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Method for preparing high molecular weight polysiloxane miniemulsion with long-chain alkyl polyoxyethylene quaternary ammonium salt emulsifier

A technology of long-chain alkyl polyoxyethylene quaternary ammonium salt and polysiloxane is applied in the field of preparing high molecular weight polysiloxane miniemulsion, which can solve the problems of increased emulsion stability, increased interface film thickness, poor emulsion stability and the like , to achieve the effect of less emulsifier dosage, uniform distribution and good stability

Active Publication Date: 2017-02-15
GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Traditional cationic emulsifiers have poor emulsion stability due to their electrostatic interaction on the surface of latex particles
The current composite emulsifier system is to compound cationic emulsifiers and nonionic emulsifiers, and through the spacing arrangement of nonionic emulsifiers and cationic emulsifiers, the interval between adjacent charges becomes larger and the force is reduced; and composite emulsification The emulsifier increases the thickness of the interfacial film, which increases the stability of the emulsion, but at the same time, the composite emulsifier sacrifices the polymerization rate, slows down the reaction, and takes a long time

Method used

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  • Method for preparing high molecular weight polysiloxane miniemulsion with long-chain alkyl polyoxyethylene quaternary ammonium salt emulsifier
  • Method for preparing high molecular weight polysiloxane miniemulsion with long-chain alkyl polyoxyethylene quaternary ammonium salt emulsifier
  • Method for preparing high molecular weight polysiloxane miniemulsion with long-chain alkyl polyoxyethylene quaternary ammonium salt emulsifier

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Preparation of octadecyl polyoxyethylene (the number of oxyethylene groups (x+y) in the structure is 10) benzyl ammonium bromide:

[0045] (a) Quaternization of fatty amine polyoxyethylene: Dissolve octadecylamine polyoxyethylene ether in ethanol (the mass of octadecylamine polyoxyethylene ether and ethanol is The ratio is 1:0.5), the temperature is raised to 70°C, and the benzyl chloride solution is added dropwise at a rate of 20 drops / min (the solvent is ethanol, the mass ratio of benzyl chloride to ethanol is 1:1), and the reflux reaction is continued for 15 hours. The whole process Carried out in N2 atmosphere to obtain a reaction product; wherein, the molar ratio of benzyl chloride to stearylamine polyoxyethylene ether is 1.2:1;

[0046] (b) Purification of long-chain alkyl polyoxyethylene quaternary ammonium salt: remove the solvent in the reaction product, dry, dissolve the dried product in ethyl acetate (solvent A), and recrystallize (60°C), Redissolve in petro...

Embodiment 2

[0048] Preparation of octadecyl polyoxyethylene (the number of oxyethylene groups (x+y) in the structure is 15) benzyl ammonium chloride:

[0049] (a) Quaternization of fatty amine polyoxyethylene: Dissolve octadecylamine polyoxyethylene ether in isopropanol under stirring (150r / min) The mass ratio of propanol is 1:0.6), the temperature is raised to 82°C, and the benzyl chloride solution is added dropwise at a rate of 25 drops / min (the solvent is isopropanol, and the mass ratio of benzyl chloride to isopropanol is 0.7:1 ), the reflux reaction was continued for 26 hours, the whole process was carried out in N2 atmosphere, and the reaction product was obtained; the molar ratio of benzyl chloride to octadecylamine polyoxyethylene ether was 1.3:1;

[0050] (b) Purification of long-chain alkyl polyoxyethylene quaternary ammonium salt: remove the solvent in the reaction product, dry, dissolve the dried product in ethyl acetate (solvent A), and recrystallize (60°C), Redissolve in pe...

Embodiment 3

[0052] Preparation of cetyl polyoxyethylene (the number of oxyethylene groups (x+y) in the structure is 10) benzyl ammonium chloride:

[0053] (a) Quaternization of aliphatic amine polyoxyethylene: Dissolve hexadecylamine polyoxyethylene ether in n-propanol under stirring (350r / min) (hexadecylamine polyoxyethylene ether and n-propanol The mass ratio of propanol is 1:0.8), the temperature is raised to 100°C, and the benzyl chloride solution is added dropwise at a rate of 22 drops / min (the solvent is methanol, and the mass ratio of benzyl chloride to methanol is 0.5:1), and the reflux is continued The reaction was carried out for 10 hours, and the whole process was carried out in an N2 atmosphere to obtain a reaction product; wherein the molar ratio of benzyl chloride to hexadecylamine polyoxyethylene ether was 1.1:1;

[0054] (b) Purification of long-chain alkyl polyoxyethylene quaternary ammonium salt: remove the solvent in the reaction product, dry it, dissolve the dried prod...

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Abstract

The present invention belongs to the technical field of organic chemistry, and discloses a method for preparing a polysiloxane mini-emulsion from a long-chain alkyl polyoxyethelene quaternary ammonium salt emulsifier. The method comprises: preparing a long-chain alkyl polyoxyethelene base quaternary ammonium salt, taking 0.3-17.5 parts by mass of the quaternary ammonium salt emulsifier, dissolving into 20-500 parts by mass of water, adding 10-175 parts by mass of an organosilicon monomer, uniformly mixing, carrying out mechanical shear, homogenizing to obtain an organosiloxane monomer emulsion, taking 30-300 parts by mass of the monomer emulsion, heating to a temperature of 50-90 DEG C, stirring, adding 0.05-3 parts by mass of an alkaline initiator, carrying out a reaction for 1.5-10 h, cooling, and neutralizing to obtain the polysiloxane emulsion. According to the invention, the method has characteristics of simple process and low emulsifier consumption, and the prepared polysiloxane emulsion has characteristics of high solid content, high conversion rate, small latex particle size, good emulsion stability, high polysiloxane molecular weight and narrow molecular weight distribution, such that the polysiloxane emulsion application range is broad.

Description

technical field [0001] The invention belongs to the technical field of organic chemistry, and relates to a new application direction of long-chain alkyl polyoxyethylene quaternary ammonium salts as high-efficiency emulsifiers, in particular to a preparation of high-molecular-weight polyoxyethylene ammonium salts with long-chain alkyl polyoxyethylene quaternary ammonium salts as emulsifiers. Silicone miniemulsion method. Background technique [0002] The chemical structure of polysiloxane is -Si-O- composed of Si and O inorganic element bonds as the main chain, and organic groups such as -CH3 as side groups. This chemical structure makes polysiloxane have organic and inorganic polymers. Two aspects of properties, such as high and low temperature resistance, high elasticity, air permeability, mold release and low surface tension, make polysiloxane widely used in the fields of textile, rubber, construction, electronic appliances and cosmetics. Based on the consideration of env...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/06C08G65/00
Inventor 沈敏敏王俊凤孙淳宁翟俊菱
Owner GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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