SU280477A1 - Method of producing organochlorosilane - Google Patents

Description

From; embedding refers to the preparation of organ and diorganodichlorosilanes of the general formula

RRSiClg

where R and R are alkyl or aryl, R may be N.

A known method of obtaining 0 | rganochlorosilanes is by direct synthesis from organically chloride and creammide (contact mass in the presence of promoters with the introduction of rhyloxanum in the amount of 1-2%.

In order to suppress the formation of low-value reaction products and the new release of diorgano and organodichlorosilanes, it is not necessary to introduce into the reaction at least 10% of organotrichlorosilane based on the weight of organic chloride, which under conditions of synthesis undergoes dissociation.

EXAMPLE 1 A reactor, which is a U-shaped glass tube with a diameter of 10 mm, is loaded with 10 g of powder and silica-copper contact material. After drying in TOiKe of nitrogen, methyl chloride is passed into the reactor for 2 hours at a temperature of 370 ° C to form a catalyst. Then the supply of methyl chloride is stopped, nitrogen is added to the reactor for 3 hours to desorb the reaction products from the surface of the contact mass until they are completely removed.

After desorption, a mixture of methyltrichlorosilane and methyl chloride is fed in a weight ratio of 2: 1 (8 and 4 g / h, respectively). In the course of 1 hour, 9.0 g of a mixture of methyl chlorosyl are obtained.

As a result of the synthesis, the following products are formed (in g):

D.methyldichlorosilane1,421

Three.methylchlo.rsilan0.069

CrCl Chloride0.088

Methyldichlorosilane 0,026

Dmmethylchlorosilane 0.001

Trichlorosilane 0.001

Miscellaneous boilers and products0.009

In a mixture with abusive products receive

7.42 g of methyltrichlorosilane. In this way,

0.58 g of methyltrichlorosilane is preferred in

dimethyldichlorosilane. The content of dimethyldichlorosilane in the resulting products

92.5%, trimethylchlorosilane 4.5%. Attitude

R / C 1 0.98.

Example 2. Example 1 and 1 to a mixture of methyltrichlorosilapa and chloride vengeance in a ratio of 3: 1 (12 and 4 g / hr, respectively) for 1 hour, 14.27 g of methylchlorosilanes are obtained.

Other products are not found. The amount of methyltrichlorosilane converted was 1.42 g. The composition of the products obtained was 96.5% dimethyldichlorosilane and 3.5% trimethylchlorosilane. The ratio R / C1 is 1.04.

EXAMPLE 3 A 23-mm L-shaped silica-copper contact mass is loaded into a reactor, which is a U-shaped glass tube with a diameter of 23 mm. The development and desorption of the mass in a stream of chloristomethyl (25 g / h) is analogous to Example 1. A mixture of 8.75 g of ethyl trne chlorosilane and 16.25 g of ethyl chloride is fed for 1 hour.

As a result of the synthesis, the following products are formed (in g):

Diethyldichlorosilane2.65

Ethyldichlorosilane2,17

Silicon tetrachloride 0,24

Returned to 7.94 g of ethyltrichlorosilane, converted into Diethyldichlorosilane 0.81 g. The composition of the obtained products; 53.5% diethyldichlorosilane and 43.7% ethyldichlorosilane.

Example 4. In an analogy of Example 1 to a reactor, when feeding a mixture of phenyltrichlorosilane and methyl chloride in a ratio of 1.5: 1 (6 and 4 g / hr), for 1 hour, 10.3 g of organochlorosilanes are obtained.

As a result of the synthesis, the following products are formed (in g):

A mixture of methylchlorosilanes3,55

Benzene and chlorobenzene0,062

Methylphenyldichlorosilane 0.227

The composition of the products obtained (in%): A mixture of methylchlorosilanes 92,5

Benzene and chlorobenzene1,6

Methylphenyldichlorosilane5.9

Subject invention

The method of producing organochlorosilals by direct synthesis from organically chloride and a silica-copper contact mass in the presence of promoters with the introduction of organotrichlorosilane followed by isolation of the target

product by known methods, characterized in that, in order to increase the yield of diorgano and organodichlorosyl, organotrichlorosilane is introduced in an amount of less than 10% of the weight of the chloride of organics.