SU1273154A1 - Method of producing sorbent for extracting ions of metals from solutions - Google Patents

Abstract

This invention relates to a process for the preparation of sorbents and permits a reduction in the duration of the process for the preparation of a sorbent. Example. To the silochrome, C-80 with the grafted α-aminopropyl groups. Pour a solution of monoiodbctic acid in ethanol and triethylamine. The slurry is boiled with stirring under reflux. The resulting sorbent is washed with ethanol and water. The capacity of the obtained sorbent for copper ions is 0.11-0.14 mg eq / g. The proposed method makes it possible to reduce the process time to 3–7 hours and to reduce the consumption of the complexing agent by a factor of 310. 1 hp f-ly, 1 tab.

Description

u 1

SAE SP

412

The invention relates to a process for the preparation of sorbents, which can be used for the extraction and separation of metal ions, in particular by chromatography.

The purpose of the invention is to reduce the duration of the process of obtaining the sorbent.

Example 1. To obtain a sorbent, a solution of 1.85 g of monoiodoacetic acid in 40 ml of ethanol and 1.4 ml of triethylamine is poured into 10 g of silochrome C-80 with grafted y-aminopropyl groups {0.3 mmol / g). The suspension is boiled with stirring under reflux for 3 hours. The resulting sorbent is washed with ethanol and water. The capacity of the obtained sorbent for copper ions Oh, 1 mg eq / g, which corresponds 0,414 groups / nm.

PRI mme R 2. All operations are similar to those shown in Example 1, except for taking a solution of 5.55 g of monoiodoacetic acid in 50 ml of ethanol and 4.2 ml of diethylacine. The capacity of the obtained sorbent for copper ion is 0.085 mEq / g, which corresponds to VT 0.320 groups / nm.

EXAMPLE 3 Analogously to Example 2, only processing is carried out for 4 hours. The capacity of the obtained sorbent for copper ions is 0.089 mg-eq / g, which corresponds to 0.335 groups / nm2.

 Example4. Analogously to example 2, only the treatment is carried out for 7 hours. EM bone of the obtained sorbent for copper ions is 0.077 mg-eq / g, which corresponds to 0.29 groups / nm.

Example 5. To obtain a sorbent, a solution of 2.78 monoiodoacetic acid in 50 ml of ethanol and 4.2 ml of triethylamine is added to 5 g of silochrome C-80 with grafted f-aminopropyl groups. The suspension is boiled with stirring under reflux for 7 hours. The resulting sorbent is washed with ethanol and water. The capacity of the sorbent for copper ions is 0.139 mg-eq / g, which corresponds to 0.523 groups / nm.

EXAMPLE 6 Analogously to Example 5j, only triethylamine is taken in an amount of 2, ml and the reaction is carried out for 3 hours. The capacity of the obtained sorbent for the copper ion is 0.137 mg-eq / g, which corresponds to 0.516 groups / nm.

Example7. The table shows the conditions of the method and product characteristics. The amount of reagents is given in grams and mmol x per gram of C-80 silica modified with U-aminopropyltriethoxysilane (the capacity of the initial sorbent is 0.30 mmol / rj.

EXAMPLE 8 To obtain a sorbent, a solution of 3.4 g (3 mmol per g) of monochloroacetic acid in 60 ml of ethanol (a and 5 ml (3 ml)) is added to 12 g of silochrome C-120 with grafted I-aminopropyl groups. mmol / g) of triethylamine. The suspension is boiled under stirring under reflux for 3 hours. The resulting sorbent is washed with distilled water.

The capacity of the obtained sorbent for copper ions is 0.10 mEq / g, which corresponds to 0.251 groups / nm {

EXAMPLE 9 To obtain a sorbent, a solution of 25.9 g of monoiodoacetic acid in 300 ml of ethanol and 19.5 ml of triethylamine is poured into 20 g of aerosil A-175 with grafted α-aminopropyl groups. The suspension is boiled under reflux with stirring for 3 hours. The product is washed with ethanol and water. The study of the obtained sorbent using the method of Z-spectroscopy shows the presence of. The sample spectrum of the absorption bands in the region of 2960 and 1460-1480 cm, which correspond to the C – H vibrations of the absorption band in the 1670 cm region of the corresponding vibrations of the carbonyl group.

and r and mep 10. The study kio - about 4-o-f

non-sorption of Si., 4i -, With the method of pH-stat. A silochrome C-80 sorbent with grafted iminodiacetate groups is placed in a recirculation cell and a 0.0 M solution of transition metal nitrate is pumped through it. Complexation occurs between the metal ions and the functional groups grafted to the surface with the equivalent amount of protons into the solution. This method makes it possible, by adding a measurable amount of alkali, to maintain a constant pH in the solution. The rate of alkali can be judged on the kinetics, 2-1 - „. A-b, 2 +

With at

sorption of ions of Cu, Ny

given pH, the difference - the amount of sorbed metal. In 3-5 minutes, sorption of “90% of the metal ion occurs. The complete process ends for any conditions in 30-60 minutes.

31273

A comparison of the proposed method e known shows that the process time is reduced from 2.0 to 3-7 hours, and the consumption of the complexing agent is reduced from 10 mmol per gram of sorbent 5 to 1-3 mmol / g. The capacity of the sorbent is not inferior to the sorbent, which is obtained by a known method.

Claims (2)

1. A method for producing a sorbent for extracting metal ions from a solution A ditch comprising treating silica modified with y-aminopropyltriethoxysilane with monohalogenoacetic acid followed by washing the product, characterized in that, in order to reduce the duration of the process, the treatment with monohalogenoacetic acid is carried out in ethanol in the presence of amine. 2. Method POP.1, characterized in that the treatment is carried out at a molar ratio of amine to acid of at least 1.