CN106268981A - A kind of waste water is except the production method of chromium polystyrene multi-component copolymer ion exchange resin - Google Patents
A kind of waste water is except the production method of chromium polystyrene multi-component copolymer ion exchange resin Download PDFInfo
- Publication number
- CN106268981A CN106268981A CN201610634560.1A CN201610634560A CN106268981A CN 106268981 A CN106268981 A CN 106268981A CN 201610634560 A CN201610634560 A CN 201610634560A CN 106268981 A CN106268981 A CN 106268981A
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- CN
- China
- Prior art keywords
- ion exchange
- exchange resin
- chromium
- aqueous phase
- oil phase
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Classifications
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/42—Treatment of water, waste water, or sewage by ion-exchange
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/42—Treatment of water, waste water, or sewage by ion-exchange
- C02F2001/425—Treatment of water, waste water, or sewage by ion-exchange using cation exchangers
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Treatment Of Water By Ion Exchange (AREA)
Abstract
The invention discloses a kind of waste water except the production method of chromium polystyrene multi-component copolymer ion exchange resin, the concrete steps of the method include the preparation of aqueous phase, oil phase, the preparation of composite resin microsphere and the synthesis of ion exchange resin, wherein resin microsphere skeleton is cross-linked by styrene, methyl methacrylate and vinyltrimethoxy silane and forms.The polystyrene multi-component copolymer ion exchange resin of the present invention had both had good high temperature resistant, chemical-resistant stability, applied widely, and mechanical strength is high simultaneously, uniform pore diameter is good, ion exchange capacity is high, especially good to the absorption property of trace chromium in water, it is adaptable to waste water processes except chromium.
Description
Technical field
The present invention relates to the production method of a kind of ion exchange resin, particularly relate to a kind of waste water except chromium polystyrene many
The production method of unit's copolymerization ion exchange resin.
Background technology
Ion exchange resin is the adsorption and separation material that a class is important, and structure belongs to porous sponge shape solid macromolecule
Material, each resin particle is made up of the network skeleton with three dimensions stereochemical structure cross-linked, and connects and permitted on skeleton
Function base that how can be movable.Its do not dissolve in general acid-base solution and organic solvent, may be used for water process, food pharmaceutical,
The various field such as petrochemical industry and environmental conservation, plays the most important effect in modern industry.
At present, applying most common ion exchange resin is the resin of polystyrene backbone, it have raw material be easy to get, price
Cheap advantage, industrialization low cost.But this resinoid heat stability is low, relatively big by using temperature to be affected, limit it
Range of application, and chemical stability is poor, and mechanical strength is bad, and especially compressive property is poor, and this also have impact on it and uses
In the life-span, therefore improve its combination property the most necessary.CN201310172597 introduces long-chain flexible unit methacrylic acid ten
Octaester is with styrene copolymerized, thus improves the comprcssive strength of ion exchange resin beads, but this method is only capable of promoting polyphenyl
The compressive property of vinyl, it is impossible to comprehensively improve the combination properties such as its homogeneity, heat stability, chemical stability, it is difficult to full
The current demand to more high mass ions exchanger resin of foot, is of limited application.
Summary of the invention
The object of the invention is contemplated to make up the defect of prior art, it is provided that a kind of Heat stability is good, mechanical strength are high, hole
The waste water that footpath is evenly distributed, exchange capacity is high is except the production method of chromium polystyrene multi-component copolymer ion exchange resin.
The present invention is achieved by the following technical solutions:
A kind of waste water is except the production method method of chromium polystyrene multi-component copolymer ion exchange resin, it is characterised in that the method
Including step in detail below:
(1) preparation of aqueous phase, described aqueous phase is prepared by the raw material of following weight parts: Polyethylene Glycol 0.5-1, tea saponin 0.1-
0.15, Tween-80 0.1-0.2, carboxymethyl cellulose 0.5-1, xanthan gum 0.3-0.5, water 80-100, described aqueous phase
Preparation process is that tea saponin, Tween-80 are added to the water dispersed with stirring 5-10min, is subsequently adding the mixing of remaining raw material molten
Solve uniformly, obtain aqueous phase；
(2) preparation of oil phase, described oil phase is prepared by the raw material of following weight parts: styrene 40-60, divinylbenzene 5-10,
Benzoyl peroxide 0.5-1, methyl methacrylate 3-5, vinyltrimethoxy silane 3-5, liquid paraffin 2-4, epoxy is big
Oleum Glycines 0.5-1, medical stone powder 2-4, the preparation process of described oil phase is first by styrene, methyl methacrylate and vinyl three
Methoxy silane is mixed is incorporated in 40-60 DEG C of stirring 0.5-1h, is subsequently adding remaining raw material mix homogeneously, obtains oil phase；
(3) preparation of composite resin microsphere, is poured slowly into the oil phase in step (2) in the aqueous phase in step (1), prior to 65-
75 DEG C of stirring reaction 1-2h, then heat to 85-95 DEG C, and first stirring reaction 2-4h, then insulation reaction 4-6h, after reaction terminates
By the product obtained through sucking filtration, wash, be dried, obtain composite resin microsphere, described oil phase with the weight ratio of aqueous phase is
1:6-1:8；
(4) synthesis of ion exchange resin, is 40-60% by the composite resin microsphere 1:1-1:2 by volume in (3) and concentration
Adding zinc chloride after chloromethyl ether mix homogeneously, zinc chloride is 1:10-1:15 with the weight ratio of composite resin microsphere, stirring reaction 2-
Taking out solids cyclic washing after 4h and obtain chlorine ball for several times, the ethanol that then chlorine ball 1:2-1:3 by volume adds 80-90% is molten
Swelling in liquid overnight the volume ratio adding triethylene tetramine, triethylene tetramine and chlorine ball is 1.5:1-2:1, stirring reaction 3-
5h, is washed till neutrality by the solids distilled water obtained, and obtains waste water except chromium polystyrene multi-component copolymer ion exchange resin.
The invention have the advantage that
One aspect of the present invention utilizes styrene, methyl methacrylate and vinyltrimethoxy silane to carry out copolymerzation with cross-linking to prepare
Resin microsphere skeleton, promotes the thermostability of ion exchange resin, crushing resistance and stability, on the one hand by aqueous phase, oil phase auxiliary agent
Selection and compound synergic effect, improve the homogeneity of ion exchange resin, and improve ion exchange capacity, make the polyphenyl prepared
Ethylene multi-component copolymer ion exchange resin had both had good high temperature resistant, chemical-resistant stability, applied widely, and machinery is strong simultaneously
Degree height, uniform pore diameter is good, and ion exchange capacity is high, especially good to the absorption property of trace chromium in water, it is adaptable to waste water removes chromium
Process.
Detailed description of the invention
A kind of waste water is except the production method of chromium polystyrene multi-component copolymer ion exchange resin, and method includes in detail below
Step:
(1) preparation of aqueous phase, described aqueous phase is prepared by the raw material of following weight parts: Polyethylene Glycol 0.5, tea saponin 0.1, poly-mountain
Pear ester-80 0.1, carboxymethyl cellulose 0.5, xanthan gum 0.3, water 80-, the preparation process of described aqueous phase is by tea saponin, poly-mountain
Pear ester-80 is added to the water dispersed with stirring 5min, is subsequently adding remaining raw material mixed dissolution uniform, obtains aqueous phase；
(2) preparation of oil phase, described oil phase is prepared by the raw material of following weight parts: styrene 40, divinylbenzene 5, peroxidating
Benzoyl 0.5, methyl methacrylate 3, vinyltrimethoxy silane 3, liquid paraffin 2, epoxy soybean oil 0.5, Maifanitum
Powder 2, the preparation process of described oil phase is first to be incorporated in mixed to styrene, methyl methacrylate and vinyltrimethoxy silane
40 DEG C of stirring 0.5h, are subsequently adding remaining raw material mix homogeneously, obtain oil phase；
(3) preparation of composite resin microsphere, is poured slowly into the oil phase in step (2) in the aqueous phase in step (1), prior to 65 DEG C
Stirring reaction 1h, then heats to 85 DEG C, first stirring reaction 2h, then insulation reaction 4h, the reaction that reaction will obtain after terminating
Product through sucking filtration, wash, be dried, obtain composite resin microsphere, described oil phase is 1:6 with the weight ratio of aqueous phase；
(4) synthesis of ion exchange resin, is that 40% chloromethyl ether mixes by the composite resin microsphere 1:1 by volume in (3) and concentration
Adding zinc chloride after closing uniformly, zinc chloride is 1:10 with the weight ratio of composite resin microsphere, takes out solids after stirring reaction 2h
Cyclic washing for several times chlorine ball, then by chlorine ball 1:2 by volume add 80% ethanol solution in swelling overnight, add three
Ethylene tetramine, triethylene tetramine is 1.5:1 with the volume ratio of chlorine ball, stirring reaction 3h, the solids distillation washing that will obtain
To neutral, obtain waste water except chromium polystyrene multi-component copolymer ion exchange resin.
Above-mentioned prepared ion exchange resin the performance test results is as follows:
Rate of small round spheres after mill: >=95%；
At pH=7,0.1g resin is added under the conditions of 25 DEG C vibration absorption 1h in the 50mL waste water containing hexavalent chromium 100mg/L,
The concentration remaining hexavalent chromium in detection water is 0.19mg/L, reaches discharging standards.
Resin is placed in 95 DEG C of waters bath with thermostatic control insulation 48h, exchange capacity loss rate≤3%.
Claims (1)
1. a waste water is except the chromium production method of polystyrene multi-component copolymer ion exchange resin, it is characterised in that the method
Including step in detail below:
(1) preparation of aqueous phase, described aqueous phase is prepared by the raw material of following weight parts: Polyethylene Glycol 0.5-1, tea saponin 0.1-
0.15, Tween-80 0.1-0.2, carboxymethyl cellulose 0.5-1, xanthan gum 0.3-0.5, water 80-100, described aqueous phase
Preparation process is that tea saponin, Tween-80 are added to the water dispersed with stirring 5-10min, is subsequently adding the mixing of remaining raw material molten
Solve uniformly, obtain aqueous phase；
(2) preparation of oil phase, described oil phase is prepared by the raw material of following weight parts: styrene 40-60, divinylbenzene 5-10,
Benzoyl peroxide 0.5-1, methyl methacrylate 3-5, vinyltrimethoxy silane 3-5, liquid paraffin 2-4, epoxy is big
Oleum Glycines 0.5-1, medical stone powder 2-4, the preparation process of described oil phase is first by styrene, methyl methacrylate and vinyl three
Methoxy silane is mixed is incorporated in 40-60 DEG C of stirring 0.5-1h, is subsequently adding remaining raw material mix homogeneously, obtains oil phase；
(3) preparation of composite resin microsphere, is poured slowly into the oil phase in step (2) in the aqueous phase in step (1), prior to 65-
75 DEG C of stirring reaction 1-2h, then heat to 85-95 DEG C, and first stirring reaction 2-4h, then insulation reaction 4-6h, after reaction terminates
By the product obtained through sucking filtration, wash, be dried, obtain composite resin microsphere, described oil phase with the weight ratio of aqueous phase is
1:6-1:8；
(4) synthesis of ion exchange resin, is 40-60% by the composite resin microsphere 1:1-1:2 by volume in (3) and concentration
Adding zinc chloride after chloromethyl ether mix homogeneously, zinc chloride is 1:10-1:15 with the weight ratio of composite resin microsphere, stirring reaction 2-
Taking out solids cyclic washing after 4h and obtain chlorine ball for several times, the ethanol that then chlorine ball 1:2-1:3 by volume adds 80-90% is molten
Swelling in liquid overnight the volume ratio adding triethylene tetramine, triethylene tetramine and chlorine ball is 1.5:1-2:1, stirring reaction 3-
5h, is washed till neutrality by the solids distilled water obtained, and obtains waste water except chromium polystyrene multi-component copolymer ion exchange resin.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610634560.1A CN106268981A (en) | 2016-08-05 | 2016-08-05 | A kind of waste water is except the production method of chromium polystyrene multi-component copolymer ion exchange resin |
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|---|---|---|---|
| CN201610634560.1A CN106268981A (en) | 2016-08-05 | 2016-08-05 | A kind of waste water is except the production method of chromium polystyrene multi-component copolymer ion exchange resin |
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| CN106268981A true CN106268981A (en) | 2017-01-04 |
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| CN201610634560.1A Withdrawn CN106268981A (en) | 2016-08-05 | 2016-08-05 | A kind of waste water is except the production method of chromium polystyrene multi-component copolymer ion exchange resin |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107722156A (en) * | 2017-09-06 | 2018-02-23 | 安徽皖东化工有限公司 | A kind of big ion exchange resin preparation method of specific surface area |
| CN113877562A (en) * | 2020-07-03 | 2022-01-04 | 中国石油化工股份有限公司 | Solid base catalyst for synthesizing methyl acrylate and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5292439A (en) * | 1990-11-22 | 1994-03-08 | Mitsubishi Kasei Corporation | Method for preparing ultrapure water |
| 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 |
| CN103012686A (en) * | 2012-11-27 | 2013-04-03 | 安徽皖东化工有限公司 | Preparation method of macroporous styrene anion resin intermediate chloromethylated bead |
| CN103275256A (en) * | 2013-05-10 | 2013-09-04 | 中国地质大学（武汉） | High compressive polystyrene-co-octadecyl methacrylate copolymer resin microsphere and preparation method thereof |
-
2016
- 2016-08-05 CN CN201610634560.1A patent/CN106268981A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5292439A (en) * | 1990-11-22 | 1994-03-08 | Mitsubishi Kasei Corporation | Method for preparing ultrapure water |
| 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 |
| CN103012686A (en) * | 2012-11-27 | 2013-04-03 | 安徽皖东化工有限公司 | Preparation method of macroporous styrene anion resin intermediate chloromethylated bead |
| CN103275256A (en) * | 2013-05-10 | 2013-09-04 | 中国地质大学（武汉） | High compressive polystyrene-co-octadecyl methacrylate copolymer resin microsphere and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 高俊刚等: "VTMS/MMA/St三元共聚物的合成与表征", 《塑料工业》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107722156A (en) * | 2017-09-06 | 2018-02-23 | 安徽皖东化工有限公司 | A kind of big ion exchange resin preparation method of specific surface area |
| CN113877562A (en) * | 2020-07-03 | 2022-01-04 | 中国石油化工股份有限公司 | Solid base catalyst for synthesizing methyl acrylate and preparation method and application thereof |
| CN113877562B (en) * | 2020-07-03 | 2024-05-03 | 中国石油化工股份有限公司 | Solid base catalyst for synthesizing methyl acrylate, and preparation method and application thereof |
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Application publication date: 20170104 |