CN103044626B - Super-oil-absorption rubber material and preparation method thereof - Google Patents
Super-oil-absorption rubber material and preparation method thereof Download PDFInfo
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- CN103044626B CN103044626B CN201110314157.8A CN201110314157A CN103044626B CN 103044626 B CN103044626 B CN 103044626B CN 201110314157 A CN201110314157 A CN 201110314157A CN 103044626 B CN103044626 B CN 103044626B
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Abstract
The invention relates to a super-oil-absorption rubber material and a preparation method thereof. The super-oil-absorption rubber material is prepared from the following raw materials in parts by mass: 30-80 parts of rubber, 20-50 parts of crosslinking monomer, 0.05-5 parts of crosslinking agent, 0.1-5 parts of initiator, 0.2-2 parts of dispersing agent, 180-500 parts of dispersion medium and 180-500 parts of solvent. The preparation method comprises the following steps: adding the rubber and crosslinking monomer into the solvent, heating to 40-90 DEG C, keeping the temperature for 10-30 minutes, cooling to 38-42 DEG C, adding the dispersing agent, stirring at constant temperature for 0.5-2 hours, heating to 60-90 DEG C, adding the crosslinking agent and initiator, stirring for 2-6 hours, cooling to 38-42 DEG C, adding the dispersion medium, continuing stirring for 0.5-2 hours, cooling to 25 DEG C, filtering, washing the product with acetone and tetrahydrofuran once, and carrying out vacuum drying to obtain the material of which the solubility parameter is most approximate to that of the oil product. The invention greatly enhances the oil absorption factor and rate, so that the oil absorption factor is three times of the prior art. The preparation method is simple and easy to operate. The super-oil-absorption rubber material can be used for absorbing crude oil, gasoline, illegal cooking oil, lubricating oil and mechanical waste oil, and has wide application prospects.
Description
Technical field
The present invention relates to a kind of super oil suction elastomeric material and preparation method thereof.
Background technology
In recent years, day by day frequent along with mankind's activity, the seriously polluted of water body is caused by a series of accidents such as oil field leakage, oil carrier leakage of oil, pipeline road break and containing the discharge of oil-polluted water waste liquid, bring immeasurable eco-catastrophe and financial loss, the Bohai Sea Gulf leakage of oil event of such as U.S. Mexico gulf and China.Therefore, urgently human development low cost, the super oil absorption material of superelevation oil number, makes it fast processing water surface greasy dirt in severe environment.
The polymkeric substance of the more high oil-absorbent material of current research low cross-linking often, it is with lipophilicity monomer for fundamental unit, and through appropriately crosslinked formation three-dimensional net structure, the oil of absorption is kept in this network with Van der Waals force.Compared with traditional oil absorption material, this exotic material oil suction multiplying power is high, oil-water selectivity good, and Oil keeping can improve greatly, not easily leakage of oil again, is a kind of high performance type material.But the oil absorption material oil suction multiplying power of exploitation is still not high at present, swelling rate is slow, reversibility difference is drained the oil in suction.A kind of high oil absorbing resin based on rubber that such as Chinese patent CN200610027826.2 develops be with rubber and ring-alkylated styrenes be matrix, the oil absorption material that synthesizes for linking agent of Vinylstyrene or diacrylate, it is up to 51 to the oil absorbency of tetracol phenixin, is up to 25 to the oil absorbency of hexanaphthene; Mitsui petroleum chemistry company take alkyl methacrylate as monomer, Vinylstyrene is the oil absorption material (Japanese Laid-Open Patent Publication 50-15882, Japanese Laid-Open Patent Publication 50-59486, Japanese Laid-Open Patent Publication 50-94092) of linking agent, and its oil suction multiplying power is very low; Catalyst chemical company of Japan take long-chain aliphatic acrylate as monomer, and diacrylate diol ester is that the highest oil suction multiplying power of oil absorption material of linking agent is also only 25.The subject matter that above-mentioned oil absorption material oil absorbency is not high is not design the solubility parameter of the oil absorption material of synthesis, therefore optimum oil suction ratio cannot be obtained, and single employing rubber can cause crosslinked too low material oil suction after easily broken, crosslinked too high oil suction multiplying power is too low, single employing acrylate monomer cannot obtain high oil suction multiplying power, therefore, the present invention is according to the solubility parameter of oil product, by with rubber and isobornyl acrylate or ethylidene norbornene for monomer, the solubility parameter of design and synthesis material, synthesize the super oil absorption material with superelevation oil suction multiple.
Summary of the invention
First technical problem to be solved by this invention is to provide a kind of super oil suction elastomeric material, pass through molecular designing, obtain the material of solubility parameter closest to oil product solubility parameter, namely snappiness and the extensibility of rubber segment is provided with, be provided with again cross-linking monomer intensity, there is the oil suction multiple of superelevation.
Second technical problem to be solved by this invention is to provide a kind of preparation method of super oil suction elastomeric material, and preparation technology is simple, and obtained material has superelevation oil suction multiple.
The present invention solves the technical scheme that above-mentioned first technical problem adopt: a kind of super oil suction elastomeric material, is characterized in that it contains the raw material of following mass fraction:
Rubber 30-80 part,
Cross-linking monomer 20-50 part,
Linking agent 0.05-5 part,
Initiator 0.1-5 part,
Dispersion agent 0.2-2 part,
Dispersion medium 180-500 part,
Solvent 180-500 part;
The molecular weight of wherein said rubber is preferably 800-600000, is preferably the mixture of one or more in terpolymer EP rubber, isoprene-isobutylene rubber, styrene-butadiene rubber(SBR), natural rubber, chloroprene rubber or divinyl rubber.
As preferably, described cross-linking monomer is isobornyl acrylate or ethylidene norbornene.
Described linking agent is Vinylstyrene.
Described initiator is dichloroazodicarbonamide or tert-butyl peroxide.
Described dispersion agent is one or more mixtures in gelatin, pectin or carrageenin.
Described dispersion medium is deionized water or pure water.
Described solvent is one or more mixtures in benzene,toluene,xylene, normal hexane, hexanaphthene, normal heptane, isoheptane, octane, octane-iso, glycerine or paraffin.
Further preferably, described solvent is one or more mixtures in toluene, dimethylbenzene, normal hexane or hexanaphthene.
Finally, described super oil suction elastomeric material is membranoid substance, its solubility parameter be no more than 0.5 by the difference of the solubility parameter of oil suction product, the high molecular crosslink system of rubber, cross-linking monomer and linking agent.
The present invention solves the technical scheme that above-mentioned second technical problem adopt: a kind of preparation method of super oil suction elastomeric material, is characterized in that step is followed successively by:
1) weighing proportioning is carried out by the mass fraction of following component:
Rubber 30-80 part,
Cross-linking monomer 20-50 part,
Linking agent 0.05-5 part,
Initiator 0.1-5 part,
Dispersion agent 0.2-2 part,
Dispersion medium 180-500 part,
Solvent 180-500 part;
2) rubber and cross-linking monomer are added in solvent, be warming up to 40-90 DEG C, after constant temperature 10-30 minute, be cooled to 38 ~ 42 DEG C, add dispersion agent, constant temperature stirred after 0.5-2 hour, was warming up to 60-90 DEG C, added linking agent, initiator, stir 2-6 hour, after being cooled to 38 ~ 42 DEG C, add dispersion medium, continue to stir 0.5-2 hour;
3) be cooled to room temperature, filter, product acetone and tetrahydrofuran (THF) cleaning, namely vacuum-drying obtain super oil suction elastomeric material.
Compared with prior art, the invention has the advantages that: pass through molecular designing, obtain the material of solubility parameter closest to oil product solubility parameter, obtained by the selection of monomer and have snappiness concurrently, the three-dimensional net structure of extensibility and intensity, the oil suction multiplying power solving the existence of existing oil absorption material is low, swelling rate is slow, cost is higher, the problems such as Oil keeping difference, substantially increase oil suction multiplying power and speed, oil suction multiplying power is made to reach 3 times of prior art, preparation method is simple simultaneously, easy to operate, can be used for crude oil, gasoline, sewer oil, lubricating oil, the absorption of waste machine oil, be with a wide range of applications.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail.
Embodiment 1:
Its component, mass fraction and preparation method are as follows:
(1) molecular designing.
Terpolymer EP rubber 30 parts
Isobornyl acrylate monomer 50 parts
Vinylstyrene 0.05 part
Solubility parameter is 7.48, and n-hexane dissolution degree parameter is 7.3, and Xylene solubility parameter is 8.8, and wherein n-hexane dissolution degree parameter is within ± 0.5, belongs to and easily absorbs oil product.
(2) preparation process.
Dichloroazodicarbonamide 0.1 part
0.2 part, gelatin
Deionized water 180 parts
Solvent 180 parts, (wherein dimethylbenzene 90 parts, normal hexane 90 parts)
Terpolymer EP rubber and isobornyl acrylate monomer are added in solvent, be warming up to 40 DEG C, constant temperature, after 10 minutes, adds dispersion agent, after stirring 0.5 hour at 40 DEG C, be warming up to 60 DEG C, add linking agent, initiator, stir 2 hours, after being cooled to 40 DEG C, add dispersion medium, continue stirring 0.5 hour.
(3) last handling process
Be cooled to 25 DEG C, filter, product acetone and tetrahydrofuran (THF) are respectively washed once, vacuum-drying.Resulting materials is membranoid substance.
It is 69.3 to the oil suction multiplying power of normal hexane, and the oil suction multiplying power of p-Xylol is 35.2, and unit is (g/g).
Embodiment 2:
Its component, mass fraction and preparation method are as follows:
(1) molecular designing.
Terpolymer EP rubber 80 parts
Isobornyl acrylate monomer 20 parts
Vinylstyrene 5 parts
Solubility parameter is 7.75, and n-hexane dissolution degree parameter is 7.3, and Xylene solubility parameter is 8.8, and wherein n-hexane dissolution degree parameter is within ± 0.5, belongs to and easily absorbs oil product.
(2) preparation process.
Tert-butyl peroxide 5 parts
Pectin 2 parts
Pure water 500 parts
Solvent 500 parts (wherein toluene 250 parts, hexanaphthene 250 parts)
Terpolymer EP rubber and isobornyl acrylate monomer are added in solvent, be warming up to 90 DEG C, constant temperature, after 30 minutes, is cooled to 40 DEG C, add dispersion agent, after stirring 2 hours at 40 DEG C, be warming up to 90 DEG C, add linking agent, initiator, stir 6 hours, after being cooled to 40 DEG C, add dispersion medium, continue stirring 2 hours.
(3) last handling process
Be cooled to 25 DEG C, filter, product acetone and tetrahydrofuran (THF) are respectively washed once, vacuum-drying.Resulting materials is membranoid substance.
It is 54.3 to the oil suction multiplying power of normal hexane, and the oil suction multiplying power of p-Xylol is 39.7, and unit is (g/g).
Embodiment 3:
(1) molecular designing.
Terpolymer EP rubber 55 parts
Isobornyl acrylate monomer 35 parts
Vinylstyrene 2.5 parts
Solubility parameter is 7.54, and n-hexane dissolution degree parameter is 7.3, and Xylene solubility parameter is 8.8, and wherein n-hexane dissolution degree parameter is within ± 0.5, belongs to and easily absorbs oil product.
(2) preparation process.
Dichloroazodicarbonamide 2.5 parts
Carrageenin 1 part
Deionized water 330 parts
Solvent 350 parts (wherein dimethylbenzene 100 parts, normal hexane 150 parts, hexanaphthene 150 parts)
Terpolymer EP rubber and isobornyl acrylate monomer are added in solvent, be warming up to 65 DEG C, constant temperature, after 20 minutes, is cooled to 40 DEG C, add dispersion agent, after stirring 1 hour at 40 DEG C, be warming up to 75 DEG C, add linking agent, initiator, stir 4 hours, after being cooled to 40 DEG C, add dispersion medium, continue stirring 1 hour.
(3) last handling process
Be cooled to 25 DEG C, filter, product acetone and tetrahydrofuran (THF) are respectively washed once, vacuum-drying.Resulting materials is membranoid substance.
It is 61.0 to the oil suction multiplying power of normal hexane, and the oil suction multiplying power of p-Xylol is 37.4, and unit is (g/g).
Embodiment 4:
Its component, mass fraction and preparation method are as follows:
(1) molecular designing.
55 parts, styrene-butadiene rubber(SBR)
Ethylidene norbornene monomer 35 parts
Vinylstyrene 2.5 parts
Solubility parameter is 7.49, and n-hexane dissolution degree parameter is 7.3, and Xylene solubility parameter is 8.8, and wherein n-hexane dissolution degree parameter is within ± 0.5, belongs to and easily absorbs oil product.
(2) preparation process.
Tert-butyl peroxide 2 parts
1 part, gelatin
Deionized water 300 parts
Solvent 350 parts (wherein dimethylbenzene 170 parts, normal hexane 180 parts)
Styrene-butadiene rubber(SBR) and ethylidene norbornene monomer are added in solvent, be warming up to 55 DEG C, constant temperature, after 20 minutes, is cooled to 40 DEG C, add dispersion agent, after stirring 1 hour at 40 DEG C, be warming up to 75 DEG C, add linking agent, initiator, stir 4 hours, after being cooled to 40 DEG C, add dispersion medium, continue stirring 1 hour.
(3) last handling process
Be cooled to 25 DEG C, filter, product acetone and tetrahydrofuran (THF) are respectively washed once, vacuum-drying.Resulting materials is membranoid substance.
It is 81.1 to the oil suction multiplying power of normal hexane, and the oil suction multiplying power of p-Xylol is 49.3, and unit is (g/g).
Embodiment 5:
Its component, mass fraction and preparation method are as follows:
(1) molecular designing.
Isoprene-isobutylene rubber 55 parts
Ethylidene norbornene monomer 35 parts
Vinylstyrene 2.5 parts
Solubility parameter is 7.45, and n-hexane dissolution degree parameter is 7.3, and Xylene solubility parameter is 8.8, and wherein n-hexane dissolution degree parameter is within ± 0.5, belongs to and easily absorbs oil product.
(2) preparation process.
Tert-butyl peroxide 2 parts
1 part, gelatin
Deionized water 300 parts
Solvent 350 parts (wherein dimethylbenzene 170 parts, normal hexane 180 parts)
Isoprene-isobutylene rubber and ethylidene norbornene monomer are added in solvent, be warming up to 55 DEG C, constant temperature, after 20 minutes, is cooled to 40 DEG C, add dispersion agent, after stirring 1 hour at 40 DEG C, be warming up to 75 DEG C, add linking agent, initiator, stir 4 hours, after being cooled to 40 DEG C, add dispersion medium, continue stirring 1 hour.
(3) last handling process
Be cooled to 25 DEG C, filter, product acetone and tetrahydrofuran (THF) are respectively washed once, vacuum-drying.Resulting materials is membranoid substance.
It is 76.5 to the oil suction multiplying power of normal hexane, and the oil suction multiplying power of p-Xylol is 30.3, and unit is (g/g).
Embodiment 6:
Its component, mass fraction and preparation method are as follows:
(1) molecular designing.
Natural rubber 55 parts
Isobornyl acrylate monomer 35 parts
Vinylstyrene 2.5 parts
Solubility parameter is 7.79, and n-hexane dissolution degree parameter is 7.3, and Xylene solubility parameter is 8.8, and wherein n-hexane dissolution degree parameter is within ± 0.5, belongs to and easily absorbs oil product.
(2) preparation process.
Tert-butyl peroxide 2 parts
1 part, gelatin
Deionized water 300 parts
Solvent 350 parts (wherein dimethylbenzene 170 parts, normal hexane 180 parts)
Natural rubber and isobornyl acrylate monomer are added in solvent, be warming up to 55 DEG C, constant temperature, after 20 minutes, is cooled to 40 DEG C, add dispersion agent, after stirring 1 hour at 40 DEG C, be warming up to 75 DEG C, add linking agent, initiator, stir 4 hours, after being cooled to 40 DEG C, add dispersion medium, continue stirring 1 hour.
(3) last handling process
Be cooled to 25 DEG C, filter, product acetone and tetrahydrofuran (THF) are respectively washed once, vacuum-drying.Resulting materials is membranoid substance.
It is 40.9 to the oil suction multiplying power of normal hexane, and the oil suction multiplying power of p-Xylol is 45.6, and unit is (g/g).
Above-mentioned experimental result shows, has good oil absorptiveness by the super oil suction elastomeric material after molecular designing, the most high energy of the oil suction multiplying power of the dimethylbenzene close with gasoline property is reached to nearly more than 3 times of open source literature maximum value, has good application prospect.
The mensuration of oil suction multiplying power:
According to ASTM F726-81.Take the super oil suction elastomeric material of 0.1g, load stainless steel and iron silk screen (4*4*2cm), put into the flat bottom beaker of 100ml together, add excessive oil product, treat that oil suction reaches capacity, take out oil absorption material, dry the solvent of material surface attachment with filter paper, and correct amount, calculate oil suction multiplying power according to the following formula:
Sample weight before oil absorbency Q (g/g)=(after oil suction before sample weight-oil suction sample weight)/oil suction.
Claims (2)
1. a super oil suction elastomeric material, is characterized in that material contains the raw material of following mass fraction:
Rubber 30-80 part,
Cross-linking monomer 20-50 part,
Linking agent 0.05-5 part,
Initiator 0.1-5 part,
Dispersion agent 0.2-2 part,
Dispersion medium 180-500 part,
Solvent 180-500 part;
The molecular weight of described rubber is 800-600000, is the mixture of one or more in terpolymer EP rubber, isoprene-isobutylene rubber, styrene-butadiene rubber(SBR), natural rubber, chloroprene rubber or divinyl rubber;
Described cross-linking monomer is ethylidene norbornene;
Described linking agent is Vinylstyrene;
Described initiator is dichloroazodicarbonamide or tert-butyl peroxide;
Described dispersion agent is one or more mixtures in gelatin, pectin or carrageenin;
Described dispersion medium is deionized water or pure water;
Described solvent is one or more mixtures in benzene,toluene,xylene, normal hexane, hexanaphthene, normal heptane, isoheptane, octane, octane-iso, glycerine or paraffin,
Super oil suction elastomeric material is made to be its solubility parameter and the high molecular crosslink system of the rubber being no more than 0.5 by the difference of the solubility parameter of oil suction product, cross-linking monomer and linking agent.
2. a preparation method for super oil suction elastomeric material as claimed in claim 1, is characterized in that step is followed successively by:
1) weighing proportioning is carried out by the mass fraction of following component:
Rubber 30-80 part,
Cross-linking monomer 20-50 part,
Linking agent 0.05-5 part,
Initiator 0.1-5 part,
Dispersion agent 0.2-2 part,
Dispersion medium 180-500 part,
Solvent 180-500 part;
2) rubber and cross-linking monomer are added in solvent, be warming up to 40-90 DEG C, after constant temperature 10-30 minute, be cooled to 38 ~ 42 DEG C, add dispersion agent, constant temperature stirred after 0.5-2 hour, was warming up to 60-90 DEG C, added linking agent, initiator, stir 2-6 hour, after being cooled to 38 ~ 42 DEG C, add dispersion medium, continue to stir 0.5-2 hour;
3) be cooled to room temperature, filter, product acetone and tetrahydrofuran (THF) cleaning, namely vacuum-drying obtain super oil suction elastomeric material.
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| CN107141417A (en) * | 2017-06-27 | 2017-09-08 | 白才蓉 | A kind of oiliness sewage treatment high oil-absorbing resin and preparation method thereof |
| CN107663316B (en) * | 2017-09-21 | 2020-05-12 | 贵州理工学院 | Preparation method of oil-absorbing expansion rubber |
| CN109224531B (en) * | 2018-08-03 | 2021-08-31 | 广东工业大学 | Oil-water separation material and preparation method and application thereof |
| CN111909317B (en) * | 2020-07-24 | 2021-05-07 | 四川大学 | Modified rubber with high oil absorption performance and preparation process thereof |
| CN111974362B (en) * | 2020-07-24 | 2023-03-24 | 四川大学 | Application of modified rubber in preparation of oil absorption material |
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