Production method of polyquaternium-10
The technology of a polyquaternium salt and a production method, which is applied in the production field of polyquaternium-10, can solve the problems of difficulty in improving the purity of the process, uneven cation replacement, poor product quality, etc., and achieves uniform cation replacement and appearance. White, strong adsorption effect
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Embodiment 1
[0035] A kind of production method of polyquaternium-10 production etherification agent, comprises the following steps:
[0036] (1) Pass epichlorohydrin into the synthesis kettle, start stirring, and pass into gaseous phase trimethylamine to react to generate cationic etherification agent ETA, trimethylamine: epichlorohydrin is 1:1, in terms of molar ratio, the temperature is 4 ℃, pH 9.5, pressure less than 0.1Mpa, after 5 hours of reaction, keep warm for 1 hour;
[0037] (2) Suction filtration to separate the reaction mother liquor to obtain a solid product, wash with butyl ether or diethyl ether at 5°C, the mass ratio of cationic etherification agent ETA to detergent is 1:4, until the residue detected by gas chromatography is <0.05% until;
[0038] (3) Dry at -0.06Mpa vacuum at 20°C for 60 minutes;
[0039] (4) Refining in the gel kettle, vacuum filtering the gas at -0.08Mpa, the temperature is 30°C, the stirring speed is 50r / min, and the time is 3 hours, to obtain the ca...
Embodiment 2
[0051] A kind of production method of polyquaternium-10 production etherification agent, comprises the following steps:
[0052] (1) Pass epichlorohydrin into the synthesis kettle, start stirring, and pass into gaseous phase trimethylamine to react to generate cationic etherification agent ETA. Trimethylamine: epichlorohydrin is 1: 1.2, in terms of molar ratio, and the temperature is 15 ℃, pH is 7.3, pressure is less than 0.1Mpa, after 2 hours of reaction, keep warm for 2 hours;
[0053] (2) Suction filtration to separate the reaction mother liquor to obtain a solid product, wash with butyl ether or diethyl ether at 20°C, the mass ratio of cationic etherification agent ETA to detergent is 1:10, until the residue detected by gas chromatography is <0.05% until;
[0054] (3) Dry at -0.08Mpa vacuum at 30°C for 20 minutes;
[0055] (4) Refining in the gel kettle, vacuum filtering the gas at -0.1Mpa, the temperature is 50°C, the stirring speed is 50r / min, and the time is 2 hours, ...
Embodiment 3
[0067] A kind of production method of polyquaternium-10 production etherification agent, comprises the following steps:
[0068] (1) Put epichlorohydrin into the synthesis kettle, start stirring, and pass into the gaseous phase trimethylamine to react to generate cationic etherification agent ETA. The ratio of trimethylamine: epichlorohydrin is 1:1.1, in terms of molar ratio, and the temperature is 8 ℃, pH 8.5, pressure less than 0.1Mpa, after 3 hours of reaction, keep warm for 1.6 hours;
[0069] (2) Suction filtration to separate the reaction mother liquor to obtain a solid product, wash with butyl ether or diethyl ether at 15°C, the mass ratio of cationic etherification agent ETA to detergent is 1:7, until the residue detected by gas chromatography is <0.05% until;
[0070] (3) Dry at -0.07Mpa vacuum at 25°C for 30 minutes;
[0071] (4) Refining in the gel kettle, vacuum filtering the gas at -0.095Mpa, the temperature is 40°C, the stirring speed is 45r / min, and the time i...
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