CN104059187A - Super-macroporous adsorbent resin and preparation method thereof - Google Patents
Super-macroporous adsorbent resin and preparation method thereof Download PDFInfo
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- CN104059187A CN104059187A CN201410251408.6A CN201410251408A CN104059187A CN 104059187 A CN104059187 A CN 104059187A CN 201410251408 A CN201410251408 A CN 201410251408A CN 104059187 A CN104059187 A CN 104059187A
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Abstract
The invention relates to a super-macroporous adsorbent resin and a preparation method thereof, belonging to the field of high polymer materials. The super-macroporous adsorbent resin is prepared from the following raw materials in parts by weight: 50-70 parts of divinylbenzene, 5-10 parts of styrene, 10-20 parts of glycol bis-methacrylate, 5-10 parts of polystyrene, 50-80 parts of diethyl phthalate, 30-50 parts of 200# gasoline, 1-2 parts of diphenyl acyl peroxide, 150-200 parts of deionized water and 1-2 parts of polyvinyl alcohol. The polystyrene and diethyl phthalate used as the pore-forming agent component for preparing the super-macroporous adsorbent resin increase the pore size of the resin and widen the application range of the resin. The second crosslinking agent increases the pore size of the resin, ensures the mechanical strength of the resin and provides the service life of the resin.
Description
Technical field
The present invention relates to a kind of polymeric adsorbent and preparation method thereof, more particularly, the present invention relates to a kind of especially big macroporous adsorbent resin and preparation method thereof, belong to technical field of polymer materials.
Technical background
Macroporous adsorbent resin is that a class is containing cation exchange groups and there is the preparation of macroporous structure, there is good macroporous netlike structure and larger specific surface area, can be by physical adsorption adsorb organic compound selectively from the aqueous solution, be the novel organic polymer sorbent material growing up the sixties in 20th century, be widely used in environmental protection, food, medicine and other fields.
Macroporous adsorbent resin claims again full porous adsorption resin, and macroporous adsorbent resin is to be prepared from through polyreaction by additives such as polymerization single polymerization monomer and linking agent, pore-creating agent, dispersion agents.After polymer formation, pore-creating agent is removed, and has left hole big and small, different, that interpenetrate in resin.Therefore macroporous adsorbent resin its inside under drying regime has higher porosity, and aperture is larger, between 100-1000nm.
It is CN101058068 that State Intellectual Property Office discloses a publication number in 2007.10.24, name is called the patent of invention of " a kind of macroporous adsorption resin special used for separating antibiotic and preparation method thereof ", this patent is taking styrene-divinylbenzene macropore copolymerization bead (St-DVB Archon) as starting material, adopt 2 ~ 4 kinds of function monomers and linking agent, under the condition existing in peroxide initiator, water and minerals, carrying out the two nets of secondary, to pass through mutually crosslinking copolymerization reaction synthetic.The formula of St-DVB Archon comprises a certain proportion of: vinylbenzene, 80% Vinylstyrene, dibenzoyl peroxide, pore-creating agent (toluene, whiteruss and gasoline etc.), gelatin and distilled water.The formula that the two nets of secondary pass through crosslinking copolymerization reaction mutually comprises a certain proportion of: St-DVB Archon, 2 ~ 4 kinds of function monomers, peroxide initiator, inert diluent, stablizer and distilled water.Synthesized resin reaches 185ku/g to the equilibrium adsorption capacity of erythromycin in streptomyces erythreus fermentation cleaner liquid, is 140% of conventional polymeric adsorbent, and its selection to pigment in fermented liquid is removed the more conventional resin of ability and improved 70-90%.
It is CN101070400 that State Intellectual Property Office discloses a publication number in 2007.11.14, name is called the patent of invention of " a kind of preparation method of imidazole modified styrene tyle macroporous adsorption resin ", and this patent provides a kind of preparation method of imidazole modified styrene tyle macroporous adsorption resin.Its preparation method divides two steps, first by the salt-forming reaction of imidazoles, on 1, introduce particular functional group, realize the functionalization of imidazoles, and then react with the styrene tyle macroporous adsorption resin of chlorination reaction, realize styrene tyle macroporous adsorption resin imidazole modified.The present invention is introduced into the imidazol ion of functionalization in styrene tyle macroporous adsorption resin, utilize the physicochemical property of imidazol ion uniqueness and the controllability of physico-chemical property thereof, both polarity and the wetting ability of resin can be increased, the separation and purification scope of styrenic macroporous adsorbent resin in the field such as food, medicine can be widened again.
Macroporous adsorbent resin has a wide range of applications in environment protection, pharmaceutical cpd separation and purification field.But the aperture of product is less at present, and the separation and purification object larger to some molecular weight is difficult to reach active adsorption, limited the application of this product.
Summary of the invention
The present invention is intended to solve the less problem in prior art macroporous adsorbent resin aperture, and a kind of especially big macroporous adsorbent resin is provided, and its aperture is large compared with general macroporous adsorbent resin, has expanded its range of application.
In order to realize foregoing invention object, its concrete technical scheme is as follows:
A kind of especially big macroporous adsorbent resin, is characterized in that: comprise following according to the raw material of parts by weight meter:
Vinylstyrene 50-70 part
Vinylbenzene 5-10 part
Ethyleneglycol dimethyacrylate 10-20 part
Polystyrene 5-10 part
Diethyl phthalate 50-80 part
No. 200 gasoline 30-50 parts
Diphenyl peroxide base acyl 1-2 part
Deionized water 150-200 part
Polyvinyl alcohol 1-2 part.
A kind of especially big macroporous adsorbent resin, is characterized in that: comprise following according to the raw material of parts by weight meter:
Vinylstyrene 56-60 part
Vinylbenzene 7-9 part
Ethyleneglycol dimethyacrylate 12-18 part
Polystyrene 8-9 part
Diethyl phthalate 57-70 part
No. 200 gasoline 40-45 parts
Diphenyl peroxide base acyl 1.5-1.8 part
Deionized water 170-180 part
Polyvinyl alcohol 1.5-1.9 part.
A preparation method for especially big macroporous adsorbent resin, is characterized in that: comprise following processing step:
A, require to take raw material and fully mix in container according to formula, obtain mixture, then mixture is added in the there-necked flask of a tool plug;
B, start and stir and system oil phase is dispersed into pearl body, then temperature of reaction is raised to 75-80 DEG C, after the pearl body-shaping that oil phase is dispersed into, temperature of reaction is risen to 85 DEG C, then maintain 85 DEG C of reaction 2h, then be warming up to 90 DEG C, reaction 4h;
C, temperature is risen to 92-95 DEG C, reaction 4h, leaches reaction product pearl body, and water repetitive scrubbing is removed pore-creating agent, leaches product and is drying to obtain especially big macroporous adsorbent resin.
The present invention, in step B, described be raised to temperature of reaction 75-80 DEG C and refer to and in 0.5-1h, be raised to 75-80 DEG C.
The present invention is in step C, and the detailed process of described removal pore-creating agent is: reaction product pearl body is removed to pore-creating agent in pore-creating agent extractor, more further remove pore-creating agent in alcohol washer, then water washes away residual alcohol.
The useful technique effect that the present invention brings:
It is large not that the present invention is intended to solve the macroporous adsorbent resin aperture of prior art, the problem that Application Areas is restricted, adopt polystyrene, diethyl phthalate as one of pore-creating agent component, increase the aperture of resin, prepare especially big macroporous adsorbent resin, widened the Application Areas of this resin; The present invention has added the second linking agent, in strengthening resin aperture, has ensured the physical strength of resin, and is provided the work-ing life of resin.
Embodiment
embodiment 1
A kind of especially big macroporous adsorbent resin, comprises following according to the raw material of parts by weight meter:
50 parts of Vinylstyrenes
5 parts of vinylbenzene
10 parts of ethyleneglycol dimethyacrylates
5 parts of polystyrene
50 parts of diethyl phthalates
30 parts, No. 200 gasoline
1 part of diphenyl peroxide base acyl
150 parts of deionized waters
1 part of polyvinyl alcohol.
embodiment 2
A kind of especially big macroporous adsorbent resin, comprises following according to the raw material of parts by weight meter:
70 parts of Vinylstyrenes
10 parts of vinylbenzene
20 parts of ethyleneglycol dimethyacrylates
10 parts of polystyrene
80 parts of diethyl phthalates
50 parts, No. 200 gasoline
2 parts of diphenyl peroxide base acyls
200 parts of deionized waters
2 parts of polyvinyl alcohol.
embodiment 3
A kind of especially big macroporous adsorbent resin, comprises following according to the raw material of parts by weight meter:
60 parts of Vinylstyrenes
7.5 parts of vinylbenzene
15 parts of ethyleneglycol dimethyacrylates
7.5 parts of polystyrene
65 parts of diethyl phthalates
40 parts, No. 200 gasoline
1.5 parts of diphenyl peroxide base acyls
175 parts of deionized waters
1.5 parts of polyvinyl alcohol.
embodiment 4
A kind of especially big macroporous adsorbent resin, comprises following according to the raw material of parts by weight meter:
59 parts of Vinylstyrenes
8.5 parts of vinylbenzene
12 parts of ethyleneglycol dimethyacrylates
8 parts of polystyrene
71 parts of diethyl phthalates
46 parts, No. 200 gasoline
1.25 parts of diphenyl peroxide base acyls
190 parts of deionized waters
1.8 parts of polyvinyl alcohol.
embodiment 5
A kind of especially big macroporous adsorbent resin, comprises following according to the raw material of parts by weight meter:
56 parts of Vinylstyrenes
7 parts of vinylbenzene
12 parts of ethyleneglycol dimethyacrylates
8 parts of polystyrene
57 parts of diethyl phthalates
40 parts, No. 200 gasoline
1.5 parts of diphenyl peroxide base acyls
170 parts of deionized waters
1.5 parts of polyvinyl alcohol.
embodiment 6
A kind of especially big macroporous adsorbent resin, comprises following according to the raw material of parts by weight meter:
60 parts of Vinylstyrenes
9 parts of vinylbenzene
18 parts of ethyleneglycol dimethyacrylates
9 parts of polystyrene
70 parts of diethyl phthalates
45 parts, No. 200 gasoline
1.8 parts of diphenyl peroxide base acyls
180 parts of deionized waters
1.9 parts of polyvinyl alcohol.
embodiment 7
A kind of especially big macroporous adsorbent resin, comprises following according to the raw material of parts by weight meter:
58 parts of Vinylstyrenes
8 parts of vinylbenzene
15 parts of ethyleneglycol dimethyacrylates
8.5 parts of polystyrene
63.5 parts of diethyl phthalates
42.5 parts, No. 200 gasoline
1.65 parts of diphenyl peroxide base acyls
175 parts of deionized waters
1.7 parts of polyvinyl alcohol.
embodiment 8
A kind of especially big macroporous adsorbent resin, comprises following according to the raw material of parts by weight meter:
59 parts of Vinylstyrenes
7.5 parts of vinylbenzene
17 parts of ethyleneglycol dimethyacrylates
8.8 parts of polystyrene
58.5 parts of diethyl phthalates
41.5 parts, No. 200 gasoline
1.7 parts of diphenyl peroxide base acyls
171 parts of deionized waters
1.8 parts of polyvinyl alcohol.
embodiment 9
A preparation method for especially big macroporous adsorbent resin, comprises following processing step:
A, require to take raw material and fully mix in container according to formula, obtain mixture, then mixture is added in the there-necked flask of a tool plug;
B, start and stir and system oil phase is dispersed into pearl body, then temperature of reaction is raised to 75 DEG C, after the pearl body-shaping that oil phase is dispersed into, temperature of reaction is risen to 85 DEG C, then maintain 85 DEG C of reaction 2h, then be warming up to 90 DEG C, reaction 4h;
C, temperature is risen to 92 DEG C, reaction 4h, leaches reaction product pearl body, and water repetitive scrubbing is removed pore-creating agent, leaches product and is drying to obtain especially big macroporous adsorbent resin.
embodiment 10
A preparation method for especially big macroporous adsorbent resin, comprises following processing step:
A, require to take raw material and fully mix in container according to formula, obtain mixture, then mixture is added in the there-necked flask of a tool plug;
B, start and stir and system oil phase is dispersed into pearl body, then temperature of reaction is raised to 80 DEG C, after the pearl body-shaping that oil phase is dispersed into, temperature of reaction is risen to 85 DEG C, then maintain 85 DEG C of reaction 2h, then be warming up to 90 DEG C, reaction 4h;
C, temperature is risen to 95 DEG C, reaction 4h, leaches reaction product pearl body, and water repetitive scrubbing is removed pore-creating agent, leaches product and is drying to obtain especially big macroporous adsorbent resin.
embodiment 11
A preparation method for especially big macroporous adsorbent resin, comprises following processing step:
A, require to take raw material and fully mix in container according to formula, obtain mixture, then mixture is added in the there-necked flask of a tool plug;
B, start and stir and system oil phase is dispersed into pearl body, then temperature of reaction is raised to 77.5 DEG C, after the pearl body-shaping that oil phase is dispersed into, temperature of reaction is risen to 85 DEG C, then maintain 85 DEG C of reaction 2h, then be warming up to 90 DEG C, reaction 4h;
C, temperature is risen to 93.5 DEG C, reaction 4h, leaches reaction product pearl body, and water repetitive scrubbing is removed pore-creating agent, leaches product and is drying to obtain especially big macroporous adsorbent resin.
embodiment 12
A preparation method for especially big macroporous adsorbent resin, comprises following processing step:
A, require to take raw material and fully mix in container according to formula, obtain mixture, then mixture is added in the there-necked flask of a tool plug;
B, start and stir and system oil phase is dispersed into pearl body, then temperature of reaction is raised to 79 DEG C, after the pearl body-shaping that oil phase is dispersed into, temperature of reaction is risen to 85 DEG C, then maintain 85 DEG C of reaction 2h, then be warming up to 90 DEG C, reaction 4h;
C, temperature is risen to 93 DEG C, reaction 4h, leaches reaction product pearl body, and water repetitive scrubbing is removed pore-creating agent, leaches product and is drying to obtain especially big macroporous adsorbent resin.
embodiment 13
On the basis of embodiment 9-12, preferred:
In step B, described temperature of reaction be raised to 75-80 DEG C and refer to and in 0.5h, be raised to 75-80 DEG C.
In step C, the detailed process of described removal pore-creating agent is: reaction product pearl body is removed to pore-creating agent in pore-creating agent extractor, more further remove pore-creating agent in alcohol washer, then water washes away residual alcohol.
embodiment 14
On the basis of embodiment 9-12, preferred:
In step B, described temperature of reaction be raised to 75-80 DEG C and refer to and in 1h, be raised to 75-80 DEG C.
In step C, the detailed process of described removal pore-creating agent is: reaction product pearl body is removed to pore-creating agent in pore-creating agent extractor, more further remove pore-creating agent in alcohol washer, then water washes away residual alcohol.
embodiment 15
On the basis of embodiment 9-12, preferred:
In step B, described temperature of reaction be raised to 75-80 DEG C and refer to and in 0.75h, be raised to 75-80 DEG C.
In step C, the detailed process of described removal pore-creating agent is: reaction product pearl body is removed to pore-creating agent in pore-creating agent extractor, more further remove pore-creating agent in alcohol washer, then water washes away residual alcohol.
embodiment 16
On the basis of embodiment 9-12, preferred:
In step B, described temperature of reaction be raised to 75-80 DEG C and refer to and in 0.8h, be raised to 75-80 DEG C.
In step C, the detailed process of described removal pore-creating agent is: reaction product pearl body is removed to pore-creating agent in pore-creating agent extractor, more further remove pore-creating agent in alcohol washer, then water washes away residual alcohol.
Claims (5)
1. an especially big macroporous adsorbent resin, is characterized in that: comprise following according to the raw material of parts by weight meter:
Vinylstyrene 50-70 part
Vinylbenzene 5-10 part
Ethyleneglycol dimethyacrylate 10-20 part
Polystyrene 5-10 part
Diethyl phthalate 50-80 part
No. 200 gasoline 30-50 parts
Diphenyl peroxide base acyl 1-2 part
Deionized water 150-200 part
Polyvinyl alcohol 1-2 part.
2. the especially big macroporous adsorbent resin of one according to claim 1, is characterized in that: comprise following according to the raw material of parts by weight meter:
Vinylstyrene 56-60 part
Vinylbenzene 7-9 part
Ethyleneglycol dimethyacrylate 12-18 part
Polystyrene 8-9 part
Diethyl phthalate 57-70 part
No. 200 gasoline 40-45 parts
Diphenyl peroxide base acyl 1.5-1.8 part
Deionized water 170-180 part
Polyvinyl alcohol 1.5-1.9 part.
3. the preparation method of a kind of especially big macroporous adsorbent resin according to claim 1 and 2, is characterized in that: comprise following processing step:
A, require to take raw material and fully mix in container according to formula, obtain mixture, then mixture is added in the there-necked flask of a tool plug;
B, start and stir and system oil phase is dispersed into pearl body, then temperature of reaction is raised to 75-80 DEG C, after the pearl body-shaping that oil phase is dispersed into, temperature of reaction is risen to 85 DEG C, then maintain 85 DEG C of reaction 2h, then be warming up to 90 DEG C, reaction 4h;
C, temperature is risen to 92-95 DEG C, reaction 4h, leaches reaction product pearl body, and water repetitive scrubbing is removed pore-creating agent, leaches product and is drying to obtain especially big macroporous adsorbent resin.
4. the preparation method of a kind of especially big macroporous adsorbent resin according to claim 3, is characterized in that: in step B, described temperature of reaction be raised to 75-80 DEG C and refer to and in 0.5-1h, be raised to 75-80 DEG C.
5. the preparation method of a kind of especially big macroporous adsorbent resin according to claim 3, it is characterized in that: in step C, the detailed process of described removal pore-creating agent is: reaction product pearl body is removed to pore-creating agent in pore-creating agent extractor, in alcohol washer, further remove pore-creating agent, then water washes away residual alcohol again.
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| CN201410251408.6A CN104059187B (en) | 2014-06-09 | 2014-06-09 | A kind of especially big macroporous adsorbent resin and preparation method thereof |
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| CN104059187B CN104059187B (en) | 2016-08-31 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107051410A (en) * | 2017-05-26 | 2017-08-18 | 辽宁科技学院 | A kind of macroporous absorbent resin and preparation method thereof |
| CN107266622A (en) * | 2017-06-27 | 2017-10-20 | 郑泽 | Macroporous absorbent resin of larger molecular weight organic matter and preparation method thereof in a kind of removal waste water |
| CN115044094A (en) * | 2022-06-22 | 2022-09-13 | 湖北工业大学 | Super absorbent resin with sponge structure and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07196752A (en) * | 1993-12-28 | 1995-08-01 | Japan Synthetic Rubber Co Ltd | Modification of crosslinked polymer particles |
| CN1927899A (en) * | 2006-09-01 | 2007-03-14 | 烟台硕德新材料有限公司 | Preparation method of micron-sized monodisperse copolymerized microspheres |
-
2014
- 2014-06-09 CN CN201410251408.6A patent/CN104059187B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07196752A (en) * | 1993-12-28 | 1995-08-01 | Japan Synthetic Rubber Co Ltd | Modification of crosslinked polymer particles |
| CN1927899A (en) * | 2006-09-01 | 2007-03-14 | 烟台硕德新材料有限公司 | Preparation method of micron-sized monodisperse copolymerized microspheres |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107051410A (en) * | 2017-05-26 | 2017-08-18 | 辽宁科技学院 | A kind of macroporous absorbent resin and preparation method thereof |
| CN107266622A (en) * | 2017-06-27 | 2017-10-20 | 郑泽 | Macroporous absorbent resin of larger molecular weight organic matter and preparation method thereof in a kind of removal waste water |
| CN115044094A (en) * | 2022-06-22 | 2022-09-13 | 湖北工业大学 | Super absorbent resin with sponge structure and preparation method thereof |
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