SU352903A1 - METHOD OF OBTAINING PHENYL OR METHYLPHENYLHLOROSYLANEUM ALLOCATION * ^ AYAPAT? -NTY0-T? K1? D, 5US BIBL-11TEN - Google Patents

Description

The invention relates to the field of the production of basic organosilicon monomers, orgaiochlorosilanes (phenyl, methylphenylchlorosilanes, etc.).

The most effective and practically the only industrial method for the preparation of organochlorosilanes is their direct synthesis from the corresponding organic chlorides and silicon-copper contact masses, activated, for example, by zinc fluoride or its mixture with zinc chloride or cadmium chloride.

Many years of experience in the development and mastering of industrial technology for the production of organochlorosilanes by direct synthesis shows that one of the main drawbacks of almost all processes is the instability of their performance, primarily due to the instability of the quality of the original technical silicon.

The properties of the latter, in turn, depend on the deposit and the composition of the micronutrients of natural quartzites, from which silicon is produced, on the raw materials from which quartzite reducing agents are obtained, and so on.

Thus, it is almost impossible to influence the quality of technical silicon; its activity varies widely, causing irreproducibility of the results of organochlorosilane synthesis and often disrupting production during a long period.

The purpose of the invention is to increase the activity of contact masses, improve and stabilize

technical and economic indicators of the process. Found that the activity of silicon-copper contact masses for the direct synthesis of organochlorosilanes, and above all the activity of the masses based on low-quality silicon, can be significantly increased and stabilized at a high level if the inorganic cobalt compound is added to the masses as an activator up to 10% by weight

contact mass.

Activation of the mass does not require additional special technological operations, it is carried out very simply by adding an appropriate amount of activator powder to the reactor before carrying out the process.

At the same time, the productivity of the contact mass (the yield of the target products per unit time per unit mass) and the wall of using silicon during the synthesis cycle (until the mass activity drops sharply) increase more than 2 times.

stainless steel with electrical heating, predgavl y1: n: with a pipe dpametrol 50 mm with con C11: l; 1azors-s :: rsel :: telny device and e1x;: 1X, 3ffpy KE: iOT 20G g of the contact weight from ciiccii iirpoiiiKOB composition,%: med55 27.5, h.tor 1sgogo kpdl; and 2.7, kppsika 1, 7, cobalt oxide 2, silicon - the rest. Gactor is gradually heated in liOTOKe nitrogen to a temperature of 430 ° C, after which chlorine-vapor vapors begin to be supplied. The input rate of chlorobenzene is 40 sj4ac, the temperature in the reactor is 430-440 ° C. During the passage of chlorbepzol for 8 hours, 318 g of a mixture of the composition,%: benzene 5, phenyltranhdoreylaia 16, diphenyl 0.7, dipheyl dihdoreilane 69, triphenylchlorosilane 7, vat residue 1 and 2.3 are obtained.

The capacity of the contact mass is 183 per 1 kg of contact mass.

Under similar conditions with the use of the cream of the same batch without activating the contact mass of cobalt, the capacity of the contact batch is 100 g / hl per 1 kg of mass.

Example 7 Under the conditions described in Example 1, 900 grams of feiylchlorosnlanes are obtained from 1 second silicon of another batch, 27%: Beizole 7, phenyltrichloroilane 19, difesla 0.6 , difepildichloroiaia 65, triphenylchloride 6, the cubic residue 2,4. The yield = - 1 kg of the mass is 50 g / h per 1 kg; Eat a mixture of phenylchloride sludge per cycle (up to coitactic mass testing) 4.5 kg per 1 kg of mass.

In the ayalpichykh ulyuhih e irimeenia cremln of the same batch, without activation by cobalt compounds and the yield of coitactic mass was 64 g / h per 1 kg, we take off ciieei-i phenylchlorosilanes during the synthesis cycle (before mass development) 1.9 kg in weight 1 kg.

E table. 1 compiled the activity of contact;, an ass of the same raw material in the synthesis of phenylchlorosilanes in the same areas (similar to those described in the irimer 1, but with the introduction of chlorobenzene 60 g / h) with addition of cobalt compounds (2% oxide 1: ln 3.5% chloride) and without fir.

T a b; i II c a 1

At m 3. In the reactor, oieyeanny in example 1, load 200 g of coitactic mass nz mixture of powders of the following composition,%: copper 35, cadmium chloride 2, zinc oxide 1, cobalt oxide 2, cremnium - the rest.

The reactor is gradually heated in a stream of nitrogen to a temperature of 37 ° C, after which the mixture of chlorobenzene and chlorine carbon fibers at a rate of 40 and 18 g / h is ejected. During 8 hours of synthesis, 406 g of a mixture of the composition,%: methyldichlorosiliaa 6, trimethylchloroilane 1, methyl trichlorosilane 16, dimethyldichlorosilaia 29, benzene 5, fenpltrichlorosilane 7, methylphenyldichloroilane 18, diphenyldichloroylane iso, isn’l, 15, 34, benzene 5, fenpltrichlorosilane 7, methylphenyldichloroilane 18, diphenyldichloroylane 15 isomer, 15%, mixtures of phenyltrichlorosilane 7, methylphenyldichloroilane 18, diphenyldichloroylane 15 iso, diphenyl dichloroyl isoylane, iso lane, is obtained.

The capacity of the contact mass of methylphenyldichlorosilapa is 46, and according to cm3 of methyltri-, dimethyldi, feiyltri-, methylfepyl- and diphenyldichlorosilapa 218, calculated with 1 kg of contact mass.

Under the conditions of using Tcii silicon in the same batch without activating the co-activity of the cobalt compounds, the performance of the contact mass in meth. Phenyldichlorosilane is 25, and in terms of the amount of methyltri-, dimethyl-, fepyltri-, methylfei-di and diphloridyl chloride, per 1 kg of contact mass.

Example 4. In the reactor described in example 1, load 200 g of contact mass from a mixture of powders of the composition,%: copper 25, cadmium chloride 2, okiyi cobalt 2, KpeiMniy - oetaly. The poitepenpo reactor is heated in a stream of nitrogen to a temperature of 470 ° C, after which the vapors of chlorobenzene (75 wt.%) And trichlorosilane (25 wt.%) Begin to be supplied. A feed rate of 40 ms / h of the mixture is available at a temperature of 470-4-80 ° C in the reactor. During the passage of the reaction mixture for 8 hours of synthesis, 288 g of a mixture of eoetava products,%: silicon tetrachloride 2, benzene 15, phenyltrichloroilane 54, difepil 0.5; diphenyldichloroilane 27, vat of 1.5. The degree of chlorobenzene conversion is 95%, the production capacity is 146 g; 1 hour per hour.

In similar areas without activation of the contact surface of cobalt chlorobenzene copolymer cobalt is 46%, the mass production is 71 g / hour with 1 kg.

table 2

Сё.ч смесн phenylchlorosilanes, kg kg

3.5% of chloride) for the total removal of the mixture of fopilchlorosilanes per synthesis cycle under conditions similar to those described in example 1 (but until the mass activity was drastically reduced) on various silicon samples:;: 1) low activity.

Subject invention

Claims (3)

1. A method for producing phenyl- or methylphenylchlorosilanes by the interaction of organic chloride and promoted silicon-copper contact mass in the presence of an activator, which is characterized by the fact that inorganic cobalt compounds, such as cobalt oxide, are used as an activator. 2. A method according to claim 1, characterized in that the cobalt compounds are taken in an amount of up to 10% by weight of the contact mass. 3. Method but n. 1, characterized in that the process is carried out in the presence of trichlorosilane in an amount of 35 wt. %