CN106749883A - A kind of chelating resin and preparation method thereof - Google Patents
A kind of chelating resin and preparation method thereof Download PDFInfo
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- CN106749883A CN106749883A CN201611045862.1A CN201611045862A CN106749883A CN 106749883 A CN106749883 A CN 106749883A CN 201611045862 A CN201611045862 A CN 201611045862A CN 106749883 A CN106749883 A CN 106749883A
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/42—Nitriles
- C08F220/44—Acrylonitrile
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/20—Aqueous medium with the aid of macromolecular dispersing agents
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F212/34—Monomers containing two or more unsaturated aliphatic radicals
- C08F212/36—Divinylbenzene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/30—Introducing nitrogen atoms or nitrogen-containing groups
- C08F8/32—Introducing nitrogen atoms or nitrogen-containing groups by reaction with amines
Abstract
The present invention relates to a kind of chelating resin and preparation method thereof.Resin of the invention includes：Oil phase：5 10 parts of hydroxy-ethyl acrylate, 5 10 parts of Glycidyl Acrylate, 30 40 parts of acrylonitrile, 30 35 parts of divinylbenzene, 50 80 parts of dimethylbenzene, 30 40 parts of isoamyl alcohol, 20 30 parts of isooctanol, 35 parts of azodiisobutyronitrile；Water phase：10% 35 parts of polyvinyl alcohol aqueous, 35 parts of gelatin, 10 20 parts of sodium chloride, 10 15 parts of calcium carbonate, 35 parts of 0.1% methylene blue aqueous, 1,500 2000 parts of deionized water.Physical and chemical performance, molecular characterization of the present invention according to uranium atom, by adding Third monomer and the 4th monomer, and hydrophilic, oleophylic mixing pore-foaming agent system is employed, under conditions of the suitable degree of cross linking is selected, divinylbenzene acrylonitrile is prepared with suspension copolymerization technique first（DVB‑AN）Resin matrix, then carries out oximation reaction again, is finally prepared for the combination property preferably chelate resin of functional group containing amidoxime.
Description
Technical field
The present invention relates to a kind of resin and preparation method thereof, it is more particularly related to a kind of chelating resin and its
Preparation method.
Background technology
In nuclear fuel pretreatment process, contained humidity, the earth's surface of person who lives in exile around dam in the neutralization slag that uranium hydrometallurgy is produced
Water and rainwater, generate tailing dam drainage problem, and the uranium of remaining forms uranium-containing waste water in slag, causes environmental pollution.It is another
Aspect, the uranium that uranium hydrometallurgy is lost in slag is also the waste very important to uranium mine resource.Therefore, uranium mill tailing dam
Wastewater treatment and trace uranium reclaim significant to control environmental pollution, saving uranium mine resource, reduction uranium hydrometallurgy cost.
Wherein, most basic is to develop and develop adsorption technology and the uranium absorption agent suitable for Waste Water of Tailings Dam treatment.Function containing amidoxime
The resin of group is considered as most rising uranium selective absorbent.Its selection performance to uranium uranium high and high holds
Amount；With excellent dynamic performance；Physics, chemistry and high to biodegradable stability, can be recycled for a long time；Can be big
Large-scale production, it is cheap.
In the prior art without the resin of combination property preferably amidoxime functional group.
The content of the invention
Present invention seek to address that the problems of the prior art, there is provided a kind of chelating resin, the resin combination property is preferable.
In order to realize foregoing invention purpose, its specific technical scheme is as follows：
A kind of chelating resin, it is characterised in that：Including following raw materials by weight：
Oil phase：
Hydroxy-ethyl acrylate 5-10 parts
Glycidyl Acrylate 5-10 parts
Acrylonitrile 30-40 parts
Divinylbenzene 30-35 parts
Dimethylbenzene 50-80 parts
Isoamyl alcohol 30-40 parts
Isooctanol 20-30 parts
3-5 parts of azodiisobutyronitrile (AIBN)；
Water phase：
10% polyvinyl alcohol（PVA1788）Aqueous 3-5 parts
Gelatin 3-5 parts
Sodium chloride 10-20 parts
Calcium carbonate 10-15 parts
0.1% 3-5 parts of methylene blue aqueous
Deionized water 1500-2000 parts.
A kind of preparation method of chelating resin, it is characterised in that：Comprise the following steps that：
A, hydroxy-ethyl acrylate, Glycidyl Acrylate, acrylonitrile, divinylbenzene, diformazan are accurately weighed according to recipe requirements
Benzene, isoamyl alcohol, isooctanol, azodiisobutyronitrile (AIBN) are sufficiently mixed uniformly in container, standby；
B, according to water phase recipe requirements, each component is added into the 5000ml there-necked flasks for having electric stirring, condenser pipe and charge door
It is interior；
C, system temperature is risen to 30-40 DEG C, start stirring until water phase each component is sufficiently mixed dissolving；The oil phase that will be prepared
Mixture is poured into there-necked flask；Keep the speed stirred in suitable reactor, make oil phase formed uniform bead be dispersed in it is pre-
In the water phase for first preparing；Adjustment mixing speed is so that dispersion oil phase bead meets technique Particle size requirements；
D, in water phase temperature is risen into 60-65 DEG C in 0.5h, keep the reaction temperature until scattered oil droplet meet the requirements；Will be poly-
Close temperature of reaction system and be raised to 72-75 DEG C, until oil phase bead does not break sizing；Polymerization reaction system temperature is raised to 80-85 DEG C,
2-3 hour of insulation；Polymerization reaction system is warming up to 85-90 DEG C, 2-3 hour is incubated；Polymerization reaction system is warming up to
95 DEG C, it is incubated 2-3 hour；
E, reaction system is cooled to room temperature, leaches resin bead；Drip washing is carried out to resin using ethanol, the cause in resin is removed
Hole agent dimethylbenzene etc. and other impurity, vacuum drying obtain product.
The Advantageous Effects that the present invention brings：
Physical and chemical performance, molecular characterization of the present invention according to uranium atom, by adding Third monomer and the 4th monomer, and adopt
With hydrophilic, oleophylic mixing pore-foaming agent system, under conditions of the suitable degree of cross linking is selected, prepared with suspension copolymerization technique first
Go out divinylbenzene-acrylonitrile（DVB-AN）Resin matrix, then carries out oximation reaction again, is finally prepared for combination property preferable
The chelate resin of functional group containing amidoxime.
Specific embodiment
Embodiment 1
A kind of chelating resin, including following raw materials by weight：
Oil phase：
5 parts of hydroxy-ethyl acrylate
5 parts of Glycidyl Acrylate
30 parts of acrylonitrile
30 parts of divinylbenzene
50 parts of dimethylbenzene
30 parts of isoamyl alcohol
20 parts of isooctanol
3 parts of azodiisobutyronitrile；
Water phase：
10% 3 parts of polyvinyl alcohol aqueous
3 parts of gelatin
10 parts of sodium chloride
10 parts of calcium carbonate
0.1% 3 parts of methylene blue aqueous
1500 parts of deionized water.
Embodiment 2
A kind of chelating resin, including following raw materials by weight：
Oil phase：
10 parts of hydroxy-ethyl acrylate
10 parts of Glycidyl Acrylate
40 parts of acrylonitrile
35 parts of divinylbenzene
80 parts of dimethylbenzene
40 parts of isoamyl alcohol
30 parts of isooctanol
5 parts of azodiisobutyronitrile；
Water phase：
10% 5 parts of polyvinyl alcohol aqueous
5 parts of gelatin
20 parts of sodium chloride
15 parts of calcium carbonate
0.1% 5 parts of methylene blue aqueous
2000 parts of deionized water.
Embodiment 3
A kind of chelating resin, including following raw materials by weight：
Oil phase：
7 parts of hydroxy-ethyl acrylate
7 parts of Glycidyl Acrylate
35 parts of acrylonitrile
32 parts of divinylbenzene
60 parts of dimethylbenzene
35 parts of isoamyl alcohol
25 parts of isooctanol
4 parts of azodiisobutyronitrile；
Water phase：
10% 4 parts of polyvinyl alcohol aqueous
4 parts of gelatin
15 parts of sodium chloride
12 parts of calcium carbonate
0.1% 4 parts of methylene blue aqueous
1700 parts of deionized water.
Embodiment 4
A kind of preparation method of chelating resin, comprises the following steps that：
A, hydroxy-ethyl acrylate, Glycidyl Acrylate, acrylonitrile, divinylbenzene, diformazan are accurately weighed according to recipe requirements
Benzene, isoamyl alcohol, isooctanol, azodiisobutyronitrile are sufficiently mixed uniformly in container, standby；
B, according to water phase recipe requirements, each component is added into the 5000ml there-necked flasks for having electric stirring, condenser pipe and charge door
It is interior；
C, system temperature is risen to 30 DEG C, start stirring until water phase each component is sufficiently mixed dissolving；The oil phase that will be prepared is mixed
Compound is poured into there-necked flask；The speed stirred in the suitable reactor of holding, makes oil phase form uniform bead and is dispersed in advance
In the water phase for preparing；Adjustment mixing speed is so that dispersion oil phase bead meets technique Particle size requirements；
D, in water phase temperature is risen into 60 DEG C in 0.5h, keep the reaction temperature until scattered oil droplet meet the requirements；Will polymerization
Temperature of reaction system is raised to 72 DEG C, until oil phase bead does not break sizing；Polymerization reaction system temperature is raised to 80 DEG C, 2 are incubated
Hour；Polymerization reaction system is warming up to 85 DEG C, 2 hours are incubated；Polymerization reaction system is warming up to 95 DEG C, insulation 2 is small
When；
E, reaction system is cooled to room temperature, leaches resin bead；Drip washing is carried out to resin using ethanol, the cause in resin is removed
Hole agent dimethylbenzene etc. and other impurity, vacuum drying obtain product.
Embodiment 5
A kind of preparation method of chelating resin, comprises the following steps that：
A, hydroxy-ethyl acrylate, Glycidyl Acrylate, acrylonitrile, divinylbenzene, diformazan are accurately weighed according to recipe requirements
Benzene, isoamyl alcohol, isooctanol, azodiisobutyronitrile are sufficiently mixed uniformly in container, standby；
B, according to water phase recipe requirements, each component is added into the 5000ml there-necked flasks for having electric stirring, condenser pipe and charge door
It is interior；
C, system temperature is risen to 40 DEG C, start stirring until water phase each component is sufficiently mixed dissolving；The oil phase that will be prepared is mixed
Compound is poured into there-necked flask；The speed stirred in the suitable reactor of holding, makes oil phase form uniform bead and is dispersed in advance
In the water phase for preparing；Adjustment mixing speed is so that dispersion oil phase bead meets technique Particle size requirements；
D, in water phase temperature is risen into 65 DEG C in 0.5h, keep the reaction temperature until scattered oil droplet meet the requirements；Will polymerization
Temperature of reaction system is raised to 75 DEG C, until oil phase bead does not break sizing；Polymerization reaction system temperature is raised to 85 DEG C, 3 are incubated
Hour；Polymerization reaction system is warming up to 90 DEG C, 3 hours are incubated；Polymerization reaction system is warming up to 95 DEG C, insulation 3 is small
When；
E, reaction system is cooled to room temperature, leaches resin bead；Drip washing is carried out to resin using ethanol, the cause in resin is removed
Hole agent dimethylbenzene etc. and other impurity, vacuum drying obtain product.
Embodiment 6
A kind of preparation method of chelating resin, comprises the following steps that：
A, hydroxy-ethyl acrylate, Glycidyl Acrylate, acrylonitrile, divinylbenzene, diformazan are accurately weighed according to recipe requirements
Benzene, isoamyl alcohol, isooctanol, azodiisobutyronitrile are sufficiently mixed uniformly in container, standby；
B, according to water phase recipe requirements, each component is added into the 5000ml there-necked flasks for having electric stirring, condenser pipe and charge door
It is interior；
C, system temperature is risen to 35 DEG C, start stirring until water phase each component is sufficiently mixed dissolving；The oil phase that will be prepared is mixed
Compound is poured into there-necked flask；The speed stirred in the suitable reactor of holding, makes oil phase form uniform bead and is dispersed in advance
In the water phase for preparing；Adjustment mixing speed is so that dispersion oil phase bead meets technique Particle size requirements；
D, in water phase temperature is risen into 62 DEG C in 0.5h, keep the reaction temperature until scattered oil droplet meet the requirements；Will polymerization
Temperature of reaction system is raised to 73 DEG C, until oil phase bead does not break sizing；Polymerization reaction system temperature is raised to 83 DEG C, insulation 2.5
Individual hour；Polymerization reaction system is warming up to 87 DEG C, 2.5 hours are incubated；Polymerization reaction system is warming up to 95 DEG C, insulation
2.5 hours；
E, reaction system is cooled to room temperature, leaches resin bead；Drip washing is carried out to resin using ethanol, the cause in resin is removed
Hole agent dimethylbenzene etc. and other impurity, vacuum drying obtain product.
Claims (2)
1. a kind of chelating resin, it is characterised in that：Including following raw materials by weight：
Oil phase：
Hydroxy-ethyl acrylate 5-10 parts
Glycidyl Acrylate 5-10 parts
Acrylonitrile 30-40 parts
Divinylbenzene 30-35 parts
Dimethylbenzene 50-80 parts
Isoamyl alcohol 30-40 parts
Isooctanol 20-30 parts
Azodiisobutyronitrile 3-5 parts；
Water phase：
10% 3-5 parts of polyvinyl alcohol aqueous
Gelatin 3-5 parts
Sodium chloride 10-20 parts
Calcium carbonate 10-15 parts
0.1% 3-5 parts of methylene blue aqueous
Deionized water 1500-2000 parts.
2. the preparation method of a kind of chelating resin according to claim 1, it is characterised in that：Comprise the following steps that：
A, hydroxy-ethyl acrylate, Glycidyl Acrylate, acrylonitrile, divinylbenzene, diformazan are accurately weighed according to recipe requirements
Benzene, isoamyl alcohol, isooctanol, azodiisobutyronitrile are sufficiently mixed uniformly in container, standby；
B, according to water phase recipe requirements, each component is added into the 5000ml there-necked flasks for having electric stirring, condenser pipe and charge door
It is interior；
C, system temperature is risen to 30-40 DEG C, start stirring until water phase each component is sufficiently mixed dissolving；The oil phase that will be prepared
Mixture is poured into there-necked flask；Keep the speed stirred in suitable reactor, make oil phase formed uniform bead be dispersed in it is pre-
In the water phase for first preparing；Adjustment mixing speed is so that dispersion oil phase bead meets technique Particle size requirements；
D, in water phase temperature is risen into 60-65 DEG C in 0.5h, keep the reaction temperature until scattered oil droplet meet the requirements；Will be poly-
Close temperature of reaction system and be raised to 72-75 DEG C, until oil phase bead does not break sizing；Polymerization reaction system temperature is raised to 80-85 DEG C,
2-3 hour of insulation；Polymerization reaction system is warming up to 85-90 DEG C, 2-3 hour is incubated；Polymerization reaction system is warming up to
95 DEG C, it is incubated 2-3 hour；
E, reaction system is cooled to room temperature, leaches resin bead；Drip washing is carried out to resin using ethanol, the cause in resin is removed
Hole agent dimethylbenzene etc. and other impurity, vacuum drying obtain product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611045862.1A CN106749883A (en) | 2016-11-25 | 2016-11-25 | A kind of chelating resin and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611045862.1A CN106749883A (en) | 2016-11-25 | 2016-11-25 | A kind of chelating resin and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106749883A true CN106749883A (en) | 2017-05-31 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611045862.1A Pending CN106749883A (en) | 2016-11-25 | 2016-11-25 | A kind of chelating resin and preparation method thereof |
Country Status (1)
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| CN (1) | CN106749883A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2741909C1 (en) * | 2020-08-28 | 2021-01-29 | Федеральное государственное бюджетное учреждение науки Институт химии Дальневосточного отделения Российской академии наук (ИХ ДВО РАН) | Selenium-derivative of n-hydroxyamidine aminofurazan for extraction of uranium from liquid media |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59155406A (en) * | 1983-02-22 | 1984-09-04 | Sumitomo Chem Co Ltd | Production of chelate resin |
| JPS6088041A (en) * | 1983-10-21 | 1985-05-17 | Mitsubishi Chem Ind Ltd | Chelating resin |
| CN102114413A (en) * | 2011-01-20 | 2011-07-06 | 福州大学 | Macroporous spherical polyacrylonitrile chelatesorbent and microwave radiating preparation process thereof |
| CN104292383A (en) * | 2014-09-16 | 2015-01-21 | 陕西华电树脂股份有限公司 | Gallium-adsorbing chelating resin and preparation method thereof |
| CN105131168A (en) * | 2015-10-23 | 2015-12-09 | 蓝星（成都）新材料有限公司 | Macropore hydroxyethyl methylacrylate resin and preparing method thereof |
-
2016
- 2016-11-25 CN CN201611045862.1A patent/CN106749883A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59155406A (en) * | 1983-02-22 | 1984-09-04 | Sumitomo Chem Co Ltd | Production of chelate resin |
| JPS6088041A (en) * | 1983-10-21 | 1985-05-17 | Mitsubishi Chem Ind Ltd | Chelating resin |
| CN102114413A (en) * | 2011-01-20 | 2011-07-06 | 福州大学 | Macroporous spherical polyacrylonitrile chelatesorbent and microwave radiating preparation process thereof |
| CN104292383A (en) * | 2014-09-16 | 2015-01-21 | 陕西华电树脂股份有限公司 | Gallium-adsorbing chelating resin and preparation method thereof |
| CN105131168A (en) * | 2015-10-23 | 2015-12-09 | 蓝星（成都）新材料有限公司 | Macropore hydroxyethyl methylacrylate resin and preparing method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 郎哲思等: "吸附铀的丙烯腈骨架螯合树脂的研制", 《湿法冶金》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2741909C1 (en) * | 2020-08-28 | 2021-01-29 | Федеральное государственное бюджетное учреждение науки Институт химии Дальневосточного отделения Российской академии наук (ИХ ДВО РАН) | Selenium-derivative of n-hydroxyamidine aminofurazan for extraction of uranium from liquid media |
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Application publication date: 20170531 |