Abstract

FIELD: ION-EXCHANGE MATERIALS.

SUBSTANCE: invention relates to a process of preparing gel-like cationites for use in treatment and purification processes. Gel-like cationites are prepared by inoculating-incoming process wherein (a) aqueous suspension of microcapsulated cross-linked styrene polymer in the form of granules and containing cross-linking agent is provided as inoculating polymer; (b) inoculating polymer is left to swell in monomer mixture composed of vinyl monomer, cross-linking agent, and radical initiator, namely peracid aliphatic ester; (c) monomer mixture is polymerized in inoculating polymer; and (d)resulting copolymer is functionalized via sulfatization. Process is characterized by that, in step (a), content of cross-linking agent in cross-linked styrene copolymer amounts to 3.5-7 wt % and inoculum-to-income ratio in step (b) amounts to 1:(0.25-1.5).

EFFECT: enabled preparation of gel-like cationites having high osmotic and mechanic stabilities as well as improved oxidation resistance.

7 cl, 9 tbl, 9 ex

 

The present invention relates to a method for producing a gel-like ion exchangers and their application in the treatment and cleanup.

Gel-type cation exchangers can be obtained by sulfonation of crosslinked polystyrene. Up to the present time in a large number of used cross-linked polystyrenes obtained seed/input method.

Thus, in European patent application EP-0098130 B1 describes the obtaining of gel polystyrene seed/supply method, in which the inflow conditions of polymerization are added to the seed, which is pre-sew 0.1 to 3 wt.% divinylbenzene. In European patent application EP-0101943 B1 describes seed/supply method, in which several tributaries with different preparative form under the conditions of polymerization successively added to the seed. In U.S. patent US 5068255 described seed/supply method, in which the first mixture of monomers will polimerizuet to becoming 10-80 wt.% and then mixed with the second mixture of monomers without a radical initiator as inflow in the conditions of polymerization. The disadvantage of these methods according to European patent applications EP-0098130 B1, EP-0101943 B1 and U.S. patent US 5068255 is a complex dosing, at which the rate of flow should be consistent with the kinetics of polymerization.

In European patent application EP-A 0826704 and application p is the awning Germany DE-A 19852667 described seed/fresh ways of using microencapsulated polymer particles as a seed. Compared to commercially available, directly synthesized by suspension polymerization of polymers polymers obtained suspension polymerization in accordance with the specified methods, have high content of unstitched soluble polymers. This unstitched soluble polymers is undesirable when translating ion exchangers, as highlighted by dissolving part of the polymer concentrate in the reaction solutions used for functionalization. In addition, an increased amount of soluble polymers can lead to undesirable wypadaniu (washout) of the ion.

Leaching can also occur due to insufficient stability of the cation oxidation. Under the proposed invention, the oxidation resistance means that the cation in the oxidation, such as typically occurs during operation of the ion-exchange resins, in combination with anion exchange resin does not emit any components in the cleaning medium, preferably water. Otherwise, the allocation of oxidation products, as a rule, polystyrenesulfonate acids, increases the conductivity of the eluate. If the selected polystyrenesulfonate acid demonstrate a high molecular weight in the range from about 10,000 to 100,000 g/mol, the leaching of cations is especially a big problem.

The present invention is the preparation of gel-type cation exchange resin with high mechanical and osmotic stability and simultaneously improved resistance to oxidation.

Therefore, an object of the present invention is a method of obtaining a gel-type cation exchangers according to the seed-supply method (ZAT is avoce/supply method), characterized in that

a) in aqueous suspension get cross-linked polystyrene in the form of pellets containing 3.5 to 7 wt.% cross-linking agent, as the seed polymer

b) leave to swell the seed polymer in the mixture of monomers of the vinyl monomer, a crosslinking agent and a radical initiator,

c) polimerizuet mixture of monomers in the seed polymer, and

d) functionalitywith obtained copolymer sulphurization.

The seed polymer from stage (a) contains 3.5 to 7 wt.%, preferably 4.5-6 wt.% cross-linking agent. As a cross-linking agent suitable are compounds that contain two or more, preferably from two to four double compounds capable of radical polymerization in the molecule. Examples of such compounds are divinylbenzene, dividercolor, trivinylbenzene, Divinington, trigeneration, simple diethylethylenediamine ether, octadiene-1,7, hexadiene-1,5, etilenglikolevykh, triethyleneglycoldinitrate, trimethylolpropane, alismataceae or methylene-N,N'-bisacrylamide. As a preferred cross-linking agent is divinylbenzene. Basically enough to use commercially available types of divinylbenzene, which along with the isomers of divinylbenzene also contain ethylvinylbenzene. The main components of the seed which is styrene. In addition to styrene and a cross-linking agent in the seed could be other monomers, e.g., in the amount of 1-15 wt.% Examples are: Acrylonitrile, vinylpyridine, methyl acrylate, acrylate, hydroxyethylmethacrylate or acrylic acid.

The particle size of the seed polymer is 5-750 μm, preferably between 20 and 500 μm, most preferably 100-400 μm. View of the distribution curve of the particle size must match the preferred cation exchangers. Therefore, in the framework of the present invention to obtain a finely distributed or monodisperse ion exchanger used finely distributed or monodisperse seed polymer. In accordance with a preferred embodiment of the present invention using monodisperse seed polymer. In this regard, the term "monodisperse" means that the ratio of the values of 90% (⊘ (90)) and values of 10% (⊘ (10)) the distribution function of the volume size of the particles is less than 2, preferably less than 1.5, most preferably less than 1.25. A value of 90% (⊘ (90)) specifies the diameter of which exceeds 90% of the particles. Accordingly, 10% of the particles exceed the diameter values of 10% (⊘ (10)). The determination of the average particle size and size distribution of particles of any suitable methods, such as sieve analysis, or electron-lucev the th analysis.

In accordance with another preferred embodiment of the present invention the seed polymer is microencapsulated. Suitable as a seed, microencapsulated polymers can be obtained according to European patent application EP-0046535 B1, the contents of which are incorporated into the present application for the invention relative to microencapsulation.

For microencapsulation of possible use of the materials known for this purpose, especially polyesters, natural and synthetic polyamides, polyurethanes, politician. The most suitable natural polyamide is gelatin. Gelatin is also used as a koatservata and complex koatservata. In the framework of the present invention under the complex koatservatov it containing gelatin, first of all, realize the combination of gelatin and synthetic polyelectrolytes. Suitable synthetic polyelectrolytes are copolymers with embedded elements, for example, maleic acid, acrylic acid, methacrylic acid, acrylamide or methacrylamide. Capsules containing gelatin, can be cured in the usual hardeners, such as formaldehyde or glutaric dialdehyde. The encapsulation of monomer droplets, for example, gelatin, koatservatov it containing gelatin or complex is acervate, contains gelatin, described in detail in European patent application EP-0046535 B1. Methods of encapsulation of synthetic polymers known. The most suitable is, for example, interfacial condensation, in which one of the reactive components dissolved in the monomer droplets (for example, isocyanate or acid chloride), interacts with the second reactive component dissolved in the aqueous phase (e.g., an amine). In accordance with the present invention, it is preferable microencapsulation with complex koatservata containing gelatin.

The seed polymer is preferably suspended in the aqueous phase, and the ratio of polymer and water can be between 2:1 and 1:20. The preferred ratio of polymer and water is from 1:1.5 to 1:5. The use of an auxiliary component, such as a surfactant or a protective colloid, is not necessary. Holding the suspension may, for example, conventional mixing, preferably use the power of moving from low to medium.

At the stage b) to the suspended seed polymer add the mixture ("flow") of the vinyl monomer, a crosslinking agent and a radical initiator.

As the vinyl monomers used monomers: styrene, vinyltoluene, atillery, alpha methylsterol, hors iron, acrylic acid, methacrylic acid, ester of acrylic acid, esters of methacrylic acid, Acrylonitrile, Methacrylonitrile, acrylamide, methacrylamide, as well as mixtures of these monomers. Preferred are mixtures of styrene and Acrylonitrile. Most preferred is a mixture of 86-98% by weight styrene and 2-14 wt.% Acrylonitrile. Absolutely preferred is a mixture of 88 to 95 wt.% styrene and 5-12 wt.% Acrylonitrile.

Cross-linking agent is divinylbenzene, dividercolor, trivinylbenzene, Divinington, trigeneration, simple diethylethylenediamine ether, octadiene-1,7, hexadiene-1,5, etilenglikolevykh, triethyleneglycoldinitrate, trimethylolpropane, alismataceae or methylene-N,N'-bisacrylamide. Preferred is polystyrene. Basically enough to use commercially available types of divinylbenzene, which along with the isomers of divinylbenzene also contain ethylvinylbenzene. The content of the crosslinking agent in the monomer mixture is 5-20 wt.%, preferably 7-15 wt.%

For the proposed in accordance with the present invention a method suitable radical initiators in the "flow" are, for example, peroxidase, such as Dibenzoyl peroxide, delauriers, bis(p-chlorobenzoyloxy), dicyclohexylurea dicarbonate, tert-butyl-2-ethyl-peroxyoctanoic 2,5-bis(2-ethylhexanoylperoxy)-2,5-dimethylhexane or tert-amyl-peroxy-2-ethylhexan, tert-butyl-peroxybenzoate, the following azo compounds such as 2,2'-azobis(isobutyronitrile) and 2,2'-azobis(2-methylisoborneol). Preferably use a mixture of radical-initiators with different kinetics of decay, for example a mixture of tert-butyl-2-ethyl-peroxyacetate and tert-butyl-peroxybenzoate. The amount of the radical initiator is usually from 0.05 to 2.5 wt.%, preferably from 0.2 to 1.5 wt.%, relative to the mixture of monomer and crosslinking agent.

The ratio of the seed polymer to which are added a mixture (ratio of seed/inflow) is usually 1:0.25 to 1:5, preferably 1:0.5 to 1:2.5 and most preferably 1:0.6 to 1:1,6. Due to the high content of crosslinking agent in the seed was unexpectedly found that adding a mixture of monomers fully swells in the seed polymer under the conditions proposed in accordance with the present invention. For a given particle size of the seed polymer ratio of seed/inflow is possible to adjust the particle size of the obtained copolymer or the resin.

The swelling monomer mixture in the seed polymer is carried out at a temperature at which it is not active, none of the added radical initiators.

Swelling usually occurs when the temperature 0-60° With and lasts for about 0.5-5 hours.

The polymerization of the swollen seed polymer to obtain a copolymer in accordance with stage C) is carried out in the presence of one or more protective colloids and, if necessary, a buffer system. In the framework of the present invention as a suitable protective colloids are natural and synthetic water-soluble polymers such as gelatin, starch, polyvinyl alcohol, polyvinylpyrrolidone, polyacrylic acid, polymethacrylic acid or copolymers of (meth)acrylic acid and esters of (meth)acrylic acid. Very well suitable are derivatives of cellulose, particularly complex or ethers of cellulose, such as carboxymethylcellulose or hydroxyethylcellulose. In the framework of the present invention, the preferred protective colloids are cellulose derivatives. The used amount of the protective colloids is usually 0.05 to 1 wt.% relative to the aqueous phase, preferably 0.1 to 0.5 wt.% The addition of the protective colloid may occur in aqueous solution and, as a rule, immediately after swelling monomer mixture in the seed.

The polymerization in accordance with stage C) can be carried out in the presence of buffer systems. Preferred is a buffer system, which regulates the level of the N aqueous phase at the beginning of polymerization between 14 and 6, preferably between 13 and 9. Under these conditions, protective colloids with groups of carboxylic acids are fully or partially salts. Thus, the action of the protective colloids is favorable. In the framework of the present invention is particularly well suitable buffer systems contain salts of phosphates or borates.

In accordance with the preferred embodiment of the present invention the aqueous phase contains dissolved inhibitor. As inhibitors used as inorganic and organic substances. Inorganic inhibitors are, for example, nitrogen compounds such as hydroxylamine, hydrazine, sodium nitrite and potassium nitrite. Organic inhibitors are, for example, phenolic compounds such as hydroquinone, simple gidrokolonoteraphy ether, resorcinol, pyrocatechol, tert-butylpyrocatechol or condensation products of phenols with aldehydes. Other organic inhibitors are compounds containing nitrogen, such as diethylhydroxylamine and isopropylacrylamide. In the framework of the present invention, the preferred inhibitor is resorcinol. The concentration of the inhibitor is 5-1000 ppm, preferably 10-500 ppm, most preferably from 20 to 250 ppm relative to the aqueous phase.

P and polymerization of the swollen seed ratio of organic phase to aqueous phase is 1:0.8 to 1:10, preferably 1:1-1:5.

When polymerization of the swollen seed polymer temperature to regulate the temperature of the collapse of the initiator used/used initiators. This temperature is usually between 50 and 150°C, preferably between 55 and 140°C. the Polymerization lasts for 2 to 20 hours. Preferably use a temperature program in which the polymerization starts at a low temperature, for example 60°and as progressive polymerization conversion of the reaction the temperature rises, for example, to 130°C. it is Found that the polymerization in a wide temperature range, especially when using at least two radical-initiators with different kinetics of decay is with great mechanical and osmotic stability.

After polymerization, the copolymer can be isolated in the usual way, for example by filtration and decantation, and, if necessary, after one or more washings dried and, if necessary, sifted.

The transformation of the copolymers in the cation exchangers in accordance with stage d) is carried out by means of sulfonation. In cancers of the present invention suitable sulfonation agents are sulfuric acid, sulfur trioxide and chlorosulfonic acid. Preferred is sulfuric acid with a concentration of 0-100 wt.%, most preferably 96-99 wt.% When the sulfonation temperature is usually 60-180°C, preferably 90-130°S, most preferably 95-110°C. it is Found that proposed in accordance with the present invention, the copolymers can be sulfonated without the addition of swelling agents (such as chlorobenzene or dichloromethane) and thus obtain homogeneous products of sulfonation.

When the sulfonation reaction mixture is stirred. And you can use different types of mixers, such as bladed agitator, anchor agitator, anchor agitator or turbine mixer. It turns out that the most appropriate is the radial mixing double turbine agitator.

In accordance with the preferred embodiment of the present invention, the sulfonation is conducted so-called "properities way." In this way the copolymer added to sulfuric acid, the temperature is evenly supported. Most preferably the dosage conducting portions.

After sulfonation, the reaction mixture of the product of sulfonation and the residual acid is cooled to room temperature and initially dilute sulfuric acid with a lower concentration and then with water.

The entire method may be continuous, periodic or preperiodic the sky. The most preferred method is carried out in technologically regulated device.

In addition, an object of the present invention are gel-type cation exchangers with improved resistance to oxidation, which receive the seed-supply method by

a) obtaining aqueous suspension of cross-linked polystyrene in the form of pellets containing 3.5 to 7 wt.% cross-linking agent, as the seed polymer

b) swelling of the seed polymer in the mixture of monomers of the vinyl monomer, a crosslinking agent and a radical initiator,

c) polymerization of the mixture of monomers in the seed polymer and

d) functionalization copolymer formed by sulfonation.

In most cases, preferably the transformation of cation exchangers obtained in accordance with the present invention, the acid in the form of sodium. This conversion is carried out with the use of caustic soda at a concentration of 1-60 wt.%, preferably 3-10 wt.%

The cation exchangers obtained in accordance with the present invention, are characterized by their high stability and purity. Such cation exchangers after prolonged use and repeated recovery shows no defects granules of ion exchangers and no bleed (leaching) of the ion.

It is found that proposed in accordance with the present invention to tianity with low content of divinylbenzene as a crosslinking agent, for example 6.5 to 7.6 wt.% DVB (divinylbenzene) copolymer, also exhibit high total throughput from 2.1 to 2.4 equivalents/L.

The cation exchangers have a large number of different applications. For example, the cation exchangers are used for drinking water treatment, to obtain high purity water (required when receiving chips in the computer industry), for the chromatographic separation of glucose and fructose, and as catalysts for various chemical reactions (for example, upon receipt of bisphenol a from phenol and acetone). For most of these applications it is desirable that the cation functioned without pollution products that may occur upon receipt of the cation or during operation due to the decomposition of the polymers. The presence of contaminants in the water resulting from the cation exchange resin, it is possible to detect due to the increase of conductivity and/or organic carbon (TOC) in the water.

Proposed in accordance with the present invention the cation is also great for full bating water. After prolonged operation of plants for desalination also do not see a high conductivity. Also, if you know not all the details of correlation structures and characteristics proposed in accordance with the crust is ashim the invention of the cation, it is likely, explanation for the favorable characteristics leaching is a special lattice structure.

Therefore, an object of the present invention is the application of the proposed in accordance with the present invention the cation

- removal of cations, dye particles or organic components from aqueous or organic solutions and condensates, such as technological or turbine condensates,

for curing in neutral exchange of aqueous or organic solutions and condensates, such as technological or turbine condensates,

- for cleaning and water treatment chemical industry, electronic industry and power plants,

for full bating aqueous solutions and/or condensates, characterized in that the cation exchange resin used in combination with gel and/or macroporous anion exchange resin

for discoloration and demineralization of whey, liquid broths on gelatin, fruit juices, fruit wines and aqueous solutions of sugar,

- in the form of a fine powder alone or, if necessary, in a mixture with a strong base anion exchange resin for filtering or desalination of water, such as condensate, or in hydrometallurgy.

Therefore, the present invention also applies to

- how full bating water races the thieves and/or condensates, for example, such as technological or turbine condensates, characterized in that the proposed in accordance with the present invention monodisperse cation exchangers are used in combination with heterodispersed or monodisperse, gel-like and/or macroporous anion exchange resin

the combinations obtained in accordance with the present invention monodisperse cation exchangers with heterodispersed or monodisperse, gel-like and/or macroporous anion exchange resin for full bating aqueous solutions and/or condensates, such as technological or turbine condensates,

- methods of cleaning and water treatment chemical industry or power plant, characterized in that the proposed use in accordance with the present invention monodisperse cation exchangers,

- ways to remove cations, dye particles or organic components from aqueous or organic solutions and condensates, such as technological or turbine condensates, characterized in that the proposed use in accordance with the present invention monodisperse cation exchangers,

- ways of curing in neutral exchange of aqueous or organic solutions and condensates, such as technological or turbine condensates, characterized in that use is redlozhenie in accordance with the present invention monodisperse cation exchangers,

- methods of bleaching and demineralization of whey, liquid broths on gelatin, fruit juices, fruit wines and aqueous solutions of sugar in sugar, starch or pharmaceutical industry or dairies, characterized in that the proposed use in accordance with the present invention monodisperse cation exchangers.

Examples

Methods of research:

Determination of electrical conductivity of the eluate of the cation

1 l of Deionized water runs in the first circuit 1 through l of the studied cation exchange resin in H-form, and then 5 ml of the anion type Mono Plus H 500®(Bayer AG, Leverkusen) with the speed of delivery of 7 l/h at a temperature of 25°C. the conductivity of the pumped water is determined after 70 h in MKM/see

Determination of molecular weight of polystyrenesulfonate acid in the eluate of the cation

The molecular weight of polystyrenesulfonate acid in water, which for 70 h circulated through the cation exchange resin and anion exchange resin, determine gel permeation chromatography using polystyrenesulfonate acid with a known molecular weight as standard.

Example 1 (reference example)

a) obtaining a copolymer

The copolymer receive in accordance with example 2A-b) European patent application EP-A 1000659.

b) obtaining cation

In 2-liter flasks is with four necks put 1400 ml 98.4%of sulfuric acid and heated to a temperature of 100° C. After 4 hours in the flask is added with stirring 10 servings, 350 g of dry copolymer of 1A). The mixture is then stirred for 6 hours at a temperature of 120°C. the resulting suspension is cooled and poured into a glass column. Sulfuric acid with a lower concentration ranging from 90 wt.% and ending at the end of clean water, filtered from the top through the column. Get 1630 ml of cation exchanger in the H form.

(C) the transfer of the cation

For translation of the cation exchange resin of H-form to Na-form 1610 ml from sulphonated product from 1b) and 540 ml of deionized water at room temperature is placed in a 6-liter glass reactor. After 120 minutes, the suspension is mixed with 2489 ml of 5%aqueous caustic soda solution. The mixture is then stirred for 15 minutes. Then the obtained product is washed with deionized water. Get 1490 ml of cation exchanger in the Na-form.

The full capacity of the Na-form (mol/l)2,01
The conductivity of the eluate after 70 h (MKM/cm)3,296
Molecular weight polystyrenesulfonate acid in the eluate (g/mol)23000

Example 2 (in accordance with the invention)

a) obtaining a copolymer

In a 4-liter glass reactor placed in an aqueous solution of 3.6 g of boric acid and 1.0 g of sodium hydroxide in 100 g of deionized water. To the resulting mixture add 600,2 g of monodisperse microencapsulated seed polymer containing 95 wt.% styrene and 5.0 wt.% divinylbenzene. The seed polymer is produced in accordance with European patent EP-0046535 B1. The wall of the capsules of the bare polymer consists of a comprehensive koatservata of gelatin and a copolymer of acrylamide/acrylic acid cured formaldehyde. The average particle size of the seed polymer is 365 μm and the value of ⊘(90)/⊘(10) is equal to 1.05. The mixture is stirred with a speed of 220 rpm Then to the resulting mixture for 30 minutes, add a mixture of 476,2 g of styrene, 48,0 g of Acrylonitrile, 76,0 g of divinylbenzene (80,6 wt.%), 2.2 g of tert-BUTYLPEROXY-2-ethylhexanoate and 1.5 g of tert-butyl peroxybenzoate as a tributary. The composition is stirred for 2 hours at a temperature of 50°S, and the gas space is washed with nitrogen. Then to the resulting product, add a solution of 2.4 g of methylhydroxyethylcellulose in 120 g of deionized water and stirred for 1 hour at a temperature of 50°C. the Composition is heated to a temperature of 63°C and maintained for 10 hours at this temperature, then stirred for 3 hours at a temperature of 130°C. the Composition is cooled, washed with deionized water through a 40-micron sieve and dried in an oven for 18 hours pritemperature 80° C. Get 1164 copolymer in the form of granules, the particle size of which is 460 μm and ⊘(90)/⊘(10) is of 1.07.

b) obtaining cation

A 2-liter flask with four necks hurt 1400 ml of 98.2%sulfuric acid and heated to a temperature of 100°C. After 4 hours in the flask is added with stirring 10 servings, 350 g of dry copolymer 2A). The mixture is then stirred for 6 hours at a temperature of 120°C. the resulting suspension is cooled and poured into a glass column. Sulfuric acid with a lower concentration ranging from 90 wt.% and ending at the end of clean water, filtered from the top through the column. Get 1460 ml of cation exchanger in the H form.

c) the transfer of the cation

For translation of the cation exchange resin of H-form to Na-form 1440 ml from sulphonated product of 2b) and 450 ml of deionized water at room temperature is placed in a 6-liter glass reactor. After 120 minutes, the suspension is mixed with 2230 ml of 5%aqueous caustic soda solution. The mixture is then stirred for 15 minutes. Then the obtained product is washed with deionized water. Receive 1340 ml of cation exchanger in the Na-form.

The full capacity of the Na-form (mol/l)2,23
The conductivity of the eluate after 70 h (MKM/cm)0,360
Molecular weight of p is literalcontrol acid in the eluate (g/mol) 1100

Example 3 (in accordance with the invention)

a) obtaining a copolymer

In a 4-liter glass reactor placed in an aqueous solution of 3.6 g of boric acid and 1.0 g of sodium hydroxide in 1100 g of deionized water. To the resulting mixture add 648,9 g of monodisperse microencapsulated seed polymer containing 95 wt.% styrene and 5.0 wt.% divinylbenzene. The seed polymer is produced in accordance with European patent EP-0046535 B1. The wall of the capsules of the bare polymer consists of a comprehensive koatservata of gelatin and a copolymer of acrylamide/acrylic acid cured formaldehyde. The average particle size of the seed polymer is 375 μm and the value of ⊘(90)/⊘(10) is equal to 1,06. The mixture is stirred with a speed of 220 rpm Then to the resulting mixture for 30 minutes, add a mixture of 430,5 g of styrene, 48,0 g of Acrylonitrile, 73,0 g of divinylbenzene (80,6 wt.%), 2.0 g of tert-BUTYLPEROXY-2-ethylhexanoate and 2.0 g of tert-butyl peroxybenzoate as a tributary. The composition is stirred for 2 hours at a temperature of 50°S, and the gas space is washed with nitrogen. Then to the resulting product, add a solution of 2.4 g of methylhydroxyethylcellulose in 120 g of deionized water and stirred for 1 hour at a temperature of 50°C. the Composition is heated to a temperature of 61°and withstand crashes-auto St is t for 10 hours at this temperature, then stirred for 3 hours at a temperature of 130°C. the Composition is cooled, washed with deionized water through a 40-micron sieve and dried in an oven for 18 hours at a temperature of 80°C. Receive 1140 g of the copolymer in the form of granules, the particle size of which is 460 μm and ⊘(90)/⊘(10) is of 1.07.

b) obtaining cation

A 2-liter flask with four necks hurt 1400 ml 98,1%sulfuric acid and heated to a temperature of 100°C. After 4 hours in the flask is added with stirring 10 servings, 350 g of dry copolymer of 3A). The mixture is then stirred for 6 hours at a temperature of 105°C. the resulting suspension is cooled and poured into a glass column. Sulfuric acid with a lower concentration ranging from 90 wt.% and ending at the end of clean water, filtered from the top through the column. Receive 1480 ml of cation exchanger in the H form.

(C) the transfer of the cation

For translation of the cation exchange resin of H-form to Na-form 1460 ml from sulphonated product of 3b) and 450 ml special water at room temperature is placed in a 6-liter glass reactor. After 120 minutes, the suspension is mixed with 2383 ml of 5%aqueous caustic soda solution. The mixture is then stirred for 15 minutes. Then the obtained product is washed with deionized water. Get 1380 ml of cation exchanger in the Na-form.

The full capacity of the Na-form (mol/l)of 2.21
The conductivity of the eluate after 70 h (MKM/cm)0,136
Molecular weight polystyrenesulfonate acid in the eluate (g/mol)<1000

Example 4 (in accordance with the invention)

a) obtaining a copolymer

In a 4-liter glass reactor placed in an aqueous solution of 3.6 g of boric acid and 1.0 g of sodium hydroxide in 1100 g of deionized water. To the resulting mixture add 631,8 g of monodisperse microencapsulated seed polymer containing 95 wt.% styrene and 5.0 wt.% divinylbenzene. The seed polymer is produced in accordance with European patent EP-0046535 B1. The wall of the capsules of the bare polymer consists of a comprehensive koatservata of gelatin and a copolymer of acrylamide/acrylic acid cured formaldehyde. The average particle size of the seed polymer is 365 μm and the value of ⊘(90)/⊘(10) is equal to 1.05. The mixture is stirred with a speed of 220 rpm Then to the resulting mixture for 30 minutes, add a mixture of 463 g of styrene, 48,0 g of Acrylonitrile, and 57.6 g of divinylbenzene (80,6 wt.%), 2.1 g of tert-BUTYLPEROXY-2-ethylhexanoate and 1.4 g of tert-butyl peroxybenzoate as a tributary. The composition is stirred for 2 hours at a temperature of 50°s, and the gas protrans is washed in nitrogen. Then to the resulting product, add a solution of 2.4 g of methylhydroxyethylcellulose in 120 g of deionized water and stirred for 1 hour at a temperature of 50°C. the Composition is heated to a temperature of 61°C and maintained for 10 hours at this temperature, then stirred for 3 hours at a temperature of 130°C. the Composition is cooled, washed with deionized water through a 40-micron sieve and dried in an oven for 18 hours at a temperature of 80°C. Receive 1121 g of the copolymer in the form of granules, the particle size of which is 450 μm and ⊘(90)/⊘(10) is equal to 1.05.

b) obtaining cation

A 2-liter flask with four necks hurt 1400 ml 98.4%of sulfuric acid and heated to a temperature of 100°C. After 4 hours in the flask is added with stirring 10 servings, 350 g of dry copolymer of 4A).

The mixture is then stirred for 6 hours at a temperature of 120°C. the resulting suspension is cooled and poured into a glass column. Sulfuric acid with a lower concentration ranging from 90 wt.% and ending at the end of clean water, filtered from the top through the column. Receive 1480 ml of cation exchanger in the H form.

(C) the transfer of the cation

For translation of the cation exchange resin of H-form to Na-form 1460 ml from sulphonated product of 4b) and 450 ml of deionized water at room temperature is placed in a 6-liter with clanny reactor. After 120 minutes, the suspension is mixed with 2400 ml of 5%aqueous caustic soda solution. The mixture is then stirred for 15 minutes. Then the obtained product is washed with deionized water. Get 1330 ml of cation exchanger in the Na-form.

The full capacity of the Na-form (mol/l)2,18
The conductivity of the eluate after 70 h (MKM/cm)0,540
Molecular weight polystyrenesulfonate acid in the eluate (g/mol)2000

Example 5 (in accordance with the invention)

a) obtaining a copolymer

In a 4-liter glass reactor placed in an aqueous solution of 3.6 g of boric acid and 1.0 g of sodium hydroxide in 1100 g of deionized water. To the resulting mixture add 600,2 g of monodisperse microencapsulated seed polymer containing 95 wt.% styrene and 5.0 wt.% divinylbenzene. The seed polymer is produced in accordance with European patent EP-0046535 B1. The wall of the capsules of the bare polymer consists of a comprehensive koatservata of gelatin and a copolymer of acrylamide/acrylic acid cured formaldehyde. The average particle size of the seed polymer is 365 μm and the value of ⊘(90)/⊘(10) is equal to 1.05. The mixture is stirred with a speed of 220 rpm Then to the resulting mixture for 30 minutes on billaut mixture of 504,6 g of styrene, 36,0 g of Acrylonitrile, to 59.6 g of divinylbenzene (80,6 wt.%), 2.2 g of tert-BUTYLPEROXY-2-ethylhexanoate and 1.5 g of tert-butyl peroxybenzoate as a tributary. The composition is stirred for 2 hours at a temperature of 50°S, and the gas space is washed with nitrogen. Then to the resulting product, add a solution of 2.4 g of methylhydroxyethylcellulose in 120 g of deionized water and stirred for 1 hour at a temperature of 50°C. the Composition is heated to a temperature of 61°C and maintained for 10 hours at this temperature, then stirred for 3 hours at a temperature of 130°C. the Composition is cooled, washed with deionized water through a 40-micron sieve and dried in an oven for 18 hours at a temperature of 80°Receive 1176 g of the copolymer in the form of granules, the amount particles which is 460 μm and ⊘(90)/⊘(10) is equal to 1,06.

b) obtaining cation

A 2-liter flask with four necks hurt 1400 ml of 98.5%sulfuric acid and heated to a temperature of 100°C. After 4 hours in the flask is added with stirring 10 servings, 350 g of dry copolymer of 5A). The mixture is then stirred for 6 hours at a temperature of 105°C. the resulting suspension is cooled and poured into a glass column. Sulfuric acid with a lower concentration ranging from 90 wt.% and ending at the end of clean water, the filter is jut from the top through the column. Get 1500 ml of cation exchanger in the H form.

c) the transfer of the cation

For translation of the cation exchange resin of H-form to Na-form 1480 ml from sulphonated product from 5b) and 450 ml of deionized water at room temperature is placed in a 6-liter glass reactor. After 120 minutes, the suspension is mixed with 2364 ml of 5%aqueous caustic soda solution. The mixture is then stirred for 15 minutes. Then the obtained product is washed with deionized water. Get 1380 ml of cation exchanger in the Na-form.

The full capacity of the Na-form (mol/l)2,19
The conductivity of the eluate after 70 h (MKM/cm)0,301
Molecular weight polystyrenesulfonate acid in the eluate (g/mol)1500

Example 6 (in accordance with the invention)

a) obtaining a copolymer

In a 4-liter glass reactor placed in an aqueous solution of 3.6 g of boric acid and 1.0 g of sodium hydroxide in 1100 g of deionized water. To the resulting mixture add 600,2 g of monodisperse microencapsulated seed polymer containing 95 wt.% styrene and 5.0 wt.% divinylbenzene. The seed polymer is produced in accordance with European patent EP-0046535 B1. The wall of the capsules of the bare polymer consists of a comprehensive koatservata of gelatin and a copolymer Smoot the amide/acrylic acid, the cured formaldehyde. The average particle size of the seed polymer is 365 μm and the value of ⊘(90)/⊘(10) is equal to 1.05. The mixture is stirred with a speed of 220 rpm Then to the resulting mixture for 30 minutes, add a mixture of 476,2 g of styrene, 48,0 g of Acrylonitrile, 76,0 g of divinylbenzene (80,6 wt.%), 2.2 g of tert-BUTYLPEROXY-2-ethylhexanoate and 1.5 g of tert-butyl peroxybenzoate as a tributary. The composition is stirred for 3 hours at a temperature of 30°S, and the gas space is washed with nitrogen. Then to the resulting product, add a solution of 2.4 g of methylhydroxyethylcellulose in 120 g of deionized water and stirred for 1 hour at a temperature of 30°C. the Composition is heated to a temperature of 61°and incubated for 8 hours at this temperature, then stirred for 3 hours at a temperature of 130°C. the Composition is cooled, washed with deionized water through a 40-micron sieve and dried in an oven for 18 hours at a temperature of 80°C. Receive 1133 g of the copolymer in the form of granules, the particle size of which is 460 μm and ⊘(90)/⊘(10) is of 1.07.

b) obtaining cation

A 2-liter flask with four necks hurt 1400 ml of 98.2%sulfuric acid and heated to a temperature of 100°C. After 4 hours in the flask is added with stirring 10 servings, 350 g, dry copoly the EPA from 6A). The mixture is then stirred for 6 hours at a temperature of 105°C. the resulting suspension is cooled and poured into a glass column. Sulfuric acid with a lower concentration ranging from 90 wt.% and ending at the end of clean water, filtered from the top through the column. Get 1440 ml of cation exchanger in the H form.

(C) the transfer of the cation

For translation of the cation exchange resin of H-form to Na-form 1420 ml from sulphonated product of 6b) and 450 ml of deionized water at room temperature is placed in a 6-liter glass reactor. After 120 minutes, the suspension is mixed with 2337 ml of 5%aqueous caustic soda solution. The mixture is then stirred for 15 minutes. Then the obtained product is washed with deionized water. Receive 1340 ml of cation exchanger in the Na-form.

The full capacity of the Na-form (mol/l)2,24
The conductivity of the eluate after 70 h (MKM/cm)of 0.333
Molecular weight polystyrenesulfonate acid in the eluate (g/mol)1000

Example 7 (in accordance with the invention)

a) obtaining a copolymer

In a 4-liter glass reactor placed in an aqueous solution of 3.6 g of boric acid and 1.0 g of sodium hydroxide in 1100 g of deionized water. To the resulting mixture add 600,2 g of monodisperse microcapsules the aqueous seed polymer, containing 95 wt.% styrene and 5.0 wt.% divinylbenzene. The seed polymer is produced in accordance with European patent application EP-0046535 B1. The wall of the capsules of the bare polymer consists of a comprehensive koatservata of gelatin and a copolymer of acrylamide/acrylic acid cured formaldehyde. The average particle size of the seed polymer is 365 μm and the value of ⊘(90)/⊘(10) is equal to 1.05. The mixture is stirred with a speed of 220 rpm Then to the resulting mixture for 30 minutes, add a mixture of 485,2 g of styrene, 48,0 g of Acrylonitrile, 67,0 g of divinylbenzene (80,6 wt.%), 2.2 g of tert-BUTYLPEROXY-2-ethylhexanoate and 1.5 g of tert-butyl peroxybenzoate as a tributary. The composition is stirred for 2 hours at a temperature of 50°S, and the gas space is washed with nitrogen. Then to the resulting product, add a solution of 2.4 g of methylhydroxyethylcellulose in 120 g of deionized water and stirred for 1 hour at a temperature of 50°C. the Composition is heated to a temperature of 63°C and maintained for 10 hours at this temperature, then stirred for 3 hours at a temperature of 130°C. the Composition is cooled, washed with deionized water through a 40-micron sieve and dried in an oven for 18 hours at a temperature of 80°C. Receive 1169 g of the copolymer in the form of granules, the particle size of which with the hat 460 microns and ⊘ (90)/⊘(10) equal 1,08.

b) obtaining cation

A 2-liter flask with four necks hurt 1400 ml 98,1%sulfuric acid and heated to a temperature of 100°C. After 4 hours in the flask is added with stirring 10 servings, 350 g of dry copolymer of 7a). The mixture is then stirred for 6 hours at a temperature of 120°C. the resulting suspension is cooled and poured into a glass column. Sulfuric acid with a lower concentration ranging from 90 wt.% and ending at the end of clean water, filtered from the top through the column. Receive 1480 ml of cation exchanger in the H form.

(C) the transfer of the cation

For translation of the cation exchange resin of H-form to Na-form 1460 ml from sulphonated product of 7b) and 450 ml of deionized water at room temperature is placed in a 6-liter glass reactor. After 120 minutes, the suspension is mixed with 2361 ml of 5%aqueous caustic soda solution. The mixture is then stirred for 15 minutes. Then the obtained product is washed with deionized water. Get 1350 ml of cation exchanger in the Na-form.

The full capacity of the Na-form (mol/l)2,17
The conductivity of the eluate after 70 h (MKM/cm)0,457
Molecular weight polystyrenesulfonate acid in the eluate (g/mol)2500

Example 8 (with the accordance with the invention)

a) obtaining a copolymer

In a 4-liter glass reactor placed in an aqueous solution of 3.6 g of boric acid, 1.0 g of sodium hydroxide and 0.10 resorcinol in 1100 g of deionized water. To the resulting mixture add 648,9 g of monodisperse microencapsulated seed polymer containing 95 wt.% styrene and 5.0 wt.% divinylbenzene. The seed polymer is produced in accordance with European patent EP-0046535 B1. The wall of the capsules of the bare polymer consists of a comprehensive koatservata of gelatin and a copolymer of acrylamide/acrylic acid cured formaldehyde. The average particle size of the seed polymer is 375 μm and the value of ⊘(90)/⊘(10) is equal to 1,06. The mixture is stirred with a speed of 220 rpm Then to the resulting mixture for 30 minutes, add a mixture of 430,5 g of styrene, 48,0 g of Acrylonitrile, 73,0 g of divinylbenzene (80,6 wt.%), 2.0 g of tert-BUTYLPEROXY-2-ethylhexanoate and 1.4 g of tert-butyl peroxybenzoate as a tributary. The composition is stirred for 2 hours at a temperature of 50°S, and the gas space is washed with nitrogen. Then to the resulting product, add a solution of 2.4 g of methylhydroxyethylcellulose in 120 g of deionized water and stirred for 1 hour at a temperature of 50°C. the Composition is heated to a temperature of 61°C and maintained for 10 hours at this temperature, then paramesh who live within 3 hours at a temperature of 130° C. the Composition is cooled, washed with deionized water through a 40-micron sieve and dried in an oven for 18 hours at a temperature of 80°C. Receive 1144 g of the copolymer in the form of granules, the particle size of which is 460 μm and ⊘(90)/⊘(10) is of 1.07.

b) obtaining cation

A 2-liter flask with four necks hurt 1400 ml of 98.5%sulfuric acid and heated to a temperature of 100°C. After 4 hours in the flask is added with stirring 10 servings, 350 g of dry copolymer from 8A). The mixture is then stirred for 6 hours at a temperature of 105°C. the resulting suspension is cooled and poured into a glass column. Sulfuric acid with a lower concentration ranging from 90 wt.% and ending at the end of clean water, filtered from the top through the column. Receive 1430 ml of cation exchanger in the H form.

c) the transfer of the cation

For translation of the cation exchange resin of H-form to Na-form 1410 ml from sulphonated product of the 8b) and 450 ml of deionized water at room temperature is placed in a 4 liter glass reactor. After 120 minutes, the suspension is mixed with 1752 ml of 5%aqueous caustic soda solution. The mixture is then stirred for 15 minutes. Then the obtained product is washed with deionized water. Receive 1325 ml of cation exchanger in the Na-form.

The full capacity of the Na-form (mol/is) 2,22
The conductivity of the eluate after 70 h (MKM/cm)0,092
Molecular weight polystyrenesulfonate acid in the eluate (g/mol)<1000

Unexpectedly, the cation exchangers obtained in accordance with the present invention demonstrate through 70 hours a distinctly lower conductivity in the eluate compared to the cation exchangers obtained in accordance with European patent application EP-A 1000659.

Example 9 (in accordance with the invention)

a) obtaining a copolymer

In a 4-liter glass reactor with a frame with a stirrer, a cooling device, a heating element, a thermostat and a recorder for recording the temperature is placed aqueous solution of 1.53 g of boric acid and 0.42 g of sodium hydroxide in 521 g of deionized water. To the obtained mixture under stirring at 200 rpm add 299,1 g of monodisperse microencapsulated seed polymer containing at 95.5 wt.% styrene and 4.5 wt.% divinylbenzene. The seed polymer is produced in accordance with European patent EP-0046535 B1. Then to the resulting mixture for 30 minutes, add the mixture to 158.0 g of styrene, and 20.3 g of Acrylonitrile, 31 g of divinylbenzene (81 wt%), 0.7 g of tert-BUTYLPEROXY-2-ethylhexanoate as the radical initiator. The composition is stirred for 2 hours at t is mperature 50° C. the Gas space is washed with nitrogen to remove air. Served a solution of 1.04 g of methylhydroxyethylcellulose in 51 g of water. The mixture is heated to a temperature of 61°C and maintained for 11 hours at this temperature, then stirred for 2 hours at a temperature of 130°C. the Mixture is cooled, washed with deionized water through a 40-micron sieve and dried. Receive 468 g of monodisperse polymer particle size is 456 mm.

b) obtaining cation

A 2-liter flask with four necks put 1500 ml of 98.5%sulfuric acid and heated to a temperature of 100°C. After 4 hours in the flask is added with stirring 10 portions, a total of 375 g of dry copolymer of (9a).

The mixture is then stirred for 6 hours at a temperature of 105°C. the resulting suspension is cooled and poured into a glass column. Sulfuric acid with a lower concentration ranging from 90 wt.% and ending with clean water, wash out the top through the column. Receive 1640 ml of cation exchanger in the H form.

(C) the transfer of the cation

For translation of the cation exchange resin of H-form to Na-form 1640 ml of cation exchanger from 9b) and 500 ml of water at room temperature is placed in a 4 liter glass reactor. After 120 minutes, the suspension is mixed with 2532 ml of 5%aqueous caustic soda solution. The mixture is then stirred for 30 minutes. Receive 1510 ml of cation exchanger in the Na-form is E.

Full capacity (Na-form, mol/l)2,18
The conductivity of the eluate after 70 h (µs/cm)0,098
Molecular weight polystyrenesulfonate acid in the eluate (g/mol)<1000

1. A method of obtaining a gel-like cation seed-supply method, in which

a) use an aqueous suspension of microencapsulated cross-linked polymer of styrene in the form of granules containing a crosslinking agent, as the seed polymer

b) leave to swell the seed polymer in the mixture of monomers of the vinyl monomer, a crosslinking agent and a radical initiator, which represents an aliphatic ester of percolate,

c) polimerizuet mixture of monomers in the seed polymer and

d) functionalitywith obtained copolymer sulphurization, characterized in that stage a) the content of the crosslinking agent crosslinked polymer of styrene is 3.5-7 wt.% and the ratio of seed/inflow at the stage b) is 1:0.25 to 1:5.

2. The method according to claim 1, characterized in that the cross-linked polymer of styrene in the form of granules at the stage a) is the size distribution of particles in which the ratio of the values of 90% and 10% of the distribution function of volume is less than 2.

3. The way p is 1, characterized in that the content of the crosslinking agent in the mixture of monomers at the stage b) is 5-20 wt.%.

4. The method according to claim 1, characterized in that the vinyl monomer at the stage b) is a mixture of 88-98 wt.% styrene and 2-12 wt.% acrylic monomer.

5. The method according to claim 4, characterized in that the acrylic monomer is Acrylonitrile.

6. The method according to claim 1, characterized in that the polymerization in stage C) is carried out in a wide temperature range 50-150°C.

7. The method according to claim 1, characterized in that the mixture of monomers at the stage b) comprises a mixture of at least two different radical initiators.



 

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