SU919989A1 - Yellow phosphorus purification method - Google Patents

Description

- one

This invention relates to the purification technology of yellow phosphorus, used for the synthesis of various compounds. neny.

; A known method of purification of yellow: phosphorus by treating it with phosphorus trichloride, taken in an amount that provides the P: RSA ratio (0.07-4): at 20–80 ° C 1.; Also known is the method of purification of yellow phosphorus 2 by treating it with a solution containing sulfuric acid, sulfur trioxide and hydrogen peroxide in the following ratio of components, weight:

2; 0-1,8

Sulfur trioxide per0.3–0.7, hydrogen is serous on acid

The closest in technical essence and the achieved result to the pre / 1gamage is the method

purifying raw phosphorus from impurities by vigorously stirring it in a molten state with water and an organohalogen solvent, followed by washing the mixture with hot water (t - 75 s) fed from bottom to top. The treatment is repeated until the content of the solid particles is reduced to 5% or less.

A disadvantage of the known methods is the incomplete purification of yellow phosphorus from organic impurities and iron. .

The purpose of the invention is to achieve complete cleaning.

This goal is achieved by the fact that in a known method, purification of yellow phosphorus by treating it with an organochlorine compound when heated, the process is carried out in the presence of hydrogen peroxide.

At the same time, organochlorine compound and hydrogen peroxide are served in

quantity, ensuring their ratio with phosphorus is equal to (2-j):: (0.03-0.1) ;: 1.

Example 1. In a reactor heated to 50-60 ° C, 100 g of yellow phosphorus with an organic matter content of 0.213% and-iron 0.0032 are loaded under a layer of water. With vigorous stirring, 150 g of carbon tetrachloride and 5 g of technical hydrogen peroxide perhydrol (31%) are added to the reactor. Stirring is carried out for 20 minutes, after which the separated phosphorus is separated, and 150 g of CC.14 and 5 perhydrol are again treated for 30 minutes. After re-treatment, the phosphorus remained practically free of impurities of organic compounds. and iron. The output of phosphorus, which contains almost no impurities, is -, lt. The ratio of hydrogen peroxide: phosphorus, weight. , 0.01: 1 0.03: 1 The degree of purification of phosphora from organic impurities,% The degree of purification of phosphorus from iron,% Experimental conditions

The ratio CHC1 CCIn: P,, weight,% The degree of purification of phosphorus from organic impurities,% 71.2 9.5

The degree of purification of phosphorus from iron,%

Conditions of experience

The optimal ratio of organochlorine reagent hydrogen peroxide and phosphorus is (2-):: (0.03-0.1.):

Thus, the proposed method allows for complete purification.

Example2. In a reactor heated to 50-60 ° C, 100 g of yellow phosphorus containing 0.1 O organic matter and 0.0087 iron are loaded under a layer of water. Then, with vigorous stirring, LOO g of trichlorethylene and 5 g of hydrogen peroxide are added to the reactor. After stirring the mixture for 1 h, the phosphorus is drained from the bottom of the reactor under a layer of hot water with a temperature of 80-90 ° C and analyzed for the content of organic impurities and iron. The degree of purification of phosphorus from organic impurities and iron is almost complete.

The results of the influence of the ratio of hydrogen peroxide and phosphorus on the degree of purification are given in Table. 1. The results of the influence of the ratio of organochlorine compound and phosphorus on the degree of purification are given in Table. 2

Table 1 95.0 82.498.0 SS: P4 3:

table 2

1: 1 2: 1 3: 1 Ts-L 6: 1

92.6 98.0 99.5 100 100: P 005: 1, f 1 h

phosphorus from organic impurities and iron.

Claims (2)

1. The method of purification of yellow phosphorus by treating it with organochlorine 0.05: 1 0.1: 1 0.2: 1 97.5 99.7 100. 99.5100100, T 1 h 98.9 South 100 5 9199896 connection when heated, about t - Sources of information, due to the fact that, when examining them, they are completely free from organic impurities and iron, the process is led to b1. USSR author's certificate the presence of hydrogen peroxide. 5 No. 729123, cl. From 01 to 25/0 7, published 2. The method of pop.1, is different-ay- 1976. u and with the fact that organochlorine 2. USSR author's certificate compound and hydrogen peroxide pod-№763261, cl. From 01 to 25/0 7, published in an amount to provide 1978. their ratio to phosphorus is about 3. US Patent H 212,355, (2-): (0.03-0.1): 1.kl. 23-223, publ. 1938