High-yield preparation method of high-purity dimethyl diallyl ammonium chloride monomer
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A dimethyl diallyl ammonium chloride, high-yield technology, applied in the field of high-yield preparation of high-purity dimethyl diallyl ammonium chloride monomer, can solve the problem of low reaction yield and process Complicated, many process steps, etc., to achieve the effect of high purity, less impurities, and low content
Active Publication Date: 2019-03-08
SHANDONG TIANCHENG CHEM CO LTD
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However, although the process has many process steps, the process is relatively complicated and the reaction yield is low.
[0027] In summary, adopting one-step meth
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Embodiment 1
[0061] A kind of preparation method of high-purity DMDAAC monomer high yield, its step is:
[0062] Tertiary amination reaction stage: pump 141kg of 40% dimethylamine aqueous solution into a sealed and pressure-resistant reactor equipped with speed-adjustable agitator, pressure gauge, online pH meter, cooling water pipe, heating water pipe, feeding pump, and vacuum pump , circulating water to maintain the temperature in the reactor at 25°C. The reaction kettle was sealed, and the pressure in the kettle was observed with a pressure gauge, and the reaction in the tertiary amination stage was started, and the temperature was controlled at 30°C. Described feeding pump, wherein chloropropene uses a pump, dimethylamine aqueous solution and sodium hydroxide aqueous solution can use a pump
[0063] Step (1): Add 60kg of allyl chloride dropwise into the reactor, and finish adding one-third of the amount of allyl chloride dropwise within 10min-20min, control the pressure in the kettle ...
Embodiment 2
[0073] A kind of preparation method of high-purity DMDAAC monomer high yield, its step is:
[0074]Tertiary amination reaction stage: pump 141kg of 40% dimethylamine aqueous solution into a sealed and pressure-resistant reactor equipped with speed-adjustable agitator, pressure gauge, online pH meter, cooling water pipe, heating water pipe, feeding pump, and vacuum pump , circulating water to maintain the temperature in the reactor at 25°C. The reaction kettle was sealed, and the pressure in the kettle was observed with a pressure gauge, and the reaction in the tertiary amination stage was started, and the temperature was controlled at 40°C. Described feeding pump, wherein chloropropene uses a pump, dimethylamine aqueous solution and sodium hydroxide aqueous solution can use a pump
[0075] Step (1): Add 65kg of allyl chloride dropwise into the reaction kettle, and finish adding one-third of the amount of allyl chloride dropwise in 10min-20min. Under reaction 1h.
[0076] St...
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Abstract
The invention belongs to the technical field of organic synthesis, and specifically relates to a high-yield preparation method of a high-purity dimethyl diallyl ammonium chloride monomer. According tothe preparation method provided by the invention, a segmented type chloropropene and sodium hydroxide solution alternative and dropwise adding method is adopted, the most suitable alternative and dropwise adding amount and the most suitable reaction time of the chloropropene and the sodium hydroxide solution can be found through a large amount of small-scale tests and by adopting an acid-base indicator, the chloropropene can be prevented from being located in strong base environment, a large amount of byproducts such as allyl alcohol can be effectively prevented from being generated, the utilization rate of the chloropropene can be effectively increased, and by adopting a pressure-proof closed reaction kettle, dimethylamine is enabled not to leak and can completely take part in reaction.A dimethyl diallyl ammonium chloride monomer solution obtained through the preparation method is light in color and less in impurities, activated carbon is not used for decoloring and removing the impurities, the purity is high, the contents of amine salt and chlorine ions are extremely low, the yield is approximate to ideal value, a product is used for homopolymerization experiments, a colorless,transparent and clear polymer solution is obtained, and the viscosity and the molecular weight of the colorless, transparent and clear polymer solution are far higher than those of like products.
Description
technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a high-yield preparation method of high-purity dimethyl diallyl ammonium chloride monomer. Background technique [0002] Dimethyl diallyl ammonium chloride (DMDAAC for short) monomer is a cationic monomer with a wide range of uses. There are two unsaturated double bonds and quaternary ammonium groups in the molecular structure, and it can be copolymerized with many unsaturated monomers. It is positively charged in aqueous solution to form cationic or zwitterionic polymers. It is mainly used to synthesize water-soluble polymers containing organic cations, which can improve the water solubility of polymers, solution rheology, increase adsorption capacity and bactericidal ability, etc. Its copolymers are widely used in water treatment, petroleum exploration, textile printing and dyeing, daily chemical industry and other fields. [0003] The synthesis of DMDAAC...
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