CN103203226A - Graphite powder-butyl rubber composite frozen gel oil absorption material and preparation method thereof - Google Patents
Graphite powder-butyl rubber composite frozen gel oil absorption material and preparation method thereof Download PDFInfo
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- CN103203226A CN103203226A CN2013101536844A CN201310153684A CN103203226A CN 103203226 A CN103203226 A CN 103203226A CN 2013101536844 A CN2013101536844 A CN 2013101536844A CN 201310153684 A CN201310153684 A CN 201310153684A CN 103203226 A CN103203226 A CN 103203226A
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- butyl rubber
- graphite powder
- oil absorption
- absorption material
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Abstract
The invention relates to a graphite powder-butyl rubber composite frozen gel oil absorption material and a preparation method thereof. The oil absorption material is crosslinked with butyl rubber under the action of S2Cl2 serving as a cross-linking agent to form a three-dimensional net porous gel material with intercommunicated pore structure, wherein the aperture is 20-50 microns; the thickness of the pore wall is 20-30 microns; the graphite powder is evenly dispersed into the three-dimensional net porous gel material; the mass of the graphite powder is 0.5-2% of that of butyl rubber; and the volume mass ratio of the cross-linking agent to butyl rubber is 6ml to 100g. The composite material disclosed by the invention is small in density, large in adsorption capacity and fast in adsorption speed, can absorb various oil products, can be repeatedly used by simple centrifuging or extruding treatment, effectively reduces the cost, and is a novel environment-friendly material. The composite frozen gel oil absorption material is wide in application, and can be used as a slow-release base material, a filter material and the like except for recovery of water oil spilling at sea or land and oily wastewater treatment.
Description
Technical field
The present invention relates to a kind of freezing gel oil absorption material and preparation method thereof, be specifically related to a kind of graphite powder-butyl rubber composite frozen gel oil absorption material and preparation method thereof.
Background technology
In recent years, oil carrier, tank leakage accident, comprise oil-containing or other insoluble organic matter sewage emissions, chemicals such as large chemical plant, industrial chemicals warehouse are concentrated the generation of storing the ground accident, cause serious pollution for soil, river, ocean and surrounding enviroment, become serious day by day problem.
For the sump oil that leaks into environment being carried out handle rapidly effectively, it is minimum that sump oil is dropped to the pollution of environment, simultaneously, in order to eliminate life with the oily environmental pollution that causes, presses for and develop oil absorption material efficiently.Natural oil absorption material such as string, wool fiber, bentonite, vermiculite, perlite etc., have that the rate of adsorption is slow, profit selectively bad, protect shortcomings such as oily rate is low.
The oil absorption material of chemical synthesis is substantially based on high molecular polymer, as efficient oil-absorbing resin, this low crosslinking degree copolymer that is constituted by several monomers, intermolecular have a three-dimensional cross-linked network structure, there is certain hole inside, and the solvation by lipophilic groups a large amount of on the macromolecular chain and oil molecule expands resin.Because the existence of cross-linked network, when crosslinking degree is suitable, a resin swelling and not dissolving, oil molecule then is wrapped in the macromolecular network structure, thereby reaches the oil suction purpose.But oil-absorbing resin mostly is bulk or graininess, and this class material exists and is not easy to reuse, and the difficult treatment of draining the oil of the resin after the oil suction is restricted its application.
At present using the most general asphalt felt is the superfine fibre sorbing material of making as raw material with polypropylene, and be applicable to the oil spill accident of handling large tracts of land crude oil, but also have many shortcomings in use: the processing time is longer, can not reuse.Therefore, need provide a kind of shortcoming that can overcome above-mentioned oil absorption material, have high oil absorption, fast can reusable high-capacity oil absorption material after oil suction and the oil suction.
Summary of the invention
One of purpose of the present invention is the defective at prior art, and a kind of graphite powder-butyl rubber freezing gel compound oil absorption material is provided..
Two of purpose of the present invention is to provide the synthetic method of this oil absorption material.
For achieving the above object, the present invention adopts following technical scheme:
A kind of graphite powder-butyl rubber composite frozen gel oil absorption material is characterized in that this oil absorption material is with S
2Cl
2Be crosslinking agent, butyl rubber is cross-linked to form the three-dimensional netted type porous gel material of the mutual UNICOM of a kind of pore structure, and wherein the aperture is 20 μ m ~ 50 μ m, thick 20 ~ 30 μ m of hole wall; Graphite powder is dispersed in the described three-dimensional netted type porous gel material, and the quality of described graphite powder is 0.5 ~ 2% of butyl rubber quality; Crosslinking agent is 6ml:100g with butyl rubber volume mass ratio.
The degree of unsaturation 1.5 ~ 1.9% of above-mentioned butyl rubber.
A kind of method for preparing above-mentioned graphite powder-butyl rubber composite frozen gel oil absorption material is characterized in that steps of the method are:
A is dissolved in the solvent under room temperature stirring and dissolving to evenly with butyl rubber, and obtaining mass volume ratio is the butyl rubber solution of 5g:100ml;
B. be dispersed in the step a gained solution graphite powder is ultrasonic, add crosslinking agent down in stirring again, in-20 ~-2 ℃ of scopes, reacted 24 hours, obtain the composite gel material in different apertures;
C. the resulting composite gel material of step b is heated up under room temperature and thaw, with composite gel material toluene, the alternately washing of methyl alcohol of cross moulding; Pass through drying at room temperature again, namely obtain graphite powder-butyl rubber composite frozen gel oil absorption material.
Above-mentioned solvent is benzene or cyclohexane.
Studies show that the shaping of freezing gel material is subjected to many condition effect.Wherein the percentage of butyl rubber lowly excessively cause that the strength of materials is low, too soft, reuse easy fracture often the time; Percentage is too high then can to cause shortcomings such as material densification, swelling weak effect, oil absorbency be low.Solvent is selected benzene (5.5 ℃ of fusing points) or cyclohexane (6.5 ℃ of fusing points) for use, and when the reaction temperature system is lower than the solvent fusing point, solvent can freeze and form the ice crystal pore.Graphite powder add the swelling that too much can influence material, so be advisable with 0.5 ~ 1.0% (w/w).Reaction temperature is spent when low, and the material pore-forming is inhomogeneous, so be the best with-5 ~-2 ℃.
The graphite powder of the inventive method manufacturing-butyl rubber freezing gel composite is the porous gel material of black, and after measured, its pore size is 20 μ m ~ 50 μ m, thick about 20 ~ 30 μ m of hole wall.
This aspect technology is simple, and it is fast to be shaped, the output height; Prepared material has that good profit is selective, and density is little, and adsorption capacity is big, and absorption as crude oil, diesel oil, gasoline, the lubricated multiple oil product of wet goods are all right recycling.
It is little that sorbing material of the present invention has density, and adsorption capacity is big, the characteristics that the rate of adsorption is fast.Energy absorption can be repeatedly used through simple centrifugal or extrusion process, and number of repetition is also not reduction of oil absorbency more than 20 times.The oil product that squeezes out can be collected recycling.Can be used for sea or the recovery of land water body oil spilling, the processing of oily waste water etc.
Sorbing material of the present invention is adsorbable organic matter also, and had good sustained release effect.Can be used as effective carrier materials such as aromatic, attractant, insecticide etc.
Description of drawings
The oil absorbency resolution chart of the oil absorption material that Fig. 1 embodiment of the invention 1 is made.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these examples of implementation are used for explanation the present invention, limit the scope of the invention and be not used in.Should be understood that in addition those skilled in the art can make various changes or modification to the present invention after having read the content that the present invention tells about, these equivalent form of values fall within the described power of the application equally must ask book institute restricted portion.
Embodiment 1
(1) butyl rubber is shredded, take by weighing 5g(5%, w/v) be dissolved in the 100mL benzene and add stirrer, under magnetic agitation, react and spend the night, the benzole soln of rubber is uniformly dispersed.
(2) take by weighing 0.025 g(0.5%, w/w) graphite powder carries out ultrasonic dispersion with 10mL benzene, pours in the above-mentioned reactant liquor, stirs.Under agitation dropwise add crosslinking aid S then
2Cl
23.0mL (6 % v/w), are filled to the mixed liquor branch in the tool plug test tube, build the back and react 24 hours under-5 ℃ in the cryogenic thermostat reactive tank.
(3) take out test tube after reaction is finished, dissolved under the room temperature 30 minutes.Solvent benzol in the material is extruded, and used toluene, methyl alcohol is washing alternately, at least respectively washes 2 times.
(4) dry in fume hood under the room temperature, namely get described oil absorption material.
Oil absorption material with the abundant drying of gained is dipped in the water, and the water absorption rate that can calculate material is 0.46g/g.Because material is non-solvent swelling state in methyl alcohol, so material is dipped in the methyl alcohol, calculate the weight difference before and after soaking, obtain the methyl alcohol weight in the hole.According to the density (0.792g/mL) of methyl alcohol, the porosity that can calculate material is 3.78mL/g again.Measure material to the absorption of various oil products with weight fraction respectively again, obtain its maximal absorptive capacity for diesel oil, crude oil, lubricating oil and can reach 19.12g/g respectively, 18.56g/g and 19.10g/g.Oil suction (water) rate and porosity calculating method are as follows:
Oil suction (water) rate=(W
2-W
1)/W
1
Porosity=(W
m-W
Dry)/0.792W
Dry
W wherein
1With W
2Be respectively the preceding weight of material oil suction (water) and absorption back weight, W
DryWith W
mWeight after being respectively the preceding dry weight of material absorption and adsorbing methyl alcohol.
Embodiment 2
(1) butyl rubber is shredded, take by weighing 5g(5 %, w/v) be dissolved in the 100mL benzene and add stirrer, under magnetic agitation, react and spend the night, the benzole soln of rubber is uniformly dispersed.
(2) take by weighing 0.05g(1%, w/w) graphite powder carries out ultrasonic dispersion with 10mL benzene, pours in the above-mentioned reactant liquor, stirs.Under agitation dropwise add crosslinking aid S then
2Cl
23.0mL (6 % v/w), are filled to the mixed liquor branch in the tool plug test tube, build the back and react 24 hours under-2 ℃ in the cryogenic thermostat reactive tank.
(3) take out test tube after reaction is finished, dissolved under the room temperature 30 minutes.Solvent benzol in the material is extruded, and used toluene, methyl alcohol is washing alternately, at least respectively washes 2 times.
(4) dry in fume hood under the room temperature, namely get described oil absorption material.
Oil absorption material with the abundant drying of gained is dipped in respectively in water and the methyl alcohol, and the water absorption rate that can calculate material is 0.25g/g, and porosity is 4.04mL/g.Measure this material respectively to the adsorption capacity of various oil products with gravimetric method respectively again, obtain its maximal absorptive capacity for diesel oil, crude oil, lubricating oil and can reach 18.66g/g respectively, 19.86g/g and 19.50g/g.Oil absorption is strong, and oil suction is effective.
Claims (4)
1. graphite powder-butyl rubber composite frozen gel oil absorption material is characterized in that this oil absorption material is with S
2Cl
2Be crosslinking agent, butyl rubber is cross-linked to form the three-dimensional netted type porous gel material of the mutual UNICOM of a kind of pore structure, and wherein the aperture is 20 μ m ~ 50 μ m, thick 20 ~ 30 μ m of hole wall; Graphite powder is dispersed in the described three-dimensional netted type porous gel material, and the quality of described graphite powder is 0.5 ~ 2% of butyl rubber quality; Crosslinking agent is 6ml:100g with butyl rubber volume mass ratio.
2. graphite powder according to claim 1-butyl rubber composite frozen gel oil absorption material is characterized in that the degree of unsaturation 1.5 ~ 1.9% of described butyl rubber.
3. method for preparing graphite powder according to claim 1 and 2-butyl rubber composite frozen gel oil absorption material is characterized in that steps of the method are:
A is dissolved in the solvent under room temperature stirring and dissolving to evenly with butyl rubber, and obtaining mass volume ratio is the butyl rubber solution of 5g:100ml;
B. be dispersed in the step a gained solution graphite powder is ultrasonic, add crosslinking agent down in stirring again, in-20 ~-2 ℃ of scopes, reacted 24 hours, obtain the composite gel material in different apertures;
C. the resulting composite gel material of step b is heated up under room temperature and thaw, with composite gel material toluene, the alternately washing of methyl alcohol of cross moulding; Pass through drying at room temperature again, namely obtain graphite powder-butyl rubber composite frozen gel oil absorption material.
4. method according to claim 3 is characterized in that described solvent is benzene or cyclohexane.
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| CN2013101536844A CN103203226A (en) | 2013-04-28 | 2013-04-28 | Graphite powder-butyl rubber composite frozen gel oil absorption material and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103834047A (en) * | 2014-03-11 | 2014-06-04 | 武汉工程大学 | Butyl rubber composite gel oil absorption material and preparation method thereof |
| CN106669629A (en) * | 2016-12-26 | 2017-05-17 | 上海大学 | Styrene/butadienyl freezing gel adsorbing material and preparation method thereof |
| CN110092927A (en) * | 2019-05-30 | 2019-08-06 | 晋江成昌鞋业有限公司 | The preparation method of lightweight rubber composite elastic body |
| CN111426734A (en) * | 2020-04-30 | 2020-07-17 | 榆林学院 | Nano Cu/graphene composite material modified electrode, preparation method thereof and application of nano Cu/graphene composite material modified electrode in detection of hydroquinone |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1324380A (en) * | 1998-10-29 | 2001-11-28 | 宾立可合伙公司 | Gel composition |
| CN102250425A (en) * | 2011-05-24 | 2011-11-23 | 深圳市博恩实业有限公司 | Multifunctional heat-conducting composite material |
| CN102952042A (en) * | 2012-11-14 | 2013-03-06 | 江苏泰仓农化有限公司 | Synthesis process of novel synthetic rubber accelerator N-cyclohexylurea |
-
2013
- 2013-04-28 CN CN2013101536844A patent/CN103203226A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1324380A (en) * | 1998-10-29 | 2001-11-28 | 宾立可合伙公司 | Gel composition |
| CN102250425A (en) * | 2011-05-24 | 2011-11-23 | 深圳市博恩实业有限公司 | Multifunctional heat-conducting composite material |
| CN102952042A (en) * | 2012-11-14 | 2013-03-06 | 江苏泰仓农化有限公司 | Synthesis process of novel synthetic rubber accelerator N-cyclohexylurea |
Non-Patent Citations (1)
| Title |
|---|
| YAN HU ET AL.: "Graphite/Isobutylene-isoprene Rubber Highly Porous Cryogels as New Sorbents for Oil Spills and Organic Liquids", 《ACS APPLIED MATERIALS & INTERFACES》, vol. 5, no. 16, 11 February 2013 (2013-02-11) * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103834047A (en) * | 2014-03-11 | 2014-06-04 | 武汉工程大学 | Butyl rubber composite gel oil absorption material and preparation method thereof |
| CN106669629A (en) * | 2016-12-26 | 2017-05-17 | 上海大学 | Styrene/butadienyl freezing gel adsorbing material and preparation method thereof |
| CN110092927A (en) * | 2019-05-30 | 2019-08-06 | 晋江成昌鞋业有限公司 | The preparation method of lightweight rubber composite elastic body |
| CN111426734A (en) * | 2020-04-30 | 2020-07-17 | 榆林学院 | Nano Cu/graphene composite material modified electrode, preparation method thereof and application of nano Cu/graphene composite material modified electrode in detection of hydroquinone |
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Application publication date: 20130717 |