide 6 (PA6).

[0022] The modified polyamide was formulated into a 1.0% solution as a sizing agent to treat the carbon fiber. The surface morphology o...

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Abstract

The invention intends to aqueously modify polyamide by phosphoric acid or fatty alcohols having different carbon numbers or phosphate according to the characteristics of the polyamide. The invention relates to a method for synthesizing an aqueous sizing agent for modified nylon carbon fibers. By the method, a plurality of water-soluble nylon sizing agents for different purposes can be synthesized.According to the method, fatty alcohols such as dodecanol, phosphate esters such as 8102P and O3P, and the polyamide such as PA6 and PA66 serve as raw materials, a solvent is added to carry out a ring opening reaction and is removed after the reaction is completed, and a product, namely the hydroxyl modified polyamide, is obtained; reaction endpoints are determined through determination of the acid value of the product, the product is neutralized by NaOH or KOH aqueous solutions to be neutral, and the water-soluble polyamide is obtained. The prepared water-soluble polyamide has a low cost, the solvent used can be reused, the preparation process is simple, and the water dissolution degree is controlled through control of the ratios of reactants and the amount of neutralizers.

Description

technical field [0001] The invention relates to a synthesis technology of water-based polyamide. It is mainly suitable for the synthesis of polyamide derivatives, especially fatty alcohols, phosphoric acid esters and phosphoric acid modified polyamides. Background technique [0002] Polyamide, commonly known as nylon, is a general term for polymers containing amide groups in the repeating unit of the main chain of the macromolecule. Polyamide can be obtained by ring-opening polymerization of lactam, or by polycondensation of diamine and dibasic acid. Because of the polar amide bond and other groups, there are hydrogen bonds between macromolecules, so it has the characteristics of high strength, corrosion resistance, weather resistance, solvent resistance, etc. It has been used in inks, hot melt adhesives, synthetic fibers and coatings, etc. fields are widely used. Polyamides can be divided into solvent polyamides and non-solvent polyamides according to their solubility. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D06M15/598D06M15/59C08G69/48D06M101/40
Inventor 周存吕静成胡允杰郑帼吴波强永勤
Owner TIANJIN POLYTECHNIC UNIV
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