CN103008022B - The production method of macroporous strong basic acrylic acid type anion exchange resin - Google Patents
The production method of macroporous strong basic acrylic acid type anion exchange resin Download PDFInfo
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- CN103008022B CN103008022B CN201210489709.3A CN201210489709A CN103008022B CN 103008022 B CN103008022 B CN 103008022B CN 201210489709 A CN201210489709 A CN 201210489709A CN 103008022 B CN103008022 B CN 103008022B
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Abstract
The invention discloses a kind of production method of macroporous strong basic acrylic acid type anion exchange resin; on traditional processing technology basis; the present invention is by reasonably combined suspension protective agent, dispersant, pore-foaming agent, complexing agent; Optimizing Process Parameters; anion exchange resin prepared by this method; even aperture distribution, the effect that exchange capacity improves, the ion exchange resin specific area that the present invention makes can reach 68m2More than/g, the mesopore ratio that is greater than 2nm is greater than 60%, and CEC reaches 5.5mmol/g.
Description
Technical field
The invention belongs to a kind of preparation method of ion exchange resin, specifically a kind of macroporous strong basic acrylic acid series the moon fromThe production method of sub-exchange resin.
Background technology
Anion and cation exchange resin is widely used for the purification of water treatment, material, concentrated, separation, substance ion compositionThe field such as decolouring and catalyst of transformation, material. Although the exchange capacity of current anion and cation exchange resin has obtainedThe raising of effect, but pore-size distribution inequality, aperture ratio is excessive, and exchange velocity is low. The problems such as exchange capacity deficiency, can not meet visitorThe requirement at family.
Summary of the invention
The object of this invention is to provide a kind of production method of macroporous strong basic acrylic acid type anion exchange resin, thisBright by the improvement of water, dispersiveness, suspension are improved, and then reach the exchange capacity that increases ion exchange resin, holeThe effect that footpath is evenly distributed.
Technical scheme of the present invention is as follows:
A production method for macroporous strong basic acrylic acid type anion exchange resin, is characterized in that:
(1) A ball is prepared in polymerization, comprises the following steps:
The water raw material that takes following weight portion, mixes, stirs:
Deionized water 500-600
Guar gum 20-25
Polyvinyl alcohol 30-35
Diethylenetriamine 15-20
Potassium chloride 30-35
Sodium sulphate 30-35
Ammonium persulfate 1-2
It is neutral adjusting PH with sulfuric acid
Take the oil phase raw material of following weight portion, after mixing, add in water, stir;
Methyl acrylate 365-375
Divinylbenzene 20-23
TAIC6-10
Isobutanol 115-125
Ferrocene 10-12
200# solvent naphtha 30-35
Isopropyl alcohol 15-20
Benzoyl peroxide 3-5
Slowly be warming up to 69-72 DEG C;
Exothermic heat of reaction is stronger, and cooling, maintains the temperature at 68-70 DEG C after heat release, insulation 2-3 hour;
Be warming up to 80-82 DEG C with 20-40 minutes and be incubated 2-3h;
Be warming up to 90-96 DEG C with 40-80 minute and be incubated 4-5h;
By hot water wash nodule number all over till limpid to water;
Drain water, dry, sub-sieve obtains A ball;
(2), aminating reaction prepares resin, comprise the following steps:
Press row weight portion and take raw material, in clean reactor, add A ball, then add 1,2 propane diamine, second twoAlcohol, stirs;
A ball 380-420
1,2 propane diamine 780-820
Ethylene glycol 880-920
Be warming up to 135-145 DEG C, insulation 4-5h; Be warming up to 155-165 DEG C, insulation 5-6h, is warming up to 165-170 DEG C,Insulation 3-4h; Be warming up to 170-175 DEG C, insulation 3-4h;
Sampling is controlled in surveying, and it is qualified that exchange is greater than 5.2mmol/g;
Take out mother liquor, washing, discharging.
The present invention is by reasonably combined suspension protective agent, dispersant, pore-foaming agent, complexing agent, and Optimizing Process Parameters, makes thisAnion exchange resin prepared by method, even aperture distribution, the effect that exchange capacity improves, the ion-exchange that the present invention makesResin specific area can reach 68m2More than/g, the mesopore ratio that is greater than 2nm is greater than 60%, and CEC reaches5.5mmol/g。
Detailed description of the invention
A kind of production method of macroporous strong basic acrylic acid type anion exchange resin:
(1) A ball is prepared in polymerization, comprises the following steps:
Take following weight (kilogram) water raw material, mix, stir:
Deionized water 600
Guar gum 20
Polyvinyl alcohol 30
Diethylenetriamine 15
Potassium chloride 30
Sodium sulphate 30
Ammonium persulfate 1
It is neutral adjusting PH with sulfuric acid
Take following weight (kilogram) oil phase raw material, after mixing, add in water, stir;
Methyl acrylate 365
Divinylbenzene 20
TAIC6
Isobutanol 115
Ferrocene 10
200# solvent naphtha 35
Isopropyl alcohol 15
Benzoyl peroxide 5
Slowly be warming up to 69-72 DEG C;
Exothermic heat of reaction is stronger, and cooling, maintains the temperature at 68-70 DEG C after heat release, insulation 2-3 hour;
Be warming up to 80-82 DEG C with 20-40 minutes and be incubated 2-3h;
Be warming up to 90-96 DEG C with 40-80 minute and be incubated 4-5h;
By hot water wash nodule number all over till limpid to water;
Drain water, dry, sub-sieve obtains A ball;
(2), aminating reaction prepares resin, comprise the following steps:
Press column weight amount (kilogram) take raw material, in clean reactor, add A ball, then add 1,2 propane diamine, secondGlycol, stirs;
A ball 380
1,2 propane diamine 780
Ethylene glycol 880
Be warming up to 135-145 DEG C, insulation 4-5h; Be warming up to 155-165 DEG C, insulation 5-6h, is warming up to 165-170 DEG C,Insulation 3-4h; Be warming up to 170-175 DEG C, insulation 3-4h;
Sampling is controlled in surveying, and it is qualified that exchange is greater than 5.2mmol/g;
Take out mother liquor, washing, discharging.
After testing, the ion exchange resin specific area that the present invention makes can reach 68m2More than/g, be greater than 2nm inBoring ratio example is greater than 60%, and CEC reaches 5.5mmol/g.
Claims (1)
1. a production method for macroporous strong basic acrylic acid type anion exchange resin, is characterized in that:
(1) A ball is prepared in polymerization, comprises the following steps:
1. the water raw material that takes following weight portion, mixes, stirs:
Deionized water 500-600
Guar gum 20-25
Polyvinyl alcohol 30-35
Diethylenetriamine 15-20
Potassium chloride 30-35
Sodium sulphate 30-35
Ammonium persulfate 1-2
It is neutral adjusting pH with sulfuric acid
2. take the oil phase raw material of following weight portion, after mixing, add in water, stir;
Methyl acrylate 365-375
Divinylbenzene 20-23
TAIC6-10
Isobutanol 115-125
Ferrocene 10-12
200# solvent naphtha 30-35
Isopropyl alcohol 15-20
Benzoyl peroxide 3-5
3. be slowly warming up to 69-72 DEG C;
4. exothermic heat of reaction is stronger, and cooling, maintains the temperature at 68-70 DEG C after heat release, insulation 2-3 hour;
5. be warming up to 80-82 DEG C of insulation 2-3h with 20-40 minutes;
6. be warming up to 90-96 DEG C with 40-80 minute and be incubated 4-5h;
7. use hot water wash nodule number all over till limpid to water;
8. drain water, dry, sub-sieve obtains A ball;
(2), aminating reaction prepares resin, comprise the following steps:
1. press row weight portion and take raw material, in clean reactor, add A ball, then add 1,2-propane diamine, ethylene glycol, stirMix;
A ball 380-420
1,2-propane diamine 780-820
Ethylene glycol 880-920
2. be warming up to 135-145 DEG C, insulation 4-5h, is warming up to 155-165 DEG C, and insulation 5-6h, is warming up to 165-170 DEG C, insulation3-4h, is warming up to 170-175 DEG C, insulation 3-4h;
3. sampling is controlled in surveying, and it is qualified that CEC is greater than 5.2mmol/g;
4. take out mother liquor, washing, discharging.
Priority Applications (1)
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CN201210489709.3A CN103008022B (en) | 2012-11-27 | 2012-11-27 | The production method of macroporous strong basic acrylic acid type anion exchange resin |
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CN201210489709.3A CN103008022B (en) | 2012-11-27 | 2012-11-27 | The production method of macroporous strong basic acrylic acid type anion exchange resin |
Publications (2)
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CN103008022A CN103008022A (en) | 2013-04-03 |
CN103008022B true CN103008022B (en) | 2016-05-25 |
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CN201210489709.3A Active CN103008022B (en) | 2012-11-27 | 2012-11-27 | The production method of macroporous strong basic acrylic acid type anion exchange resin |
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Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH06327984A (en) * | 1993-05-27 | 1994-11-29 | Sumitomo Chem Co Ltd | Anion-exchange resin |
CN101781437A (en) * | 2010-01-12 | 2010-07-21 | 南京大学 | Magnetic acrylic acid series strongly basic anion exchange microballoon resin and preparation method thereof |
CN102234352A (en) * | 2011-04-20 | 2011-11-09 | 安徽美佳新材料股份有限公司 | Preparation method of D213 macroporous strong-basic acrylic cation exchange resin |
-
2012
- 2012-11-27 CN CN201210489709.3A patent/CN103008022B/en active Active
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH06327984A (en) * | 1993-05-27 | 1994-11-29 | Sumitomo Chem Co Ltd | Anion-exchange resin |
CN101781437A (en) * | 2010-01-12 | 2010-07-21 | 南京大学 | Magnetic acrylic acid series strongly basic anion exchange microballoon resin and preparation method thereof |
CN102234352A (en) * | 2011-04-20 | 2011-11-09 | 安徽美佳新材料股份有限公司 | Preparation method of D213 macroporous strong-basic acrylic cation exchange resin |
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CN103008022A (en) | 2013-04-03 |
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