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A kind of preparation method of siloxane quaternary ammonium salt

A technology of siloxane and quaternary ammonium salts, which is applied in the field of preparation of siloxane quaternary ammonium salts, can solve problems such as dark product color, waste, and influence on product yield and quality, and achieve product yield and quality improvement. Product quality, the effect of avoiding adverse effects

Active Publication Date: 2020-09-25
GUANGZHOU TINCI MATERIALS TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The synthesis steps of this method are cumbersome and time-consuming, so it is not suitable for industrial production schemes
[0006] In addition, it can also be prepared by a nucleophilic substitution reaction between a quaternary ammonium salt with an epoxy group and a silane coupling agent. However, in this method, because the epoxy group is more active and prone to self-polymerization, the reaction process epoxy The actual effective amount of the group is far lower than its added amount, causing waste and producing more by-products that affect the stability of the product, such as the patent CN103387588A
The polyether substitution degree in the siloxane quaternary ammonium salt prepared by these methods is high, so that the molecular chain is particularly hydrophilic and completely soluble in water, so that when the fabric is processed, it is not easy to adhere to the fabric but is taken by water. The separation system makes the effect on fabric softness, antistatic and antibacterial treatment very poor
Zhou Yupeng, etc. (Synthesis and application of high-grade shampoo conditioner-polysiloxane quaternary ammonium salt [J]. Silicone materials and applications. 1999.3 (2): 12~15) disclosed a polysiloxane quaternary ammonium salt However, this method uses monochloroacetic acid as an acylating reagent, and the water generated during the esterification reaction will seriously affect the yield and quality of the product. Moreover, the temperature of the esterification process is too high, and the color of the resulting product is too dark, which has caused domestic Good quality polysiloxane quaternary ammonium salt products were not obtained

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Allyl polyether (CH 2 CHCH 2 CH 2 CH 2 OCH 2 CH 2 OH), the hydrogen-containing silicone oil (number-average molecular weight 500) with a hydrogen content of 0.30%, is a mixed solution and toluene of 1.2:1 with a material molar ratio, and a chloroplatinic acid (2ppm) catalyst is added in the reaction kettle, and in a nitrogen atmosphere Heat to 130°C, stir evenly, react for 5 hours, distill off toluene and low boilers at a vacuum of 0.05MPa to obtain a transparent viscous liquid that is polyether modified siloxane. The obtained polyether siloxane must be lowered at 100°C for 2 hours under a vacuum of 5mbar to ensure that its moisture content is less than 500ppm.

[0026] (2) Take 250 g of the polyether-modified siloxane obtained in step (1) in a four-necked flask, add 100 g of ethyl acetate, heat up to 60 ° C, and start to add 16.46 g of chloroacetyl chloride dropwise for 2.0 hours , then keep warm for 1h, then cool to 15°C, add 10g sodium ethoxide and 100g eth...

Embodiment 2

[0029] (1) Allyl polyether (CH 2 CHCH 2 CH 2 CH 2 OCH 2 CH 2 OH), the hydrogen-containing silicone oil (number-average molecular weight 1000) with a hydrogen content of 0.35%, is a mixed solution and toluene of 1.2: 1 with a material molar ratio, and chloroplatinic acid (4ppm) catalysts are added in the reactor, and in a nitrogen atmosphere Heat to 130°C, stir evenly, react for 5 hours, distill off toluene and low boilers at a vacuum of 0.05MPa to obtain a transparent viscous liquid that is polyether modified siloxane. The obtained polyether siloxane must be lowered at 100°C for 2 hours under a vacuum of 5mbar to ensure that its moisture content is less than 500ppm.

[0030](2) Take 250 g of the polyether-modified siloxane obtained in step (1) in a four-necked flask, add 100 g of dichloroethane, raise the temperature to 60° C., start to drop 16.46 g of chloroacetyl chloride, and the dropping time is 2.5 h, then keep warm for 1 h, then cool to 15°C, add 10 g sodium ethoxi...

Embodiment 3

[0033] (1) Allyl polyether (CH 2 CHCH 2 CH 2 CH 2 OCH 2 CH 2 OH), the hydrogen-containing silicone oil (number-average molecular weight 1500) with a hydrogen content of 0.35%, is a mixed solution and toluene of 1.3: 1 with a material molar ratio, and chloroplatinic acid (5ppm) catalysts are added in the reactor, and in a nitrogen atmosphere Heat to 130°C, stir evenly, react for 5 hours, distill off toluene and low boilers at a vacuum of 0.05MPa to obtain a transparent viscous liquid that is polyether modified siloxane. The obtained polyether siloxane must be lowered at 100°C for 2 hours under a vacuum of 5mbar to ensure that its moisture content is less than 500ppm.

[0034] (2) Take 250 g of the polyether-modified siloxane obtained in step (1) in a four-necked flask, add 100 g of dichloroethane, raise the temperature to 60° C., start to drop 16.46 g of chloroacetyl chloride, and the dropping time is 2.5 h, then keep warm for 0.5h, then cool to 15°C, add 10g sodium ethox...

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PUM

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Abstract

The invention belongs to the field of organic silicon materials, and discloses a preparation method of a siloxane quaternary ammonium salt. The preparation method comprises the following steps of making allyl polyether carry out a hydrosilylation reaction with hydrogen-containing silicon oil under the action of a catalyst, so as to obtain polyether modified siloxane, afterwards, making the polyether modified siloxane carry out a reaction with chloracetyl chloride at 50 to 70 DEG C, after the reaction is completed, adding alkoxide of alkali metal and alcohol which serve as a neutralization reagent and a thinner respectively into a reaction system until the pH (potential of Hydrogen) value of the system is 8.8 to 9.5, filtering an obtained first mixture to remove a generated slat, so as to obtain acylated polyether modified siloxane, and then adding a quaternization reagent into the acylated polyether modified siloxane to carry out a quaternization reaction, removing a low-boiling-point substance, and filtering an obtained second mixture, so as to obtain the siloxane quaternary ammonium salt. According to the preparation method, the chloracetyl chloride is adopted as an acylation reagent; the alkoxide of the alkali metal is used as a neutralizer; the reaction activity is high; the condition is mild; water is not generated; side reactions are few; the yield is high; the product quality is favorable. The siloxane quaternary ammonium salt can be used as a self-emulsifying fabric softener.

Description

technical field [0001] The invention belongs to the field of organosilicon materials, and in particular relates to a preparation method of siloxane quaternary ammonium salt. Background technique [0002] Siloxane quaternary ammonium salt combines two structures of siloxane and cationic, has special conditioning properties, and can skillfully avoid the instability of siloxane and the biostimulation of quaternary ammonium salt. In terms of application characteristics, the treated fabric has the effect of smoothness, softness and antistatic property, and on the other hand, it also has antibacterial effect. Due to such structural characteristics and application characteristics, silicone quaternary ammonium salts are widely used in industries such as textile softeners, hair care and inks as a safe, non-toxic and degradable conditioner. [0003] When polysiloxane quaternary ammonium salt is synthesized, polysiloxane is generally synthesized first, and then quaternized. When synt...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/388C08G77/385C08G77/38
CPCC08G77/38C08G77/385C08G77/388
Inventor 汤仲标吴海龙雷秋芬李泽勇户献雷
Owner GUANGZHOU TINCI MATERIALS TECH
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