CN104998617A - Composite based spherical active carbon added with hard polyurethane foam wastes and preparation method for spherical active carbon - Google Patents
Composite based spherical active carbon added with hard polyurethane foam wastes and preparation method for spherical active carbon Download PDFInfo
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- CN104998617A CN104998617A CN201510407329.4A CN201510407329A CN104998617A CN 104998617 A CN104998617 A CN 104998617A CN 201510407329 A CN201510407329 A CN 201510407329A CN 104998617 A CN104998617 A CN 104998617A
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Abstract
The invention discloses a composite based spherical active carbon added with hard polyurethane foam wastes. The composite based spherical active carbon is characterized by being prepared from the following raw materials in parts by weight: 44-46 parts of benzyl methacrylate, 39-41 parts of methacrylonitrile, 26-29 parts of ethyl acetate, 2-3 parts of azodiisobutyronitrile, 1.5-2 parts of diisocyanate, 2-3 parts of polyvinyl alcohol, 0.8-1 part of polyethylene oxide lauryl ether, a proper amount of distilled water, a proper amount of acetone, 25-28 parts of sulfonated bitumen powder, 4-5 parts of the hard polyurethane foam wastes, 8-9 parts of silica sol with the solid content being 3% and 0.8-1 part of vinyl triethoxysilane. According to the composite based spherical active carbon, the hard polyurethane foam wastes are taken as main modification components and soaked with the silica sol, so that the roughness is improved; the hard polyurethane foam wastes are modified with vinyl triethoxysilane, so that the hard polyurethane foam wastes are endowed with hydrophobic and oleophylic performances; and the hard polyurethane foam wastes are added into bitumen coating liquid, and a quick adsorption layer can be formed on the spherical surface of polymer resin, so that the oil-water separation effect is enhanced.
Description
Technical field
The present invention relates to Material Field, particularly a kind of composite base spherical activated charcoal adding hard polyurethane foams waste material 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, develop high-effect pitch, resin compounded spherical activated charcoal is a kind of existing quick adsorption desorption performance, oil-water separation is good, has again the spherical activated charcoal of high mechanical properties, is a kind of excellent absorbent charcoal material.
Polyurethane foam has very large absorptive capacity, but its oil-water selectivity is very poor, a large amount of water will be absorbed when being used as the oil absorption material of marine oil overflow or industrial waste oil recovery, can not meet the requirement as efficient oil absorption material, good profit resolving effect and can be modified the material of low-surface-energy at rough surface and obtain by structure rough surface.
Summary of the invention
The object of this invention is to provide a kind of composite base spherical activated charcoal adding hard polyurethane foams waste material and preparation method thereof.The present invention utilizes hard polyurethane foams waste material as main altered contents, soak with Ludox, enhance roughness, again by the modification of VTES, make it have hydrophobic oleophilic oil performance, be added in pitch coating liquid, quick adsorption layer can be formed on fluoropolymer resin ball surface, enhance oil-water separation.
In order to realize object of the present invention, the present invention is by following scheme implementation:
Add a composite base spherical activated charcoal for hard polyurethane foams waste material, be made up of the raw material of following weight portion: benzyl methacrylate 44-46, methacrylonitrile 39-41, ethyl acetate 26-29, azodiisobutyronitrile 2-3, vulcabond 1.5-2, polyvinyl alcohol 2-3, PEO lauryl ether 0.8-1, distilled water are appropriate, acetone in proper, sulfonated gilsonite powder 25-28, hard polyurethane foams waste material 4-5, solid content are 3% Ludox 8-9, VTES 0.8-1;
A kind of composite base spherical activated charcoal adding hard polyurethane foams waste material of the present invention, be made up of following concrete steps:
(1) polyvinyl alcohol is added in the distilled water of 100 times amount, be heated to dissolve completely, after slow cooling to room temperature, add PEO lauryl ether, be stirred to and be uniformly dispersed, then ethyl acetate is added slowly successively under nitrogen protection, azodiisobutyronitrile, vulcabond, benzyl methacrylate, methacrylonitrile, 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 5 times amount, stirring stand-by to dissolving the formation aqueous solution completely;
(3) hard polyurethane foams waste material is put into disintegrating machine and be broken into fritter, then put into pulverizer and be ground into 80 order powder, powder being immersed in solid content is in the Ludox of 3%, soak 40 minutes under normal temperature, then suction filtration, extract sediment, after cleaning 3 times with distilled water, the baking oven putting into 100 DEG C is dried, again by the powder after drying and the distilled water of 5 times amount, VTES puts into ball mill, be warming up to 60-70 DEG C, ball milling 2 hours, cooling leaves standstill, taking precipitate, baking oven is put into after repeatedly cleaning with distilled water, to dry and to obtain the mixture of modification under the condition of 80 DEG C,
(4) aqueous solution that step (2) obtains is mixed with the mixture of the modification of step (3), 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 benzyl methacrylate etc. for raw material, add the compositions such as pore-foaming agent ethyl acetate, the polymer microballoon of different-diameter is obtained by the method for suspension polymerisation, 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 spherical activated charcoal with high-specific surface area.
The present invention utilizes hard polyurethane foams waste material as main altered contents, soak with Ludox, enhance roughness, again by the modification of VTES, make it have hydrophobic oleophilic oil performance, be added in pitch coating liquid, quick adsorption layer can be formed on fluoropolymer resin ball surface, enhance oil-water separation.The spherical activated charcoal ash content that the present invention produces is few, harmless, and hardness is large, and regenerating easily, is very suitable for water treatment and water-oil separating etc.
Specific embodiments
Below by instantiation, the present invention is described in detail.
Add a composite base spherical activated charcoal for hard polyurethane foams waste material, be made up of the raw material of following weight portion (kilogram): benzyl methacrylate 44, methacrylonitrile 39, ethyl acetate 26, azodiisobutyronitrile 2, vulcabond 1.5, polyvinyl alcohol 2, PEO lauryl ether 0.8, distilled water are appropriate, acetone in proper, sulfonated gilsonite powder 25, hard polyurethane foams waste material 4, solid content are 3% Ludox 8, VTES 0.8;
A kind of composite base spherical activated charcoal adding hard polyurethane foams waste material of the present invention, be made up of following concrete steps:
(1) polyvinyl alcohol is added in the distilled water of 100 times amount, be heated to dissolve completely, after slow cooling to room temperature, add PEO lauryl ether, be stirred to and be uniformly dispersed, then ethyl acetate is added slowly successively under nitrogen protection, azodiisobutyronitrile, vulcabond, benzyl methacrylate, methacrylonitrile, 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 5 times amount, stirring stand-by to dissolving the formation aqueous solution completely;
(3) hard polyurethane foams waste material is put into disintegrating machine and be broken into fritter, then put into pulverizer and be ground into 80 order powder, powder being immersed in solid content is in the Ludox of 3%, soak 40 minutes under normal temperature, then suction filtration, extract sediment, after cleaning 3 times with distilled water, the baking oven putting into 100 DEG C is dried, again by the powder after drying and the distilled water of 5 times amount, VTES puts into ball mill, be warming up to 60-70 DEG C, ball milling 2 hours, cooling leaves standstill, taking precipitate, baking oven is put into after repeatedly cleaning with distilled water, to dry and to obtain the mixture of modification under the condition of 80 DEG C,
(4) aqueous solution that step (2) obtains is mixed with the mixture of the modification of step (3), 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 1235m
2/ g, mechanical strength is 6.09N.
Claims (2)
1. one kind is added the composite base spherical activated charcoal of hard polyurethane foams waste material, it is characterized in that, be made up of the raw material of following weight portion: benzyl methacrylate 44-46, methacrylonitrile 39-41, ethyl acetate 26-29, azodiisobutyronitrile 2-3, vulcabond 1.5-2, polyvinyl alcohol 2-3, PEO lauryl ether 0.8-1, distilled water are appropriate, acetone in proper, sulfonated gilsonite powder 25-28, hard polyurethane foams waste material 4-5, solid content are 3% Ludox 8-9, VTES 0.8-1.
2. a kind of composite base spherical activated charcoal adding hard polyurethane foams waste material according to claim 1, is characterized in that, be made up of following concrete steps:
(1) polyvinyl alcohol is added in the distilled water of 100 times amount, be heated to dissolve completely, after slow cooling to room temperature, add PEO lauryl ether, be stirred to and be uniformly dispersed, then ethyl acetate is added slowly successively under nitrogen protection, azodiisobutyronitrile, vulcabond, benzyl methacrylate, methacrylonitrile, 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 5 times amount, stirring stand-by to dissolving the formation aqueous solution completely;
(3) hard polyurethane foams waste material is put into disintegrating machine and be broken into fritter, then put into pulverizer and be ground into 80 order powder, powder being immersed in solid content is in the Ludox of 3%, soak 40 minutes under normal temperature, then suction filtration, extract sediment, after cleaning 3 times with distilled water, the baking oven putting into 100 DEG C is dried, again by the powder after drying and the distilled water of 5 times amount, VTES puts into ball mill, be warming up to 60-70 DEG C, ball milling 2 hours, cooling leaves standstill, taking precipitate, baking oven is put into after repeatedly cleaning with distilled water, to dry and to obtain the mixture of modification under the condition of 80 DEG C,
(4) aqueous solution that step (2) obtains is mixed with the mixture of the modification of step (3), 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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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 |
| CN103131041A (en) * | 2013-01-18 | 2013-06-05 | 青岛科技大学 | Surface modification polyurethane oil absorption material and preparation method 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 |
| CN103693641A (en) * | 2013-12-12 | 2014-04-02 | 天津大学 | Method for preparing spherical active carbon employing water soluble bitumen |
| CN103723729A (en) * | 2013-12-27 | 2014-04-16 | 黑龙江工程学院 | Preparation method of gradient activated carbon |
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2015
- 2015-07-13 CN CN201510407329.4A patent/CN104998617A/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 |
| CN103131041A (en) * | 2013-01-18 | 2013-06-05 | 青岛科技大学 | Surface modification polyurethane oil absorption material and preparation method 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 |
| CN103693641A (en) * | 2013-12-12 | 2014-04-02 | 天津大学 | Method for preparing spherical active carbon employing water soluble bitumen |
| CN103723729A (en) * | 2013-12-27 | 2014-04-16 | 黑龙江工程学院 | Preparation method of gradient activated carbon |
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