CN102796226B - Preparation method for high oil absorbency resin by cotton cellulose macroinitiator - Google Patents
Preparation method for high oil absorbency resin by cotton cellulose macroinitiator Download PDFInfo
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- CN102796226B CN102796226B CN 201210304825 CN201210304825A CN102796226B CN 102796226 B CN102796226 B CN 102796226B CN 201210304825 CN201210304825 CN 201210304825 CN 201210304825 A CN201210304825 A CN 201210304825A CN 102796226 B CN102796226 B CN 102796226B
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- cotton cellulose
- butyl methacrylate
- high oil
- modification
- copper powder
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Abstract
The invention discloses a preparation method for high oil absorbency resin by a cotton cellulose macroinitiator, and is characterized by modifying cotton cellulose into the macroinitiator, dissolving a monomer of butyl methacrylate, a crosslinking agent of pentaerythritol triacrylate, a catalyst of copper powder and a ligand of hexamethylenetetramine in an N,N-dimethylformamide solvent and stirring to uniform, then adding the modified cotton cellulose macroinitiator to perform single electron transfer living radical polymerization, washing the product by nitric acid, extracting by ethanol, and drying to obtain the high oil absorbency resin. The high oil absorbency resin, which has oil absorption multiplying power of 29 times for chloroform, can be obtained by the preparation method disclosed by the invention.
Description
Technical field
The present invention relates to the method that a kind of cotton cellulose macromole evocating agent prepares high oil-absorbing resin, specifically is a kind ofly to prepare the method for high oil-absorbing resin based on the single electron transfer active free radical polymerization, belongs to functional high polymer material field.
Background technology
Along with the continuous development of world industryization, the oil pollution problem is on the rise, wherein liquid waste, oily(waste)water, and oil carrier, and the oil tank oil accident not only causes the pollution of river, ocean, and the mankind's environment and life constituted greatly threatens.Natural oil absorption material such as clay, lime, it is poor that peat bog, kapok etc. has oil-retaining, and pressurized leakage of oil, also shortcoming such as suction are simultaneously carried out surface modification with traditional material and can finely be overcome above-mentioned shortcoming.
Advantages such as in recent years, the single electron transfer living radical polymerization technique is noticeable, and it is low to have temperature of reaction, and catalyst levels is few, and is easy and simple to handle, and polymerization velocity is fast.The cotton cellulose that extensively exists with occurring in nature is that matrix prepares oil absorption material, comprehensive production cost is reduced greatly, but also can utilize the tiny internal structure of Mierocrystalline cellulose, improves oil absorptiveness.Simultaneously, because cellulose materials itself has good degradability, also can eliminate discarded synthetic oil-absorbing resin to the pollution of environment, maintaining ecological balance.
Summary of the invention
The object of the present invention is to provide a kind of cotton cellulose macromole evocating agent to prepare the method for high oil-absorbing resin.
The invention provides the method that a kind of cotton cellulose macromole evocating agent prepares high oil-absorbing resin, comprise the steps:
With through 2-bromine isobutyl acylbromide, the 4-methylamino pyridine, the cotton cellulose of triethylamine modification is macromole evocating agent, with the monomer butyl methacrylate, the linking agent pentaerythritol triacrylate, catalyst copper powder, the part hexamethylenetetramine is dissolved into N, stir in the dinethylformamide solvent, add the cotton cellulose macromole evocating agent after the modification then, wherein, the mass ratio of butyl methacrylate and modification cotton cellulose is 100:3～100:6, the volume ratio of butyl methacrylate and pentaerythritol triacrylate is 100:0.2～100:1.8, the mol ratio of butyl methacrylate and copper powder is 200:0.1～200:0.5, the mol ratio of copper powder and hexamethylenetetramine is 0.1:0.6～0.5:0.6, butyl methacrylate and N, the volume ratio of dinethylformamide is 1:0.5～1:3, polymeric reaction temperature is 65～85 degrees centigrade, carry out the single electron transfer active free radical polymerization, reacted at least 8 hours, product washs through nitric acid, the ethanol extracting, drying obtains high oil-absorbing resin.
Compared with the prior art the present invention has following advantage: the single electron transfer living free radical polymerization is a kind of emerging " activity "/controllable polymerization method, and is easy and simple to handle.The cotton cellulose matrix is carried out modification afterwards as initiator, adopt the macromole surface to cause and carry out three-dimensional graft polymerization at matrix surface, can form more perfect three-dimensional net structure.Gained high oil-absorbing resin oil absorbency is big, oil-retaining strong, regeneration rate height.
Embodiment
Describe the present invention below in detail and provide several embodiment:
Synthetic cotton cellulose macromole evocating agent.With 2-bromine isobutyl acylbromide, 4-methylamino pyridine, the triethylamine modification obtains the cotton cellulose macromole evocating agent.All use the macromole evocating agent of this type of modification among the embodiment.
Embodiment one:
With the 10ml butyl methacrylate, 0.1ml pentaerythritol triacrylate, 0.0060g copper powder, 0.0265g hexamethylenetetramine is dissolved into 10ml N, stir in the dinethylformamide, the cotton cellulose macromole evocating agent that adds the 0.5g modification then, three logical nitrogen-vacuumize-the Tong nitrogen cycle repeatedly, move into then in 75 degrees centigrade the constant temperature oil bath and carry out the single electron transfer active free radical polymerization, reacted 12 hours, product washs through nitric acid, the ethanol extracting, drying obtains high oil-absorbing resin.
The gained high oil-absorbing resin is 29 times to the oil suction multiplying power of chloroform, is 17 times to the oil suction multiplying power of toluene.
Embodiment two:
With the 10ml butyl methacrylate, 0.06ml pentaerythritol triacrylate, 0.0060g copper powder, 0.0265g hexamethylenetetramine is dissolved into 10ml N, stir in the dinethylformamide, the cotton cellulose macromole evocating agent that adds the 0.5g modification then, three logical nitrogen-vacuumize-the Tong nitrogen cycle repeatedly, move into then in 70 degrees centigrade the constant temperature oil bath and carry out the single electron transfer active free radical polymerization, reacted 12 hours, product washs through nitric acid, the ethanol extracting, drying obtains high oil-absorbing resin.
The gained high oil-absorbing resin is 25 times to the oil suction multiplying power of chloroform, is 14 times to the oil suction multiplying power of toluene.
Embodiment three:
With the 10ml butyl methacrylate, 0.1ml pentaerythritol triacrylate, 0.0040g copper powder, 0.0265g hexamethylenetetramine is dissolved into 10ml N, stir in the dinethylformamide, add the cotton cellulose macromole evocating agent of 0.3g modification then, repeatedly three logical nitrogen-vacuumize-the Tong nitrogen cycle, move into then in 75 degrees centigrade the constant temperature oil bath and carry out the single electron transfer active free radical polymerization, reacted 12 hours, product washs through nitric acid, the ethanol extracting, drying obtains high oil-absorbing resin.
The gained high oil-absorbing resin is 21 times to the oil suction multiplying power of chloroform, is 12 times to the oil suction multiplying power of toluene.
Embodiment four:
With the 10ml butyl methacrylate, 0.1ml pentaerythritol triacrylate, 0.0060g copper powder, 0.0265g hexamethylenetetramine is dissolved into 10ml N, stir in the dinethylformamide, add the cotton cellulose macromole evocating agent of 0.5g modification then, repeatedly three logical nitrogen-vacuumize-the Tong nitrogen cycle, move into then in 75 degrees centigrade the constant temperature oil bath and carry out the single electron transfer active free radical polymerization, reacted 8 hours, product washs through nitric acid, the ethanol extracting, drying obtains high oil-absorbing resin.
The gained high oil-absorbing resin is 17 times to the oil suction multiplying power of chloroform, is 9 times to the oil suction multiplying power of toluene.
Claims (1)
1. a cotton cellulose macromole evocating agent prepares the method for high oil-absorbing resin, it is characterized in that: with through 2-bromine isobutyl acylbromide, the 4-methylamino pyridine, the cotton cellulose of triethylamine modification is macromole evocating agent, with the monomer butyl methacrylate, the linking agent pentaerythritol triacrylate, catalyst copper powder, the part hexamethylenetetramine is dissolved into N, stir in the dinethylformamide solvent, add the cotton cellulose macromole evocating agent after the modification then, wherein, the mass ratio of butyl methacrylate and modification cotton cellulose is 100:3～100:6, the volume ratio of butyl methacrylate and pentaerythritol triacrylate is 100:0.2～100:1.8, the mol ratio of butyl methacrylate and copper powder is 200:0.1～200:0.5, the mol ratio of copper powder and hexamethylenetetramine is 0.1:0.6～0.5:0.6, butyl methacrylate and N, the volume ratio of dinethylformamide is 1:0.5～1:3, polymeric reaction temperature is 65～85 degrees centigrade, carry out the single electron transfer active free radical polymerization, reacted at least 8 hours, product washs through nitric acid, the ethanol extracting, drying obtains high oil-absorbing resin.
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| CN 201210304825 CN102796226B (en) | 2012-08-25 | 2012-08-25 | Preparation method for high oil absorbency resin by cotton cellulose macroinitiator |
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| CN 201210304825 CN102796226B (en) | 2012-08-25 | 2012-08-25 | Preparation method for high oil absorbency resin by cotton cellulose macroinitiator |
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| CN102796226A CN102796226A (en) | 2012-11-28 |
| CN102796226B true CN102796226B (en) | 2013-10-02 |
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| US9587062B2 (en) * | 2014-12-15 | 2017-03-07 | Henkel IP & Holding GmbH and Henkel AG & Co. KGaA | Photocrosslinkable block copolymers for hot-melt adhesives |
| CN110975832A (en) * | 2019-12-11 | 2020-04-10 | 安徽大学 | Straw-based hydrogel adsorbent for efficiently removing heavy metal ions and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101067015A (en) * | 2007-06-01 | 2007-11-07 | 华东理工大学 | Polypeptide-polyacrylic acid copolymer and its prepn process |
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| US7196142B2 (en) * | 2002-04-04 | 2007-03-27 | The University Of Akron | Polyisobutylene-based block anionomers and cationomers and synthesis thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101067015A (en) * | 2007-06-01 | 2007-11-07 | 华东理工大学 | Polypeptide-polyacrylic acid copolymer and its prepn process |
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