SU1574611A1 - Method of obtaining selective chelate forming ionite - Google Patents

Abstract

The invention relates to the field of polymer chemistry and allows to obtain a chelating ionite selective for palladium ions, having a high capacity (69.9 - 101.3 mg / g) for palladium ions and a low capacity (0.20 - 0.31 mg / g) for copper ions with their joint presence, which is achieved by treating 1 mol of chloromethylated copolymer of styrene and divinylbenzene with 1 - 2 mol of rhodanine of general formula H ₂ C (O) ⁵ -NH-C = S at 80 - 110 ° C for 10 - 15 h in the presence of triethanolamine. 1 tab.

Description

(21) 4407601 / 31-05

(22) 04/08/88

(46) 06/30/90. Bul No. 24

(71) Kazakh State University named after SM Kirov

(72) E.E.Ergozhin, B.A.Utkalov and V.A. Nazarenko

(53) 678.744.13 (088.8) (56) M Soedova G.V., Bolshakova M.I., Savin S.B. Chelate sorbents based on copolymers of styrene with divinylbenzene. - Journal of analytic chemistry, 1971, v.26, p.2081.

Reactions on polymer substrates in organic chemistry. Ed. P. Ho-jes, J. Sherrington. M .: Mir, 1983 p.565.

(54) TREATMENT OF SELECTIVE CHELATE-FORMING IONITE (57) The invention relates to the chemistry of polymers and allows to obtain a chelating ionite selective to palladium ions, having a high capacity (69.9-101.3 mg / g) for palladium ions and low capacity (0.20-0.31 mg / g) for copper ions with their joint presence, which is achieved by treating 1 mol of chloromethylated copolymer of styrene and diphenylbenzene 1-2 mol of rhodanine v-O g

of the formula H4C-C (0) -NH-C S at 80-110 ° C for 10-15 hours in the presence of triethanolamine. 1 tab.

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The invention relates to polymer chemistry, namely, a method for producing a selective chelating ion exchanger, and can be used to create heterogeneous homogeneous catalysts, sorbents for chromatographic separations in biotechnology, analytical chemistry and hydrometallurgy for the selective extraction of palladium ions from solutions.

The aim of the invention is to increase the selectivity and binding ability of an ion exchanger with respect to palladium ions.

An industrial granular macroporous chloromethylated styrene copolymer containing

102; divinylbenzene and 21.3% chlorine, having an average granule size of 0.25 0.50 mm. As a chelating agent used rhodanine formula

about with

I

H, Cv

sh

cl

vj

four

Cft

on TU 6-09-14-1830-75. .

The invention is disclosed by the following examples.

Example 1: A three-necked reactor equipped with a reflux condenser, a thermometer and a mechanical stirrer is charged with 1.65 g (0.01 basis mole) of 0.25-0.5 mm HMS granules; 2.66 g (0.02 mol) of rhodanine and 15 ml of triethanolamine. Reaction mixture

heated at 110 ° C with stirring for 10 hours. Then the mixture is cooled, the ion exchanger granules are washed with water from an excess of rhodamine and triethanolamine to colorless wash water, washed with sulfuric ether in a Soxhlet apparatus and dried at 80 ° C to constant weight. The yield of the resin exchanger is 2.18 g. According to the elemental analysis data, the product contains 12.1% sulfur. The static exchange capacity of the sorbent for palladium ions is 89.7 mg / g (pH 0.40), copper 0.21 ml / g (pH 4.35). The coefficient of selectivity of the sorption of palladium and copper ions from solutions containing their equivalent amounts at pH 2.97 calculated by the formula

d - with

| -.

m

CU

m

RS

where m and m are the equilibrium concentrations

corresponding ions in the ion exchanger phase

and in solution, is 1.6-103,

The synthesized ionite is a spherical granule of light brown color, insoluble in acids. In the IR spectrum of the ion exchanger, characteristic rhodanine spectra of absorption bands appear in the region of 1720 and 1230 cm 1, which refer to stretching vibrations and groups.

EXAMPLE 2 The preparation method is carried out as in Example 1, but in contrast, the synthesis is carried out for 15 hours. The yield of the ion exchanger is 2.32 g. According to the elemental analysis, the product contains 14.7% sulfur. The static exchange capacity for palladium ions is 101.2 mg / g, for copper ion, 0.20 mg / g, and the selectivity coefficient T Co is 6 ,.

EXAMPLE 3. The preparation method is carried out as in Example 1, but in contrast, the process is carried out at 100 ° C for 8 hours and used at 1.65 XMC (0.01 basis-mole) 2.0 g (0.015 mol) of rhodanine. The yield of ion exchanger is 2.1 g. The product contains 11.0% sulfur. The static exchange capacity for palladium ions is 69.9 mg / g, for copper ions, 0.25 mg / g, the T Cu selectivity is

4.2-102.

EXAMPLE 4. The method is carried out as in Example 1, but in contrast, the synthesis is carried out for 12 hours,

at 100 ° C, using 1.65 g (0.01 basis-mol) CMS 2.0 g (0.015 mol) of rhodanine. The yield of ion exchanger is 2.18 g. The static exchange capacity for palladium ions is 78.4 mg / g, copper 0.22 mg / g. The coefficient of selectivity T is equal to 8.1-102 PRI me R 5 (control). The method is carried out as in example 1, but in contrast, the synthesis is carried out for 18 hours at 120 ° C and used on 1.65 g (0.01 basis-mole) CMS

2.0g (0.015 mol) of rhodanine. The yield of ion exchanger is 2.35 g. According to elemental analysis data, the polymer contains 13.2% sulfur. The static exchange capacity for palladium ions is 100.9 mg / g, for copper ions, 0.23 mg / g. The coefficient of selectivity T ffd is equal to

5.1-SW.

PRI me R 6 (control). The method is carried out as in Example 1, but in contrast, the synthesis is carried out for 15 hours, taking per 1.65 g (0.01 basis-moles) of CMS 3.06 g (2.3 mol) of rhodanine. The yield of ion exchanger is 2.38 g. According to elemental analysis, the product contains 14.8% sulfur. Its static exchange capacity for palladium ions is 101.3 mg / g for copper ions, 0.26 mg / g. The coefficient of selectivity T is 6.4--103.

Example (control). The method is carried out as in Example 1, but in contrast, the synthesis is carried out for 15 hours and 0.93 g (0.7 mol) of rotanin is used for 1.65 g (0.01 basis-mole) CMS. Ionite yield It is 1.96 g. According to elemental analysis, the ion exchanger contains 10.7% sulfur. Its static exchange capacity for palladium ions is 59.6 mg / g, for copper ions, 0.6 mg / g. The coefficient of selectivity T is equal to 1.4.102.SU

Pr and Ne 8, The method is carried out as in Example 1, but in contrast, the synthesis is carried out for 15 hours at 80 ° C. The yield of the ion exchanger is 2.23 g. According to the elemental analysis data, the product contains 13.0% sulfur and has a static exchange capacity for palladium ions 91.3 mg / g, for copper ions O, 30 mg / g. The selectivity coefficient T QO is 1.2103.

PRI me R 9 (control). The method is carried out as in example 1, but in contrast, the synthesis is carried out in

515

for 15 hours at 70 ° C. The yield of the ion exchanger is 2.13 g. The product obtained contains 11.8% sulfur. The static exchange capacity for palladium ions is 70.1 mg / g, copper 0.30 mg / g. The coefficient of selectivity T is equal to 3.7 J2. The separation is carried out over the entire pH range. Carrying out the process at a temperature of less than 80 ° C for less than 10 hours and using CMS less than 1 mole of rhodanine per 1-mole results in a product with a reduced sorption capacity with respect to palladium ions. Increasing the amount of rhodanine more than 2.0 mol per 1 basic mole of CMS, the reaction time is more than 15 hours and temperatures above 110 ° C is impractical because it does not increase the sorption capacity of the product and increase its selectivity.

Data on the properties of a chelating ion exchanger are given in the table.

Claims (1)

Invention Formula A method for producing a selective chelating ionite by treating a chloromethylated crosslinked styrene-divinylbenzene copolymer with a chelating agent when heated, characterized in that rohanine, of general formula about ssh about and the process is carried out at a molar ratio of chloromethylated crosslinked copolymer: rhodanine, equal to 1.0: 1,0116 2.0 at 80-100 ° C for 10-15 hours in triethanolamine. Properties of selective chelating ion exchangers  A copolymer of styrene and divinylbenzene, aminated, diazotized and treated with rhodanine, containing diazo groups. ) Copolymer of chloromethylated cross-linked styrene copolymer, treated with isooctylthioglycollate. Binding was carried out at 0.1N. NSYu-.