A kind of synthetic method of ternary copolymerization block silicone oil

A synthesis method and technology of block silicone oil, which is applied in the fields of silicon organic compounds, textiles and papermaking, fiber treatment, etc., can solve problems such as difficult washing, poor stability of amino-modified silicone emulsion, sticking rollers, etc., to ensure fluffy feeling, No demulsification and delamination, good hand feeling effect

Active Publication Date: 2015-08-26
ZHEJIANG JIEFA TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The shortcomings are mainly manifested in the fact that the fabrics treated by it are hydrophobic, feel stuffy and difficult to wash when worn; the light-colored and white fabrics treated with it will appear yellowing to varying degrees after high-temperature baking, and many The stability of amino-modified silicone emulsion is very poor, and the phenomenon of "breaking demulsification and floating oil" often occurs in the process of storage, transportation and application; sticking phenomenon occurs in the process of padding and rolling
[0003] In order to overcome the above-mentioned shortcomings of traditional amino silicone oil, various methods have been adopted to improve it, such as side chain polyether modification, epoxy modification or carboxyl modification, the modified silicone oil has improved stability, but the hand feel is deviated.

Method used

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] The general idea of ​​the present invention is as follows: first, under the catalysis of platinum metal, hydrogen-containing silicone oil at the end and allyl glycidyl ether are catalyzed by platinum metal, and the hydrogen bond at the siloxane end is added to the carbon double bond to generate an epoxy double-end cap at the end (also can be It is a commercially available end epoxy double head), and then the end epoxy double head is ring-opened with D4 (octamethylcyclotetrasiloxane) or DMC (dimethylcyclosiloxane) to form an end epoxy silicone oil , Then, the adduct is reacted and condensed with polyether under solvent conditions. The reaction formula is as follows:

[0016] .

[0017] Concrete reaction steps of the present invention are as follows:

[0018] A. Add 100g of DMC (dimethylcyclosiloxane) or D4 (octamethylcyclotetrasiloxane) to a 250ml three-necked flask; add 4g of epoxy double-capping agent; then add 15 parts of dimethylacetamide , raise the temperature...

Embodiment 2

[0023] Embodiment 2 of the present invention: Step A and the rest are the same as in Embodiment 1, and will not be described in detail. The difference is that in the reaction step B, the epoxy-terminated silicone oil obtained in the step A is added to a 500ml three-necked flask: 90g, polyether multi-component Alcohol 203: 5g, polyether polyol 206: 2.5g, polyether polyol 209: 2.5g, isopropanol: 150g, carry out reflux reaction at 80°C for 12h, and finally remove isopropanol under reduced pressure or add propylene glycol to replace the solvent , to obtain a light yellow and transparent amino polyether block silicone oil, that is, a tertiary block copolymerized silicone oil.

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Abstract

The invention discloses a synthesis method for terpolymer block silicone oil. The synthesis method is characterized by comprising the steps of: (A) adding 100 parts by weight of dimethyl cyclosiloxane or octamethyl cyclotetrasiloxane, 4 parts by weight of epoxy-terminated disiloxane and 15 parts by weight of dimethylacetamide, raising the temperature to 70-80 DEG C, adding 0.02-0.1 part by weight of base catalyst, raising the temperature to 110-120 DEG C, reacting for 3-4 hours, slowly opening vacuum, extracting solvents and low molecular weight matters, continuously raising the temperature to 140-145 DEG C, maintaining the temperature and the vacuum for 2 hours, so as to obtain epoxy silicone oil; and (B) adding 80-100 parts by weight of epoxy-terminated silicone oil, 6-30 parts by weight of polyether polyol and 150 parts by weight of isopropyl alcohol, carrying out backflow reaction for 6-15 hours at 80-86 DEG C, and decompressing and removing the isopropyl alcohol or adding a propylene glycol displacement solvent, so as to obtain amino polyether block silicone oil. By utilizing the terpolymer block silicone oil disclosed by the invention, the fabric has good hand feel, namely fluffy feel and smooth feel, cannot be yellowed or is slightly yellowed.

Description

technical field [0001] The invention relates to a method for synthesizing modified silicone oil, in particular to a method for synthesizing terpolymerized block silicone oil. Background technique [0002] At present, softeners based on various amino-modified silicone oil emulsions are widely used in the finishing of textiles such as cotton, silk, wool and polyester. The finished fabrics are soft, smooth, beautiful, washable and comfortable to wear. performance. Such products have been accepted by people. The shortcomings are mainly manifested in the fact that the fabrics treated by it are hydrophobic, feel stuffy and difficult to wash when worn; the light-colored and white fabrics treated with it will appear yellowing to varying degrees after high-temperature baking, and many The stability of the amino-modified silicone emulsion is very poor, and the phenomenon of "breaking demulsification and floating oil" often occurs during storage, transportation and application; stick...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G81/00C08G77/18D06M15/647C07F7/08
Inventor 邵国标
Owner ZHEJIANG JIEFA TECH
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