Method for separating oil-phase dichloropropanol from mixed aqueous solution of dichloropropanol and chlorine hydride

A technology of dichloropropanol and mixed solution, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of hydroxyl compounds, etc., can solve problems such as increased equipment investment, difficulty in decanting, increased cost, etc., and can increase the amount of three wastes treated , Separation operation is simple, the effect of occupying less land

Active Publication Date: 2012-03-28
CHINA TIANCHEN ENG +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0013] The extraction method requires additional solvents, and more equipment is invested. It is necessary to increase equipment such as multi-stage extraction towers, and the extraction process needs to be equipped with a series of equipment such as extractant distillation and separation towers, which increases equipment investment; Contaminated liquids such as chlorinated alkanes, esters, ethers, etc. are easy to leak during the production process, resulting in residual pollution in saponification wastewater or low boiling substances, which increases the cost of production
[0014] Although the separation of dichloropropanol pseudo-azeotrope by decantation is simple to operate, it is difficult to realize the operation due to the different composition of dichloropropanol, water and hydrogen chloride mixture after the reaction, which may easily lead to difficulties in decantation.

Method used

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  • Method for separating oil-phase dichloropropanol from mixed aqueous solution of dichloropropanol and chlorine hydride

Examples

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Embodiment 1

[0034] A method for separating dichloropropanol oil phase from dichloropropanol hydrogen chloride mixed aqueous solution, comprising the steps:

[0035] (1) the dichloropropanol hydrogen chloride mixed aqueous solution that produces after the completion of the glycerol chlorination reaction of 10kg is put into the reactor (dichloropropanol hydrogen chloride mixed aqueous solution comprises the water of 53% weight, the 1,3 dichloropropanol of 33% weight Chloropropanol and 14% weight hydrogen chloride), the calcium chloride of 1.3kg is joined in the reactor, mixes and obtains the mixed solution containing calcium chloride;

[0036] (2) Heat the mixed solution containing calcium chloride to 130°C and stir for 5 hours. Hydrogen chloride, water and a small amount of dichloropropanol escape continuously in the reactor, and the oil phase and water phase of dichloropropanol are decanted and analyzed. layer, the water phase containing calcium chloride is sent to the drying section for ...

Embodiment 2

[0038] A method for separating dichloropropanol oil phase from dichloropropanol hydrogen chloride mixed aqueous solution, comprising the steps:

[0039] (1) put the dichloropropanol hydrogen chloride mixed aqueous solution that ferric trichloride and chloropropene method reaction finishes to produce in the reactor and mix to obtain the mixed solution that contains ferric chloride; After concentration, ferric chloride and dichlorohydrin The weight ratio of the mixed aqueous solution of chloropropanol and hydrogen chloride is 1:99; (after testing: the mixed aqueous solution of dichloropropanol and hydrogen chloride includes 73% by weight of water, 15% by weight of 1,3 dichloropropanol and 12% by weight of hydrogen chloride)

[0040] (2) Heat the mixed solution containing ferric chloride to 200° C., and stir for 8 hours under full vacuum to separate the dichloropropanol oil phase from the mixed solution.

Embodiment 3

[0042] A method for separating dichloropropanol oil phase from dichloropropanol hydrogen chloride mixed aqueous solution, comprising the steps:

[0043](1) Potassium bromide and propylene acetate method dichloropropanol hydrogen chloride mixed aqueous solution are put into the reactor and mixed to obtain a mixed solution containing potassium bromide; the weight ratio of potassium bromide and dichloropropanol hydrogen chloride mixed aqueous solution is 60 : 40; (through testing: dichloropropanol hydrogen chloride mixed aqueous solution comprises the water of 57% by weight, the 1 of 30% by weight, the hydrogen chloride of 3 dichloropropanol and 13% by weight)

[0044] (2) The mixed solution containing potassium bromide was mechanically stirred for 10 h under the conditions of 20° C. and 100 KPa gauge pressure, so that the dichloropropanol oil phase was separated from the mixed solution.

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Abstract

The invention discloses a method for separating oil-phase dichloropropanol from a mixed aqueous solution of dichloropropanol and chlorine hydride, which comprises the following steps of: mixing a metal halide with the mixed aqueous solution of dichloropropanol and chlorine hydride to obtain a metal halide-contained mixed solution; and carrying out mechanical agitation for 0.5-10 hours under the condition of heating or evaporation or rectification on the metal halide-contained mixed solution, so as to separate the oil-phase dichloropropanol from the mixed solution. According to the method disclosed by the invention, the principle of salt effect is utilized, the azeotropic point of the existing mixed aqueous solution of dichloropropanol and chlorine hydride is broken through adding the metal halide, so that the separation of the mixed aqueous solution of dichloropropanol and chlorine hydride is realized; and further, the metal halide is recycled, and thus, the handling capacity of three wastes is not increased. The investment on the whole device is little, the occupation of land is little, and the operation for separating dichloropropanol is simple.

Description

technical field [0001] The invention belongs to the field of production of epichlorohydrin and dichloropropanol, in particular to a method for separating dichloropropanol oil phase from dichloropropanol hydrogen chloride mixed aqueous solution. Background technique [0002] Epichlorohydrin (alias epichlorohydrin), the chemical name is 1-chloro-2,3-epoxypropane, and the molecular formula is C 3 h 5 OCl, with a boiling point of 115.2°C and a freezing point of -57.2°C, is a volatile and unstable colorless liquid, slightly soluble in water and miscible with various organic solvents. [0003] Epichlorohydrin is an important organic chemical raw material and fine chemical product. It is a large variety of propylene derivatives. It is mainly used in the synthesis of glycerin, epoxy resin, epichlorohydrin rubber, nitroglycerin explosives, etc. It can also be used It is used as a solvent for cellulose esters, resins and cellulose ethers; it is also the main raw material for the pro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/36C07C29/80
Inventor 杨克俭王国亮赵敏伟任君王志远陈剑波李荣罗汉金梁军湘张红梅袁学民周明生
Owner CHINA TIANCHEN ENG
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