Method for producing 1,2-dichloroethane and device for producing 1,2-dichloroethane

 

(57) Abstract:

The method of obtaining high-purity 1,2-dichloroethane was used as solvent with heat recovery from equimolar amounts of ethylene and chlorine, in 1,2-dichloroethane as the solvent, in the presence of tetrachloroferrate (1-)-catalyst, at 75 - 200°C and pressures of 1 to 15 bar. Summary of the invention in an upstream zone of mixing of dissolved chlorine gas in the circulating 1,2-dichloroethane, optionally connected to the reaction zone ethylene gas transfer in the dispersed liquid phase with a diameter of bubbles, maximum, 2.0 mm; this is the phase speed of 0.3 - 1 m/s reaction time of 2.5 - 25 designed for the liquid phase passes through the reaction zone, and then the resulting final product containing 500 ppm (m-1) chlorinated by-products in gaseous form is removed by evaporation under reduced pressure. The device consists of a mixer with a chlorine inlet, "static mixer" with the intake of ethylene, vessel rarefaction, circulation pump and Teploobmennik, and the mixer, static mixer, vessel pressure relief, circulation pump and the heat exchanger in the course of the stream connected to each other, the pressure vessel is connected through the dross is gas. 2 S. and 2 C.p. f-crystals, 1 Il.

The invention concerns a method of obtaining high-purity 1,2-dichloroethane with heat recovery by the reaction of ethylene and chlorine in a liquid 1,2-dichloroethane in the presence of a special catalyst, and other undesirable chlorinated products are formed only in small quantities, so that the resulting 1,2-dichloroethane does not require distillatively cleaning. A device for implementing this method.

Catalytic attachment of chlorine to ethylene to 1,2-dichloroethane as the solvent proceeds in 3 stages:

1. dissolving chlorine gas in 1,2-dichloroethane;

2. the dissolution of gaseous ethylene into 1,2-dichloroethane;

3. the reaction of the dissolved reagents to form 1,2-dichloroethane.

While the process at steps 1 and 3 occurs rapidly, in stage 2, probably because only a small solubility of ethylene in 1,2-dichloroethane slow and this step is therefore determines the reaction rate. On the basis of this technology is still carried out obtaining 1,2-dichloroethane in the reactors, which consist of the main reactor with sufficient processing time and additional (final) Rea is,2-dichloroethane as the solvent react in two-loop reactor with an additional reactor. In the main reactor for fine separation of the reaction gas is loaded with filler, the mixing zone. The reaction time is from 1 to 15 hours Purification of 1,2-dichloroethane is in addition connected distillation columns.

To obtain 1,2-dichloroethane in the application EP-O 111 203 A1 (US-A-4.774.373) there is a special catalyst, which is observed only minor corrosion rate on steel surfaces of the parts of the device. This special catalyst consists of anhydrous tetrachloroferrate (1-), in which the cation is an ion of an alkaline, alkaline-earth metal or ammonium ion.

Thus, the task is known to change modes (principles) and devices to such an extent that the total amount of the resulting chlorinated by-products in 1,2-dichloroethane did not exceed the value of 500 ppm (m-1), and no longer be a need for both large main and additional reactors and distillation cleaning (office) - products and the enthalpy of the reaction in different ways can be completely disposed of in another way.

Thus, the subject invention is a method for weak solvent, in the presence of tetrachloroferrate (1-)-catalyst at a temperature in the reaction zone from 75 to 200aboutC and a pressure of from 1 to 15 bar, which is characterized in that the upstream zone of mixing of dissolved chlorine gas in the circulating 1,2-dichloroethane, optionally connected to the reaction zone ethylene gas transfer in the dispersed liquid phase with a diameter of bubbles, maximum, 2.0 mm, this finely dispersed liquid phase speeds ranging from 0.3 to 1 m/s, with reaction times ranging from 2.5 to 25 C, calculated for the liquid phase passes through the reaction zone, and then the resulting high-purity 1,2-dichloroethane, which contains less than 500 ppm (m-1) chlorinated by-products in gaseous form is removed by evaporation under reduced pressure.

The method can differ by the fact that the diameter of the bubbles ethylene gas is less than 1.5 mm

According to the invention offers a very simple method of preparation of high-purity 1,2-dichloroethane. After evaporation of gaseous 1,2-dichloroethane is condensed and highlighted with a purity of more than 99.95 wt.%. It contains, as an essential side component, 1,1,2-trichloroethane. Released during the condensation heat can for example be used for distilled 1,2-DIH is completely unnecessary distillation column, necessary to obtain 1,2-dichloroethane according to the method of direct chlorination, to separate low-boiling and high-boiling fractions. Thereby saving both investment costs and operating (maintenance) costs. Outputs 1,2-dichloroethane make up 99.7% (based on C2H4in 99.7 per cent per Cl2.

Proposed by the invention, a method is crucial fine dispersion of the ethylene gas. It is not enough that the ethylene gas in finely dispersed form uduwela in 1,2-dichloroethane as the ethylene gas bubbles quickly merge into larger bubbles, and then the reaction rate strongly decreases. Therefore, you should take care to avoid merge into larger bubbles ethylene gas. Such a fine dispersion of the ethylene gas is achieved in the so-called "static mixtures", as described in Chemie-Ingenieur-Technik 52 (1980), No. 4, pp.285-291.

Next, a device for implementing the method, which is different mixer 1 with a chlorine inlet 11, "statistical mixer" 2 inlet ethylene 5, the vessel pressure relief 3, the circulation pump 6 and the heat exchanger 7, and the mixer 1, "static mixer" 2, the vessel pressure relief 3, circulated via the inductor 4 to the condenser 8, and from the capacitor 8 departs drain the product line and the exhaust line (outgoing) gas.

The device may, if necessary, to show that

a) "static mixer" 2 is used with a sloped front of the wall;

b) leaves in a "static mixer" 2 perforated, cut, have teeth and/or Gavrilovna;

(C) the leaves form a tortuous channels, or formed of crossed channels;

d) between "static mixer" 2 and the vessel pressure relief 3 is a block pressure 12;

e) near blokirovki pressure vessel 12 is located pressure relief 3 at a height of from 8 to 12 m above "static mixer" 2.

Increase therefore in the "static mixer" 2 pressure prevents boiling 1,2-dichloroethane in the reaction zone, there was observed a decrease of the reaction rate.

The vessel pressure relief 3, the heat exchanger 7, the zone of displacement of 1, and "static mixer" 2 filled with 1,2-dichloroethane, and by means of the circulation pump 6 is set to the stream of 1,2-dichloroethane 200 m3/h Through the inlet 11 2867 kg/h chlorine gas injected into the mixing zone 1. The mixing zone 1 made in the form of a mixing nozzle. Loaded with chlorine 1,2-dichlorvos inlet 5 are dosed 1134 kg/h of ethylene gas. As a "static mixer" 2 uses SMV mixer company Sulzer, Winterthur/Switzerland, corrugated sheets, which form open, intersecting channels.

The diameter of bubbles ethylene gas is 1.0-1.5 mm; 1,2-dichloroethane passes through the static mixer" 2 with a speed of 0.4 m/s

After the establishment of the stationary state in the condenser 8 are heated 7.5 m3/h of water up to 60aboutWith; in the heat exchanger 7 warm 20,0 m3/h water up to 96aboutC. Circulation 1,2-dichloroethane operates at 125aboutC and a pressure of 4 bar. The resulting 1,2-dichloroethane in a gaseous form from the vessel pressure relief 3 via a direct adjustment is supplied to the condenser 8 through the orifice 4. Hourly discharged 3997 kg 1,2-dichloroethane through the output of dichloroethane 9. Through the gas outlet line 10 non-condensable gases are supplied to the burning.

The obtained 1,2-dichloroethane as chlorinated impurities contains: 400 ppm (m-1) 1,1,2-three

chlorate 50 ppm 1,1-dichloro-

ethane 5 ppm TRANS-1,2-di

chlorethylene.

The output is

99,7% (based on C2H4and

99,7% per Cl2.

1. Method for producing 1,2-dichloroethane inter is harpert (1-)-catalyst at a temperature of 75 200oC and a pressure of 1 to 15 bar, in the reaction zone, wherein the chlorine gas is dissolved in the circulating 1,2-dichloroethane in separately connected to the mixing zone, and in addition is connected to the reaction zone ethylene gas transfer in the dispersed liquid phase with a maximum diameter of bubbles of 2.0 mm, then this finely dispersed liquid phase with a speed of 0.3 to 1.0 m/s reaction time of 2.5 - 25 in the calculation of the liquid phase is passed through a reaction zone and then the resulting high-purity 1,2-dichloroethane containing less than 500 ppm of chlorinated by-products, in the gaseous form is removed by evaporation under reduced pressure.

2. The method according to p. 1, wherein the process is conducted when the diameter of bubbles ethylene-gas less than 1.5 mm

3. Device for producing 1,2-dichloroethane containing the reactor with a mixer and vessel pressure relief, condenser, heat exchanger and piping, characterized in that on input line circulating 1,2-dichloroethane in the reactor is set mixer with a pipe for input of chlorine gas, and the reactor is made in the form of a static mixer with a pipe for input of ethylene, the reactor outlet posted by the vessel pressure relief and throttling device, the air circuit, supplied with a pump.

4. Installation under item 1, characterized in that between the reactor and the vessel pressure relief is a means for locking the pressure.

 

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