CN1003517B - Synthesis of marcopore double functional group anion exchange resin - Google Patents
Synthesis of marcopore double functional group anion exchange resin Download PDFInfo
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- CN1003517B CN1003517B CN86108388.1A CN86108388A CN1003517B CN 1003517 B CN1003517 B CN 1003517B CN 86108388 A CN86108388 A CN 86108388A CN 1003517 B CN1003517 B CN 1003517B
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- resin
- functional group
- anion exchange
- exchange resin
- double functional
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Abstract
The present invention relates to a synthesizing method of macropore double functional group anion exchange resin, which uses industrial isooctane as the pore-forming agent of the copolymerization reaction of phenylethylene-divinylbenzene and mixed amine composed of dimethylamine and trimethylamine as an aminating agent. The quantity of the dimethylamine in the mixed amine is controlled, and the macropore double functional group anion exchange resin comprising different strong alkali bases and weak alkali bases can be prepared. The macropore double functional group anion exchange resin can be used for extracting gold and silver from different materials, and the total exchange capacity of the resin can reach 4.0 milligram equivalents/gram of dry resin. The absorption capacity of the gold of the resin can reach 30 milligrams/gram of dry resin, the absorption capacity of the silver of the resin can reach 10 milligrams/gram of dry resin, and the mechanical strength of the resin is larger than 99%.
Description
The present invention relates to a kind of synthetic method of macromolecular compound, particularly a kind of anionite-exchange resin of macroporous network structure synthetic.
People once extracted gold with strongly basic anion exchange resin and weak base anion-exchange resin from the prussiate medium.The strongly basic anion exchange resin rate of adsorption is fast, but poor selectivity, desorb is difficulty relatively; Weak base anion-exchange resin has selectivity preferably to gold, and easily drip washing, but loading capacity is low, pH greater than 10 prussiate medium in chemical stability poor.For this reason, russian patent 394391 has disclosed a kind of synthetic method of marcopore double functional group anion exchange resin, and synthetic has the marcopore double functional group anion exchange resin of strong-base group and weak base base, has taken into account above-mentioned both advantages.The synthetic method of this kind resin is to be the pore-creating agent of vinylbenzene-divinylbenzene copolymerization with solvent oil-BP-2, makes macropore copolymerization pearl body, and through chloromethylation, amination forms marcopore double functional group anion exchange resin.Used aminating agent is the dimethylamine methanol solution during amination.Yet, according to russian patent 394391 synthetic resins, physical strength only 90%, total exchange capacity is 3.12 milligramequivalents/gram dried resin.
Task of the present invention is that will to synthesize a kind of physical strength good, total high marcopore double functional group anion exchange resin of exchange capacity, and it can be used for extracting Jin Heyin from the prussiate medium.
Task of the present invention is done in such a way that in the presence of the pore-creating agent octane-iso, carries out vinylbenzene-divinylbenzene suspension copolymerization, generate macropore copolymerization pearl body, carry out chloromethylation then, use the mixed amine amination again, make marcopore double functional group anion exchange resin.
Vinylbenzene-divinylbenzene suspension copolymerization is fashionable, select for use technical octane cheap and easy to get as pore-creating agent, its consumption is 40～100% of a total monomer weight, under the initiation of benzoyl peroxide, reacted 10～15 hours down in 75～85 ℃, make the macropore copolymerization pearl body of White-opalescent.The pearl body that obtains thus, even pore distribution, the aperture is suitable, and the pore distribution of pearl body more than 90% is 100～300
Between, the dynamic performance of resin at this moment, antioxidant property and physical strength all have satisfactory result.In the presence of the catalyzer Zinc Chloride Anhydrous, macropore vinylbenzene-divinylbenzene copolymerization pearl body is carried out chloromethylation with chloromethyl ether.For shortening the time of chloromethylation, effectively crosslinked pair of reaction of adjacent chloromethyl in the inhibited reaction process, improve the cl content of chloromethylation copolymerization pearl body, the Controllable Temperature of chloromethylation is built in 44～55 ℃, reacts thus that cl content is not less than 15% in the macropore chlorine ball that obtains after 15～20 hours.
In above-mentioned macropore chlorine ball after benzene expands, add the mixed amine amination, reacted 15～25 hours down at 15～28 ℃.Product after transition, promptly gets marcopore double functional group anion exchange resin through hydrochloric acid.Mixed amine is meant dimethylamine and Trimethylamine 99, controls the add-on of dimethylamine in the mixed amine, can obtain the marcopore double functional group anion exchange resin of different strong-base groups and weak base base ratio.For being suitable for extracting Jin Heyin from various materials, the add-on of mixed amine is 0.2～2.0 times of vinylbenzene-divinylbenzene copolymerization pearl body weight.Wherein the dimethylamine add-on is 20～90% of a mixed amine gross weight.
According to institute of the present invention synthetic marcopore double functional group anion exchange resin, be suitable for from various materials, extracting Jin Heyin.Loading capacity to gold can reach 30 milligrams/gram dried resin, can reach 10 milligrams/gram dried resin to silver-colored loading capacity.The salient features of resin: total exchange capacity 4.0 milligramequivalent/grams are done; Specific surface is 40～60 a meters/gram; Moisture content 52～58%, physical strength is more than or equal to 99%, 0.6～1.2 millimeter of particle diameter.And press russian patent 394391 synthetic resin salient featuress: total exchange capacity 3.1 milligramequivalent/grams are done, and specific surface is 32 a meters/gram, moisture content 52～58%, and physical strength is 90%, particle diameter is 0.6～1.2 millimeter.
Because the present invention uses technical octane cheap and easy to get as pore-creating agent, the resin cost is comparatively cheap.
Be embodiments of the invention below.
Example one:
Add technical gelatine 8 grams in filling 2000 milliliters of there-necked flasks of 800 ml distilled waters, stirring and dissolving gelatin under 45 ℃ of conditions adds an amount of 0.1% the blue aqueous solution of methyne then.Make it to mix.Water is stand-by.
Take by weighing technical benzene ethene 165.2 grams of removing stopper in the beaker of cleaning, divinylbenzene 34.8 grams add chemical pure benzoyl peroxide 2 grams again, stir and make the benzoyl peroxide dissolving.Add technical octane 160 grams at last, join above-mentioned aqueous phase after stirring and go.Be warming up to 80 ℃, under agitation reacted 10 hours.After reaction finishes, filter, obtain macropore copolymerization pearl body with B.Wash pearl body and oven dry again with water, its polymeric beads body of 0.5～1.0 millimeter particle diameter of screening.
Get above-mentioned pearl body 100 grams, add thermometer is housed, in 1000 milliliters of there-necked flasks of refrigerating unit and whipping appts, add 450 milliliters of chloromethyl ethers then, under room temperature, expanded 4 hours, start whipping appts again, add Zinc Chloride Anhydrous 60 grams, be warming up to 54 ℃ and under this temperature, reacted 6 hours, cooling, filter with B, with the methyl alcohol * that gives a baby a bath on the third day after its birth, water is taken out pump and is drained in B then.
Use in the benzene expansible chlorine ball above-mentioned, add mixed amine 〈 ﹠﹠ while stirring 0 gram, wherein dimethylamine accounts for 90% of mixed amine gross weight.Be warming up to 28 ℃ then, reaction is 15 hours under this temperature, and after reaction finished, dilute with water washed with water again, is washed till effluent liquid neutrality, made the transition 12 hours with 2.5% hydrochloric acid again, washed with water to neutrality at last.The moisture preservation of resin.Gained resin strong-base group content accounts for 6% of total exchange capacity, and specific surface is 60 a meters/gram.
Example two adds mixed amine 100 grams, and wherein dimethylamine is 40% of a mixed amine gross weight, and other step is with example one, and strong-base group content accounts for 40% of total exchange capacity in the gained resin, and specific surface is 51 a meters/gram.
Example three adds 100 gram technical octanes, and other step is with example one, and to account for 6% specific surface of total exchange capacity be 43 meters/gram to strong-base group content in the gained resin.
Claims (2)
1, a kind of synthetic method of marcopore double functional group anion exchange resin, be in the presence of pore-creating agent, by the synthetic macropore pearl body of vinylbenzene-divinylbenzene suspension copolymerization, pass through chloromethylation and amination again, feature of the present invention is that the mixed amine of forming with dimethylamine and Trimethylamine 99 in the amination process is an aminating agent, and the add-on of technical octane is the 40-100% of total monomer weight.
2, as the said resin synthetic method of claim 1, the add-on that it is characterized in that mixed amine is 0.5-2.0 a times of vinylbenzene-divinylbenzene copolymerization pearl body weight, and wherein the add-on of dimethylamine is 20～90% of a mixed amine gross weight.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN86108388.1A CN1003517B (en) | 1986-12-13 | 1986-12-13 | Synthesis of marcopore double functional group anion exchange resin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN86108388.1A CN1003517B (en) | 1986-12-13 | 1986-12-13 | Synthesis of marcopore double functional group anion exchange resin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN86108388A CN86108388A (en) | 1988-07-06 |
| CN1003517B true CN1003517B (en) | 1989-03-08 |
Family
ID=4803910
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN86108388.1A Expired CN1003517B (en) | 1986-12-13 | 1986-12-13 | Synthesis of marcopore double functional group anion exchange resin |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1003517B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102463155B (en) * | 2010-11-17 | 2013-08-14 | 核工业北京化工冶金研究院 | Method for preparing macroporous alkalescent anion exchange resin |
| CN103537325A (en) * | 2013-10-21 | 2014-01-29 | 东南大学 | Preparation method of difunctional group weak-base anion exchange resin |
| FI125833B (en) * | 2014-06-05 | 2016-03-15 | Outotec Finland Oy | Silver recovery by ion exchange |
| CN108084302A (en) * | 2016-11-22 | 2018-05-29 | 中国科学院大连化学物理研究所 | A kind of preparation method of alkalescence anion-exchange resin |
-
1986
- 1986-12-13 CN CN86108388.1A patent/CN1003517B/en not_active Expired
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| Publication number | Publication date |
|---|---|
| CN86108388A (en) | 1988-07-06 |
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