A kind of 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-purity dimethyl diallyl ammonium chloride monomer high-yield preparation, can solve the problem of low reaction yield and process Complicated, many process steps, etc., to achieve the effect of low content, less impurities and high purity
Active Publication Date: 2020-08-04
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 method and two-step method synthetic technique all have its deficiency, all can not obtain the dimethyl diallyl ammonium chloride monomer of high purity and high yield
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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 present invention belongs to the technical field of organic synthesis, and particularly relates to a method for preparing a high purity dimethyl diallyl ammonium chloride monomer in high yield. The preparation method provided by the present invention involves stagewise and alternating addition of allyl chloride and sodium hydroxide solution dropwise, the optimum alternate addition amounts and reaction times of allyl chloride and sodium hydroxide being determined using an acid-base indicator through extensive tests. The preparation method prevents allyl chloride from being present in a highly alkaline environment, which avoids generation of byproducts such as allyl alcohol in large amounts, and increases the utilization rate of allyl chloride. Further, the preparation method employs a pressure-resistant closed reaction vessel to ensure that dimethylamine does not leak and can participate completely in the reaction. The dimethyl diallyl ammonium chloride monomer solution obtained by the preparation method has a light color and few impurities, does not require decoloration and impurity removal with activated carbon, and has a high purity, has very low contents of amine salts and chlorine ions, and a yield approximate to an ideal value. Use of the product in a homopolymerization experiment affords a colorless, transparent and clear polymer solution, with the viscosity and molecular weight thereof being far superior to 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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