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Fluoride-free water-repellent softening agent as well as preparation method and application thereof

A fluorine-free water-repellent and softener technology, which is applied in the direction of improved hand-feeling fibers, textiles and papermaking, fiber treatment, etc., and can solve the problems of insufficient softness and smoothness of fabric touch

Active Publication Date: 2021-09-14
NINGBO RUNHE HIGH TECH MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, the fabrics finished by fluorine-containing waterproofing agents on the market are not soft enough to the touch. Therefore, more and more people are devoting their energy to the research field of fluorine-free fabric waterproofing agents, using water-repellent silane segments to make fabrics have certain Water-repellent effect with soft feel

Method used

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  • Fluoride-free water-repellent softening agent as well as preparation method and application thereof
  • Fluoride-free water-repellent softening agent as well as preparation method and application thereof
  • Fluoride-free water-repellent softening agent as well as preparation method and application thereof

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preparation example Construction

[0027] The application provides a method for preparing a fluorine-free water-repellent softener, comprising the following steps:

[0028] S1, mixing the silicone monomer, emulsifier and water to prepare the first emulsion;

[0029] S2, adding a catalyst to the first emulsion for reaction to obtain a first product, the first product includes polysiloxane whose terminal group is a hydroxyl group;

[0030] S3, remove the low boiler in the first product, obtain the second product, in the second product, octamethylcyclotetrasiloxane (D4), decamethylcyclopentasiloxane (D5), dodecamethylcyclopentasiloxane The content of hexasiloxane (D6) is lower than 1000ppm;

[0031] S4, adding an aminosilane coupling agent to the second product for reaction to obtain a third product, the third product includes polysiloxane whose end group is hydroxyl and whose chain segment contains amino groups.

[0032] Those skilled in the art can understand that the low boilers in the first product mainly re...

Embodiment 1

[0057] Step 1: Put 9g of fatty alcohol polyoxyethylene ether and 28g of silicone monomer (DMC) into the mixer, start stirring to mix evenly;

[0058] Step 2: Put the uniformly mixed material in step 1 into a high-pressure homogenizer, add 60g of water, and homogenize until the liquid turns bluish. After the particle size of the emulsion is tested to be less than 100nm, stop the homogenization;

[0059] Step 3: Put the homogenized liquid into a clean reactor, raise the temperature to 70°C, add 0.01g of sodium hydroxide, raise the temperature to 80°C, and keep it warm for 7 hours;

[0060] Step 4: Raise the temperature to 130°C, keep the vacuum at -0.1MPa for 10 hours, until the gas chromatography detects that the low ring body content is lower than 800ppm, and stop the vacuum;

[0061] Step 5: Add 2.5 g of γ-aminopropyltriethoxysilane and keep warm for 5 hours;

[0062] Step 6: Cool down to 45°C, add 0.5g of pH adjuster, stir evenly, and discharge.

Embodiment 2

[0064] Step 1: Put 8g of fatty alcohol polyoxyethylene ether and 29g of silicone monomer (DMC) into the mixer, start stirring to mix evenly;

[0065] Step 2: Put the uniformly mixed material in step 1 into a high-pressure homogenizer, add 59g of water, and homogenize until the liquid turns bluish. After the particle size of the emulsion is tested to be less than 100nm, stop the homogenization;

[0066] Step 3: Put the homogenized liquid into a clean reactor, raise the temperature to 70°C, add 0.01g of sodium hydroxide, raise the temperature to 90°C, and keep it warm for 8 hours;

[0067] Step 4: Raise the temperature to 150°C, keep the vacuum at -0.08MPa for 12 hours, until the gas chromatography detects that the low ring body content is lower than 800ppm, and stop the vacuum;

[0068] Step 5: Add 3 g of γ-aminopropyltrimethoxysilane and keep warm for 5-6 hours;

[0069] Step 6: Cool down to 45°C, add 0.5g of pH adjuster, stir evenly, and discharge.

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Abstract

The invention discloses a fluoride-free water-repellent softening agent and a preparation method and application thereof, and the preparation method of the fluoride-free water-repellent softening agent comprises the following steps: S1, mixing an organosilicon monomer, an emulsifier and water to prepare a first emulsion; S2, adding a catalyst into the first emulsion for reaction to obtain a first product; S3, removing low-boiling-point substances in the first product to obtain a second product; and S4, adding an amino silane coupling agent into the second product for a reaction to obtain a third product. The two ends of a molecular chain of the fluorine-free water-repellent softening agent have active group hydroxyl groups, and a chain segment also has amino groups, so that a fabric can be endowed with an excellent water-repellent effect, the softening agent does not contain fluorine substances and is high in environmental protection property, the contents of low-ring bodies D4, D5 and D6 in the softening agent are all lower than 1000ppm, and the fluorine-free water-repellent softening agent disclosed by the invention has a smooth hand feeling when being applied to fabrics.

Description

technical field [0001] The present application relates to the field of fabric finishing agents, in particular to a fluorine-free water-repellent softener, its preparation method and its application. Background technique [0002] The fabric waterproofing agents currently on the market are mainly fluorine-containing compounds, but their production and use will have harmful effects on the human body and the environment. Since July 4, 2020, the European Union has officially begun to control PFOA, its salts and related substances. REACH has a limit value of 25ppb for PFOA-related substances. In addition, the fabrics finished by fluorine-containing waterproofing agents on the market are not soft enough to the touch. Therefore, more and more people are devoting their energy to the research field of fluorine-free fabric waterproofing agents, using water-repellent silane segments to make fabrics have certain Water-repellent, yet soft to the touch. In the synthesis process of silic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/26D06M15/643
CPCC08G77/26D06M15/6436D06M2200/12D06M2200/50
Inventor 章东升皮碧荣顾海钗李冰林付公仆
Owner NINGBO RUNHE HIGH TECH MATERIAL CO LTD
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