CN103012654B - The production method of macroporous strong basic methyl acrylate anionite-exchange resin - Google Patents
The production method of macroporous strong basic methyl acrylate anionite-exchange resin Download PDFInfo
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- CN103012654B CN103012654B CN201210489598.6A CN201210489598A CN103012654B CN 103012654 B CN103012654 B CN 103012654B CN 201210489598 A CN201210489598 A CN 201210489598A CN 103012654 B CN103012654 B CN 103012654B
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Abstract
The invention discloses a kind of production method of macroporous strong basic methyl acrylate anionite-exchange resin; on traditional processing technology basis; the present invention is by reasonably combined suspension protective material, dispersion agent, pore-creating agent, complexing agent; Optimizing Process Parameters; make anionite-exchange resin prepared by present method; even aperture distribution, the effect that exchange capacity improves, the ion exchange resin specific surface area that the present invention obtains can reach 65m
2/ g? do you above, be greater than 2nm? mesopore proportion be greater than 55%, complete exchange capacity reaches 5.5mmol/g.
Description
Technical field
The invention belongs to a kind of preparation method of ion exchange resin, specifically a kind of production method of macroporous strong basic methyl acrylate anionite-exchange resin.
Background technology
Anion and cation exchange resin be widely used for water treatment, material purification, concentrated, be separated, the transformation of substance ion composition, the field such as the decolouring of material and catalyzer.Although the exchange capacity of current anion and cation exchange resin obtains effective raising, pore size distribution is uneven, and aperture ratio is excessive, and exchange velocity is low.The problems such as exchange capacity is not enough, can not meet the requirement of client.
Summary of the invention
The object of this invention is to provide a kind of production method of macroporous strong basic methyl acrylate anionite-exchange resin, the present invention is by the improvement of aqueous phase, dispersiveness, suspension are improved, and then reaches the exchange capacity increasing ion exchange resin, the effect of even aperture distribution.
Technical scheme of the present invention is as follows:
The production method of macroporous strong basic methyl acrylate anionite-exchange resin, is characterized in that:
(1) polymerization preparation A ball, comprises the following steps:
press row weight part and take oil phase raw material:
Methyl acrylate 365-375
Triethylene glycol diacetate esters 50-60
Divinylbenzene 20-23
TAIC6-10
Isopropylcarbinol 115-125
Benzoyl peroxide 1-2
Diisopropyl azodicarboxylate 3-5
prepare aqueous phase by following parts by weight of raw materials, stir, the oil phase raw material mixed is added in aqueous phase, stir;
Aqueous phase:
Deionized water 400-450
Guar gum 10-12
Polyvinyl alcohol 10-15
Triethylene tetramine 15-20
Sodium-chlor 40-45
Sodium Persulfate 1-2
PH is adjusted to be 6.8-7.2 with sulfuric acid
slowly be warming up to 69-72 DEG C;
exothermic heat of reaction is than stronger, and cooling, maintains the temperature at 68-70 DEG C after heat release, insulation 2-3 hour;
80-82 DEG C of insulation 2-3h is warming up to 20-40 minutes;
90-96 DEG C of insulation 4-5h is warming up to 40-80 minute;
with hot water wash ball number all over to water is limpid;
drain water, dry, sub-sieve obtains A ball;
(2), amination reaction prepares resin, comprises the following steps:
press row weight part and take raw material, in clean reactor, add A ball, then add 1,2 propylene diamine, ethylene glycol, stir;
A ball 380-420
1,2 propylene 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 4.2mmol/g;
take out mother liquor, washing, discharging.
The present invention is by reasonably combined suspension protective material, dispersion agent, pore-creating agent, complexing agent; Optimizing Process Parameters, makes anionite-exchange resin prepared by present method, even aperture distribution; the effect that exchange capacity improves, the ion exchange resin specific surface area that the present invention obtains can reach 65m
2/ more than g, the mesopore proportion being greater than 2nm is greater than 50%, and complete exchange capacity reaches 5.5mmol/g.
Embodiment
The production method of macroporous strong basic methyl acrylate anionite-exchange resin:
(1) polymerization preparation A ball, comprises the following steps:
press column weight amount (kilogram) and take oil phase raw material:
Methyl acrylate 365
Triethylene glycol diacetate esters 50
Divinylbenzene 20
TAIC10
Isopropylcarbinol 115
Benzoyl peroxide 1
Diisopropyl azodicarboxylate 3
prepare aqueous phase by following raw material weight (kilogram), stir, the oil phase raw material mixed is added in aqueous phase, stir;
Aqueous phase:
Deionized water 400
Guar gum 12
Polyvinyl alcohol 10
Triethylene tetramine 15
Sodium-chlor 40
Sodium Persulfate 1
PH is adjusted to be neutral with sulfuric acid
slowly be warming up to 69-72 DEG C;
exothermic heat of reaction is than stronger, and cooling, maintains the temperature at 68-70 DEG C after heat release, insulation 2-3 hour;
80-82 DEG C of insulation 2-3h is warming up to 30-40 minutes;
90-96 DEG C of insulation 4-5h is warming up to 60-80 minute;
with hot water wash ball number all over to water is limpid;
drain water, dry, sub-sieve obtains A ball;
(2), amination reaction prepares resin, comprises the following steps:
press column weight amount (kilogram) and take raw material, in clean reactor, add A ball, then add 1,2 propylene diamine, ethylene glycol, stir;
A ball 380
1,2 propylene 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 4.2mmol/g;
take out mother liquor, washing, discharging.
The ion exchange resin specific surface area that the present invention obtains can reach 65m
2/ more than g, the mesopore proportion being greater than 2nm is greater than 50%, and complete exchange capacity reaches 5.5mmol/g.
Claims (1)
1. the production method of macroporous strong basic methyl acrylate anionite-exchange resin, it is characterized in that: (1) polymerization preparation A ball, comprise the following steps: press row weight part and take oil phase raw material: methyl acrylate 365-375 triethylene glycol diacetate esters 50-60 divinylbenzene 20-23TAIC6-10 isopropylcarbinol 115-125 benzoyl peroxide 1-2 Diisopropyl azodicarboxylate 3-5 prepares aqueous phase by following parts by weight of raw materials, stir, the oil phase raw material mixed is added in aqueous phase, stirs; Aqueous phase: deionized water 400-450 guar gum 10-12 polyvinyl alcohol 10-15 triethylene tetramine 15-20 sodium-chlor 40-45 Sodium Persulfate 1-2 sulfuric acid adjusts pH to be that 6.8-7.2 is slowly warming up to 69-72 DEG C; Exothermic heat of reaction is than stronger, and cooling, maintains the temperature at 68-70 DEG C after heat release, insulation 2-3 hour; 80-82 DEG C of insulation 2-3h is warming up to 20-40 minutes; 90-96 DEG C of insulation 4-5h is warming up to 40-80 minute; With hot water wash ball number all over to water is limpid; Drain water, dry, sub-sieve obtains A ball; (2), amination reaction prepares resin, comprises the following steps: press row weight part and take raw material, add A ball, then add 1 in clean reactor, 2 propylene diamine, ethylene glycol, stirs; A ball 380-4201,2 propylene diamine 780-820 ethylene glycol 880-920 are 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 complete exchange capacity is greater than 4.2mmol/g; Take out mother liquor, washing, discharging.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210489598.6A CN103012654B (en) | 2012-11-27 | 2012-11-27 | The production method of macroporous strong basic methyl acrylate anionite-exchange resin |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210489598.6A CN103012654B (en) | 2012-11-27 | 2012-11-27 | The production method of macroporous strong basic methyl acrylate anionite-exchange resin |
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| CN103012654A CN103012654A (en) | 2013-04-03 |
| CN103012654B true CN103012654B (en) | 2016-04-27 |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104974284A (en) * | 2015-05-27 | 2015-10-14 | 安徽皖东树脂科技有限公司 | Method for producing macroporous alkalescent acrylic anion exchange resin |
| CN105037663A (en) * | 2015-07-09 | 2015-11-11 | 安徽皖东化工有限公司 | Preparation method for inorganic modified macroporous weakly basic anion exchange resin |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN101829609A (en) * | 2010-05-25 | 2010-09-15 | 中蓝晨光化工研究院有限公司 | Tertiary-amino-containing macroporous anion exchange 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 |
| CN102641754A (en) * | 2012-05-11 | 2012-08-22 | 南开大学 | Preparation method for weak-base anion-exchange resin of novel acrylate skeleton |
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2012
- 2012-11-27 CN CN201210489598.6A patent/CN103012654B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN101829609A (en) * | 2010-05-25 | 2010-09-15 | 中蓝晨光化工研究院有限公司 | Tertiary-amino-containing macroporous anion exchange 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 |
| CN102641754A (en) * | 2012-05-11 | 2012-08-22 | 南开大学 | Preparation method for weak-base anion-exchange resin of novel acrylate skeleton |
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| CN103012654A (en) | 2013-04-03 |
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