CN102924657B - Oil absorption material containing silicon polymer and preparation methods thereof - Google Patents

Oil absorption material containing silicon polymer and preparation methods thereof Download PDF

Info

Publication number
CN102924657B
CN102924657B CN201210436173.9A CN201210436173A CN102924657B CN 102924657 B CN102924657 B CN 102924657B CN 201210436173 A CN201210436173 A CN 201210436173A CN 102924657 B CN102924657 B CN 102924657B
Authority
CN
China
Prior art keywords
absorption material
monomer
oil absorption
containing polymer
silicon
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201210436173.9A
Other languages
Chinese (zh)
Other versions
CN102924657A (en
Inventor
方军
张昌明
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Xiamen University
Original Assignee
Xiamen University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Xiamen University filed Critical Xiamen University
Priority to CN201210436173.9A priority Critical patent/CN102924657B/en
Publication of CN102924657A publication Critical patent/CN102924657A/en
Application granted granted Critical
Publication of CN102924657B publication Critical patent/CN102924657B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)

Abstract

The invention provides an oil absorption material containing a silicon polymer and preparation methods thereof and relates to a macromolecule oil absorption material. The oil absorption material containing the silicon polymer is formed by copolymerizing an acrylic monomer A and an organic monomer B. One preparation method comprises the steps of adding the monomer A, the monomer B, clean water, an initiator, a cross-linking agent, a dispersing agent and a pore-foaming agent in a reactor, removing air in the reactor, leading inert gas into the reactor and performing sealing; mixing and heating materials to perform polymerization reaction; terminating the reaction and depositing, cleaning and drying a product to obtain the oil absorption material containing the silicon polymer. The other preparation method comprises the steps of adding the monomer A, the monomer B, a solvent, a photoinitiator, a cross-linking agent and a pore-foaming agent in the reactor, sealing and stirring the materials to be mixed evenly; placing the reactor into an ultraviolet light irradiation device to be irradiated and perform reaction; and terminating the reaction and depositing, cleaning and drying a product to obtain the oil absorption material containing the silicon polymer.

Description

Silicon-containing polymer oil absorption material and preparation method thereof
Technical field
The present invention relates to a kind of polymer oil absorption material, especially a kind of silicon-containing polymer oil absorption material and preparation method thereof.
Background technology
As the various oils of industry blood, in transport, replacing, use procedure, due to reasons such as water clock, leakage, sputterings, the ecotope that yard pollutes surrounding in one's power can be affected; Also a large amount of oily(waste)waters can be produced in the production process and mechanical industry lubricating oil process of cooling of the oil recovery of petroleum industry, oil refining and petrochemical complex, foodstuffs industry etc., polluted water environment, harm hydrobiont, even enters human body by food chain, is detrimental to health; Also a large amount of cooking fume atmosphere pollution is had in catering trade and daily life; Kitchen tools are scrubbed in daily life, a large amount of waste water containing edible oil do not do any process and flow into water drain, of long duration, meeting clog sewer line, bring inconvenience to the life of people, the oil absorption material therefore developing excellent property has become current research emphasis and focus.
At present, all have the exploitation of synthesis oil-absorbing resin both at home and abroad, but special emphasis is different, its synthesis material can be divided into esters of acrylic acid and alpha-olefines.Because the latter is expensive, therefore many esters of acrylic acid materials that adopts again synthesize.Synthetic method mainly adopts suspension polymerization and letex polymerization, and with esters of acrylic acid material for raw material, oil soluble thing is that initiator is polymerized.
1966, The Dow Chemical Co. (US) 2030 Dow Center, Abbott Road, Midland, Michigan 48640, applied for the patent of high oil absorbing resin, and Japan also starts to study after 20 century 70s, and the major companies such as catalyst chemical company apply for a patent in succession, as Japanese Patent JP06-269664, JP07-102248 etc.Wherein, Japanese catalyst chemical company has the production equipment of 100 tons/year.
A kind of high oil absorbing resin is disclosed in Chinese patent CN1095727, with vinylformic acid, esters of acrylic acid material for monomer, with N, N-methylene-bisacrylamide, EDIA class are linking agent, with gelatin, polyvinyl alcohol, Mierocrystalline cellulose, inorganic salt powder if the materials such as magnesiumcarbonate, talcum powder, calcium phosphate are for dispersion agent, calcium dodecylbenzene sulphonate is dispersion aids, initiator is radical polymerization initiator, as azo or organo-peroxide class, by suspension polymerization, synthesize high oil absorbing resin.When synthesizing high oil absorbing resin, arbitrary change of monomer system, cross linker system, initiator system, dispersant system, polymerization system all can cause the difference of high oil absorbing resin in performance synthesized, as the change of oil absorbency, and for the different oil absorbency that different oily matter shows.General high oil absorbing resin, higher general at about 20 times to chloroparaffin oil absorbency, to the large oil of viscosity as heavy oil, oil absorbency is then less, generally only has several times.
Summary of the invention
The object of the present invention is to provide a kind of silicon-containing polymer oil absorption material with high oil absorbency and preparation method thereof.
Described silicon-containing polymer oil absorption material is formed by acrylic ester monomer A and siliceous organic monomer B copolymerization, and its general structure is as follows:
Wherein R 1for H or CH 3, R 2for carbonatoms 1 ~ 18 alkyl; R 3, R 4for CH 3, C 2h 5, OCH 3, OC 2h 5in any one, R 5for CH 3or C 2h 5, m and n is the polymerization degree, m=100 ~ 2000, n=20 ~ 200, m and n is integer.
The general structure of described acrylic ester monomer A is as follows:
Wherein R 1for H or CH 3, R 2c atomicity be 1 ~ 18.
Described siliceous Orqanics Monomer B general structure is as follows:
Wherein R 3, R 4for CH 3, C 2h 5, OCH 3, OC 2h 5in any one, R 5for CH 3or C 2h 5.
Described silicon-containing polymer oil absorption material can adopt suspension polymerization to prepare, and concrete steps are as follows:
1) add acrylic ester monomer A, siliceous Orqanics Monomer B, clean water, initiator, linking agent, dispersion agent, pore-creating agent in the reactor, the air in removing reactor, passes into rare gas element, sealing;
2) by mixing of materials, then copolymerization is carried out in heating;
3) termination reaction, product is through precipitation, and cleaning, after drying, obtains silicon-containing polymer oil absorption material.
In step 1), the mass ratio of described acrylic ester monomer A and siliceous Orqanics Monomer B can be 1: 10 ~ 20: 1;
The consumption of described clean water is reaction system with reaction system total mass in mass ratio: water=1: (1 ~ 8);
Described initiator can be azo-initiator, and described azo-initiator can be selected from Diisopropyl azodicarboxylate, benzoyl peroxide, the one in ceric ammonium nitrate etc., and the consumption of described initiator can be 0.5% ~ 3.0% of reaction system total mass by mass percentage;
Described linking agent can be Vinylstyrene, Phthalic acid, diallyl ester, polyethylene glycol dimethacrylate, polyethyleneglycol diacrylate, 1,4-butylene glycol dimethacrylate or 1, one in 4-butylene glycol diacrylate etc., the consumption of described linking agent can be 0.5% ~ 2.0% of monomer total mass by mass percentage;
Described dispersion agent can be polyvinyl alcohol (PVA), and the consumption of described dispersion agent can be 0.5% ~ 3.0% of monomer total mass by mass percentage;
Described pore-creating agent can be toluene or acetone etc., and the consumption of described pore-creating agent can be 5% ~ 20% of monomer total mass by mass percentage.
In step 2) in, the temperature of described heating can be 60 ~ 90 DEG C, and the time of described copolymerization can be 5 ~ 9h.
In step 3), described precipitation can adopt alcohol settling, and described cleaning can adopt washed with de-ionized water, and the temperature of described drying can be 60 ~ 100 DEG C.
Described silicon-containing polymer oil absorption material can adopt ultraviolet initiated polymerization legal system standby, and concrete steps are as follows:
1) add acrylic ester monomer A, siliceous Orqanics Monomer B, solvent, light trigger, linking agent, pore-creating agent in the reactor, sealing is stirred, and makes mixing of materials even;
2) reactor is put into ultraviolet light irradiation equipment irradiation, reaction;
3) termination reaction, after the process of product drying, obtains silicon-containing polymer oil absorption material.
In step 1), the mass ratio of described acrylic ester monomer A and siliceous Orqanics Monomer B can be 1: 10 ~ 20: 1;
Described solvent can be selected from the one in methyl alcohol, ethanol, DMF etc.; Described solvent consumption in mass ratio can be 1 ~ 5 times of reaction system total mass;
Described light trigger can be selected from benzophenone or bitter almond oil camphor and derivative etc., and described benzophenone can be selected from the one in benzophenone, 2,4 dihydroxyl benzophenone, Michler's keton etc.; Described bitter almond oil camphor and derivative can be selected from the one in st-yrax, benzoin dimethylether, Benzoin ethyl ether, benzoin isopropyl ether, benzoin isobutyl ether etc., and described light trigger consumption by mass percentage can be 0.5% ~ 3.0% of reaction system total mass;
Described linking agent can be selected from Vinylstyrene, Phthalic acid, diallyl ester, polyethylene glycol dimethacrylate, polyethyleneglycol diacrylate, 1,4-butylene glycol dimethacrylate, 1, one in 4-butylene glycol diacrylate etc., described linking agent consumption by mass percentage can be 0.5% ~ 2.0% of acrylic ester monomer A and siliceous Orqanics Monomer B total mass;
Described pore-creating agent can be selected from toluene or acetone etc., and described pore-creating agent consumption by mass percentage can be 5% ~ 20% of acrylic ester monomer A and siliceous Orqanics Monomer B total mass.
In step 2) in, the power of described irradiation can be 9500mW/cm 2, the condition of described reaction can be reacts 70 ~ 150min at 40 ~ 60 DEG C.
In step 3), the temperature of described drying treatment can be 60 ~ 100 DEG C.
Silicon-containing polymer oil absorption material prepared by the present invention has the following advantages:
1) with siliceous organism for principal monomer, because it has oleophylic and hydrophobic grouping-Si-O ,-Si-C, effectively can improve the hydrophobic performance of oil absorption material, strengthen thermal stability and weathering resistance that oil absorptiveness also can strengthen polymkeric substance simultaneously.Prepared polymer materials oil-water selectivity is strong, while oil suction, produce sorption hardly to water.2) oil suction multiplying power is high, and the Oil keeping after oil suction can be good.3) polymkeric substance after oil suction can Reusability after specific desorption process.
Accompanying drawing explanation
Fig. 1 is the infrared spectrogram of silicon-containing polymer oil absorption material prepared in embodiment 1.In FIG, X-coordinate is wave number Wavenumber (cm -1).
The thermogravimetric analysis figure of the silicon-containing polymer oil absorption material that Fig. 2 obtains for embodiment 1.In fig. 2, X-coordinate is temperature Temperature (DEG C), and ordinate zou is mass percent Weight(%).
Embodiment
Below by embodiment, the present invention will be further described.
Embodiment 1
Methyl methacrylate 1.000g, vinyl methyl dimethoxysilane 10.000g, Vinylstyrene 0.055g, benzoyl peroxide 0.055g, toluene 0.550g, polyvinyl alcohol 0.055g, clean water 11.660g are joined in reactor, under nitrogen protection in more than stirring at room temperature 30min; Then reactor is warming up to 60 DEG C, termination reaction after 9h.Product by washed with de-ionized water, puts into vacuum drying oven after alcohol settling, can obtain silicon-containing polymer oil absorption material after 60 DEG C of oven dry.
Prepared silicon-containing polymer oil absorption material infrared analysis spectrogram as shown in Figure 1,2961cm -1there is the nonsymmetrical vibration of aliphatics c h bond in place, can judge that product has CH 3group; 2875cm in addition -1it is the symmetric vibration of CH2.1728cm -1there is the charateristic avsorption band of ester group C=O key.Si-O charateristic avsorption band appears at 1068cm -1and 1020cm -1place, another 1242cm -1for the charateristic avsorption band of Si-C.Infrared analysis result describes the required silicon-containing polymer oil absorption material successfully prepared.
The thermostability of the silicon-containing polymer oil absorption material prepared by test, probe temperature is 30 ~ 800 DEG C, and temperature rise rate is 10 DEG C/min.As can be seen from the thermogravimetric analysis figure of Fig. 2, product starts at 150 DEG C the decomposition occurring molecular weight polymers, has just decomposed completely when 450 DEG C, illustrates that this silicon-containing polymer oil absorption material has good thermostability.
The oil absorptiveness of gained silicon-containing polymer oil absorption material is tested, its to the oil suction multiplying power of all kinds of oil product in table 1.
Embodiment 2
Lauryl methacrylate 10.000g, vinyl ethyldimethoxysilane 2.000g, Phthalic acid, diallyl ester 0.120g, Diisopropyl azodicarboxylate 0.120g, toluene 1.200g, polyvinyl alcohol 0.180g, clean water 40.320g are joined in reactor, under nitrogen protection in more than stirring at room temperature 30min; Then reactor is warming up to 70 DEG C, termination reaction after 7h.Product by washed with de-ionized water, puts into vacuum drying oven after alcohol settling, can obtain silicon-containing polymer oil absorption material after 80 DEG C of oven dry.Gained silicon-containing polymer oil absorption material to the oil suction multiplying power of all kinds of oil product in table 1.
Embodiment 3
Stearyl methacrylate 10.000g, vinyl-dimethyl methoxylsilane 0.500g, polyethylene glycol dimethacrylate 0.210g, ceric ammonium nitrate 0.315g, acetone 2.100g, polyvinyl alcohol 0.315g, clean water 105.000g are joined in reactor, under nitrogen protection in more than stirring at room temperature 30min; Then reactor is warming up to 90 DEG C, termination reaction after 5h.Product by washed with de-ionized water, puts into vacuum drying oven after alcohol settling, can obtain silicon-containing polymer oil absorption material after 100 DEG C of oven dry.Gained silicon-containing polymer oil absorption material to the oil suction multiplying power of all kinds of oil product in table 1.
Embodiment 4
By dodecyl acrylate 5.000g, vinyltrimethoxy silane 1.000g, 1,4-butylene glycol dimethacrylate 0.060g, Diisopropyl azodicarboxylate 0.060g, acetone 0.600g, polyvinyl alcohol 0.090g, clean water 20.160g join in reactor, under nitrogen protection in more than stirring at room temperature 30min; Then reactor is warming up to 80 DEG C, termination reaction after 6h.Product by washed with de-ionized water, puts into vacuum drying oven after alcohol settling, can obtain silicon-containing polymer oil absorption material after 70 DEG C of oven dry.Gained silicon-containing polymer oil absorption material to the oil suction multiplying power of all kinds of oil product in table 1.
Embodiment 5
Adopt the method identical with embodiment 2, be methyl acrylate unlike monomer A used, monomers B is vinyl monomethyl ethyl methoxy silane, and linking agent is polyethyleneglycol diacrylate, gained silicon-containing polymer oil absorption material to the oil suction multiplying power of all kinds of oil product in table 1.
Embodiment 6
Adopt the method identical with embodiment 2, be octadecyl acrylate unlike monomer A used, monomers B is vinyl methyl diethoxy silane, and linking agent is 1,4-butylene glycol diacrylate, gained silicon-containing polymer oil absorption material to the oil suction multiplying power of all kinds of oil product in table 1.
Embodiment 7
Dodecyl acrylate is mixed 5.000g, vinyl methyl methoxy-ethoxy-silane 1.000g, 1 altogether with methyl acrylate with mass ratio 1: 1,4-butylene glycol dimethacrylate 0.060g, Diisopropyl azodicarboxylate 0.060g, toluene 0.600g, polyvinyl alcohol 0.090g, clean water 20.160g join in reactor, under nitrogen protection in more than stirring at room temperature 30min; Again reactor is warming up to 80 DEG C, termination reaction after 6h.Product by washed with de-ionized water, puts into vacuum drying oven after alcohol settling, namely obtains silicon-containing polymer oil absorption material after 60 DEG C of oven dry.Gained silicon-containing polymer oil absorption material to the oil suction multiplying power of all kinds of oil product in table 1.
Embodiment 8
Adopting the method identical with embodiment 7, is lauryl methacrylate and methyl methacrylate unlike monomer A used.Gained silicon-containing polymer oil absorption material to the oil suction multiplying power of all kinds of oil product in table 1.
The oil suction multiplying power of all kinds of oil product of table 1.
Embodiment 9 ~ 17
Adopt the method identical with embodiment 2, unlike changing monomers B used.Monomers B used and prepare gained silicon-containing polymer oil absorption material to the oil suction multiplying power of all kinds of oil product in table 2.
The oil suction multiplying power of all kinds of oil product of table 2.
Embodiment 18
By methyl methacrylate 1.000g, vinyl methyl dimethoxysilane 10.000g, Vinylstyrene 0.055g, benzophenone 0.055g, toluene 0.550g, methyl alcohol 11.000g in reactor, more than stirred at ambient temperature 90min; Then 40 DEG C are warming up to, simultaneously ultraviolet lighting, off-response after 150min; The gel aggregated into is put into vacuum drying oven dry, after 60 DEG C of oven dry, namely obtain silicon-containing polymer oil absorption material.
The oil absorptiveness of gained silicon-containing polymer oil absorption material is tested, its to the oil suction multiplying power of all kinds of oil product in table 3.
Embodiment 19
By lauryl methacrylate 10.000g, vinyl ethyldimethoxysilane 2.000g, Phthalic acid, diallyl ester 0.120g, Benzoin ethyl ether 0.120g, toluene 1.200g, ethanol 36.000g in reactor, more than stirred at ambient temperature 90min; Then 50 DEG C are warming up to, simultaneously ultraviolet lighting, off-response after 110min; The gel aggregated into is put into vacuum drying oven dry, after 100 DEG C of oven dry, namely obtain silicon-containing polymer oil absorption material.Gained silicon-containing polymer oil absorption material to the oil suction multiplying power of all kinds of oil product in table 3.
Embodiment 20
Get stearyl methacrylate 10.000g, vinyl-dimethyl methoxylsilane 0.500g, polyethylene glycol dimethacrylate 0.210g, benzophenone 0.315g, acetone 2.100g, N, dinethylformamide 52.500g, in reactor, stirs more than 90min; Then 60 DEG C are warming up to, simultaneously ultraviolet lighting, off-response after 70min; The gel aggregated into is put into vacuum drying oven dry, after 80 DEG C of oven dry, namely obtain silicon-containing polymer oil absorption material.Gained silicon-containing polymer oil absorption material to the oil suction multiplying power of all kinds of oil product in table 3.
Embodiment 21
Get dodecyl acrylate 5.000g, vinyltrimethoxy silane 1.000g, BDO dimethacrylate 0.060g, benzophenone 0.060g, acetone 0.600g, ethanol 18.000g in reactor, stir more than 90min; Then 60 DEG C are warming up to, simultaneously ultraviolet lighting, off-response after 70min; The gel aggregated into is put into vacuum drying oven dry, after 70 DEG C of oven dry, namely obtain silicon-containing polymer oil absorption material.Gained silicon-containing polymer oil absorption material to the oil suction multiplying power of all kinds of oil product in table 3.
Embodiment 22
Dodecyl acrylate is mixed 5.000g, vinyl methyl methoxy-ethoxy-silane 1.000g, 1 altogether with methyl acrylate with mass ratio 1:1,4-butylene glycol dimethacrylate 0.060g, benzoin isobutyl ether 0.060g, toluene 0.600g, ethanol 18.000g, in reactor, stir more than 90min; Then 60 DEG C are warming up to, simultaneously ultraviolet lighting, off-response after 70min; The gel aggregated into is put into vacuum drying oven dry, after 60 DEG C of oven dry, namely obtain silicon-containing polymer oil absorption material.Gained silicon-containing polymer oil absorption material to the oil suction multiplying power of all kinds of oil product in table 3.
Embodiment 23
Adopting the method identical with embodiment 22, is lauryl methacrylate and methyl methacrylate unlike monomer A used.Gained silicon-containing polymer oil absorption material to the oil suction multiplying power of all kinds of oil product in table 3.
Embodiment 24
Adopting the method identical with embodiment 2, is methyl acrylate unlike monomer A used, and monomers B is vinyl monomethyl ethyl methoxy silane, and linking agent is polyethyleneglycol diacrylate.Gained silicon-containing polymer oil absorption material to the oil suction multiplying power of all kinds of oil product in table 3.
Embodiment 25
Adopting the method identical with embodiment 2, is octadecyl acrylate unlike monomer A used, and monomers B is vinyl methyl diethoxy silane, and linking agent is 1,4 butanediol diacrylate.Gained silicon-containing polymer oil absorption material to the oil suction multiplying power of all kinds of oil product in table 3.
The oil suction multiplying power of all kinds of oil product of table 3.
Embodiment 26 ~ 34
Adopt the method identical with embodiment 19, unlike changing monomers B used.
The oil suction multiplying power of all kinds of oil product of table 4.
Monomers B used and prepare gained silicon-containing polymer oil absorption material to the oil suction multiplying power of all kinds of oil product in table 4.

Claims (8)

1. the preparation method of silicon-containing polymer oil absorption material, it is characterized in that described silicon-containing polymer oil absorption material is formed by acrylic ester monomer A and siliceous organic monomer B copolymerization, its general structure is as follows:
Wherein R 1for H or CH 3, R 2for carbonatoms 1 ~ 18 alkyl; R 3, R 4for CH 3, C 2h 5, OCH 3, OC 2h 5in any one, R 5for CH 3or C 2h 5, m and n is the polymerization degree, m=100 ~ 2000, n=20 ~ 200, m and n is integer;
The general structure of described acrylic ester monomer A is as follows:
Wherein R 1for H or CH 3, R 2c atomicity be 1 ~ 18;
Described siliceous Orqanics Monomer B general structure is as follows:
Wherein R 3, R 4for CH 3, C 2h 5, OCH 3, OC 2h 5in any one, R 5for CH 3or C 2h 5;
The preparation method of described silicon-containing polymer oil absorption material comprises the following steps:
1) add acrylic ester monomer A, siliceous Orqanics Monomer B, clean water, initiator, linking agent, dispersion agent, pore-creating agent in the reactor, the air in removing reactor, passes into rare gas element, sealing; The mass ratio of described acrylic ester monomer A and siliceous Orqanics Monomer B is 1: 10 ~ 20: 1; The consumption of described linking agent is 0.5% ~ 2.0% of monomer total mass by mass percentage; The consumption of described pore-creating agent is 5% ~ 20% of monomer total mass by mass percentage;
2) by mixing of materials, then copolymerization is carried out in heating;
3) termination reaction, product is through precipitation, and cleaning, after drying, obtains silicon-containing polymer oil absorption material.
2. the preparation method of silicon-containing polymer oil absorption material as claimed in claim 1, is characterized in that in step 1) in, the consumption of described clean water is reaction system with reaction system total mass in mass ratio: water=1: (1 ~ 8);
Described initiator is azo-initiator, and described azo-initiator is selected from Diisopropyl azodicarboxylate, benzoyl peroxide, the one in ceric ammonium nitrate, and the consumption of described initiator is 0.5% ~ 3.0% of reaction system total mass by mass percentage;
Described linking agent is the one in Vinylstyrene, Phthalic acid, diallyl ester, polyethylene glycol dimethacrylate, polyethyleneglycol diacrylate, BDO dimethacrylate or 1,4 butanediol diacrylate;
Described dispersion agent is polyvinyl alcohol, and the consumption of described dispersion agent is 0.5% ~ 3.0% of monomer total mass by mass percentage;
Described pore-creating agent is toluene or acetone.
3. the preparation method of silicon-containing polymer oil absorption material as claimed in claim 1, is characterized in that in step 2) in, the temperature of described heating is 60 ~ 90 DEG C, and the time of described copolymerization is 5 ~ 9h.
4. the preparation method of silicon-containing polymer oil absorption material as claimed in claim 1, is characterized in that in step 3) in, described precipitation adopts alcohol settling, and described cleaning adopts washed with de-ionized water, and the temperature of described drying is 60 ~ 100 DEG C.
5. the preparation method of silicon-containing polymer oil absorption material, it is characterized in that described silicon-containing polymer oil absorption material is formed by acrylic ester monomer A and siliceous organic monomer B copolymerization, its general structure is as follows:
Wherein R 1for H or CH 3, R 2for carbonatoms 1 ~ 18 alkyl; R 3, R 4for CH 3, C 2h 5, OCH 3, OC 2h 5in any one, R 5for CH 3or C 2h 5, m and n is the polymerization degree, m=100 ~ 2000, n=20 ~ 200, m and n is integer;
The general structure of described acrylic ester monomer A is as follows:
Wherein R 1for H or CH 3, R 2c atomicity be 1 ~ 18;
Described siliceous Orqanics Monomer B general structure is as follows:
Wherein R 3, R 4for CH 3, C 2h 5, OCH 3, OC 2h 5in any one, R 5for CH 3or C 2h 5;
The preparation method of described silicon-containing polymer oil absorption material comprises the following steps:
1) add acrylic ester monomer A, siliceous Orqanics Monomer B, solvent, light trigger, linking agent, pore-creating agent in the reactor, sealing is stirred, and makes mixing of materials even; The mass ratio of described acrylic ester monomer A and siliceous Orqanics Monomer B is 1: 10 ~ 20: 1; Described linking agent consumption is by mass percentage 0.5% ~ 2.0% of acrylic ester monomer A and siliceous Orqanics Monomer B total mass; Described pore-creating agent consumption is by mass percentage 5% ~ 20% of acrylic ester monomer A and siliceous Orqanics Monomer B total mass;
2) reactor is put into ultraviolet light irradiation equipment irradiation, reaction;
3) termination reaction, after the process of product drying, obtains silicon-containing polymer oil absorption material.
6. the preparation method of silicon-containing polymer oil absorption material as claimed in claim 5, is characterized in that in step 1) in, the one in described solvent selected from methanol, ethanol, DMF; Described solvent consumption is in mass ratio 1 ~ 5 times of reaction system total mass;
Described light trigger is selected from benzophenone or bitter almond oil camphor and derivative, and described benzophenone is selected from the one in benzophenone, 2,4 dihydroxyl benzophenone, Michler's keton; Described bitter almond oil camphor and derivative are selected from the one in st-yrax, benzoin dimethylether, Benzoin ethyl ether, benzoin isopropyl ether, benzoin isobutyl ether, and described light trigger consumption is by mass percentage 0.5% ~ 3.0% of reaction system total mass;
Described linking agent is selected from the one in Vinylstyrene, Phthalic acid, diallyl ester, polyethylene glycol dimethacrylate, polyethyleneglycol diacrylate, BDO dimethacrylate, 1,4 butanediol diacrylate;
Described pore-creating agent is selected from toluene or acetone.
7. the preparation method of silicon-containing polymer oil absorption material as claimed in claim 5, is characterized in that in step 2) in, the power of described irradiation is 9500mW/cm 2, the condition of described reaction is react 70 ~ 150min at 40 ~ 60 DEG C.
8. the preparation method of silicon-containing polymer oil absorption material as claimed in claim 5, is characterized in that in step 3) in, the temperature of described drying treatment is 60 ~ 100 DEG C.
CN201210436173.9A 2012-11-02 2012-11-02 Oil absorption material containing silicon polymer and preparation methods thereof Active CN102924657B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201210436173.9A CN102924657B (en) 2012-11-02 2012-11-02 Oil absorption material containing silicon polymer and preparation methods thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201210436173.9A CN102924657B (en) 2012-11-02 2012-11-02 Oil absorption material containing silicon polymer and preparation methods thereof

Publications (2)

Publication Number Publication Date
CN102924657A CN102924657A (en) 2013-02-13
CN102924657B true CN102924657B (en) 2014-12-24

Family

ID=47639601

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201210436173.9A Active CN102924657B (en) 2012-11-02 2012-11-02 Oil absorption material containing silicon polymer and preparation methods thereof

Country Status (1)

Country Link
CN (1) CN102924657B (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106995513B (en) * 2017-05-18 2019-05-07 贵州理工学院 A kind of short-chain branch system oil-absorbing resin and preparation method thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0207627A2 (en) * 1985-06-06 1987-01-07 BP Chemicals Limited Polymer composition
CN1095727A (en) * 1993-05-27 1994-11-30 天津理工学院 Synthetic resin with high oil absorbency
CN1154707A (en) * 1995-05-08 1997-07-16 耐尔科化学公司 DADMAC/vinyl trialkoxysilane copolymers and their use in waste water treatment
CN1442438A (en) * 2002-03-01 2003-09-17 中国石油天然气股份有限公司 High oil absorption resin and its synthesis method
CN1973944A (en) * 2006-09-25 2007-06-06 厦门大学 Making process of integral stirring rod for solid phase extraction

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0207627A2 (en) * 1985-06-06 1987-01-07 BP Chemicals Limited Polymer composition
CN1095727A (en) * 1993-05-27 1994-11-30 天津理工学院 Synthetic resin with high oil absorbency
CN1154707A (en) * 1995-05-08 1997-07-16 耐尔科化学公司 DADMAC/vinyl trialkoxysilane copolymers and their use in waste water treatment
CN1442438A (en) * 2002-03-01 2003-09-17 中国石油天然气股份有限公司 High oil absorption resin and its synthesis method
CN1973944A (en) * 2006-09-25 2007-06-06 厦门大学 Making process of integral stirring rod for solid phase extraction

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
"Incorporation of alkoxysilanes into model latex system: vinyl copolymerization of vinyltriethoxysilane and n-butyl acrylate";Ioan Macru等;《Macromolecules》;20050430;第36卷;第328页摘要,第330页表1 *

Also Published As

Publication number Publication date
CN102924657A (en) 2013-02-13

Similar Documents

Publication Publication Date Title
Zhou et al. Synthesis and characterization of a novel high‐oil‐absorbing resin
CN104341546B (en) A kind of preparation method of shelly oil absorbing polymer microsphere
Li et al. Hydrophobic modification of polyurethane foam for oil spill cleanup
CN101215355B (en) High oil absorption resin and synthetic method thereof
CN101967212B (en) Acrylate polymer high oil absorption resin and preparation method and application thereof
US4093570A (en) Production of porous polymers
CN102952236A (en) Molecularly imprinted polymeric microsphere resin applicable to aqueous solution system and preparing method thereof
CN104356318A (en) Lignin-based starlike thermoplastic elastomer and preparation method thereof
Galicia-Aguilar et al. Synthesis and characterization of AN/EGDMA-based adsorbents for phenol adsorption
CN109174011B (en) Super-hydrophobic metal organic framework composite material and preparation method and application thereof
CN112675824A (en) Fe3O4Chemically grafted polyacrylic acid-chitosan composite hydrogel and preparation method thereof
CN103333286B (en) A kind of oil-absorbing resin and preparation method thereof
CN102924657B (en) Oil absorption material containing silicon polymer and preparation methods thereof
CN105366789A (en) Multifunctional amphoteric polymer flocculant and preparation method thereof
CN107200810B (en) A kind of polyacrylate high oil-absorbing resin and preparation method thereof
CN101456937A (en) Polymethano-poly(methyl)acrylic ester two-block copolymer and preparation method thereof
Chen et al. Synthesis of well-defined structurally silica–nonlinear polymer core–shell nanoparticles via the surface-initiated atom transfer radical polymerization
KR20170041740A (en) Filtration material, filtration filter, method for manufacturing filtration material, filtration method, copolymer, and method for manufacturing copolymer
Ji et al. Synthesis of novel high oil‐absorption resins of poly (methyl methacrylate–butyl methacrylate) by surface‐initiated atom transfer radical polymerization using activators regenerated by electron transfer for efficient removal of oil
CN113996272B (en) Molecularly imprinted polymer and preparation method and application thereof
Fan et al. Protein–polymer hybrid oil–absorbing gel using hair keratin as macroinitiator by SET-LRP
Zhou et al. Synthesis and properties of novel high oil‐absorbing resin based on poly (ethylene‐propylene‐diene/α‐methylstyrene/itaconic acid)
Kizil et al. Reusable organosilicon hybrid sorbents with tunable oil interest via PEG-PPG copolymer
CN110655601A (en) Acrylic acid adsorption resin and ultraviolet polymerization preparation method and application thereof
CN110585762B (en) Polymer oil absorption material and preparation method thereof

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
CP02 Change in the address of a patent holder

Address after: 363000 the southern tip of Xiamen University Zhangzhou campus, Zhangzhou, Fujian

Patentee after: XIAMEN University

Address before: Xiamen City, Fujian Province, 361005 South Siming Road No. 422

Patentee before: XIAMEN University

CP02 Change in the address of a patent holder