CN104151484A - Porous resin with easy recycle and high oil absorption and preparation method - Google Patents
Porous resin with easy recycle and high oil absorption and preparation method Download PDFInfo
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Abstract
The invention relates to a porous resin with easy recycle and high oil absorption and a preparation method therefor. In the preparation method, raw materials in reasonable ratios are subjected to suspension polymerization and the porous resin with easy recycle and high oil absorption is prepared. The preparation method comprises steps of dispersive mixing, suspension polymerization, extraction and the like. The resin has a special physical-chemcial composite crosslinking structure, thus the resin has a high oil absorption rate, and after the resin is used repeatedly, the resin is subjected to recovery processing in a simple chemical method or the like. The porous resin has advantages of high recovery rate, low cost and the like in the later recycling process compared with traditional oil absorbing resins.
Description
Technical field
The invention belongs to filed of functional, be specifically related to a kind of porousness and easily reclaim high oil absorbing resin and preparation method thereof.
Background technology
In recent years, along with going deep into of the exploitations such as petroleum prospecting, the problem of environmental pollution that oil leak etc. cause and oily(waste)water, waste liquid increase the weight of day by day to the destruction of water resources, have caused and have had a strong impact on to human lives.Therefore in the urgent need to developing good oil absorption material, to tackle the oil pollution problem of current sternness.
High oil absorbing resin is the low crosslinking degree polymkeric substance that lipophilicity monomer forms.Intermolecular have a three-dimensional cross-linked reticulated structure, and there is certain micropore inside, can swelling decades of times oil product.Mainly can be divided into mineral-type oil-absorbing resin and organic oil-absorbing resin, wherein organic oil-absorbing resin can be divided into again natural adsorptive type and synthesis type two classes.But the problem such as current common high oil absorbing resin exists adsorption rate slow, and efficiency is low, this has just limited its application greatly.In order to improve the problem of existing high oil absorbing resin, people have carried out large quantity research, one of them is exactly by introducing the synthetic high oil-absorbing resin of physical-chemical composite crosslinking, and its swelling rate is wanted obviously faster than the synthetic high oil-absorbing resin obtaining of single chemically crosslinked.
Resin after oil suction is through manipulation of regeneration, and recyclable institute oil suction product, avoid secondary pollution on the one hand, and high oil absorbing resin is reusable on the other hand.The secondary pollution causing for fear of resin after oil suction, need carry out manipulation of regeneration to the resin after oil suction, and that traditional high oil absorbing resin is finally recycled high oil absorbing resin after Reusability is difficult, recycling rate is low.
Summary of the invention
The problem that the present invention is directed to above-mentioned prior art existence provides a kind of porousness easily to reclaim high oil absorbing resin and preparation method thereof.
Porousness of the present invention easily reclaims the preparation method of high oil absorbing resin, comprises the following steps:
A) dispersion agent is dispersed in and in solvent, is mixed with solution;
B) polymerization single polymerization monomer, initiator, linking agent and pore-creating agent are added in the solution that step a) obtains, and mix under inert atmosphere protection;
C) under stirring, the reaction system of step b) is heated to 70 DEG C～85 DEG C and carries out suspension polymerization 4.5～7.5 hours, then reaction system is warming up to 86 DEG C～95 DEG C and carries out slaking reaction 0.5～2.5 hour;
D) cooling step reaction system c), to room temperature, is filtered, and gets solid ultrasonic extraction in extraction agent and removes pore-creating agent;
E) filter, with absolute ethanol washing, vacuum-drying 24-48 hour obtains product.
Porousness of the present invention easily reclaims in high oil absorbing resin preparation method, and the part by weight of each raw material closes and is: polymerization single polymerization monomer: 100 parts; Solvent: 250～600 parts; Dispersion agent: 1～5 part; Linking agent: 0.8～5 part; Initiator: 0.3～2.5 part; Pore-creating agent: 80～200 parts.
In step a), described solvent is deionized water; Described dispersion agent is one or more in polyvinyl alcohol (PVA), methylcellulose gum, starch, pectin.
In step b), described polymerization single polymerization monomer is the mixture of methacrylic acid monomer and alkyl-acrylates monomer, and the mol ratio of described methacrylic acid monomer and alkyl-acrylates monomer is 1: 4～1: 6; Described alkyl-acrylates monomer is selected from one or more the mixture in dodecylacrylate, aliphatic acrylate, vinylformic acid stearyl.
In step b), described initiator is selected from one or more in Diisopropyl azodicarboxylate, dibenzoyl peroxide, persulphate and peroxide benzoate.
In step b), described linking agent is physical crosslinking agent and the mixing of chemical cross-linking agent; Described physical crosslinking agent is organically-modified nano-silica SiClx, be preferably cetyl trimethylammonium bromide modified manometer silicon dioxide, it mainly plays the effect of physical crosslinking point, it can also can be prepared and be obtained by easy method purchased from professional production firm, as cetyl trimethylammonium bromide joined in ultrasonic scattered nano silicon dioxide sol, under mechanical agitation, in 85 DEG C of reaction 4h, make by filtering to purify; Described chemical cross-linking agent is selected from one or more in glycol diacrylate, ethylene glycol dimethacrylate, Vinylstyrene, Diethylene Glycol dimethacrylate, propylene glycol diacrylate, propylene glycol dimethacrylate and Phthalic acid, diallyl ester, and it mainly plays chemically crosslinked effect.
In step b), described pore-creating agent is one or more in ethyl acetate, butylacetate, normal hexane, ethylene dichloride, benzene, toluene, paraffin, butanone and tetracol phenixin.
In described steps d) in, extraction agent used is selected from one or more in methyl alcohol, ethanol, acetone, isopropylcarbinol and hexanol.The consumption of described extraction agent is 1: 1～6:1 with the part by weight of the pore-creating agent adding.
Steps d) in, supersound process power is 60-300W, the treatment time is 20-60 minute.
The present invention compared with prior art, has the following advantages:
1. the prepared porousness of the present invention easily reclaims high oil absorbing resin and introduces the cross-linking set of organically-modified nano silicon as high oil-absorbent material, coordinates the crosslinked synthetic high oil-absorbing resin of " physical-chemical " composite crosslinking that has with other linking agents.
2. the prepared porousness of the present invention easily reclaims high oil absorbing resin and in recycling, has very significantly advantage, use easy chemical process can destroy " hydrogen bond " that organically-modified nano-silica surface hydroxyl in high oil absorbing resin and polymethyl acrylic acid-alkyl acrylate form, be physical crosslinking point, and after processing, recovery yield of monomer is high, cost recovery is low.
Embodiment
Following examples are only for illustrating the present invention; and to the present invention without any restriction; those skilled in the art are appreciated that it is all feasible that technical scheme of the present invention is carried out to suitable amendment after reading following examples, and any technical scheme that does not depart from essence of the present invention also falls in protection scope of the present invention.
Except special instruction, the raw material adopting is commercially available raw material, test apparatus used is the conventional instrument using in laboratory below.
embodiment 1
2.5 parts of dispersion agent methylcellulose gum are added in 450 parts of deionized waters of 80 DEG C, be stirred to completely and dissolve, be cooled to room temperature.Then added in the four-hole bottle that agitator, reflux exchanger, thermometer are housed.Then by totally 100 parts of polymerization single polymerization monomer methacrylic acid and dodecylacrylate (mol ratio is 1: 6), 1 part of initiator Diisopropyl azodicarboxylate, 3 parts of 1.5 parts of linking agent Phthalic acid, diallyl esters and cetyl trimethylammonium bromide modified manometer silicon dioxides, pore-creating agent normal hexane totally 150 parts add wherein and stir, logical nitrogen 30 minutes simultaneously, the air of driving away in reactor carries out under nitrogen atmosphere with guarantee suspension polymerization.Under stirring, reaction system is heated to 80 DEG C and carries out suspension polymerization 7.5 hours, then reaction system is warming up to 95 DEG C and carries out slaking reaction 1 hour.Under stirring, product is cooled to room temperature, filters.The solid product obtaining is mixed with the isopropylcarbinol of 260 parts, add (power 250W) in ultrasonic apparatus ultrasonic 40 minutes.The product obtaining is filtered, and with absolute ethanol washing, vacuum-drying obtains high oil absorbing resin for 24 hours.Performance test is in table 1.
embodiment 2
3.5 parts of dispersion agent starch are added in 550 parts of the deionized waters of 80 DEG C, be stirred to completely and dissolve, be cooled to room temperature; Then added in the four-hole bottle that agitator, reflux exchanger, thermometer are housed, by totally 100 parts of polymerization single polymerization monomer methacrylic acid and aliphatic acrylates, mol ratio is 1: 4.5,1.46 parts of initiator Sodium Persulfates, 4 parts of 1 part of linking agent Vinylstyrene and cetyl trimethylammonium bromide modified manometer silicon dioxides, 200 parts of pore-creating agent butylacetates add wherein and stir, logical nitrogen 30 minutes simultaneously, the air of driving away in reactor carries out under nitrogen atmosphere with guarantee suspension polymerization; Under stirring, reaction system is heated to 85 DEG C and carries out suspension polymerization 5.5 hours, then reaction system is warming up to 93 DEG C and carries out slaking reaction 2 hours; Under stirring, product is cooled to room temperature, filters, the solid product obtaining is mixed with the isopropylcarbinol of 260 parts, adding power is in the ultrasonic apparatus of 250W, ultrasonic 40 minutes; And the product obtaining is filtered, with absolute ethanol washing, vacuum-drying obtains high oil absorbing resin for 48 hours.Performance test is in table 1.
embodiment 3
4 parts of polyethylene of dispersing agent alcohol are added in 400 parts of the deionized waters of 80 DEG C, be stirred to completely and dissolve, be cooled to room temperature; Then added in the four-hole bottle that agitator, reflux exchanger, thermometer are housed, totally 100 parts of the polymerization single polymerization monomer methacrylic acid that is 1: 5.5 by mol ratio and aliphatic acrylate, vinylformic acid stearyl, 1.46 parts of initiator Sodium Persulfates, 2 parts of 2 parts of linking agent glycol diacrylates and cetyl trimethylammonium bromide modified manometer silicon dioxides, 150 parts of pore-creating agent trichloromethanes add wherein and stir, logical nitrogen 15 minutes simultaneously, the air of driving away in reactor carries out under nitrogen atmosphere with guarantee suspension polymerization; Under stirring, reaction system is heated to 70 DEG C and carries out suspension polymerization 6.5 hours, then reaction system is warming up to 86 DEG C and carries out slaking reaction 2.5 hours; Under stirring, product is cooled to room temperature, filters, by the methanol mixed of the solid product obtaining and 220 parts, adding power is in the ultrasonic apparatus of 250W, ultrasonic 30 minutes; And the product obtaining is filtered, with absolute ethanol washing, vacuum-drying obtains high oil absorbing resin for 24 hours.Performance test is in table 1.
embodiment 4
3 parts of polyethylene of dispersing agent alcohol are added in 450 parts of the deionized waters of 80 DEG C, be stirred to completely and dissolve, be cooled to room temperature; Then added in the four-hole bottle that agitator, reflux exchanger, thermometer are housed, totally 100 parts of the polymerization single polymerization monomer methacrylic acid that is 1: 5 by mol ratio and vinylformic acid stearyl, 1.6 parts of initiator dibenzoyl peroxide, 3.4 parts of 1.5 parts of linking agent ethylene glycol dimethacrylates and cetyl trimethylammonium bromide modified manometer silicon dioxides, 80 parts of pore-creating agent normal hexanes add wherein and stir, logical nitrogen 30 minutes simultaneously, the air of driving away in reactor carries out under nitrogen atmosphere with guarantee suspension polymerization; Under stirring, reaction system is heated to 80 DEG C and carries out suspension polymerization 4.5 hours, then reaction system is warming up to 95 DEG C and carries out slaking reaction 2.5 hours; Under stirring, product is cooled to room temperature, filters, the solid product obtaining is mixed with the ethanol of 260 parts, adding power is in the ultrasonic apparatus of 250W, ultrasonic 40 minutes; And the product obtaining is filtered, with absolute ethanol washing, vacuum-drying obtains high oil absorbing resin for 48 hours.Performance test is in table 1.
embodiment 5
3 parts of 1 part of dispersion agent methylcellulose gum and polyvinyl alcohol are added in 450 parts of the deionized waters of 80 DEG C, be stirred to completely and dissolve, be cooled to room temperature; Then added in the four-hole bottle that agitator, reflux exchanger, thermometer are housed, totally 100 parts of the polymerization single polymerization monomer methacrylic acid that is 1: 5 by mol ratio and dodecylacrylate, 1.3 parts of initiator dibenzoyl peroxide, 4 parts of 0.8 part of linking agent propylene glycol dimethacrylate and cetyl trimethylammonium bromide modified manometer silicon dioxides, 120 parts of pore-creating agent butylacetates add wherein and stir, logical nitrogen 30 minutes simultaneously, the air of driving away in reactor carries out under nitrogen atmosphere with guarantee suspension polymerization; Under stirring, reaction system is heated to 78 DEG C and carries out suspension polymerization 7.5 hours, then reaction system is warming up to 90 DEG C and carries out slaking reaction 0.5 hour; Under stirring, product is cooled to room temperature, filters, the solid product obtaining is mixed with the propyl alcohol of 260 parts, adding power is in the ultrasonic apparatus of 250W, ultrasonic 40 minutes; And the product obtaining is filtered, with absolute ethanol washing, vacuum-drying obtains high oil absorbing resin for 36 hours.Performance test is in table 1.
embodiment 6
2 parts of 2 parts of dispersion agent methylcellulose gum and polyvinyl alcohol are added in 450 parts of the deionized waters of 80 DEG C, be stirred to completely and dissolve, be cooled to room temperature; Then added in the four-hole bottle that agitator, reflux exchanger, thermometer are housed, totally 100 parts of the polymerization single polymerization monomer methacrylic acid that is 1: 6 by mol ratio and dodecylacrylate, totally 2.1 parts of initiator peroxide benzoates, 4.2 parts of 0.8 part of linking agent propylene glycol diacrylate and cetyl trimethylammonium bromide modified manometer silicon dioxides, 140 parts of pore-creating agent ethyl acetate add wherein and stir, logical 30 minutes simultaneously, the air of driving away in reactor carried out under nitrogen atmosphere with guarantee suspension polymerization; Under stirring, reaction system is heated to 85 DEG C and carries out suspension polymerization 5.5 hours, then reaction system is warming up to 95 DEG C and carries out slaking reaction 1.5 hours; Under stirring, product is cooled to room temperature, filters, the solid product obtaining is mixed with the hexanol of 260 parts, adding power is in the ultrasonic apparatus of 250W, ultrasonic 30 minutes; And the product obtaining is filtered, with absolute ethanol washing, vacuum-drying obtains high oil absorbing resin for 48 hours.Performance test is in table 1.
The performance test that resin is easily reclaimed in the high oil suction of table 1 the present invention
By finding above data analysis: the prepared porousness of the present invention easily reclaims high oil absorbing resin, by physics-chemically composited being cross-linked, on the one hand, increase the stickiness of three-dimensional molecular net, increase the viscosity coefficient that oil molecule spreads in resin; On the other hand, form again the better three-dimensional molecular net of rebound resilience, increased the Young's modulus of resin, made this oil absorption material show good oil suction and protect oily effect.
Claims (10)
1. porousness easily reclaims a preparation method for high oil absorbing resin, it is characterized in that, comprises the following steps:
A) dispersion agent is dispersed in and in solvent, is mixed with solution;
B) polymerization single polymerization monomer, initiator, linking agent and pore-creating agent are added in the solution that step a) obtains, and mix under inert atmosphere protection;
C) under stirring, the reaction system of step b) is heated to 70 DEG C～85 DEG C and carries out suspension polymerization 4.5～7.5 hours, then reaction system is warming up to 86 DEG C～95 DEG C and carries out slaking reaction 0.5～2.5 hour;
D) cooling step reaction system c), to room temperature, is filtered, and gets solid ultrasonic extraction in extraction agent and removes pore-creating agent;
E) filter, with absolute ethanol washing, vacuum-drying 24-48 hour obtains product.
2. porousness according to claim 1 easily reclaims the preparation method of high oil absorbing resin, it is characterized in that, the part by weight of each raw material closes and is: polymerization single polymerization monomer: 100 parts; Solvent: 250～600 parts; Dispersion agent: 1～5 part; Linking agent: 0.8～5 part; Initiator: 0.3～2.5 part; Pore-creating agent: 80～200 parts.
3. porousness according to claim 1 easily reclaims the preparation method of high oil absorbing resin, it is characterized in that, in step a), described solvent is deionized water; Described dispersion agent is at least one in polyvinyl alcohol, methylcellulose gum, starch, pectin.
4. porousness according to claim 1 easily reclaims the preparation method of high oil absorbing resin, it is characterized in that, in step b), described polymerization single polymerization monomer is the mixture of methacrylic acid monomer and alkyl-acrylates monomer, and the mol ratio of described methacrylic acid monomer and alkyl-acrylates monomer is 1: 4～1: 6; Described alkyl-acrylates monomer is selected from one or more the mixture in dodecylacrylate, aliphatic acrylate, vinylformic acid stearyl.
5. porousness according to claim 1 easily reclaims the preparation method of high oil absorbing resin, it is characterized in that, in step b), described initiator is selected from least one in Diisopropyl azodicarboxylate, dibenzoyl peroxide, persulphate and peroxide benzoate.
6. porousness according to claim 1 easily reclaims the preparation method of high oil absorbing resin, it is characterized in that, in step b), described linking agent is physical crosslinking agent and the mixing of chemical cross-linking agent, wherein said physical crosslinking agent is organically-modified nano-silica SiClx, is preferably cetyl trimethylammonium bromide modified manometer silicon dioxide; Described chemical cross-linking agent is selected from least one in glycol diacrylate, ethylene glycol dimethacrylate, Vinylstyrene, Diethylene Glycol dimethacrylate, propylene glycol diacrylate, propylene glycol dimethacrylate and Phthalic acid, diallyl ester.
7. porousness according to claim 1 easily reclaims the preparation method of high oil absorbing resin, it is characterized in that, in step b), described pore-creating agent is at least one in ethyl acetate, butylacetate, normal hexane and trichloromethane.
8. porousness according to claim 1 easily reclaims the preparation method of high oil absorbing resin, it is characterized in that, in described steps d) in, extraction agent used is selected from least one in methyl alcohol, ethanol, acetone, isopropylcarbinol and hexanol.
9. porousness according to claim 8 easily reclaims the preparation method of high oil absorbing resin, it is characterized in that steps d) in, the consumption of described extraction agent is 1: 1～6: 1 with the part by weight of the pore-creating agent adding.
10. porousness according to claim 1 easily reclaims the preparation method of high oil absorbing resin, it is characterized in that steps d) in, supersound process power is 60-300W, the treatment time is 20-60 minute.
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| CN107641171A (en) * | 2017-10-09 | 2018-01-30 | 浙江卫星新材料科技有限公司 | A kind of high oil absorption based on graphene and high antibiotic property oil-absorbing resin and its application |
| CN107641171B (en) * | 2017-10-09 | 2020-06-16 | 浙江卫星新材料科技有限公司 | Graphene-based high-oil-absorption and high-antibacterial-property oil-absorption resin and application thereof |
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