CN101875005A - Benzene adsorption material and preparation method thereof - Google Patents
Benzene adsorption material and preparation method thereof Download PDFInfo
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- CN101875005A CN101875005A CN2010102280297A CN201010228029A CN101875005A CN 101875005 A CN101875005 A CN 101875005A CN 2010102280297 A CN2010102280297 A CN 2010102280297A CN 201010228029 A CN201010228029 A CN 201010228029A CN 101875005 A CN101875005 A CN 101875005A
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- styrene
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Abstract
The invention provides a benzene adsorption material and a preparation method thereof. The benzene adsorption material is styrene-divinybenzene copolymer, the weight of the styrene is 10-30 percent of that of the divinybenzene, and the weight of water is 0-100 percent of that of divinybenzene. The preparation method comprises the following steps of: reacting in presence of styrene and divinybenzene used as monomers, azodiisobutyronitrile used as a polymerization initiator, and tetrahydrofuran used as a solvent and a template, or adding water as a cosolvent, and then vacuum drying the reaction product to obtain the styrene-divinybenzene copolymer. The obtained material has very high lipophilicity and hydrophobicity, can absorb organic matters under the condition of coexisting of oil and water, absorbs benzene reaching 1600% (18mL/g), and is not dissolved in water. An organic phase after the adsorption is in gel state, and can be removed through filtering or similar method so that the aftertreatmetn is simple and convenient.
Description
Technical field
The present invention relates to a kind of porous material and preparation method thereof, relate in particular to styrene diethylene benzene copoly mer of a kind of hydrophobic microporous and preparation method thereof.
Background technology
Benzene is aromatic compound, is colourless liquid under the room temperature, and is inflammable, volatile, contacts excessive benzene and poison easily.And benzene molecular is a kind of common pollutant, and its toxicity, consumption are all bigger, and seeking suitable benzene adsorption material has significant meaning to environmental protection, industrial chemistry etc.Wherein, the method for disposal of benzene leakage accident needs to improve the problem of considering especially.
The emergency disposal conventional method of benzene leakage accident mainly comprises: cut off burning things which may cause a fire disaster, will reveal the contaminated area personnel by speed and withdraw to the safety area, and isolate, strict restriction is come in and gone out.During small leakage, use closed container to collect as far as possible and reveal liquid, absorb raffinate with sand, activated carbon or other inert materials, the emulsion of perhaps using the noninflammability dispersant to make is scrubbed, and puts into waste water system after the washing lotion dilution and handles.During a large amount of the leakage, construct the circle dike or dig pit and accommodate, use foam coverage, reduce the steam disaster or use the spray form water cooling and dilute steam.
After benzene was revealed, a liquid benzene part of oozing out formed liquid pool on ground, generally adopted cotton goods to cover absorption, or used foam coverage to reduce its volatile quantity; A part is infiltrated ground, and when ground was earth, the packaging bag of generally contaminated earth emergence being packed into was transported to the appointed place and handled, and when local plane materiel matter is concrete, generally uses high steam to clean.Simultaneously, when the benzene of revealing with vapor form during to Atmospheric Diffusion, the mode of generally taking to spray spray water cooling and dilution steam in air reduces the pollution of benzene to ambient atmosphere.
In addition, the problem that benzene leaks on the water surface does not have comparatively suitable processing method so far, develop a kind of can be necessary at a large amount of materials that leak benzene of water surface absorption.This material must satisfy following three characteristics, can reach requirement: the first, and this material must can adsorb a large amount of benzene moleculars; The second, this material must be highly hydrophobic, even otherwise adsorbed benzene, also can bring water into, do not reach the separation purpose; The 3rd, this material must be easy to separate from water surface, easily simplifies the follow-up treatment step of absorption.
[Studies in Surface Science and Catalysis such as Guan Lianxiu, 2007,165:885-888.] be the silicon source by hydrogen containing polysiloxane (PMHS) and ethyl orthosilicate (TEOS), under the condition of no template agent, room temperature, synthesized hydrophobic microporous/mesoporous material, though have certain adsorbing separation ability for benzene molecular, but its adsorbance is less, can not satisfy the needs of practical application.
Summary of the invention
The objective of the invention is to disclose a kind of benzene adsorption material and preparation method thereof,, satisfy the needs in relevant field to overcome the above-mentioned defective that prior art exists.
Described benzene adsorption material is styrene diethylene benzene copoly mer, cinnamic quality be divinylbenzene quality 10～30%, the quality of water be divinylbenzene quality 0～100%.
Preferably, cinnamic quality be divinylbenzene quality 20～25%, the quality of water be divinylbenzene quality 0%.
The preparation method of benzene adsorption material involved in the present invention, comprise the steps: that with styrene (St), divinylbenzene (DVB) be monomer, with azodiisobutyronitrile (AIBN) is polymerization initiator, with oxolane (THF) as solvent and template agent, perhaps adding entry again and react, then product is carried out the room temperature vacuum drying as cosolvent, vacuum is-0.06MPa～-0.1MPa, be 8～72 hours drying time, obtains styrene diethylene benzene copoly mer;
The mass ratio of each component is:
Styrene: divinylbenzene: azodiisobutyronitrile: oxolane=0.001～100: 1: 0.001～1: 4～400;
Oxolane and water quality ratio are 10～12: 1;
Reaction temperature is 20～300 ℃, and the reaction time is 1～300 hour;
The present invention's implementation condition preferably is:
The mass ratio of each component is:
Styrene: divinylbenzene: azodiisobutyronitrile: oxolane=0.05～1: 1: 0.05: 20～40.
Reaction temperature is 60～180 ℃, and the reaction time is 12～72 hours.
The addition of monomer styrene can not be too much, and to add the 22～27% better of divinylbenzene quality, preferred 25% is suitable, this moment the adsorbance maximum, and relative cost is lower.
And the adding of water does not have the raising effect to this material absorption benzene.
Method of the present invention, solvent process for thermosynthesizing for a kind of styrene diethylene benzene copoly mer, the material that obtains, have very high lipophile and hydrophobicity, can be under the situation of oil-water coexistence adsorb organic compound, the adsorbance of benzene is reached 1600% (18mL/g), and it is water insoluble, organic facies after the absorption is a gel, can remove by filtration or similar approach, and post processing is easy.
Description of drawings
Fig. 1 is thermogravimetric analysis (TGA) figure of the product of embodiment 1.
Fig. 2 is adsorption-desorption thermoisopleth (BET) figure of the product of embodiment 1.
Fig. 3 is transmission electron microscope (TEM) figure of the product of embodiment 1.
Fig. 4 is the variation relation figure of benzene adsorbance with different materials.
Fig. 5 is the swelling ratio comparison diagram of sorbing material.
The specific embodiment
Following example will be described further the synthetic method of benzene adsorption material provided by the invention.The implication of the symbol that uses in following examples is:
With DVB is quality criteria 1, and the quality relative scale of unclassified stores and DVB is the numeral of its front.
Embodiment 1
With 2g divinylbenzene, 0.5g styrene as monomer, 0.1g azodiisobutyronitrile is as initator, 26.6g oxolane is as solvent and template agent, at room temperature stir and made its abundant mixing in 5 hours, change over to then in the polytetrafluoroethylene (PTFE) reactor, reactor is placed in 120 ℃ the baking oven, leaves standstill solvent thermal reaction 48h.Reactor is taken out, vacuum is-0.08MPa under room temperature vacuum drying 48h, obtain DVB-0.25St.
The thermogravimetric analysis of product (TGA) figure sees Fig. 1, and adsorption-desorption thermoisopleth (BET) figure of product sees Fig. 2.The transmission electron microscope of product (TEM) figure sees Fig. 3.As seen from Figure 3, this material is a loose structure.
The benzene adsorbance adopts following method to detect, and testing result is seen Fig. 4.
At first take by weighing the sorbing material of certain mass, place beaker; Add benzene to be adsorbed then in batches gradually, after each the adding, allow it fully adsorb, add next group benzene again after absorption is finished; So circulation can not be adsorbed (remaining benzene is promptly arranged) up to this material fully to benzene, and write down the content of organics of adding this moment, can obtain the adsorbance of this material to benzene.
Swelling ratio adopts following method to detect, and the results are shown in Figure 5.
At first testing sample is ground into uniform powder, places graduated cylinder, read volume V1; Next adds a certain amount of organic matter, allows it fully adsorb and swelling; After treating that then absorption is stable, read volume V2; Can obtain the swelling ratio of this material at last with V2/V1.
Embodiment 2
With 2g divinylbenzene, 0.5g styrene as monomer, 0.1g azodiisobutyronitrile is as initator, 26.6g oxolane is as solvent and template agent, 2g water at room temperature stirred mixing 5 hours as cosolvent, change over to then in the polytetrafluoroethylene (PTFE) reactor, reactor is placed in 120 ℃ the baking oven, leaves standstill solvent thermal reaction 48h.Reactor is taken out, vacuum is-0.08MPa under room temperature vacuum drying 48h, obtain DVB-0.25 St-H
2O.
Detection method is with embodiment 1.
Swelling ratio the results are shown in Figure 5.
Benzene adsorbance testing result is seen Fig. 4.
Embodiment 3
With 2g divinylbenzene, 0.5g styrene as monomer, 0.1g azodiisobutyronitrile is as initator, 26.6g oxolane is as solvent and template agent, at room temperature stir and made its abundant mixing in 5 hours, change over to then in the polytetrafluoroethylene (PTFE) reactor, reactor is placed in 120 ℃ the baking oven, leaves standstill solvent thermal reaction 48h.Reactor is taken out, and standing and drying in the air at room temperature obtains DVB-0.25St-air.
Detection method is with embodiment 1.
Swelling ratio the results are shown in Figure 5.
Benzene adsorbance testing result is seen Fig. 4.
Claims (10)
1. benzene adsorption material is characterized in that, is styrene diethylene benzene copoly mer, cinnamic quality be divinylbenzene quality 10～30%, the quality of water be divinylbenzene quality 0～100%.
2. benzene adsorption material according to claim 1 is characterized in that, cinnamic quality be divinylbenzene quality 20～25%, the quality of water be divinylbenzene quality 0%.
3. the preparation method of benzene adsorption material, it is characterized in that, comprise the steps: that with styrene, divinylbenzene be monomer, with the azodiisobutyronitrile is polymerization initiator, with oxolane as solvent and template agent, perhaps add entry again and react, then product is carried out vacuum drying, obtain styrene diethylene benzene copoly mer as cosolvent.
4. method according to claim 3 is characterized in that, mass ratio is: styrene: divinylbenzene=0.001～100: 1.
5. method according to claim 3 is characterized in that, mass ratio is: styrene: divinylbenzene=0.05～1: 1.
6. method according to claim 3 is characterized in that, the mass ratio of each component is:
Styrene: divinylbenzene: azodiisobutyronitrile: oxolane=0.001～100: 1: 0.001～1: 4～400.
7. method according to claim 3 is characterized in that, the mass ratio of each component is: styrene: divinylbenzene: azodiisobutyronitrile: oxolane=0.05～1: 1: 0.05: 20～40.
8. according to the described method of claim 3, it is characterized in that reaction temperature is 20～300 ℃, the reaction time is 1～300 hour.
9. method according to claim 3 is characterized in that, reaction temperature is 60～180 ℃, and the reaction time is 12～72 hours.
10. according to each described method of claim 3～9, it is characterized in that, during vacuum drying, vacuum is-0.06MPa～-0.1MPa, be 8～72 hours drying time.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108745314A (en) * | 2018-06-15 | 2018-11-06 | 广州市环境保护设备厂有限公司 | A kind of polystyrene crosslinked divinylbenzene resin honeycomb ceramics and preparation method thereof |
| CN108940230A (en) * | 2018-06-15 | 2018-12-07 | 广州市环境保护设备厂有限公司 | A kind of polystyrene crosslinked divinylbenzene cylindrical particle and preparation method thereof adsorbing VOCs |
| CN110331303A (en) * | 2019-08-13 | 2019-10-15 | 包头稀土研究院 | The method of heavy rare earth chloride solution in continuous extraction separation |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108745314A (en) * | 2018-06-15 | 2018-11-06 | 广州市环境保护设备厂有限公司 | A kind of polystyrene crosslinked divinylbenzene resin honeycomb ceramics and preparation method thereof |
| CN108940230A (en) * | 2018-06-15 | 2018-12-07 | 广州市环境保护设备厂有限公司 | A kind of polystyrene crosslinked divinylbenzene cylindrical particle and preparation method thereof adsorbing VOCs |
| CN108940230B (en) * | 2018-06-15 | 2019-10-25 | 广东龙贲环境设计院有限公司 | A kind of polystyrene crosslinked divinylbenzene cylindrical particle and preparation method thereof adsorbing VOCs |
| CN108745314B (en) * | 2018-06-15 | 2019-10-29 | 广州市环境保护设备厂有限公司 | A kind of polystyrene crosslinked divinylbenzene resin honeycomb ceramics and preparation method thereof |
| CN110331303A (en) * | 2019-08-13 | 2019-10-15 | 包头稀土研究院 | The method of heavy rare earth chloride solution in continuous extraction separation |
| CN110331303B (en) * | 2019-08-13 | 2022-03-18 | 包头稀土研究院 | Method for continuously extracting and separating medium-heavy rare earth chloride solution |
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Application publication date: 20101103 |