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Process for preparing vinylidene chloride from rectifying residual liquid of dichloroethane

A technology for producing vinylidene chloride and vinylidene chloride is applied in the field of preparation of vinylidene chloride, which can solve problems such as environmental pollution and waste of raw materials, and achieve the effects of reducing the discharge of three wastes and achieving good social and economic benefits.

Active Publication Date: 2004-12-15
SHANGHAI CHLOR ALKALI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

If the rectification raffinate is discharged into the three-waste treatment device, it will not only pollute the environment, but also cause waste of raw materials

Method used

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  • Process for preparing vinylidene chloride from rectifying residual liquid of dichloroethane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] The rectification raffinate enters the first reactor, and flows into a plurality of reactors thereafter in sequence, while the sodium hydroxide solution with a weight concentration of 15% flows into the second reactor 2 and the third reactor 3, and the reaction temperature is 80°C. The residence time is 40 minutes, and the vapor phase products of multiple reactors enter the condenser liquid collector 4 connected therewith to collect vapor phase components such as vinylidene chloride.

[0041] Components and weight percentages of the rectification raffinate include:

[0042] 1,1,2-Trichloroethane 5% (wt), 1,2-Dichloroethane 80% (wt), 1,1,2,2-Tetrachloroethane 6% (wt), Pentachloro Ethane 7% (wt), polychloride 2% (wt);

[0043] In the first and second stills, the mol ratio of 1,1,2-trichloroethane and sodium hydroxide is 1: 0.2;

[0044] The molar ratio of 1,1,2-trichloroethane to sodium hydroxide in the third reaction kettle is 1:1.1.

[0045] The conversion rate reach...

Embodiment 2

[0047] Adopt the process condition and the device of embodiment 1, wherein, residence time is 30min, and the component and weight percent content of described rectification raffinate comprise:

[0048] 1,1,2-Trichloroethane 50% (wt), 1,2-Dichloroethane 40% (wt), 1,1,2,2-Tetrachloroethane 6% (wt), Pentachloro Ethane 2% (wt), polychloride 2% (wt)

[0049] 1,1,2-Trichloroethane 5% (wt), 1,2-Dichloroethane 80% (wt), 1,1,2,2-Tetrachloroethane 6% (wt), Pentachloro Ethane 7% (wt), polychloride 2% (wt);

[0050] In the first and second stills, the mol ratio of 1,1,2-trichloroethane and sodium hydroxide is 1: 0.9;

[0051] The molar ratio of 1,1,2-trichloroethane to sodium hydroxide in the third reaction kettle is 1:1.4.

[0052] The conversion rate reached 94.5%.

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Abstract

The present invention discloses the preparation process of vinylidene chloride from dichloroethane rectifying residual liquid. The preparation process includes making the residual liquid flow successively through several serially connected reactors with sodium hydroxide solution and trichloroethane, and collecting vinylidene chloride from the gas phase product from the reactors in conventional method. The first and the second reactors have excessive trichloroethane, and the last reactor has excessive sodium hydroxide, reaction temperature of 70-90 deg.c and retaining time of 10-45 min. The said process has vinylidene chloride yield up to 90%, and can produce vinylidene chloride product and reduce environmental pollution.

Description

technical field [0001] The present invention relates to the preparation method of vinylidene chloride. Background technique [0002] Vinylidene chloride (referred to as VDC, the same below), its chemical name is 1,1-dichloroethylene, and its structural formula is CH 2 =CCl 2 , is a monomer, a colorless liquid with a special smell at room temperature, volatile and gasified. Melting point -122.5°C, boiling point 31.7°C, relative density 1.212 (20°C), refractive index 1.425 (20°C), flash point -17.8°C, autoignition point 570°C, almost insoluble in water, soluble in various organic solvents. It is mainly used in the synthesis of polymers, especially copolymers. At present, polyvinylidene chloride has yet to be developed and applied, and the demand for this product has great potential in this regard. [0003] There are many production methods for VDC. Conventional VDC is prepared by using 1,1,2-trichloroethane (1,1,2-TCE) as a raw material for alkaline removal of hydrogen chl...

Claims

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Application Information

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IPC IPC(8): C07C17/25C07C21/08
Inventor 胡妹华袁向前袁茂全谢声礼宋宏宇
Owner SHANGHAI CHLOR ALKALI CHEM
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