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Method for preparing epoxy chloropropane

A technology of epichlorohydrin and calcium hydroxide, which is applied in the direction of alkali metal chloride, calcium/strontium/barium chloride, calcium/strontium/barium halide, etc., which can solve the problem of large amount of organic solvent, large environmental pollution, and raw material High cost and other problems, to achieve the effects of easy separation, low environmental pollution, and high yield of the product epichlorohydrin

Inactive Publication Date: 2018-05-01
JIANGSU SOPO GRP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process is more complicated, the cost of raw materials is higher, the amount of organic solvent is large, and the pollution to the environment is greater

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Take by weighing 29.5 g calcium hydroxide, 2 g sodium hydroxide and 70 g water and mix and stir to form soda-lime milk, for subsequent use;

[0021] Put 100 g of the crude glycerin chlorination product in an ice-water bath, under stirring, add milk of soda lime in batches to prevent the exothermic acid-base reaction. Slowly heat up to 20°C and keep it warm for 1 h. After the saponification reaction, let stand and cool to obtain reaction solution A; filter reaction solution A under reduced pressure, adjust the pH of the filtrate to neutral with hydrochloric acid, and then distill under reduced pressure to obtain Solution of epichlorohydrin and isolated solid;

[0022] The results show that the conversion rate of dichloropropanol is 99.2%, and the yield of epichlorohydrin is 97.4%;

[0023] Dissolve the separated solid in hot distilled water, filter while hot, cool the filtrate to crystallize, filter the cooled filtrate, and dry the crystal to obtain NaCl and CaCl 2 Mix...

Embodiment 2

[0025] Take by weighing 29.5 g calcium hydroxide, 5 g sodium hydroxide and 70 g water and mix and stir to form soda lime milk, for subsequent use;

[0026] Put 100 g of the crude glycerin chlorination product in an ice-water bath, add soda-lime milk in batches under stirring, to prevent the exothermic acid-base reaction, the temperature of the reaction solution suddenly rises, first keep it at 0-5 °C for 0.5 h, then Slowly heat up to 15°C and keep it warm for 2 hours. After the saponification reaction, let stand and cool to obtain reaction solution A; filter reaction solution A under reduced pressure, adjust the pH of the filtrate to neutral with hydrochloric acid, and then distill under reduced pressure to obtain Solution of epichlorohydrin and isolated solid;

[0027] The result shows that dichloropropanol conversion rate is 99.9%, and epichlorohydrin yield is 98.5%;

[0028] Dissolve the separated solid in hot distilled water, filter while hot, cool the filtrate to crystal...

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PUM

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Abstract

The invention relates to a method for preparing epoxy chloropropane, and belongs to the technical field of organic synthesis. The method comprises the following steps: (1) weighing calcium hydroxide and sodium hydroxide, mixing the weighed calcium hydroxide and sodium hydroxide with water, and carrying out stirring for forming a soda lime emulsion for later use, wherein the mass of the water is 200-400% of the mass of the calcium hydroxide, and the mass of the sodium hydroxide is 3-18% of the calcium hydroxide; (2) placing a crude glycerol chlorination crude product in an ice water bath, adding the soda lime emulsion prepared in the step (1) while stirring, keeping the temperature at 0-5 DEG C for 0.5-1 hour firstly, then carrying out heating slowly to a reaction temperature, carrying outstanding after saponification is completed, carrying out cooling and reduced pressure suction filtration, regulating the pH value to neutral, and carrying out reduced pressure distillation to obtain asolution containing epoxy chloropropane and a separated solid. The method provided by the invention has cheap raw materials and simple operation process, the obtained product is easily separated, andthus the method has an industrial value.

Description

technical field [0001] The invention relates to a method for preparing epichlorohydrin, belonging to the technical field of organic synthesis. Background technique [0002] Epichlorohydrin, whose chemical name is 3-chloro-1,2-propylene oxide, is a volatile, unstable, colorless liquid with a pungent odor similar to chloroform and ether. Epichlorohydrin is slightly soluble in water, miscible with a variety of organic solvents, and can form azeotropes with a variety of organic liquids. As a very important organic chemical raw material and fine chemical product, epichlorohydrin is widely used in the production of epoxy resin, synthetic glycerin, epichlorohydrin rubber and other fine chemical products. These products are widely used in chemical industry, transportation , medicine, electronic appliances and other fields. In addition, epichlorohydrin can also be used to synthesize nitroglycerin explosives, glass fiber reinforced plastics, electrical insulation products, surfactan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D301/26C07D303/08C01D3/04C01F11/24
CPCC01D3/04C01F11/24C07D301/26C07D303/08
Inventor 朱桂生殷恒波凌荣春邵守言刘玲马克和唐丽黄诚
Owner JIANGSU SOPO GRP
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