The method of obtaining chlorohydrocarbons methane number

 

(57) Abstract:

The invention relates to chemical technology, in particular to improvements in the method of producing chlorohydrocarbons methane number, which find use as solvents and raw materials for the production of perchloroethane. The objective of the invention is to reduce the consumption of sulfuric acid and a weak hydrochloric acid contaminated with impurities, and an adequate improvement of the environmental parameters and efficiency of production through utilization of by-products hydrochlorination of methane. The problem is solved due to the fact that in the method of producing chloropetalum methane number at least part of the hydrogen chloride before treatment with methanol is subjected to isothermal absorption 27-32% hydrochloric acid with getting 35-45% hydrochloric acid, which might be fatal to the purification of methyl chloride from dimethyl ether, generated during the processing of hydrogen chloride with methanol, and processed 35-45% hydrochloric acid is fed to the processing of methanol, and formed with getting 35-45% hydrochloric acid exhaust gases, containing hydrogen chloride, is subjected to adiabatic absorption azeotropic hydrochloric calotomus, obtained at the stage adiabatic absorption, is subjected to the absorption of methanol, which is cooled. Absorbed sent to the machining stage of hydrogen chloride with methanol, the specified stage is carried out in boiling azeotropic hydrochloric acid, resulting azeotropic waste acid purified from methanol and direct on stage adiabatic absorption, and methyl chloride after cleaning prior to chlorination condense. 99 C.p. f-crystals, 13 ill.

The invention relates to the field of chemical technology, in particular to improvements in the method of producing chlorohydrocarbons methane number, which find use as solvents and raw materials for the production of perchloroethane.

A method of obtaining chlorohydrocarbons methane series, in particular chloroform, by gas-phase chlorination of organic raw materials with chlorine at an elevated temperature in a fluidized bed of solid inert carrier with the separation of the target product and recycling the remainder of the reaction mass, which is used as raw material mixture of methyl chloride to methylene chloride in a mass ratio (0,17-0,46): 1, the process is carried out at the reed of 0.5-0.7 in a single reactor under hydrodynamic conditions of the fluidized bed, ensure full mixing of the solid particles and the mode of displacement in the gas phase under continuous circulation of the coolant and cooling it in the circulation system outside the reactor (SU authorship, 1578119, class C 07 C 19/04, 17/10, 1990).

Closest to the invention to the technical essence and the achieved result is a method for chlorohydrocarbons methane number by the chlorination of methyl chloride or its mixture with methylene chloride at an elevated temperature and an elevated pressure to obtain the reaction mixture containing methylene chloride, chloroform, chetyrehhloristy carbon and hydrogen chloride, the selection of these products by condensation and distillation, and processing the resulting hydrogen chloride-methanol to obtain methyl chloride, part of which is purified and sent for chlorination (SU, patent, 619096, class C 07 C 17/10, 1978).

The disadvantages of the known technical solutions are:

- education as a by-product stage condensation of hydrogen chloride and methanol dimethyl ether, polluting methyl chloride;

- education is treated with sulfuric acid from the stage of purification of methyl chloride from dimethyl ether;

These by-products and their mixtures do not find practical application and require the creation of facilities for decontamination, because I acquired them in environmentally unacceptable, which greatly complicates the technology and increases the cost of the target product.

The objective of the invention is to reduce the consumption of sulfuric acid and formation of weak hydrochloric acid contaminated with impurities, and an adequate improvement of the environmental parameters and efficiency of production through utilization of by-products hydrochlorination of methanol.

The problem is solved due to the fact that the method of obtaining chlorohydrocarbons methane number by the chlorination of methyl chloride or its mixture with methylene chloride at an elevated temperature and an elevated pressure to obtain the reaction mixture containing methylene chloride, chloroform, carbon tetrachloride and hydrogen chloride, the selection of these products by condensation and distillation, and treatment with this hydrogen chloride-methanol to obtain methyl chloride, at least part of which is purified and sent for chlorination at least an hour what with getting 35-45% hydrochloric acid, which is directed to the purification of methyl chloride from dimethyl ether, generated during the processing of hydrogen chloride with methanol, and an elaborate 35-45% hydrochloric acid is fed to the processing of methanol, and formed with getting 35-45% hydrochloric acid exhaust gases, containing hydrogen chloride, is subjected to adiabatic absorption azeotropic hydrochloric acid, to obtain 27-32% hydrochloric acid, which is sent on the stage isothermal absorption, gas-vapor mixture obtained in stage adiabatic absorption, is subjected to the absorption of methanol, which is cooled, resulting absorbate sent to the machining stage hydrogen chloride-methanol, the specified stage is carried out in boiling azeotropic hydrochloric acid, the resulting waste azeotropic hydrochloric acid purified from methanol and direct on stage adiabatic absorption, and methyl chloride after cleaning prior to chlorination condense.

This can get the chloroform.

Isothermal absorption can lead at a temperature of from minus 5oC to minus 10oC.

35-45% hydrochloric acid before purification of methyl chloride from dimethyl ether can the led in the liquid phase.

Saturation azeotropic hydrochloric acid exhaust gases, containing hydrogen chloride, can lead mode adiabatic absorption.

Unfused gases stage adiabatic absorption of hydrogen chloride can undergo absorption purification from chlorohydrocarbons countercurrent treatment with methanol, cooled to a temperature of from minus 8oC to minus 15oC.

Methanol can be cooled by passing through the heat exchanger by gravity or force pump, and Teploobmennik cool, mainly brine with a temperature of minus 15oC.

After cooling, the methanol can apply for the irrigation of the absorption column, designed for cleaning gases condensation of methyl chloride.

After absorption absorbed can collect the holding tank for subsequent transportation with dissolved hydrogen chloride and methyl chloride.

Purified exhaust gases containing a small amount of methanol and traces of hydrogen chloride, can be subjected to purification by filing in small absorption column, which is irrigated with water, then purified exhaust gases vented into the atmosphere and water with a small colitis in the reactor hydrochlorination of methanol.

The emission of fully purified gases can be carried out through the arrester.

Processing of hydrogen chloride methanol can implement in full refractory-lined reactor, equipped with top of the distillation console.

The process in the reactor can perform in the mode of boiling azeotropic hydrochloric acid at a temperature of 99-107oC and the pressure in the upper part of the reactor, equal to 1.1 to 1.6 ATA.

Processing of hydrogen chloride with methanol in the reactor can spend with the supply of energy.

Heat can lead to the contents of the reactor from the heated steam boilers with natural and/or forced circulation of the reaction mass.

Gas-vapor mixture from the reactor can be submitted in rectifying the console, and then condensation.

The condensation can be accomplished by feeding the reaction gas containing methyl chloride, hydrogen chloride, a small amount of dimethyl ether, water vapor and unreacted methanol in the capacitors, and condensed in these heat exchangers hydrochloric acid with dissolved methanol is returned to the reactor.

Condensation can be achieved by posledovatelnogo is SUP>oC.

The reaction gas containing hydrogen chloride and a small amount of water and dimethyl ether, can apply for a cleaning disc in the absorption column, which is water cooled to a temperature of from minus 8oC to minus 15oC strong (35-45%) hydrochloric acid.

Clearing of dimethyl ether can produce up to content less than 0.01 wt. % with the simultaneous release of reactive gas from a moisture content of less than 0,008 wt.%

Moisture can display in the form of azeotropic hydrochloric acid by draining the excess water to maintain a constant liquid level in the reactor.

Dissolved methanol from waste hydrochloric acid can be removed by Stripping in a Packed column.

Heating the desorption column can perform boilers, heated by steam 120 - 130oC, and the desorption of lead in the mode Stripping of hydrochloric acid with the conclusions of the bottom of the column purified azeotropic hydrochloric acid, and the top - of methanol vapor, hydrogen chloride, water and methyl chloride, which is added to the reaction gas leaving the reactor.

Boiling azeotrope of hydrochloric acid can be selected from the cube to the desorption column level, proposal dumped into the corresponding cumulative capacity, and weak hydrochloric acid from the storage tank pump serves partly to strengthen in the column isothermal absorption, and in the number corresponding to the reaction and input from the outside of the water - column diabeticheskoi absorption, and before serving in this column the acid is cooled brine with a temperature of minus 15oC in the heat exchanger.

Strengthening the acid in the column isothermal absorption can produce hydrogen chloride from the stage chlorination of methyl chloride.

Unabsorbed gases from the column isothermal absorption can be attached to the reaction gas leaving the reactor, and strong (35-45%) hydrochloric acid to drain into the appropriate storage capacity, after which the acid pump serves in the tank and is cooled by a brine with a temperature of minus 15oC, and then served in the column purification of methyl chloride.

Removal of heat absorption of hydrogen chloride can be made by cooling 35-45% hydrochloric acid circulating in the accumulation tank-pump-heat exchanger-Packed column - storage capacity, and the heat exchanger is cooled by a brine with a temperature of minus 15oC, the qi system is IDA in the column.

Emerging from the column purification of strong hydrochloric acid can be discharged into the corresponding cumulative tank, where the pump be returned to the reactor through the heat exchanger.

To avoid the desorption of hydrogen chloride from 35-45% hydrochloric acid when mixed with warmer acid, condensed from the reaction gas, and education as a result of the gas tubes strong (35-45%) hydrochloric acid may be submitted initially in the heat recovery heat exchanger, where it is heated to 55-65oC to a transition of hydrogen chloride and water vapor in the vapor-gas phase, after which the phases are separated in the separator, vapor phase under pressure from 1.8 to 2.3 ATA directed to the supply line of hydrogen chloride in the hydrochlorination reactor, the liquid phase in the return line to the condensate acid selected from the reaction gas hydrochlorination of methanol.

Methyl chloride from the top of the column purification can send a combined filter, where released from the droplet entrainment of hydrochloric acid on the attachment and the fog.

Use the nozzle in the form of a package PTFE mesh or shavings, and exemption from fog can produce on the layer of fluoropolymer or glass felt.

Melhorar with zeolite, after condensing in the heat exchanger and drain into the corresponding cumulative capacity.

Methyl chloride containing dissolved hydrogen chloride, from the tank by the pump can bring to a chlorination step.

The absorber containing zeolite can be regenerated at least once in two months.

Regeneration of the adsorber can produce air, preheated in a furnace to a temperature of 400-450oC, after which regeneration is sent for incineration.

Before regeneration after regeneration of the adsorber can be purged with nitrogen to prevent the formation of explosive mixtures of air with methyl chloride.

Simultaneously with the blowing of the adsorber can be heated to a temperature of 100-150oC at the beginning of regeneration in a stream of dry nitrogen to prevent condensation of hydrochloric acid on the cold walls of the apparatus from the gas stream present in the adsorber, and moisture present in the air.

After regeneration can make the final cooling below 200-300oC simultaneously with the blowing of dry nitrogen.

Broken adsorber can protect from atmospheric moisture.

Nscontainerframe in the heat exchanger gases containing sooty, from the reaction gas hydrochlorination of methanol 1.2 to 1.5 ATA can apply for clearance through the absorption of methanol in the absorption column.

Excess hydrogen chloride from the stage of chlorination is not used for the synthesis of methyl chloride, can bring in a Packed column to obtain side abgaznaya hydrochloric acid, while the column from top to irrigate with fresh water and a weak acid, condensed in isothermal absorber of the vapor generated by the heat absorption of hydrogen chloride, and the second section of the column enter the azeotrope of hydrochloric acid, the number corresponding to the reaction water process hydrochlorination of methanol and water, introduced into a small absorption column for absorption of methanol emissions from inert gases.

Exhaust gases from isothermal absorber cooled circulating water can be delivered to the line of the reaction gas hydrochlorination of methanol before condensation from him hydrochloric acid.

Agathou hydrochloric acid coming from the bottom of the Packed column with a temperature of 90-100oC can cool the circulating water in the heat exchanger and collected in the appropriate storage capacity, periodically pump Tkachev the ionic column, in the upper part of which is distilled dissolved hydrogen chloride, which is sent to the reactor hydrochlorination of methanol, and the bottom select commodity methyl chloride.

Chlorination of methyl chloride produced in chloretone vaporized chlorine in the liquid phase in the presence of the initiator.

As the initiator can use porofor (bisaso-butyronitrile).

The concentration of porofor in a solution of methylene chloride can be taken equal to 1.5-3%.

To prepare the solution of the initiator can use dry porofor, and the dissolution of porofor in methylene chloride to produce with the help of a mixer in alternately operating the tanks.

Can use charator in the form of a bubbling apparatus, partitioned perforated plates and provided with internal circulation pipe.

When the chlorination in the lower part of charator can submit the vaporized chlorine from the buffer, the methyl chloride from the stage of synthesis, a solution of porofor from the tank pump recycling of methylene chloride from the main column and recycling of methylene chloride condensation and Stripping columns, and the chlorination is carried out at a temperature of 70-80oC and a pressure of 7.0 to 8.0 ATA.

To save the cold ohlord cooled brine with a temperature of minus 8-15oC, and in the heat exchanger, the cooled brine with a temperature of minus 25-40oC.

Coming out of the top of charator pair of chlorine-methanes and hydrogen chloride can be sent to the first column phase separation and there to serve from charator liquid stream of chlorine-methanes.

Filing can be done from the tank and pump.

Submission can be made directly through the hydraulic lock.

When the chlorination can provide a molar ratio of chlorine to the calculated stoichiometric amount of methyl chloride at the entrance to XLERATOR equal to 1.9 and 2.1.

The molar ratio of the liquid flow at the outlet of the reactor to the stoichiometrically calculated amount of the source of methyl chloride at the entrance to XLERATOR can take is equal to 3.0 to 3.5.

Separation of the products of the chlorination of methyl chloride can produce on consecutive distillation columns continuous action.

On the first column - condensation-Stripping can produce Department under pressure 6,8-7,5 ATA from the reaction mixture of hydrogen chloride and unreacted methyl chloride, and in the middle of the column in masterelite space wadati columns served in a pair of heat exchangers, cooled to a temperature of minus 8 to minus 15oC and minus 25 to minus 40oC, respectively, where separating methyl chloride, which is returned to the column in the form of phlegmy.

Hydrogen chloride can apply for phase hydrochlorination of methanol and to obtain hydrochloric acid.

Liquid methyl chloride mixed with dissolved hydrogen chloride can select from condensation and Stripping distillation columns in the corresponding accumulation tank, and then pump to return to the stage chlorination.

To avoid accumulation of moisture in chloretone and exclusions of education azeotrope with water on the line of recycling of methyl chloride can set the adsorber with the zeolite.

Filing a bottom liquid of condensation and Stripping columns in the column selection methylene chloride can produce under pressure of 2.7 to 3.2 ATA directly due to the pressure difference when stabilizing or using a pump and the corresponding cumulative capacity, which is simultaneously used for decoupling system of rectification after separation of free from hydrogen chloride raw chlorine-methanes.

Between the rectification column can install additional paoloni rectification - the column selection methylene chloride, which represents a methylene chloride purity of 99.7%, partially can be selected as a commodity product.

Condensed in the reflux condenser, the distillate of the second column rectification column selection methylene chloride, which represents a methylene chloride purity of 99.7%, partially or completely can be returned to the chlorination reactor to obtain the maximum amount of chloroform.

The ratio of the obtained chloroform and carbon tetrachloride can define the amount of recycling of methylene chloride.

Part of the recycling of methylene chloride can be directed to the preparation of a solution of proforma used as the initiator of the chlorination process, the remaining portion of the recycle is fed directly to the chlorination reactor.

On-line recycling of methylene chloride can install additional adsorber with the zeolite in order to avoid the return of moisture in charator with methylene chloride.

Once in 2-4 months can carry out the regeneration of the zeolites in the adsorbers.

Regeneration of zeolites in the adsorbers can be air heated to a temperature of 400 - 450oC after purging with nitrogen.

After purging purge the Sosa can apply for the power of the third column for distillation of her residual methylene chloride.

Filing a bottom liquid can be made from the conditions to ensure the contents of methylene chloride released in the following columns commodity chloroform no more than 0,002%.

To ensure environmental cleanliness of the process air line connecting a column of atmosphere, after a dephlegmator can install the heat exchanger, the cooled brine.

The product taken from the rectification column, representing a mixture of methylene chloride and chloroform, can direct the power of the previous columns.

Third column - to-column distillation of the methylene chloride - can work under pressure of 2.5-3.0 ATA, and pair it condense in the heat exchanger, and condensate, which are a mixture of methylene chloride and chloroform, from the tank by the pump is directed to flamerobin the same columns and the power of the previous columns, and cubic liquid to the third pillar level in the cube by pump or by gravity serves as food to the next column, which emit commodity chloroform-compliant.

Fourth column - to-column selection commodity chloroform - can work under atmospheric pressure, and a couple from the top of the column condense in the heat exchanger and the FDS is her columns and to the warehouse, and cubic liquid consisting of chloroform and carbon tetrachloride, from the cube on the level of the pump serves to supply the last column.

A couple from the top of the last column - the column of the distillation of chloroform and allocation of carbon tetrachloride, working under atmospheric pressure, can condense in the reflux condenser, and a mixture of chloroform and carbon tetrachloride be directed by gravity to flamerobin and the power of the previous columns.

The last column can perform with a side selection of the steam space of the cube from which the vapor output of commodity carbon tetrachloride, and its vapor condenses in the heat exchanger and collected in a suitable container, and cubic liquid, a mixture of decomposition products of poroporo, Asmolov and residues of carbon tetrachloride, with the help of the pump through the tank output to thermal deactivation, with the same pump provide forced circulation through the boiler to increase the heat transfer coefficient and reduce the possibility pitch.

All vozdushno columns can merge together and connect with a canister filled with activated charcoal, and regenerat the tion can be carried out at a temperature of 120-150oC ferry, which at the outlet of the adsorber condense together with chlororganic in the heat exchanger, cooled by water.

Chlororganic separated from the water in the clarifier is collected in the tank and the pump is sent for incineration.

Before start-up phase synthesis of methyl chloride, the reactor may be heated to a temperature of 100-105oC, and then begin feeding methanol and hydrogen chloride or concentrated hydrochloric acid.

Before you start the entire system can be purged with nitrogen while heating to start the flow of coolant, steam and establish irrigation columns.

Simultaneously with the heating of the hydrochlorination reactor can produce warm-up and start-up of the reactor chlorination of methyl chloride.

Upon reaching the boiling temperature in the reactor can set the working pressure by means of a flow in the nitrogen system, and then begin to apply the solution poroporo in methylene chloride.

Upon reaching the desired concentration poroporo in the reactor can begin to submit methyl chloride and chlorine in a minimum quantity with a gradual increase consumption of reagents to design value.

When it starts warming up of the reactor can be done by the Ute under pressure of 2.5-3.5 ATM in the amount of 20-40 m3per hour for 3-4 hours.

When it starts warming up of the reactor can be done by pumping the reaction mixture through the condensation-Stripping tower.

In repeated runs can carry out heating of charator when filling it with methylene chloride, and after reaching a temperature of 60-70oC start the dosage of the solution poroporo in methylene chloride, and upon reaching the required concentration of porofor include the submission of methyl chloride, and then chlorine.

In any start-up supply of chlorine can produce in the last turn, and when any stoppage of the flow of chlorine off in the first place.

To the pressure in the system 7-8 ATM can carry out the operation of the reactor without the release of vapor and liquid in the condensation-Stripping tower, and the liquid phase is poured into the container, and after the set pressure to open the outlet vapor in the condensation-Stripping tower and produce the dosage there is a liquid phase from the vessel.

After the release of condensation and Stripping columns on the regime and achieve the necessary parameters and compositions of distillate and Cuba can start the selection of hydrogen chloride in phase hydrochlorination of methanol and the dosage of the bottom liquid is named columns highlight methylene chloride can start a stage of preparation of a solution of poroporo.

When the temperature in chloretone in the first place can turn off the flow of chlorine, then the solution poroporo, methyl chloride and recycling of condensation and Stripping columns and columns selection of methylene chloride.

When the pressure in the system chlorination disconnect systems from the reactor can be implemented in the following sequence: chlorine, methyl chloride, recycling of methyl chloride, recycling of methylene chloride and the solution poroporo in methylene chloride.

At least part of the housing, at least a reactor, and/or any capacity, and/or one column, and/or bubbling apparatus can perform circular or elliptical or oval, or ovoidalnaya shape in transverse and/or longitudinal section, and/or combinations and/or combinations of these configurations.

At least one accumulation tank can perform a partitioned at least in the plan.

At least one accumulation tank and/or the reactor, and/or columns can be performed in three-dimensional bodies combined configuration that includes a combination of at least one cylindrical section circular and/or elliptical and/or oval and/or ovoidalnaya configuration with a tapered and/or hyperonymy, and/or the third and the or fourth order curvature.

The bottom of the tank and/or columns may contain at least one site of mono - and polyconic form.

The bottom of the storage tank can be done in the form of a narrowing down of the shell, representing at least part of the body of rotation with a generatrix in the form of unbloody, or branch of a hyperbola, or a combination configuration, including a combination of straight or broken areas, or combinations thereof with at least one curved element.

The bottom of the storage tank can provide not less than one means to drain that is placed in the lower part of the bottom.

Means for draining can apply multiplizieren and placed symmetrically relative to the vertical axis of the cumulative capacity.

Means for draining can be placed asymmetrically relative to the vertical axis of the cumulative capacity, mainly in the area adjacent to the side wall of the vessel, and/or at least partially inset in the bottom area of the side wall.

At least a portion of the wall of the storage tank can be done in the form of diaphragms made of chemically resistant material.

The axis of at least one accumulation tank may be oriented horizontally.

The axis of at least one accumulation tank or at least one section of the storage tank may be oriented obliquely.

Cumulative capacity can do with perception hydrostatic and/or dynamic pressure supplied to it liquid or gas.

Delivery of methanol to the place of work may take place in the rail and/or road tanks, and after delivery are overload of methanol to the warehouse.

The overload of methanol to the warehouse can produce by squeezing it in the tank.

Methanol can prelaminate in the tank, made of black steel STD.

Reactors, columns and storage tanks are made of black steel FTZ and gummiboot inside of a vulcanized rubber, over which is applied a layer of the lining of the at least one layer diabase tile with sealed seams between the tiles.

Seal the joints between the tiles can be done by processing Arsenicum.

Commodity methyl chloride can download transportationa and/or road tank black steel STD.

Commodity chloroform can be subjected to cleaning with sulfuric acid, and then neutralized, and then used for Halocarbon 22.

Halocarbon 22 can be subjected to pyrolysis to obtain divorceby, and then tetrafluoroethylene, which is used to produce fluoropolymers for the production of non-stick coatings.

Halocarbon 22 can be used to produce aerosols and refrigeration industry.

The technical result provided by the specified set of features, is that provided the maximum possible reduction in labor and materialsfrom due to the fact that drying of methyl chloride and its purification from dimethyl ether are sulfuric and hydrochloric acid, leaving a safety douchka on zeolites, excluded stage neutralization of methyl chloride with an alkaline solution; excludes stage kompremirovannyj of methyl chloride prior to its condensation, condensation of methyl chloride is carried out by cooling, and the resulting condensate is fed into the chlorination reactor, the feed to the reactor hydrochlorination of methanol hydrogen chloride is carried out partially in the gaseous form, and partly in the form of strong hydrochloric acid after espondence; is possible to avoid an excessive increase in the load on the condensation-Stripping tower due to the fact that in the scheme of rectification column remains Ogonki of methylene chloride to return it to charator and dramatically decreases the probability of a pitch of the target product - chloroform, and is also the possibility of the release of methyl chloride and methylene chloride as commercial products.

In Fig. 1 shows a flow chart of the process according to the claimed method;

In Fig. 2 - site of gas purification from methanol;

in Fig. 3 - site supply of heat to the reactor hydrochlorination of methanol;

in Fig. 4 - node separation of unreacted methanol and cooling azeotropic hydrochloric acid;

in Fig. 5 - node heat removal in the column isothermal absorption of hydrogen chloride;

in Fig. 6 - reactor, side view;

in Fig. 7 is transverse or longitudinal section of the hull of the storage tank, a variant elliptical;

in Fig. 8 - this is the same version of the oval form;

in Fig. 9 - this is the same option ovoidalnaya form;

in Fig. 10 - variant execution capacity of a partitioned;

in Fig. 11 is an embodiment of the bottom of the storage tank in the form of a tapering kN is rest to drain relative to the longitudinal axis;

in Fig. 13 is an embodiment of the wall of the storage tank in the form of diaphragms, one of which has in the upper part of the funds for the message of partitioned areas of the storage tank.

The method is as follows.

Chlorine from line 1, methyl chloride from line 2, the condensate condensation and Stripping columns from line 3 enter the reactor 4, which is chlorination. In this reactor support the increased pressure caused by the resistance of the technological scheme, and the appropriate conditions necessary for carrying out the chlorination of methyl chloride and methylene chloride to chloroform. In the absence of a catalyst the reaction is carried out usually at a temperature of about 350 - 500oC. the Reaction can be carried out in the presence of a catalyst by initiating actinic light, perioxidase. Can be used as liquid-phase and gas-phase conditions. However, the reaction of chlorination shall be carried out in anhydrous conditions.

The reaction products leaving the reactor 4 containing neproreagirovavshimi methyl chloride, methylene chloride, chloroform and carbon tetrachloride and byproduct hydrogen chloride is introduced into the condensing-Stripping tower 5. Wysocki the condensation and Stripping columns 5 through line 6 into the system, the acceleration of the reaction products (not shown).

Condensation condensation and Stripping columns 5 of the capacitor 7 through the gas-liquid separator 8 is divided into two streams, one stream in the form of phlegmy returns to irrigation condensation and Stripping columns 5, another on line 3 returns to the chlorination reactor 4.

Non-condensable gases from the gas-liquid separator 8 is fed to the column isothermal absorption 9 hydrogen chloride, irrigated chilled in the refrigerator for 10 27-32% hydrochloric acid. There is a possibility of non-condensable gases from the gas-liquid separator 8 through line 11 to the condensation of the methanol in the reactor 12. Hydrochloric acid from the column isothermal absorption 9 with a concentration of 35-45% in line 13 is directed through the condenser 14 to the purification of methyl chloride from dimethyl ether in a column of 1.5. Exhaust gases from the column isothermal absorption 9 hydrogen chloride in line 16 is directed to the column adiabatic absorption 17 hydrogen chloride, irrigated purified from methanol azeotropic hydrochloric acid supplied through the line 18, and the condensate from the condenser 19 which is separated from the gas stream in a gas-liquid separator 20.

Gas-vapor phase of the gas-liquid separator 20 through line 21 is fed to an absorption column column 22 output line 25.

Absorbed from the column 22 output line 26 and is directed to condensation with methanol in the reactor 12. Condensation of hydrogen chloride and methanol is carried out in boiling hydrochloric acid. Gas-vapor phase of the reactor 12 is sent to the condenser 27, the condensate from the gas-liquid separator 28 are returned to the reactor 12. Waste hydrochloric acid from the reactor 12 through line 29 is fed to the column 30 for cleaning neproreagirovavshikh methanol. Vapor-gas phase from the column 30 is sent to the condenser 27, and purified from methanol hydrochloric acid from the cube column 30 through line 18 is directed to the strengthening in column 17. Excessive amounts of 27-32% hydrochloric acid is shown by line 31.

Gaseous products hydrochlorination of methanol from the gas-liquid separator 28 are cleaned from dimethyl ether in column 15, irrigated chilled in the refrigerator 14 35-45% hydrochloric acid.

Exempt from dimethyl ether, methyl chloride through line 32 is supplied to the condensation in the condenser 33. Condensation of methyl chloride is collected in the accumulator tank 34 where line 2 is supplied to the chlorination reactor 4.

Neskondensirovannyh in the condenser 33 gases through line 35 do additional cleanup from provsional columns 22, contaminated vapors of methanol, is removed by line 25 (Fig. 1) and sent for treatment in column 36, which is irrigated by the water line 37. Purified exhaust gases from the column 36 vented into the atmosphere through the arrester 38. The water absorbed by the methanol from the column 36 is poured into the accumulation tank 39, thence pump 40 serves in the reactor hydrochlorination of methanol 12.

Reaction mass from the reactor 12 hydrochlorination of methanol transload 41 flows into the intermediate tank 42. The reaction mass from the intermediate tank 42 by the pump 43 is served in the heater 44, where the heated reaction mass is fed into the reactor 12 hydrochlorination of methanol.

An excessive amount of the reaction mass is directed to the column 30 for separation of unreacted methanol from the azeotropic hydrochloric acid (Fig. 4), the heating of the column is performed by the heater 45, the heated steam 120-130oC. Output bottom cleaned azeotrope of hydrochloric acid on line 18 is transported in column 17 (Fig. 1). To use heat azeotropic hydrochloric acid is passed through the heat exchanger-recuperator 46, where it is cooled to a temperature of 65-70oC strong chlorine hydrochloric acid from the column 15 (Fig. 1) and collected in the accumulation capacitance is well isothermal absorption and column adiabatic absorption 17 (the second option).

Removal of heat absorption of hydrogen chloride in the column isothermal absorption 9 is realized by means of cooling 35-45% hydrochloric acid circulating in the accumulation tank 49 and pump 50 to the heat exchanger 51 (Fig. 5), and the circulation system are selected 35-45% hydrochloric acid with a flow rate of 10-15% of the circulating flow and line 13 is directed to the drying and purification of methyl chloride from dimethyl ether in column 15.

Coming out of the column 15 purification of methylene chloride from dimethyl ether proven strong hydrochloric acid is poured into the appropriate cumulative capacity (not shown), where a pump (not shown) in line 52 through the heat exchanger-recuperator 46 fed into the reactor 12. To exclude gas tubes warmed strong hydrochloric acid from the heat exchanger-recuperator 46 serves in the separator 49. Vapor-gas phase from separator 49 is sent to the supply line of hydrogen chloride reactor 12 hydrochlorination, and the liquid in the return line to the condensate separator 28.

Methyl chloride from the top of the column purification 15 line 32 is directed to condensation. On line 32 are combined from the Teflon filter mesh or chips and a glass of felt for EvoBus zeolites for dowski of methyl chloride (adsorber in the diagram is not specified).

The system of the distillation product of the chlorination of methyl chloride consists of conventional distillation columns used for its intended purpose, therefore, their locations, and tie not included.

If necessary, the methyl chloride can be removed from the system through line 35 and is aimed at ordinary rectification (rectification scheme of methyl chloride not shown).

Before start-up phase synthesis of methyl chloride reactors 4, 12 can be heated to a temperature of 100-105oC, and then begin feeding methanol and hydrogen chloride or concentrated hydrochloric acid.

Before you start the entire system can be purged with nitrogen while heating to start the flow of coolant, steam, and to establish irrigation columns.

Simultaneously with the heating of the reactor 4 hydrochlorination can produce warm-up and start-up of the reactor 12 chlorination of methyl chloride.

Upon reaching the boiling temperature in the reactor can set the working pressure by means of a flow in the nitrogen system, and then begin to apply the solution poroporo in methylene chloride.

Upon reaching the desired concentration poroporo in the reactor can begin to submit methyl chloride and chlorine in a minimum amount of the EB of the reactor can be done by pumping the reaction mixture through an external heat exchanger, heated steam, which is fed under pressure of 2.5-3.5 ATM in the amount of 20-40 m3per hour for 3-4 hours.

When it starts warming up of the reactor can be carried out by pumping the reaction mixture through the condensation-Stripping tower 5.

In repeated runs can carry out heating of charator when filling it with methylene chloride, and after reaching a temperature of 60-70oC start the dosage of the solution poroporo in methylene chloride, and upon reaching the required concentration of porofor include the submission of methyl chloride, and then chlorine.

In any start-up supply of chlorine can produce in the last turn, and when lubach stops the flow of chlorine off in the first place.

To the pressure in the system 7-8 ATM operation of the reactor can be carried out without the release of vapor and liquid in the condensation-Stripping column 5, and the liquid phase is poured into the accumulation tank, and after the set pressure to open the outlet vapor in the condensation-Stripping tower 5 and produce the dosage is there a liquid phase of the storage capacitor.

After the release of condensation and Stripping columns 5 on the regime and achieve the necessary parameters and compositions of distillate and Cuba mohanna, and then make consecutive start system rectification.

After entering the mode, the column selection methylene chloride can start a stage of preparation of a solution of poroporo.

When the temperature in chloretone in the first place can turn off the flow of chlorine, then the solution poroporo, methyl chloride and recycling of condensation and Stripping columns and columns selection of methylene chloride.

When the pressure in the system chlorination disconnect systems from the reactor can be implemented in the following sequence: methyl chloride, recycling of methyl chloride, recycling of methylene chloride and the solution poroporo in methylene chloride.

At least part of the housing, at least a reactor and/or of any capacity, and/or one column, and/or bubbling apparatus can perform round (not shown), or elliptic 53, or oval 54, or ovoidalnaya 55 shape in transverse and/or longitudinal section, and/or combinations of these configurations (not shown).

At least one accumulation tank can perform a partitioned 56 at least in the plan.

At least one accumulation tank 34, and/or the reactor, and/or column can perform as vol is Oh, and/or elliptical and/or oval and/or ovoidalnaya configuration with a tapered and/or GIPRODORNII, and/or combined parcels, including at least one planar face, or at least one insertion of the second, or third, or fourth order curvature (not shown).

The bottom 57 of the storage tank 34 and/or columns may contain at least one site of mono - or polyconic form.

The bottom 57 of the storage tank 34 can be performed in the form tapering downwards shell, representing at least part of the body of rotation with a generatrix in the form of unbloody, or branch of a hyperbola, or a combination configuration, including a combination of straight or broken sections or combinations thereof with at least one curved element (not shown).

The bottom 57 of the storage tank can provide not less than one means 58 to drain that is placed in the lower part of the bottom.

The means 58 for draining can apply multiplizieren and placed symmetrically relative to the vertical axis of the cumulative capacity.

The means 58 for draining can be placed asymmetrically relative to the vertical axis 59 cumulative eat the th in the bottom area of the side wall.

At least a portion of the wall of the storage tank can be done in the form of diaphragms 60,61 made of chemically resistant material.

At least one aperture 61 in the upper and/or lower part can perform the means 62 for messages partitioned zones of the cumulative capacity.

The axis of at least one accumulation tank may be oriented horizontally (not shown).

The axis of at least one section of the storage tank may be oriented obliquely (not shown).

Cumulative capacity can do with perception hydrostatic and/or dynamic pressure supplied to it liquid or gas.

Delivery of methanol to the place of production may take place in the rail and/or road tanks, and after delivery are overload of methanol to the warehouse.

The overload of methanol to the warehouse can produce by squeezing it in the tank. Methanol can predavlivali in the tank, made of black steel STD. Reactors, columns and storage tanks can run out of black steel FTZ and Gumirovich inside vulcanized rubber, on top of which (not shown). The sealing of the joints between the tiles can be done by processing Arsenicum.

Commodity methyl chloride can be loaded into the shipping container and send to the consumer. As the transport containers may use rail and/or road tank black steel STD.

Commodity chloroform can be subjected to cleaning with sulfuric acid and then neutralized, and then be used to obtain halon 22.

Halocarbon 22 can be subjected to pyrolysis to obtain divorceby, and then tetrafluoroethylene, which can be used to obtain fluoropolymers for the production of non-stick coatings.

Halocarbon 22 can be used to produce aerosols and refrigeration industry.

Example 1. 57,71 mol/h of chlorine, 30,97 mol/h of methyl chloride contaminated hydrogen chloride (0.97 mol/h), and 281,04 mol/h return chlorohydrocarbons, containing 127,51 mol/h of methyl chloride, 148,03 mol/h of methylene chloride, 5.3 mol/h of hydrogen chloride and 0.20 mol/h of chloroform, served in the reactor 4. In recent supported operating pressure of 8 bar and a temperature of 80oC. as an initiator of the chlorination process in the reactor 4 enter placebocontrolled stream from the reactor 4 directly enters the condensing-Stripping tower 5. The pressure at the outlet of the gas-liquid separator 8 are supported by about 7 MPa and a temperature of about minus 10oC. From the cube column output line 6 high-boiling products of chlorination, containing 26,88 mol/h of chloroform, 1,24 mol/h of carbon tetrachloride with a decomposition product of bestbuyrentacar and impurities of methylene chloride. The output of chloroform converted to chlorine - 94,13%. Neskondensirovannyh the product of the gas-liquid separator 8 consisting of hydrogen chloride, loaded with methyl chloride, was divided into two streams. One thread in the amount of 19,38 mol/h of hydrogen chloride and of 1.02 mol/h of methyl chloride was sent on the line 11 to the reactor hydrochloridebuy methanol. Another thread in the number amounted to 38.66 mol/h of hydrogen chloride and 2.03 mol/h of methyl chloride directed in column 9 for/cross/ concentrated hydrochloric acid. Hydrochloric acid with a concentration of 40 wt.% hydrogen chloride in the amount of 19,73 mol/h of hydrogen chloride and 60.0 mol/h of water was cooled to -10oC in the refrigerator 14 and applied to the irrigation of the column 15 for the purification of methyl chloride from dimethyl ether and methanol. Waste hydrochloric acid mixed with dimethyl ether (0.04 mol/h) and methanol (0.07 mol/h) was sent to hydrochlo the technical 30% hydrochloric acid in column 17. Freed from hydrogen chloride gases are sent to an adsorption treatment in the column 22, irrigated cooled to minus 100oC methanol. Methanol was filed with the speed 28,48 mol/hour. The sorbate from the column 22 was applied to the hydrochlorination reactor 12. The hydrochlorination reaction was carried out at boiling of the reaction mixture (about 105-110oC).

Waste azeotropic hydrochloric acid, contaminated with methanol, was sent to clean the methanol distillation column 30. Purified hydrochloric acid was used to enhance in column 17. Gas-vapor phase of the hydrochlorination reactor 12 and Stripping columns was cooled, the condensate is returned to the hydrochlorination and neskondensirovannyh gaseous methyl chloride 32.76ˆ mol/h of hydrogen chloride, 0.64 mol/h, methanol 0.06 mol/h and the dimethyl ether of 0.04 mol/h were sent to the purification column 15 chilled 40% hydrochloric acid. The cleaned gas is directed to the condensation, the condensation of methyl chloride was applied for chlorination. Non-condensable gases filed on absorptio source methanol. The degree of purification of gases from methyl chloride cooled methanol full.

The output of chloroform filed on methanol is carbon tetrachloride

In to the/h

Example 2. Source materials are the same as in example 1. Equipment and process operations are the same to line 11. All descendancies the flow of the gas-liquid separator 8 was applied only to the column 9 to obtain concentrated hydrochloric acid. Line 11 was closed for the passage of gas. With the column 9 was selected by 45% of hydrochloric acid in the amount 62,7 mol/h of hydrogen chloride. Hydrochloric acid was cooled to -10oC and applied for irrigation of the column 15 for the purification of methyl chloride from dimethyl ether. The degree of purification is complete. (The detection sensitivity of dimethyl ether of 0.001%).

The output of chloroform, carbon tetrachloride and hydrochloric acid similar to example 1.

Example 3. Source materials, equipment and process operations are the same as in example 2, except for the increase of supply in the system methanol to 32.50 mol/H. In this case, the system displayed an excess of methyl chloride in the amount of 3.8 mol/H. With this reduced number of side hydrochloric acid. The output of chloroform was

carbon tetrachloride,

and methyl chloride,

about

1. The method of obtaining chlorohydrocarbons methane number by the chlorination of methyl chloride or its mixture with methylene chloride at higher carbon tetrachloride and hydrogen chloride, the selection of these products by condensation and distillation and processing of the resulting hydrogen chloride-methanol to obtain methyl chloride, at least a portion of which was subjected to purification from dimethyl ether using an acidic agent and then sent to the chlorination, characterized in that at least part of the resulting hydrogen chloride is subjected to isothermal absorption 27 - 32% hydrochloric acid with getting 35 - 45% of hydrochloric acid, which is used as sour agent for the purification of methyl chloride from dimethyl ether with obtaining waste 35 - 45% of hydrochloric acid, the latter serves on the stage of processing of methanol, and the formed while getting 35 - 45% of hydrochloric acid exhaust gases, containing hydrogen chloride, is subjected to adiabatic Assortie azeotropic hydrochloric acid with obtaining a 27 - 32% hydrochloric acid, which is sent to the stage isothermal absorption, and gas-vapor mixture, which is subjected to the absorption of methanol, pre-cooled, resulting absorbed sent to the machining stage of hydrogen chloride with methanol, and the above processing is carried out in boiling azeotropic hydrochloric acid, obtained when it is lifted absorption, and methyl chloride obtained in the processing phase, methanol, clear, condensed and sent to the chlorination.

2. The method according to p. 1, characterized in that the major secreted product is chloroform.

3. The method according to p. 1, wherein the isothermal absorption is carried out at a temperature of from -5 to -10oC.

4. The method according to p. 1, characterized in that 35 - 45% hydrochloric acid prior to the purification step of methyl chloride from dimethyl ether cooled to -10 to -15oC.

5. The method according to p. 1, characterized in that the processing of hydrogen chloride with methanol is carried out in the liquid phase.

6. The method according to p. 1, characterized in that the station adiabatic absorption gas mixture containing hydrogen chloride, serves methanol countercurrent with temperatures ranging from -8 to -15oC.

7. The method according to PP. 1 and 6, characterized in that methanol is cooled by passing through the heat exchanger by gravity or force pump, the heat exchanger is cooled mainly by brine with a temperature of -15oC.

8. The method according to PP. 1 and 7, characterized in that the exhaust gases stage adiabatic absorption, containing a small amount of methanol and traces of hydrogen chloride is completely purified exhaust gases vented into the atmosphere, and water with a small amount of methanol is poured into the accumulation tank where gravity or forced by a pump fed into the reactor hydrochlorination of methanol.

9. The method according to p. 8, characterized in that the emission of fully purified gases are carried out through the arrester.

10. The method according to p. 1, characterized in that the processing of hydrogen chloride with methanol is carried out in a floor lined reactor, equipped with top of the distillation console.

11. The method according to p. 10, wherein the process is carried out in a reactor in boiling azeotropic hydrochloric acid at a temperature of 99 - 107oC and the pressure in the upper part of the reactor of 1.1 to 1.6 ATA.

12. The method according to PP.10 and 11, characterized in that the gas-vapor mixture obtained in the processing of hydrogen chloride with methanol from the reactor served in rectifying the console, and from thence by a condensation reaction gas.

13. The method according to p. 12, characterized in that the condensation reaction gas containing methyl chloride, hydrogen chloride, a small amount of dimethyl ether, water vapor and unreacted methanol, leading to the condensers, and condensed them in hydrochloric acid with rastvoreniyu through the consistent use of refrigerators on the back of the water and refrigerators, cooled brine with a temperature of -15oC.

15. The method according to PP.12 to 14, characterized in that the reaction gas after the condensation is fed to the cleaning disc in the absorption column, which is water cooled to a temperature of -8 to -15oC 35 - 45% hydrochloric acid and purified from dimethyl ether lead to content less than 0.001 wt.% with simultaneous cleaning of water content less than 0,008 wt.%.

16. The method according to p. 15, characterized in that the water output in the form of hydrochloric acid by draining the excess water by maintaining a constant liquid level in the absorption column.

17. The method according to p. 16, characterized in that of hydrochloric acid in removing dissolved methanol and methyl chloride by desorption in a Packed desorption column.

18. The method according to p. 17, characterized in that the desorption column is equipped with immersion heaters, heated water vapor with a temperature of 120 - 130oC and desorption are in the mode of distillation with the conclusion from the bottom of the cube columns boiling azeotropic hydrochloric acid, and the top - of methanol vapor, hydrogen chloride, water and methyl chloride, which is added to the reaction gas leaving the reactor processing of methanol.

19. The method according to p. 1 the t through the heat exchanger, cooled to a temperature of 65 - 70oC cold 35 - 45% hydrochloric acid and output to the corresponding cumulative capacity.

20. The method according to PP.1 and 3, characterized in that the isothermal absorption of lead into the column, and unabsorbed gases from the column isothermal absorption added to the reaction gas leaving the hydrochlorination reactor, and the resulting 35 - 45% hydrochloric acid is poured into the appropriate storage capacity, after which the acid pump serves in the tank and is cooled by a brine with a temperature of -15oC, and then served in the column purification of methyl chloride from dimethyl ether.

21. The method according to p. 20, wherein the removal of heat in the column isothermal absorption is realized by means of cooling 35 - 45% hydrochloric acid circulating in the accumulation tank - pump - heat exchanger - column isothermal absorption - storage capacity, and the heat exchanger is cooled by a brine with a temperature of -15oC from the circulation system selected 35 - 45% hydrochloric acid in amount of 10 - 15% of the circulating flow and direct to the stage of purification of methyl chloride.

22. The method according to p. 21, characterized capitalnew capacity, where the pump is served in the hydrochlorination reactor.

23. The method according to PP.1, 3 and 20 to 22, characterized in that to prevent the desorption of hydrogen chloride from 35 - 45% of hydrochloric acid and education as a result of the gas tubes 35 - 45% hydrochloric acid serves first in the heat recovery heat exchanger, where it is heated to 55 to 65oC, with hydrogen chloride and water vapor passes into the vapor-gas phase, after which the phases are separated in the separator for gas-vapor phase, which is under pressure from 1.8 to 2.3 ATA directed to the supply line of hydrogen chloride in the reactor hydrochlorination of methanol, and the liquid phase, which is linked to acid isolated from the reaction gas hydrochlorination of methanol.

24. The method according to p. 15, characterized in that methyl chloride is taken from the top of the absorption column purification and directed to a combined filter for removing hydrochloric acid from the water.

25. The method according to p. 24, characterized in that the use of filter layers PTFE mesh or chips and fluoropolymer or glass felt.

26. The method according to PP. 15 and 24, characterized in that methyl chloride additionally cleaned by passing through the adsorber with the zeolite, after which it the outdoor is investing.

27. The method according to p. 26, characterized in that the adsorber containing zeolite, regenerate at least once in two months.

28. The method according to p. 27, characterized in that the regeneration of the adsorber is produced by air heated to a temperature of 400 - 450oC, after which regeneration is sent for incineration.

29. The method according to PP.27 and 28, characterized in that prior to regeneration after regeneration of the adsorber is blown with nitrogen at a temperature of 100 - 150oC.

30. The method according to PP.26 to 29, characterized in that after the regeneration of the adsorber is cooled to a temperature below 200 - 300oC by blowing dry nitrogen.

31. The method according to PP.26 to 30, characterized in that the non adsorber protect against the ingress of atmospheric moisture.

32. The method according to p. 23, characterized in that is not condensed in the heat exchanger gases containing nitrogen, hydrogen chloride and methyl chloride, is fed to the purification using the absorption of methanol in the absorption column.

33. The method according to p. 1, characterized in that neproreagirovavshimi hydrogen chloride from the stage chlorination of methyl chloride is served in a Packed column to obtain abgaznaya hydrochloric acid, while the column from top to irrigate with fresh water and then a weak acid, the MSE of the different topics what agathou hydrochloric acid coming from the bottom of the Packed column with a temperature of 99 - 100oC, cooled circulating water in the heat exchanger and collected in the appropriate cumulative capacity, from which periodically pump pumped storage.

35. The method according to PP.1 and 4, characterized in that, if necessary, the allocation of commodity methyl chloride it is served in a distillation column, the top of which is distilled hydrogen chloride, which is sent to the reactor hydrochlorination of methanol, and the bottom select commodity methyl chloride.

36. The method according to p. 1, characterized in that the chlorination of methyl chloride produced in chloretone vaporized chlorine in the liquid phase in the presence of the initiator.

37. The method according to p. 36, characterized in that as the initiator of the use porofor-azobisisobutyronitrile used in the solution of methylene chloride with a concentration of 1.5 - 3%, while for solution of initiator used dry porofor, and the dissolution of porofor in methylene chloride produced using the mixer in additional capacity.

38. The method according to PP.1, 3, 6 and 37, characterized in that use charator in the form of a bubbling apparatus, partitioned perforated the different topics when the chlorination in the lower part of charator serves vaporized chlorine from the buffer capacity, methyl chloride, the solution poroporo and methylene chloride, separated from the reaction mass chlorination, the chlorination is carried out at a temperature of 70 - 80oC and a pressure of 8 7,0 - 8,0 ATA at a molar ratio of chlorine to methyl chloride of 1.9 to 2.1 : 1.

40. The method according to PP.1 and 39, characterized in that the reaction mass leaving charator containing chlorine-methanes and hydrogen chloride, is cooled in the heat exchanger, the cooled brine with a temperature of -8 - -15oC and then in a heat exchanger, cooled by brine with a temperature of -25 to -40oC and with the help of the pump through a hydraulic lock sent to consistently located distillation column continuous action.

41. The method according to PP.1 and 36 to 40, wherein the process is conducted at a molar ratio of the flow rate of the liquid phase at the reactor exit chlorination to the stoichiometrically calculated amount of the source of methyl chloride 3.0 to 3.5 : 1.

42. The method according to p. 40, characterized in that the reaction mass is directed first in the condensation-Stripping tower where the lead Department under pressure 6,8 - 7,5 ATA from the reaction mixture of hydrogen chloride and neprieinama the leading from the upper part of the column of hydrogen chloride and methyl chloride are served in successively spaced heat exchangers, cooled to a temperature (-8) - (-15)oC and (-25) - (-40)oC, respectively, where separate methyl chloride, which is returned to the column in the form of phlegmy, with the withdrawal of the principal amount of methyl chloride in the form of a bottom liquid.

43. The method according to PP.1 and 4, characterized in that hydrogen chloride is used in the stages of hydrochlorination of methanol and obtain hydrochloric acid.

44. The method according to p. 42, characterized in that the portion of the liquid methyl chloride mixed with dissolved hydrogen chloride is withdrawn from the condensing-Stripping distillation columns in the corresponding accumulation tank, and then pump back to the stage chlorination.

45. The method according to PP.43 and 44, characterized in that on-line recycling of methyl chloride establish the adsorber with the zeolite.

46. The method according to PP.42 to 45, characterized in that the cubic liquid from condensation and Stripping column is fed to the column selection methylene chloride, where are the selection of the product under pressure of 2.7 to 3.2 ATA that supports using a pump, if necessary, and supply additional product from the appropriate storage capacity.

47. The method according to PP.41 to 46, characterized in that between the columns rectify is on PP.41 - 47, characterized in that the methylene chloride with a purity of 99.7% is isolated in the form of distillate second column rectification column selection methylene chloride, which is partially selected as the target product.

49. The method according to PP.41 to 48, characterized in that the methylene chloride allocated with a purity of 99.7%, partially or fully returned to the chlorination reactor in case of obtaining the maximum yield of chloroform.

50. The method according to PP.1 to 49, wherein the process is conducted while maintaining the ratio of the obtained chloroform and carbon tetrachloride, determined based on the amount of recycling of methylene chloride.

51. The method according to PP.1 - 50, characterized in that the part recyclization of methylene chloride is directed to the preparation of a solution of porofor used as the initiator of the chlorination process, the remaining portion recyclization of methylene chloride is fed directly to the chlorination reactor.

52. The method according to p. 51, characterized in that on-line recycling of methylene chloride install additional adsorbers with zeolite.

53. The method according to p. 52, characterized in that one every 2 to 4 months carry out the regeneration of the zeolites in the adsorbers.

54. The method according to p. 53, characterized in that RegioC.

55. The method according to p. 53, characterized in that the purge gases after purging sent for incineration.

56. The method according to PP.39 - 53, characterized in that the cubic liquid from the second rectification column with a pump serves as the power of the third column for distillation of her residual methylene chloride.

57. The method according to p. 56, characterized in that the cubic liquid served in such quantity, to ensure that the content of the methylene chloride in the funds allocated to the next column rectification chloroform no more than 0,002%.

58. The method according to PP. 41 - 57, characterized in that the air line connecting the distillation column with the atmosphere, after a dephlegmator install the heat exchanger, the cooled brine.

59. The method according to PP.41 - 58, characterized in that a mixture of methylene chloride and chloroform, taken from the third to the rectification column, refer to the previous power of the second column.

60. The method according to PP.41 - 59, characterized in that in the third column - column distillation of the methylene chloride - set pressure of 2.5 - 3.0 ATA, and pair it condense in the heat exchanger, and condensate, which are a mixture of methylene chloride and chloroform, from the tank by the pump is directed to and served by gravity as a power in the fourth column, at which emit chloroform as the target product.

61. The method according to PP.41 to 60, characterized in that the chloroform release in a fourth distillation column under atmospheric pressure, and couples with the top of the column condense in the heat exchanger and collected in a suitable container from which chloroform pump is directed to the irrigation of the previous columns and selected as the target product with collecting it in an intermediate tank if necessary, and cubic liquid consisting of chloroform and carbon tetrachloride, the pump serves to supply the last fifth column - column distillation of chloroform and allocation of carbon tetrachloride.

62. The method according to PP.41 - 61, characterized in that a pair of top of the last fifth column operating under atmospheric pressure, condensed in the reflux condenser, and a mixture of chloroform and carbon tetrachloride is directed by gravity for irrigation and nutrition of the fourth column.

63. The method according to PP.41 - 62, characterized in that last, fifth column perform with a side selection of the steam space of the cube from which the vapor output target carbon tetrachloride, vapours condense in the heat exchanger and collected in a suitable rechargethe carbon the pump serves in the capacity and output to thermal deactivation.

64. The method according to PP.40 - 63, characterized in that all air lines distillation columns joined together and connected to a canister filled with activated carbon for the adsorption of chlorine-methanes, and regeneration of coal carried out sporadically when breakthrough of chlorine-methanes after adsorbers.

65. The method according to p. 63, wherein the regeneration is carried out at a temperature of 120 - 150oC ferry, which at the outlet of the adsorber condense together with organochlorine products and water in the heat exchanger, cooled by water.

66. The method according to p. 65, characterized in that the chlorinated products are separated from the water in the clarifier is collected in the tank and the pump is sent for incineration.

67. The method according to p. 1, characterized in that the start of the hydrochlorination reactor start with heating it to a temperature of 100 - 105oC, and then begin feeding methanol and hydrogen chloride or concentrated 35 - 45% of hydrochloric acid.

68. The method according to PP.1 - 67, characterized in that before starting the whole system is blown with nitrogen while heating to start the flow of cooling fluids into the respective heat e is I, that heating of the hydrochlorination reactor are performed simultaneously with the heating and reactor startup chlorination of methyl chloride.

70. The method according to p. 69, characterized in that after reaching the boiling temperature in the chlorination reactor establish the working pressure by means of a flow in the nitrogen system, and then begin to apply the solution poroporo in methylene chloride.

71. The method according to p. 70, wherein upon reaching the required concentration poroporo in the chlorination reactor begin to submit methyl chloride and chlorine, with a gradual increase consumption of reagents to a predetermined value.

72. The method according to p. 71, characterized in that when you re-start the system after it is stopped heating reactors operate by pumping the reaction mixture through a heat exchanger, heated by steam, which is fed under a pressure of 2.5 - 3.5 bar (20 - 40 m3/h for 3 to 4 hours or by pumping the reaction mixture through the condensation-Stripping tower.

73. The method according to p. 72, characterized in that the re-runs of the chlorination reactor is heated while filling it with methylene chloride to a temperature of 60 - 70oC and then submit a solution of porofor in methylene chloride, and dostatochino fact, when any system starts the flow of chlorine produced in the last turn, and when any stoppage of the flow of chlorine is stopped in the first place.

75. The method according to PP.1, 40 and 73, characterized in that to achieve a pressure in the chlorination reactor 7 - 8 ATA vaporous products are not removed from the reactor and the liquid phase is poured into the container, and upon reaching a predetermined pressure vaporous products is served on the condensation-Stripping tower and produce the dosage there is a liquid phase from the vessel.

76. The method according to PP.1, 43, 44 and 75, characterized in that after the release of condensation and Stripping columns on the regime and achieve the necessary parameters and compositions of distillate cube and start the selection of hydrogen chloride in phase hydrochlorination of methanol and the output of the bottom liquid of the column, and then make consecutive start system rectification.

77. The method according to PP. 37, 38, characterized in that after the mode of the column selection methylene chloride to produce the start-up stage of preparation of a solution of poroporo.

78. The method according to PP.1, 37 to 40, characterized in that when the temperature in the chlorination reactor is higher than the defined first shut off the flow of chlorine, then the solution poroporo, Metalab on PP.37 - 40, characterized in that when the pressure in the chlorination reactor is higher than the disconnection of the system from the reactor is carried out in the following sequence: chlorine, methyl chloride, recycling of methyl chloride, recycling of methylene chloride and the solution poroporo in methylene chloride.

80. The method according to PP.1 - 79, characterized in that at least the reactor, and/or any vessel, and/or column perform circular or ellipsoidal or oval, or ovoidalnaya shape in transverse and/or longitudinal section and/or in combination, and/or combinations of these configurations.

81. The method according to p. 80, characterized in that at least one accumulation tank perform partitioned at least in the plan.

82. The method according to PP. 1 - 81, characterized in that at least one accumulation tank, and/or the reactor, and/or the column is carried out in a solid combination configuration, including a combination of at least one cylindrical section of the round, and/or ellipsoidal, and/or oval and/or ovoidalnaya configuration with a tapered and/or hyperonymy, and/or combined parcels, including at least one planar face, or at least one insertion of the second, or third, or fourth order curvature.

84. The method according to PP.1 - 83, characterized in that the bottom of the storage tank is performed in the form of a narrowing down of the shell, representing at least part of the body of rotation with a generatrix in the form of unbloody, or branch of a hyperbola, or a combination configuration, including a combination of straight or broken sections or combinations thereof with at least one curved element.

85. The method according to PP. 83 and 84, characterized in that the bottom of the storage tank supply not less than one means to drain that is placed in the bottom of the bottom.

86. The method according to p. 85, characterized in that the means for draining placed symmetrically relative to the vertical axis of the cumulative capacity.

87. The method according to PP. 84 and 85, characterized in that the means for draining placed asymmetrically relative to the vertical axis of the cumulative capacity, mainly in the area adjacent to the side wall of the vessel, and/or at least partially inset in the bottom area of the side wall.

88. The method according to PP. 1 - 87, wherein at least a portion of the wall of the storage tank are in the form of diaphragms made of chemically resistant material.

89. The method according to p. 88, otlichayushchayasya zones cumulative capacity.

90. The method according to PP.1 - 89, characterized in that the axis of at least one accumulation tank is oriented horizontally.

91. The method according to PP.1 - 90, characterized in that the axis of at least one accumulation tank or at least one section of the storage tank is oriented obliquely.

92. The method according to PP. 1 - 91, characterized in that the cumulative capacity do with perception hydrostatic and/or dynamic pressure supplied to it liquid or gas.

93. The method according to PP.1 - 92, characterized in that the delivery of methanol to the place of work carried out in the rail and/or road tanks, and after delivery are overload of methanol to the warehouse.

94. The method according to p. 93, characterized in that the overload of methanol to the warehouse produced by squeezing it in the tank.

95. The method according to p. 94, characterized in that the methanol perelavlivaet in the tank, made of black steel ST3.

96. The method according to PP.1 - 95, characterized in that the reactors, columns and storage tanks are made of black steel ST3 and humorous inside of a vulcanized rubber, over which is applied a layer of the lining of krichayshiy fact, what is the sealing of joints between tiles is carried out by processing Arsenicum.

98. The method according to PP. 1 - 97, characterized in that commodity methyl chloride load in the shipping container and sent to the consumer.

99. The method according to p. 98, wherein the transport containers are used rail and/or road tank black steel ST3.

100. The method according to PP.1 - 99, characterized in that the target chloroform purified sulfuric acid, and then neutralized, and then used for hcfc22 - intermediate for obtaining the fluoropolymer for the production of non-stick coatings, or for the production of aerosols, or in refrigeration.

 

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The invention relates to the development of industrial technology for Pentafluoroethane and/or freon fluoridation of paliperidone - titrator, trifter-defloration or their mixtures with cobalt TRIFLUORIDE

The invention relates to methods of chlorination of paraffins, widely used in polymer compositions as plasticizers in the production of building materials, paints and varnishes, synthetic films and leathers, rubber industry, as well as ontamarama additives to various polymers

The invention relates to chemical technology, namely to methods for 1,1,1-diperchlorate (HFC-142), which is low-toxic and low to the ozone layer of the refrigerant, is used as a refrigerant and as raw material for production of 1,1-defloration (monomer 2)
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