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A kind of preparation method of straight-chain tertiary amine block amino silicone oil

A block amino silicone oil, chain tertiary amine type technology, applied in the direction of improved hand-feeling fibers, fiber processing, textiles and papermaking, etc., can solve the problems of decreased softening effect, yellowing of fabrics, hydrophobicity, etc., to reduce environmental protection pressure and eliminate The effect of yellowing and improving washing fastness

Active Publication Date: 2021-02-02
ZHEJIANG HAPPY CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These two types of finishing auxiliaries have their own advantages, but also have the following disadvantages: 1. Amino silicone oil: ①Poor emulsion stability, ②Poor compatibility, ③The finished textiles are hydrophobic and have static electricity; ④It is easy to cause yellowing and discoloration of the fabric Change
Di-block silicone oil: ①The washing fastness is not good, ②Contains solvents, ③The effect of block silicone oil on natural fibers is not as good as that of amino silicone oil, and the dosage is large
[0003] In order to overcome the shortcomings of amino silicone oil and block silicone oil in the application, the usual method is: graft polyether hydrophilic groups on the branch chain of amino silicone oil, block the active hydrogen on the amino group, improve yellowing and discoloration, Improves hydrophilicity and antistatic properties, but causes a decrease in softening effect; in the preparation of block silicone oil, a low-solvent or solvent-free manufacturing process is used, but there are many restrictions on the raw materials and conditions of the synthesis process, and the obtained product is effective in use Not as good as the original block silicone oil

Method used

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  • A kind of preparation method of straight-chain tertiary amine block amino silicone oil
  • A kind of preparation method of straight-chain tertiary amine block amino silicone oil
  • A kind of preparation method of straight-chain tertiary amine block amino silicone oil

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0020] The first two-end epoxy silicone oil (chemical formula is Each of the following embodiments is the same as this) the raw material and the methylethanolamine raw material are pretreated, specifically: vacuumize at a temperature of 105 to 110°C, control the vacuum at -0.01 to -0.03MPa, and stir for 2 hours , to remove the dimethylsiloxane ring and moisture remaining in the raw material.

[0021] Weigh 136.6 grams of the first double-ended epoxy silicone oil with a siloxane chain link a of 50, 3.02 grams of methyl ethanolamine, add it to a 500 ml four-necked reaction flask, put it into an ultrasonic machine, heat up and stir, and control the temperature at 75 ~80°C, ultrasonic power 40 watts, and react for 2 hours.

[0022] Adding silica link a 1 Be the second two-end epoxy silicone oil of 1 (chemical formula is Each of the following embodiments is the same as this) 7.24 grams, add 1.5 grams of N-(γ'-dimethylaminopropyl)-γ-aminopropylmethyldimethoxysilane, heat up to ...

example 2

[0024] The first double-ended epoxy silicone oil as raw material and the raw material methylethanolamine need to be pretreated, specifically: vacuumize at a temperature of 105-110°C, control the vacuum degree at -0.01-0.03MPa, and stir for 2 hours. Remove dimethylsiloxane rings and moisture remaining in raw materials.

[0025] Weigh 136.6 grams of the first double-ended epoxy silicone oil with a siloxane chain link a of 50, 3.02 grams of methyl ethanolamine, add it to a 500 ml four-necked reaction flask, put it into an ultrasonic machine, heat up and stir, and control the temperature at 75 ~80°C, ultrasonic power 40 watts, and react for 2 hours.

[0026] Adding silica link a 1 17.8 grams of the second double-ended epoxy silicone oil of 5, add 1 gram of N-(γ'-dimethylaminopropyl)-γ-aminopropylmethyldimethoxysilane, three-(dimethylaminomethyl Base) 1 gram of phenol, heated to 110 ° C, ultrasonic power 100 watts, stirred for 6 hours, added 1 gram of glacial acetic acid, stirred...

example 3

[0028] The first double-ended epoxy-based silicone oil and the raw material methylethanolamine should be pretreated, specifically: vacuumize at a temperature of 105-110°C, with a vacuum degree of -0.01-0.03MPa, stir for 2 hours, remove Dimethicone rings and moisture remaining in raw materials.

[0029] Weigh 189.4 grams of the first double-ended epoxy silicone oil with a siloxane chain link a of 70, and 3.02 grams of methylethanolamine, add it to a 500 ml four-necked reaction flask, put it into an ultrasonic machine, heat up and stir, and control the temperature at 75 ~80°C, ultrasonic power of 40 watts, and reaction for 3 hours.

[0030] Adding silica link a 1 7.24 grams of the second double-ended epoxy silicone oil of 1, 2.5 grams of N-(γ'-dimethylaminopropyl)-γ-aminopropylmethyldimethoxysilane was added, the temperature was raised to 110°C, and the ultrasonic power was 100 watts, stirring and reacting for 6 hours, adding 1 g of glacial acetic acid, stirring for 30 minutes...

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Abstract

The invention discloses a preparation method of linear tertiary amine type block amino silicone oil. The specific preparation method is as follows: (1) using the first double-end oxidized silicone oil with 50-100 silicone chain members to react with methylethanolamine , to generate hydroxyl-terminated straight-chain tertiary amine amino silicone oil; (2) the hydroxyl-terminated straight-chain tertiary amine amino silicone oil prepared in step (1) and the second double-ended epoxy-based silicone oil with siloxane chain members of 1 to 5 In the presence of a tertiary amine catalyst, the ultrasonic reaction produces a linear tertiary amine type block amino silicone oil. The straight-chain tertiary amine-type block amino silicone oil prepared according to the method of this case has no active hydrogen, which prevents yellowing and discoloration during storage and use. ; and no organic solvent is used in the whole preparation process, which improves the washing fastness and reduces the pressure on environmental protection. In the textile finishing process, the amount used to achieve the same hand feeling is less than that of conventional block silicone oil.

Description

technical field [0001] The invention relates to a preparation method of linear tertiary amine type block amino silicone oil. Background technique [0002] At present, there are two main types of silicone used in the textile finishing market, amino silicone oil and block silicone oil. These two types of finishing auxiliaries have their own advantages, but also have the following disadvantages: 1. Amino silicone oil: ①Poor emulsion stability, ②Poor compatibility, ③The finished textiles are hydrophobic and have static electricity; ④It is easy to cause yellowing and discoloration of the fabric. Change. Diblock silicone oil: ①The washing fastness is not good, ②Contains solvent, ③Block silicone oil is not as effective for natural fibers as amino silicone oil, and the dosage is large. [0003] In order to overcome the shortcomings of amino silicone oil and block silicone oil in the application, the usual method is: graft polyether hydrophilic groups on the branch chain of amino s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/44D06M15/643
CPCC08G77/44D06M15/6436D06M2200/50
Inventor 雷志涛陶海峰陈贵龙
Owner ZHEJIANG HAPPY CHEM
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