CN107126978A - A kind of high-adsorption-capacity styrenic anion exchanger resin - Google Patents
A kind of high-adsorption-capacity styrenic anion exchanger resin Download PDFInfo
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- CN107126978A CN107126978A CN201710321802.6A CN201710321802A CN107126978A CN 107126978 A CN107126978 A CN 107126978A CN 201710321802 A CN201710321802 A CN 201710321802A CN 107126978 A CN107126978 A CN 107126978A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J41/00—Anion exchange; Use of material as anion exchangers; Treatment of material for improving the anion exchange properties
- B01J41/08—Use of material as anion exchangers; Treatment of material for improving the anion exchange properties
- B01J41/12—Macromolecular compounds
- B01J41/14—Macromolecular compounds obtained by reactions only involving unsaturated carbon-to-carbon bonds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
- C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F212/06—Hydrocarbons
- C08F212/08—Styrene
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Abstract
The invention discloses a kind of high-adsorption-capacity styrenic anion exchanger resin, its raw material includes by weight：30 50 parts of styrene, 37 parts of divinylbenzene, 0.5 0.7 parts of potassium peroxydisulfate, 0.4 0.8 parts of potassium chloride, 8 12 parts of composite diatomite urea, 48 parts of hydroxymethyl cellulose, 50 70 parts of dichloromethane, 80 120 parts of water, 24 parts of carbon tetrachloride, 130 170 parts of sulfuric acid solution.Not only chemical stability is good by the present invention, high mechanical strength, adsorption capacity is very big, surface-active is high, and can effectively promote storeroom high degree of dispersion, and reaction stability is fabulous, particle uniformity coefficient is high simultaneously, a large amount of permanent micropores are contained in inside, and reduction reaction intermediate is deposited on duct, to reach raising yield, shorten reaction time, simplified later separation process, the purpose realized continuous production, improve yield.
Description
Technical field
Exchanged the present invention relates to ion-exchange resin technique field, more particularly to a kind of high-adsorption-capacity styrenic anion
Resin.
Background technology
Ion exchange resin is a kind of functional high molecule material containing ion-exchange group in cross-linked polymer structures.
Insoluble in general acid-base solution and many organic solvents.It can be widely applied to water process.Phenylethylene resin series in the prior art,
Including styrene-divinylbenzene, styrenic anion exchanger resin etc. has obtained extensive as adsorbent and ion-exchanger
Using, but at present there is reaction intermediate and be easy to be deposited on duct in styrene ion exchange resin, and adsorption capacity is met
Not the problem of demand, it would be highly desirable to solve.
The content of the invention
The present invention proposes a kind of high-adsorption-capacity styrenic anion exchanger resin, high mechanical strength, and intermediate product is not
It is easy to be deposited on duct.
A kind of high-adsorption-capacity styrenic anion exchanger resin proposed by the present invention, its raw material includes by weight：Benzene
30-50 parts of ethene, 3-7 parts of divinylbenzene, 0.5-0.7 parts of potassium peroxydisulfate, 0.4-0.8 parts of potassium chloride, composite diatomite urea 8-
12 parts, 4-8 parts of hydroxymethyl cellulose, 50-70 parts of dichloromethane, 80-120 parts of water, 2-4 parts of carbon tetrachloride, sulfuric acid solution 130-
170 parts.
Preferably, sulfuric acid solution concentration is 95-98%.
Preferably, composite diatomite urea is prepared using following technique：Sodium hydroxide, urea, water are well mixed, added
After microcrystalline cellulose stirring and dissolving, solidify, filter, washing adds 2,2,6,6- tetramethyl piperidine -1- epoxides, sodium bromide, 3- chlorine
Propyl trimethoxy silicane, acidifying diatomite, water stirring, add liquor natrii hypochloritis and stir, and regulation system pH value is 10-
10.8, filtering obtains prefabricated material；Deionized water, endecatylene amido propyl betaine, prefabricated material are well mixed, added double
Oxygen water heating stirring, separation, solids is washed with deionized in neutrality, dries, obtain composite diatomite urea.
Preferably, composite diatomite urea is prepared using following technique：Sodium hydroxide, urea, water are well mixed, added
After microcrystalline cellulose stirring and dissolving, solidify 15-25min, filter, washing adds 2,2,6,6- tetramethyl piperidine -1- epoxides, bromine
Change sodium, 3- r-chloropropyl trimethoxyl silanes, acidifying diatomite, water stirring 15-25min, addition concentration is 8-16wt% hypochlorous acid
Sodium solution stirs, and regulation system pH value is 10-10.8, and filtering obtains prefabricated material；By deionized water, endecatylene acid amides
CAB, prefabricated material are well mixed, and it is that 34-38wt% hydrogen peroxide mixes 40- for 70-80 DEG C in temperature to add concentration
60min, separation, solids is washed with deionized in neutrality, is dried, is obtained composite diatomite urea.
Preferably, composite diatomite urea is prepared using following technique：By weight by 10-15 parts of sodium hydroxides, 20-30
Part urea, 120-160 parts of water are well mixed, and are added after 15-25 parts of microcrystalline cellulose stirring and dissolvings, are solidified 15-25min, filter,
Washing, adds the tetramethyl piperidine -1- epoxides of 0.6-1.2 parts 2,2,6,6-, 4-8 parts of sodium bromides, 4-8 parts of 3- r-chloropropyl trimethoxyls
Silane, 10-20 parts of acidifying diatomite, 100-140 parts of water stirring 15-25min, it is 8-16wt% hypochlorous acid to add 2-4 parts of concentration
Sodium solution stirs, and regulation system pH value is 10-10.8, and filtering obtains prefabricated material；By weight by 100 parts of deionized waters,
10-20 parts of endecatylene amido propyl betaines, 30-50 parts of prefabricated material are well mixed, and it is 34-38wt% to add 4-8 parts of concentration
Hydrogen peroxide is washed with deionized in neutrality in 70-80 DEG C of mixing 40-60min of temperature, separation, solids, dries, obtain
To composite diatomite urea.
Cost of the present invention is relatively low, is difficult to degrade because of oxidation, hydrolysis or high temperature, reproducibility is good, available for various in water
The removal of zwitterion, utilizes the poisonous ion in ion exchange resin recycle-water；And in composite diatomite urea, urea
Reacted in the basic conditions with microcrystalline cellulose, using 2,2,6,6- tetramethyl piperidine -1- epoxide oxidation processes, permeability is good,
The introducing of sodium hypochlorite simultaneously can effectively strengthen adsorptivity, and endecatylene amido propyl betaine is containing alkyl functional group and acyl
Amidine functional group, can be with 3- r-chloropropyl trimethoxyl silanes, acidifying diatomite reaction, and not only chemical stability is good for product, machinery
Intensity is high, and greatly, surface-active is high, and can effectively promote storeroom high degree of dispersion, and reaction stability is fabulous for adsorption capacity,
Particle uniformity coefficient is high simultaneously, and composite diatomite urea is compounded with carbon tetrachloride, can form the bone of mandruka columnar structure
Frame, not only mechanical strength is high, and containing a large amount of permanent micropores inside product, and microsphere surface accumulates very big, microballoon ball wall
There are many holes, and the addition of composite diatomite urea can increase space steric effect, reduction reaction intermediate is deposited on hole
Road, yield, shortening reaction time, simplified later separation process, the mesh realized continuous production, improve yield are improved to reach
's.
Embodiment
Below, technical scheme is described in detail by specific embodiment.
Embodiment 1
A kind of high-adsorption-capacity styrenic anion exchanger resin proposed by the present invention, its raw material includes by weight：Benzene
30 parts of ethene, 7 parts of divinylbenzene, 0.5 part of potassium peroxydisulfate, 0.8 part of potassium chloride, 8 parts of composite diatomite urea, hydroxymethyl cellulose
8 parts, 50 parts of dichloromethane, 120 parts of water, 2 parts of carbon tetrachloride, 170 parts of sulfuric acid solution.
Embodiment 2
A kind of high-adsorption-capacity styrenic anion exchanger resin proposed by the present invention, its raw material includes by weight：Benzene
50 parts of ethene, 3 parts of divinylbenzene, 0.7 part of potassium peroxydisulfate, 0.4 part of potassium chloride, 12 parts of composite diatomite urea, hydroxylmethyl cellulose
4 parts of element, 70 parts of dichloromethane, 80 parts of water, 4 parts of carbon tetrachloride, 130 parts of sulfuric acid solution.
Composite diatomite urea is prepared using following technique：Sodium hydroxide, urea, water are well mixed, crystallite is added fine
After the plain stirring and dissolving of dimension, solidify, filter, washing adds 2,2,6,6- tetramethyl piperidine -1- epoxides, sodium bromide, 3- chloropropyls three
Methoxy silane, acidifying diatomite, water stirring, add liquor natrii hypochloritis and stir, and regulation system pH value is 10-10.8,
Filtering, obtains prefabricated material；Deionized water, endecatylene amido propyl betaine, prefabricated material are well mixed, hydrogen peroxide liter is added
Temperature stirring, separation, solids is washed with deionized in neutrality, is dried, is obtained composite diatomite urea.
Embodiment 3
A kind of high-adsorption-capacity styrenic anion exchanger resin proposed by the present invention, its raw material includes by weight：Benzene
35 parts of ethene, 6 parts of divinylbenzene, 0.55 part of potassium peroxydisulfate, 0.7 part of potassium chloride, 9 parts of composite diatomite urea, hydroxylmethyl cellulose
7 parts of element, 55 parts of dichloromethane, 110 parts of water, 2.5 parts of carbon tetrachloride, concentration is 98% 140 parts of sulfuric acid solution.
Composite diatomite urea is prepared using following technique：Sodium hydroxide, urea, water are well mixed, crystallite is added fine
After the plain stirring and dissolving of dimension, solidify 20min, filter, washing adds 2,2,6,6- tetramethyl piperidine -1- epoxides, sodium bromide, 3- chlorine
Propyl trimethoxy silicane, acidifying diatomite, water stirring 20min, it is that 12wt% liquor natrii hypochloritises stir to add concentration,
Regulation system pH value is 10-10.8, and filtering obtains prefabricated material；By deionized water, endecatylene amido propyl betaine, prefabricated
Material is well mixed, and it is that 36wt% hydrogen peroxide mixes 50min, separation, solids deionization for 75 DEG C in temperature to add concentration
Water washing is dried in neutrality, obtains composite diatomite urea.
Embodiment 4
A kind of high-adsorption-capacity styrenic anion exchanger resin proposed by the present invention, its raw material includes by weight：Benzene
45 parts of ethene, 4 parts of divinylbenzene, 0.65 part of potassium peroxydisulfate, 0.5 part of potassium chloride, 11 parts of composite diatomite urea, hydroxylmethyl cellulose
5 parts of element, 65 parts of dichloromethane, 90 parts of water, 3.5 parts of carbon tetrachloride, concentration is 95% 160 parts of sulfuric acid solution.
Composite diatomite urea is prepared using following technique：By weight by 10 parts of sodium hydroxides, 30 parts of urea, 120 parts
Water is well mixed, and is added after 25 parts of microcrystalline cellulose stirring and dissolvings, solidifies 15min, is filtered, and washing adds 1.2 part 2,2,6,6-
Tetramethyl piperidine -1- epoxides, 4 parts of sodium bromides, 8 parts of 3- r-chloropropyl trimethoxyl silanes, 10 parts of acidifying diatomite, 140 parts of water are stirred
15min is mixed, it is that 8wt% liquor natrii hypochloritises stir to add 4 parts of concentration, regulation system pH value is 10-10.8, filtering is obtained
To prefabricated material；100 parts of deionized waters, 20 parts of endecatylene amido propyl betaines, 30 parts of prefabricated material are mixed equal by weight
Even, it is that 34wt% hydrogen peroxide mixes 40min for 80 DEG C in temperature to add 8 parts of concentration, and separation, solids is washed with deionized
To in neutrality, dry, obtain composite diatomite urea.
Embodiment 5
A kind of high-adsorption-capacity styrenic anion exchanger resin proposed by the present invention, its raw material includes by weight：Benzene
40 parts of ethene, 5 parts of divinylbenzene, 0.6 part of potassium peroxydisulfate, 0.6 part of potassium chloride, 10 parts of composite diatomite urea, hydroxylmethyl cellulose
6 parts of element, 60 parts of dichloromethane, 100 parts of water, 3 parts of carbon tetrachloride, concentration is 96% 150 parts of sulfuric acid solution.
Composite diatomite urea is prepared using following technique：By weight by 15 parts of sodium hydroxides, 20 parts of urea, 160 parts
Water is well mixed, and is added after 15 parts of microcrystalline cellulose stirring and dissolvings, solidifies 25min, is filtered, and washing adds 0.6 part 2,2,6,6-
Tetramethyl piperidine -1- epoxides, 8 parts of sodium bromides, 4 parts of 3- r-chloropropyl trimethoxyl silanes, 20 parts of acidifying diatomite, 100 parts of water are stirred
25min is mixed, it is that 16wt% liquor natrii hypochloritises stir to add 2 parts of concentration, regulation system pH value is 10-10.8, filtering is obtained
To prefabricated material；100 parts of deionized waters, 10 parts of endecatylene amido propyl betaines, 50 parts of prefabricated material are mixed equal by weight
Even, it is that 38wt% hydrogen peroxide mixes 60min in temperature 70 C to add 4 parts of concentration, and separation, solids is washed with deionized
To in neutrality, dry, obtain composite diatomite urea.
Performance measurement is carried out to the gained high-adsorption-capacity styrenic anion exchanger resin of embodiment 5：Full exchange capacity is
2.73mmol/g, adsorption capacity reduced by only water after 2.3%, processing and can reach drinking water standard after regenerating ten times
(GB5749-2011)。
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art the invention discloses technical scope in, technique according to the invention scheme and its
Inventive concept is subject to equivalent substitution or change, should all be included within the scope of the present invention.
Claims (5)
1. a kind of high-adsorption-capacity styrenic anion exchanger resin, it is characterised in that its raw material includes by weight：Styrene
30-50 parts, 3-7 parts of divinylbenzene, 0.5-0.7 parts of potassium peroxydisulfate, 0.4-0.8 parts of potassium chloride, 8-12 parts of composite diatomite urea,
4-8 parts of hydroxymethyl cellulose, 50-70 parts of dichloromethane, 80-120 parts of water, 2-4 parts of carbon tetrachloride, 130-170 parts of sulfuric acid solution.
2. high-adsorption-capacity styrenic anion exchanger resin according to claim 1, it is characterised in that sulfuric acid solution concentration
For 95-98%.
3. high-adsorption-capacity styrenic anion exchanger resin according to claim 1, it is characterised in that composite diatomite is urinated
Element is prepared using following technique：Sodium hydroxide, urea, water are well mixed, added after microcrystalline cellulose stirring and dissolving, solidification,
Filtering, washing adds 2,2,6,6- tetramethyl piperidine -1- epoxides, sodium bromide, 3- r-chloropropyl trimethoxyl silanes, acidifying diatom
Soil, water stirring, add liquor natrii hypochloritis and stir, and regulation system pH value is 10-10.8, and filtering obtains prefabricated material；It will go
Ionized water, endecatylene amido propyl betaine, prefabricated material are well mixed, and add hydrogen peroxide heating stirring, and separation, solids is used
Deionized water is washed in neutrality, is dried, is obtained composite diatomite urea.
4. high-adsorption-capacity styrenic anion exchanger resin according to claim 1 or claim 2, it is characterised in that tripolite compound
Urea is closed to prepare using following technique：Sodium hydroxide, urea, water are well mixed, added after microcrystalline cellulose stirring and dissolving, Gu
Change 15-25min, filter, washing adds 2,2,6,6- tetramethyl piperidine -1- epoxides, sodium bromide, 3- r-chloropropyl trimethoxyl silicon
Alkane, acidifying diatomite, water stirring 15-25min, it is that 8-16wt% liquor natrii hypochloritises stir to add concentration, regulation system
PH value is 10-10.8, filtering, obtains prefabricated material；Deionized water, endecatylene amido propyl betaine, prefabricated material are mixed equal
Even, it is that 34-38wt% hydrogen peroxide mixes 40-60min, separation, solids deionization for 70-80 DEG C in temperature to add concentration
Water washing is dried in neutrality, obtains composite diatomite urea.
5. according to any one of the claim 1-3 high-adsorption-capacity styrenic anion exchanger resins, it is characterised in that diatom
Native composite urea is prepared using following technique：By weight by 10-15 parts of sodium hydroxides, 20-30 parts of urea, 120-160 parts of water
It is well mixed, add after 15-25 parts of microcrystalline cellulose stirring and dissolvings, solidify 15-25min, filter, washing adds 0.6-1.2 parts
2,2,6,6- tetramethyl piperidine -1- epoxides, 4-8 parts of sodium bromides, 4-8 parts of 3- r-chloropropyl trimethoxyl silanes, 10-20 parts of acidifying silicon
Diatomaceous earth, 100-140 parts of water stir 15-25min, and it is that 8-16wt% liquor natrii hypochloritises stir to add 2-4 parts of concentration, is adjusted
System pH is 10-10.8, filtering, obtains prefabricated material；By weight by 100 parts of deionized waters, 10-20 parts of endecatylene acid amides
CAB, 30-50 parts of prefabricated material are well mixed, and it is 34-38wt% hydrogen peroxide in 70-80 DEG C of temperature to add 4-8 part concentration
40-60min, separation are mixed, solids is washed with deionized in neutrality, dries, obtain composite diatomite urea.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710321802.6A CN107126978A (en) | 2017-05-09 | 2017-05-09 | A kind of high-adsorption-capacity styrenic anion exchanger resin |
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| CN201710321802.6A CN107126978A (en) | 2017-05-09 | 2017-05-09 | A kind of high-adsorption-capacity styrenic anion exchanger resin |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103012658A (en) * | 2012-11-27 | 2013-04-03 | 安徽皖东化工有限公司 | Production method for strongly basic anion exchange resin |
| CN105037783A (en) * | 2015-07-09 | 2015-11-11 | 安徽皖东化工有限公司 | Preparation method for rare earth modified strongly acidic styrene cation exchange resin |
| CN105218722A (en) * | 2015-09-21 | 2016-01-06 | 安徽皖东化工有限公司 | A kind of preparation method of water purification polystyrene sulfonic acid type ion exchange resin |
| CN105642237A (en) * | 2016-02-17 | 2016-06-08 | 济南大学 | Preparation method of undecylene amido propyl betaine modified diatomite |
-
2017
- 2017-05-09 CN CN201710321802.6A patent/CN107126978A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103012658A (en) * | 2012-11-27 | 2013-04-03 | 安徽皖东化工有限公司 | Production method for strongly basic anion exchange resin |
| CN105037783A (en) * | 2015-07-09 | 2015-11-11 | 安徽皖东化工有限公司 | Preparation method for rare earth modified strongly acidic styrene cation exchange resin |
| CN105218722A (en) * | 2015-09-21 | 2016-01-06 | 安徽皖东化工有限公司 | A kind of preparation method of water purification polystyrene sulfonic acid type ion exchange resin |
| CN105642237A (en) * | 2016-02-17 | 2016-06-08 | 济南大学 | Preparation method of undecylene amido propyl betaine modified diatomite |
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Application publication date: 20170905 |