CN101555313B - Ethylene rhodanate/epoxide resin microballoon and preparation method thereof - Google Patents
Ethylene rhodanate/epoxide resin microballoon and preparation method thereof Download PDFInfo
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- CN101555313B CN101555313B CN2009100313683A CN200910031368A CN101555313B CN 101555313 B CN101555313 B CN 101555313B CN 2009100313683 A CN2009100313683 A CN 2009100313683A CN 200910031368 A CN200910031368 A CN 200910031368A CN 101555313 B CN101555313 B CN 101555313B
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- microballoon
- epoxide resin
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Abstract
The invention discloses an ethylene rhodanate/epoxide resin microballoon and a preparation method thereof. The ethylene rhodanate/epoxide resin microballoon is synthesized by taking ethylene rhodanateresin, amine and derivative thereof, epoxide resin and the like as the main material. The prepared microballoon has high heat resistance and excellent hydrophobic property. The preparation method has the characteristics of simple operation technique and good experiment repetitiveness. The synthesized microballoon is expected to be used for toughening modification of resin matrix and composite mat erial thereof and further has wide application scope in the aspects such as refining, separating and purifying biological chemicals, etc.
Description
Technical field
The present invention relates to a kind of ethylene rhodanate/epoxide resin microballoon and preparation method thereof, belong to technical field of polymer materials.
Background technology
Polymer microballoon is a kind of new function material of excellent property, has characteristics such as surface effects, volume effect, magnetic effect, biocompatibility, functional group.In separation fields such as standard metering, biomedicine, information, analytical chemistry, colloid science and chromatogram, be widely used.After introducing the types of functionality group on the polymer microballoon, it also has a good application prospect in many high-tech sectors such as biotechnology, immunity inspection, electronics and microelectronics, information industry, high performance liquid chromatography, and the filler that especially the hard list disperses, the non-porous polymer microballoon is matrix is one of focus of studying in efficient hydrophobic interaction chromatogram (HPHIC) stationary phase.As polymer microballoon, except having above-mentioned described application, the application that polymer microballoon is joined in resin base and the matrix material thereof has obtained paying close attention to widely.Microballoon is applied to gives effects such as material is fire-retardant, toughness reinforcing in resin base and the matrix material thereof.Can be used at present resin and and the kind of the microballoon of matrix material comparatively single, very few in particular for the microballoon of the performance resins of high-temperature molding and matrix material thereof.As seen, the microballoon of synthetic resistance to elevated temperatures, for expand its resin of high-temperature molding and associated materials application have active effect.
Resins, epoxy is the resin of a class excellent performance, have that cohesiveness is strong, shrinking percentage is little, the performance of a series of excellences such as dielectric properties, mechanical property and chemical stability are good, and can be by the optimization design of molecular structure, use different solidifying agent, adopt different conditions of cure to be met the material of different application.Cyanate ester resin has excellent dielectric properties, high heat resistance, good comprehensive mechanical properties and extremely low water-intake rate.Being raw material with the cyanate has positive effect as the wall material of microballoon to aspects such as the thermotolerance that improves microballoon, water tolerance.Therefore, can believe, with cyanate and Resins, epoxy is that main raw material synthetic polymer microballoon has high thermotolerance, and have excellent hydrophobic property, can in the material of high-temperature molding, be applied, in addition, but this microsphere surface contains-reactive groups such as OH, by the purpose surface modification is arranged, can give that it is different functional, have important researching value and wide prospect at chromatographic technique.
Summary of the invention
The object of the present invention is to provide a kind of have thermotolerance height, ethylene rhodanate/epoxide resin microballoon that hydrophobicity is good and preparation method thereof.
The technical scheme that realizes the foregoing invention purpose provides a kind of ethylene rhodanate/epoxide resin microballoon, unit meter by weight, and its composition proportioning is:
Cyanate ester resin 5～50b
Resins, epoxy 2～100b
Amine and derivative 5～200b thereof
Wherein, b is a weight unit.
Described cyanate ester resin is bisphenol A cyanate ester resin, dicyclopentadiene type ethylene rhodanate resin and phenol aldehyde type cyanate ester resin.
Described Resins, epoxy is glycidyl ether based epoxy resin, glycidyl ester based epoxy resin, Racemic glycidol amine epoxy resin, line style aliphatic category Resins, epoxy or alicyclic based epoxy resin.
Described amine and derivative thereof are imidazoles and 2-ethyl-4-methylimidazole.
Described tensio-active agent is: Sudan Gum-arabic, Sodium dodecylbenzene sulfonate and sodium lauryl sulphate.
A kind of preparation method of ethylene rhodanate/epoxide resin microballoon, its step comprises:
A. under agitation condition, be weight unit, by weight, 5～50b cyanate ester resin and 5～200b amine and derivative thereof put in an amount of alcohol solvent that control reaction temperature is incubated 5～6 hours at 60～90 ℃, obtains the cyanate prepolymer solution with b;
B. 2～100b Resins, epoxy is joined in the surfactant soln, stir through the homogeneous stirrer and obtain epoxy resin latex;
C. at 60～90 ℃, under the agitation condition, epoxy resin latex in the B step is joined in the cyanate prepolymer solution in the A step, react after 2～4 hours, promptly obtain ethylene rhodanate/epoxide resin microballoon suspension, through cooling, solution washing, suction filtration, drying obtains light yellow ethylene rhodanate/epoxide resin microballoon finished product
The beneficial effect that the present invention has is: prepared ethylene rhodanate/epoxide resin microballoon has high heat resistance and water tolerance.The preparation method who is adopted has wide, the operating procedure characteristic of simple of suitability.Can be used for the toughness reinforcing of high-temperature molding thermosetting resin reaches with in the separation technology field.
Embodiment
Below in conjunction with embodiment the present invention is further described:
Embodiment 1:
Present embodiment technical scheme concrete steps are as follows:
A. in disposing the there-necked flask of condensing works, under the agitation condition 10g bisphenol A cyanate ester resin and 1g imidazoles are put into the 50g alcohol solvent, control reaction temperature is incubated 2～6 hours at 60～90 ℃, obtains the cyanate prepolymer solution;
B. 10g glycidyl ether based epoxy resin (E-51) is added concentration and be in 3% the 50 gram Sodium dodecylbenzene sulfonate solution, stir through the homogeneous stirrer and obtain epoxy resin latex;
C. at 60～90 ℃, it is 600rpm that stir speed (S.S.) is set, epoxy resin latex in the B step is joined cyanate prepolymer solution in the A step, react after 2～4 hours, promptly obtain ethylene rhodanate/epoxide resin microballoon suspension, through cooling, solution washing, suction filtration, drying obtain light yellow microcapsule finished product.
Embodiment 2:
A. in disposing the there-necked flask of condensing works, under the agitation condition 10g bisphenol A cyanate ester resin and 2g2-ethyl-4-methylimidazole are put into the 60g alcohol solvent, control reaction temperature is incubated 2～6 hours and obtains the cyanate prepolymer solution at 60～90 ℃;
B. in the 50 gram sodium dodecyl sulfate solutions with 10g glycidyl ether based epoxy resin (E-51) adding 3%, obtain epoxy resin latex through the stirring of homogeneous stirrer;
C. at 60～90 ℃, it is 600rpm that stir speed (S.S.) is set, epoxy resin latex in the B step is joined cyanate prepolymer solution in the A step,, react after 2～4 hours, promptly obtain ethylene rhodanate/epoxide resin microballoon suspension, through cooling, solution washing, suction filtration, drying obtains light yellow microcapsule finished product.
Embodiment 3:
A. in disposing the there-necked flask of condensing works, under the agitation condition 10g dicyclopentadiene type ethylene rhodanate resin and 2g2-ethyl-4-methylimidazole are put into the 70g alcohol solvent, control reaction temperature is incubated 2～6 hours and obtains the cyanate prepolymer solution at 60～90 ℃;
B. in the 50 gram gum arabic solutions with 10g glycidyl ether based epoxy resin (E-51) adding 3%, obtain epoxy resin latex through the stirring of homogeneous stirrer;
C. at 60～90 ℃, it is 800rpm that stir speed (S.S.) is set, epoxy resin latex in the B step is joined cyanate prepolymer solution in the A step,, react after 2～4 hours, promptly obtain ethylene rhodanate/epoxide resin microballoon suspension, through cooling, solution washing, suction filtration, drying obtains light yellow microcapsule finished product.
Claims (1)
1. the preparation method of an ethylene rhodanate/epoxide resin microballoon is characterized in that step comprises:
A. under agitation condition, be weight unit, by weight, 5～50b cyanate ester resin and 5～200b amine and derivative thereof put in the adequate amount of ethanol solvent that control reaction temperature is incubated 5～6 hours at 60～90 ℃, obtains the cyanate prepolymer solution with b;
B. 2～100b Resins, epoxy is joined in the surfactant soln, stir through the homogeneous stirrer and obtain epoxy resin latex; Described tensio-active agent is: Sudan Gum-arabic, Sodium dodecylbenzene sulfonate or sodium lauryl sulphate;
C. at 60～90 ℃, under the agitation condition, epoxy resin latex in the B step is joined in the cyanate prepolymer solution in the A step, react after 2～4 hours, promptly obtain ethylene rhodanate/epoxide resin microballoon suspension, through cooling, solution washing, suction filtration, drying obtains light yellow ethylene rhodanate/epoxide resin microballoon finished product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100313683A CN101555313B (en) | 2009-04-30 | 2009-04-30 | Ethylene rhodanate/epoxide resin microballoon and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100313683A CN101555313B (en) | 2009-04-30 | 2009-04-30 | Ethylene rhodanate/epoxide resin microballoon and preparation method thereof |
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| Publication Number | Publication Date |
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| CN101555313A CN101555313A (en) | 2009-10-14 |
| CN101555313B true CN101555313B (en) | 2011-04-20 |
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| CN2009100313683A Expired - Fee Related CN101555313B (en) | 2009-04-30 | 2009-04-30 | Ethylene rhodanate/epoxide resin microballoon and preparation method thereof |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104497486A (en) * | 2014-12-16 | 2015-04-08 | 浙江华正新材料股份有限公司 | Anti-yellowing modified halogen-free white resin composition, laminated board and preparation method of composition |
| CN107880492A (en) * | 2017-12-21 | 2018-04-06 | 河南省科学院化学研究所有限公司 | A kind of self toughening epoxide resin microballoon material |
| CN111187517B (en) * | 2020-01-07 | 2021-01-29 | 江南大学 | Preparation method of epoxidized soybean oil containing thermosetting epoxy resin microspheres |
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Address after: Suzhou City, Jiangsu province 215137 Xiangcheng District Ji Road No. 8 Patentee after: Soochow University Address before: 215123 Suzhou City, Suzhou Province Industrial Park, No. love road, No. 199 Patentee before: Soochow University |
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Granted publication date: 20110420 Termination date: 20140430 |