CN103183755A - Method for preparing macroporous weak-base anion resin - Google Patents
Method for preparing macroporous weak-base anion resin Download PDFInfo
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- CN103183755A CN103183755A CN201310078880XA CN201310078880A CN103183755A CN 103183755 A CN103183755 A CN 103183755A CN 201310078880X A CN201310078880X A CN 201310078880XA CN 201310078880 A CN201310078880 A CN 201310078880A CN 103183755 A CN103183755 A CN 103183755A
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Abstract
The invention discloses a method for preparing macroporous weak-base anion resin, and belongs to the field of high polymer chemistry. The method comprises the following steps: polymerization reaction phase, namely obtaining polystyrene-DVE by material preparation, stirring, warming and reacting; chlorination reaction phase, namely placing the polystyrene-DVE ball into a reaction kettle, and obtaining a chloromethylated bead by adding ether chloride, zinc chloride and the other reactions; and amination reaction phase, namely performing amination reaction on the chloromethylated bead and dimethylamine water to obtain the macroporous weak base anion resin. According to the macroporous weak base anion resin prepared by the invention, the mechanical strength of the resin is enhanced, and the service life of the resin is prolonged; as the specific surface area is larger, and the aperture is more uniform, the exchange capacity and the pollution-resistant capability of the resin is improved; and accordingly, the manufacturing cost is decreased, and the economic benefit of the product is improved.
Description
Technical field
The present invention relates to technical field of polymer chemistry, be specifically related to a kind of preparation method of macropore weak base anion resins.
Background technology
The macropore weak base anion resins is widely used in water softening, de-salted water, pure water preparation, and hydrometallurgy, rare elements separation, pharmacy, sugar industry, fields such as amino acid absorption.Widespread use D301 in the market.This product value-rising height, but it can produce a large amount of toxic gases in process of production, cause workman and the peripheral masses carcinogenic and unhealthful easily, so, many enterprises can't ordinary production or hide and produce in frequent replacing workman's mode in the mountain area, have therefore influenced production and the application of macropore weak base anion resins greatly.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of preparation method of macropore weak base anion resins, has not only improved the intensity of product, and make the specific surface area of resin bigger, the aperture is even, improves exchange capacity and the contamination resistance of resin.
Technical problem to be solved by this invention realizes by the following technical solutions:
A kind of preparation method of macropore weak base anion resins is characterized in that: its preparation method comprises the steps:
Step 1: polyreaction: a. at first will prepare benzene feedstock ethene, TXB, initiator and pore-creating agent and put into the still of getting the raw materials ready to stir 30min standby; Dispersion agent and water are dropped in the reactor, temperature is risen to 50 ℃, and stirred 1 hour;
B. the raw material that stirred in the still of will getting the raw materials ready joins in the reactor, and temperature is warming up to 80 ℃, and insulation 2 as a child rose to temperature between 85 ℃-95 ℃ again, and was incubated four hours; Again temperature is risen to more than 95 ℃, be incubated cooling after 6 hours, cool the temperature to below 45 ℃, obtain Archon;
C. the Archon in the reactor is put into to wash in the material still and cleans, limpid up to water outlet;
D. will wash good Archon and send into oven dry in the drying machine, filter out the qualified Archon of granularity after the oven dry;
Step 2: chlorination reaction: qualified Archon and chlorinated ether are put into the chlorination reaction still carry out chlorination reaction, temperature is controlled at 30 ℃, and the time is 2 hours; 2 as a child added zinc chloride in the chlorination reaction still, temperature is warming up between 45 ℃-48 ℃, reacted to cool the temperature to below 30 ℃ after 15 hours to obtain the chlorine ball;
Step 3: amination reaction: dimethylamine water is splashed in the chlorine ball fast, stablize and begin behind the 30min to stir, after stirring temperature is risen to 43 ℃, be incubated sampling survey moisture after 8 hours, water content can obtain the macropore weak base anion resins greater than 53%.
Described chlorethyl ether is to be mixed with chlorination mother solution by methylal, adds chlorsulfonic acid and formaldehyde reaction and generates.
Described initiator, pore-creating agent and dispersion agent are respectively isopropylcarbinol, TXA and polyvinyl alcohol.
The invention has the beneficial effects as follows:
1, adopts novel material TXB to replace divinylbenzene of the prior art, improved the physical strength of resin greatly, prolonged the work-ing life of resin;
2, adopting novel material TXA is pore-creating agent, makes that the resin specific surface area is bigger, the aperture is even, improves the exchange capacity of resin, and contamination resistance strengthens;
3, reduce production cost, improved the economic benefit of product.
Embodiment
For technique means, creation characteristic that the present invention is realized, reach purpose and effect is easy to understand, further set forth the present invention.
Embodiment one
A kind of preparation method of macropore weak base anion resins is characterized in that: its preparation method comprises the steps:
Step 1: polyreaction: a. at first will prepare benzene feedstock ethene, TXB, initiator isopropylcarbinol and pore-creating agent TXA and put into the still of getting the raw materials ready to stir 30min standby; The polyethylene of dispersing agent alcohol and water is dropped in the reactor, temperature is risen to 50 ℃, and stirred 1 hour;
B. the raw material that stirred in the still of will getting the raw materials ready joins in the reactor, and temperature is warming up to 80 ℃, and insulation 2 as a child rises to temperature 90 ℃ again, and is incubated four hours; Temperature is risen to 98 ℃ again, be incubated cooling after 6 hours, cool the temperature to 40 ℃, obtain Archon;
C. the Archon in the reactor is put into to wash in the material still and cleans, limpid up to water outlet;
D. will wash good Archon and send into oven dry in the drying machine, filter out the qualified Archon of granularity after the oven dry;
Step 2: chlorination reaction: qualified Archon and chlorinated ether are put into the chlorination reaction still carry out chlorination reaction, temperature is controlled at 30 ℃, and the time is 2 hours; 2 as a child added zinc chloride in the chlorination reaction still, temperature is warming up to 46 ℃, reacted to cool the temperature to 25 ℃ after 15 hours and can obtain the chlorine ball;
Step 3: amination reaction: dimethylamine water is splashed in the chlorine ball fast, stablize and begin behind the 30min to stir, after stirring temperature is risen to 43 ℃, be incubated sampling survey moisture after 8 hours, water content can obtain the macropore weak base anion resins greater than 53%.
Described chlorethyl ether is to be mixed with chlorination mother solution by methylal, adds chlorsulfonic acid and formaldehyde reaction and generates.
More than show and described ultimate principle of the present invention and principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; that describes in above-described embodiment and the specification sheets just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.The claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (3)
1. the preparation method of a macropore weak base anion resins, it is characterized in that: its preparation method comprises the steps:
Step 1: polyreaction: a. at first will prepare benzene feedstock ethene, TXB, initiator and pore-creating agent and put into the still of getting the raw materials ready to stir 30min standby; Dispersion agent and water are dropped in the reactor, temperature is risen to 50 ℃, and stirred 1 hour;
B. the raw material that stirred in the still of will getting the raw materials ready joins in the reactor, and temperature is warming up to 80 ℃, and insulation 2 as a child rose to temperature between 85 ℃-95 ℃ again, and was incubated four hours; Again temperature is risen to more than 95 ℃, be incubated cooling after 6 hours, cool the temperature to below 45 ℃, obtain Archon;
C. the Archon in the reactor is put into to wash in the material still and cleans, limpid up to water outlet;
D. will wash good Archon and send into oven dry in the drying machine, filter out the qualified Archon of granularity after the oven dry;
Step 2: chlorination reaction: qualified Archon and chlorinated ether are put into the chlorination reaction still carry out chlorination reaction, temperature is controlled at 30 ℃, and the time is 2 hours; 2 as a child added zinc chloride in the chlorination reaction still, temperature is warming up between 45 ℃-48 ℃, reacted to cool the temperature to below 30 ℃ after 15 hours to obtain the chlorine ball;
Step 3: amination reaction: dimethylamine water is splashed in the chlorine ball fast, stablize and begin behind the 30min to stir, after stirring temperature is risen to 43 ℃, be incubated sampling survey moisture after 8 hours, water content can obtain the macropore weak base anion resins greater than 53%.
2. according to the preparation method of the described a kind of macropore weak base anion resins of claim 1, it is characterized in that: described chlorethyl ether is to be mixed with chlorination mother solution by methylal, adds chlorsulfonic acid and formaldehyde reaction and generates.
3. according to the preparation method of the described a kind of macropore weak base anion resins of claim 1, it is characterized in that: described initiator, pore-creating agent and dispersion agent are respectively isopropylcarbinol, TXA and polyvinyl alcohol.
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| CN201310078880XA CN103183755A (en) | 2013-03-12 | 2013-03-12 | Method for preparing macroporous weak-base anion resin |
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| CN201310078880XA CN103183755A (en) | 2013-03-12 | 2013-03-12 | Method for preparing macroporous weak-base anion resin |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103483474A (en) * | 2013-09-18 | 2014-01-01 | 蚌埠市天星树脂有限责任公司 | Preparation method for macroporous weak-base anion resin |
| CN106854683A (en) * | 2016-12-05 | 2017-06-16 | 浙江海洋大学 | A kind of cation saccharified liquid discoloration method |
| CN106866863A (en) * | 2015-12-11 | 2017-06-20 | 北京大学深圳研究生院 | A kind of preparation method of porous polymer microballoon anion filler |
Citations (3)
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| CN101703950A (en) * | 2009-11-16 | 2010-05-12 | 江苏苏青水处理工程集团有限公司 | Dedicated ion exchange resin for condensed water precision processing and preparation method thereof |
| CN101781379A (en) * | 2009-12-31 | 2010-07-21 | 安徽皖东化工有限公司 | Preparation method of D301 macroporous weekly acidic styrene type anion exchange resin |
| CN101954299A (en) * | 2009-07-15 | 2011-01-26 | 中国船舶重工集团公司第七一八研究所 | Method for preparing anion exchange resin |
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2013
- 2013-03-12 CN CN201310078880XA patent/CN103183755A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101954299A (en) * | 2009-07-15 | 2011-01-26 | 中国船舶重工集团公司第七一八研究所 | Method for preparing anion exchange resin |
| CN101703950A (en) * | 2009-11-16 | 2010-05-12 | 江苏苏青水处理工程集团有限公司 | Dedicated ion exchange resin for condensed water precision processing and preparation method thereof |
| CN101781379A (en) * | 2009-12-31 | 2010-07-21 | 安徽皖东化工有限公司 | Preparation method of D301 macroporous weekly acidic styrene type anion exchange resin |
Non-Patent Citations (1)
| Title |
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| 吴艳等: "强碱弱酸两性树脂的合成、结构性能及吸附性能", 《食品与生物技术》, vol. 21, no. 1, 31 January 2002 (2002-01-31), pages 24 - 26 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103483474A (en) * | 2013-09-18 | 2014-01-01 | 蚌埠市天星树脂有限责任公司 | Preparation method for macroporous weak-base anion resin |
| CN106866863A (en) * | 2015-12-11 | 2017-06-20 | 北京大学深圳研究生院 | A kind of preparation method of porous polymer microballoon anion filler |
| CN106854683A (en) * | 2016-12-05 | 2017-06-16 | 浙江海洋大学 | A kind of cation saccharified liquid discoloration method |
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Application publication date: 20130703 |