SU1348331A1 - Method of producing chlorhydrines - Google Patents

Abstract

The invention relates to halogen-substituted alcohols, in particular to the preparation of chlorohydrins (CG). The goal is to simplify the process, reduce the consumption of chlorine and eliminate wastewater. Preparation of CG is carried out from unsaturated hydrocarbon and chlorine with constant electrochemical treatment of CG acid circulating solution (CCD) with continuous supply of reagents, separation and removal of the resulting products in the form of an organic phase. HC1 or alkali metal chloride is used as a source of chlorine in the CCR. The method provides a simplification of the process due to the formation of concentrated solutions of CG, the complete utilization of chlorine ions and the elimination of wastewater. 1 3.p. f-ly, 1 ill. i ate with 4 00 00 with

Description

13483312

unidentified organics (EX) 2.78. The output DHGG on converted AH 88%.

Example 2. The process is carried out analogously to example 1, loading into the circulation circuit a saturated solution of DHGH containing 10 g / l of HCl. Instead of C1, the system serves 20%

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This invention relates to an improved process for the preparation of chlorohydrins, important products of organic synthesis.

The purpose of the invention is to simplify the process, reduce the consumption norms and eliminate wastewater, which is achieved by a constant electrochemical treatment of the circulating water-Q aqueous solution of HC1 (216 g / h). With the first solution of dichlorohydrin and continuous loading onto the electrolyzer 57 A and by means of separation and removal of the generation of 3.4 V. The feed rate of the AH state product as organic is 56 g / h. The water supply is carried out at the rate of maintaining a constant volume of the reaction mixture in the circulation loop. The temperature of the circulation reaction mixture. From the X-8 separator, at a speed of 93.42 g / h, the organic phase of the composition, May, is taken. %: AH 7, 1 1; ECG 0.33; THP4,8; DHGG84.58; HE 0.28; EX 0,28 .. The output DHGG 89,7%.

Example 3. The process is carried out analogously to example 1, loading organic phase X-8, diaphragm-25 into the circulation loop saturated electrolyzer with ruthenium oxide-DHGG oxide solution containing 10 g / l HC1. Instead of C1, chloride systems are supplied to the system, as well as T-3 refrigerators, sodium at a rate of 85.8 g / h with Na-T-4 and T-5 to maintain a given load on the electrolyzer 65 A and for example - temperatures of 30 ° C. 3.8 V. Circulating temperature. Measurement 1. The process of carrying out the reaction mixture is 15-17 ° C. Phases. Hydrogen chloride or alkali metal chloride is used as a source of chlorine.

The drawing shows the setup diagram that implements the proposed method.

The installation includes an acid solution circulation system with circulation pumps P-1 and R-2, which also perform the role of mixers, a system for separating gas and liquid F-7 water and

on a circulation installation that includes pumps P-1 and P-2, gas-liquid F-7 separation system and liquid-liquid X-8, diaphragm-free electrolyzer with oxide ruthenium titanium anodes and titanium cohorts E-6 , refrigerators T-3, T-4 and T-5 and rotameters 1 and 2.

A pre-prepared in an amount of 4 l of dichlorohydrin glycerin (DHGG), an aqueous solution containing 3.55 g / l of HC1 is loaded into the circulation loop. Pumps Р-1 and Р-2 are commissioned and the solution is circulated around the circuit: Т-3-Х-8-Р-2 -10-Т-5- 3-6-Ф-7-Р-1 with speed 200 l / h The electrolyzer is switched on (load 73 A, voltage 4 V) and allyl chloride is fed at a rate of 183.5 g / h, chlorine (C) 68.5 g / h and water 54.1 g / h. The temperature in the circuit is 20 ° C. From the separator X-8, constantly at a rate of 295.1 g / h, the organic phase is selected, containing, in wt.%: Allyl chloride (AH) 11.08; epichlorohydrin (ECH) 0,3; trichloropropane (TCP) 3.22; DHGG 80.25; chlorine ethers (CE) 2.37;

483312

unidentified organics (EX) 2.78. The output DHGG on converted AH 88%.

Example 2. The process is carried out analogously to example 1, loading into the circulation circuit a saturated solution of DHGH containing 10 g / l of HCl. Instead of C1, the system serves 20%

Q aqueous solution of HC1 (216 g / h). When loaded onto the electrolyzer 57 A and at a voltage of 3.4 V. The feed rate of the AH is 56 g / h. The water supply is carried out at the rate of maintaining a constant volume of the reaction mixture in the circulation loop. The temperature of the circulation reaction mixture. From the X-8 separator, at a speed of 93.42 g / h, the organic phase of the composition, May, is taken. %: AH 7, 1 1; ECG 0.33 THP4.8; DHGG84.58; HE 0.28; EX 0.28. The output DHGG 89,7%.

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Cottage AH 70.2 g / h. From the separator X-8 with a speed of 112 g / h select the organic phase composition, wt.%: AH 12.09; ECG 0.64; TCP 5.18; DHGG 80.05; HE 0.3; EX 1.74. The output DHGG 89%.

Example 4. The process is carried out analogously to example 1, loading into the circulation loop of 4.0 l of a styrene-saturated aqueous solution with HC1 content of 3.55 g / l. During the whole experiment HC1 67.5 g / h is supplied to the system; styrene 99 g / h and water to maintain a constant volume of the reaction mixture. The load on the electrolyzer is 70 A, the voltage is 3.9 V. The temperature is 20-23 ° C. From the separator X-8 with a speed of 99.2 g / h select the organic phase composition, may. %: styrene 1,26; styrene chlorohydrin 94.71; dichlorostyrene 2,12; EX1.91. The output of styrene chlorohydrin 64%.

Example 5. The process is carried out analogously to example 1, loading into the circulation circuit 4 liters of an aqueous solution saturated with propylene dichlorohydrin with a HC1 content of 10 g / l. Throughout the experiment, propylene is fed into the system - 33.3 g / h; sodium chloride 91.3 g / h; and water to maintain a constant volume of the reaction mixture. The load on the electrolyzer is 72 A at a voltage of A. The temperature is 20-22 C. From the X-8 separator at a rate of 34 g / h, the organic phase is selected, containing, wt.%: Propylene 1.57; propylene chlorohydrin 93.64; dichloropropane 2.97; EX 1,82, the yield of propylene-chlorohydrin 43%,

The proposed method allows to simplify the process due to the preparation of concentrated chlorohydrin solutions, the complete utilization of chlorine ions.

Claims (1)

and sewage disposal. Invention Formula 1, Method for producing chlorhydrins by unsaturated carbon interaction hydrogen and chlorine in an acidic circulating chlorohydrin solution with a continuous supply of reagents and removal of the resulting products, characterized in that, in order to simplify the process, reduce the consumption of chlorine and eliminate wastewater, the process is carried out with a constant electrochemical treatment of the acidic circulating solution and continuous separation and removing the formed products as an organic phase, 2, Method 1, characterized in that hydrogen chloride or alkali metal chloride is used as a source of chlorine in the circulating acidic solution. P-1 Compiled by N, Kapitanova Editor N, Kishtulinets Tehred A. Kravchuk Order 5161/23 Circulation 371 Subscription VNIIPI USSR State Committee for inventions and discoveries 113035, Moscow, Zh-35, Raushsk nab ,, d, 4/5 Production and printing company, Uzhgorod, st. Project, 4 P-2 Proofreader and Muska