CN105032349A - Asphaltic resin composite spherical activated carbon with expanded graphite enhanced oil absorption property and preparation method therefor - Google Patents
Asphaltic resin composite spherical activated carbon with expanded graphite enhanced oil absorption property and preparation method therefor Download PDFInfo
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- CN105032349A CN105032349A CN201510407153.2A CN201510407153A CN105032349A CN 105032349 A CN105032349 A CN 105032349A CN 201510407153 A CN201510407153 A CN 201510407153A CN 105032349 A CN105032349 A CN 105032349A
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Abstract
The invention discloses asphaltic resin composite spherical activated carbon with an expanded graphite enhanced oil absorption property. The asphaltic resin composite spherical activated carbon is characterized by being prepared from the following raw materials in parts by weight: 40-43 parts of tert-butyl methacrylate, 40-42 parts of ortho-methylstyrene, 25-28 parts of ethanol, 2-3 parts of tert-butyl hydroperoxide, 1.5-2.5 parts of bisphenol A epoxy dimethyl acrylic acid, 2-3 parts of gelatin, 0.5-0.8 part of OP-10, a proper volume of distilled water, a proper volume of acetone, 25-28 parts of sulfonated asphalt powder, 4-5 parts of expanded graphite, 2-3 parts of clay powder, 3-4 parts of corncob powder, 2-3 parts of 1% sodium hydroxide solution, 3-4 parts of citric acid and 2-3 parts of emulsified paraffin. The asphaltic resin composite spherical activated carbon contains ingredients such as the modified expanded graphite, the clay powder, the corncob powder and the like, and the modified expanded graphite and the like exist in three-dimensional fiber-net-shaped molecular structures, so that a large number of oil molecules can be adsorbed, meanwhile, the oil absorption speed is high, the oil-water selectivity is high, and the oil retention property is good.
Description
Technical field
The present invention relates to Material Field, particularly a kind of expanded graphite strengthens asphaltic resin composite base spherical activated charcoal of oil absorbency 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 a kind ofly not only had quick adsorption desorption performance, oil-water separating function, but also has the spherical activated charcoal of high mechanical properties, is a kind of excellent absorbent charcoal material.
Summary of the invention
The object of this invention is to provide a kind of expanded graphite and strengthen asphaltic resin composite base spherical activated charcoal of oil absorbency and preparation method thereof.The present invention utilizes the compositions such as expanded graphite, carclazyte powder, maize cob meal to add in pitch coating liquid by a series of modified technique, by forming quick adsorption layer on fluoropolymer resin ball surface, simultaneously, expanded graphites etc. exist the netted molecular structure of dimensional fibre can adsorbed oil molecule in a large number, has good oils absorption property.
In order to realize object of the present invention, the present invention is by following scheme implementation:
Expanded graphite strengthens the asphaltic resin composite base spherical activated charcoal of oil absorbency, is made up of the raw material of following weight portion: Tert-butyl Methacrylate 40-43, ortho methyl group styrene 40-42, ethanol 25-28, TBHP 2-3, bisphenol-A epoxy base dimethacrylate 1.5-2.5, gelatin 2-3, OP-100.5-0.8, distilled water in right amount, acetone in proper, sulfonated gilsonite powder 25-28, expanded graphite 4-5, carclazyte powder 2-3, maize cob meal 3-4, concentration be 1% sodium hydroxide solution 2-3, citric acid 3-4, emulsified wax 2-3;
A kind of expanded graphite of the present invention strengthens the asphaltic resin composite base spherical activated charcoal of oil absorbency, is made up of following concrete steps:
(1) gelatin is added in the distilled water of 100 times amount, be heated to dissolve completely, slow cooling is to room temperature, add OP-10, be stirred to and be uniformly dispersed, then ethanol is added slowly successively under nitrogen protection, TBHP, bisphenol-A epoxy base dimethacrylate, Tert-butyl Methacrylate, ortho methyl group 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 5 times amount, stirring stand-by to dissolving the formation aqueous solution completely;
(3) maize cob meal, expanded graphite, carclazyte powder are put into pulverizer, be ground into 200 order powder stand-by, then mixing is put into the sodium hydroxide solution immersion treatment 2 hours at normal temperatures that concentration is 1%, rinse in neutral with aqueous citric acid solution again, last and emulsified wax puts into mixer, take out after stirring 30 minutes with the speed of 600 revs/min, then put into baking oven, to dry to obtain mixed-powder under the condition of 90 DEG C;
(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 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 Tert-butyl Methacrylate etc. for raw material, add the compositions such as pore-foaming agent ethanol, 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 includes the composition such as expanded graphite, carclazyte powder, maize cob meal of modification, modified expanded graphites etc. exist the netted molecular structure of dimensional fibre can adsorbed oil molecule in a large number, have good oils absorption property, speed of oil absorption is fast simultaneously, oil-water selectivity is high, Oil keeping good.Present invention process is convenient to Industry Control, is beneficial to and realizes automation, and product is a kind of high performance active carbon, can be applicable to the gas treatment of the environmental Kuznets Curves of high-cleanness, high, filter etc., solvent recovery, water-oil separating etc.
Specific embodiments
Below by instantiation, the present invention is described in detail.
Expanded graphite strengthens an asphaltic resin composite base spherical activated charcoal for oil absorbency, is made up of the raw material of following weight portion (kilogram): Tert-butyl Methacrylate 40, ortho methyl group styrene 40, ethanol 25, TBHP 2, bisphenol-A epoxy base dimethacrylate 1.5, gelatin 2, OP-100.5, distilled water are appropriate, acetone in proper, sulfonated gilsonite powder 25, expanded graphite 4, carclazyte powder 2, maize cob meal 3, concentration are 1% sodium hydroxide solution 2, citric acid 3, emulsified wax 2;
A kind of expanded graphite of the present invention strengthens the asphaltic resin composite base spherical activated charcoal of oil absorbency, is made up of following concrete steps:
(1) gelatin is added in the distilled water of 100 times amount, be heated to dissolve completely, slow cooling is to room temperature, add OP-10, be stirred to and be uniformly dispersed, then ethanol is added slowly successively under nitrogen protection, TBHP, bisphenol-A epoxy base dimethacrylate, Tert-butyl Methacrylate, ortho methyl group 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 5 times amount, stirring stand-by to dissolving the formation aqueous solution completely;
(3) maize cob meal, expanded graphite, carclazyte powder are put into pulverizer, be ground into 200 order powder stand-by, then mixing is put into the sodium hydroxide solution immersion treatment 2 hours at normal temperatures that concentration is 1%, rinse in neutral with aqueous citric acid solution again, last and emulsified wax puts into mixer, take out after stirring 30 minutes with the speed of 600 revs/min, then put into baking oven, to dry to obtain mixed-powder under the condition of 90 DEG C;
(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 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 969m
2/ g, mechanical strength is 6.11N.
Claims (2)
1. the asphaltic resin composite base spherical activated charcoal of an expanded graphite enhancing oil absorbency, it is characterized in that, be made up of the raw material of following weight portion: Tert-butyl Methacrylate 40-43, ortho methyl group styrene 40-42, ethanol 25-28, TBHP 2-3, bisphenol-A epoxy base dimethacrylate 1.5-2.5, gelatin 2-3, OP-100.5-0.8, distilled water is appropriate, acetone in proper, sulfonated gilsonite powder 25-28, expanded graphite 4-5, carclazyte powder 2-3, maize cob meal 3-4, concentration is the sodium hydroxide solution 2-3 of 1%, citric acid 3-4, emulsified wax 2-3.
2. a kind of expanded graphite strengthens the asphaltic resin composite base spherical activated charcoal of oil absorbency according to claim 1, it is characterized in that, is made up of following concrete steps:
(1) gelatin is added in the distilled water of 100 times amount, be heated to dissolve completely, slow cooling is to room temperature, add OP-10, be stirred to and be uniformly dispersed, then ethanol is added slowly successively under nitrogen protection, TBHP, bisphenol-A epoxy base dimethacrylate, Tert-butyl Methacrylate, ortho methyl group 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 5 times amount, stirring stand-by to dissolving the formation aqueous solution completely;
(3) maize cob meal, expanded graphite, carclazyte powder are put into pulverizer, be ground into 200 order powder stand-by, then mixing is put into the sodium hydroxide solution immersion treatment 2 hours at normal temperatures that concentration is 1%, rinse in neutral with aqueous citric acid solution again, last and emulsified wax puts into mixer, take out after stirring 30 minutes with the speed of 600 revs/min, then put into baking oven, to dry to obtain mixed-powder under the condition of 90 DEG C;
(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 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 (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109201006A (en) * | 2018-09-03 | 2019-01-15 | 中成未来新材料（福建）有限公司 | A kind of environmental-protection adsorption material and preparation method thereof based on burning ash |
| CN110339826A (en) * | 2019-07-11 | 2019-10-18 | 刘建恒 | A kind of mesoporous filtrate of lightweight and preparation method thereof |
| CN113549334A (en) * | 2021-08-18 | 2021-10-26 | 鄂尔多斯市路泰新材料科技发展有限公司 | High-elasticity high-weather-resistance modified asphalt and preparation method thereof |
| CN114507451A (en) * | 2022-03-29 | 2022-05-17 | 邯郸市交通运输局公路工程管理处 | VOCs composite inhibition type asphalt 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 |
| CN1072869A (en) * | 1991-12-02 | 1993-06-09 | 浙江省临安县工业科学研究所 | Make the modified argil that the insulating oil purifying adsorbent is used |
| CN1579615A (en) * | 2004-05-18 | 2005-02-16 | 清华大学 | Preparation of oil pollution adsorbent and its recovery and regeneration method |
| 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
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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 |
| CN1072869A (en) * | 1991-12-02 | 1993-06-09 | 浙江省临安县工业科学研究所 | Make the modified argil that the insulating oil purifying adsorbent is used |
| CN1579615A (en) * | 2004-05-18 | 2005-02-16 | 清华大学 | Preparation of oil pollution adsorbent and its recovery and regeneration method |
| CN103693641A (en) * | 2013-12-12 | 2014-04-02 | 天津大学 | Method for preparing spherical active carbon employing water soluble bitumen |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109201006A (en) * | 2018-09-03 | 2019-01-15 | 中成未来新材料（福建）有限公司 | A kind of environmental-protection adsorption material and preparation method thereof based on burning ash |
| CN110339826A (en) * | 2019-07-11 | 2019-10-18 | 刘建恒 | A kind of mesoporous filtrate of lightweight and preparation method thereof |
| CN113549334A (en) * | 2021-08-18 | 2021-10-26 | 鄂尔多斯市路泰新材料科技发展有限公司 | High-elasticity high-weather-resistance modified asphalt and preparation method thereof |
| CN114507451A (en) * | 2022-03-29 | 2022-05-17 | 邯郸市交通运输局公路工程管理处 | VOCs composite inhibition type asphalt and preparation method thereof |
| CN114507451B (en) * | 2022-03-29 | 2022-11-29 | 邯郸市交通运输局公路工程管理处 | VOCs composite inhibition type asphalt and preparation method thereof |
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