The method of producing vinyl chloride

 

(57) Abstract:

The invention relates to a method for producing vinyl chloride by thermal pyrolysis of dichloroethane. The process involves feeding the pyrogas through the HRSG in a convoy of vintage, above which the output gaseous phase containing vinyl chloride, dichloroethane and hydrogen chloride. After cooling, partial condensation and separation of reflux liquid remaining products of this phase are served in the distillation column for separation of hydrogen chloride, vinyl chloride and dichloroethane. Cooling pyrogas is carried out in a recovery boiler water, preheated gaseous phase columns quenching, to obtain the high-pressure steam. HRSG top connected with a partitioned container, the upper part of which serves heated water. Partly this chilled water gaseous phase is further cooled in a heat exchanger-the heat source dichloroethane, which is then fed to a pyrolysis furnace. In the process of obtaining vinyl chloride is achieved using the heat of the reaction gases. 2 C. p. F.-ly, 1 table. , 1 Il.

The invention relates to the chemical industry in obtaining chlorine-containing monomer is of chloretone followed by quenching of the resulting mixture and the rectification [application Germany 2925720, MCI C 07 C 21/06] . From the furnace of pyrolysis mixture formed during the decomposition of dichloroethane at a temperature of 480-560oC and a pressure of 1.5-2.5 MPa vinyl chloride and other products, is introduced into the heat exchanger. The last cool liquid and gaseous substances to dramatically reduce the temperature to 120-220oWith (preferably 100-150oC). For this purpose, use, for example, water, mineral oil, diphenyl silicone oil. Further cooling is carried out with application containing more than 50 % of dichloroethane mixture, which is injected into the gas stream or in contact with him in counter-flow quenching column. The cooling rate of the gas mixture should be (oC/C) 1/4-1/9 (preferably 1/5-1/7) the gas temperature entering the cooling system. The heat extracted from the gas mixture, is used to heat the cube distillation columns. Usually apply a two-stage cooling: at the first stage gas from the furnace is cooled to 120-220oWith the second - to 60-100oC.

The disadvantages of the method include a lack of full use of the heat of the reaction gases.

Closest to the proposed technical solution is the method of producing vinyl chloride by thermal pyrolysis jam. The gas discharged from the reaction zone of the furnace with a temperature of approximately 500oC and a pressure of 15 at, cooled to 160-200oWith mixed with dichloroethane. The latter is withdrawn from the quench column with a temperature of 140oC. This dichloroethane contains up to 15% of high-boiling compounds. Then the sin is cooled in a quench column to 130-150oWith simultaneous separation of high-boiling compounds, coke and tar from the reaction gas. Coming on top of the quenching column, a gas containing chloride, dichloroethane and hydrogen chloride, cooled to 90-110 (preferably 100)oWith the condenser of the column with water. When this gets 0.4 tonnes of process steam with a pressure of 1.7 at 1 t of vinyl chloride. Part of the resulting condensate is returned to the quenching column in the form of phlegmy, and the other part together with the gas fed into the heat exchanger. Gas and condensate from the heat exchanger with a temperature of 40-60oWith subjected to rectification in two columns and get hydrogen chloride, vinyl chloride and dichloroethane. Taken from the cube hardening of the column a mixture of high-boiling compounds and tar is distilled in a distillation column. Part of the obtained distillate with a boiling point of 130oAnd below, containing dichloroethane, after condensation in the cation impurity content of butadiene in the resulting vinyl chloride to ethylene dichloride, return to a distillation column, periodically add fresh dichloroethane. The latter contains not more than 1400 ppm of chlorine and no more than 40 ppm of iron. Consumption of this dichloroethane is not more than 1 (preferably of 0.05-0.2) mol. percent of dichloroethane fed to the furnace. This dichloroethane receive, for example, by chlorination of ethylene in the presence of iron compounds.

The main disadvantage of this method is not sufficiently rational use of high-grade (high-temperature) heat of the reaction gases and the deposition of coke and tar on the plates and in the reboiler of the distillation column.

Object of the present invention to provide a vinyl chloride by pyrolysis of dichloroethane with a more rational and full use of the heat of the reaction gases.

The problem is solved by the proposed method of producing vinyl chloride by pyrolysis of dichloroethane, comprising cooling the obtained pyrogas and column quenching for separating a gaseous phase containing vinyl chloride, hydrogen chloride and dichloroethane, and exhaust from the top of the column hardening, and high-boiling compounds concentrating in Cuba columns. Gaseous SMEs column quenching, and the remaining part of the condensate together with the gas phase is sent to consistently located distillation columns for separation of hydrogen chloride, vinyl chloride and dichloroethane. High-boiling cubic fraction from the column quenching is directed to the selection of her dichloroethane returned to the process, and removing resinous.

Under the proposed method of cooling the pyrogas is carried out in a recovery boiler, in which the upper part is connected with a partitioned plates capacity, in the upper part of which serves preheated in the first downstream heat exchanger-the heat coming out of the pillar of quenching the gaseous mixture of water through evaporation which receive high pressure steam, the original dichloroethane before serving in the pyrolysis furnace pre-heated in the second heat exchanger-the heat exchanger due to residual heat of the cooled gaseous mixture in it columns hardening, and further cooling the gaseous mixture is performed in the third heat exchanger-the heat exchanger air which after heating is served in the pyrolysis furnace burners for combustion of gaseous or liquid fuel.

In addition, under the proposed method cubic liquid malls and coke, and a pair of dichloroethane is sent to distillation column excretion of hydrogen chloride. The system includes clarification tank, the pump and the evaporator, through which the cubic liquid column quenching flow with a linear velocity of 10-100 m/s

The process of thermal pyrolysis or dehydrochlorinating dichloroethane is in the decomposition of dichloroethane at temperatures up to 480-520oWith the vinyl chloride and hydrogen chloride.

Phase pyrolysis of dichloroethane includes oven pyrolysis, column tempering pyrogas, node condensation of vapours from the top of the column, the node clarification of VAT quenching column, distillation column, intended to highlight faction dichloroethane returned to the process, and the fraction of high-boiling by-products, sent for incineration.

The proposed method differs from the known fact that the cooling of the pyrogas is carried out in a recovery boiler, in which the upper part is connected with a partitioned plates capacity, in the upper part of which serves preheated in the heat exchanger-the heat exchanger through heat recovery from the column quenching gaseous mixture of water through evaporation which receive postepowanie-exchanger due to residual heat of the cooled gaseous mixture in it of the column vacancy.

In addition, further cooling the gaseous mixture is performed in the following (third) heat exchanger-the heat exchanger by the air, which after heating is served in the pyrolysis furnace burners for combustion of fuel.

Cubic liquid from the column quenching passed through a system of clarification, including the tank, pump and evaporator, with the speed of 10-100 m/s for separating the liquid phase containing the resin and Cox, dichloroethane vapor directed into a distillation column for the separation of hydrogen chloride.

The drawing shows a scheme for vinyl chloride by thermal pyrolysis of dichloroethane by the proposed method. The dichloroethane is rectified with a basic substance content of at least 99.3% served in the coil of the furnace pyrolysis of dichloroethane R-1.

Microwave pyrolysis consists of 3 cameras - radiant, transient (shock) and convective United by a common frame, chimney, mounted in the side walls of the furnace burners, duct systems and the supply of fuel to the burners, and also located inside the furnace coil. The latter is divided into several zones.

Located in the convection chamber of the furnace portion of the coil is a heating zone dichloroethane, where he built up area is overheating and where a pair of dichloroethane to overheat 320-370oC. Located in the radiant chamber portion of the coil is reactionary. It is the process of pyrolysis of dichloroethane.

It is known that the coke formation occurs with appreciable velocity at the contact of liquid hydrocarbons with a metal surface heated to a temperature above 300oC.

Pyrolysis of dichloroethane is carried out at a temperature of 320-370oWith input and 480-520oWith the outlet and the inlet pressure of 20-25 kg/cm2and the output 16-24 kgf/cm2the reaction zone.

The reaction gases of the pyrolysis temperature 480-520oWith serves in the HRSG HRSG-1, during the passage through which the temperature of the gases is reduced to a temperature preventing condensation of chloro-organic products due to the heat pre-heated to 140-150oWith boiler feed water. The boiler is a device in which the pyrolysis gas passes at high speed through a pipe submerged in a layer of liquid water condensate. The upper part of the boiler is a partitioned plates capacity. In this capacity there is a saturation of water vapor due to its ozonation through the layer of water. In addition, with this capacity level, it pyrogas.

Installation of boiler KU-1 directly after pyrolysis furnace gives you the ability to regenerate most of the heat pyrolysis gases with obtaining the water vapor pressure of 12 ATA.

The reaction gases of the pyrolysis after the recovery boiler KU-1 with a temperature of 150-300oWith serves in the lower part of the column quenching K-1, where they bubbled through the liquid layer to quickly reduce the temperature up to 170-200oC. the Gaseous mixture is subjected to a first purification from gone hardening liquid drops on the failed plates and further rectification in the upper part of the column on the plates by contact with flowing phlegm.

Temperature phlegmy support within 50-80oC, and the temperature of the cube column - 170-200oC. In the distillation isolated from the products of pyrolysis of the main part of the high-boiling organic and chlorinated organic by-products and resins, bringing them from the column with kubovy stream.

Coming on top of the column K-1 gaseous mixture not containing coke and tarry, with a temperature of 160-170oServed with first counterflow heat exchanger-a heat exchanger TU-1, where it is cooled boiler water. The latter is heated up to 100-140oAnd then what of the heat exchanger TU-1 is directed into the heat exchanger-the heat exchanger TU-2, where it is cooled to a temperature of 100-120oC. Supplied in this heat exchanger, the refrigerant - dichloroethane from the storage tank is heated to a temperature of 80-100oC and then injected into the coil, located in the convective zone of the pyrolysis furnace.

Liquid-vapor mixture of pyrolysis products coming out of the second heat-exchanger TU-2, separated into gaseous and liquid streams.

Further cooling to 50-70oWith a gaseous mixture by condensation of the main part of dichloroethane and significant parts of vinyl chloride is carried out in a heat exchanger-the heat exchanger TU-3 air, which, after preheating fall into the pyrolysis furnace burners for combustion of fuel.

The cooled liquid from the last two heat exchangers TU-2 and TU-3 is sent to the reflux tank E-1, from which part of the liquid fed into the column top vintage K-1 as phlegmy, and the remaining part of the liquid is directed to the separation in the column allocation hydrogen chloride K-2.

Neskondensirovannyh gas stream from the heat-exchanger TU-3 serves in the heat exchanger T-1, which is cooled cooled gaseous hydrogen chloride, is withdrawn from the top of the column selection hydrogen chloride K-2. PE phase from the tank E-2 is directed to the separation in the column allocation hydrogen chloride streams.

CBM product columns hardening To-1 containing coke, resinous products and high-boiling side components, cleanse the system of clarification. From the tank E-3 with pump N-1 CBM product pumped with the linear speed of 10-100 m/s through the evaporator T-type 2 "pipe in pipe" for heating the circulating mixture to boiling point. For this purpose, use a heating steam pressure of 1.2 MPa. Vapor-liquid mixture from the evaporator T-2 return in tank E-3, where the extender installed above the tank, separating the vapor phase from the liquid. Vapour phase, not containing coke and tar products, is served in a distillation column K-2. A liquid containing a resin and a coke from the tank E-3 periodically taken for incineration.

Distillation column K-2 is used to obtain hydrogen chloride. Ê-2 equipped with a condenser T-3 and boiler T-4. Cubic liquid of the column is sent to the column K-3 for the separation of vinyl chloride and unreacted during pyrolysis of dichloroethane. Distillation column K-3 has a capacitor T-5 and boiler T-6.

Thus, the proposed scheme node quenching pyrolysis gases allows to utilize high-grade and low-grade Tr: In accordance with the proposed process (see the drawing) of the original dichloroethane in the number 54,6 t/h pre-heated to 140oWith the heat exchanger-the heat exchanger TU-2 due to the heat of pyrolysis gases leaving the heat-exchanger TU-1. Next, the heated source dichloroethane is evaporated and overheat in located in the convection chamber of the furnace of pyrolysis R-1 side of the coil. Overheated a couple of dichloroethane come in the reaction zone of the pyrolysis furnace at a temperature of 360oC and a pressure of 25 kgf/cm2. The reaction gases of the pyrolysis of temperature 500oC and a pressure of 21 kgf/cm2is sent to the HRSG HRSG-1. In the HRSG HRSG-1 serves the condensed water, preheated to 140oWith the heat exchanger-the heat exchanger TU-1 due to the heat of pyrolysis gases leaving the top of the column hardening To-1. When passing through the HRSG HRSG-1 the temperature of the gases is reduced to 300oC due to the heat loss of the heated to 150oWith the water condensate. The result is the vapor pressure of 12 kgf/cm2(1.2 MPa).

HRSG HRSG-1 is a two-piece apparatus, in which the pyrolysis gases passing with a speed of 33 m/s through a pipe located in the lower section and immersed in a water condensate. Polucen is="ptx2">

The cooled pyrolysis products that do not contain condensed chlorinated organic products, is served in the lower part of the quench column K-1. Due to ozonation through the layer of liquid products of pyrolysis cooled to a temperature of the bottom liquid 178oC. the Gaseous mixture is purified from gone hardening liquid drops 2 failed plates and then rectificate in the upper part of the column 16 mesh plates by contact with flowing phlegm. Temperature phlegmy support 60oC, and the temperature of the top of the column - 160oC.

Coming on top of the column K-1 gaseous mixture not containing coke and tar, served in a counter-current heat exchanger-a heat exchanger TU-1, where cool water condensate to a temperature of 150oC. Condensate of 7 m3per hour heat up with 20-30 140oC and served in the HRSG to produce steam. Excess superheated condensate in the amount of 0.2 m3/h return in the training of condensate.

Liquid-vapor mixture of pyrolysis products after the first heat-exchanger TU-1 served in the second counterflow heat exchanger-a heat exchanger TU-2 for pre-heating to 140 gas mixture of pyrolysis products from the condensation of the main parts of dichloroethane and significant parts of vinyl chloride is carried out in a heat exchanger-the heat exchanger TU-3, air-cooled. Last after heating is used for combustion in the burners of the furnace of pyrolysis.

The fluid from the heat exchangers TU-1, TU-2 and TU-3 is sent to the reflux tank E-1. From the tank E-1 22.6 t/h of liquid served in the upper part of the column quenching as phlegmy, and the remaining portion of the liquid output to the separation in the column allocation hydrogen chloride K-2.

Neskondensirovannyh gas stream from the heat exchanger TU-3 is sent to the heat exchanger T-1, which is cooled cooled to a temperature of minus 27oWith gaseous hydrogen chloride supplied from the collector phlegmy columns highlight of hydrogen chloride. Vapor-liquid mixture from the heat exchanger T-1 is sent to the tank E-2, in which the mixture is separated into gas and liquid phases. Both phases of capacity served after discharge pressure up to 1.3 MPa separation in the column allocation hydrogen chloride streams.

CBM product hardening of the column containing 9.2 % coke, resinous products and high-boiling side components, continuously output in tank E-3 in the amount of kg/h of the Liquid from the tank E-3 with a pump pumped at a rate of 100 m/s through a pipe of evaporator type "pipe in pipe", deaut 0.5 MPa. Heating is carried out by heating with steam pressure of 1.2 MPa. Vapor-liquid mixture from the evaporator is returned to the tank E-3, where the extender installed above the tank, separating the vapor phase from the liquid.

Vapour phase, not containing coke and tar products, served in the distillation column allocation hydrogen chloride K-2. Concentrated product containing resin and a coke from the tank E-3 periodically take to burn in number, on average 120 kg/h

In table. 1 presents comparative results of the technological mode for two types of node quenching pyrolysis gases:

option 1 - prototype;

option 2 - the proposed process implemented according to the drawing.

To facilitate evaluation of the results in the table. 1 performance in the second embodiment is reduced to the value specified in the prototype.

In both cases there is a complete selection of products of pyrolysis coke and tar together with kubovy the product of the quenching column.

However, in the proposed process are disposed of 3.7 Gcal/h of high-potential and 2.9 Gcal/h heat, while in the prototype utilized only 2.1 Gcal/h of heat. In rez is kg/h source dichloroethane is heated in the heat exchanger-the heat exchanger TU-2 to 140oS. For comparison, in a process carried out on the prototype, receive only 4 t/h of water vapor under the pressure of 0.17 MPa.

Using system clarification of distillation columns hardening makes it possible to reduce more than 4.3 times compared to prototype a number of high-boiling compounds and resins in the power of the column selection and high-boiling resinous K-2 and thus greatly facilitate the operation mode of the column.

1. The method of producing vinyl chloride by thermal pyrolysis of dichloroethane, followed by cooling of the pyrogas and feeding it to the column quenching for separating high-boiling compounds from the gaseous phase containing vinyl chloride, dichloroethane and hydrogen chloride supplied to the cooling compartment formed condensate, partially returned to the column quenching in the form of phlegmy, and feeding another part of the condensate with steam phase in the distillation column for separation of hydrogen chloride, vinyl chloride and dichloroethane, with the output from the cube hardening of the column a mixture of high-boiling compounds and resinous, the selection of the fraction enriched with ethylene dichloride and returned to the process, characterized in that what cooling pyrogas is carried out in the boiler-utilizatori heated in the heat exchanger-the heat coming out of the pillar of quenching the gaseous mixture of water, as a result of evaporation which receive high pressure steam, the original dichloroethane before serving in the pyrolysis furnace pre-heated in another heat exchanger-the heat exchanger due to residual heat of the cooled gaseous mixture in it columns hardening.

2. The method according to p. 1, characterized in that the gaseous mixture column quenching after cooling source dichloroethane is subjected to further cooling in heat exchanger-the heat exchanger by the air, which after heating is served in the pyrolysis furnace burners for combustion of fuel.

3. The method according to p. 1, characterized in that the cubic liquid from the column quenching passed through a system of clarification, including the tank, pump and evaporator, with the speed of 10-100 m/s for separating the liquid phase containing the resin and Cox, dichloroethane vapor returned to the process.

 

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40, 9 tbl, 3 dwg, 31 ex

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61 cl, 8 tbl, 32 ex

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EFFECT: improved method of synthesis.

2 cl, 1 tbl, 1 dwg, 4 ex

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EFFECT: the invention provides, that the presented design of the reactor allows to increase the selectivity of the process of production of the chlorinated allyl.

1 ex, 1 dwg

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