The method of purification of ethyl chloride

 

(57) Abstract:

The invention relates to the purification of ethyl chloride. Chloride ethyl, obtained by catalytic hydrochloridebuy ethylene in the liquid phase in the presence of aluminium chloride, purified from aluminum chloride by the method of single distillation with obtaining VAT residue containing 5-35 wt.% aluminum chloride, which is mixed with kubovy the residue obtained during the distillation purification of ethyl chloride from viscida impurities, at mass ratio of 1:0,52,5 respectively. After separation of the ethyl chloride the mixture is treated with water at a mass ratio of the mixture bottoms: water of 1:1-2, and separated by settling on the organic and aqueous phase. The technical result is an increase in the yield of ethylchloride.

The invention relates to a method of purification of ethyl chloride, obtained by catalytic hydrochloridebuy ethylene in the liquid phase in the presence of aluminum chloride (AlCl3), and can be used in industrial organic synthesis.

A known method of purification of ethyl chloride raw, containing AlCl3in the amount of 0.2-0.5 wt.%, as well as above - and nukiyama compounds such is Oromo chloride ethyl-raw comes in a cube column neutralization, irrigated 10% alkali solution, and is exempt from AlCl3and hydrogen chloride. Wet pair ethyl chloride raw fed to the dehydration of concentrated (92-95%) sulfuric acid, and then ethyl chloride is subjected to distillation purification from viscida impurities (Industrial organochlorine products. The Handbook. Under.ed. L. A. Osina. M , Chemistry, 1978, S. 50). This method has several disadvantages: the use of alkali and acid leads to additional costs, to the formation of large amounts of wastewater, there is considerable corrosion of the equipment. In addition, the resulting product has a sufficiently high acidity and contains impurities that are made of sulfuric acid, deteriorating its quality.

The closest in technical essence and the achieved result is a method of purification of ethyl chloride, obtained by catalytic hydrochloridebuy ethylene in the liquid phase in the presence of AlCl3(0.2 to 0.5 wt.%), at a temperature of 0 to minus 10o(Ed. mon. 335923 C 07 C 7/00, 1969) In this method, chloride ethyl-raw cleanse from catalyst AS3using the gradual distillation in an evaporator at a temperature not exceeding 35oC, to obtain the cubic mod synthesis as a catalyst. Catalytic activity support it by adding fresh AlCl3. Pair ethyl chloride is further clear from the following and wyskida impurities using rectification. Distillation residues obtained in the purification of ethyl chloride from viscida impurities, proceed to burning. This method has the following main disadvantages. Gradual distillation, a high residence time and circulation VAT residue from concentration of the catalyst is AlCl3no higher than 6-7% lead to accumulation viscida impurities in chloride-ethyl-raw and result in rapid loss of catalytic activity recirculated VAT residue. Add the fresh catalyst is AlCl3quickly passivated in this mass as a result of interaction with wysokiej impurities and formation of oligomeric compounds with ethyl chloride. According to the method, the yield of the target ethyl chloride is 80% due to losses as formed above and nukiyama impurities - products of the conversion of ethyl chloride, detachable next distillation purification.

The present invention allows to increase the yield of the target product and to solve the problem of processing bottoms, SIA, obtained by catalytic hydrochloridebuy ethylene in the liquid phase in the presence of lCl3carry out the method of a single distillation with obtaining VAT residue containing 5-35 wt.% AlCl3that mixed with kubovy the residue obtained during the distillation purification of ethyl chloride from viscida impurities, at mass ratio of 1:0,52,5 respectively, and after separation of ethyl chloride, the mixture is treated with water at a mass ratio of the mixture bottoms : water 1:12 and separated by settling on the organic and aqueous phase.

VAT residue generated in terms of a single distillation ethyl chloride raw and containing 5-35 wt.% AlCl3is not more than 0.06 wt. hours from the original ethyl chloride raw. Its exclusion from the technological cycle of synthesis and purification the main mass of ethyl chloride increases the yield of the target product more 96,0% instead of 80% of the prototype, and also provides high stability of the technological process as a whole. Department All3by a single distillation provides a sharp decline in thermochemical transformations due to the small residence time of ethyl chloride raw in the heating zone, which bring the interval of concentrations AlCl3as residue complicated technology of its processing. In the case of increasing the concentration of AlCl3more 35,0% VAT residue strongly osmoses loses fluidity, are formed in the side impurities, reducing the quality of ethyl chloride, and there are insurmountable difficulties in the further processing. A mixture of still bottoms resulting from a single distillation and rectification, at mass ratio of 1:0,52,5 accordingly allows to extract the contained ethyl chloride, for example, by distillation, and attach it to the main stream ethyl chloride, coming to a distillation treatment. Subsequent decomposition of the mixture of still residue with water at a mass ratio of the mixture bottoms : water 1:12 provides translation AlCl3in an aqueous solution of aluminium oxychloride containing traces of organic substances. This solution can be used for different purpose, for example as a coagulant wastewater chemical industries.

Example 1. Chloride ethyl-raw, obtained in industrial conditions by hydrochloridebuy ethylene in the liquid phase, in the presence of AlCl3with composition, wt.%: AlCl3- 0,29; hydrogen chloride - 0,76; the tion, within 24 h, with an average load 1037 kg/h served in the lower part of the tubular graphite evaporator, where the separation AlCl3by a single distillation. From the upper part of the evaporator vapor-liquid mixture enters the separator. VAT residue, containing, wt.%: ll3to 5.0, chloride ethyl - 80,0; high-boiling chlorinated organic compounds to 8.3; polymers - 6,7 60 kg/h, is removed from the separator in the collection. Chloride ethyl-raw, not containing AlCl3from the head part of the separator serves to distillation purification from viscida impurities, where isolated in the form of VAT residue in the amount of 30 kg/h, with content, wt.%: ethyl chloride - 56,6; dichloroethane and other high-boiling impurities - 43,4;

The distillate of the column in liquid form with an average consumption 1012 kg/h to send a distillation purification from nukiyama impurities, where they are separated in the amount of 12 kg/h, discharge to the sanitary column, irrigated water. Fraction nukiyama component has a composition, by weight. %: hydrogen chloride - 66,67, vinyl chloride - 0,42; ethylene - 9,16, chloride ethyl - 23,75.

From the cube column separation nukiyama impurities continuously taken ethyl chloride in the amount of 1000 kg/h containing 99.9% of the principal wishes and distillation residues, obtained after separation from ethyl chloride viscida impurities are mixed in a ratio of 1/0,5 and distilled 65 kg/h ethyl chloride containing 92,30% of the basic substance, which is then combined with the main then ethyl chloride raw, going to the Department viscida impurities. 600 kg/day residue containing AlCl3, organochlorine high-boiling substance and the polymer is treated with water in an amount of 600 kg (i.e., in a ratio of 1/1). After settling and separation get 672,2 kg of the aqueous layer with content (wt.%) hydrochloride aluminum in recalculation on All3-10,71, organic compounds - 0.03 and 527,8 kg organic layer, which is used for the known purpose. Output ethyl chloride amounts to 98.6%.

Example 2. Chloride ethyl-raw, as in example 1 for 24 h with medium load 1040 kg/h is fed to the purification from lCl3Receive 15 kg/h (360 kg/day) VAT residue, containing, wt.%: AlCl3-20,00; chloride ethyl - 30,00; high-boiling chlorinated organic compounds - 21,30; polymers increased by 28.70, which derive in the collection. Chloride ethyl-raw, not containing AlCl3served on distillation purification from viscida impurities, as in example 1. Wysokiej impurities in the form of VAT residue in colerado.

The distillate of the column with the average consumption 1015 kg/h to send clean nukiyama impurities, as in example 1.15 kg/h fraction nukiyama impurities, composition, wt.%: hydrogen chloride - 64,06; vinyl chloride - 0,35; chloride ethyl - 22,93; ethylene - 12,66 discharge to the sanitary column, irrigated water.

From the cube column select chloride ethyl 1000 kg/h, with a mass content of the basic substance of 99.9% meeting the requirements of GOST 2769-92 at the highest grade.

Distillation residues containing 20 wt.% AlCl3and distillation residues obtained after separation from ethyl chloride viscida impurities are mixed in a ratio of 1/2 and distilled 20 kg/h (480 kg/day) ethyl chloride containing 85,0% of the basic substance, which is then combined with the main stream ethyl chloride raw, going to the Department viscida impurities.

25 kg/h (600 kg/day) VAT residue containing AlCl3, organochlorine high-boiling substances and polymers, treated with water in an amount of 600 kg (i.e., in a ratio of 1/1). After settling and separation get 672,2 kg/day aqueous layer with content, wt.%: hydrochloride aluminum in terms of AlCl3- 10,71, organic compounds 0.03 and 527,8 kg/day organic layer, use raw received hydrochloridebuy ethylene, composition as in example 1 for 24 h with medium load 1067,0 kg/h is fed to the purification from AlCl3as in example 1. Get 8.6 kg/h (206,4 kg/day) VAT residue, containing, wt.%: AlCl3of 34.8; chloride ethyl - 5,8; high-boiling chlorinated components - 1,2; polymers to 58.2. Chloride ethyl-raw, not containing AlCl3served on distillation purification from viscida impurities, as in example 1. Wysokiej impurities in the form of VAT residue in the amount of 40 kg/h (960 kg/day) containing 26.5 percent ethyl chloride, collected in a collection and sent for further processing.

The distillate of the column with the average consumption 1024,5 kg/h to send clean nukiyama impurities, as in example 1. 24,5 kg/h fraction nukiyama impurities composition, wt.%: hydrogen chloride - 53,5; vinyl chloride - 0,2; chloride ethyl - 29,8; ethylene - 16,5%, discharge to the sanitary column, irrigated water. From the cube column select chloride ethyl - 1000 kg/h containing and 99.8 wt.% the main substance that meets the requirements of GOST 2769-92 at the highest grade.

Distillation residues containing 34.8 wt.% AlCl3and distillation residues obtained after separation from ethyl chloride viscida admixtures, mix the th next unite with the main stream ethyl chloride raw going to the Department viscida impurities,

540 kg/day residue containing AlCl3organochlorine high-boiling substances and polymers, treated with water in an amount of 1080 kg (i.e., in the ratio of 1/2). After settling and separation get 1152,5 kg/day aqueous layer containing, by weight. %: hydrochloride aluminum in terms of AlCl3- 6,24, organic compounds - 0.04 and 467,5 kg/day organic layer, to be used further for the known purpose. The yield of the desired ethyl chloride is 96,0%.

The method of purification of ethyl chloride, obtained by catalytic hydrochloridebuy ethylene in the liquid phase in the presence of aluminum chloride by distillation for the separation of aluminum chloride and subsequent distillation for separation of the target product, characterized in that the purification of ethyl chloride from aluminum chloride is performed by the method of a single distillation with obtaining VAT residue containing 5-35 weight. % aluminum chloride, which is mixed with kubovy the residue obtained during the distillation purification of ethyl chloride from viscida impurities, at mass ratio of 1: (0,52,5), respectively, and after separation of the ethyl chloride the mixture is treated with water at mass

 

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