CN105032346A - Nano zinc oxide zirconium oxide modified asphalt resin composite spherical active carbon and preparation method thereof - Google Patents
Nano zinc oxide zirconium oxide modified asphalt resin composite spherical active carbon and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a nano zinc oxide zirconium oxide modified asphalt resin composite spherical active carbon. The nano zinc oxide zirconium oxide modified asphalt resin composite spherical active carbon is prepared from, by weight, 45 to 49 parts of 2-ethyl hexyl acrylate, 40 to 43 parts of ortho-ethylstyrene, 2 to 3 parts of peroxy-2-ethylhexoic acid, 1.5 to 2 parts of divinyl benzene, 25 to 29 parts of ethyl formate, 1 to 2 parts of sodium lauryl sulfate, an appropriate amount of distilled water, an appropriate amount of acetone, 2 to 3 parts of nano zinc oxide, 2 to 3 parts of nano zirconium oxide, 1.5 to 2.5 parts of liquid silicon dioxide, 0.7 to 0.9 part of n-dodecyltrimethoxysilane, and 25 to 28 parts of sulfonated bitumen powder. According to a preparation method, after surface modification, nano zinc oxide and nano zirconium oxide are added into an asphalt coated liquid, micro holes are formed on the surfaces of polymer micro spheres, adsorbability is increased, and high temperature resistance and compressive strength of the surface of an asphalt base are increased at the same time. Application prospect is promising; and the nano zinc oxide zirconium oxide modified asphalt resin composite spherical active carbon can be applied to environmental control and gas treatment.
Description
Technical field
The present invention relates to Material Field, asphaltic resin complex spherical active carbon of particularly a kind of nano zine oxide zirconia modification and preparation method thereof.
Background technology
Spherical activated charcoal, because having that sphericity is good, packed 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 catalyst carrier.Spherical activated charcoal is mainly divided three classes by raw material difference: coal-based spherical activated charcoal, macromolecule resin base globe activated char and asphalt-base spherical activated carbon.Wherein, the advantage of coal-based spherical activated charcoal 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 mechanical strength is low, thus limits its application and development.The spherical activated charcoal being precursor power with polymeric resin matrix and pitch is because having that content of ashes 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 mechanical strength of asphalt-base spherical activated carbon and resin based sphere active carbon are different.Asphalt-base spherical activated carbon has the advantages that adsorption capacity is large and adsorption desorption speed is fast, and polymer-based spherical activated charcoal then has larger specific area and higher mechanical strength.If the spherical activated charcoal prepared has both features concurrently, then significant to the expansion of its application.Therefore, developing high-effect pitch, resin compounded spherical activated charcoal is a kind of spherical activated charcoal not only having had quick adsorption desorption performance but also had high mechanical properties, is a kind of excellent absorbent charcoal material.
Summary of the invention
Asphaltic resin complex spherical active carbon that the object of this invention is to provide the modification of a kind of nano zine oxide zirconia and preparation method thereof.The composition such as nano zine oxide, nano zircite is added in pitch coating liquid by special process by the present invention, is coated on resin microsphere, forms micro-pore, adds adsorptivity, also enhance heat-resisting quantity simultaneously, and compression strength.
In order to realize object of the present invention, the present invention is by following scheme implementation:
An asphaltic resin complex spherical active carbon for nano zine oxide zirconia modification, be made up of the raw material of following weight portion: 2-ethylhexyl acrylic acid 45-49, ortho position ethyl styrene 40-43, peroxidating-2 ethyl hexanoic acid 2-3, divinylbenzene 1.5-2, Ethyl formate 25-29, NaLS 1-2, distilled water are appropriate, acetone in proper, nano zine oxide 2-3, nano zircite 2-3, liquid silica gel 1.5-2.5, dodecyl trimethoxy silane 0.7-0.9, sulfonated gilsonite powder 25-28;
The asphaltic resin complex spherical active carbon of a kind of nano zine oxide zirconia of the present invention modification, be made up of following concrete steps:
(1) NaLS is added in the distilled water of 200 times amount, be stirred to the speed of 300 revs/min and dissolve completely, add Ethyl formate slowly successively under nitrogen protection, peroxidating-2 ethyl hexanoic acid, divinylbenzene, 2-ethylhexyl acrylic acid, ortho position ethyl styrene, controlling mixing speed 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 reactant liquor, hard resin ball distilled water is washed 2 times, dry in baking oven at 50 DEG C, in the resin balls of drying, add the acetone of 3 times amount, heating water bath is to 65-75 DEG C while stirring, keeps acetone to be that reflux state stops backflow after 24 hours, then resin balls is taken out, wash 3 times, dry stand-by in the baking oven at 50 DEG C with distilled water,
(2) sulfonated gilsonite powder is added the distilled water washing of 2 times amount, through stirring 60 minutes under rotating speed is the condition of 600 revs/min, supernatant is collected after it leaves standstill, then supernatant is put into baking oven, dry with the temperature of 100 DEG C, then dried supernatant being added the distilled water of 6 times amount, stirring stand-by to dissolving the formation aqueous solution completely;
(3) by nano zine oxide, that nano zircite puts into stirrer for mixing is even, add dodecyl trimethoxy silane, 30-40 minute is stirred with the speed of 600-800 rev/min, put into after taking-up after baking oven dries 120-150 minute with 50-60 DEG C and mix with all the other residual components, put into ball mill, namely ball milling obtains mixture in 15 minutes;
(4) aqueous solution that step (2) obtains is mixed with the mixture of step (3), be heated to 40-50 DEG C, stir with the speed of 600 revs/min and within 30 minutes, form asphaltic base mixing coating solution, the resin balls that step (1) obtains is put into seed-coating machine, the feeding temperature controlling coating solution is 60-80 DEG C, operating pressure is 0.2-0.5MPa, asphaltic base mixing coating solution is wrapped in resin balls surface equably, obtains composite pellets;
(5) composite pellets step (4) obtained is sent in high temperature furnace; 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 spherical activated charcoal that particle diameter is 0.2-0.8mm.
The invention has the beneficial effects as follows: the present invention with monomers such as ortho position ethyl styrene etc. for raw material, add the compositions such as pore-foaming agent Ethyl formate, the polymer microballoon of different pore size is obtained by the method for suspension polymerisation, 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 spherical activated charcoal with high-specific surface area.
Nano zine oxide, nano zircite etc. by adding in pitch coating liquid after surface modification, being formed micro-pore on polymer globules surface, adding adsorptivity, also enhance heat-resisting quantity and the compression strength on asphaltic base surface simultaneously by the present invention.The present invention is resin content and top layer water-based bitumen content proportioning science overall, total pore volume and the average pore size of spherical activated charcoal can not only be improved, but also can effectively improve its mechanical strength, the rate of adsorption of adsorption process maintains quick adsorption desorption performance substantially simultaneously.
The application prospect of product of the present invention is extensive, can be applicable to the material for trapping that uses in the gas treatment of the environmental Kuznets Curves of high-cleanness, high, filter etc., solvent recovery, water treatment, the filler of cigarette filter, haemodialysis and pharmaceuticals industry, chromatography of gases or packing material, sorbing material etc. that fine chemistry industry uses.
Specific embodiments
Below by instantiation, the present invention is described in detail.
An asphaltic resin complex spherical active carbon for nano zine oxide zirconia modification, is made up of the raw material of following weight portion (kilogram): 2-ethylhexyl acrylic acid 45, ortho position ethyl styrene 40, peroxidating-2 ethyl hexanoic acid 2, divinylbenzene 1.5, Ethyl formate 25, NaLS 1, distilled water are appropriate, acetone in proper, nano zine oxide 2, nano zircite 2, liquid silica gel 1.5, dodecyl trimethoxy silane 0.7, sulfonated gilsonite powder 25;
The asphaltic resin complex spherical active carbon of a kind of nano zine oxide zirconia of the present invention modification, be made up of following concrete steps:
(1) NaLS is added in the distilled water of 200 times amount, be stirred to the speed of 300 revs/min and dissolve completely, add Ethyl formate slowly successively under nitrogen protection, peroxidating-2 ethyl hexanoic acid, divinylbenzene, 2-ethylhexyl acrylic acid, ortho position ethyl styrene, controlling mixing speed 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 reactant liquor, hard resin ball distilled water is washed 2 times, dry in baking oven at 50 DEG C, in the resin balls of drying, add the acetone of 3 times amount, heating water bath is to 65-75 DEG C while stirring, keeps acetone to be that reflux state stops backflow after 24 hours, then resin balls is taken out, wash 3 times, dry stand-by in the baking oven at 50 DEG C with distilled water,
(2) sulfonated gilsonite powder is added the distilled water washing of 2 times amount, through stirring 60 minutes under rotating speed is the condition of 600 revs/min, supernatant is collected after it leaves standstill, then supernatant is put into baking oven, dry with the temperature of 100 DEG C, then dried supernatant being added the distilled water of 6 times amount, stirring stand-by to dissolving the formation aqueous solution completely;
(3) by nano zine oxide, that nano zircite puts into stirrer for mixing is even, add dodecyl trimethoxy silane, 30 minutes are stirred with the speed of 600 revs/min, put into after taking-up after baking oven dries 120 minutes with 50-60 DEG C and mix with all the other residual components, put into ball mill, namely ball milling obtains mixture in 15 minutes;
(4) aqueous solution that step (2) obtains is mixed with the mixture of step (3), be heated to 40-50 DEG C, stir with the speed of 600 revs/min and within 30 minutes, form asphaltic base mixing coating solution, the resin balls that step (1) obtains is put into seed-coating machine, the feeding temperature controlling coating solution is 60-80 DEG C, operating pressure is 0.2MPa, asphaltic base mixing coating solution is wrapped in resin balls surface equably, obtains composite pellets;
(5) composite pellets step (4) obtained is sent in high temperature furnace; 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 spherical activated charcoal 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 area is 1230m
2/ g, mechanical strength is 6.2N.
Claims (2)
1. the asphaltic resin complex spherical active carbon of nano zine oxide zirconia modification, it is characterized in that, be made up of the raw material of following weight portion: 2-ethylhexyl acrylic acid 45-49, ortho position ethyl styrene 40-43, peroxidating-2 ethyl hexanoic acid 2-3, divinylbenzene 1.5-2, Ethyl formate 25-29, NaLS 1-2, distilled water are appropriate, acetone in proper, nano zine oxide 2-3, nano zircite 2-3, liquid silica gel 1.5-2.5, dodecyl trimethoxy silane 0.7-0.9, sulfonated gilsonite powder 25-28.
2. the asphaltic resin complex spherical active carbon of a kind of nano zine oxide zirconia modification according to claim 1, is characterized in that, be made up of following concrete steps:
(1) NaLS is added in the distilled water of 200 times amount, be stirred to the speed of 300 revs/min and dissolve completely, add Ethyl formate slowly successively under nitrogen protection, peroxidating-2 ethyl hexanoic acid, divinylbenzene, 2-ethylhexyl acrylic acid, ortho position ethyl styrene, controlling mixing speed 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 reactant liquor, hard resin ball distilled water is washed 2 times, dry in baking oven at 50 DEG C, in the resin balls of drying, add the acetone of 3 times amount, heating water bath is to 65-75 DEG C while stirring, keeps acetone to be that reflux state stops backflow after 24 hours, then resin balls is taken out, wash 3 times, dry stand-by in the baking oven at 50 DEG C with distilled water,
(2) sulfonated gilsonite powder is added the distilled water washing of 2 times amount, through stirring 60 minutes under rotating speed is the condition of 600 revs/min, supernatant is collected after it leaves standstill, then supernatant is put into baking oven, dry with the temperature of 100 DEG C, then dried supernatant being added the distilled water of 6 times amount, stirring stand-by to dissolving the formation aqueous solution completely;
(3) by nano zine oxide, that nano zircite puts into stirrer for mixing is even, add dodecyl trimethoxy silane, 30-40 minute is stirred with the speed of 600-800 rev/min, put into after taking-up after baking oven dries 120-150 minute with 50-60 DEG C and mix with all the other residual components, put into ball mill, namely ball milling obtains mixture in 15 minutes;
(4) aqueous solution that step (2) obtains is mixed with the mixture of step (3), be heated to 40-50 DEG C, stir with the speed of 600 revs/min and within 30 minutes, form asphaltic base mixing coating solution, the resin balls that step (1) obtains is put into seed-coating machine, the feeding temperature controlling coating solution is 60-80 DEG C, operating pressure is 0.2-0.5MPa, asphaltic base mixing coating solution is wrapped in resin balls surface equably, obtains composite pellets;
(5) composite pellets step (4) obtained is sent in high temperature furnace; 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 spherical activated charcoal that particle diameter is 0.2-0.8mm.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106077438A (en) * | 2016-06-22 | 2016-11-09 | 马鞍山市创诚铸造有限公司 | A kind of novel environment friendly molding sand using nano zircite modified animal glue as bonding agent and preparation method thereof |
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| JPH03187908A (en) * | 1989-12-18 | 1991-08-15 | Nippon Carbon Co Ltd | Production of spherical carbon material |
| CN102015913A (en) * | 2008-04-25 | 2011-04-13 | 3M创新有限公司 | Process for the surface modification of particles |
| CN102114406A (en) * | 2009-12-30 | 2011-07-06 | 中国石油化工股份有限公司 | Zirconic desulphurization adsorbent, preparation method and application thereof |
| CN103476707A (en) * | 2011-04-28 | 2013-12-25 | 株式会社德山 | Metal oxide powder and method for producing same |
| CN103693641A (en) * | 2013-12-12 | 2014-04-02 | 天津大学 | Method for preparing spherical active carbon employing water soluble bitumen |
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- 2015-07-06 CN CN201510389423.1A patent/CN105032346A/en active Pending
Patent Citations (5)
| 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 |
| CN102015913A (en) * | 2008-04-25 | 2011-04-13 | 3M创新有限公司 | Process for the surface modification of particles |
| CN102114406A (en) * | 2009-12-30 | 2011-07-06 | 中国石油化工股份有限公司 | Zirconic desulphurization adsorbent, preparation method and application thereof |
| CN103476707A (en) * | 2011-04-28 | 2013-12-25 | 株式会社德山 | Metal oxide powder and method for producing same |
| CN103693641A (en) * | 2013-12-12 | 2014-04-02 | 天津大学 | Method for preparing spherical active carbon employing water soluble bitumen |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106077438A (en) * | 2016-06-22 | 2016-11-09 | 马鞍山市创诚铸造有限公司 | A kind of novel environment friendly molding sand using nano zircite modified animal glue as bonding agent and preparation method thereof |
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