A method of producing high purity sulfonic cation exchanger

 

(57) Abstract:

Usage: in the electronics industry, final filters in deep water desalination. Essence: conduct sequential processing swollen technical sulfonic cation exchanger in a dynamic environment, the first 8 - 10% water solution of alkali to obtain the oxidation of the alkali solution in equilibrium conditions is not more than 0.4 - 0.8 MgO2/ DM3higher initial solution, then washing demineralized water, and then treated with 10 - 13% solution of mineral acid prior to the termination of leaching in the filtrate iron ions and finish the laundering of demineralized water. At the same time as mineral acids, nitric, or sulfuric, or hydrochloric acid, and treatment with an aqueous solution of alkali is carried out at 18 - 80oC. for 2 h. p. F.-ly, 2 tab.

The invention relates to the production of a strongly acidic cation exchange resin of high purity (nuclear grade, electronic grade), which are used in the final filters in deep water desalination, in particular in the electronics industry.

The resins of these classes are increased requirements on the residual content of impurities. is whether the cation is significant residual content of cations of iron and alkali metals, and soluble organic substances.

Known methods for producing highly pure cation chemical and (or) electrochemical conditioning. The most complete removal of the cation metal ions and washed organic impurities occurs when sequential processing is 3-5 M acid solution and an electric current at the rate of 30 A-h in 1 l of cation exchanger. However, these methods have only preparative application and cannot be made as large-scale production due to low productivity, high cost of electricity, the need to use expensive electrodes and ion-exchange membranes.

Analysis of the current level of technology shows that closest to the proposed to the technical essence is a method of producing high purity sulfonic cation exchanger marks KU-2-8. Serial processing in dynamic conditions at room temperature 1.5 M solution of hydrochloric acid, distilled water, 0.5 M sodium hydroxide solution and again with distilled water. The disadvantage of this method is the lack of quality sulfonic cation exchanger due to the presence of metal cations and organic contaminants, as evidenced by the industry for use in circuits receiving globalisasyon water, does not contain organic impurities.

The objective of the invention is to reduce the content of impurities in the sulfonic cation exchanger, particularly related to net ion nuclear class.

The task is solved in that for obtaining high purity sulfonic cation exchanger spend sequential processing swollen technical sulfonic cation exchanger in a dynamic environment, the first 8-10% aqueous alkali solution to obtain the oxidation of the alkali solution in equilibrium conditions is not more than 0.4 to 0.8 MgO2/DM3higher oxidation source solution, then washing demineralized water, then 10-13% solution of mineral acid prior to the termination of leaching in the filtrate iron ions and finish washing globalisasyon water. At the same time as mineral acids, nitric or sulfuric, or hydrochloric acid, and treatment with an aqueous solution of alkali is carried out at a temperature of 18-80aboutC.

This allows to reduce the content of organic cation impurities to 0-0,25 and the cations of iron, not more than 0,006%

In addition, the operation of the cation exchanger obtained by the proposed method improves the kinetics of removal of ions from dilute solutions, allowing you took

New salient features of the invention are:

the increase in the concentration of the processing solutions of acids and alkalies;

the processing sequence in the beginning with alkali, then acid;

control at the stages of processing content in the filtrate is washed out of the organic impurities is not more than 0.4-0.8 and to the lack of iron cations;

treatment with alkali solution when 18-80aboutC;

use for cleaning desalted and globalisasyon water.

It is known that increasing the concentration of the alkaline solution leads to an increase in the extraction of organic substances. However, for a cation of three-dimensional polymeric structure decreases the swelling properties, which affects the removal of organic impurities. The use of solutions of alkali with a concentration of more than 10% acid by more than 13% and temperature of the alkaline solution, more than 80aboutWith no leads to improved quality of the final product, but increases the cost of the process and the impurities in the wastewater.

The use of acid solutions with concentrations of less than 10% and alkali less than 8% reduces the efficiency of processing.

Of significant importance is the fact that the end of the treatment process is ESA and alkali after as permanganate oxidation at the insistence by no more than 0.4 to 0.8 .

As the source sulfonic cation exchanger domestic use technical cation exchange resin KU-2-8 on the basis of a copolymer of styrene with divinylbenzene according to GOST 20298-74 you can also use industrial cation exchange resin KU-2-CC and KU-23, 15/100, manufactured according to the same standard.

As aqueous solutions of alkali hydroxide use of sodium, potassium, ammonium.

As the aqueous acid solutions using solutions of sulphuric, nitric and hydrochloric acids.

As demineralized water use water after 1-2 degrees of demineralization without filter mixed (OST 11.029.003-88). Globalisasyon water get clean demineralized water to the filtrate mixed )OST 11.029.003-88).

Since the cation exchange resin obtained by the proposed method contains almost no organic impurities, for their quantitative evaluation was the method of extraction of contaminants from the cation exchange resin with a solution of sulfuric acid. For determination of traces of iron used known methods. The method is illustrated by the following examples.

P R I m e R 1. 100 cm3technical sulfonic cation exchanger helebore sodium chloride for 2 h for swelling. Then the contents of the glass is transferred into a glass column with a diameter of 322 mm, soldered glass filter and a heating jacket. The shirt is served from thermostat water with a temperature of 202aboutWith over 2 hours a Solution of sodium chloride descend to the level of the cation exchange resin, the column is connected to a pressurized bottle with a tube, from which through the cation exchanger from top to bottom with a flow rate of 200 cm3/h serves a 9% solution of caustic soda. In the heating jacket at the same time continue to apply water with a temperature of 202aboutC. Filing of the alkali solution can periodically stop for 2 h, then resume.

The alkaline solution is passed up until his permanganate oxidation after cessation of filtration and infusion over 1-2 h does not exceed the oxidation of the original alkali solution more than 0.8 MgO2/DM3.

The alkaline solution extracted from a column, bottom fill demineralized water and washed down 500 cm3water with a flow rate of 400 cm3/H. Then in the same direction through sulfonation miss 11% solution of nitric acid with a flow rate of 200 cm3/h before the termination of the leaching in the filtrate of iron cations. Acid extracted from a column, fill globalisasyon vlance under a layer of water. Characteristics of the obtained high purity sulfonic cation exchanger are presented in table. 1.

P R I m e R s 2-7. Experimental treatment of the cation is performed with the setup described in example 1 with the same sequence of stages. Processing modes and the results are shown in table. 1.

P R I m e R 9. Processing of the cation exchange resin is carried out as in example 1, but instead of the sodium hydroxide solution is sodium hydroxide solution. The results in table. 1.

P R I m e R 10. Modes and solutions as in example 1, but is a macroporous cation exchange resin patterns KU-23 modification 15/100. The results in table. 1.

P R I m e R s 11, 12 (comparative). Carried out analogously to example 1, the machining conditions and the results are presented in table. 1.

P R I m e p 13 (the prototype). Processing of the cation exchange resin KU-2-8 was performed on the same setup. Swollen in water, the cation exchanger 100 cm3was loaded into the column and with the same costs down consistently missed a 5.5% solution of hydrochloric acid, distilled water, 2% sodium hydroxide solution and again with distilled water. The processing stages adopted as in example 1. The results in table. 1.

In table. 2 shows comparative ocenkam.

As can be seen from the table. 1 and 2, the proposed method allows to obtain the cation exchange resin with a low content of impurities of iron (metal cations) 0,003-0,006% and organic matter content not greater than 0.25 .

In the method prototype received the cation exchange resin contains substantially more cations of iron and 2.5 times more washed out of organic substances.

The effect of the application of the proposed sulfonic cation exchanger is primarily manifested on the quality globalisasyon water when using it in the filter mixed with the anion exchange resin of high purity. It is known that the use for the same purpose industrial exchange resin KU-2-cs and AV-17-cs accompanied by the release of these metal ions and organic impurities in globalisasyon water.

In addition, the cation exchange resin obtained by the proposed method has a better kinetic properties and is available in a working hydrogen form. This allows you to increase the performance of facilities using the proposed sulfonation, as the consumer is an extra effect: the absence of a phase transfer sulfonic cation exchanger in the working form and the possibility of increasing the speed of filtration of the purified solutions.

1. METHOD of OBTAINING is that in dynamic conditions with aqueous solutions of mineral acids and alkalis interim and final washing with water, characterized in that the processing start 8 10% aqueous solution of alkali, and guide you to obtain the oxidation of the alkali solution in equilibrium conditions is not more than 0.4 to 0.8 mg O2/DM3higher initial solution, the intermediate washing spend demineralized water, then treated with 10 13% solution of mineral acid prior to the termination of leaching in the filtrate iron ions and finish washing globalisasyon water.

2. The method according to p. 1, characterized in that as the mineral acids, nitric, or sulfuric or hydrochloric acids.

3. The method according to p. 1, characterized in that the treatment with an aqueous solution of alkali is carried out at 18 90oC.

 

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