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Method for titrating primary amine content of natural protein fibers

A protein fiber, primary amine technology, applied in material analysis by observing the influence of chemical indicators, and analysis by chemical reaction of materials, etc., can solve the problem that natural protein fibers cannot be applied, and the molecular structure of natural protein fibers is destroyed. , inaccurate results, etc.

Inactive Publication Date: 2013-10-02
WUHAN TEXTILE UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method can only be suitable for natural cellulose fibers, not natural protein fibers, because natural cellulose fibers only contain hydroxyl groups that can react with isocyanates, while natural protein fibers contain both hydroxyl groups and primary amines that can react with isocyanates. react
Moreover, due to the mutual interference between hydroxyl groups and primary amines, this method cannot separately titrate the content of hydroxyl groups and the content of primary amines in natural protein fibers
In addition, di-n-butylamine is an alkaline liquid, and natural protein fibers are prone to degradation when exposed to alkali, destroying the molecular structure of natural protein fibers, resulting in inaccurate results
Therefore, this method is not suitable as a titration method for hydroxyl content in natural protein fibers, let alone as a titration method for primary amines in natural protein fibers

Method used

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  • Method for titrating primary amine content of natural protein fibers
  • Method for titrating primary amine content of natural protein fibers
  • Method for titrating primary amine content of natural protein fibers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] A Esterification of wool

[0056] Submerge 1 g of the cleaned wool in acetone with a bath ratio of 1:50, add 0.02 g of a silane coupling agent whose organophilic group is an alkane long molecular chain, and carry out esterification reaction with the extracted wool at a reaction temperature of 70 °C. After 3 hours of reaction, a Soxhlet extractor was used to remove unreacted silane coupling agent. The extraction agent was acetone, and the extraction temperature was 80 oC. After 3 hours of extraction, it was placed in a vacuum oven for drying. Mpa, after drying for 5h, wool is obtained after esterification;

[0057] B Reaction of wool with MDI after esterification

[0058] Put the esterified wool obtained in step A into toluene, the bath ratio is 1:20, add 0.5gMDI to react with the esterified wool, the reaction temperature is 35 oC, and take the reacted wool out of toluene after 20 minutes of reaction , using xylene to clean the reacted wool, the bath ratio is 1:10, the...

Embodiment 2

[0072] A. Esterification of cashmere

[0073] Immerse 1 g of cashmere after cleaning in acetone, the bath ratio is 1:60, add 0.017 g of silane coupling agent whose organophilic group is methyl and carry out esterification reaction with the cashmere after cleaning, the reaction temperature is 75 oC, after 4 hours of reaction Use a Soxhlet extractor to remove unreacted silane coupling agent. The extraction agent is acetone. The extraction temperature is 80 oC. After extraction for 4 hours, it is placed in a vacuum oven for drying. The drying temperature is 135 oC and the vacuum degree is -0.1Mpa. After 6h, obtain cashmere after esterification;

[0074] B. Reaction of cashmere and TDI after esterification

[0075] Put the cashmere after esterification obtained through step A into xylene, the bath ratio is 1:25, add 0.33g TDI to react with the cashmere after esterification, the reaction temperature is 40 ℃, react the cashmere after reaction for 30min from two Take out from tolue...

Embodiment 3

[0089] A Esterification reaction of silk

[0090] Immerse 1g of silk after cleaning in acetone, the bath ratio is 1:70, add 0.014g of silane coupling agent whose organophilic group is vinyl to carry out esterification reaction with silk after cleaning, the reaction temperature is 8-0 oC, the reaction After 5 hours, use a Soxhlet extractor to remove the unreacted silane coupling agent. The extraction agent is acetone, and the extraction temperature is 80 oC. After 5 hours of extraction, it is placed in a vacuum oven for drying. , after drying for 7 hours, the esterified silk was obtained;

[0091] B Reaction of silk and HDI after esterification

[0092] Put the esterified silk obtained in step A into acetone, the bath ratio is 1:30, add 0.2g HDI to react with the esterified silk, the reaction temperature is 45 oC, after 40min, take the reacted silk out of the acetone , using xylene to clean the silk after the reaction, the bath ratio is 1:30, the cleaning temperature is 45 o ...

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Abstract

The invention provides a method for titrating primary amine content of natural protein fibers. The method comprises the following steps of: cleaning and drying the natural protein fibers, performing esterification reaction between the natural protein fibers and a coupling agent, reacting the esterified natural protein fibers with isocyanate, reacting di-n-butyl amine with excessive isocyanate, performing back titration on the di-n-butyl amine by using a standard hydrochloric acid solution, and calculating the primary amine content of the natural protein fibers according to a formula. The titrating method is simple, does not need additional complex conditions, and is sensitive and quick in measurement and high in precision.

Description

technical field [0001] The invention relates to a titration method for primary amine content, in particular to a titration method for primary amine content in natural protein fibers. Background technique [0002] Natural protein fibers include silk, wool, cashmere, down, human hair, rabbit fur, mohair, etc., which are renewable natural materials with excellent performance. At present, natural protein fibers are widely used in people's daily life. In addition to clothing and bedding, they also appear in automotive interiors, decorations, and high-end luxury goods. With the improvement of human living standards, further in-depth research is needed on natural protein fibers, especially the research on primary amines in natural protein fibers, because primary amines affect the dyeing performance, hygroscopicity, comfort and functionalization of natural protein fibers Modification feasibility and options. [0003] The measurement of primary amines in natural protein fibers incl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/78
Inventor 刘欣陈凤翔程远佳吴勇敏徐卫林
Owner WUHAN TEXTILE UNIV
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