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Method For The Synthesis Of Epichlorohydrin

Shandong Minji Chemical Co.,Ltd | Updated: Jul 17, 2017

Table Chloro Alcohol chemical name is 1-chloro 2, 3-propylene oxide, molecular type C3H5OCL, molecular weight 92.85, is a volatile, unstable colorless liquid, with chloroform, ether similar irritant odor, density 1.1806g/cm3, Boiling 115.2 ℃, solidification Point-57.2 ℃, refractive index (ND20) 1.4382, Flash Point (Open Cup) 40.6 ℃, spontaneous ignition point 415 ℃, slightly soluble in water, can be mixed with a variety of organic solvents, Epi+D13:K14chlorohydrin with a variety of organic liquids to form azeotrope.

Table Chloro-Alcohol is an important organic chemical raw materials and fine chemicals consumption of chlorine products, mainly used in the production of epoxy resin, synthetic glycerin, chlorine alcohol rubber and other fine chemical products, Epi+D13:K14chlorohydrin and these products are widely used in chemical industry, light industry, transportation, medicine, electronic and electrical appliances and other fields.

Table Chloro Alcohol synthesis method and process:

1. The mixed acid was synthesized in the esterification reaction unit with mixed acid 198g, methanol 192g, toluene 120g, sodium hydrogen sulfate 9. 9g, equipped with mixing device, water separator, condenser tube, temperature control instrument, etc., heating so that mixed acid dissolved, stirring reaction, temperature of 74 ℃ began to water. The water produced in the reaction process and the two-element constant boiling material formed by toluene are steamed out from the system, and the water is left in the water by the condensation of toluene back to the reaction body yarn. Epi+D13:K14chlorohydrin After the reaction is finished, the solvent is distilled, and then the decompression distillation is collected 0. 74mpal20~180℃ fractions, mixed methyl esters (dimethyl butadiene, dimethyl valerate, dimethyl adipate) were obtained.

2. Mixed methyl ester with two vinyl amine reaction in an electric stirrer, thermometer, condenser 250mL three-port bottle, add two ethylene amine 36g, 55g mixed methyl ester, began to stir, 10min observed after the temperature rose to 47 ℃, began to heat, the color of the reactants changed, yellow → orange → amber. When the material temperature of 120 ℃: Around, can be seen in the lower end of the condenser condensate droplets, Epi+D13:K14chlorohydrin reaction temperature is l50~160℃, reaction 3h, the temperature will rise to 180 ℃, reaction 30min, the reaction ended. Cooling the material to 60 ℃, adding 68g water, stirring evenly, the product is amber, transparent viscous liquid, that is, Epi+D13:K14chlorohydrin poly amide polyamine, the mass fraction is 50%, the viscosity is 0. 55~o. 9pa· S (25 ℃).

3. The synthesis of poly-amide polyurethane resin was installed on the 250mL four-port reaction bottle, respectively, with electric stirrer, drip funnel, thermometer, condenser and poly amide polyamine 25. 9g (mass fraction 50%), distilled water 80g, stirring evenly, the temperature rises to 28 ℃, starts to drip adds the table chlorine alcohol, in the 30min about will this drop adds completes, Epi+D13:K14chlorohydrin then starts to heat up, the temperature maintains in the 73~75℃, the reaction 4h, drops down to the room temperature, supplements with the 25g distillate amide amine table chlorine alcohol abbreviation MPPE-1, the quality score is 12. About 5%. Viscosity in 0. 03~0. 09pa· The mass density of s (25 ℃) is 1. 03G/ML (25 ℃).

Optimum process conditions the molar ratio of ester to amine in 1: (1). 05~1. 1), the reaction time 3h, can get the viscosity of 0. 7~1 1pa· Intermediate products of S (25 ℃); mixed polyamide polyamine: $number. 6:1, the reaction temperature is 73~75℃, the reaction is relatively mild, and the viscosity is easy to control.


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