CN105273138B - A kind of adsorbent resin with ultra-high specific surface area and preparation method thereof - Google Patents
A kind of adsorbent resin with ultra-high specific surface area and preparation method thereof Download PDFInfo
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Abstract
The present invention discloses a kind of adsorbent resin with ultra-high specific surface area and preparation method thereof, including the component of following mass fraction:30 40 parts of styrene, 10 15 parts of acrylic acid methyl ester., 0.5 1 parts of composite pore-forming, 10 12 parts of initiator and 15 parts of catalyst.The present invention adopts low-temperature catalyzed scion grafting synthesis and secondary suspension copolymerization technology, and ratio produces plain edition acrylic resin energy-conservation more than 30%.Using composite pore-forming, improve specific surface area and the exchange capacity of adsorbent resin, enhance the mechanical strength of resin, extend the usage cycles of resin, chemical stability is good.On the other hand, preferably improve the contamination resistance of resin, decrease the discharging of waste liquid causing because of resin regeneration, environmental protection.
Description
Technical field
The invention belongs to technical field of polymer chemistry is and in particular to a kind of adsorbent resin with ultra-high specific surface area and its preparation
Method.
Background technology
In recent years, porous organic material is due to having the advantages that big specific surface area, low skeletal density and multiformity,
People are caused widely to study.It is because adsorbance is higher, easy desorption and regeneration and selectivity good the features such as, have very in adsorbing domain
Big application prospect.Conventional propylene acid resin is little due to there is specific surface area, broken, unstable properties, anti-organic contamination energy
The shortcomings of power difference, during production and use, resin chips or organic residue are easily mixed in treated object, cause secondary dirt
Dye is it is impossible to meet the use requirement of user.
The synthetic method of Porous-Organic adsorbent mainly has suspension polymerization, phase separation method, hard template method, additional friendship at present
Connection method etc., but these methods exist and have to synthon that certain restriction or synthesis technique are complicated, reaction cost is higher etc. and lack
Point.Document CN101987291A discloses a kind of new superhigh cross-linking macroporous adsorbent resin of base containing diketone and preparation method thereof, should
Invention with styrene as monomer, with multi-vinyl monomer as cross-linking agent, porogen exist under conditions of suspension polymerisation obtain white
Ball, gained Archon and paraphthaloyl chloride carry out Friedel-Crafts acylation reaction, gained resin in the presence of a catalyst
It is the new macroporous adsorbent resin containing diketone base superhigh cross-linking, the adsorbent resin being obtained has high mechanical strength, compares table
Area is big, and containing series of advantages such as ketone group polar groups, but synthetic method is complex, and the response time is long, and efficiency is low.
Document CN102527352A discloses a kind of system of the macroporous adsorbent resin for adsorbing and desulfurizing catalytic cracking gasoline
Preparation Method, takes skeleton raw material, polymerized monomer, initiator, cross-linking agent, perforating agent, dispersant is added in deionized water, fills respectively
Divide mix and blend, be warming up to reaction temperature 70-80 DEG C, react 2.5-3.5 hour, polyreaction terminates, the aqueous phase that reaction produces
After suspension polymer solid-liquid separation, solid phase, with 75-85 DEG C of water, is washed 3-5 time, is obtained milky spherical particle, milky white chromosphere
Shape granule deionized water at normal temperature cleans removal reaction residue, is washed with ethanol after washing, removes perforating agent toluene, is washed with water
Go residual ethanol, in 65 DEG C of constant temperature ovens drying, cross 30-50 mesh sieve, this invention desulfurization degree is high, easily, repeating makes for dissociation
With having saved cost.Document CN103483474A discloses a kind of preparation method of macropore weak base anion resins, its preparation side
Method includes polymerization stage, obtains Archon by getting the raw materials ready, stirring, heat up, react;In the chlorination reaction stage, Archon is put into chlorine
Change in reactor, obtain chlorine ball by adding the reaction such as chlorinated ether, zinc chloride;With the aminating reaction stage, by chlorine ball and dimethylamine
Water aminating reaction obtains macropore weak base anion resins.The macropore weak base anion resins that this invention is obtained not only increase resin
Mechanical strength, extend the service life of resin, and specific surface area be bigger, uniform pore diameter, the exchange that improve resin is held
Amount and contamination resistance, and reduce production cost, improve the economic benefit of product.But the preparation temperature of the method is relatively
Height, and the resin specific surface area of its preparation is relatively low, limits it and extensively applies.
Content of the invention
The purpose of the present invention is that to there is specific surface area for acrylic resin in prior art little, and broken, performance is not
Stable, anti-organic the problems such as stain ability, provide that a kind of exchange capacity is big, high mechanical strength, resistant to pollution super large specific surface
Long-pending adsorbent resin and preparation method thereof.
For achieving the above object, the present invention carries out technical scheme below:
A kind of adsorbent resin with ultra-high specific surface area, including the component of following mass fraction:
Styrene 30-40 part,
Acrylic acid methyl ester. 10-15 part,
Composite pore-forming 0.5-1 part,
Initiator 10-12 part,
Catalyst 1-5 part.
Preferably, described composite pore-forming is the mixture of methyl cyclopropane and methylisobutylketone, and the mass ratio of the two is
1-3:1.
Preferably, described catalyst is one or two of iron chloride and zinc chloride.
Preferably, described initiator is peroxidating phenyl-diformyl.
A kind of preparation method of adsorbent resin with ultra-high specific surface area, comprises the following steps:
(1)The aqueous solution of sodium chloride is added in reactor, is warming up to 45 DEG C;By styrene, acrylic acid methyl ester, compound cause
The raw material of hole agent, initiator and catalyst composition, in 45 DEG C of stirring mixing 10-15min, adds in aforesaid reaction vessel, stirring is all
Even, it is warming up to 65 DEG C with the speed of 2-3 DEG C/min, is incubated 3-4 hour, then rises to 80 DEG C with the speed of 1 DEG C/min, be incubated 3-
5 hours, then lower the temperature and obtain Archon;
(2)Archon in reactor is put into cleaning in Material-washing kettle, is re-fed into drying in drying machine, after drying, filters out grain
Spend qualified Archon;
(3)To step(2)Add appropriate styrene and acrylic acid methyl ester. in the Archon obtaining, stir 30min, add appropriate
Composite pore-forming, initiator and catalyst, in 45 DEG C of stirring mixing 10-15min, obtain mixed material;Add chlorine in a kettle.
Change after sodium solution is warming up to 45 DEG C and add described mixed material, stir, be warming up to 65 DEG C with the speed of 2-3 DEG C/min, protect
Warm 3-4 hour, then rises to 80 DEG C with the speed of 1 DEG C/min, is incubated 3-5 hour, obtains resin balls after cooling;
(4)Using ethanol by step(3)The resin balls cleaning obtaining, is then washed, and is re-fed into drying in drying machine,
Adsorbent resin with ultra-high specific surface area is obtained after drying.
Preferably, the concentration of described sodium chloride is 6-10wt%.
Preferably, the concentration of described sodium chloride is 8wt%.
Preferably, described step(1)Middle raw material is 1 with the mass ratio of sodium-chloride water solution:5-7.
Preferably, described step(3)The quality of middle styrene and acrylic acid methyl ester. is step(2)The Archon quality obtaining
20-35%.
Preferably, described step(3)Middle styrene, acrylic acid methyl ester, composite pore-forming, initiator and catalyst quality ratio
With described step(1)In identical.
Preferably, described step(3)Middle styrene, acrylic acid methyl ester, the quality of composite pore-forming, initiator and catalyst
Mass ratio with sodium-chloride water solution is 1:5-7.
The present invention adopts low-temperature catalyzed scion grafting synthesis and secondary suspension copolymerization technology, and ratio produces plain edition acrylic resin
Energy-conservation more than 30%.Using composite pore-forming, improve specific surface area and the exchange capacity of adsorbent resin, enhance the machine of resin
Tool intensity, extends the usage cycles of resin, and chemical stability is good.On the other hand, preferably improve the contamination resistance of resin,
Decrease the discharging of waste liquid causing because of resin regeneration, environmental protection.
Adsorbent resin with ultra-high specific surface area prepared by the present invention has advantages below:(1)Specific surface area is big, 1400m2/
G,(2)There is excellent anti-organic contamination ability, do not result in secondary pollution;(3)High mechanical strength, not broken, application is wide
General.
Specific embodiment
Embodiment 1
A kind of adsorbent resin with ultra-high specific surface area, including the component of following mass fraction:
36 parts of styrene,
12 parts of acrylic acid methyl ester.,
0.6 part of composite pore-forming,
11 parts of initiator,
3 parts of catalyst.
Described composite pore-forming is the mixture of methyl cyclopropane and methylisobutylketone, and the mass ratio of the two is 2:1.
Described catalyst is the mixture of iron chloride and zinc chloride, and the mass ratio of the two is 1:1.
Described initiator is peroxidating phenyl-diformyl.
The preparation method of described adsorbent resin with ultra-high specific surface area, comprises the following steps:
(1)The aqueous solution of sodium chloride is added in reactor, is warming up to 45 DEG C;By styrene, acrylic acid methyl ester, compound cause
The raw material of hole agent, initiator and catalyst composition, in 45 DEG C of stirring mixing 10-15min, adds in aforesaid reaction vessel, stirring is all
Even, it is warming up to 65 DEG C with the speed of 2-3 DEG C/min, is incubated 3-4 hour, then rises to 80 DEG C with the speed of 1 DEG C/min, be incubated 3-
5 hours, then lower the temperature and obtain Archon;
(2)Archon in reactor is put into cleaning in Material-washing kettle, is re-fed into drying in drying machine, after drying, filters out grain
Spend qualified Archon;
(3)To step(2)Add appropriate styrene and acrylic acid methyl ester. in the Archon obtaining, stir 30min, add appropriate
Composite pore-forming, initiator and catalyst, in 45 DEG C of stirring mixing 10-15min, obtain mixed material;Add chlorine in a kettle.
Change after sodium solution is warming up to 45 DEG C and add described mixed material, stir, be warming up to 65 DEG C with the speed of 2-3 DEG C/min, protect
Warm 3-4 hour, then rises to 80 DEG C with the speed of 1 DEG C/min, is incubated 3-5 hour, obtains resin balls after cooling;
(4)Using ethanol by step(3)The resin balls cleaning obtaining, is then washed, and is re-fed into drying in drying machine,
Adsorbent resin with ultra-high specific surface area is obtained after drying.
The concentration of described sodium chloride is 8wt%.
Described step(1)Middle raw material is 1 with the mass ratio of sodium-chloride water solution:6.
Described step(3)The quality of middle styrene and acrylic acid methyl ester. is step(2)The 30% of the Archon quality obtaining.
Described step(3)Middle styrene, acrylic acid methyl ester, composite pore-forming, initiator and catalyst quality than with described
Step(1)In identical.
Described step(3)Middle styrene, acrylic acid methyl ester, the quality of composite pore-forming, initiator and catalyst and chlorination
The mass ratio of sodium water solution is 1:6.
Embodiment 2
A kind of adsorbent resin with ultra-high specific surface area, including the component of following mass fraction:
30 parts of styrene
15 parts of acrylic acid methyl ester.
0.5 part of composite pore-forming
10 parts of initiator
1 part of catalyst
Described composite pore-forming is the mixture of methyl cyclopropane and methylisobutylketone, and the mass ratio of the two is 1:1.
Described catalyst is zinc chloride.
Described initiator is peroxidating phenyl-diformyl.
Make following preparation according to above proportioning, comprise the following steps:
(1)The aqueous solution of sodium chloride is added in reactor, is warming up to 45 DEG C;By styrene, acrylic acid methyl ester, compound cause
The raw material of hole agent, initiator and catalyst composition, in 45 DEG C of stirring mixing 10-15min, adds in aforesaid reaction vessel, stirring is all
Even, it is warming up to 65 DEG C with the speed of 2-3 DEG C/min, is incubated 3-4 hour, then rises to 80 DEG C with the speed of 1 DEG C/min, be incubated 3-
5 hours, then lower the temperature and obtain Archon;
(2)Archon in reactor is put into cleaning in Material-washing kettle, is re-fed into drying in drying machine, after drying, filters out grain
Spend qualified Archon;
(3)To step(2)Add appropriate styrene and acrylic acid methyl ester. in the Archon obtaining, stir 30min, add appropriate
Composite pore-forming, initiator and catalyst, in 45 DEG C of stirring mixing 10-15min, obtain mixed material;Add chlorine in a kettle.
Change after sodium solution is warming up to 45 DEG C and add described mixed material, stir, be warming up to 65 DEG C with the speed of 2-3 DEG C/min, protect
Warm 3-4 hour, then rises to 80 DEG C with the speed of 1 DEG C/min, is incubated 3-5 hour, obtains resin balls after cooling;
(4)Using ethanol by step(3)The resin balls cleaning obtaining, is then washed, and is re-fed into drying in drying machine,
Adsorbent resin with ultra-high specific surface area is obtained after drying.
The concentration of described sodium chloride is 6wt%.
Described step(1)Middle raw material is 1 with the mass ratio of sodium-chloride water solution:5.
Described step(3)The quality of middle styrene and acrylic acid methyl ester. is step(2)The 35% of the Archon quality obtaining.
Described step(3)Middle styrene, acrylic acid methyl ester, composite pore-forming, initiator and catalyst quality than with described
Step(1)In identical.
Described step(3)Middle styrene, acrylic acid methyl ester, the quality of composite pore-forming, initiator and catalyst and chlorination
The mass ratio of sodium water solution is 1:5.
Embodiment 3
A kind of adsorbent resin with ultra-high specific surface area, including the component of following mass fraction:
40 parts of styrene
10 parts of acrylic acid methyl ester.
1 part of composite pore-forming
12 parts of initiator
5 parts of catalyst
Described composite pore-forming is the mixture of methyl cyclopropane and methylisobutylketone, and the mass ratio of the two is 3:1.
Described catalyst is iron chloride.
Described initiator is peroxidating phenyl-diformyl.
Make following preparation according to above proportioning, comprise the following steps:
(1)The aqueous solution of sodium chloride is added in reactor, is warming up to 45 DEG C;By styrene, acrylic acid methyl ester, compound cause
The raw material of hole agent, initiator and catalyst composition, in 45 DEG C of stirring mixing 10-15min, adds in aforesaid reaction vessel, stirring is all
Even, it is warming up to 65 DEG C with the speed of 2-3 DEG C/min, is incubated 3-4 hour, then rises to 80 DEG C with the speed of 1 DEG C/min, be incubated 3-
5 hours, then lower the temperature and obtain Archon;
(2)Archon in reactor is put into cleaning in Material-washing kettle, is re-fed into drying in drying machine, after drying, filters out grain
Spend qualified Archon;
(3)To step(2)Add appropriate styrene and acrylic acid methyl ester. in the Archon obtaining, stir 30min, add appropriate
Composite pore-forming, initiator and catalyst, in 45 DEG C of stirring mixing 10-15min, obtain mixed material;Add chlorine in a kettle.
Change after sodium solution is warming up to 45 DEG C and add described mixed material, stir, be warming up to 65 DEG C with the speed of 2-3 DEG C/min, protect
Warm 3-4 hour, then rises to 80 DEG C with the speed of 1 DEG C/min, is incubated 3-5 hour, obtains resin balls after cooling;
(4)Using ethanol by step(3)The resin balls cleaning obtaining, is then washed, and is re-fed into drying in drying machine,
Adsorbent resin with ultra-high specific surface area is obtained after drying.
The concentration of described sodium chloride is 10wt%.
Described step(1)Middle raw material is 1 with the mass ratio of sodium-chloride water solution:7.
Described step(3)The quality of middle styrene and acrylic acid methyl ester. is step(2)The 20% of the Archon quality obtaining.
Described step(3)Middle styrene, acrylic acid methyl ester, composite pore-forming, initiator and catalyst quality than with described
Step(1)In identical.
Described step(3)Middle styrene, acrylic acid methyl ester, the quality of composite pore-forming, initiator and catalyst and chlorination
The mass ratio of sodium water solution is 1:7.
Embodiment 4
A kind of adsorbent resin with ultra-high specific surface area, including the component of following mass fraction:
36 parts of styrene,
12 parts of acrylic acid methyl ester.,
0.6 part of composite pore-forming,
11 parts of initiator,
3 parts of catalyst.
Described composite pore-forming is the mixture of methyl cyclopropane and methylisobutylketone, and the mass ratio of the two is 1:3.
Described catalyst is the mixture of iron chloride and zinc chloride, and the mass ratio of the two is 1:1.
Described initiator is peroxidating phenyl-diformyl.
The preparation method of described adsorbent resin with ultra-high specific surface area, comprises the following steps:
(1)The aqueous solution of sodium chloride is added in reactor, is warming up to 45 DEG C;By styrene, acrylic acid methyl ester, compound cause
The raw material of hole agent, initiator and catalyst composition, in 45 DEG C of stirring mixing 10-15min, adds in aforesaid reaction vessel, stirring is all
Even, it is warming up to 65 DEG C with the speed of 2-3 DEG C/min, is incubated 3-4 hour, then rises to 80 DEG C with the speed of 1 DEG C/min, be incubated 3-
5 hours, then lower the temperature and obtain Archon;
(2)Archon in reactor is put into cleaning in Material-washing kettle, is re-fed into drying in drying machine, after drying, filters out grain
Spend qualified Archon;
(3)To step(2)Add appropriate styrene and acrylic acid methyl ester. in the Archon obtaining, stir 30min, add appropriate
Composite pore-forming, initiator and catalyst, in 45 DEG C of stirring mixing 10-15min, obtain mixed material;Add chlorine in a kettle.
Change after sodium solution is warming up to 45 DEG C and add described mixed material, stir, be warming up to 65 DEG C with the speed of 2-3 DEG C/min, protect
Warm 3-4 hour, then rises to 80 DEG C with the speed of 1 DEG C/min, is incubated 3-5 hour, obtains resin balls after cooling;
(4)Using ethanol by step(3)The resin balls cleaning obtaining, is then washed, and is re-fed into drying in drying machine,
Adsorbent resin is obtained after drying.
The concentration of described sodium chloride is 8wt%.
Described step(1)Middle raw material is 1 with the mass ratio of sodium-chloride water solution:6.
Described step(3)The quality of middle styrene and acrylic acid methyl ester. is step(2)The 30% of the Archon quality obtaining.
Described step(3)Middle styrene, acrylic acid methyl ester, composite pore-forming, initiator and catalyst quality than with described
Step(1)In identical.
Described step(3)Middle styrene, acrylic acid methyl ester, the quality of composite pore-forming, initiator and catalyst and chlorination
The mass ratio of sodium water solution is 1:6.
Embodiment 5
A kind of adsorbent resin with ultra-high specific surface area, including the component of following mass fraction:
36 parts of styrene,
12 parts of acrylic acid methyl ester.,
0.6 part of porogen,
11 parts of initiator,
3 parts of catalyst.
Described porogen is methyl cyclopropane.
Described catalyst is the mixture of iron chloride and zinc chloride, and the mass ratio of the two is 1:1.
Described initiator is peroxidating phenyl-diformyl.
The preparation method of described adsorbent resin with ultra-high specific surface area, comprises the following steps:
(1)The aqueous solution of sodium chloride is added in reactor, is warming up to 45 DEG C;By styrene, acrylic acid methyl ester, compound cause
The raw material of hole agent, initiator and catalyst composition, in 45 DEG C of stirring mixing 10-15min, adds in aforesaid reaction vessel, stirring is all
Even, it is warming up to 65 DEG C with the speed of 2-3 DEG C/min, is incubated 3-4 hour, then rises to 80 DEG C with the speed of 1 DEG C/min, be incubated 3-
5 hours, then lower the temperature and obtain Archon;
(2)Archon in reactor is put into cleaning in Material-washing kettle, is re-fed into drying in drying machine, after drying, filters out grain
Spend qualified Archon;
(3)To step(2)Add appropriate styrene and acrylic acid methyl ester. in the Archon obtaining, stir 30min, add appropriate
Composite pore-forming, initiator and catalyst, in 45 DEG C of stirring mixing 10-15min, obtain mixed material;Add chlorine in a kettle.
Change after sodium solution is warming up to 45 DEG C and add described mixed material, stir, be warming up to 65 DEG C with the speed of 2-3 DEG C/min, protect
Warm 3-4 hour, then rises to 80 DEG C with the speed of 1 DEG C/min, is incubated 3-5 hour, obtains resin balls after cooling;
(4)Using ethanol by step(3)The resin balls cleaning obtaining, is then washed, and is re-fed into drying in drying machine,
Adsorbent resin is obtained after drying.
The concentration of described sodium chloride is 8wt%.
Described step(1)Middle raw material is 1 with the mass ratio of sodium-chloride water solution:6.
Described step(3)The quality of middle styrene and acrylic acid methyl ester. is step(2)The 30% of the Archon quality obtaining.
Described step(3)Middle styrene, acrylic acid methyl ester, composite pore-forming, initiator and catalyst quality than with described
Step(1)In identical.
Described step(3)Middle styrene, acrylic acid methyl ester, the quality of composite pore-forming, initiator and catalyst and chlorination
The mass ratio of sodium water solution is 1:6.
Embodiment 6
A kind of adsorbent resin with ultra-high specific surface area, including the component of following mass fraction:
36 parts of styrene,
5 parts of acrylic acid methyl ester.,
0.2 part of composite pore-forming,
11 parts of initiator,
3 parts of catalyst.
Described composite pore-forming is the mixture of methyl cyclopropane and methylisobutylketone, and the mass ratio of the two is 2:1.
Described catalyst is iron chloride.
Described initiator is peroxidating phenyl-diformyl.
The preparation method of described adsorbent resin with ultra-high specific surface area, comprises the following steps:
(1)The aqueous solution of sodium chloride is added in reactor, is warming up to 45 DEG C;By styrene, acrylic acid methyl ester, compound cause
The raw material of hole agent, initiator and catalyst composition, in 45 DEG C of stirring mixing 10-15min, adds in aforesaid reaction vessel, stirring is all
Even, it is warming up to 65 DEG C with the speed of 2-3 DEG C/min, is incubated 3-4 hour, then rises to 80 DEG C with the speed of 1 DEG C/min, be incubated 3-
5 hours, then lower the temperature and obtain Archon;
(2)Archon in reactor is put into cleaning in Material-washing kettle, is re-fed into drying in drying machine, after drying, filters out grain
Spend qualified Archon;
(3)To step(2)Add appropriate styrene and acrylic acid methyl ester. in the Archon obtaining, stir 30min, add appropriate
Composite pore-forming, initiator and catalyst, in 45 DEG C of stirring mixing 10-15min, obtain mixed material;Add chlorine in a kettle.
Change after sodium solution is warming up to 45 DEG C and add described mixed material, stir, be warming up to 65 DEG C with the speed of 2-3 DEG C/min, protect
Warm 3-4 hour, then rises to 80 DEG C with the speed of 1 DEG C/min, is incubated 3-5 hour, obtains resin balls after cooling;
(4)Using ethanol by step(3)The resin balls cleaning obtaining, is then washed, and is re-fed into drying in drying machine,
Adsorbent resin is obtained after drying.
Described step(1)Middle raw material is 1 with the mass ratio of water:6.
Described step(3)The quality of middle styrene and acrylic acid methyl ester. is step(2)The 30% of the Archon quality obtaining.
Described step(3)Middle styrene, acrylic acid methyl ester, composite pore-forming, initiator and catalyst quality than with described
Step(1)In identical.
Described step(3)Middle styrene, acrylic acid methyl ester, the quality of composite pore-forming, initiator and catalyst and water
Mass ratio is 1:10.
Performance test is carried out to the adsorbent resin prepared by embodiment 1-6, test result is listed in Table 1 below.
The performance data of table 1 adsorbent resin
As known from Table 1, the performance of the adsorbent resin prepared by embodiments of the invention 1-3 is significantly better than embodiment 4-6 institute
The adsorbent resin of preparation, the specific surface area of adsorbent resin reaches 1400m2/ g, pore volume and average pore size are also apparently higher than embodiment
4-6.So the adsorbent resin prepared by the application has more excellent performance, each component proportion of adsorbent resin, and compound pore
Agent has important impact to the performance of adsorbent resin.
A kind of adsorbent resin with ultra-high specific surface area above embodiment of the present invention being provided and preparation method thereof, is carried out
It is discussed in detail, specific case used herein is set forth to the principle of the present invention and embodiment, above example
Illustrate that being only intended to help understands the method for the present invention and its core concept;Simultaneously for one of ordinary skill in the art, according to
According to the thought of the present invention, all will change in specific embodiments and applications, in sum, this specification content
Should not be construed as limitation of the present invention.
Claims (5)
1. a kind of adsorbent resin with ultra-high specific surface area is it is characterised in that be obtained by the component reaction including following mass fraction:
Styrene 30-40 part,
Acrylic acid methyl ester. 10-15 part,
Composite pore-forming 0.5-1 part,
Initiator 10-12 part,
Catalyst 1-5 part;
Described composite pore-forming is the mixture of methyl cyclopropane and methylisobutylketone, and the mass ratio of the two is 1-3:1;
The preparation method of described adsorbent resin, comprises the following steps:
(1)The aqueous solution of sodium chloride is added in reactor, is warming up to 45 DEG C;By styrene, acrylic acid methyl ester., compound pore
The raw material of agent, initiator and catalyst composition, in 45 DEG C of stirring mixing 10-15min, adds in aforesaid reaction vessel, stirs,
It is warming up to 65 DEG C with the speed of 2-3 DEG C/min, is incubated 3-4 hour, then rises to 80 DEG C with the speed of 1 DEG C/min, 3-5 is little for insulation
When, then lower the temperature and obtain Archon;
(2)Archon in reactor is put into cleaning in Material-washing kettle, is re-fed into drying in drying machine, filter out granularity after drying and close
The Archon of lattice;
(3)To step(2)Addition styrene and acrylic acid methyl ester. in the Archon obtaining, stirring 30min, addition composite pore-forming,
Initiator and catalyst, in 45 DEG C of stirring mixing 10-15min, obtain mixed material;Add sodium chloride solution liter in a kettle.
Temperature adds described mixed material to after 45 DEG C, stirs, is warming up to 65 DEG C with the speed of 2-3 DEG C/min, is incubated 3-4 hour,
Then rise to 80 DEG C with the speed of 1 DEG C/min, be incubated 3-5 hour, after cooling, obtain resin balls;
Wherein, described step(3)The quality of middle styrene and acrylic acid methyl ester. is step(2)The 20- of the Archon quality obtaining
35%;
Described step(3)Middle styrene, acrylic acid methyl ester., composite pore-forming, initiator and catalyst quality than with described step
(1)In identical;
Described step(3)The quality of middle styrene, acrylic acid methyl ester., composite pore-forming, initiator and catalyst and sodium chloride water
The mass ratio of solution is 1:5-7;
(4)Using ethanol by step(3)The resin balls cleaning obtaining, is then washed, and is re-fed into drying in drying machine, dries
Obtain adsorbent resin with ultra-high specific surface area afterwards.
2. adsorbent resin according to claim 1 is it is characterised in that described catalyst is one kind of iron chloride and zinc chloride
Or two kinds.
3. adsorbent resin according to claim 1 is it is characterised in that described initiator is peroxidating phenyl-diformyl.
4. adsorbent resin according to claim 1 is it is characterised in that the concentration of described sodium chloride is 6-10wt%.
5. adsorbent resin according to claim 1 is it is characterised in that described step(1)Middle raw material and sodium-chloride water solution
Mass ratio be 1:5-7.
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CN100390211C (en) * | 2006-11-11 | 2008-05-28 | 南开大学 | High polarity polystyrene adsorption resin preparation method and its uses in separating bocconine |
CN101200515A (en) * | 2007-11-30 | 2008-06-18 | 天津市中宝制药有限公司 | Weak-polar macroporous adsorption resin and method for synthesizing the same |
CN101255218B (en) * | 2007-12-18 | 2010-06-30 | 兰州理工大学 | Method for preparing adsorption resin |
CN102702412A (en) * | 2012-06-27 | 2012-10-03 | 淄博东大弘方化工有限公司 | Preparation technology of selective resin for removing trace nitrate ion in water |
CN103772578A (en) * | 2014-01-07 | 2014-05-07 | 中国农业科学院特产研究所 | Method of removing procymidone residue in ginseng and American ginseng extracts by resin method |
CN103772573B (en) * | 2014-02-24 | 2016-08-17 | 艾美科健(中国)生物医药有限公司 | A kind of superhigh cross-linking macroporous adsorbent resin being applicable to clavacin removing |
CN104231149B (en) * | 2014-08-15 | 2016-08-24 | 太仓康盛化工有限公司 | A kind of porous micro-capsule adsorptive resin and preparation method thereof |
CN104788599B (en) * | 2015-03-27 | 2018-03-30 | 徐州浩通新材料科技股份有限公司 | A kind of preparation method of macroporous weakly basic anion exchange resin |
CN104888738A (en) * | 2015-05-26 | 2015-09-09 | 安徽皖东树脂科技有限公司 | Preparation method of adsorbent resin |
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