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Synthetic method of flexible finishing agent for polysiloxane flax in comb structure

A soft finishing agent and polysiloxane technology, applied in fiber treatment, textiles and papermaking, plant fiber, etc., to achieve high conversion rate, sufficient addition reaction, and good biological aging resistance

Inactive Publication Date: 2014-02-26
QIQIHAR UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Using macromolecules and polymethylhydrogensiloxane with a certain chain length for hydrosilylation reaction, starting with acrylate monomers, the research and application of carboxyl and amino graft modified polysiloxanes have been carried out in China. Applying for related patents, and using acrylonitrile and monoallylamine as monomers to graft and modify polymethylhydrogensiloxane to obtain amphoteric silicone modified products, there is no public report in China

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Step 1: In a 100mL four-necked flask equipped with a reflux condenser and a dropping funnel, add 10.46g of polymethylhydrogensiloxane, 9.56g of toluene, and the quality of the polymerization inhibitor phenothiazine as acrylonitrile and monoallyl 0.05% of the total mass of base amine, the quality of chloroplatinic acid-isopropanol catalyst solution is 60ppm of the total mass of graft modified monomers;

[0014] Step 2: Open condensed water, pass nitrogen gas for 5 minutes, heat and stir to dissolve polymethylhydrogensiloxane in toluene, and raise the temperature of the reaction system to 70°C;

[0015] Step 3: Use a constant pressure dropping funnel to drop the mixed solution containing 5.0g toluene and 1.99g acrylonitrile, control the time to add dropwise within 1~1.5h, heat the reaction system to 77°C, continue to stir and keep the constant temperature reaction for 15h Stop the reaction and measure the conversion rate;

[0016] Step 4: Lower the reaction temperature t...

Embodiment 2

[0019] Step 1: Add polymethylhydrogensiloxane 10.46g, toluene 10.38g, polymerization inhibitor phenothiazine in a 100mL four-neck flask equipped with a reflux condenser and dropping funnel. 0.05% of the total mass of the amine, the quality of the chloroplatinic acid-isopropanol catalyst solution is 50ppm of the total mass of the graft modified monomer;

[0020] Step 2: Open condensed water, pass nitrogen gas for 5 minutes, heat and stir to dissolve polymethylhydrogensiloxane in toluene, and raise the temperature of the reaction system to 70°C;

[0021] Step 3: Use a constant pressure dropping funnel to drop the mixed solution containing 5.0g toluene and 2.18g acrylonitrile, control the time to add dropwise within 1~1.5h, heat the reaction system to 82°C, continue to stir and keep the constant temperature reaction for 15h Stop the reaction and measure the conversion rate;

[0022] Step 4: Lower the reaction temperature to 50°C, add dropwise a mixed solution containing 5.0g tol...

Embodiment 3

[0025] Step 1: Add polymethylhydrogensiloxane 10.46g, toluene 11.43g, polymerization inhibitor phenothiazine in a 100mL four-necked flask equipped with a reflux condenser and dropping funnel. 0.05% of the total mass of the amine, the quality of the chloroplatinic acid-isopropanol catalyst solution is 40ppm of the total mass of the graft modified monomer;

[0026] Step 2: Open condensed water, pass nitrogen gas for 5 minutes, heat and stir to dissolve polymethylhydrogensiloxane in toluene, and raise the temperature of the reaction system to 70°C;

[0027] Step 3: Use a constant pressure dropping funnel to drop the mixed solution containing 5.0g toluene and 2.36g acrylonitrile, control the time to add dropwise within 1~1.5h, heat the reaction system to 86.0°C, continue to stir and keep the constant temperature reaction for 15h Stop the reaction and measure the conversion rate;

[0028] Step 4: Lower the reaction temperature to 50°C, add dropwise a mixed solution containing 5.0g...

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Abstract

The invention discloses a synthetic method of a flexible finishing agent for polysiloxane flax in a comb structure, particularly relates to a synthetic method of carboxyl amino grafted and modified polysiloxane in a comb structure, and belongs to the technical field of synthesis of flexible finishing agents of flax. By taking polymethylhydrosiloxane, acrylonitrile and monoallyl amine as raw materials which are wide in source, moderate in price and full in addition reaction, the product is feasible to separate and purify, so that the obtained carboxyl amino grafted and modified polysiloxane in the comb structure is high in yield. As the matter serving as a flexible finishing agent of flax is one of compounds in stable structure, the compounds are better in biological aging resistance, free from rejecting phenomenon to animal bodies, free from harmful effect to the environment and environment-friendly. Secondarily, by means of hydrosilylation, the method is concise in reaction line and higher in conversion ratio.

Description

technical field [0001] The invention relates to a method for synthesizing a comb-shaped polysiloxane softening agent for linen, in particular to a method for synthesizing a comb-structure polysiloxane modified by carboxyl amino grafting, and belongs to the technical field of synthesis of a flax softening agent . Background technique [0002] The carboxyl group introduced into the main chain of silicone oil has reactivity. Using the adsorption and reactivity of the carboxy group, the carboxy group silicone oil is used in fabric softening agents, polishing agents, tape lubricants and film release agents, drug slow-release materials, and personal protection products. , Successful application of leather waterproofing agent. In addition to retaining the inherent hydrophobicity and releasability of dimethyl silicone oil, the aminohydrocarbon group also endows it with reactivity, adsorption, lubricity and softness, so it is used in fabric softening agents, coating additives, It i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/388C08G77/12D06M15/643D06M101/06
Inventor 宋秘钊郝诚诚张慧君王硕赵欣任志会张原
Owner QIQIHAR UNIVERSITY
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