The method of producing methyl chloride

 

(57) Abstract:

The present invention relates to bezkatalizatorny process for the production of methyl chloride by reacting hydrogen chloride with methyl alcohol in the liquid phase and can be used in the chemical industry. The technical objective of the proposed invention is to increase the conversion of hydrogen chloride, reducing the temperature and pressure of the production of methyl chloride. This result is achieved by the fact that carry out interaction of hydrogen chloride with methyl alcohol in the absence of a catalyst with the formation in the reaction zone of the organic and aqueous components of the reaction mixture with the release of methyl chloride from the organic component, and hydrogen chloride and methyl alcohol interaction serves a counter-current swimming and water component continuously away from the reaction zone; in addition, it is possible to conduct the salt distillation of the water component of the aqueous solutions of metal chlorides with the release of hydrogen chloride and methyl alcohol is carried out in a stoichiometric ratio. 2 E. p. F.-ly, 1 tab., 1 Il.)s

The present invention relates to bezkatalizatorny ways PTI used in the chemical industry.

Known methods for producing methyl chloride in the liquid phase without the use of a catalyst. For example, a known method of producing methyl chloride, in accordance with which the process is carried out in a capacitive reactor operating under pressure to 3 ATM when heated with an excess of one of the original components with the implementation of recyclo the reaction mixture as in the main reactor and auxiliary equipment, which complicates the process flow and process management. In addition, the reactor complete mixing does not provide effective separation of gas and liquid phases, which causes the need for additional hardware and leads to high energy consumption [1]

A known method of producing alkylchloride on which the process is carried out in the device column type at high pressures (up to 27 ATM) in excess of hydrogen chloride with the filing of the initial reagents in a column parallel and implementation recyclo the reaction mixture, which leads to the need for special equipment and high energy consumption [2]

The closest in technical essence to the proposed solution is the method of producing methyl chloride, in which the process is carried out in a column equipped with the East of hydrogen with methyl alcohol in the absence of catalyst with the formation in the reaction zone of the organic and aqueous components of the reaction mixture and the release of methyl chloride from the organic component. The filing of the original components carry out parallel, and the process is carried out at high pressure (10 ATM); the use of excessive quantities of methyl alcohol (20% to 200%) can increase the degree of conversion of hydrogen chloride from 70% to 95% of the process carried out by heating (100oC-200oC).

The disadvantages of this method are the following. The use of excess amounts of methyl alcohol leads to the necessity of creating recyclo liquid phase, along with the implementation of the basic process at elevated temperature and pressure leads to increased energy consumption and complicates the selection and operation of the main technological equipment; in addition, excess alcohol leads to the formation of dimethyl ether, polluting methyl chloride.

An object of the invention is to increase the conversion of hydrogen chloride, reducing the temperature and pressure of the production of methyl chloride.

This result is achieved in that a method of producing methyl chloride is carried out by interaction of hydrogen chloride with methyl alcohol in the absence of a catalyst with the formation in the reaction zone of the organic and aqueous sostavlyayuscyeye alcohol interaction serves a counter-current swimming and water component continuously away from the reaction zone; in addition, it is possible to conduct the salt distillation of the water component of the aqueous solutions of metal chlorides with the release of hydrogen chloride, which is returned to the reaction zone, the feed of hydrogen chloride and methyl alcohol is carried out in a stoichiometric ratio.

The method is as follows. Hydrogen chloride in the gaseous state are served in the lower part of the synthesis reactor (Fig. 1), and liquid methyl alcohol in its upper part. In the counter-current interaction of the source reagents are formed methyl chloride and water. Methyl chloride is removed from the upper part of the reactor and sent to a condensing system, where you catch the vapors of methyl alcohol, returning them to the synthesis reactor. The water with dissolved hydrogen chloride moves down the reactor, accumulating her away from the cube-heater in the form of hydrochloric acid with a concentration of hydrogen chloride is close to 20% wt. The temperature in the cube when it was 108oC-110oC, and the temperature along the height of the reactor was changed from the 50oC to 90oC. Resulting in the synthesis of methyl chloride, the water slows the interaction of initial reagents and binds to part of the hydrogen chloride in the area of the th tap of the last of the zone of fusion.

For carrying out the process of obtaining methyl chloride as a reactor can be used distillation column (see drawing).

The method provides for the possibility of filing in the lower part of the reactor aqueous solutions of metal chlorides, for example, chlorides of calcium or magnesium to process salt distillation of hydrochloric acid. Vydelyayuschiysya while hydrogen chloride flows upward through the reactor together with the main flow is involved in the synthesis, which enables to increase the conversion rate of hydrogen chloride with 88,9% to 99.3% and to file the original components in stoichiometric ratio. As a consequence, the probability of formation of dimethyl ether is significantly reduced. The spent solution of metal chloride away from the cube-heater and is directed to the regeneration of known methods, and the solution was again returned to the process. The temperature in the cube is 120oC-130oC, and the reactor 60oC-110oC. Pressure in the reactor is determined by the resistance of the system and does not exceed 1.15 ATM.

Thus, in the proposed method of carrying out counter-current interaction of methyl alcohol and hydrogen chloride with simultaneous continuous Otwock temperature and pressure synthesis.

The method is illustrated by the following examples.

Example 1. Gaseous hydrogen chloride in the amount of 17.1 g/h and liquid methyl alcohol in the amount of 13.5 g/hour was applied to the reactor after its release on the stationary operating mode; when the steady-state operating temperatures and stable yield of methyl chloride were selected for analysis of liquid and gas phase. The amount of methyl chloride withdrawn from the upper part of the reactor was 21 g/hour, and the amount of exhaust from the cube-heater hydrochloric acid was 9.4 g/hour (when the content of hydrogen chloride of about 20% wt.). The content of methyl chloride in the gas phase (after cooler) not less than 98,5% by weight. methyl alcohol to 1.5% wt. Conversion of initial reagents in methyl chloride was: hydrogen chloride 88,9% methanol 98.5% of the Temperature in the upper part of the reactor 48oC-53oC, in the zone of introduction of hydrogen chloride 85oC-92oC, in the cube 108oC-110oC; excess pressure in the synthesis process does not exceed 0.15 ATM.

Example 2. Gaseous hydrogen chloride in the amount of 15.3 g/h and liquid methyl alcohol in the amount of 13.5 g/h, and 52% aqueous solution of calcium chloride in the amount of 16.6 g/hour was applied to the reactor after its release on the STI on the analysis of liquid and gas phase. The amount of methyl chloride withdrawn from the upper part of the reactor was 21 g/hour, the amount of exhaust from the cube of an aqueous solution amounted to 24.2 g/h, which contained about 36 wt.%. calcium chloride and 0.5% wt. hydrogen chloride. The content of methyl chloride in the gas phase (after cooler) not less than 98,5% by weight. and methyl alcohol not more than 1.5% wt. Conversion of initial reagents in methyl chloride was: hydrogen chloride 99.3% of methyl alcohol, 98.5% of the Temperature in the upper part of the reactor 60oC-65oC, in the feed area of the calcium chloride 110oC-116oC, in Cuba 121oC-127oC; excess pressure in the synthesis process does not exceed 0.15 ATM.

Example 3. Gaseous hydrogen chloride in the amount of 15.3 g/h, liquid methyl alcohol in the amount of 13.5 g/hour and 42% aqueous solution of magnesium chloride in the amount of 28.2 g/hour was applied to the reactor after its release on the stationary operating mode; when the steady-state operating temperatures and stable yield of methyl chloride were selected for analysis of liquid and gas phase. The amount of methyl chloride withdrawn from the upper part of the reactor was 21 g/hour, the amount of exhaust from the cube-heater aqueous solution was equal to 35.8 g/h, containing about 33% by weight. chimenea to 98.5 wt. and methyl alcohol not more than 1.5% wt. Conversion of initial reagents in methyl chloride was: hydrogen chloride 99.3 percent methyl alcohol 98.5% of the Temperature in the upper part of the reactor 60oC-65oC, in the area of supply of a solution of magnesium chloride 102oC-110oC, in a cube 122oC-126oC; excess pressure in the synthesis process does not exceed 0.15 ATM.

In all experiments, the content of hydrogen chloride was determined by titrimetric and methyl chloride and methyl alcohol by gas chromatography; the duration of the experiments 3-6,5 hours.

Data examples are summarized in table N-1, for comparison it also shows the data of the prototype.

Analysis of the solutions taking into account the achieved technical result allows to conclude that the proposed decision criteria invention of "novelty" and "inventive step". Examples of implementation of the proposed solution confirm its compliance with the criterion of "industrial applicability".

Literature

1. U.S. patent N 3983180, publ. 28.09.1976.

2. U.S. patent N 3981938, publ. 21.09.1976.

3. European patent N 0352799b1, publ. 18.03.92 (prototype).

1. The method of obtaining the promotional area of the organic and aqueous components of the reaction mixture and the release of methyl chloride from the organic component, characterized in that hydrogen chloride and methyl alcohol interaction serves a counter-current swimming and water component continuously away from the reaction zone.

2. The method according to p. 1, characterized in that the aqueous component is subjected to salt distillation of aqueous solutions of metal chlorides with the release of hydrogen chloride, which is returned to the reaction zone.

3. The method according to PP.1 and 2, characterized in that the interaction of hydrogen chloride and methyl alcohol is carried out in a stoichiometric ratio.

 

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