CN105016336A - Environmental-friendly type asphalt resin mixed base spherical activated carbon obtained through utilization of waste and preparation method of environmental-friendly type asphalt resin mixed base spherical activated carbon - Google Patents
Environmental-friendly type asphalt resin mixed base spherical activated carbon obtained through utilization of waste and preparation method of environmental-friendly type asphalt resin mixed base spherical activated carbon Download PDFInfo
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- CN105016336A CN105016336A CN201510407262.4A CN201510407262A CN105016336A CN 105016336 A CN105016336 A CN 105016336A CN 201510407262 A CN201510407262 A CN 201510407262A CN 105016336 A CN105016336 A CN 105016336A
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Abstract
The invention discloses environmentally-friendly type asphalt resin mixed base spherical activated carbon obtained through the utilization of waste. The environmental-friendly type asphalt resin mixed base spherical activated carbon is characterized by being prepared from the following raw materials in parts by weight: 43-45 parts of methyl methacrylate, 40-43 parts of N-vinyl pyrrolidone, 26-29 parts of ethyl acetate, 2-3 parts of peroxide di tert butyl carbonate, 2-2.5 parts of pentaerythritol tetramethylacrylate, 2-3 parts of carboxymethyl cellulose, an appropriate amount of distilled water, an appropriate amount of acetone, 25-28 parts of sulfonated asphalt powder, 3-4 parts of shrimp shells, 3-4 parts of municipal sludge, 1-2 parts of polyvinyl alcohol, 8-10 parts of a hydrochloric acid solution of which the concentration is 2%, and 2-3 parts of sodium bicarbonate. When asphalt coated liquid is prepared, the components of the shrimp shells, the municipal sludge and the like are added, and a series of modifying technologies are adopted, so that the specific surface area is enlarged, and the adsorption capacity is improved; besides, the waste is utilized, the production cost is reduced, energy is saved, the consumption is reduced, and the treatment problems of the municipal sludge and the like are solved. The environmental-friendly type asphalt resin mixed base spherical activated carbon disclosed by the invention is innovative in the technology, and the industrial production is easy to realize.
Description
Technical field
The present invention relates to Material Field, particularly a kind of utilization of waste material environment-friendly type bituminous resins mixed base ball shape active carbon 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, develop high-effect pitch, resin compounded ball shape active carbon is a kind of existing quick adsorption desorption performance, oil-water separation is good, has again the ball shape active carbon of high mechanical strength, is a kind of excellent absorbent charcoal material.
Summary of the invention
The object of this invention is to provide a kind of utilization of waste material environment-friendly type bituminous resins mixed base ball shape active carbon and preparation method thereof.The present invention by utilizing shrimp shell, municipal sludge the like waste carries out modifiedly adding in pitch coating liquid, by forming quick adsorption layer on fluoropolymer resin ball surface, increasing specific surface area simultaneously, enhancing adsorptive power.
In order to realize object of the present invention, the present invention is by following scheme implementation:
A kind of utilization of waste material environment-friendly type bituminous resins mixed base ball shape active carbon, be made up of the raw material of following weight part: methyl methacrylate 43-45, NVP 40-43, ethyl acetate 26-29, peroxidation di tert butyl carbonate 2-3, pentaerythritol tetramethylacrylate 2-2.5, carboxymethyl cellulose 2-3, distilled water in right amount, acetone in proper, sulfonated gilsonite powder 25-28, shrimp shell 3-4, municipal sludge 3-4, polyvinyl alcohol 1-2, concentration be 2% hydrochloric acid soln 8-10, sodium bicarbonate 2-3;
A kind of utilization of waste material environment-friendly type bituminous resins mixed base ball shape active carbon of the present invention, be made up of following concrete steps:
(1) carboxymethyl cellulose is added in the distilled water of 100 times amount, be heated to dissolve completely, slow cooling is to room temperature, add ethyl acetate slowly successively under nitrogen protection, peroxidation di tert butyl carbonate, pentaerythritol tetramethylacrylate, methyl methacrylate, NVP, 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) shrimp shell, municipal sludge are put into baking oven and dehydrated, be then that the hydrochloric acid soln of 2% mixes with concentration, soak after 3 hours, with the cleaning of water distilled water to neutral, putting into baking oven crushed after being dried becomes 200 order powder stand-by, is dissolved in by polyvinyl alcohol in the distilled water of 10 times amount, mixes with the powder after pulverizing, add sodium bicarbonate again, after mixing, then in retort furnace, with the temperature calcination 3-4 hour of 300-350 DEG C, room temperature cooling after taking out, ground 200 mesh sieves 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 monomers such as methyl methacrylate etc. for raw material, add the compositions such as pore-creating agent ethyl acetate, the polymer microballoon of different diameter is obtained by the method for suspension polymerization, again the water-soluble pitch 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.
The present invention, when preparing pitch coating liquid, adds the compositions such as shrimp shell, municipal sludge, by a series of modified technique, increase specific surface area, enhance adsorptive power, utilization of waste material simultaneously, reduce production cost, energy-saving and cost-reducing, solve the process problems such as municipal sludge simultaneously; The processing method that the present invention adopts, not only there is novelty, and be convenient to production control, be easy to realize suitability for industrialized production, product safety is effective, ash content is few, harmless, the gas processing of the environmental Kuznets Curves of high-cleanness, high, strainer etc., solvent recuperation, water treatment, the filler of cigarette filter, hemodialysis and pharmaceutical industries can be widely used in.
Specific embodiments
Below by specific examples, the present invention is described in detail.
A kind of utilization of waste material environment-friendly type bituminous resins mixed base ball shape active carbon, is made up of the raw material of following weight part (kilogram): methyl methacrylate 43, NVP 40, ethyl acetate 26, peroxidation di tert butyl carbonate 2, pentaerythritol tetramethylacrylate 2, carboxymethyl cellulose 2, distilled water are appropriate, acetone in proper, sulfonated gilsonite powder 25, shrimp shell 3, municipal sludge 3, polyvinyl alcohol 1, concentration are 2% hydrochloric acid soln 8, sodium bicarbonate 2;
A kind of utilization of waste material environment-friendly type bituminous resins mixed base ball shape active carbon of the present invention, be made up of following concrete steps:
(1) carboxymethyl cellulose is added in the distilled water of 100 times amount, be heated to dissolve completely, slow cooling is to room temperature, add ethyl acetate slowly successively under nitrogen protection, peroxidation di tert butyl carbonate, pentaerythritol tetramethylacrylate, methyl methacrylate, NVP, 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) shrimp shell, municipal sludge are put into baking oven and dehydrated, be then that the hydrochloric acid soln of 2% mixes with concentration, soak after 3 hours, with the cleaning of water distilled water to neutral, putting into baking oven crushed after being dried becomes 200 order powder stand-by, is dissolved in by polyvinyl alcohol in the distilled water of 10 times amount, mixes with the powder after pulverizing, add sodium bicarbonate again, after mixing, then in retort furnace, with the temperature calcination 3 hours of 300-350 DEG C, room temperature cooling after taking out, ground 200 mesh sieves 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 0.2MPa, 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 1108m
2/ g, physical strength is 5.98N.
Claims (2)
1. a utilization of waste material environment-friendly type bituminous resins mixed base ball shape active carbon, it is characterized in that, be made up of the raw material of following weight part: methyl methacrylate 43-45, NVP 40-43, ethyl acetate 26-29, peroxidation di tert butyl carbonate 2-3, pentaerythritol tetramethylacrylate 2-2.5, carboxymethyl cellulose 2-3, distilled water are appropriate, acetone in proper, sulfonated gilsonite powder 25-28, shrimp shell 3-4, municipal sludge 3-4, polyvinyl alcohol 1-2, concentration are 2% hydrochloric acid soln 8-10, sodium bicarbonate 2-3.
2. a kind of utilization of waste material environment-friendly type bituminous resins mixed base ball shape active carbon according to claim 1, is characterized in that, be made up of following concrete steps:
(1) carboxymethyl cellulose is added in the distilled water of 100 times amount, be heated to dissolve completely, slow cooling is to room temperature, add ethyl acetate slowly successively under nitrogen protection, peroxidation di tert butyl carbonate, pentaerythritol tetramethylacrylate, methyl methacrylate, NVP, 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) shrimp shell, municipal sludge are put into baking oven and dehydrated, be then that the hydrochloric acid soln of 2% mixes with concentration, soak after 3 hours, with the cleaning of water distilled water to neutral, putting into baking oven crushed after being dried becomes 200 order powder stand-by, is dissolved in by polyvinyl alcohol in the distilled water of 10 times amount, mixes with the powder after pulverizing, add sodium bicarbonate again, after mixing, then in retort furnace, with the temperature calcination 3-4 hour of 300-350 DEG C, room temperature cooling after taking out, ground 200 mesh sieves 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.
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| CN201510407262.4A CN105016336A (en) | 2015-07-13 | 2015-07-13 | Environmental-friendly type asphalt resin mixed base spherical activated carbon obtained through utilization of waste and preparation method of environmental-friendly type asphalt resin mixed base spherical activated carbon |
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| CN201510407262.4A CN105016336A (en) | 2015-07-13 | 2015-07-13 | Environmental-friendly type asphalt resin mixed base spherical activated carbon obtained through utilization of waste and preparation method of environmental-friendly type asphalt resin mixed base spherical activated carbon |
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Citations (4)
| 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 |
| CN102701200A (en) * | 2012-05-14 | 2012-10-03 | 北京工业大学 | Method for preparing active carbon from municipal sludge by two-step thermal decomposition |
| CN103420353A (en) * | 2012-05-15 | 2013-12-04 | 北京化工大学 | Porous carbon material and preparation method and application thereof |
| 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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- 2015-07-13 CN CN201510407262.4A patent/CN105016336A/en active Pending
Patent Citations (4)
| 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 |
| CN102701200A (en) * | 2012-05-14 | 2012-10-03 | 北京工业大学 | Method for preparing active carbon from municipal sludge by two-step thermal decomposition |
| CN103420353A (en) * | 2012-05-15 | 2013-12-04 | 北京化工大学 | Porous carbon material and preparation method and application thereof |
| 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: 20151104 |