CN105273138A - Super-large specific surface area adsorbent resin and preparation method thereof - Google Patents
Super-large specific surface area adsorbent resin and preparation method thereof Download PDFInfo
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Abstract
The invention discloses super-large specific surface area adsorbent resin and a preparation method thereof. The super-large specific surface area adsorbent resin comprises the following components in parts by mass: 30-40 parts of styrene, 10-15 parts of methyl acrylate, 0.5-1 part of a composite pore-foaming agent, 10-12 parts of an initiator and 1-5 parts of a catalyst. By using low-temperature catalysis grafting synthesis and secondary suspension copolymerization techniques, more than or equal to 30% of energy can be saved when being compared with that for producing ordinary acrylic acid series resin. By using the composite pore-foaming agent, the specific surface area and the exchange capacity of adsorbent resin can be increased, the mechanical strength of resin is improved, the service life of resin is prolonged, and the chemical stability is good; on the other hand, the contamination resistance of resin is well improved, waste liquid discharge caused by regeneration of resin is reduced, and the environment can be protected.
Description
Technical field
The invention belongs to technical field of polymer chemistry, be specifically related to a kind of adsorbent resin with ultra-high specific surface area and preparation method thereof.
Background technology
In recent years, porous organic material, owing to having the advantages such as large specific surface area, low skeletal density and diversity, causes people to study widely.It, because of higher, the easy desorption and regeneration of adsorptive capacity and the feature such as selectivity is good, has very large application prospect in adsorbing domain.Conventional propylene acid resin is little owing to there is specific surface area, the shortcomings such as easy fragmentation, unstable properties, anti-organic contamination ability, in the process of producing and use, resin chips or organic residue are easily mixed in treated object, cause secondary pollution, the service requirements of user can not be met.
The synthetic method of current Porous-Organic sorbent material mainly contains suspension polymerization, phase separation method, hard template method, additive-crosslinking method etc., but these methods exist and have the shortcomings such as certain restriction or synthesis technique are complicated, reaction cost is higher to synthon.Document CN101987291A discloses a kind of novel containing diketone base superhigh cross-linking macroporous adsorbent resin and preparation method thereof, this invention take vinylbenzene as monomer, take multi-vinyl monomer as linking agent, Archon is obtained in the polymerization of pore-creating agent existent condition low suspension, gained Archon and p-phthaloyl chloride carry out Friedel-Crafts acylation reaction in the presence of a catalyst, gained resin is the novel macroporous adsorbent resin containing diketone base superhigh cross-linking, it is high that the polymeric adsorbent obtained has physical strength, specific surface area is large, containing series of advantages such as ketone group polar groups, but synthetic method is comparatively complicated, long reaction time, efficiency is low.
Document CN102527352A discloses a kind of preparation method of the macroporous adsorbent resin for adsorbing and desulfurizing catalytic cracking gasoline, get skeleton raw material respectively, polymerization single polymerization monomer, initiator, linking agent, perforating agent, dispersion agent joins in deionized water, abundant mix and blend, be warming up to temperature of reaction 70-80 DEG C, reaction 2.5-3.5 hour, polyreaction terminates, after the aqueous suspension polymerization thing solid-liquid separation that reaction produces, the solid phase water of 75-85 DEG C, wash 3-5 time, obtain oyster white spherical particle, reaction residue is removed in the deionized water at normal temperature cleaning of oyster white spherical particle, wash with ethanol after washing, remove perforating agent toluene, wash residual ethanol with water again, dry at the constant temperature ovens of 65 DEG C, cross 30-50 mesh sieve, this invention desulfurization degree is high, dissociate easily, reusable, save cost.Document CN103483474A discloses a kind of preparation method of macropore weak base anion resins, and its preparation method comprises polymerization stage, by getting the raw materials ready, stirring, heat up, be obtained by reacting Archon; In the chlorination reaction stage, Archon being put into chlorinating container, being obtained by reacting chlorine ball by adding chlorinated ether, zinc chloride etc.; With the amination reaction stage, chlorine ball and dimethylamine water amination reaction are obtained macropore weak base anion resins.The macropore weak base anion resins that this invention obtains not only increases the physical strength of resin, extend the work-ing life of resin, and specific surface area is larger, uniform pore diameter, improves exchange capacity and the contamination resistance of resin, and reduce production cost, improve the economic benefit of product.But the preparation temperature of the method is higher, and its resin specific surface area prepared is lower, limits its widespread use.
Summary of the invention
The object of the invention is to there is specific surface area for acrylic resin in prior art little, easy fragmentation, unstable properties, anti-organicly stain the problems such as ability, provide that a kind of exchange capacity is large, physical strength is high, resistant to pollution adsorbent resin with ultra-high specific surface area and preparation method thereof.
For achieving the above object, the present invention carries out following technical scheme:
A kind of adsorbent resin with ultra-high specific surface area, comprises the component of following mass fraction:
Vinylbenzene 30-40 part,
Methyl acrylate 10-15 part,
Composite pore-forming 0.5-1 part,
Initiator 10-12 part,
Catalyzer 1-5 part.
Preferably, described composite pore-forming is the mixture of methyl cyclopropane and mibk, and the mass ratio of the two is 1-3:1.
Preferably, described catalyzer is one or both of iron(ic) chloride and zinc chloride.
Preferably, described initiator is peroxidation phenyl-diformyl.
A preparation method for adsorbent resin with ultra-high specific surface area, comprises the following steps:
(1) aqueous solution of sodium-chlor is added in reactor, be warming up to 45 DEG C; The raw material that vinylbenzene, acrylic acid methyl esters, composite pore-forming, initiator and catalyzer form is uniformly mixed 10-15min at 45 DEG C, add in aforesaid reaction vessel, stir, 65 DEG C are warming up to the speed of 2-3 DEG C/min, insulation 3-4 hour, then rise to 80 DEG C with the speed of 1 DEG C/min, insulation 3-5 hour, then cooling obtains Archon;
(2) Archon in reactor is put into wash in material still and cleans, then send in drying machine and dry, after oven dry, filter out the Archon that granularity is qualified;
(3) add appropriate vinylbenzene and methyl acrylate in the Archon obtained to step (2), stir 30min, add appropriate composite pore-forming, initiator and catalyzer and be uniformly mixed 10-15min at 45 DEG C, obtain mixing raw material; Add in a kettle. after sodium chloride solution is warming up to 45 DEG C and add described mixing raw material, stir, be warming up to 65 DEG C with the speed of 2-3 DEG C/min, insulation 3-4 hour, then rise to 80 DEG C with the speed of 1 DEG C/min, insulation 3-5 hour, obtains resin balls after cooling;
(4) the resin balls cleaning adopting ethanol step (3) to be obtained, then washes, then sends into oven dry in drying machine, namely obtains adsorbent resin with ultra-high specific surface area after oven dry.
Preferably, the concentration of described sodium-chlor is 6-10wt%.
Preferably, the concentration of described sodium-chlor is 8wt%.
Preferably, the mass ratio of described step (1) Raw and sodium chloride aqueous solution is 1:5-7.
Preferably, in described step (3), the quality of vinylbenzene and methyl acrylate is the 20-35% of the Archon quality that step (2) obtains.
Preferably, in described step (3), vinylbenzene, acrylic acid methyl esters, composite pore-forming, initiator and catalyst quality ratio is identical with described step (1).
Preferably, in described step (3), the quality of vinylbenzene, acrylic acid methyl esters, composite pore-forming, initiator and catalyzer and the mass ratio of sodium chloride aqueous solution are 1:5-7.
The present invention adopts low-temperature catalyzed scion grafting synthesis and secondary suspension copolymerization technology, than production coventional type acrylic resin energy-conservation more than 30%.Adopt composite pore-forming, improve specific surface area and the exchange capacity of polymeric adsorbent, enhance the physical strength of resin, extend the life cycle of resin, chemical stability is good.On the other hand, improve the contamination resistance of resin better, decrease the discharging of waste liquid caused because of resin regeneration, protection of the environment.
Adsorbent resin with ultra-high specific surface area prepared by the present invention has the following advantages: (1) specific surface area is large, 1400m
2/ g, (2) have excellent anti-organic contamination ability, can not cause secondary pollution; (3) physical strength is high, not easily broken, is widely used.
Embodiment
Embodiment 1
A kind of adsorbent resin with ultra-high specific surface area, comprises the component of following mass fraction:
Vinylbenzene 36 parts,
Methyl acrylate 12 parts,
Composite pore-forming 0.6 part,
Initiator 11 parts,
Catalyzer 3 parts.
Described composite pore-forming is the mixture of methyl cyclopropane and mibk, and the mass ratio of the two is 2:1.
Described catalyzer is the mixture of iron(ic) chloride and zinc chloride, and the mass ratio of the two is 1:1.
Described initiator is peroxidation phenyl-diformyl.
The preparation method of described adsorbent resin with ultra-high specific surface area, comprises the following steps:
(1) aqueous solution of sodium-chlor is added in reactor, be warming up to 45 DEG C; The raw material that vinylbenzene, acrylic acid methyl esters, composite pore-forming, initiator and catalyzer form is uniformly mixed 10-15min at 45 DEG C, add in aforesaid reaction vessel, stir, 65 DEG C are warming up to the speed of 2-3 DEG C/min, insulation 3-4 hour, then rise to 80 DEG C with the speed of 1 DEG C/min, insulation 3-5 hour, then cooling obtains Archon;
(2) Archon in reactor is put into wash in material still and cleans, then send in drying machine and dry, after oven dry, filter out the Archon that granularity is qualified;
(3) add appropriate vinylbenzene and methyl acrylate in the Archon obtained to step (2), stir 30min, add appropriate composite pore-forming, initiator and catalyzer and be uniformly mixed 10-15min at 45 DEG C, obtain mixing raw material; Add in a kettle. after sodium chloride solution is warming up to 45 DEG C and add described mixing raw material, stir, be warming up to 65 DEG C with the speed of 2-3 DEG C/min, insulation 3-4 hour, then rise to 80 DEG C with the speed of 1 DEG C/min, insulation 3-5 hour, obtains resin balls after cooling;
(4) the resin balls cleaning adopting ethanol step (3) to be obtained, then washes, then sends into oven dry in drying machine, namely obtains adsorbent resin with ultra-high specific surface area after oven dry.
The concentration of described sodium-chlor is 8wt%.
The mass ratio of described step (1) Raw and sodium chloride aqueous solution is 1:6.
In described step (3), the quality of vinylbenzene and methyl acrylate is 30% of the Archon quality that step (2) obtains.
In described step (3), vinylbenzene, acrylic acid methyl esters, composite pore-forming, initiator and catalyst quality are than identical with described step (1).
In described step (3), the quality of vinylbenzene, acrylic acid methyl esters, composite pore-forming, initiator and catalyzer and the mass ratio of sodium chloride aqueous solution are 1:6.
Embodiment 2
A kind of adsorbent resin with ultra-high specific surface area, comprises the component of following mass fraction:
Vinylbenzene 30 parts
Methyl acrylate 15 parts
Composite pore-forming 0.5 part
Initiator 10 parts
Catalyzer 1 part
Described composite pore-forming is the mixture of methyl cyclopropane and mibk, and the mass ratio of the two is 1:1.
Described catalyzer is zinc chloride.
Described initiator is peroxidation phenyl-diformyl.
Do following preparation according to above proportioning, comprise the following steps:
(1) aqueous solution of sodium-chlor is added in reactor, be warming up to 45 DEG C; The raw material that vinylbenzene, acrylic acid methyl esters, composite pore-forming, initiator and catalyzer form is uniformly mixed 10-15min at 45 DEG C, add in aforesaid reaction vessel, stir, 65 DEG C are warming up to the speed of 2-3 DEG C/min, insulation 3-4 hour, then rise to 80 DEG C with the speed of 1 DEG C/min, insulation 3-5 hour, then cooling obtains Archon;
(2) Archon in reactor is put into wash in material still and cleans, then send in drying machine and dry, after oven dry, filter out the Archon that granularity is qualified;
(3) add appropriate vinylbenzene and methyl acrylate in the Archon obtained to step (2), stir 30min, add appropriate composite pore-forming, initiator and catalyzer and be uniformly mixed 10-15min at 45 DEG C, obtain mixing raw material; Add in a kettle. after sodium chloride solution is warming up to 45 DEG C and add described mixing raw material, stir, be warming up to 65 DEG C with the speed of 2-3 DEG C/min, insulation 3-4 hour, then rise to 80 DEG C with the speed of 1 DEG C/min, insulation 3-5 hour, obtains resin balls after cooling;
(4) the resin balls cleaning adopting ethanol step (3) to be obtained, then washes, then sends into oven dry in drying machine, namely obtains adsorbent resin with ultra-high specific surface area after oven dry.
The concentration of described sodium-chlor is 6wt%.
The mass ratio of described step (1) Raw and sodium chloride aqueous solution is 1:5.
In described step (3), the quality of vinylbenzene and methyl acrylate is 35% of the Archon quality that step (2) obtains.
In described step (3), vinylbenzene, acrylic acid methyl esters, composite pore-forming, initiator and catalyst quality are than identical with described step (1).
In described step (3), the quality of vinylbenzene, acrylic acid methyl esters, composite pore-forming, initiator and catalyzer and the mass ratio of sodium chloride aqueous solution are 1:5.
Embodiment 3
A kind of adsorbent resin with ultra-high specific surface area, comprises the component of following mass fraction:
Vinylbenzene 40 parts
Methyl acrylate 10 parts
Composite pore-forming 1 part
Initiator 12 parts
Catalyzer 5 parts
Described composite pore-forming is the mixture of methyl cyclopropane and mibk, and the mass ratio of the two is 3:1.
Described catalyzer is iron(ic) chloride.
Described initiator is peroxidation phenyl-diformyl.
Do following preparation according to above proportioning, comprise the following steps:
(1) aqueous solution of sodium-chlor is added in reactor, be warming up to 45 DEG C; The raw material that vinylbenzene, acrylic acid methyl esters, composite pore-forming, initiator and catalyzer form is uniformly mixed 10-15min at 45 DEG C, add in aforesaid reaction vessel, stir, 65 DEG C are warming up to the speed of 2-3 DEG C/min, insulation 3-4 hour, then rise to 80 DEG C with the speed of 1 DEG C/min, insulation 3-5 hour, then cooling obtains Archon;
(2) Archon in reactor is put into wash in material still and cleans, then send in drying machine and dry, after oven dry, filter out the Archon that granularity is qualified;
(3) add appropriate vinylbenzene and methyl acrylate in the Archon obtained to step (2), stir 30min, add appropriate composite pore-forming, initiator and catalyzer and be uniformly mixed 10-15min at 45 DEG C, obtain mixing raw material; Add in a kettle. after sodium chloride solution is warming up to 45 DEG C and add described mixing raw material, stir, be warming up to 65 DEG C with the speed of 2-3 DEG C/min, insulation 3-4 hour, then rise to 80 DEG C with the speed of 1 DEG C/min, insulation 3-5 hour, obtains resin balls after cooling;
(4) the resin balls cleaning adopting ethanol step (3) to be obtained, then washes, then sends into oven dry in drying machine, namely obtains adsorbent resin with ultra-high specific surface area after oven dry.
The concentration of described sodium-chlor is 10wt%.
The mass ratio of described step (1) Raw and sodium chloride aqueous solution is 1:7.
In described step (3), the quality of vinylbenzene and methyl acrylate is 20% of the Archon quality that step (2) obtains.
In described step (3), vinylbenzene, acrylic acid methyl esters, composite pore-forming, initiator and catalyst quality are than identical with described step (1).
In described step (3), the quality of vinylbenzene, acrylic acid methyl esters, composite pore-forming, initiator and catalyzer and the mass ratio of sodium chloride aqueous solution are 1:7.
Embodiment 4
A kind of adsorbent resin with ultra-high specific surface area, comprises the component of following mass fraction:
Vinylbenzene 36 parts,
Methyl acrylate 12 parts,
Composite pore-forming 0.6 part,
Initiator 11 parts,
Catalyzer 3 parts.
Described composite pore-forming is the mixture of methyl cyclopropane and mibk, and the mass ratio of the two is 1:3.
Described catalyzer is the mixture of iron(ic) chloride and zinc chloride, and the mass ratio of the two is 1:1.
Described initiator is peroxidation phenyl-diformyl.
The preparation method of described adsorbent resin with ultra-high specific surface area, comprises the following steps:
(1) aqueous solution of sodium-chlor is added in reactor, be warming up to 45 DEG C; The raw material that vinylbenzene, acrylic acid methyl esters, composite pore-forming, initiator and catalyzer form is uniformly mixed 10-15min at 45 DEG C, add in aforesaid reaction vessel, stir, 65 DEG C are warming up to the speed of 2-3 DEG C/min, insulation 3-4 hour, then rise to 80 DEG C with the speed of 1 DEG C/min, insulation 3-5 hour, then cooling obtains Archon;
(2) Archon in reactor is put into wash in material still and cleans, then send in drying machine and dry, after oven dry, filter out the Archon that granularity is qualified;
(3) add appropriate vinylbenzene and methyl acrylate in the Archon obtained to step (2), stir 30min, add appropriate composite pore-forming, initiator and catalyzer and be uniformly mixed 10-15min at 45 DEG C, obtain mixing raw material; Add in a kettle. after sodium chloride solution is warming up to 45 DEG C and add described mixing raw material, stir, be warming up to 65 DEG C with the speed of 2-3 DEG C/min, insulation 3-4 hour, then rise to 80 DEG C with the speed of 1 DEG C/min, insulation 3-5 hour, obtains resin balls after cooling;
(4) the resin balls cleaning adopting ethanol step (3) to be obtained, then washes, then sends into oven dry in drying machine, namely obtains polymeric adsorbent after oven dry.
The concentration of described sodium-chlor is 8wt%.
The mass ratio of described step (1) Raw and sodium chloride aqueous solution is 1:6.
In described step (3), the quality of vinylbenzene and methyl acrylate is 30% of the Archon quality that step (2) obtains.
In described step (3), vinylbenzene, acrylic acid methyl esters, composite pore-forming, initiator and catalyst quality are than identical with described step (1).
In described step (3), the quality of vinylbenzene, acrylic acid methyl esters, composite pore-forming, initiator and catalyzer and the mass ratio of sodium chloride aqueous solution are 1:6.
Embodiment 5
A kind of adsorbent resin with ultra-high specific surface area, comprises the component of following mass fraction:
Vinylbenzene 36 parts,
Methyl acrylate 12 parts,
Pore-creating agent 0.6 part,
Initiator 11 parts,
Catalyzer 3 parts.
Described pore-creating agent is methyl cyclopropane.
Described catalyzer is the mixture of iron(ic) chloride and zinc chloride, and the mass ratio of the two is 1:1.
Described initiator is peroxidation phenyl-diformyl.
The preparation method of described adsorbent resin with ultra-high specific surface area, comprises the following steps:
(1) aqueous solution of sodium-chlor is added in reactor, be warming up to 45 DEG C; The raw material that vinylbenzene, acrylic acid methyl esters, composite pore-forming, initiator and catalyzer form is uniformly mixed 10-15min at 45 DEG C, add in aforesaid reaction vessel, stir, 65 DEG C are warming up to the speed of 2-3 DEG C/min, insulation 3-4 hour, then rise to 80 DEG C with the speed of 1 DEG C/min, insulation 3-5 hour, then cooling obtains Archon;
(2) Archon in reactor is put into wash in material still and cleans, then send in drying machine and dry, after oven dry, filter out the Archon that granularity is qualified;
(3) add appropriate vinylbenzene and methyl acrylate in the Archon obtained to step (2), stir 30min, add appropriate composite pore-forming, initiator and catalyzer and be uniformly mixed 10-15min at 45 DEG C, obtain mixing raw material; Add in a kettle. after sodium chloride solution is warming up to 45 DEG C and add described mixing raw material, stir, be warming up to 65 DEG C with the speed of 2-3 DEG C/min, insulation 3-4 hour, then rise to 80 DEG C with the speed of 1 DEG C/min, insulation 3-5 hour, obtains resin balls after cooling;
(4) the resin balls cleaning adopting ethanol step (3) to be obtained, then washes, then sends into oven dry in drying machine, namely obtains polymeric adsorbent after oven dry.
The concentration of described sodium-chlor is 8wt%.
The mass ratio of described step (1) Raw and sodium chloride aqueous solution is 1:6.
In described step (3), the quality of vinylbenzene and methyl acrylate is 30% of the Archon quality that step (2) obtains.
In described step (3), vinylbenzene, acrylic acid methyl esters, composite pore-forming, initiator and catalyst quality are than identical with described step (1).
In described step (3), the quality of vinylbenzene, acrylic acid methyl esters, composite pore-forming, initiator and catalyzer and the mass ratio of sodium chloride aqueous solution are 1:6.
Embodiment 6
A kind of adsorbent resin with ultra-high specific surface area, comprises the component of following mass fraction:
Vinylbenzene 36 parts,
Methyl acrylate 5 parts,
Composite pore-forming 0.2 part,
Initiator 11 parts,
Catalyzer 3 parts.
Described composite pore-forming is the mixture of methyl cyclopropane and mibk, and the mass ratio of the two is 2:1.
Described catalyzer is iron(ic) chloride.
Described initiator is peroxidation phenyl-diformyl.
The preparation method of described adsorbent resin with ultra-high specific surface area, comprises the following steps:
(1) aqueous solution of sodium-chlor is added in reactor, be warming up to 45 DEG C; The raw material that vinylbenzene, acrylic acid methyl esters, composite pore-forming, initiator and catalyzer form is uniformly mixed 10-15min at 45 DEG C, add in aforesaid reaction vessel, stir, 65 DEG C are warming up to the speed of 2-3 DEG C/min, insulation 3-4 hour, then rise to 80 DEG C with the speed of 1 DEG C/min, insulation 3-5 hour, then cooling obtains Archon;
(2) Archon in reactor is put into wash in material still and cleans, then send in drying machine and dry, after oven dry, filter out the Archon that granularity is qualified;
(3) add appropriate vinylbenzene and methyl acrylate in the Archon obtained to step (2), stir 30min, add appropriate composite pore-forming, initiator and catalyzer and be uniformly mixed 10-15min at 45 DEG C, obtain mixing raw material; Add in a kettle. after sodium chloride solution is warming up to 45 DEG C and add described mixing raw material, stir, be warming up to 65 DEG C with the speed of 2-3 DEG C/min, insulation 3-4 hour, then rise to 80 DEG C with the speed of 1 DEG C/min, insulation 3-5 hour, obtains resin balls after cooling;
(4) the resin balls cleaning adopting ethanol step (3) to be obtained, then washes, then sends into oven dry in drying machine, namely obtains polymeric adsorbent after oven dry.
The mass ratio of described step (1) Raw and water is 1:6.
In described step (3), the quality of vinylbenzene and methyl acrylate is 30% of the Archon quality that step (2) obtains.
In described step (3), vinylbenzene, acrylic acid methyl esters, composite pore-forming, initiator and catalyst quality are than identical with described step (1).
In described step (3), the quality of vinylbenzene, acrylic acid methyl esters, composite pore-forming, initiator and catalyzer and the mass ratio of water are 1:10.
Carry out performance test to the polymeric adsorbent prepared by embodiment 1-6, test result is listed in table 1.
The performance data of table 1 polymeric adsorbent
As known from Table 1, the performance of the polymeric adsorbent prepared by embodiments of the invention 1-3 is significantly better than the polymeric adsorbent prepared by embodiment 4-6, and the specific surface area of polymeric adsorbent reaches 1400m
2/ g, pore volume and mean pore size are also apparently higher than embodiment 4-6.So the polymeric adsorbent prepared by the application has more excellent performance, each component proportion of polymeric adsorbent, and the performance of composite pore-forming on polymeric adsorbent has important impact.
Above to a kind of adsorbent resin with ultra-high specific surface area that the embodiment of the present invention provides and preparation method thereof, be described in detail, apply specific case herein to set forth principle of the present invention and embodiment, the explanation of above embodiment just understands method of the present invention and core concept thereof for helping; Meanwhile, for one of ordinary skill in the art, according to thought of the present invention, all will change in specific embodiments and applications, in sum, this description should not be construed as limitation of the present invention.
Claims (10)
1. an adsorbent resin with ultra-high specific surface area, is characterized in that, comprises the component of following mass fraction:
Vinylbenzene 30-40 part,
Methyl acrylate 10-15 part,
Composite pore-forming 0.5-1 part,
Initiator 10-12 part,
Catalyzer 1-5 part.
2. polymeric adsorbent according to claim 1, is characterized in that, described composite pore-forming is the mixture of methyl cyclopropane and mibk, and the mass ratio of the two is 1-3:1.
3. polymeric adsorbent according to claim 1, is characterized in that, described catalyzer is one or both of iron(ic) chloride and zinc chloride.
4. polymeric adsorbent according to claim 1, is characterized in that, described initiator is peroxidation phenyl-diformyl.
5. a preparation method for adsorbent resin with ultra-high specific surface area, is characterized in that, comprises the following steps:
(1) aqueous solution of sodium-chlor is added in reactor, be warming up to 45 DEG C; The raw material that vinylbenzene, acrylic acid methyl esters, composite pore-forming, initiator and catalyzer form is uniformly mixed 10-15min at 45 DEG C, add in aforesaid reaction vessel, stir, 65 DEG C are warming up to the speed of 2-3 DEG C/min, insulation 3-4 hour, then rise to 80 DEG C with the speed of 1 DEG C/min, insulation 3-5 hour, then cooling obtains Archon;
(2) Archon in reactor is put into wash in material still and cleans, then send in drying machine and dry, after oven dry, filter out the Archon that granularity is qualified;
(3) add appropriate vinylbenzene and methyl acrylate in the Archon obtained to step (2), stir 30min, add appropriate composite pore-forming, initiator and catalyzer and be uniformly mixed 10-15min at 45 DEG C, obtain mixing raw material; Add in a kettle. after sodium chloride solution is warming up to 45 DEG C and add described mixing raw material, stir, be warming up to 65 DEG C with the speed of 2-3 DEG C/min, insulation 3-4 hour, then rise to 80 DEG C with the speed of 1 DEG C/min, insulation 3-5 hour, obtains resin balls after cooling;
(4) the resin balls cleaning adopting ethanol step (3) to be obtained, then washes, then sends into oven dry in drying machine, namely obtains adsorbent resin with ultra-high specific surface area after oven dry.
6. preparation method according to claim 5, is characterized in that, the concentration of described sodium-chlor is 6-10wt%.
7. preparation method according to claim 5, is characterized in that, the mass ratio of described step (1) Raw and sodium chloride aqueous solution is 1:5-7.
8. preparation method according to claim 5, is characterized in that, in described step (3), the quality of vinylbenzene and methyl acrylate is the 20-35% of the Archon quality that step (2) obtains.
9. preparation method according to claim 5, is characterized in that, in described step (3), vinylbenzene, acrylic acid methyl esters, composite pore-forming, initiator and catalyst quality are than identical with described step (1).
10. preparation method according to claim 5, is characterized in that, in described step (3), the quality of vinylbenzene, acrylic acid methyl esters, composite pore-forming, initiator and catalyzer and the mass ratio of sodium chloride aqueous solution are 1:5-7.
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| CN116037221A (en) * | 2023-02-07 | 2023-05-02 | 蚌埠市天星树脂有限责任公司 | Preparation process of cation exchange resin for treating wastewater and waste gas |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1970592A (en) * | 2006-11-11 | 2007-05-30 | 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 |
| CN101255218A (en) * | 2007-12-18 | 2008-09-03 | 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 |
| CN103772573A (en) * | 2014-02-24 | 2014-05-07 | 山东鲁抗立科药业有限公司 | Ultrahigh cross-linked macro-porous adsorption resin applicable to removal of patulin |
| CN104231149A (en) * | 2014-08-15 | 2014-12-24 | 太仓康盛化工有限公司 | Porous microcapsule adsorptive resin and preparation method thereof |
| CN104788599A (en) * | 2015-03-27 | 2015-07-22 | 徐州浩通新材料科技股份有限公司 | Preparation method for macroporous weak-base 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 |
-
2015
- 2015-11-25 CN CN201510833870.1A patent/CN105273138B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1970592A (en) * | 2006-11-11 | 2007-05-30 | 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 |
| CN101255218A (en) * | 2007-12-18 | 2008-09-03 | 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 |
| CN103772573A (en) * | 2014-02-24 | 2014-05-07 | 山东鲁抗立科药业有限公司 | Ultrahigh cross-linked macro-porous adsorption resin applicable to removal of patulin |
| CN104231149A (en) * | 2014-08-15 | 2014-12-24 | 太仓康盛化工有限公司 | Porous microcapsule adsorptive resin and preparation method thereof |
| CN104788599A (en) * | 2015-03-27 | 2015-07-22 | 徐州浩通新材料科技股份有限公司 | Preparation method for macroporous weak-base 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 |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116037221A (en) * | 2023-02-07 | 2023-05-02 | 蚌埠市天星树脂有限责任公司 | Preparation process of cation exchange resin for treating wastewater and waste gas |
| CN116037221B (en) * | 2023-02-07 | 2023-08-18 | 蚌埠市天星树脂有限责任公司 | Preparation process of cation exchange resin for treating wastewater and waste gas |
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