CN102199242B - Preparation method of porous high-oil-absorbing resin - Google Patents
Preparation method of porous high-oil-absorbing resin Download PDFInfo
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- CN102199242B CN102199242B CN 201110080891 CN201110080891A CN102199242B CN 102199242 B CN102199242 B CN 102199242B CN 201110080891 CN201110080891 CN 201110080891 CN 201110080891 A CN201110080891 A CN 201110080891A CN 102199242 B CN102199242 B CN 102199242B
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Abstract
The invention discloses a preparation method of a porous high-oil-absorbing resin. The method is characterized by comprising the following steps: firstly, adding an initiator (azobisisobutyronitrile), an emulsifier span-80, a porogenic agent and a cross-linking agent in a monomer octadecyl methacrylate; evenly stirring; dropwise adding an aqueous solution of anhydrous calcium chloride at a constant speed while stirring; after dropwise adding, continuing to stir; then carrying out high internal phase emulsion template polymerization; cooling, separating, extracting by utilizing a Soxhlet extractor and carrying out vacuum drying on the product so as to obtain the porous high-oil-absorbing resin. By virtue of the preparation method disclosed by the invention, the porous high-oil-absorbing resin the oil-absorbing multiplying factor of which on chloroform is 20 times is obtained.
Description
Technical field
The present invention relates to a kind of preparation method of porous high-oil-absorbing resin, specifically a kind of method for preparing porous high-oil-absorbing resin based on the high internal phase ratio emulsions template polymerization, belong to functional high polymer material field.
Background technology
Along with the development of world industry, the greasy dirt problem is very serious, oily(waste)water particularly, and liquid waste and oil carrier, the oil tank oil accident increases and causes the river, and the pollution of ocean consists of great threat to the mankind's environment and human lives.In order to administer greasy dirt, most study is the high oil absorbing resin that preparation contains chemically crosslinked at present, and traditional preparation method is suspension polymerization and emulsion polymerization.
In recent years, high internal phase ratio emulsions template polymerization technology is noticeable in the research of material preparation technology.The high internal phase ratio emulsions template polymerization can prepare size and the controlled porous material of pore size distribution with hole, rarely has report but use it for the preparation porous high-oil-absorbing resin.Along with the enhancing of people's environmental consciousness, will increase rapidly the demand of high-efficiency environment friendly with oil absorption material, the development of new high oil-absorbing resin has huge economic benefit and social benefit.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of porous high-oil-absorbing resin.
The invention provides a kind of preparation method of porous high-oil-absorbing resin, comprise the steps:
at first with the initiator Diisopropyl azodicarboxylate, class of emulsifying agent department 80, pore-creating agent, linking agent joins in the monomer stearyl methacrylate, stir, at the uniform velocity drip the Calcium Chloride Powder Anhydrous aqueous solution under stirring, continue to be stirred to few 0.5 hour after dropwising, then carry out the high internal phase ratio emulsions template polymerization, reaction was carried out 12 hours at least, wherein, monomer and initiator mol ratio are 5: 1～15: 1, emulsifying agent occupies 25%～40% of machine phase volume, 4%～15% of linking agent and organic phase volume, pore-creating agent occupies 25%～41% of machine phase volume, calcium chloride water concentration is 0.0015 grams per milliliter～0.01 grams per milliliter, the water volume fraction is 77%～85%, stir speed (S.S.) is 200～500 rev/mins, temperature of reaction is 65～90 degrees centigrade, product is through cooling, separate, apparatus,Soxhlet's extracting at least 12 hours, vacuum-drying obtains porous high-oil-absorbing resin.
When preparing this resin, linking agent used is Vinylstyrene, pentaerythritol triacrylate, tetramethylol methane tetraacrylate etc., and pore-creating agent is hexanaphthene, normal heptane etc.
Compared with the prior art the present invention has following advantage: preparation method provided by the invention is simple and easy to do, by the adjusting to initiator, linking agent, emulsifier, control the reaction conditionss such as stir speed (S.S.), temperature, can control the size of polymerisate particle, obtain the high oil-absorbing resin of outward appearance porous, gained porous high-oil-absorbing resin oil absorbency is large, oil-retaining strong, the regeneration rate is high.
Embodiment
The below describes the present invention in detail and provides several embodiment:
Embodiment one:
0.1 gram Diisopropyl azodicarboxylate, 80,5.0 milliliters of hexanaphthenes of 4.8 milliliters of classes of department, 0.5 milliliter of pentaerythritol triacrylate are joined in 2.0 milliliters of stearyl methacrylates, rotating speed with 350 rev/mins stirs, at the uniform velocity drip 50.0 milliliters of aqueous solution that are dissolved with 0.2 gram Calcium Chloride Powder Anhydrous under stirring, dropwising rear continuation stirred 0.5 hour, then move into and carry out high internal phase ratio emulsions template polymerization reaction 12 hours in the constant temperature oil bath of 75 degrees centigrade, product obtains porous high-oil-absorbing resin through cooling, separation, apparatus,Soxhlet's extracting 12 hours, vacuum-drying.
The gained high oil-absorbing resin is 20 times to the oil suction multiplying power of chloroform, is 11 times to the oil suction multiplying power of toluene, is 13 times to the oil suction multiplying power of benzene.
Embodiment two:
0.2 gram Diisopropyl azodicarboxylate, 80,5.5 milliliters of hexanaphthenes of 5.5 milliliters of classes of department, 0.75 milliliter of pentaerythritol triacrylate are joined in 3.0 milliliters of stearyl methacrylates, rotating speed with 400 rev/mins stirs, at the uniform velocity drip 60.0 milliliters of aqueous solution that are dissolved with 0.5 gram Calcium Chloride Powder Anhydrous under stirring, dropwising rear continuation stirred 35 minutes, then move into and carry out high internal phase ratio emulsions template polymerization reaction 14 hours in the constant temperature oil bath of 80 degrees centigrade, product obtains porous high-oil-absorbing resin through cooling, separation, apparatus,Soxhlet's extracting 15 hours, vacuum-drying.
The gained high oil-absorbing resin is 18 times to the oil suction multiplying power of chloroform, is 12 times to the oil suction multiplying power of toluene, is 10 times to the oil suction multiplying power of benzene.
Embodiment three:
0.18 gram Diisopropyl azodicarboxylate, 80,3.5 milliliters of hexanaphthenes of 4.0 milliliters of classes of department, 1.5 milliliters of Vinylstyrenes are joined in 3.2 milliliters of stearyl methacrylates, rotating speed with 200 rev/mins stirs, at the uniform velocity drip 48.0 milliliters of aqueous solution that are dissolved with 0.1 gram Calcium Chloride Powder Anhydrous under stirring, dropwising rear continuation stirred 45 minutes, then move into and carry out high internal phase ratio emulsions template polymerization reaction 15 hours in the constant temperature oil bath of 75 degrees centigrade, product obtains porous high-oil-absorbing resin through cooling, separation, apparatus,Soxhlet's extracting 16 hours, vacuum-drying.
The gained high oil-absorbing resin is 14 times to the oil suction multiplying power of chloroform, is 8 times to the oil suction multiplying power of toluene, is 5 times to the oil suction multiplying power of benzene.
Embodiment four:
0.25 gram Diisopropyl azodicarboxylate, 80,4.5 milliliters of hexanaphthenes of 5.0 milliliters of classes of department, 2.0 milliliters of tetramethylol methane tetraacrylates are joined in 5.4 milliliters of stearyl methacrylates, rotating speed with 450 rev/mins stirs, at the uniform velocity drip 60.0 milliliters of aqueous solution that are dissolved with 0.2 gram Calcium Chloride Powder Anhydrous under stirring, dropwising rear continuation stirred 40 minutes, then move into and carry out high internal phase ratio emulsions template polymerization reaction 17 hours in the constant temperature oil bath of 75 degrees centigrade, product obtains porous high-oil-absorbing resin through cooling, separation, apparatus,Soxhlet's extracting 20 hours, vacuum-drying.
The gained high oil-absorbing resin is 9 times to the oil suction multiplying power of chloroform, is 7 times to the oil suction multiplying power of toluene, is 5 times to the oil suction multiplying power of benzene.
Embodiment five:
0.12 gram Diisopropyl azodicarboxylate, 80,5.0 milliliters of normal heptanes of 3.0 milliliters of classes of department, 1.0 milliliters of pentaerythritol triacrylates are joined in 2.0 milliliters of stearyl methacrylates, rotating speed with 250 rev/mins stirs, at the uniform velocity drip 60.0 milliliters of aqueous solution that are dissolved with 0.1 gram Calcium Chloride Powder Anhydrous under stirring, dropwising rear continuation stirred 50 minutes, then move into and carry out high internal phase ratio emulsions template polymerization reaction 18 hours in the constant temperature oil bath of 65 degrees centigrade, product obtains porous high-oil-absorbing resin through cooling, separation, apparatus,Soxhlet's extracting 14 hours, vacuum-drying.
The gained high oil-absorbing resin is 13 times to the oil suction multiplying power of chloroform, is 7 times to the oil suction multiplying power of toluene, is 8 times to the oil suction multiplying power of benzene.
Claims (2)
1. the preparation method of a porous high-oil-absorbing resin, it is characterized in that: at first with the initiator Diisopropyl azodicarboxylate, class of emulsifying agent department 80, pore-creating agent, linking agent joins in the monomer stearyl methacrylate, stir, at the uniform velocity drip the Calcium Chloride Powder Anhydrous aqueous solution under stirring, continue to be stirred to few 0.5 hour after dropwising, then carry out the high internal phase ratio emulsions template polymerization, reaction was carried out 12 hours at least, wherein, monomer and initiator mol ratio are 5: 1～15: 1, emulsifying agent occupies 25%～40% of machine phase volume, linking agent occupies 4%～15% of machine phase volume, pore-creating agent occupies 25%～41% of machine phase volume, calcium chloride water concentration is 0.0015 grams per milliliter～0.01 grams per milliliter, the water volume fraction is 77%～85%, stir speed (S.S.) is 200～500 rev/mins, temperature of reaction is 65～90 degrees centigrade, product is through cooling, separate, apparatus,Soxhlet's extracting at least 12 hours, vacuum-drying obtains porous high-oil-absorbing resin.
2. when it is characterized in that preparing this resin according to the preparation method of the described a kind of porous high-oil-absorbing resin of claim 1., linking agent used is Vinylstyrene, pentaerythritol triacrylate, tetramethylol methane tetraacrylate, and pore-creating agent is hexanaphthene, normal heptane.
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| CN 201110080891 CN102199242B (en) | 2011-03-26 | 2011-03-26 | Preparation method of porous high-oil-absorbing resin |
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| CN 201110080891 CN102199242B (en) | 2011-03-26 | 2011-03-26 | Preparation method of porous high-oil-absorbing resin |
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| CN102199242B true CN102199242B (en) | 2013-05-08 |
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| CN102850475B (en) * | 2012-08-24 | 2014-07-09 | 武汉工程大学 | Method for preparing fast oil-absorption resin |
| CN103342990A (en) * | 2013-07-11 | 2013-10-09 | 上海大学 | Preparation method of pomelo peel oil absorption material |
| CN104710554A (en) * | 2015-01-05 | 2015-06-17 | 泰山医学院 | Preparation method of interpenetrating network porous polymer composite material |
| CN106478866A (en) * | 2016-10-07 | 2017-03-08 | 琼州学院 | A kind of preparation method of organic porous material |
| CN107617427B (en) * | 2017-10-09 | 2020-06-16 | 浙江卫星新材料科技有限公司 | Preparation method of graphene high oil absorption resin |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5210104A (en) * | 1992-10-15 | 1993-05-11 | Shell Oil Company | Process for preparing low density porous crosslinked polymeric materials |
| WO1999009070A1 (en) * | 1997-08-15 | 1999-02-25 | The Dow Chemical Company | High internal phase emulsions and porous materials prepared therefrom |
| CN101215355A (en) * | 2008-01-09 | 2008-07-09 | 苏州大学 | High oil absorption resin and synthetic method thereof |
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| CA2488981C (en) * | 2003-12-15 | 2008-06-17 | Rohm And Haas Company | Oil absorbing composition and process |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5210104A (en) * | 1992-10-15 | 1993-05-11 | Shell Oil Company | Process for preparing low density porous crosslinked polymeric materials |
| WO1999009070A1 (en) * | 1997-08-15 | 1999-02-25 | The Dow Chemical Company | High internal phase emulsions and porous materials prepared therefrom |
| CN101215355A (en) * | 2008-01-09 | 2008-07-09 | 苏州大学 | High oil absorption resin and synthetic method thereof |
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