A kind of preparation method of low-solvent block type polyether amino silicone oil

A technology of block polyether and amino silicone oil, which is applied in the direction of improved handle fiber, fiber treatment, textiles and papermaking, etc., can solve the problems of high labor intensity, long segmented reaction line, and low process controllability, etc., to achieve Conducive to transportation and storage, good hydrophilicity and firm combination

Active Publication Date: 2021-12-14
浙江理工大学桐乡研究院有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, there are a series of problems in the segmented reaction, such as long lines, complicated process, high worker operation intensity and low process controllability.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] A preparation method of low-solvent block type polyether amino silicone oil, the specific steps are as follows:

[0029] (1) Mix 100g terminal hydrogen-containing silicone oil, 12g allyl epoxy polyether and 5.6g N-N dimethylformamide (DMF) evenly, stir and heat up to 80°C, add 0.3ml chloroplatinic acid catalyst, and keep warm for 3h , cooled to 30 ° C to take out the terminal epoxy intermediate.

[0030] In this example, the molar ratio of terminal hydrogen-containing silicone oil to allyl epoxy polyether is 1:2, wherein the molecular weight of terminal hydrogen-containing silicone oil is 8000, and the molecular weight of allyl epoxy polyether is 480.

[0031] (2) Mix 80g of epoxy-terminated intermediate prepared in step (1) with 2.8g of polyetheramine (D230) evenly (the molar ratio of epoxy-terminated intermediate to polyetheramine is 1:1.2), and stir After raising the temperature to 80°C, continue to react for 6 hours until the solution becomes transparent, then add ...

Embodiment 2

[0033] A method for preparing low-solvent block type polyether amino silicone oil, the specific steps are the same as in Example 1, the difference is: (1) 100g of terminal hydrogen-containing silicone oil, 9.6g of allyl epoxy polyether and 5.6g of Mix N-N dimethylformamide (DMF) evenly, stir and raise the temperature to 80°C, add 0.3ml of chloroplatinic acid catalyst, keep the temperature for 3 hours, cool down to 30°C, and take out the terminal epoxy intermediate.

[0034] In this example, the molar ratio of the terminal hydrogen-containing silicone oil to the allyl epoxy polyether is 1:2, wherein the molecular weight of the terminal hydrogen-containing silicone oil is 10,000, and the molecular weight of the allyl epoxy polyether is 480.

[0035] (2) Mix 80g of terminal epoxy intermediate and 2.2g of polyetheramine (D230) evenly, stir and heat up to 80°C and react for 6h until the solution becomes transparent, then add glacial acetic acid to adjust to 6~7 at room temperature, ...

Embodiment 3

[0037] A method for preparing low-solvent block type polyether amino silicone oil, the specific steps are the same as in Example 1, (1) 100g terminal hydrogen-containing silicone oil, 12g allyl glycidyl ether and 5.6g N-N dimethyl formamide ( DMF) and mix evenly, stir and raise the temperature to 80°C, add 0.3ml of chloroplatinic acid catalyst, keep the reaction for 3h, cool down to 30°C, and take out the terminated epoxy intermediate.

[0038] In this example, the molar ratio of the terminal hydrogen-containing silicone oil to the allyl epoxy polyether is 1:2, wherein the molecular weight of the terminal hydrogen-containing silicone oil is 8000, and the molecular weight of the allyl epoxy polyether is 480.

[0039] (2) Mix 80g of terminal epoxy intermediate and 10.8g of polyether amine (ED-900) evenly, stir and heat up to 80°C for 6h until the solution becomes transparent, then add glacial acetic acid to adjust to 6~7 at room temperature, Finally, 9.1 g of fatty alcohol polyo...

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PUM

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Abstract

The invention relates to a preparation method of low-solvent block type polyether amino silicone oil, which belongs to the technical field of organic silicon. The method includes the following steps: (1) Preparation of terminal epoxy intermediate: Mix terminal hydrogen-containing silicone oil, allyl epoxy polyether and DMF evenly, stir and heat up to 70‑80°C, add appropriate amount of catalyst, and react 2~4 Hours, the temperature is lowered to obtain an epoxy-terminated intermediate; (2) Preparation of block polyether amino silicone oil: The epoxy-terminated intermediate prepared in step (1) is mixed with polyether amine, and reacted at 80-110°C for 5- After 8 hours, the mixture was obtained. After cooling down to room temperature, an emulsifier of 8-12% of the total mass of the mixture was added to the mixture for emulsification, and the pH was adjusted to 6-7 to obtain a low-solvent block polyether amino silicone oil. The preparation process of the method is simple, the preparation raw materials are easy to obtain, the use of organic solvents is greatly reduced, and the prepared softening agent can endow the fabric with a thick, crisp and smooth hand feeling, so as to overcome the shortcomings of the prior art.

Description

technical field [0001] The invention relates to a preparation method of low-solvent block type polyether amino silicone oil, which belongs to the technical field of organic silicon. Background technique [0002] In 1940, Patnode, an American, used dimethyldichlorosilane in the waterproof treatment of fibers, which opened up the application of silicone in the textile field. After more than 70 years of development, silicone textile auxiliaries have experienced dimethyl silicone oil mechanical mixture (first-generation silicone finishing agent); hydroxyl silicone oil emulsion (second-generation silicone finishing agent); functional group modified silicone oil (third-generation silicone finishing agent) Silicone finishing agent), such as polyether / epoxy silicone oil (CGF), amino silicone oil, carboxyl silicone oil, polyether / amino silicone oil, etc., and new block-type silicone finishing agents with a linear structure that have emerged in recent years, the so-called Ternary blo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/46D06M15/647
CPCC08G77/46D06M15/647D06M15/6436D06M2200/50
Inventor 李永强王娟曹志海许海军
Owner 浙江理工大学桐乡研究院有限公司
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