The method of producing chlormethyl

 

(57) Abstract:

Usage: in synthesis of halide Akilov, in particular, chlormethyl, which is used as an intermediate in the synthesis of methylchlorosilanes, solvents. The invention is: to increase the output of chlormethyl and suppress the formation of by - product-dimethyl ether - synthesis lead to a large (2 or more moles of a) the excess of hydrogen chloride in the presence of a catalyst in two stages. In the first stage at room temperature produces a saturated solution of hydrogen chloride in water-methanol mixture, and then heating the resulting solution to 106 - 110oC, emit gaseous methyl chloride. To use the excess hydrogen chloride VAT residue recycle on site saturation. 1 C. p. F.-ly.

The invention relates to the synthesis of alkylhalogenide, in particular to a method for producing methyl chloride, which is used as a solvent and the starting material at the receiving methylchlorosilanes.

A known method of producing chlormethyl hydrochloridebuy methanol with redistribution of the injected methanol [1] in aqueous medium at a temperature of 100 - 200oC and a pressure of 1 to 5 ATM. in precursores lead to three, series-connected reactors, and more than 95% of Hcl fed to the first reactor together with 30 to 40% methanol. The remaining 70% of the methanol is distributed between the reactors.

The redistribution of the injected methanol enables to maintain the selected ratio of CH3OH: HCl and reduce the formation of unwanted by-product dimethyl ether. The degree of conversion of methanol of 97.8%

The disadvantage of this method is:

1. the formation of methyl ether; 0,53% source of methanol consumed in the formation of dimethyl ether.

2. leaving the last reactor weak solution of Hcl contaminated with chloride of zinc.

The purpose of this invention is the elimination of these shortcomings.

This goal is achieved by the fact that pre-get rich water-methanol solution of hydrogen chloride at room temperature and in the presence of aniline as a catalyst, followed by heating the resulting solution to 110oC and separation of gaseous chlormethyl. The resulting after separation of the methyl chloride waste liquid is recycled to the stage of saturation. The use of a threefold excess of hydrogen chloride ru is 1 mol) of methanol, busy 36,6 g (1 mol) of hydrogen chloride at a temperature of 10 20oC add 441,2 g (4 mol) of a 33% aqueous solution of hydrogen chloride. The mixture is heated to 106 110oC, while methylene chloride is withdrawn from the reaction mass in the form of gas, which, after washing-off of hydrogen chloride condense. Cubic liquid after removal of the hydrogen chloride, return to the node saturation.

Get chloromethyl, not containing methanol and dimethyl ether. Conversion of methanol 98,9%

Example 2. The reactor is placed 32 g (1 mol) of methanol and 218 g of a bottom liquid containing up to 0.1% of methanol and the remainder of the hydrogen chloride to 20% miss 36,6 g of hydrogen chloride. The mixture is heated to 106oC. the released gaseous methyl chloride is washed with water from hydrogen chloride, dried and condensed. Conversion of methanol 99% VAT residue after removal of the methyl chloride recycle on the stage of saturation.

Example 3. Into the reactor containing 32 g (1 mol) of methanol, 221,2 g bottom liquid and 0.03 aniline, miss 36,6 g of hydrogen chloride with 5 - 20oC. the Mixture is heated to 110oC. the Released gaseous methylene chloride washed and condense. Get chloromethyl, not containing dimethyl ether. oredom in the aquatic environment at a temperature of 106 110oC and a pressure of 0 to 3 ATM with the separation of the reaction mass to the target product and cubic liquid, a water-methanol solution of hydrogen chloride, wherein the process is conducted in three or more molar excess of hydrogen chloride, which pre-saturate the original methanol, with recirculation above the bottom of the liquid.

2. The method according to p. 1, wherein the process is conducted using a catalyst amine type, such as, aniline.

 

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