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Low-solvent synthesis method for terpolymer block silicone oil

A technology of ternary copolymerization block and synthesis method, which is applied in the direction of improved hand feeling fiber, fiber type, textile and papermaking, etc., can solve the problems of reducing solvent usage, easy demulsification, fabric hydrophobicity, etc. Roll, improve catalytic efficiency, increase the effect of effective content

Active Publication Date: 2018-06-22
JIANGSU NIMATE SCI & TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this kind of post-finishing additives generally has the following deficiencies: ①Many products are difficult to emulsify, the stability of the emulsion is poor, easy to break the emulsion, float oil, stick to the roller, and will form silicone oil spots that are difficult to remove on the processed fabric; ②Poor compatibility, Difficult to use in the same bath with other additives (especially additives with different charges); ③Due to the oxidation of amino groups, it is easy to cause yellowing and discoloration of the fabric; ④The finished fabric is hydrophobic and does not absorb sweat; ⑤The finished fabric It is not easy to repair the color, and it is generally necessary to remove the silicone oil before it can be repaired and dyed; ⑥ Some finished fabrics are prone to pinholes or even tear the fabric during sewing
[0005] However, at present, most of the three-component copolymerization block silicone oils use isopropanol or ethylene glycol monobutyl ether as the solvent in the synthesis process and the amount is large. Reducing the amount of solvent used in the synthesis of silicone oil has become a difficult problem

Method used

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  • Low-solvent synthesis method for terpolymer block silicone oil
  • Low-solvent synthesis method for terpolymer block silicone oil
  • Low-solvent synthesis method for terpolymer block silicone oil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Prepare the product of embodiment 1 according to the following steps:

[0038] (1) Take 40 parts by mass of hydrogen-terminated silicone oil with a molecular weight of 13000 in a three-necked flask, stir and heat to 90°C,

[0039] (2) Add 1 mass part of allyl glycidyl ether AGE and 0.04 mass part of chloroplatinic acid, heat and stir to keep the temperature at 115-126 ° C, and react for 2 hours,

[0040] (3) Add 16 parts by mass of polyetheramine ED-2003, and at the same time add 16 parts by mass of 2-methyl-2,4-pentanediol and 32 parts by mass of ethylene glycol monobutyl ether at 140-150°C After reacting for 6 hours, adjust the pH to 6-7 with glacial acetic acid to obtain the finished block silicone oil.

Embodiment 2

[0042] Prepare the product of embodiment 2 according to the following steps:

[0043] (1) Take 35 parts by mass of hydrogen-terminated silicone oil with a molecular weight of 15000, stir and heat it to 90°C in a three-necked flask,

[0044] (2) Add 1 mass part of allyl glycidyl ether AGE and 0.035 mass part of chloroplatinic acid, heat and stir to keep the temperature at 115-126 ° C, and react for 2 hours,

[0045] (3) Add 12.25 parts by mass of polyetheramine ED-2003, and at the same time add 14 parts by mass of 2-methyl-2,4-pentanediol and 28 parts by mass of ethylene glycol monobutyl ether at 140-150°C After reacting for 6 hours, adjust the pH to 6-7 with glacial acetic acid to obtain the finished block silicone oil.

Embodiment 3

[0047] The product of embodiment 3 is prepared according to the following steps:

[0048] (1) Take 40 parts by mass of hydrogen-terminated silicone oil with a molecular weight of 13000 in a three-necked flask, stir and heat to 90°C,

[0049] (2) Add 1 mass part of allyl glycidyl ether AGE and 0.04 mass part of chloroplatinic acid, heat and stir to keep the temperature at 115-126 ° C, and react for 2 hours,

[0050] (3) Add 16 parts by mass of polyetheramine ED-2003, and at the same time add 20 parts by mass of 2-methyl-2,4-pentanediol and 28 parts by mass of ethylene glycol monobutyl ether at 140-150°C After reacting for 6 hours, adjust the pH to 6-7 with glacial acetic acid to obtain the finished block silicone oil.

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Abstract

The invention provides a low-solvent synthesis method for terpolymer block silicone oil. The method is characterized by comprising the following steps: 1) adding hydrogen-terminated silicone oil withmolecular weight of 13,000-15,000 to a reaction container, and performing heating to about 80-90 DEG C while performing stirring; 2) adding allyl glycidyl ether and a catalyst chloroplatinic acid, performing heating, keeping the temperature at 115-126 DEG C, and performing a reaction for about 2 h; 3) adding polyether amine ED-2003, adding 2-methyl 2,4-pentanediol and ethylene glycol monobutyl ether simultaneously, performing a reaction at 140-150 DEG C for 6-8 h, and adjusting pH to 6-7 with glacial acetic acid to obtain the product. A mixed solvent consisting of 2-methyl 2,4-pentanediol andethylene glycol monobutyl ether is used, the quantity of solvents used in synthesis is reduced, the hydrogen-terminated silicone oil with molecular weight of 13,000-15,000 and polyether amine ED-2003are used for synthesis, and excellent handfeel is achieved.

Description

technical field [0001] The invention relates to a method for synthesizing low-solvent terpolymerized block silicone oil. Background technique [0002] Before the popularization of block silicone oil, amino silicone oil emulsion was the main finishing aid widely used in the market. However, such post-finishing additives generally have the following deficiencies: ①Many products are difficult to emulsify, and the stability of the emulsion is poor, easy to break the emulsion, float oil, stick to the roller, and will form silicone oil spots that are difficult to remove on the processed fabric; ②Poor compatibility, Difficult to use in the same bath with other additives (especially additives with different charges); ③Due to the oxidation of amino groups, it is easy to cause yellowing and discoloration of the fabric; ④The finished fabric is hydrophobic and does not absorb sweat; ⑤The finished fabric It is not easy to repair the color, and it is generally necessary to remove the sil...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/46C08G77/38C08G77/06C08G77/08D06M15/647D06M13/165D06M101/32
CPCC08G77/06C08G77/08C08G77/38C08G77/46D06M13/165D06M15/647D06M2101/32D06M2200/50
Inventor 徐美君朱宇澄徐俊红其他发明人请求不公开姓名
Owner JIANGSU NIMATE SCI & TECH CO LTD
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