Amphion type amino silicone oil and preparation method thereof

A technology of amino silicone oil and zwitterion, applied in the field of zwitterionic amino silicone oil and its preparation, can solve the problems of easy yellowing of fabrics, and achieve the effects of reducing yellowing, improving stability and lasting sterilization.

Active Publication Date: 2013-03-06
上海氟聚化学产品股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The amino silicone oil synthesized by this method contains diamino groups, and there are more active hydrogens on the N atom. U...

Method used

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  • Amphion type amino silicone oil and preparation method thereof
  • Amphion type amino silicone oil and preparation method thereof
  • Amphion type amino silicone oil and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] The structural formula of a kind of zwitterionic amino silicone oil is:

[0038]

[0039] in:

[0040]

[0041] x, y, z are all positive integers, 5≤x+y+z≤1000.

[0042] The preparation method of above-mentioned zwitterionic amino silicone oil, concrete steps are as follows:

[0043](1) Add 70.03g of D4 (octamethylcyclotetrasiloxane) and 0.37g of MM (hexamethyldisiloxane) into a dry reaction flask equipped with a thermometer, condenser tube, stirring paddle, and nitrogen protection , heated up to 80°C; add glycidyloxypropylmethyldimethoxysilane solution (29.60g glycidoxypropylmethyldimethoxysilane, hydrolyzed by adding 26.8g water), and stir at constant temperature for 1 hour Finally, distill methanol and water, etc.; add 0.01g KOH, heat up to 130°C, and after constant temperature reaction for 8 hours, vacuumize to evaporate low boilers; cool down to 80°C, add 0.011g acetic acid for neutralization, and continue to cool down to 60°C °C, filter, and discharge to ...

Embodiment 2

[0049] The structural formula of a kind of zwitterionic amino silicone oil is:

[0050]

[0051] in:

[0052]

[0053] x, y, z are all positive integers, 5≤x+y+z≤1000.

[0054] The preparation method of above-mentioned zwitterionic amino silicone oil, concrete steps are as follows:

[0055] (1) Add 77.55g (octamethylcyclotetrasiloxane) D4 and 1.02g dodecyl-terminated dimethyl silicone oil to a dry reaction flask equipped with a thermometer, condenser, stirring paddle and protected by nitrogen gas (Viscosity 5CST), heat up to 80°C; add glycidyloxypropyltrimethoxysilane solution (21.43g glycidoxypropyltrimethoxysilane, hydrolyzed by adding 16.3g water), stir at constant temperature for 0.5 hours, Evaporate methanol and water, etc.; add 0.01g NaOH, heat up to 100°C, and react at constant temperature for 36 hours, then vacuumize to evaporate low boilers; cool down to 80°C, add 0.015g acetic acid for neutralization, continue to cool down to 60°C, Filter and discharge to ob...

Embodiment 3

[0062] The structural formula of a kind of zwitterionic amino silicone oil is:

[0063]

[0064] in:

[0065] R 3 -C 3 h 6 CH 2 H(OH)CH 2 N(CH 2 h 3 ) 2

[0066]

[0067] x, y, z are all positive integers, 5≤x+y+z≤1000.

[0068] The preparation method of above-mentioned zwitterionic amino silicone oil, concrete steps are as follows:

[0069] (1) Add 81.19g of D4 (octamethylcyclotetrasiloxane) and 0.44g of 1,1,3,3-tetramethyl to a dry reaction flask equipped with a thermometer, condenser tube, stirring paddle, and nitrogen protection Base-1,3-dimethoxydisiloxane, heat up to 80°C; add glycidoxypropylmethyldiethoxysilane solution (18.37g glycidoxypropylmethyldiethoxysilane , hydrolyzed by adding 13.3g of water), after stirring at constant temperature for 2 hours, distill ethanol and water, etc.; Boiling matter: cool down to 80°C, add 0.013g of acetic acid to neutralize, continue to cool down to 60°C, filter, and discharge to obtain a transparent viscous liquid, ...

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Abstract

The present invention relates to amphion type amino silicone oil and a preparation method thereof. The amphion type amino silicone oil has a structural formula represented by the following formula, wherein R1 is C1-C12 alkyl, alkoxy or hydroxy, R2 is methyl or hydroxy, R3 is a monoamine group, R4 is an anion modified monoamine group, x, y and z are positive integers, and a sum of x, y and z is more than or equal to 5 and is less than or equal to 1000. The structure characteristics comprise that the main chain contains a silicone-oxygen repeating unit, and the branched chain contains alkyl, amino, hydroxy, a quaternary ammonium cation group and an anion group. The preparation method comprises that: octamethylcyclotetrasiloxane and an epoxy silane cross-linking agent are polymerized to obtain epoxy modified silicone oil; the epoxy modified silicone oil reacts with a monoamine compound to obtain amino modified silicone oil; and finally the amino modified silicone oil reacts with an anion modification agent to obtain the product. With the modified organic silicone oil product, emulsion stability and reactivity during fabric treating are improved, and the treated fabric has good yellowing resistance, washing fastness and fluffy feeling.

Description

technical field [0001] The invention relates to a modified amino silicone oil, in particular to a zwitterionic amino silicone oil and a preparation method thereof. Background technique [0002] Silicone emulsions, especially amino-modified silicone emulsions, have a long history of development as fabric finishing agents and are currently the most widely used of all modified silicone emulsions. The fabric finished with amino silicone oil emulsion is soft, smooth, elastic, anti-wrinkle, and has good antistatic and certain washability. However, the amino-modified fabric is prone to yellowing, poor hygroscopicity, etc., and needs further improvement. [0003] The general method for preparing amino silicone oil is: cyclic siloxane (for example, octamethylcyclotetrasiloxane, DMC, hexamethylcyclotrisiloxane) and amino coupling agent (for example, N-β-aminoethyl N-γ-aminopropylmethyldimethoxysilane, N-β-aminoethyl-γ-aminopropyltrimethoxysilane, N-β-aminoethyl-γ-aminopropylmethyldi...

Claims

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Application Information

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IPC IPC(8): C08G77/398C08G77/388D06M15/643
Inventor 胡逊曹华斌武利杨坡
Owner 上海氟聚化学产品股份有限公司
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