SU854939A1 - Method of producing sorbent for iron extraction from salt solution - Google Patents

Description

The invention relates to a method for producing nitrogen-containing polymeric sorbents for the extraction of iron from salt solutions in the production of chlorine and caustic by mercury and diaphragm methods. Known and used in industry as a sorbent for extracting iron from salt solutions methylcellulose, EDE-10P anion exchange resin, containing in its structure primary secondary and tertiary amino groups Cl. The disadvantage of using methylcellulose is the low degree of brine purification. The EDE-UP anion exchanger is effective when used in acidic media (iron capacity at PH2J2-3 1.76 m-g - eq / g). The closest in technical essence to the present invention is a method of obtaining anion exchange resin capable of sorbing iron by reacting a styrene-maleic anhydride copolymer with diethylene glycol and pyridine in benzene when heated, followed by aminating with gaseous ammonia 2. metals, however, the technology of their production is difficult, suggests the use of a large number of α-reagents, including toxic pyridine. The purpose of the invention is to simplify the technology of sorbent production. The goal is achieved in that according to the method of obtaining a sorbent for extracting iron from brine by reacting a styrene-maleic anhydride copolymer in a solvent, when heated, amines or a mixture of amines with two or more reactive primary or secondary amino groups are used as the aminating agent. For the purpose of utilization of production wastes, a mixture of 20-30 wt.% Di- is used as the aminating agent. ethylene triamine, 30-40 wt.% K- (2-aminoethyl) piperazine, 20-30 wt.% triethylene tetramine and 5-10 wt.% higher polyethylene polyamines. Alcohol or ketone or cyclic ether is used as a solvent. This mixture of amines is a by-product of the production of ethylene diamine, and therefore its use is economically viable.

As amines can be used individual listed amines, as well as ethylenediamine.

The advantage of using this nitrogen-containing sorbent is a high degree of iron extraction from brine, as well as ease of manufacture of the sorbent.

Example 1. In a three-neck, equipped with a mechanical stirrer with a thermometer and reflux condenser, loading of 20 g (1M) styromal (mol, chain weight) in 200 ml of 1,4-dioxane and heated until the copolymer dissolves at the boiling point of dioxane, then 10.3 g (0.1 M) diethylenetriamine at this temperature. The reaction mixture is heated at 100-105 ° C for 5 hours. The precipitate obtained is washed with distilled water and dried at. 28.4 g (94%) of product are obtained, mp. 263-2bbs.

Example 2. Under conditions analogous to example 1, 20 g (-0.1 M) styromal was charged into 200 ml of dioxane and 12.9 g (0.1 M) of N-p -s1-aminoethylpiperazgine was added, heated at 100 -120 s for 4 h. The precipitate is washed with distilled water, dried at lOO-llO C. 31.9 (96%) of product are obtained, charring temperature 20Q ° C.

Example 3. Under the conditions of example 1, 20 g of styromal is loaded into 200 ml of acetone and heated at the boiling point of acetone until complete dissolution, then 14.6 g (0.1 M) of triethylene tetramine are added. The reaction mixture is heated for 5 h at bO-b3 C. The precipitate is washed with water, dried by the above method. 31.8 g (92%) of the product are obtained, t. Pl. 268-272С.

Example 4. In the conditions of example 1, a modification of 20 g (0.1 M) of styromal in 200 ml of ethyl alcohol with 6 g (0.1 M) of ethylenediamine at 7585 ° C gave 25.2 g (97%) of product, mp. . 340 ° C

Example 5. Under the conditions of example 1, to 20 g of styromal in 200 ml of dioxane was added 13 g of polyethylene polyethylene composition, wt%: diethylenetriamine 20-30; N-f-11minoethylpiperazine 30-40; triethylene tetramine and higher polyethylene polyamines 20-30 are heated at lOO-llO C for 5-6 hours. The precipitate is washed with distilled water, dried at 90 ° IOS. Poluchens. 29.7 g (90%), so pl. 258-264C.

Comparative results, purification of brine from the iron of the proposed sorbent and methylcellulose are given in the table.

As can be seen from the danich table, the sorption capacity of the proposed sorbents is 10–13% higher than that of methylcellulose.

Claims (2)

1. A method for producing a sorbent for extracting iron from brine by reacting a copolymer of styrene and maleic anhydride with an aminating agent in a solvent when heated, characterized in that, in order to simplify the technology. obtaining a sorbent, amines or a mixture of amines with two or more reactive primary or secondary amine groups are used as the aminating agent. 2, the method according to claim 1, about tl and h and y- "Q y and with the fact that, in order to dispose of waste / production, a mixture of 20-30 wt.% Diethylenetriamine, 6 30- 40% by weight of N- (2-aminoethyl) piperazine, 20-30% by weight of triethylene tetramine and 5-10% by weight of higher polyethylene polyamines. 3. The way pop. 1, characterized by the fact that alcohol or ketone or cyclic ether, is used as a solvent,. Sources of information taken into account in the examination 1. Saldadze KM and etc. Ion exchange high molecular compounds. M., Goskhimizdat, 1960, p. 20. 2. Patent of France No. 1466860, cl. C .08 f, pub. 1967 (prototype).