SU1479411A1 - Method of producing polymerig phosphorus monoxyde - Google Patents

Abstract

The invention relates to the chemistry of phosphorus compounds, in particular, to the technology of producing polymeric phosphorus monoxide used in organic and organoelemental synthesis. The aim of the invention is to increase the yield of the product. The method consists in mixing red phosphorus with an equimolar amount of hexamethyldisiloxane and air oxidation in the presence of copper monochloride in an amount of 0.0005-0.001 g / mol red phosphorus at the boiling point of hexamethyldisiloxane.

Description

one

The invention relates to the chemistry of phosphorus compounds, in particular, to the technology of producing polymeric phosphorus monoxide used in organic and elemental organic synthesis.

The aim of the invention is to increase the yield of the product.

Example 1. A mixture of 3.1 g (0.1 mol) of red phosphorus and 16.2 g (0.1 mol) of hexamethyldisiloxane in the presence of 0.00005 g of copper chloride (1) is boiled for 2 hours while blowing air. The desired product is isolated by filtration and washed 2-3 times with a solution of aqueous ammonia, alcohol, and absolute ether. Output 3,05 g (65% of theoretical) black or dark brown powder of polymeric phosphorus monoxide.

Found,%: P 66.24, 0 33.60.

Calculated,%: R 65.96, O 34.04. I

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IR spectrum (cm -1): 470 (P-0); 1050-1200 (oasP-0).

Polymeric phosphorus monoxide is X-ray amorphous, under high vacuum (5 mm Hg) does not decompose to 400 ° C and does not sublimate. It ignites in air at temperatures above 230-240 ° C. The compound is insoluble in most organic solvents and water.

Example 2. A mixture of 6.2 g (0.2 mol) of red phosphorus and 24.3 g (0.15 mol) of hexamethyldisiloxane is boiled in the presence of 0.0001 g of copper (I) chloride for 2 hours.

Yield 6.05 g (63%).

Example 3. A mixture of 3.1 g (0.1 mol) of red phosphorus and 16.2 g (0.1 mol) of hexamethyldisiloxane in the presence of 0.0001 g of copper (I) chloride is heated to 80CC for 2 hours.

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CO 4b

31479411

Yield 6.01 g (62%), the product is contaminated with impurity red phosphorus in the amount of 0.2-0.3 g.

Example 4. A mixture of 3.1 g (0.1 mol) of red phosphorus and 8.1 g (0.05 mol) of hexamethyldisiloxane in the presence of 0.0001 g of copper (I) chloride is heated to boiling (SO) for 2 hours. Jq

Yield 6-, O g (61%), the product is heavily polluted with red phosphorus sublimated in vacuum.

Example 5. A mixture of 3.1 g

Example 7. The process is carried out analogously to example 6 in the presence of 0.001 g of copper (I) chloride.

The yield of the target product is 30.2 g (63%).

Example 8. The process is conducted in the presence of 0.00075 g of copper (I) chloride.

The yield of the target product is 29.4 g (60%).

Reducing the addition of honey chloride to values less than 0.0005 g / mol results in as

(0.1 mol) of red phosphorus and 16.2 g of J5 mixture of the starting red phosphorus, (0.1 mol) of hexamethyldisiloxane in the presence of 0.0001 g of copper (I) chloride are boiled (100 ° С) for 1.5 h, blowing air.

Yield 6.01 g (62%); the product is partially contaminated with red phosphorus sublimated in vacuum.

Example 6. A mixture of 31 g (1 mol) of red phosphorus and 162 g (1 mol) of hexamethyldisiloxane in 25 in the presence of 0.0005 g of copper (I) chloride is boiled for 2 hours while blowing air. The treatment of the reaction product is carried out analogously to example 1.

Claims (1)

which must be removed from a horse product by sublimation under vacuum Increasing the amount of honey chloride to more than 0.001 g / mol does not make more effective The formula was invented A method for producing polymeric phosphorus oxide m, which is different in that, in order to increase the course of the product, red phosphorus is mixed with equimole a substantial amount of g of samythyl disiloxane and oxidized with air oxygen in the presence of monochloride copper, used in the amount of 0.0005-0.001 g / mol red Yield 29.5 g (61%) of polymeric mono-30 Phosphorus, at boiling point Example 7. The process is carried out analogously to example 6 in the presence of 0.001 g of copper (I) chloride. The yield of the target product is 30.2 g (63%). Example 8. The process is conducted in the presence of 0.00075 g of copper (I) chloride. The yield of the target product is 29.4 g (60%). The reduction of copper chloride additives to values less than 0.0005 g / mol results in starting red phosphorus as a mixture, the mixture of the original red phosphorus, which must be removed from the final product by sublimation under vacuum. An increase in the amount of copper chloride more than 0.001 g / mol does not produce an effect. DETAILED DESCRIPTION OF THE INVENTION Method for producing polymeric phosphorus monoxide, characterized in that, in order to increase product yield, red phosphorus is mixed with an equimolar amount of hexamethyldisiloxane and oxidized with oxygen in the presence of copper monochloride used in an amount of 0.0005-0.001 g / mol red phosphorus oxide. hexamethyldisiloxane.