CN101445573A - Method for preparing single-dispersibility polystyrene-DVE - Google Patents
Method for preparing single-dispersibility polystyrene-DVE Download PDFInfo
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- CN101445573A CN101445573A CNA2007101710845A CN200710171084A CN101445573A CN 101445573 A CN101445573 A CN 101445573A CN A2007101710845 A CNA2007101710845 A CN A2007101710845A CN 200710171084 A CN200710171084 A CN 200710171084A CN 101445573 A CN101445573 A CN 101445573A
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Abstract
The invention provides a method for preparing single-dispersibility polystyrene-DVE, comprising the steps as follows: mixed solution consisting of cinnamene (St), divinylbenzene (DVB) and benzoyl peroxide (BPO) is poured in polyvinyl alcohol solution, mixed for 0.2-1h at the temperature of 20-35 DEG C and heated to the temperature of 70-80 DEG C; subsequently, the temperature is kept for 0.75-1.0h; surfactant solution is added in the mixed solution with the temperature kept for 0.5-1.0h; subsequently, the mixed solution is heated to the temperature of 85-95 DEG C and the temperature is kept for 0.75-1.0h; subsequently, the mixed solution is aged and the single-dispersibility polystyrene-DVE is collected out of the reaction products. The cross-linked polystyrene-DVE provided by the method has the advantages of excellent performance, high mechanical strength, high attrition sphericity not less than 90%, and meeting the requirement of ion exchange resin framework with all indexes.
Description
Technical field
The present invention relates to the preparation method of polystyrene Archon.
Technical background
The styrene suspension crosslinking polymerization is the polymerization process a kind of commonly used that is used to prepare ion exchange resin skeleton multipolymer.Use suspension polymerization and prepare polymer microsphere, controllability and monodispersity that its main technic index is a microspherulite diameter.
In the suspension polymerization process, in the presence of stirring, monomeric drop is ceaselessly carrying out assembling and is disperseing.Along with the increase of extent of polymerization, the viscosity of liquid also can increase gradually, when transformation efficiency reaches certain degree, the drop of monomer and polymkeric substance is clamminess, and at this moment during two kinds of droplet collisions, just can stick together, stir promotion caking on the contrary, enter suspension polymerization and lump critical days.For controlling the size-grade distribution of pearl body in the styrene suspension copolymerization effectively, prevent to expect that the bonding of grain is most important.
In the reaction of the suspension copolymerization of vinylbenzene and divinylbenzene, be water miscible organic polymer as the polyvinyl alcohol or the gelatin of dispersion agent, make monomer mutually and the aqueous phase interface interlayer form protective layer, can make the drop dispersion and prevent that they are adhered to one another.But along with the increase of polymerisation conversion in the reaction process, the viscosity of drop also increases thereupon, and list can not effectively prevent that with polyvinyl alcohol or gelatin drop from owing to collision merges, needing to add the dissemination that dispersion aids improves suspension system.
At present, the preparation method of traditional single-dispersibility polystyrene-DVE, effective yield of the single-dispersibility polystyrene-DVE that is obtained is lower, generally only is about 75%, and cost height, complex process can not adapt to need of industrial production simultaneously.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of single-dispersibility polystyrene-DVE, to overcome the above-mentioned defective that prior art exists.
Method of the present invention comprises the steps:
Vinylbenzene (St), divinylbenzene (DVB) and benzoyl peroxide (BPO) mixed solution are poured in the polyvinyl alcohol water solution, then under 20～35 ℃, stir 0.2～1h, be warming up to 70～80 ℃, be incubated 0.75～1.0 hour, add water phase surfactant mixture, behind insulation 0.5～1h, be warming up to 85～95 ℃, insulation 0.75～1.0h slaking, make drop hardening balling-up, from reaction product, collect single-dispersibility polystyrene-DVE then.
Said tensio-active agent is selected from nonionic surface active agent, anion surfactant, cats product or amphoterics;
Said nonionic surface active agent such as fiber are derivative or dehydration sorb sugar ester etc.;
Said anion surfactant such as carboxylate salt, vitriol, sulfonate or phosphoric acid salt etc.;
Said cats product such as quaternary amine etc.;
Said amphoterics such as amino acid etc.
Can be a kind of of above-mentioned tensio-active agent or its mixture;
The weight concentration of water phase surfactant mixture is 0.005%～0.1%;
The weight concentration of polyvinyl alcohol water solution is 0.05～1.0%;
In the reaction system, the parts by weight of each component are:
40～100 parts of vinylbenzene (St)
0～20 part of divinylbenzene (DVB)
0.1～0.8 part of benzoyl peroxide (BPO)
0.05～1.0 part of polyvinyl alcohol water solution
0.005～0.1 part of water phase surfactant mixture.
The present invention prepares the polymerization reaction late stage of polystyrene Archon process at suspension polymerization, by adding the method for tensio-active agent, the viscosity of control reaction system, the heat transfer efficiency of improvement system, strengthen the dissemination of suspension system, to prevent to lump and the generation of fine powder, improve the yield of the effective sphere diameter of polystyrene Archon, the yield of 26 orders～effective sphere diameter of 60 orders is more than 95%.Crosslinked polystyrene Archon material property provided by the invention is good, has higher physical strength, mill rate of small round spheres 〉=90%, and every index satisfies the requirement of ion exchange resin skeleton.
Embodiment
If no special instructions, be weight part among the embodiment.
Comparative Examples 1
The mixed solution of 75 parts of vinylbenzene (St), 11 parts of divinylbenzenes (DVB), 0.4 part of benzoyl peroxide (BPO) is poured in the aqueous solution of 100 parts of deionized waters and 0.2 part of polyvinyl alcohol composition, under the room temperature, mechanical stirring 0.5h is warming up to 75 ℃, behind insulation 0.75h under 75 ℃, be warming up to 92 ℃, and insulation 1h, enter maturation stage, make drop hardening balling-up, ball is filtered, washs, dries, sieves, and obtaining granularity is the qualified copolymerization Archons of 26 orders～60 purposes.
Size distribution is as follows:
| The order number | 26 orders | 26～30 orders | 30～40 orders | 40～60 orders | ＜60 orders |
| Quality percentage yield | 25.3 | 3.6 | 10.8 | 50.4 | 9.9 |
Have a large amount of macrobead adhesive and＜60 purpose fine powders, the 26 orders～effective sphere diameter copolymerization of 60 purposes Archon only is 64.8%.
Embodiment 1
The mixed solution of 75 parts of vinylbenzene (St), 11 parts of divinylbenzenes (DVB), 0.4 part of benzoyl peroxide (BPO) is poured in the aqueous solution of 100 parts of deionized waters and 0.2 part of polyvinyl alcohol composition, then under 35 ℃, stir 1h, be warming up to 80 ℃, be incubated 1.0 hours, add 0.01 part of lauryl sodium sulfate aqueous solution, behind the insulation 1h, be warming up to 95 ℃, insulation 1.0h slaking, make drop hardening balling-up, filter then, wash, dry, sieve, obtaining granularity is the qualified copolymerization Archons of 26 orders～60 purposes.
The weight concentration of lauryl sodium sulfate aqueous solution is 0.005%.
Size distribution is as follows:
| The order number | 26 orders | 26～30 orders | 30～40 orders | 40～60 orders | ＜60 orders |
| Quality percentage yield | 1.9 | 3.0 | 9.9 | 84.2 | 1.0 |
A spot of macrobead adhesive and＜60 purpose fine powders are only arranged, and 26 orders～the effective sphere diameter copolymerization of 60 purposes Archon is up to 97.1%, and major part concentrates between 40～60 orders.
Embodiment 2
The mixed solution of 75 parts of vinylbenzene (St), 5 parts of divinylbenzenes (DVB), 0.4 part of benzoyl peroxide (BPO) is poured in the aqueous solution of 100 parts of deionized waters and 0.2 part of polyvinyl alcohol composition, then under 20 ℃, stir 0.2h, be warming up to 70 ℃, be incubated 0.75 hour, the aqueous solution that adds 0.03 part of polysorbate60, behind the insulation 0.5h, be warming up to 85 ℃, insulation 0.75h slaking, make drop hardening balling-up, filter then, wash, dry, sieve, obtaining granularity is the qualified copolymerization Archons of 26 orders～60 purposes.
The weight concentration of the polysorbate60 aqueous solution is 0.1%.
Size distribution is as follows:
| The order number | 26 orders | 26～30 orders | 30～40 orders | 40～60 orders | ＜60 orders |
| Quality percentage yield | 1.5 | 2.5 | 11.3 | 83.5 | 1.2 |
A spot of macrobead adhesive and＜60 purpose fine powders are only arranged, and 26 orders～the effective sphere diameter copolymerization of 60 purposes Archon is up to 97.3%, and major part concentrates between 40～60 orders.
Embodiment 3
The mixed solution of 75 parts of vinylbenzene (St), 9 parts of divinylbenzenes (DVB), 0.5 part of benzoyl peroxide (BPO) is poured in the aqueous solution of 100 parts of deionized waters and 0.15 part of polyvinyl alcohol composition, then under 20 ℃, stir 0.2h, be warming up to 70 ℃, be incubated 0.75 hour, the aqueous solution that adds 0.02 part of cetyl trimethylammonium bromide, behind the insulation 0.5h, be warming up to 85 ℃, insulation 0.75h slaking, make drop hardening balling-up, filter then, wash, dry, sieve, obtaining granularity is the qualified copolymerization Archons of 26 orders～60 purposes.
The weight concentration of the cetyl trimethylammonium bromide aqueous solution is 0.01%.
Size distribution is as follows:
| The order number | 26 orders | 26～30 orders | 30～40 orders | 40～60 orders | ＜60 orders |
| Quality percentage yield | 1.3 | 2.1 | 18.9 | 75.5 | 2.2 |
A spot of macrobead adhesive and＜60 purpose fine powders are only arranged, and 26 orders～the effective sphere diameter copolymerization of 60 purposes Archon is up to 96.5%, and major part concentrates between 40～60 orders.
Claims (8)
1. the preparation method of single-dispersibility polystyrene-DVE, it is characterized in that comprising the steps: vinylbenzene (St), divinylbenzene (DVB) and benzoyl peroxide (BPO) mixed solution are poured in the polyvinyl alcohol water solution, then under 20～35 ℃, stir 0.2～1h, be warming up to 70～80 ℃, be incubated 0.75～1.0 hour, add water phase surfactant mixture, behind insulation 0.5～1h, be warming up to 85～95 ℃, single-dispersibility polystyrene-DVE is collected in insulation 0.75～1.0h slaking then from reaction product.
2. method according to claim 1 is characterized in that said tensio-active agent is selected from more than one in nonionic surface active agent, anion surfactant, cats product or the amphoterics.
3. method according to claim 1 is characterized in that, said nonionic surface active agent such as fiber are derivative or dehydration sorb sugar ester.
4. method according to claim 1 is characterized in that, said anion surfactant such as carboxylate salt, vitriol, sulfonate or phosphoric acid salt.
5. method according to claim 1 is characterized in that, said cats product such as quaternary amine.
6. method according to claim 1 is characterized in that, said amphoterics such as amino acid.
7. method according to claim 1 is characterized in that, the weight concentration of water phase surfactant mixture is 0.005%～0.1%, and the weight concentration of polyvinyl alcohol water solution is 0.05～1.0%.
8. according to each described method of claim 1～7, it is characterized in that in the reaction system, the parts by weight of each component are:
40～100 parts of vinylbenzene (St)
0～20 part of divinylbenzene (DVB)
0.1～0.8 part of benzoyl peroxide (BPO)
0.05～1.0 part of polyvinyl alcohol water solution
0.005～0.1 part of water phase surfactant mixture.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102641752A (en) * | 2012-04-28 | 2012-08-22 | 宁波争光树脂有限公司 | Solvent-less cation resin preparation process |
| CN105254790A (en) * | 2015-11-11 | 2016-01-20 | 青岛埃仑色谱科技有限公司 | Preparing method for ion exchange resin, negative ion chromatographic column prepared from ion exchange resin prepared through method and application of negative ion chromatographic column |
| CN106478856A (en) * | 2016-10-14 | 2017-03-08 | 北京海岸鸿蒙标准物质技术有限责任公司 | For calibrating standard substance and its preparation and the valued methods of PM10 sickle |
| CN106554451A (en) * | 2016-06-29 | 2017-04-05 | 宁夏海诚电化信息科技有限公司 | A kind of Archon production technology |
| CN108558660A (en) * | 2018-04-13 | 2018-09-21 | 怀化学院 | A kind of method of rare earth modified catalyzing cation exchange resin synthetic benzyl acetate |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1032017A (en) * | 1988-10-27 | 1989-03-29 | 成都科技大学 | The method of making large-pore white balls used for synthesizing ion-exchange resins |
| CN1431233A (en) * | 2002-09-02 | 2003-07-23 | 杭州余杭亚太化工有限公司 | Method for preparing cinnamene copolymerization homogeneous resin and its preparing method |
-
2007
- 2007-11-27 CN CN2007101710845A patent/CN101445573B/en active Active
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102641752A (en) * | 2012-04-28 | 2012-08-22 | 宁波争光树脂有限公司 | Solvent-less cation resin preparation process |
| CN102641752B (en) * | 2012-04-28 | 2014-09-10 | 宁波争光树脂有限公司 | Solvent-less cation resin preparation process |
| CN105254790A (en) * | 2015-11-11 | 2016-01-20 | 青岛埃仑色谱科技有限公司 | Preparing method for ion exchange resin, negative ion chromatographic column prepared from ion exchange resin prepared through method and application of negative ion chromatographic column |
| CN105254790B (en) * | 2015-11-11 | 2018-08-14 | 青岛埃仑色谱科技有限公司 | The preparation method of ion exchange resin, anion chromatographic column and its application made of the ion exchange resin of this method preparation |
| CN106554451A (en) * | 2016-06-29 | 2017-04-05 | 宁夏海诚电化信息科技有限公司 | A kind of Archon production technology |
| CN106478856A (en) * | 2016-10-14 | 2017-03-08 | 北京海岸鸿蒙标准物质技术有限责任公司 | For calibrating standard substance and its preparation and the valued methods of PM10 sickle |
| CN108558660A (en) * | 2018-04-13 | 2018-09-21 | 怀化学院 | A kind of method of rare earth modified catalyzing cation exchange resin synthetic benzyl acetate |
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Inventor after: Gu Shunchao Inventor after: Zhu Aiqin Inventor after: Zhou Jinxin Inventor after: Chen You Inventor before: Gu Shunchao Inventor before: Zhou Jinxin Inventor before: Chen You |
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