CN109851702A - A kind of preparation method of multifunctional exchange resin - Google Patents
A kind of preparation method of multifunctional exchange resin Download PDFInfo
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- CN109851702A CN109851702A CN201811616947.XA CN201811616947A CN109851702A CN 109851702 A CN109851702 A CN 109851702A CN 201811616947 A CN201811616947 A CN 201811616947A CN 109851702 A CN109851702 A CN 109851702A
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Abstract
A kind of preparation method of multifunctional exchange resin of the present invention belongs to high score field of material technology, multiple steps such as preparation, polystyrene chloromethylation, amination including compound resin microballoon, nano-inorganic substance and nanometer organic matter are introduced simultaneously, the ion exchange resin obtained from is the composition of multiple groups parting, different kinds of ions can be exchanged simultaneously, simple process, exchange capacity is big, it is good to exchange effect, especially suitable for handling containing phenol, halogen, sulfur-containing waste water processing.
Description
Technical field
A kind of preparation method of multifunctional exchange resin of the present invention can be used for what is involved is a kind of new type chemical material
The processing of boiler feed water, belongs to technical field of polymer materials.
Background technique
Ion exchange resin is with functional group (active group for having exchange ion), has reticular structure, insoluble
High-molecular compound.Usually spheric granules object.The various types of ion exchange resin have because of chemical composition and structure difference
There are different function and characteristic, is adapted to different purposes.Ion exchange resin is mainly used in water treatment field, is in addition eating
Product industry, pharmaceutical industry, synthesis chemistry and petro chemical industry, environmental protection, hydrometallurgy etc. also have more answer
With.Ion-exchange treatment is carried out using ion exchange resin, it is necessary to (referred to as be exchanged with a kind of substance for being referred to as ion-exchanger
Agent) Lai Jinhang.When this substance meets water, the ion in certain ion possessed by itself and water with symbol can mutually be handed over
It changes, there are many type of ion-exchanger, there is natural and artificial, organic and inorganic, cationic and anionic etc..But it is single
Often applicable surface is more narrow for the ion exchange resin of one type, and when sewage composition is more complex, traditional ion exchange resin exists
It there is certain limitation in use process.
In order to overcome above-mentioned insufficient, it can be achieved that exchange to more kinds of ions, preferably meets in the market to complicated ingredient
Sewage treatment there is an urgent need to the preparation method for inventing a kind of multifunctional exchange resin is very necessary.
Summary of the invention
The purpose of the present invention is inventing a kind of preparation method of multifunctional exchange resin, a kind of multifunction ion friendship
The preparation method for changing resin has the characteristics that cost of manufacture is lower, easy for construction.
A kind of preparation method of multifunctional exchange resin takes following scheme to realize:
A kind of preparation method of multifunctional exchange resin, it is characterised in that the following steps are included:
(1) each raw material is weighed respectively by following mass fraction:
(2) by after raw material mixed at room temperature each in above-mentioned steps (1), it is warming up to 60-100 DEG C, then in 3000-5000r/min
Revolving speed under stir evenly；
(3) each raw material is weighed respectively by following mass fraction:
(4) each raw material in above-mentioned steps (3) is uniformly mixed, then mixed liquor is gradually added drop-wise to what step (2) obtained
In solution, time for adding 3-5h is kept for 30-50 DEG C of reaction temperature；
(5) continue to stir after being added dropwise to complete, and be warming up to 60-90 DEG C, react 1-2h；It is warming up to 90-120 DEG C again later,
The reaction was continued 0.5-1.5h；
(6) stop heating, be cooled to room temperature while stirring, then reaction product is filtered, wash, is dried, is obtained
Compound resin microballoon；
(7) each raw material is weighed respectively by following mass fraction:
(8) distilled water, chloromethyl ether and zinc chloride are added in reaction kettle, stir evenly, is then answered what step (6) obtained
Resin microballoon divides 3-5 addition, every minor tick 30-60min, and temperature is controlled at 40-50 DEG C, keeps the temperature 6-8h；It later will reaction
Object is washed with deionized to neutrality；Ethyl alcohol is added, stands 10-20h after stirring evenly；
(9) triethylene tetramine, time for adding 0.5-1h, later by temperature control are added dropwise in the reactant that step (8) obtains
System reacts 2-4h at 10-40 DEG C；N, N- dimethyl cyclohexyl amine, time for adding 10-20min is added dropwise again later, and is warming up to 38-
40 DEG C, keep the temperature 6-8h；Reactant is washed with deionized to neutrality later, is filtered, low temperature drying.
The nanometer wollastonite, partial size 20-80nm.
The nano lignin, partial size 10-50nm.
The dispersing agent is one of polyvinyl alcohol, carboxymethyl cellulose, hydroxypropyl cellulose.
A kind of preparation method of multifunctional exchange resin of the invention is closed in polystyrene chloromethylation, amination etc.
Key step is all different from traditional method, while introducing nano-inorganic substance and nanometer organic matter, the ion exchange obtained from
Resin is the composition of multiple groups parting, thus, different kinds of ions can be exchanged simultaneously, simple process, exchange effect is good, especially suitable for
Processing is containing phenol, halogen, sulfur-containing waste water processing.
Specific embodiment
Embodiment 1:
A kind of preparation method of multifunctional exchange resin, it is characterised in that the following steps are included:
(1) each raw material is weighed respectively by following mass fraction:
(2) by after raw material mixed at room temperature each in above-mentioned steps (1), 80 DEG C are warming up to, then stir under the revolving speed of 4000r/min
It mixes uniformly；
(3) each raw material is weighed respectively by following mass fraction:
(4) each raw material in above-mentioned steps (3) is uniformly mixed, then mixed liquor is gradually added drop-wise to what step (2) obtained
In solution, time for adding 4h is kept for 40 DEG C of reaction temperature；
(5) continue to stir after being added dropwise to complete, and be warming up to 75 DEG C, react 1.5h；It is warming up to 105 DEG C again later, continues anti-
Answer 1h；
(6) stop heating, be cooled to room temperature while stirring, then reaction product is filtered, wash, is dried, is obtained
Compound resin microballoon；
(7) each raw material is weighed respectively by following mass fraction:
(8) distilled water, chloromethyl ether and zinc chloride are added in reaction kettle, stir evenly, is then answered what step (6) obtained
4 additions of resin microballoon point, every minor tick 45min, temperature are controlled at 45 DEG C, keep the temperature 7h；Later by reactant deionization
Water washing is to neutrality；Ethyl alcohol is added, stands 15h after stirring evenly；
(9) triethylene tetramine is added dropwise in the reactant that step (8) obtains, time for adding 0.75h later controls temperature
At 25 DEG C, 3h is reacted；N, N- dimethyl cyclohexyl amine, time for adding 15min is added dropwise again later, and is warming up to 39 DEG C, keeps the temperature 7h；It
Reactant is washed with deionized to neutrality afterwards, is filtered, low temperature drying.
Embodiment 2:
A kind of preparation method of multifunctional exchange resin, it is characterised in that the following steps are included:
(1) each raw material is weighed respectively by following mass fraction:
(2) by after raw material mixed at room temperature each in above-mentioned steps (1), 60 DEG C are warming up to, then stir under the revolving speed of 3000r/min
It mixes uniformly；
(3) each raw material is weighed respectively by following mass fraction:
(4) each raw material in above-mentioned steps (3) is uniformly mixed, then mixed liquor is gradually added drop-wise to what step (2) obtained
In solution, time for adding 3h is kept for 30 DEG C of reaction temperature；
(5) continue to stir after being added dropwise to complete, and be warming up to 60 DEG C, react 1h；It is warming up to 90 DEG C again later, the reaction was continued
0.5h；
(6) stop heating, be cooled to room temperature while stirring, then reaction product is filtered, wash, is dried, is obtained
Compound resin microballoon；
(7) each raw material is weighed respectively by following mass fraction:
(8) distilled water, chloromethyl ether and zinc chloride are added in reaction kettle, stir evenly, is then answered what step (6) obtained
Resin microballoon is added three times, every minor tick 30min, and temperature is controlled at 40 DEG C, keeps the temperature 6h；Later by reactant deionization
Water washing is to neutrality；Ethyl alcohol is added, stands 10h after stirring evenly；
(9) triethylene tetramine is added dropwise in the reactant that step (8) obtains, time for adding 0.5h later controls temperature
At 10 DEG C, 2h is reacted；N, N- dimethyl cyclohexyl amine, time for adding 10min is added dropwise again later, and is warming up to 38 DEG C, keeps the temperature 6h；It
Reactant is washed with deionized to neutrality afterwards, is filtered, low temperature drying.
Embodiment 3:
A kind of preparation method of multifunctional exchange resin, it is characterised in that the following steps are included:
(1) each raw material is weighed respectively by following mass fraction:
(2) by after raw material mixed at room temperature each in above-mentioned steps (1), 100 DEG C are warming up to, then under the revolving speed of 5000r/min
It stirs evenly；
(3) each raw material is weighed respectively by following mass fraction:
(4) each raw material in above-mentioned steps (3) is uniformly mixed, then mixed liquor is gradually added drop-wise to what step (2) obtained
In solution, time for adding 5h is kept for 50 DEG C of reaction temperature；
(5) continue to stir after being added dropwise to complete, and be warming up to 90 DEG C, react 2h；It is warming up to 120 DEG C again later, the reaction was continued
1.5h；
(6) stop heating, be cooled to room temperature while stirring, then reaction product is filtered, wash, is dried, is obtained
Compound resin microballoon；
(7) each raw material is weighed respectively by following mass fraction:
(8) distilled water, chloromethyl ether and zinc chloride are added in reaction kettle, stir evenly, is then answered what step (6) obtained
5 additions of resin microballoon point, every minor tick 60min, temperature are controlled at 50 DEG C, keep the temperature 8h；Later by reactant deionization
Water washing is to neutrality；Ethyl alcohol is added, stands 20h after stirring evenly；
(9) triethylene tetramine is added dropwise in the reactant that step (8) obtains, time for adding 1h later controls temperature
40 DEG C, react 4h；N, N- dimethyl cyclohexyl amine, time for adding 20min is added dropwise again later, and is warming up to 40 DEG C, keeps the temperature 8h；Later
Reactant is washed with deionized to neutrality, is filtered, low temperature drying.
Embodiment 4:
A kind of preparation method of multifunctional exchange resin, it is characterised in that the following steps are included:
(1) each raw material is weighed respectively by following mass fraction:
(2) by after raw material mixed at room temperature each in above-mentioned steps (1), 80 DEG C are warming up to, then stir under the revolving speed of 5000r/min
It mixes uniformly；
(3) each raw material is weighed respectively by following mass fraction:
(4) each raw material in above-mentioned steps (3) is uniformly mixed, then mixed liquor is gradually added drop-wise to what step (2) obtained
In solution, time for adding 5h is kept for 30 DEG C of reaction temperature；
(5) continue to stir after being added dropwise to complete, and be warming up to 75 DEG C, react 2h；It is warming up to 90 DEG C again later, the reaction was continued
1h；
(6) stop heating, be cooled to room temperature while stirring, then reaction product is filtered, is washed, under it is dry, obtain
Compound resin microballoon；
(7) each raw material is weighed respectively by following mass fraction:
(8) distilled water, chloromethyl ether and zinc chloride are added in reaction kettle, stir evenly, is then answered what step (6) obtained
4 additions of resin microballoon point, every minor tick 60min, temperature are controlled at 40 DEG C, keep the temperature 7h；Later by reactant deionization
Water washing is to neutrality；Ethyl alcohol is added, stands 20h after stirring evenly；
(9) triethylene tetramine is added dropwise in the reactant that step (8) obtains, time for adding 0.5h later controls temperature
At 25 DEG C, 4h is reacted；N, N- dimethyl cyclohexyl amine, time for adding 10min is added dropwise again later, and is warming up to 39 DEG C, keeps the temperature 8h；It
Reactant is washed with deionized to neutrality afterwards, is filtered, low temperature dry in.
Embodiment 5:
A kind of preparation method of multifunctional exchange resin, it is characterised in that the following steps are included:
(1) each raw material is weighed respectively by following mass fraction:
(2) by after raw material mixed at room temperature each in above-mentioned steps (1), 100 DEG C are warming up to, then under the revolving speed of 3000r/min
It stirs evenly；
(3) each raw material is weighed respectively by following mass fraction:
(4) each raw material in above-mentioned steps (3) is uniformly mixed, then mixed liquor is gradually added drop-wise to what step (2) obtained
In solution, time for adding 3h is kept for 40 DEG C of reaction temperature；
(5) continue to stir after being added dropwise to complete, and be warming up to 90 DEG C, react 1h；It is warming up to 105 DEG C again later, the reaction was continued
1.5h；
(6) stop heating, be cooled to room temperature while stirring, then reaction product is filtered, wash, is dried, is obtained
Compound resin microballoon；
(7) each raw material is weighed respectively by following mass fraction:
(8) distilled water, chloromethyl ether and zinc chloride are added in reaction kettle, stir evenly, is then answered what step (6) obtained
5 additions of resin microballoon point, every minor tick 30min, temperature are controlled at 45 DEG C, keep the temperature 8h；Later by reactant deionization
Water washing is to neutrality；Ethyl alcohol is added, stands 10h after stirring evenly；
(9) triethylene tetramine is added dropwise in the reactant that step (8) obtains, time for adding 0.75h later controls temperature
At 40 DEG C, 2h is reacted；N, N- dimethyl cyclohexyl amine, time for adding 15min is added dropwise again later, and is warming up to 40 DEG C, keeps the temperature 6h；It
Reactant is washed with deionized to neutrality afterwards, is filtered, low temperature drying.
Embodiment 6:
A kind of preparation method of multifunctional exchange resin, it is characterised in that the following steps are included:
(1) each raw material is weighed respectively by following mass fraction:
(2) by after raw material mixed at room temperature each in above-mentioned steps (1), 60 DEG C are warming up to, then stir under the revolving speed of 4000r/min
It mixes uniformly；
(3) each raw material is weighed respectively by following mass fraction:
(4) each raw material in above-mentioned steps (3) is uniformly mixed, then mixed liquor is gradually added drop-wise to what step (2) obtained
In solution, time for adding 4h is kept for 50 DEG C of reaction temperature；
(5) continue to stir after being added dropwise to complete, and be warming up to 60 DEG C, react 1.5h；It is warming up to 120 DEG C again later, continues anti-
Answer 0.5h:
(6) stop heating, be cooled to room temperature while stirring, then reaction product is filtered, wash, is dried, is obtained
Compound resin microballoon；
(7) each raw material is weighed respectively by following mass fraction:
(8) distilled water, chloromethyl ether and zinc chloride are added in reaction kettle, stir evenly, is then answered what step (6) obtained
Resin microballoon is added three times, every minor tick 45min, and temperature is controlled at 50 DEG C, keeps the temperature 6h；Later by reactant deionization
Water washing is to neutrality；Ethyl alcohol is added, stands 15h after stirring evenly；
(9) triethylene tetramine is added dropwise in the reactant that step (8) obtains, time for adding 1h later exists temperature degree system
10 DEG C, react 3h；N, N- dimethyl cyclohexyl amine, time for adding 20min is added dropwise again later, and is warming up to 38 DEG C, keeps the temperature 7h；Later
Reactant is washed with deionized to neutrality, is filtered, low temperature dry in.
Embodiment 7:
A kind of preparation method of multifunctional exchange resin, it is characterised in that the following steps are included:
(1) each raw material is weighed respectively by following mass fraction:
(2) by after raw material mixed at room temperature each in above-mentioned steps (1), 90 DEG C are warming up to, then stir under the revolving speed of 4500r/min
It mixes uniformly；
(3) each raw material is weighed respectively by following mass fraction:
(4) each raw material in above-mentioned steps (3) is uniformly mixed, then mixed liquor is gradually added drop-wise to what step (2) obtained
In solution, time for adding 3.5h is kept for 35 DEG C of reaction temperature；
(5) continue to stir after being added dropwise to complete, and be warming up to 78 DEG C, react 1.2h；It is warming up to 100 DEG C again later, continues anti-
Answer 0.8h:
(6) stop heating, be cooled to room temperature while stirring, then reaction product is filtered, wash, is dried, is obtained
Compound resin microballoon；
(7) each raw material is weighed respectively by following mass fraction:
(8) distilled water, chloromethyl ether and zinc chloride are added in reaction kettle, stir evenly, is then answered what step (6) obtained
4 additions of resin microballoon point, every minor tick 50min, temperature are controlled at 47 DEG C, keep the temperature 6.8h；Later by reactant spend from
Sub- water washing is to neutrality；Ethyl alcohol is added, stands 13h after stirring evenly；
(9) triethylene tetramine is added dropwise in the reactant that step (8) obtains, time for adding 0.6h later controls temperature
At 30 DEG C, 2.5h is reacted；N, N- dimethyl cyclohexyl amine, time for adding 18min is added dropwise again later, and is warming up to 38.5 DEG C, keeps the temperature
6.5h；Lower neutrality is washed with deionized in reactant later, is filtered, low temperature drying.
Illustrate the effect of embodiment 1 by detection to face:
Through detecting, 1 full exchange capacity of embodiment: 11.5mmol/g, volume-exchange capacity: 4.82mmol/g, real density:
1.27g/ml, apparent density: 0.86g/ml, effective grain size: 0.51mm, coefficient of uniformity: 1.6.
Testing result shows that a kind of resulting multifunctional exchange resin of embodiment 1 has biggish aperture and exchange
Capacity, ion-exchange effect are good.
Claims (4)
1. a kind of preparation method of multifunctional exchange resin, it is characterised in that the following steps are included:
(1) each raw material is weighed respectively by following mass fraction:
(2) it after raw material mixed at room temperature each in above-mentioned steps (1), will be warming up to 60-100 DEG C, then turned in 3000-5000r/min
It is stirred evenly under speed；
(3) each raw material is weighed respectively by following mass fraction:
(4) each raw material in above-mentioned steps (3) is uniformly mixed, then mixed liquor is gradually added drop-wise to the solution that step (2) obtains
In, time for adding 3-5h is kept for 30-50 DEG C of reaction temperature；
(5) continue to stir after being added dropwise to complete, and be warming up to 60-90 DEG C, react 1-2h；It is warming up to 90-120 DEG C again later, continues
React 0.5-1.5h；
(6) stop heating, be cooled to room temperature while stirring, then reaction product is filtered, wash, is dried, obtain compound
Resin microsphere；
(7) symbol raw material is weighed respectively by following mass fraction:
(8) distilled water, chloromethyl ether and zinc chloride are added in reaction kettle, are stirred evenly, the compound tree for then obtaining step (6)
Lipid microspheres divide 3-5 addition, every minor tick 30-60min, and temperature is controlled at 40-50 DEG C, keep the temperature 6-8h；Reactant is used later
Deionized water is washed to neutrality；Ethyl alcohol is added, stands 10-20h after stirring evenly；
(9) triethylene tetramine is added dropwise in the reactant that step (8) obtains, time for adding 0.5-1h later controls temperature
10-40 DEG C, react 2-4h；N, N- dimethyl cyclohexyl amine, time for adding 10-20min is added dropwise again later, and is warming up to 38-40 DEG C,
Keep the temperature 6-8h；Reactant is washed with deionized to neutrality later, is filtered, low temperature drying.
2. a kind of preparation method of multifunctional exchange resin according to claim 1, it is characterised in that described receives
Rice wollastonite, partial size 20-80nm.
3. a kind of preparation method of multifunctional exchange resin according to claim 1, it is characterised in that described receives
Rice lignin, partial size 10-50nm.
4. a kind of preparation method of multifunctional exchange resin according to claim 1, it is characterised in that point
Powder is one of polyvinyl alcohol, carboxymethyl cellulose, hydroxypropyl cellulose.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102500430A (en) * | 2011-10-19 | 2012-06-20 | 厦门大学 | Modified anion exchange resin with double long carbon chains and preparation method and application thereof |
| 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 |
| CN106188370A (en) * | 2016-08-05 | 2016-12-07 | 安徽皖东化工有限公司 | A kind of production method of Phenol-Containing Wastewater Treatment polystyrene multi-component copolymer ion exchange resin |
| CN106238011A (en) * | 2016-08-05 | 2016-12-21 | 安徽皖东化工有限公司 | A kind of production method of magnalium brucite composite polystyrene multi-component copolymer ion exchange resin |
-
2018
- 2018-12-27 CN CN201811616947.XA patent/CN109851702A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102500430A (en) * | 2011-10-19 | 2012-06-20 | 厦门大学 | Modified anion exchange resin with double long carbon chains and preparation method and application thereof |
| 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 |
| CN106188370A (en) * | 2016-08-05 | 2016-12-07 | 安徽皖东化工有限公司 | A kind of production method of Phenol-Containing Wastewater Treatment polystyrene multi-component copolymer ion exchange resin |
| CN106238011A (en) * | 2016-08-05 | 2016-12-21 | 安徽皖东化工有限公司 | A kind of production method of magnalium brucite composite polystyrene multi-component copolymer ion exchange resin |
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