The method of obtaining selective sorbent copper

 

(57) Abstract:

Use: receive a selective sorbent copper for separation, purification and recovery of metals from different types of waters. The inventive amination of macroporous klimatisierung copolymer and divinising connection with hexamethylenetetramine in an environment of methanol at 35 to 45C. Subsequent addition of demineralized water and exposure in this environment, the processing in the environment of methanol mineral acid. Karboksimetilirovaniya monochloracetate sodium in an alkaline environment. As divinising connections use divinylbenzene with a ratio of meta - and para - isomers (3 and 2.5) : 1, as the environment at the aminating use a methanolic alkali solution with a concentration of 0.6 - 1%, when carboxymethylamino impose additional salt of copper in the amount of 0.03 to 0.05 wt. transfers to the solution monochloracetate sodium and karboksimetilirovaniya carried out at a pH of 7.2 and 7.5. table 2.

The invention relates to methods for selective sorbent copper, which is used for separation, purification and recovery of metals from solutions in analytical chemistry, hydrometallurgy, and for removing non-ferrous metals ions from wastewater.

Known) in methanol-methylol environment with subsequent spirit-acid treatment in the presence of a catalyst and carboxymethylamino monochloracetate sodium [1]

The main disadvantage of this method is the impossibility of achieving the comprehensive degree of conversion at the stage of aminirovaniya. Solubility it has been in a mixture of methanol and matilla is only 6.5% which also affects the degree of conversion and reaction rate. Low degree of transformation requires diaminononane, which increases waste and rinse water. The use of hydrochloric acid increases the amount of liquid phase due to the introduction of water and reduce the amount of finished product per unit volume of equipment. The presence of water makes inefficient and uneconomical use of the catalyst at this stage.

The closest in technical essence and the achieved result to the claimed invention is a method for selective sorbent copper aminating macroporous klimatisierung copolymer of styrene and divinylbenzene connection with hexamethylenetetramine in an environment of methanol at 35-45aboutC, followed by addition of demineralized water in this environment, the processing of the mineral acid in the environment of methanol and carboxyethylgermanium monochloracetate sodium in an alkaline environment [2]

The disadvantages of this method is negotiationarticle low separation factor, not a high degree of desorption of the metal (copper) is equivalent to the amount of eluent.

The aim of the invention is the improvement of operational properties and increase selectivity (selectivity) of the sorbent copper from solutions of complex salt composition, containing, along with copper ions other three - and divalent metals.

The problem is solved in that in the method of obtaining selective sorbent copper aminating macroporous klimatisierung copolymer of styrene and divinising connection with hexamethylenetetramine in an environment of methanol at 35-45aboutC, followed by addition of demineralized water and exposure in this environment, the processing of the mineral acid in the environment of methanol and carboxyethylgermanium monochloracetate sodium in an alkaline environment, as divinising connections use divinylbenzene at a ratio of meta - and para - isomers (3-2,5):1, as the environment at the aminating use a methanolic alkali solution with a concentration of 0.6-1% when carboxymethylamino impose additional salt of copper in the amount of 0.05-0.03 wt.h. and the solution monochloracetate sodium and karboksimetilirovaniya lead at pH 7,2-7,5.

In table.1 presents the parameters of the existence of the tx2">

P R I m e R 1. In a glass three-neck round bottom flask with reflux condenser, provided with a device for mixing, measuring temperature, heating and cooling load 1 wt.h. klimatisierung copolymer (HMS) of styrene (St) and divinylbenzene (DVB) (M-DVB: p-DVB 3:1) modification 8/100 (8% DVB, 100% solvent). To CMS add to 1.67 wt.h. methanol, 1 wt. hours of hexamethylenetetramine (it has been) and 0,030 wt.h. caustic soda, which is 0.8% of the Mixture incubated for 1-2 hours, raise the temperature to 40aboutC. After holding at this temperature for a period of 7.5-8 h into the reactor type of 0.65 wt. including demineralized water and continue holding at that temperature for 5.5-6 hours Then separated from the mother liquor, download 5 Mac.h. methanol and dispense 1.8 wt.h. sulfuric acid (95% concentration). The mass was incubated for 2 h without heating, then connect direct to the fridge and carry out heating of the mass to 63-68aboutWith simultaneous distillation of the resulting metella. The reaction is 13-414 hours Then the mass is cooled, squeeze the liquor, wash the resin twice fivefold excess of demineralized water. Then add 7 wt. including solution monochloracetate sodium (30%) and 0.04 wt.h. CuSO4produce heating of the mass to 80aboutWith constant re is washed five times excess of demineralized water. The sorbent yield of 1.2 wt.h. (based on the absolutely dry mass).

Properties of the obtained sorbent are shown in table.2.

P R I m e R s 2-4. Production technology is similar to that described in example 1, when the process parameters and the ratio of the components listed in table.1. Properties of the sorbent are shown in table.2.

The tests were carried out according to the following methods.

Determination of sorption capacity was performed from the standard solution under static conditions when the ratio of phases T:W 1:100 (1 g of the resin in 100 ml of solution). The time of contact until equilibrium is 2-3 days. According to the analytical determination of the content of sorbed material in the initial and equilibrium solutions calculated sorption capacity

CEMWITH1and C2the concentration of metal ions in the initial and equilibrium solution, respectively, mg-EQ/g;

V is the volume of the liquid phase, ml;

g sample of the resin in terms of the original substance,

When sorption of the target (M1component of the technological solution the efficiency of the process is characterized by the partition coefficient CuMM1in relation to the associated components (Mi), which is calculated ilavamo component (Cu2+) and trace metal (e.g. Fe3+, Zn2+Ca2+respectively, mg-EQ/g);

WITHM1and CMthe equilibrium concentration of M1and Miaccordingly, mEq/ml.

Desorption of absorbed metals implemented a 20% solution of sulfuric acid in static and in dynamic conditions at a constant unit load eluent (volumes of eluent through the volume of resin per hour, V/Vwithh).

The less specific consumption of eluent ceteris paribus, the more effective the desorption process and, therefore, so it is easier to produce.

As follows from the table.2, the task accomplished:

the obtained sorbents provide maximum completeness desorption of copper equivalent amount of acid in static conditions (from 86 to 90% compared to 70% on prototype)

specific consumption of eluent is reduced from 10 to 60% in comparison with the prototype, which provides a more concentrated eluent, suitable for further processing with the aim of identifying saleable copper.

The obtained samples have a high selectivity to copper in the presence of other components of the solution.

The separation factor with respect to Zn2+26-32 in transient separation in relation to the CA2+139-151 in comparison with 131 of the prototype.

The METHOD of OBTAINING SELECTIVE SORBENT COPPER aminating macroporous klimatisierung copolymer of styrene and divinising connection with hexamethylenetetramine in an environment of maranola 35 45oWith the subsequent addition demineralizing water and exposure in this environment, the processing of the mineral acid in the environment of methanol and carboxyethylgermanium monochloracetate sodium in an alkaline medium, characterized in that as the source of the copolymer used macroporous klimatisierung copolymer of styrene with divinylbenzene at a ratio of meta to para-isomers 3 2,5 1, as the environment at the aminating use a methanolic alkali solution with a concentration of 0.6 to 1% when carboxymethylamino impose additional salt of copper in quantities of 0.05 to 0.03 wt. including 1 wt.h. solution monochloracetate sodium and karboksimetilirovaniya carried out at a pH of 7.2 to 7.5.

 

Same patents:

The invention relates to high-molecular cross-link copolymers and is a copolymer of diaminodiphenylamine/ polyacrylic acid/ divinylbenzene and ethylstyrene the following formula:

-CH-CH2--CHwhere K = 34,1 to 58.6, L = 30,7 - 45,5, m = 2,1 - 5,1, n = 1,9 - 4,6 mol

The invention relates to a method for producing polymeric sorbents for molecular chromatography containing the nitro group, and can be used for the separation of mixtures of organic compounds or the concentration of trace contaminants from gas and liquid media

The invention relates to the field of synthesis of ion-exchange materials used for wastewater treatment and in particular to the extraction of chromium (VI) from solutions

The invention relates to a method for complexing resins and can be used in hydrometallurgy of non-ferrous and rare metals

The invention relates to high-molecular cross-link copolymers and is a copolymer of diaminodiphenylamine/ polyacrylic acid/ divinylbenzene and ethylstyrene the following formula:

-CH-CH2--CHwhere K = 34,1 to 58.6, L = 30,7 - 45,5, m = 2,1 - 5,1, n = 1,9 - 4,6 mol

The invention relates to a method for producing polymeric sorbents for molecular chromatography containing the nitro group, and can be used for the separation of mixtures of organic compounds or the concentration of trace contaminants from gas and liquid media

The invention relates to the field of synthesis of ion-exchange materials used for wastewater treatment and in particular to the extraction of chromium (VI) from solutions

The invention relates to a method for complexing resins and can be used in hydrometallurgy of non-ferrous and rare metals

The invention relates to high-molecular cross-link copolymers and is a copolymer of diaminodiphenylamine/ polyacrylic acid/ divinylbenzene and ethylstyrene the following formula:

-CH-CH2--CHwhere K = 34,1 to 58.6, L = 30,7 - 45,5, m = 2,1 - 5,1, n = 1,9 - 4,6 mol

The invention relates to methods of producing sorbents for water purification from radionuclides, pesticides and other common anthropogenic pollutants

The invention relates to a process for the production of sorbents based on porous materials (silica clay, diatomaceous earth, diatomite, and other) and can be used for treatment of industrial and domestic wastewater from ions of heavy metals, phenols, chloramine B, surfactants, etc

The invention relates to methods of producing composite sorbents based hexacyanoferrate transit metals and organic media, as well as to the composite sorbents obtained by this method has a high degree of extraction of caesium radionuclides (up to 98.9 per cent), strontium (up to 85.5%), thallium (to 96.7%), and a low degree of solubility in water, which constitutes less than 0.01%

FIELD: sorption technique for purification of industrial emissions and individual pipe security facilities.

SUBSTANCE: method for production of sorbent catalyst includes preparation of impregnating solution by introducing ammonium carbonate and copper and chromium compounds into ammonia water in ratio ammonia water/ammonium carbonate/copper basic carbonate/chrome anhydride of 1:(0.07-0.15):(0.03-0.06):(0.02-0.04); impregnation with metal-containing carbon solution; aging; and granule thermal treatment.

EFFECT: sorbent catalyst with prolonged protective action in relation to chlorocyanide and decreased cost.

4 cl, 3 ex

Up!