CN105129793A - Composite asphalt resin spherical active carbons with magnetism and preparation method thereof - Google Patents

Composite asphalt resin spherical active carbons with magnetism and preparation method thereof Download PDF

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Publication number
CN105129793A
CN105129793A CN201510389520.0A CN201510389520A CN105129793A CN 105129793 A CN105129793 A CN 105129793A CN 201510389520 A CN201510389520 A CN 201510389520A CN 105129793 A CN105129793 A CN 105129793A
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parts
speed
distilled water
revs
resin
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沈向洋
吴克
余志敏
蒋涌
吴杰
吴育兵
樊云
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ANHUI CHENGFANG NEW MATERIAL TECHNOLOGY Co Ltd
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ANHUI CHENGFANG NEW MATERIAL TECHNOLOGY Co Ltd
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Abstract

The invention discloses composite asphalt resin spherical active carbons with magnetism. The composite asphalt resin spherical active carbons with magnetism are characterized by being prepared from the following materials by weight: 39-43 parts of ethyl methacrylate, 46-50 parts of vinyl laurate, 2-3 parts of diisopropylperoxydicarbonate, 1-1.5 parts of diethylene glycol diacrylate, 25-28 parts of butylene glycol, 1-2 parts of poly(ethylene oxide) lauryl ether, 3-4 parts of iron dust core, 1-2 parts of azodicarbonamide, 2-3 parts of silica sol, 1-2 parts of polyvinyl alcohol, a proper amount of distilled water and acetone, and 25-28 parts of sulfonated asphalt powder. In the invention, asphalt coating liquid, containing the iron dust core, the azodicarbonamide, etc., coats the surfaces of resin polymer spheres by a special process to form spheres with a uniform size; the coated spheres have surfaces with good fluidity, hardness of resin and a quick adsorption function of asphalt. The composite asphalt resin spherical active carbons have the advantages of wide material source, the preparation method of the composite asphalt resin spherical active carbons with magnetism is a innovative process and convenient for industrial control, and is suitable for using in sewage processing and liquid recovery etc.

Description

A kind of tool magnetic bituminous resins complex spherical gac and preparation method thereof
Technical field
The present invention relates to Material Field, particularly a kind of tool magnetic bituminous resins complex spherical gac and preparation method thereof.
Background technology
Ball shape active carbon, because having that sphericity is good, tamped density is high, particles from getting loose is few and the feature such as adsorption desorption speed is fast, has been widely used in the association areas such as medicine, environmental protection and support of the catalyst.Ball shape active carbon is mainly divided three classes by raw material difference: coal-based ball shape active carbon, macromolecule resin base globe activated char and asphalt-base spherical activated carbon.Wherein, the advantage of coal-based ball shape active carbon is that cost of material is cheap, wide material sources, but the ash content of active carbon from coal is high, and impurity is many, and physical strength is low, thus limits its application and development.The ball shape active carbon being precursor power with polymeric resin matrix and pitch is because having that ash oontent is low, Carbon yield is high and the advantage such as pore size distribution is easy to control and receiving much concern.
Due to the difference on molecular structure, pore passage structure and the physical strength of asphalt-base spherical activated carbon and resin based sphere active carbon are different.Asphalt-base spherical activated carbon has the advantages that loading capacity is large and adsorption desorption speed is fast, and polymer-based ball shape active carbon then has larger specific surface area and higher physical strength.If the ball shape active carbon prepared has both features concurrently, then significant to the expansion of its Application Areas.Therefore, developing high-effect pitch, resin compounded ball shape active carbon a kind ofly not only has quick adsorption desorption performance but also have high mechanical strength, has the ball shape active carbon of magnetic effect simultaneously, is a kind of excellent absorbent charcoal material.
Summary of the invention
The object of this invention is to provide a kind of tool magnetic bituminous resins complex spherical gac and preparation method thereof.The present invention utilizes ferrocart core, Cellmic C 121, silicon sol etc. to be added in pitch coating liquid by a series of technique, while forming quick adsorption layer on fluoropolymer resin ball surface, there is certain magnetic, can be used in water treatment or liquids recovery etc.
In order to realize object of the present invention, the present invention is by following scheme implementation:
A kind of tool magnetic bituminous resins complex spherical gac, be made up of the raw material of following weight part: β-dimethyl-aminoethylmethacrylate 39-43, vinyl laurate 46-50, diisopropyl peroxide carbonate 2-3, diethylene glycol diacrylate 1-1.5, butyleneglycol 25-28, polyethylene oxide lauryl ether 1-2, ferrocart core 3-4, Cellmic C 121 1-2, silicon sol 2-3, polyvinyl alcohol 1-2, distilled water in right amount, acetone in proper, sulfonated gilsonite powder 25-28;
A kind of tool of the present invention magnetic bituminous resins complex spherical gac, be made up of following concrete steps:
(1) polyethylene oxide lauryl ether is added in the distilled water of 200 times amount, after being stirred to dissolving with the speed of 600 revs/min, add butyleneglycol slowly successively under nitrogen protection, diisopropyl peroxide carbonate, diethylene glycol diacrylate, β-dimethyl-aminoethylmethacrylate, vinyl laurate, controlling stirring velocity is 1000 revs/min, then 60 DEG C are slowly warming up to, stirring reaction is after 60 minutes, continue to be warming up to 80 DEG C, with the speed stirring reaction 4 hours of 400 revs/min, use filtered on buchner funnel reaction solution, by solid resin ball distilled water wash 2 times, dry in baking oven at 50 DEG C, in the resin balls of drying, add the acetone of 3 times amount, heating in water bath is to 65-75 DEG C while stirring, keeps acetone to be that reflux state stops backflow after 24 hours, then by resin balls taking-up, with distilled water wash 3 times, dries stand-by in the baking oven at 50 DEG C,
(2) sulfonated gilsonite powder is added the distilled water wash of 2 times amount, through stirring 60 minutes under rotating speed is the condition of 600 revs/min, supernatant liquor is collected after it leaves standstill, then supernatant liquor is put into baking oven, dry with the temperature of 100 DEG C, then dried supernatant liquor being added the distilled water of 5 times amount, stirring stand-by to dissolving the formation aqueous solution completely;
(3) added by polyvinyl alcohol in the water of 3 times amount, heating direct, to dissolving completely, then evenly forms mixed solution with silicon sol blending dispersion; Ferrocart core is put into ball mill ball milling 60-90 minute, then mix with Cellmic C 121, ball milling is evenly rear to be mixed with mixed solution, 100-120 minute is stirred with the speed of 300 revs/min, then allow in baking oven, at 90-105 DEG C, be dried to constant weight, obtain mixed powder;
(4) aqueous solution that step (2) obtains is mixed with the mixed powder of step (3), stir with the speed of 600 revs/min and within 30 minutes, form asphaltic base mixing coating liquid, the resin balls that step (1) obtains is put into seed-coating machine, the feeding temperature controlling coating liquid is 60-80 DEG C, operating pressure is 0.2-0.5MPa, asphaltic base mixing coating liquid is wrapped in resin balls surface equably, obtains composite pellets;
(5) composite pellets step (4) obtained is sent in High Temperature Furnaces Heating Apparatus; under helium protection; 600-650 DEG C is warming up to the speed of 1-2 DEG C/min; insulation charing 2 hours; be warming up to 750-850 DEG C of activation 2 hours again with the speed of 3-4 DEG C/min again, after being cooled to room temperature, obtain the ball shape active carbon that particle diameter is 0.2-0.8mm.
The invention has the beneficial effects as follows: the present invention with monomer methacrylic acid ethyl ester, vinyl laurate etc. for raw material, add the compositions such as pore-creating agent butyleneglycol, the polymer microballoon of different diameter, different pore size is obtained by the method for suspension polymerization, again the water-soluble pitch coating liquid after process is coated on polymer microballoon surface equably, then after charing, activation, makes surface have black glossy, size evenly and the ball shape active carbon with high-specific surface area.
Containing the composition such as ferrocart core, Cellmic C 121 in pitch coating liquid of the present invention, resinous polymer bead surface is coated on by special process, formed uniform spherical, mobility is good, have the function of the quick adsorption of resin-based hardness and asphaltic base concurrently, and wide material sources of the present invention, process innovation and be convenient to Industry Control, be beneficial to and realize suitability for industrialized production, product of the present invention is a kind of high performance active carbon, can use under multiple liquid and gas environment, be applicable to sewage disposal, liquids recovery etc.
Specific embodiments
Below by specific examples, the present invention is described in detail.
A kind of tool magnetic bituminous resins complex spherical gac, is made up of the raw material of following weight part (kilogram): β-dimethyl-aminoethylmethacrylate 39, vinyl laurate 46, diisopropyl peroxide carbonate 2, diethylene glycol diacrylate 1, butyleneglycol 25, polyethylene oxide lauryl ether 1, ferrocart core 3, Cellmic C 121 1, silicon sol 2, polyvinyl alcohol 1, distilled water are appropriate, acetone in proper, sulfonated gilsonite powder 25;
A kind of tool of the present invention magnetic bituminous resins complex spherical gac, be made up of following concrete steps:
(1) polyethylene oxide lauryl ether is added in the distilled water of 200 times amount, after being stirred to dissolving with the speed of 600 revs/min, add butyleneglycol slowly successively under nitrogen protection, diisopropyl peroxide carbonate, diethylene glycol diacrylate, β-dimethyl-aminoethylmethacrylate, vinyl laurate, controlling stirring velocity is 1000 revs/min, then 60 DEG C are slowly warming up to, stirring reaction is after 60 minutes, continue to be warming up to 80 DEG C, with the speed stirring reaction 4 hours of 400 revs/min, use filtered on buchner funnel reaction solution, by solid resin ball distilled water wash 2 times, dry in baking oven at 50 DEG C, in the resin balls of drying, add the acetone of 3 times amount, heating in water bath is to 65-75 DEG C while stirring, keeps acetone to be that reflux state stops backflow after 24 hours, then by resin balls taking-up, with distilled water wash 3 times, dries stand-by in the baking oven at 50 DEG C,
(2) sulfonated gilsonite powder is added the distilled water wash of 2 times amount, through stirring 60 minutes under rotating speed is the condition of 600 revs/min, supernatant liquor is collected after it leaves standstill, then supernatant liquor is put into baking oven, dry with the temperature of 100 DEG C, then dried supernatant liquor being added the distilled water of 5 times amount, stirring stand-by to dissolving the formation aqueous solution completely;
(3) added by polyvinyl alcohol in the water of 3 times amount, heating direct, to dissolving completely, then evenly forms mixed solution with silicon sol blending dispersion; Ferrocart core is put into ball mill ball milling 60 minutes, then mix with Cellmic C 121, ball milling is evenly rear to be mixed with mixed solution, stirs 100 minutes, then allow in baking oven, be dried to constant weight, obtain mixed powder at 90-105 DEG C with the speed of 300 revs/min;
(4) aqueous solution that step (2) obtains is mixed with the mixed powder of step (3), stir with the speed of 600 revs/min and within 30 minutes, form asphaltic base mixing coating liquid, the resin balls that step (1) obtains is put into seed-coating machine, the feeding temperature controlling coating liquid is 60-80 DEG C, operating pressure is 0.2MPa, asphaltic base mixing coating liquid is wrapped in resin balls surface equably, obtains composite pellets;
(5) composite pellets step (4) obtained is sent in High Temperature Furnaces Heating Apparatus; under helium protection; 600-650 DEG C is warming up to the speed of 2 DEG C/min; insulation charing 2 hours; be warming up to 750-850 DEG C of activation 2 hours again with the speed of 4 DEG C/min again, after being cooled to room temperature, obtain the ball shape active carbon that particle diameter is 0.2-0.8mm.
Product of the present invention is the glossiness spherical particle of black bands, detects it, and specific surface area is 987m 2/ g, physical strength is 5.98N.

Claims (2)

1. a tool magnetic bituminous resins complex spherical gac, it is characterized in that, be made up of the raw material of following weight part: β-dimethyl-aminoethylmethacrylate 39-43, vinyl laurate 46-50, diisopropyl peroxide carbonate 2-3, diethylene glycol diacrylate 1-1.5, butyleneglycol 25-28, polyethylene oxide lauryl ether 1-2, ferrocart core 3-4, Cellmic C 121 1-2, silicon sol 2-3, polyvinyl alcohol 1-2, distilled water are appropriate, acetone in proper, sulfonated gilsonite powder 25-28.
2. a kind of tool magnetic bituminous resins complex spherical gac according to claim 1, is characterized in that, be made up of following concrete steps:
(1) polyethylene oxide lauryl ether is added in the distilled water of 200 times amount, after being stirred to dissolving with the speed of 600 revs/min, add butyleneglycol slowly successively under nitrogen protection, diisopropyl peroxide carbonate, diethylene glycol diacrylate, β-dimethyl-aminoethylmethacrylate, vinyl laurate, controlling stirring velocity is 1000 revs/min, then 60 DEG C are slowly warming up to, stirring reaction is after 60 minutes, continue to be warming up to 80 DEG C, with the speed stirring reaction 4 hours of 400 revs/min, use filtered on buchner funnel reaction solution, by solid resin ball distilled water wash 2 times, dry in baking oven at 50 DEG C, in the resin balls of drying, add the acetone of 3 times amount, heating in water bath is to 65-75 DEG C while stirring, keeps acetone to be that reflux state stops backflow after 24 hours, then by resin balls taking-up, with distilled water wash 3 times, dries stand-by in the baking oven at 50 DEG C,
(2) sulfonated gilsonite powder is added the distilled water wash of 2 times amount, through stirring 60 minutes under rotating speed is the condition of 600 revs/min, supernatant liquor is collected after it leaves standstill, then supernatant liquor is put into baking oven, dry with the temperature of 100 DEG C, then dried supernatant liquor being added the distilled water of 5 times amount, stirring stand-by to dissolving the formation aqueous solution completely;
(3) added by polyvinyl alcohol in the water of 3 times amount, heating direct, to dissolving completely, then evenly forms mixed solution with silicon sol blending dispersion; Ferrocart core is put into ball mill ball milling 60-90 minute, then mix with Cellmic C 121, ball milling is evenly rear to be mixed with mixed solution, 100-120 minute is stirred with the speed of 300 revs/min, then allow in baking oven, at 90-105 DEG C, be dried to constant weight, obtain mixed powder;
(4) aqueous solution that step (2) obtains is mixed with the mixed powder of step (3), stir with the speed of 600 revs/min and within 30 minutes, form asphaltic base mixing coating liquid, the resin balls that step (1) obtains is put into seed-coating machine, the feeding temperature controlling coating liquid is 60-80 DEG C, operating pressure is 0.2-0.5MPa, asphaltic base mixing coating liquid is wrapped in resin balls surface equably, obtains composite pellets;
(5) composite pellets step (4) obtained is sent in High Temperature Furnaces Heating Apparatus; under helium protection; 600-650 DEG C is warming up to the speed of 1-2 DEG C/min; insulation charing 2 hours; be warming up to 750-850 DEG C of activation 2 hours again with the speed of 3-4 DEG C/min again, after being cooled to room temperature, obtain the ball shape active carbon that particle diameter is 0.2-0.8mm.
CN201510389520.0A 2015-07-06 2015-07-06 Composite asphalt resin spherical active carbons with magnetism and preparation method thereof Pending CN105129793A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH03187908A (en) * 1989-12-18 1991-08-15 Nippon Carbon Co Ltd Production of spherical carbon material
CN102153079A (en) * 2011-05-03 2011-08-17 北京华福神雾工业炉有限公司 Method and system for preparing active carbon from industrial coal by using oxygen carbonization method
WO2012146048A1 (en) * 2011-04-28 2012-11-01 深圳市芭田生态工程股份有限公司 Preparation method for asphalt-based spherical active carbon with no need for non-melting process
CN103521179A (en) * 2013-09-29 2014-01-22 福建工程学院 One-step method for preparing sludge-based formed magnetic active carbon
CN103641115A (en) * 2013-11-19 2014-03-19 苏州丹百利电子材料有限公司 Preparation method of spherical active carbon

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH03187908A (en) * 1989-12-18 1991-08-15 Nippon Carbon Co Ltd Production of spherical carbon material
WO2012146048A1 (en) * 2011-04-28 2012-11-01 深圳市芭田生态工程股份有限公司 Preparation method for asphalt-based spherical active carbon with no need for non-melting process
CN102153079A (en) * 2011-05-03 2011-08-17 北京华福神雾工业炉有限公司 Method and system for preparing active carbon from industrial coal by using oxygen carbonization method
CN103521179A (en) * 2013-09-29 2014-01-22 福建工程学院 One-step method for preparing sludge-based formed magnetic active carbon
CN103641115A (en) * 2013-11-19 2014-03-19 苏州丹百利电子材料有限公司 Preparation method of spherical active carbon

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Application publication date: 20151209