CN103920438B - A kind of preparation method of phenolic resins/poly styrene composite material - Google Patents
A kind of preparation method of phenolic resins/poly styrene composite material Download PDFInfo
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- CN103920438B CN103920438B CN201410169661.7A CN201410169661A CN103920438B CN 103920438 B CN103920438 B CN 103920438B CN 201410169661 A CN201410169661 A CN 201410169661A CN 103920438 B CN103920438 B CN 103920438B
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Abstract
A preparation method for phenolic resins/poly styrene composite material, it relates to a kind of preparation method of phenolic resins/poly styrene composite material.The present invention seeks to the problem that will solve existing phenolic resin microspheres size heterogeneity, there is adhesive.Method: dibenzoyl peroxide and divinylbenzene are added in styrene, from room temperature to 95 DEG C after dissolving completely, polymerisation, then add phenolic resin microspheres, stir and continue reaction, after this viscosity of system becomes large gradually, to viscosity is 20Pas, naturally cools to room temperature, spend deionized water twice, ethanol washing once, is placed in baking oven inner drying, namely obtains phenolic resins/poly styrene composite material.The present invention is mainly for the preparation of phenolic resins/poly styrene composite material.
Description
Technical field
The present invention relates to a kind of preparation method of phenolic resins/poly styrene composite material.
Background technology
Spheric active material with carbon element, due to its special geometry and porous, obtains application study in many aspects.In the past in report general all with phenolic resins, Lauxite for raw material, adopt suspension polymerisation or emulsion polymerisation to prepare phenolic resin microspheres.But these methods all processing technology is complicated, the reaction time long, have the shortcomings such as accessory substance generation.And there is size heterogeneity, there is the problem of adhesive in existing phenolic resin microspheres.
Summary of the invention
The present invention seeks to the problem that will solve existing phenolic resin microspheres size heterogeneity, there is adhesive, and a kind of preparation method of phenolic resins/poly styrene composite material is provided.
A kind of preparation method of mono-dispersion microballoon of size uniformity, specifically carry out according to following steps: one, first resorcinol is dissolved in deionized water, add ethyl orthosilicate and benzaldehyde after mixing, be stir 10min ~ 30min under the water bath condition of 50 DEG C in temperature, be uniformly mixed liquid; Two, first the liquid that is uniformly mixed in step one is transferred in polytetrafluoroethyllining lining reactor, be placed on after sealing in Muffle furnace, 160 ~ 200 DEG C are risen to from room temperature with the heating rate of 1 ~ 3 DEG C/min, and 4h ~ 8h is reacted at temperature is 160 ~ 200 DEG C, room temperature is put in cooling, obtains reacting rear solution; Three, deionized water washing 2 ~ 3 times are adopted by obtaining reacting rear solution in step 2, ethanol is adopted to wash again 2 ~ 3 times, then ultrasonic disperse is to even, centrifugation under 7000r/min ~ 10000r/min condition again, it is dry 4h ~ 8h in 60 ~ 90 DEG C of baking ovens that the solid that separation obtains is placed on temperature, namely obtains phenolic resin microspheres;
The quality of the resorcinol described in step one and the volume ratio of deionized water are (1 ~ 6) g:200mL;
The quality of the resorcinol described in step one and the volume ratio of ethyl orthosilicate are (2 ~ 21) g:14mL;
The quality of the resorcinol described in step one and the volume ratio of benzaldehyde are (2 ~ 15) g:10mL.
Advantage of the present invention: the present invention, on the basis of one kettle way, introduces phenyl ring, adds ethyl orthosilicate, makes original phenolic resin ball have more homogeneous size, dispersed better.Just because of the characteristic that these are excellent, such that its catalytic activity when making catalyst is high, long catalytic life, large availability; Stability as carrier is high.The processing technology of phenolic resin ball is in the past compared, and method of the present invention is more easy, and the product obtained is more excellent, and performance is more outstanding.
Accompanying drawing explanation
Fig. 1 is SEM (SEM) figure of phenolic resin microspheres prepared by test one;
Fig. 2 is the X-ray diffractogram (XRD) of phenolic resin microspheres prepared by test one;
Fig. 3 is Fourier transform infrared spectroscopy (FTIR) figure of phenolic resin microspheres prepared by test one.
Detailed description of the invention
Detailed description of the invention one: present embodiment is a kind of preparation method of mono-dispersion microballoon of size uniformity, specifically carry out according to following steps: one, first resorcinol is dissolved in deionized water, ethyl orthosilicate and benzaldehyde is added after mixing, be stir 10min ~ 30min under the water bath condition of 50 DEG C in temperature, be uniformly mixed liquid; Two, first the liquid that is uniformly mixed in step one is transferred in polytetrafluoroethyllining lining reactor, be placed on after sealing in Muffle furnace, 160 ~ 200 DEG C are risen to from room temperature with the heating rate of 1 ~ 3 DEG C/min, and 4 ~ 8h is reacted at temperature is 160 ~ 200 DEG C, room temperature is put in cooling, obtains reacting rear solution; Three, deionized water washing 2 ~ 3 times are adopted by obtaining reacting rear solution in step 2, ethanol is adopted to wash again 2 ~ 3 times, then ultrasonic disperse is to even, centrifugation under 7000r/min ~ 10000r/min condition again, it is dry 4h ~ 8h in 60 ~ 90 DEG C of baking ovens that the solid that separation obtains is placed on temperature, namely obtains phenolic resin microspheres.
The quality of the resorcinol described in present embodiment step one and the volume ratio of deionized water are (1 ~ 6) g:200mL.
The quality of the resorcinol described in present embodiment step one and the volume ratio of ethyl orthosilicate are (2 ~ 21) g:14mL.
The quality of the resorcinol described in present embodiment step one and the volume ratio of benzaldehyde are (2 ~ 15) g:10mL.
Ethyl orthosilicate described in present embodiment step one is the ethyl orthosilicate that distillation purifying is crossed.
The volume of polytetrafluoroethyllining lining reactor described in present embodiment step 2 and the volume ratio of Homogeneous phase mixing liquid are 4:5.
Present embodiment solves these problems, and adopts hydro-thermal method successfully to synthesize the single dispersing phenolic resin microspheres of size uniformity.Hydro-thermal method be utilize the aqueous solution of HTHP make those in atmospheric conditions insoluble or indissoluble substance dissolves, or reaction generates the lysate of this material, generation convection current is made to separate out the method for grown crystal to form hypersaturated state by the temperature difference controlling solution in autoclave.Hydro-thermal method produce have be that particle purity is high, good dispersion, good crystalline and can control, the features such as production cost is low.
Microballoon prepared by present embodiment may be used for the structure of catalysis, pharmaceutical carrier, structure complexity, nanometer casting and electrochemistry.This microballoon is high as the catalytic activity of catalyst, large availability, long catalytic life.Stability as carrier is high.But microballoon homogeneity is in the past bad, bad dispersibility, this just limits its application in medicine carrying, water treatment, catalysis etc. greatly.In order to apply carbon ball in practice better, prepare a class uniform, the microballoon of good dispersion is necessary.
Detailed description of the invention two: present embodiment and detailed description of the invention one unlike: the quality of the resorcinol described in step one and the volume ratio of deionized water are (2 ~ 4) g:200mL.Other are identical with detailed description of the invention one.
Detailed description of the invention three: one of present embodiment and detailed description of the invention one to two unlike: the quality of the resorcinol described in step one and the volume ratio of ethyl orthosilicate are (5 ~ 15) g:14mL.Other are identical with detailed description of the invention one to two.
Detailed description of the invention four: one of present embodiment and detailed description of the invention one to three unlike: the quality of the resorcinol described in step one and the volume ratio of benzaldehyde are (5 ~ 10) g:10mL.Other are identical with detailed description of the invention one to three.
Detailed description of the invention five: one of present embodiment and detailed description of the invention one to four unlike: first the liquid that is uniformly mixed in step one is transferred in polytetrafluoroethyllining lining reactor in step 2, be placed on after sealing in Muffle furnace, 170 ~ 190 DEG C are risen to from room temperature with the heating rate of 1 ~ 3 DEG C/min, and 5h ~ 7h is reacted at temperature is 170 ~ 190 DEG C, room temperature is put in cooling, obtains reacting rear solution.Other are identical with detailed description of the invention one to four.
Detailed description of the invention six: one of present embodiment and detailed description of the invention one to five unlike: adopt deionized water to wash 2 times by obtaining reacting rear solution in step 2 in step 3, ethanol is adopted to wash 2 times again, then ultrasonic disperse is to even, centrifugation under 8000r/min ~ 9000r/min condition again, it is dry 5h ~ 7h in 70 ~ 80 DEG C of baking ovens that the solid that separation obtains is placed on temperature, namely obtains phenolic resin microspheres.Other are identical with detailed description of the invention one to five.
Adopt following verification experimental verification effect of the present invention:
Test one: a kind of preparation method of mono-dispersion microballoon of size uniformity, specifically carry out according to following steps:
One, be first dissolved in 70mL deionized water by 1.2g resorcinol, add 4mL ethyl orthosilicate and 2.5mL benzaldehyde after mixing, be stir 20min under the water condition of 50 DEG C in temperature, be uniformly mixed liquid; Two, first the liquid that is uniformly mixed in step one is transferred in polytetrafluoroethyllining lining reactor, be placed on after sealing in Muffle furnace, rise to 180 DEG C with the heating rate of 2 DEG C/min from room temperature, and react 6h at temperature is 180 DEG C, room temperature is put in cooling, obtains reacting rear solution; Three, deionized water is adopted to wash 2 times by obtaining reacting rear solution in step 2, wash 2 times with ethanol again, then ultrasonic disperse is to even, then centrifugation under 9000r/min condition, it is dry 6h in 80 DEG C of baking ovens that the solid that separation obtains is placed on temperature, namely obtains phenolic resin microspheres.
Ethyl orthosilicate described in this test procedure one is the ethyl orthosilicate that distillation purifying is crossed.
The volume of polytetrafluoroethyllining lining reactor described in this test procedure two is 50mL.
In polytetrafluoroethyllining lining reactor described in this test procedure two, the volume of Homogeneous phase mixing liquid is 100mL.
Adopt the phenolic resin microspheres of this test of sem observation preparation; As shown in Figure 1, Fig. 1 is SEM (SEM) figure of phenolic resin microspheres prepared by test one; Phenolic resin microspheres size uniformity, monodispersity are good as seen in Figure 1.
X-ray diffractometer is adopted to observe the alkyd resin based carbosphere of this test preparation; As shown in Figure 2, Fig. 2 is the X-ray diffractogram (XRD) of phenolic resin microspheres prepared by test one; Can find out there is obvious characteristic diffraction peak at 25.5 ° by Fig. 2.
Test two: a kind of application of monodisperse resin microballoon of size uniformity, specifically carry out according to following steps:
First 250mgBPO (dibenzoyl peroxide) and 3.5g divinylbenzene are added in 20g styrene, from room temperature to 95 DEG C after dissolving completely, and be 95 DEG C of polymerization 2h in temperature, add the phenolic resin microspheres of 5g test one preparation again, stir and continue reaction, after this viscosity of system becomes large gradually, (namely viscosity is 20Pas) is got final product to similar to glycerine viscosity, naturally cool to room temperature, spend deionized water twice, ethanol washing once, is 80 baking oven inner dryings as temperature, namely obtains phenolic resins/poly styrene composite material.
Adopt the phenolic resins/poly styrene composite material of this test of sem observation preparation; As shown in Figure 3, Fig. 3 is SEM (SEM) figure of phenolic resins/poly styrene composite material prepared by test two, and the polystyrene/phenolic resin composite material adopting test two to prepare has excellent toughness, good electric conductivity, high temperature resistant damping and amortization are good.Phenolic resin microspheres size uniformity, the Heat stability is good prepared with the present invention, be applicable to being mixed with composite with polystyrene.
Claims (1)
1. a preparation method for phenolic resins/poly styrene composite material, is characterized in that it carries out according to following steps:
First 250mg dibenzoyl peroxide and 3.5g divinylbenzene are added in 20g styrene, from room temperature to 95 DEG C after dissolving completely, and be 95 DEG C of polymerization 2h in temperature, then add 5g phenolic resin microspheres, stir and continue reaction, after this viscosity of system becomes large gradually, to viscosity is 20Pas, naturally cools to room temperature, spend deionized water twice, once, being placed in temperature is 80 baking oven inner dryings, namely obtains phenolic resins/poly styrene composite material in ethanol washing;
Described phenolic resin microspheres is prepared according to the following steps:
One, be first dissolved in 70mL deionized water by 1.2g resorcinol, add 4mL ethyl orthosilicate and 2.5mL benzaldehyde after mixing, be stir 20min under the water condition of 50 DEG C in temperature, be uniformly mixed liquid; Two, first the liquid that is uniformly mixed in step one is transferred in polytetrafluoroethyllining lining reactor, be placed on after sealing in Muffle furnace, rise to 180 DEG C with the heating rate of 2 DEG C/min from room temperature, and react 6h at temperature is 180 DEG C, room temperature is put in cooling, obtains reacting rear solution; Three, deionized water is adopted to wash 2 times by obtaining reacting rear solution in step 2, wash 2 times with ethanol again, then ultrasonic disperse is to even, then centrifugation under 9000r/min condition, it is dry 6h in 80 DEG C of baking ovens that the solid that separation obtains is placed on temperature, namely obtains phenolic resin microspheres;
Ethyl orthosilicate described in step one is the ethyl orthosilicate that distillation purifying is crossed;
The volume of the reactor of polytetrafluoroethyllining lining described in step 2 is 50mL;
In the reactor of polytetrafluoroethyllining lining described in step 2, the volume of Homogeneous phase mixing liquid is 100mL.
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| CN101624437B (en) * | 2008-11-24 | 2011-08-10 | 鲁东大学 | Preparation method of phenolic resin polymer microspheres |
| KR101109096B1 (en) * | 2009-11-03 | 2012-02-09 | 주식회사 폴리크롬 | Manufacture method of Nano particle impregnated Phytoncide |
| CN102321228B (en) * | 2011-04-01 | 2012-11-07 | 黄石理工学院 | Method for preparing organic silicon modified thermal plastic phenolic resin |
| CN102352003B (en) * | 2011-07-19 | 2013-01-02 | 黑龙江大学 | Preparation method of phenolic resin microballoons and method for preparing phenolic resin-based carbon spheres by use of preparation method |
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