The method of producing epichlorohydrin

 

(57) Abstract:

The invention relates to techniques for the production of oxides of galeolaria the dehydrochlorination haloesters alcohols and can be used in the production of epichlorohydrin. In the method of producing epichlorohydrin by dehydrochlorination of dichlorohydrin glycerin sodium hydroxide using anhydrous dichlorohydrin glycerin, alkali concentration of 25-30%, the process is conducted at a temperature of 55-77oC and a reduced pressure of 0.6-0.7 ATM. The technical result - the reduction of wastewater. 1 Il.

The invention relates to techniques for the production of oxides halogen-olefins by dehydrochlorination haloesters alcohols and can be used in the chemical industry in the production of epichlorohydrin and synthetic glycerin.

Well-known and widely used in industry in the method of producing epichlorohydrin (EPG) by dehydrochlorination 2-5-percentage aqueous solutions of dichlorohydrin glycerol (GHG) water sustancia calcium hydroxide. The main disadvantage of this method is the large number of wastewater from 50 to 100 tons per tonne EPG contaminated mineral, organic and chlorinated organic impurities, purification of which ve is isdi wastewater such production equals and even exceeds the cost of the equipment itself the production EPG. Great and operational costs of such cleanup.

In industry, this method of obtaining EPG goes in two stages: first, from allyl chloride and hypochlorous acid to obtain an aqueous solution DHG, and the second is the resulting aqueous solution is treated with an alkaline agent and received EPG allocate distillation. Thus process water from both stages is summarized and is contaminated by the products of both reactions.

There are several patented at different times of the attempts to reduce the amount of wastewater, limited mainly to increasing concentrations of solutions DHG and alkaline agents, which should thus reduce the amount of waste water. However this way met serious obstacles: reduce yields of target products and malaysiensis quantity and composition of the contaminants in the wastewater. For these reasons, these attempts have not been implemented in practice.

Closest to the present invention is a method of producing epichlorohydrin, in which 4-5% aqueous solution of dichlorohydrin glycerol is subjected to dehydrochlorination aqueous solutions of calcium hydroxide (lime milk) or sodium hydroxide (caustic soda) with concentrational agent 1,1-1,12 (L. A. Oshin. Production of synthetic glycerin, M.: Chemistry, 1974, page 105).

The disadvantage of this method is the large number of sewage.

The present invention is to develop a practically closed method of producing epichlorohydrin.

The task is solved in that the proposed method of producing epichlorohydrin by dehydrochlorination of dichlorohydrin glycerin sodium hydroxide, which is used anhydrous dichlorohydrin glycerol, the concentration of alkali 25-30%, and the process is conducted at a temperature of 55-77oC and a reduced pressure of 0.6-0.7 ATM.

The essence of the proposed method is illustrated by a drawing.

In the reactor R-1 do: anhydrous DHG and 25-30% solution of sodium hydroxide. When the temperature 55-77oWith a residual pressure of 0.6-0.7 ATM formed EPG Argonauts with water in the form of azeotropic mixtures, vapours which condense in K-2 and the fluid is stratified. Water containing 7-8% EPG, is returned to the reactor and concentrated EPG containing up to 2% of water and other impurities is supplied to the cleaning method of rectification. From a bottom part of the reactor output water containing 20-22% sodium chloride and small amounts of organic primecap can be used in the production of chlorine and in this case, the production of epichlorohydrin is almost closed.

EXAMPLE. 654 g of anhydrous GHG mixed with an aqueous solution of sodium hydroxide, the concentration of 28%, in a molar ratio of 1:1. The time of reaction and distillation, azeotropic mixtures DHG + water - 10 minutes With the resulting 438,5 g EPG, the output of which was 93.5%. VAT residue obtained 1312 g containing sodium chloride and 22.6%, glycerin 0.2% and traces DHG and EPG, and it can be used as raw materials in the electrolysis to obtain chlorine.

Thus, in comparison with the prototype, the proposed method has the main advantage that there are no contaminated process waters, requiring expensive clean-up, the yield of the target product of epichlorohydrin is not reduced.

The method of producing epichlorohydrin by dehydrochlorination of dichlorohydrin glycerin sodium hydroxide, characterized in that use anhydrous dichlorohydrin glycerol, the concentration of alkali 25-30%, and the process is conducted at a temperature of 55-77oC and a reduced pressure of 0.6-0.7 ATM.

 

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3 tbl, 3 ex

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3 cl, 3 tbl, 6 ex

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15 cl, 4 ex, 3 tbl

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20 cl, 6 ex, 5 tbl

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