CN102850475B - Method for preparing fast oil-absorption resin - Google Patents

Method for preparing fast oil-absorption resin Download PDF

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Publication number
CN102850475B
CN102850475B CN201210303763.4A CN201210303763A CN102850475B CN 102850475 B CN102850475 B CN 102850475B CN 201210303763 A CN201210303763 A CN 201210303763A CN 102850475 B CN102850475 B CN 102850475B
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oil
resin
monomer
linking agent
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CN102850475A (en
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喻发全
马立彬
薛亚楠
朱三
蔡宁
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Wuhan Hua Yuan Science And Technology Ltd
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Wuhan Institute of Technology
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Abstract

The invention relates to a method for preparing a fast oil-absorption resin. The method comprises the steps of: first adding an emulsifying agent and a crosslinking agent to monomers; stirring evenly; introducing nitrogen and stirring; dropwise adding deionized water to obtain an emulsion; adding a prepared initiator to the emulsion; reacting for 3 hours; and subjecting the product to vacuum drying to obtain the oil-absorption resin with fast oil-absorption rate. The invention has the following advantages: the fast oil-absorption resin has large porosity and good connectivity, so as to gain fast oil absorption rate; no pore-foamingagent is used; and while achieving a same saturated oil absorption amount, the resin provided by the invention can reach oil absorption saturation in 15-30 minutes. The invention has advantages of mild reaction temperature, convenient preparation method, environment-friendliness and no discharge of three wastes; in addition, the resin obtained by the invention has good reusability, and basically unchanged oil absorption amount after repeated usage, to overcome defect of declined performance of a general resin after repeated usage, thereby reducing the cost.

Description

A kind of preparation method of fast absorbing oil resin
Technical field
The preparation method who the present invention relates to a kind of fast absorbing oil resin, belongs to functional high polymer material field.
Background technology
Along with the fast development of China's economy, sudden great Environment Pollution Event increases increasingly.According to statistics, this type of event root of nearly 80% is in leakage, blast and the wastewater from chemical industry discharge of chemical industry.The chemical enterprise of China is close to water system mostly, once there is sudden accident, tends to river basin ecotope to cause severe contamination and destruction, even will constitute a serious threat to drinking water safety.For this type of sudden accident, often need to carry out at short notice quick emergency processing, the oil absorption resin that therefore exploitation has fast absorbing oil speed just seems particularly important.
At present, to the research of oil absorption resin, mainly concentrate on the number of oil number, and the common swelling rate of this resinoid is lower, generally needs a few hours oil number that just can reach capacity.In addition, the resin with fast absorbing oil speed that existing document is synthetic, need to add pore-creating agent mostly.Fast absorbing oil resin prepared by the present invention, without using pore-creating agent, in realizing equal saturated oil number, the oil number that can reach capacity in 15 ~ 30 minutes, has very fast swelling rate, and has good repetition oil suction use properties.Along with the enhancing of people's environmental consciousness, will improve constantly the demand of efficient oil absorption material, therefore, the exploitation of novel fast absorbing oil rosin products will have broad prospects.
Summary of the invention
Technical problem to be solved by this invention is the preparation method that a kind of fast absorbing oil resin is provided for above-mentioned prior art, overcome the slow problem of traditional oil absorption resin swelling rate, in reply burst and oil pollution event in need of immediate treatment, there is good effect, and fast absorbing oil resin prepared by the present invention, without using pore-creating agent, in realizing equal saturated oil number, oil number can reach capacity in 15 ~ 30 minutes, there is very fast swelling rate, and there is good repetition oil suction use properties.
The present invention solves the problems of the technologies described above adopted technical scheme: a kind of preparation method of fast absorbing oil resin: it is characterized in that comprising the steps: first emulsifying agent and linking agent being joined in monomer, stir, pass into nitrogen, low whipping speed is at the uniform velocity to drip deionized water under 400 ~ 1200 revs/min of speed, after dropwising, obtain emulsion, again the initiator of configuration is joined in the emulsion of gained, under 25 ~ 50 degrees Celsius, react after 3 hours, product is through vacuum-drying, can obtain having the oil absorption resin of fast absorbing oil speed, wherein, it is 5% ~ 30% that emulsifying agent accounts for monomer mass mark, it is 4% ~ 20% that linking agent accounts for monomer mass mark, it is 1% ~ 6% that initiator accounts for monomer mass mark, to add deionized water be 5 ~ 10 times of monomer mass.
Press such scheme, described monomer is the mixing of any one or they in acrylic ester monomer and methyl acrylic ester monomer.
Press such scheme, described acrylic ester monomer is: n-butyl acrylate, dodecyl acrylate or Process Conditions of Cetane Acrylate; Described methyl acrylic ester monomer is: n-BMA, methacrylic dodecyl gallate or methacrylic acid hexadecyl ester.
Press such scheme, described initiator is that Oxidizing and Reducing Agents is the water soluble oxidized-reduction initiating system of 0.9 ~ 1.2:1 composition in molar ratio, wherein said oxygenant is persulphate, and described reductive agent is hydrosulphite, sulphite or thiosulphate.
Press such scheme, described persulphate is ammonium persulphate or Sodium Persulfate, and described hydrosulphite is sodium bisulfite or Potassium hydrogen sulfite, and described sulphite is S-WAT, and described thiosulphate is Sulfothiorine.
Press such scheme, described emulsifying agent is the compound emulsifying agent of the class of department 80, class of department 60 and the class of department 80 and polysorbate60 composition.
Press such scheme, described linking agent is diene class linking agent or ester class linking agent.
Press such scheme, described diene class linking agent is Vinylstyrene; Described ester class linking agent is glycol diacrylate or Ethylene glycol dimethacrylate.
The preparating mechanism of fast absorbing oil resin of the present invention: water soluble oxidized reduction system causes oil-soluble monomer and carries out at ambient temperature Raolical polymerizable, prepares the resin with tridimensional network.
Compared with the prior art the present invention has the following advantages: fast absorbing oil resin has very large porosity, and there is good connectedness, therefore there is very fast swelling rate, overcome the general slow problem of oil absorption resin swelling rate, in reply burst and oil pollution event in need of immediate treatment, there is good effect.And without using pore-creating agent, in realizing equal saturated oil number, it is saturated that gained resin can reach oil suction in 15 ~ 30 minutes; Temperature of reaction gentleness of the present invention, preparation method is convenient, environmental protection produces without the three wastes; In addition, gained resin reusability of the present invention is good, and after Reusability, oil number is substantially constant, has overcome general resin and has repeatedly used the shortcoming of rear degradation, thereby reduced cost.
Accompanying drawing explanation
Fig. 1 is the swelling rate curve of embodiment 1 gained fast absorbing oil resin;
Fig. 2 is the repeat performance of embodiment 1 gained fast absorbing oil resin;
Fig. 3 is the scanning electron microscope (SEM) photograph of embodiment 1 gained fast absorbing oil resin.
Embodiment
In order to make the object, technical solutions and advantages of the present invention clearer, below in conjunction with accompanying drawing, the present invention is described in further detail:
Embodiment 1:
80,0.551 grams of Vinylstyrenes of 0.501 gram of class of department are joined in 6.258 grams of n-BMAs, pass at least 20 minutes excluding airs of nitrogen, under the stirring velocity of 1000 revs/min, at the uniform velocity drip 50 grams of deionized waters.After dropwising, take respectively 0.163 gram of ammonium persulphate (0.715 mmole) and 0.074 gram of sodium bisulfite (0.712 mmole) is mixed with the aqueous solution, add in above-mentioned emulsion, 40 degrees Celsius of reactions after 3 hours, product, through vacuum-drying, can obtain oil absorption resin.
Gained oil absorption resin is 8.5 times to the oil suction multiplying power of toluene, is 15.4 times to the oil suction multiplying power of chloroform; Its required time that reaches capacity is 30 minutes.
Fig. 1 is the swelling rate curve of gained resin, as can be seen from Figure 1, and the resin oil number that can reach capacity at 30 minutes.This is to have substantial connection due to the swelling rate of resin and the specific surface area of resin: the specific surface area of resin is larger, and swelling rate is faster.And the resin of gained of the present invention has very large specific surface area, therefore there is higher swelling rate;
Fig. 2 is the repeat performance of gained resin, and as can be seen from Figure 2, through the repetition oil suction experiment of five times, the oil number of resin is substantially constant, illustrates that resin has good repeat performance;
Fig. 3 is the scanning electron microscope (SEM) photograph of gained resin, and as can be seen from Figure 3, a large amount of random cavernous structure distributing in resin makes its specific surface area larger, thereby provides safeguard for fast absorbing oil.
Embodiment 2:
80 and 0.081 grams of polysorbate60s of 1.064 grams of classes of department, 0.551 gram of Vinylstyrene are joined in 6.3 grams of n-butyl acrylates, pass at least 20 minutes excluding airs of nitrogen, under the stirring velocity of 1000 revs/min, at the uniform velocity drip 32 grams of deionized waters.After dropwising, take respectively 0.23 gram of ammonium persulphate (1.009 mmole) and 0.105 gram of sodium bisulfite (1.01 mmole), be mixed with the aqueous solution, join in above-mentioned emulsion, 30 degrees Celsius of reactions, after 3 hours, product, through vacuum-drying, can obtain oil absorption resin.
Gained oil absorption resin is 5.5 times to the oil suction multiplying power of toluene, is 11.1 times to the oil suction multiplying power of chloroform; Its required time that reaches capacity is 20 minutes.
Embodiment 3:
80,0.676 grams of Ethylene glycol dimethacrylate of 1.064 grams of classes of department are joined in 6.3 grams of n-butyl acrylates, pass at least 20 minutes excluding airs of nitrogen, under the stirring velocity of 1200 revs/min, at the uniform velocity drip 32 grams of deionized waters.After dropwising, take respectively 0.133 gram of ammonium persulphate (0.583 mmole) and 0.092 gram of Sulfothiorine (0.582 mmole) is mixed with the aqueous solution, join in above-mentioned emulsion, 40 degrees Celsius of reactions after 3 hours, product, through vacuum-drying, can obtain oil absorption resin.
Gained oil absorption resin is 6.7 times to the oil suction multiplying power of toluene, is 13.2 times to the oil suction multiplying power of chloroform; Its required time that reaches capacity is 30 minutes.
Embodiment 4:
80,0.734 grams of Vinylstyrenes of 1.252 grams of classes of department are joined in 3.129 grams of n-BMAs and 3.143 grams of n-butyl acrylates, pass at least 20 minutes excluding airs of nitrogen, under the stirring velocity of 1000 revs/min, at the uniform velocity drip 32 grams of deionized waters.After dropwising, take respectively 0.134 gram of ammonium persulphate (0.588 mmole) and 0.074 gram of S-WAT (0.587 mmole) is mixed with the aqueous solution, join in above-mentioned emulsion, 40 degrees Celsius of reactions after 3 hours, product, through vacuum-drying, can obtain oil absorption resin.
Gained oil absorption resin is 7.8 times to the oil suction multiplying power of toluene, is 14.5 times to the oil suction multiplying power of chloroform; Its required time that reaches capacity is 25 minutes.
Embodiment 5:
80,0.547 grams of Ethylene glycol dimethacrylate of 0.931 gram of class of department are joined in 6.258 grams of n-BMAs, pass at least 20 minutes excluding airs of nitrogen, under the stirring velocity of 1000 revs/min, at the uniform velocity drip 32 grams of deionized waters.After dropwising, take respectively 0.23 gram of Sodium Persulfate (0.966 mmole) and 0.103 gram of sodium bisulfite (0.99 mmole) is mixed with the aqueous solution, join in above-mentioned emulsion, 40 degrees Celsius of reactions after 3 hours, product, through vacuum-drying, can obtain oil absorption resin.
Gained oil absorption resin is 5.9 times to the oil suction multiplying power of toluene, is 11 times to the oil suction multiplying power of chloroform; Its required time that reaches capacity is 20 minutes.

Claims (5)

1. the preparation method of a fast absorbing oil resin, it is characterized in that being prepared by following steps: first emulsifying agent and linking agent are joined in monomer, stir, pass into nitrogen, low whipping speed is at the uniform velocity to drip deionized water under 400 ~ 1200 revs/min of speed, after dropwising, obtain emulsion, again the initiator of configuration is joined in the emulsion of gained, under 25 ~ 50 degrees Celsius, react after 3 hours, product is through vacuum-drying, can obtain having the oil absorption resin of fast absorbing oil speed, wherein, it is 5% ~ 30% that emulsifying agent accounts for monomer mass mark, it is 4% ~ 20% that linking agent accounts for monomer mass mark, it is 1% ~ 6% that initiator accounts for monomer mass mark, to add deionized water be 5 ~ 10 times of monomer mass, described initiator is that Oxidizing and Reducing Agents is the water soluble oxidized-reduction initiating system of 0.9 ~ 1.2:1 composition in molar ratio, wherein said oxygenant is persulphate, described reductive agent is hydrosulphite, sulphite or thiosulphate, described persulphate is ammonium persulphate or Sodium Persulfate, described hydrosulphite is sodium bisulfite or Potassium hydrogen sulfite, described sulphite is S-WAT, described thiosulphate is Sulfothiorine, described emulsifying agent is class of department 80, the compound emulsifying agent of class of department 60 or class 80 of department and polysorbate60 composition.
2. the preparation method of fast absorbing oil resin according to claim 1, is characterized in that described monomer is the mixing of any one or they in acrylic ester monomer and methyl acrylic ester monomer.
3. the preparation method of fast absorbing oil resin according to claim 2, is characterized in that described acrylic ester monomer is: n-butyl acrylate, dodecyl acrylate or Process Conditions of Cetane Acrylate; Described methyl acrylic ester monomer is: n-BMA, methacrylic dodecyl gallate or methacrylic acid hexadecyl ester.
4. the preparation method of fast absorbing oil resin according to claim 1, is characterized in that described linking agent is diene class linking agent or ester class linking agent.
5. the preparation method of fast absorbing oil resin according to claim 4, is characterized in that described diene class linking agent is Vinylstyrene; Described ester class linking agent is glycol diacrylate or Ethylene glycol dimethacrylate.
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CN103333286B (en) * 2013-07-23 2015-11-11 中蓝晨光化工研究设计院有限公司 A kind of oil-absorbing resin and preparation method thereof
CN106366240B (en) * 2016-10-10 2018-09-11 四川奎能环保科技有限公司 A kind of oil-absorbing resin material and preparation method thereof
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
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
CN109485782A (en) * 2018-09-27 2019-03-19 江苏师范大学 A kind of preparation method of new hydrophobic oleophilic resin

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102199242A (en) * 2011-03-26 2011-09-28 鲁东大学 Preparation method of porous high-oil-absorbing resin
CN102504072A (en) * 2011-11-09 2012-06-20 西北师范大学 Porous high-oil-absorption resin and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102199242A (en) * 2011-03-26 2011-09-28 鲁东大学 Preparation method of porous high-oil-absorbing resin
CN102504072A (en) * 2011-11-09 2012-06-20 西北师范大学 Porous high-oil-absorption resin and preparation method thereof

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
丙烯酸系高性能吸油树脂的合成及性能研究;南粉益;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》;20100520;第3.2.5节,第3.2.4节 *
张慧婷 等.氧化还原引发AA/AM/AMPS超浓反相乳液聚合及乳液稳定性的研究.《化学与生物工程》.2012,第29卷(第1期),第25-28页. *
氧化还原引发AA/AM/AMPS超浓反相乳液聚合及乳液稳定性的研究;张慧婷 等;《化学与生物工程》;20120125;第29卷(第1期);第26页第1.2节 *

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