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Preparation processes of chlorine oil and trichloracetic aldehyde

A preparation process, a technology for trichloroacetaldehyde, applied in the directions of oxidative preparation of carbonyl compounds, electrolysis process, organic chemistry, etc., can solve the problem of increasing the impurity content in the finished product of trichloroacetaldehyde, hindering the complete chlorination of ethanol raw materials, yield and quality Increase difficulties and other problems to achieve good social and environmental protection benefits, protect the natural ecological environment, and reduce production costs

Inactive Publication Date: 2021-06-29
王剑
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

And domestic generally take ethanol as raw material, carry out continuous chlorination in step type or tower type equipment, do not use catalyst in the reaction process, thus produce chloral (100%), consume 95% ethanol per ton up to 500~560kg, Chloral yield is only about 58.6~65.6% (its theoretical consumption 95% ethanol 328kg)
[0004] At present, the technical process of domestic production of chloral is still relatively backward, and industry associations have organized domestic manufacturers many times to work together, prepare funds and technology, and work hard to tackle key problems. The yield has increased from 49% in the past to 65%, and the technology is advancing. A big step forward, but there is still a big gap from the theoretical yield
Its reason is: in the reaction process of existing chloral production process, inevitably produce a large amount of ethyl chloride by-products, also contain not chlorinated complete monochloroacetaldehyde, dichlorohydrate acetaldehyde, Chloroacetaldehyde hemiacetal, semi-intermediates such as dichloroacetaldehyde hemiacetal, the existing chloral process has greatly hindered the chlorination of ethanol raw material completely, increased the content of impurity in the chloral finished product, to It is difficult to increase the yield and quality of subsequent products such as trichlorfon
[0005] It can be seen that ethanol will inevitably produce hydrogen chloride in the process of chlorination, and hydrogen chloride will continue to react with ethanol to generate ethyl chloride, which is the main reason for the lower yield. The difficulty in solving this problem is that hydrogen chloride and ethanol cannot be avoided in the system. reaction, and the hydrogen chloride cannot be completely removed in the system, and can only be absorbed by water in the chlorination tail gas to generate hydrochloric acid in the later stage

Method used

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  • Preparation processes of chlorine oil and trichloracetic aldehyde
  • Preparation processes of chlorine oil and trichloracetic aldehyde

Examples

Experimental program
Comparison scheme
Effect test

no. 1 example

[0034] refer to figure 1 , a preparation process of chlorine oil, comprising the steps of:

[0035] (1) Check whether the gas source valve of the chlorine regulating valve and the shut-off valve is open, and confirm on site whether the DCS manually opens the regulating valve and the shut-off valve, and whether the opening is consistent with the DCS display; after the inspection, open the inlet valve of the ethanol pump, Start the ethanol pump, open the outlet valve, pour ethanol into the ethanol high level tank, and stop the pump in time when the liquid level of the ethanol high level tank is 5 tons.

[0036] (2) Turn on the dilute hydrochloric acid pump, adjust the rotameter to control the flow of dilute hydrochloric acid at 400L / h as required, enter the falling film absorber and packed tower, check whether the flow of the falling film absorber and packed tower is normal; turn on the lye circulating pump , adjust the lye flow at 20m 3 / h.

[0037] (3) Open the tail gas val...

no. 2 example

[0054] refer to figure 1 , a preparation process of chlorine oil, comprising the steps of:

[0055] (1) Check whether the gas source valve of the chlorine regulating valve and the shut-off valve is open, and confirm on site whether the DCS manually opens the regulating valve and the shut-off valve, and whether the opening is consistent with the DCS display; after the inspection, open the inlet valve of the ethanol pump, Start the ethanol pump, open the outlet valve, and inject the ethanol into the ethanol high tank. Stop the pump in time when the liquid level of the ethanol high level tank is 5 tons.

[0056] (2) Turn on the dilute hydrochloric acid pump, adjust the rotameter to control the flow of dilute hydrochloric acid at 400L / h as required, enter the falling film absorber and packed tower, check whether the flow of the falling film absorber and packed tower is normal; turn on the lye circulating pump , adjust the lye flow at 20m 3 / h.

[0057] (3) Open the tail gas va...

no. 3 example

[0074] refer tofigure 1 , a preparation process of chlorine oil, comprising the steps of:

[0075] (1) Check whether the gas source valve of the chlorine regulating valve and the shut-off valve is open, and confirm on site whether the DCS manually opens the regulating valve and the shut-off valve, and whether the opening is consistent with the DCS display; after the inspection, open the inlet valve of the ethanol pump, Start the ethanol pump, open the outlet valve, and inject the ethanol into the ethanol high tank. Stop the pump in time when the liquid level of the ethanol high level tank is 5 tons.

[0076] (2) Turn on the dilute hydrochloric acid pump, adjust the rotameter to control the flow of dilute hydrochloric acid at 400L / h as required, enter the falling film absorber and packed tower, check whether the flow of the falling film absorber and packed tower is normal; turn on the lye circulating pump , adjust the lye flow at 20m 3 / h.

[0077] (3) Open the tail gas valv...

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Abstract

The invention relates to the technical field of trichloracetic aldehyde, in particular to preparation processes of chlorine oil and trichloracetic aldehyde. The preparation process of the chlorine oil comprises the following steps: (1) in stepped or tower-type equipment, adding an electrode in a high-position kettle, and installing a long-wave ultraviolet lamp in each reaction kettle; and (2) electrifying the electrode, turning on the ultraviolet lamps, adding ethanol or acetaldehyde from the high-position kettle, adding chlorine from a low-position kettle, and collecting the generated chlorine oil. The preparation process of the trichloracetic aldehyde comprises the following steps: adding the chlorine oil and concentrated sulfuric acid into a distillation kettle in proportion, carrying out heating and refluxing, then performing distilling and dehydrating, and collecting the trichloracetic aldehyde. According to the processes, hydrogen chloride is removed by electrolyzing the hydrogen chloride in a system, so the hydrogen chloride generated in the system can be effectively removed, and the reaction of the hydrogen chloride with ethanol is reduced or even avoided; and thus, chloroethane gas is reduced or even not generated, the consumption of ethanol and chlorine is greatly reduced, and production cost is remarkably reduced.

Description

technical field [0001] The invention relates to the technical field of trichloroacetaldehyde, in particular to a preparation process of chlorine oil and trichloroacetaldehyde. Background technique [0002] The following content in the background technology only refers to the information related to the present invention understood by the inventor, and aims to increase the understanding of the present invention by explaining some basic technical knowledge related to the present invention. Knowledge known to those of ordinary skill in the art. [0003] Currently, there are only two processes for the production of chloral, ethanol chlorination and acetaldehyde chlorination. In foreign countries, the acetaldehyde chlorination method is generally the main route, and antimony trioxide (SbO 3 ), antimony trichloride (SbCl 3 ) etc. as catalysts, the yield of chloral is about 72-80%. And domestic generally take ethanol as raw material, carry out continuous chlorination in step typ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B3/11C25B3/07C25B3/27C07C47/16C07C45/29
CPCC07C45/29C07C47/16
Inventor 王健
Owner 王剑