CN111234231A - Preparation method of copolymerized organic silicon resin microspheres - Google Patents
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G77/04—Polysiloxanes
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Abstract
The invention relates to the field of chemical industry, in particular to a preparation method of a copolymerized organic silicon resin microsphere; the method is characterized in that a vinyl-siloxane polymer, vinyl tri (dimethylsiloxy) silane, 1,3, 3-tetramethyldisiloxane and a platinum catalyst form microemulsion copolymerization in a high-efficiency microemulsion; the invention relates to a preparation method of a copolymerization organic silicon resin microsphere, which adopts a copolymerization method to prepare the organic silicon resin microsphere, adopts a high-efficiency microemulsion agent, can prepare raw materials into water-in-oil single-phase microemulsion under the condition of fully and uniformly mixing, provides an ideal nano particle synthesis environment for manufacturing a nano-scale micro-reactor for reaction, can accurately control the morphology of nano particles, and ensures that the synthesized organic silicon resin microsphere has very complete spherical morphology.
Description
Technical Field
The invention relates to the field of chemical industry, in particular to a preparation method of a copolymerized organic silicon resin microsphere.
Background
Compared with inorganic filler, the organic silicon resin micro powder has the characteristics of low relative density, heat resistance, weather resistance, lubricating property, and hydration property, and can be widely used as filler and modified additive of plastics, rubber, paint, cosmetics, and the like. For example, the application effects of the epoxy resin have attracted attention for improving the cracking resistance of epoxy resins and the like, increasing the lubricity and blocking resistance of plastic films, improving the performance of plastic products and cosmetics, and the like.
201811228071.1 discloses a hydrophilic organic silicon microsphere and its preparation method. The preparation method comprises the following steps: firstly, adding a silane monomer A, a silane monomer B and deionized water into a reactor, and adding an acid catalyst to perform hydrolysis reaction; then adding an alkaline catalyst to carry out polycondensation reaction, and after the reaction is finished, carrying out centrifugal separation, filtering and washing to obtain a white solid which is then dispersed in deionized water to form a dispersion liquid; stirring and heating the dispersion liquid, adding a hydrophilic monomer C containing carbon-carbon double bonds and a catalyst D at the same time, then continuing to carry out heat preservation reaction, and after the reaction is finished, centrifuging, filtering, washing and drying to obtain the hydrophilic organic silicon microspheres. The particle size of the organic silicon microsphere is controlled to be 1.0-15 mu m, the organic silicon microsphere has excellent hydrophilicity, is used for water-based resin, has simple synthesis steps and low raw material cost, uses deionized water as a solvent or a dispersion liquid in the production process, is non-toxic, environment-friendly and high in added value, and is suitable for large-scale production.
201611093734.4 provides a low resistance adsorbent based on resin microsphere, which has a larger overall dimension than microsphere, and when used in a fixed bed, the bed resistance is small, and the problem of internal diffusion is small, and the adsorption and exchange capacity and precision are not reduced basically; the adsorption or ion exchange resin microsphere is formed by bonding a plurality of adsorption or ion exchange resin microspheres with a spherical, strip, honeycomb, cylindrical or special-shaped body which has a larger overall dimension than the microsphere, wherein micropores in the resin microspheres are not blocked at most of openings on the outer surface of the microspheres, and the resin microspheres are directly communicated with the outer surface of an adsorption material and/or are communicated through pore channels among the microspheres; can be used for organic solvent recovery and removal treatment of organized and unorganized exhaust VOCs and deoiling treatment of oily water.
201610219317.3 discloses a polyester resin-based light diffusion composite material, which is prepared by mixing the following raw materials in parts by weight: 100 parts of matrix resin, 0.3-1.5 parts of light diffusant, 0.1-0.6 part of antioxidant and 0.1-0.5 part of release agent; the matrix resin is formed by combining 30-90% of polycarbonate and 10-70% of polyester terephthalate by weight percentage, wherein the polyester terephthalate is selected from one or more of PET, APET and PETG. The invention comprehensively utilizes the advantages of a plurality of resins, makes up for the deficiencies of each other, and overcomes the defects of poor notch sensitivity, poor organic chemical resistance and the like of the traditional PC resin for the LED; the cost of the light diffusion material for the LED is greatly reduced, and the LED lighting system has positive promotion effect on the convenience brought by the modern science and technology when the LED lighting system enters the ordinary family for a long time.
The organic silicon resin microspheres provided by the above technology and the existing patent have the defect of incomplete spherical structure, influence on the light diffusion effect and limit the application of the organic silicon resin microspheres in the field of light diffusers.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of copolymerized organic silicon resin microspheres. Prepared by hydrosilylation reaction:
a preparation method of copolymerized organic silicon resin microspheres comprises the following operation steps:
adding 40-68 parts of vinyl tri (dimethylsiloxane) silane into a reactor according to the mass parts, stirring and mixing uniformly, adding 8-19 parts of 1,1,3, 3-tetramethyldisiloxane, heating to 40-60 ℃, stirring and mixing for 60-90min, then adding 400-700 parts of purified water, 0.1-0.5 part of potassium trichlorovinyl platinum (II), 0.5-3 parts of high-efficiency microemulsion, 0.5-2.3 parts of 1, 4-dibromoacetoxyl-2-butene and 0.03-0.6 part of zinc undecylenate, stirring and mixing at a high speed for 20-30min, then ultrasonically dispersing for 10-30min to form a microemulsion, heating to 40-60 ℃, reacting for 120min, adding 30-70 parts of ammonia water after the reaction is completed, heating to 65-85 ℃, continuously reacting for 30-60 min; after the reaction is finished, centrifugal sedimentation, filtration and drying are carried out, and the copolymerized organic silicon resin microsphere can be obtained.
The high-efficiency microemulsion is prepared by the following steps:
according to the mass portion, 10-24 portions of nonenyl succinic anhydride and 8-16 portions of fatty alcohol-polyoxyethylene ether are stirred and mixed evenly, the temperature is controlled at 40-60 ℃, and the temperature is controlled at 200-2Under the irradiation of ultraviolet light, the reaction lasts for 30-120 min; then adding 3-8 parts of polyoxyethylene sorbitan monostearate, 1-5 parts of sorbitan oleate, 0.5-1.8 parts of spiro quaternary ammonium tetrafluoroborate, 0.1-0.9 part of terpene styrene, 2-7 parts of sodium carbonate and 0.8-2.6 parts of ammonium persulfate into a reactor, stirring and mixing uniformly, controlling the temperature to be 180-260 ℃ under the protection of nitrogen, and reacting for 40-120 min; after the reaction is finished, the temperature is reduced to 50-80 ℃, 0.6-1.4 parts of cross-linking agent is added, and the high-efficiency micro-emulsifier can be obtained after stirring for 30-60 min.
The reaction mechanism of the copolymerized organic silicon resin microspheres is as follows:
under the action of potassium trichlorovinyl platinum (II), vinyltris (dimethylsiloxy) silane and 1,1,3, 3-tetramethyldisiloxane respectively undergo hydrosilylation with 1, 4-dibromoacetoxyl-2-butene and zinc undecylenate, and then are hydrolyzed to generate the copolymerized organic silicon resin microspheres.
Vinyltris (dimethylsiloxy) silane, 1, 4-dibromoacetoxy-2-butene and zinc undecylenate are subjected to hydrosilylation reaction respectively to generate an intermediate product with the following structure, and the structural formula is shown as follows:
the cross-linking agent is ethylenediamine, triethylenetetramine, 1,4,7,10, 10-hexamethyltriethylenetetramine or diethylaminopropylamine.
The ultrasonic dispersion adopts the frequency of 20KHz and the power of 2000-4200W.
The homopolymerized organic silicon resin microsphere is used as an excellent light diffusant
The invention relates to a preparation method of a copolymerization organic silicon resin microsphere, which adopts a hydrosilylation copolymerization method to prepare the organic silicon resin microsphere, adopts a high-efficiency microemulsion, has a spiral ring structure with high temperature resistance, can prepare raw materials into water-in-oil single-phase microemulsion under the condition of full uniform mixing, provides an ideal nano particle synthesis environment for manufacturing a nano-scale micro reactor by reaction, can accurately control the morphology of nano particles, and ensures that the synthesized organic silicon resin microsphere has complete spherical morphology.
1, 4-dibromo acetoxyl-2-butylene and zinc undecylenate react with a copolymer of vinyl tri (dimethylsiloxy) silane through hydrosilylation, bromo acetoxyl and a zinc salt group are brought into the copolymerized organic silicon resin microsphere, so that the effect of inhibiting photodegradation is achieved, and the aging resistance and yellowing resistance of the organic silicon resin microsphere are further improved.
Drawings
FIG. 1 is a Fourier infrared spectrum of a sample of copolymerized silicone resin microspheres prepared in example 2.
Detailed Description
The invention is further illustrated by the following specific examples:
placing the polyorganosiloxane resin microspheres for 120 days at 50 ℃ under the LED illumination, and then detecting.
Measuring the average particle size and the particle size polydispersity index of the product by using a Coulter LS230 type laser particle sizer, wherein the smaller the particle size polydispersity index value is, the narrower the particle size distribution of the particles is; and observing the spherical structure of the product by adopting a scanning electron microscope.
Whether yellowing occurred was visually observed.
Example 1
A preparation method of copolymerized organic silicon resin microspheres comprises the following operation steps:
adding 40g of vinyl tri (dimethylsiloxane) silane into a reactor, stirring and mixing uniformly, adding 8g of 1,1,3, 3-tetramethyldisiloxane, heating to 40 ℃, stirring and mixing for 60min, adding 400g of purified water, 0.1g of potassium trichlorovinyl platinum (II) and 0.5g of efficient microemulsion, 0.5g of 1, 4-dibromoacetoxy-2-butene and 0.03g of zinc undecylenate, stirring and mixing at a high speed for 20min, performing ultrasonic dispersion for 10min to form microemulsion, heating to 40 ℃, reacting for 120min, adding 30g of ammonia water after the reaction is finished, heating to 65 ℃, and continuing to react for 30 min; after the reaction is finished, centrifugal sedimentation, filtration and drying are carried out, and the copolymerized organic silicon resin microsphere can be obtained.
The high-efficiency microemulsion is prepared by the following steps:
stirring and mixing 10g of nonenyl succinic anhydride and 8g of fatty alcohol-polyoxyethylene ether uniformly, controlling the temperature at 40 ℃ and controlling the temperature at 200 mu W/cm2Under the irradiation of ultraviolet light, the reaction lasts for 30 min; then adding 3g of polyoxyethylene sorbitan monostearate, 1g of sorbitan oleate, 0.5g of spiro quaternary ammonium tetrafluoroborate, 0.1g of terpene styrene, 2g of sodium carbonate and 0.8g of ammonium persulfate into a reactor, stirring and mixing uniformly, and then controlling the temperature to be 180 ℃ under the protection of nitrogen to react for 40 min; after the reaction is finished, the temperature is reduced to 50 ℃, 0.6g of cross-linking agent is added, and the mixture is stirred for 30min, so that the high-efficiency microemulsion can be obtained.
The cross-linking agent is ethylenediamine.
The ultrasonic dispersion adopts the frequency of 20KHz and the power of 2000W.
The homopolymerization organic silicon resin microsphere is used as an excellent light diffusant.
The average particle size of the organic silicon resin microspheres prepared in the experiment is 650nm, and the particle size polydispersity index is 1.817; SEM shows that the spherical structure of the product is complete and has no yellowing phenomenon by visual inspection.
Example 2
A preparation method of copolymerized organic silicon resin microspheres comprises the following operation steps:
adding 45g of vinyl tri (dimethylsiloxane) silane into a reactor, stirring and mixing uniformly, adding 11g of 1,1,3, 3-tetramethyldisiloxane, heating to 50 ℃, stirring and mixing for 67min, adding 455g of purified water, 0.2g of potassium trichlorovinyl platinum (II) and 1g of efficient microemulsion, 1g of 1, 4-dibromoacetoxy-2-butene and 0.09g of zinc undecylenate, stirring and mixing at a high speed for 25min, performing ultrasonic dispersion for 18min to form microemulsion, heating to 50 ℃, reacting for 180min, adding 50g of ammonia water after the reaction is finished, heating to 69 ℃, and continuing to react for 40 min; after the reaction is finished, centrifugal sedimentation, filtration and drying are carried out, and the copolymerized organic silicon resin microsphere can be obtained.
The high-efficiency microemulsion is prepared by the following steps:
stirring and mixing 18g of nonenyl succinic anhydride and 12g of fatty alcohol-polyoxyethylene ether uniformly, controlling the temperature to be between 40 and 60 ℃, and controlling the temperature to be between 200 ℃ and 300 mu W/cm2Under the irradiation of ultraviolet light, the reaction lasts for 80 min; then adding 5g of polyoxyethylene sorbitan monostearate, 3g of sorbitan oleate, 1.4g of spiro quaternary ammonium tetrafluoroborate, 0.5g of terpene styrene, 5g of sodium carbonate and 1.4g of ammonium persulfate into a reactor, stirring and mixing uniformly, and then controlling the temperature to be 220 ℃ under the protection of nitrogen and reacting for 80 min; after the reaction is finished, the temperature is reduced to 60 ℃, 1.2g of cross-linking agent is added, and the mixture is stirred for 30-60min, so that the high-efficiency microemulsion can be obtained.
The cross-linking agent is triethylene tetramine.
The ultrasonic dispersion adopts the frequency of 20KHz and the power of 3200W.
The homopolymerization organic silicon resin microsphere is used as an excellent light diffusant.
The average grain diameter of the organic silicon resin microspheres prepared in the experiment is 620nm, and the grain diameter polydispersity index is 1.641; SEM shows that the spherical structure of the product is complete and has no yellowing phenomenon by visual inspection.
As can be seen from fig. 1: at 1050/867cm-1The absorption peak of silicon oxygen exists nearby, and is 2968cm-1The antisymmetric stretching vibration absorption peak of the hydrocarbon exists nearby, which shows that the vinyltris (dimethylsiloxy) silane participates in the reaction; at 1412/1264cm-1An absorption peak of silicon carbon exists nearby, which indicates that 1,1,3, 3-tetramethyl disiloxane participates in the reaction; at 1800cm-1An absorption peak of carbonyl of an ester group exists nearby, which indicates that 1, 4-dibromoacetoxyl-2-butene participates in the reaction; at 1601cm-1An antisymmetric telescopic vibration absorption peak of carboxylate ions exists nearby, and the zinc undecylenate participates in the reaction.
Example 3
A preparation method of copolymerized organic silicon resin microspheres comprises the following operation steps:
adding 68g of vinyl tri (dimethylsiloxane) silane into a reactor, stirring and mixing uniformly, adding 19g of 1,1,3, 3-tetramethyldisiloxane, heating to 60 ℃, stirring and mixing for 90min, adding 700g of purified water, 0.5g of potassium trichlorovinyl platinum (II) and 3g of efficient microemulsion, 2.3g of 1, 4-dibromoacetoxy-2-butene and 0.6g of zinc undecylenate, stirring and mixing at a high speed for 30min, ultrasonically dispersing for 30min to form microemulsion, heating to 60 ℃, reacting for 240min, adding 70g of ammonia water after the reaction is finished, heating to 85 ℃, and continuing to react for 60 min; after the reaction is finished, centrifugal sedimentation, filtration and drying are carried out, and the copolymerized organic silicon resin microsphere can be obtained.
The high-efficiency microemulsion is prepared by the following steps:
stirring and mixing 24g of nonenyl succinic anhydride and 16g of fatty alcohol-polyoxyethylene ether uniformly, controlling the temperature at 60 ℃ and controlling the temperature at 300 mu W/cm2Under the irradiation of ultraviolet light, the reaction lasts for 120 min; then adding 8g of polyoxyethylene sorbitan monostearate, 5g of sorbitan oleate, 1.8g of spiro quaternary ammonium tetrafluoroborate, 0.9g of terpene styrene, 7g of sodium carbonate and 2.6g of ammonium persulfate into a reactor, stirring and mixing uniformly, and then controlling the temperature to be 260 ℃ under the protection of nitrogen to react for 120 min; after the reaction is finished, the temperature is reduced to 80 ℃, 1.4g of cross-linking agent is added, and the mixture is stirred for 60min, so that the high-efficiency microemulsion can be obtained.
The cross-linking agent is 1,1,4,7,10, 10-hexamethyltriethylenetetramine.
The ultrasonic dispersion adopts the frequency of 20KHz and the power of 4200W.
The homopolymerization organic silicon resin microsphere is used as an excellent light diffusant.
The average grain diameter of the organic silicon resin microspheres prepared by the experiment is 610nm, and the grain diameter polydispersity index is 1.588; SEM shows that the spherical structure of the product is complete and has no yellowing phenomenon by visual inspection.
Comparative example 1
A preparation method of copolymerized organic silicon resin microspheres comprises the following operation steps:
adding 45g of vinyl tri (dimethylsiloxane) silane into a reactor, stirring and mixing uniformly, adding 11g of 1,1,3, 3-tetramethyldisiloxane, heating to 50 ℃, stirring and mixing for 67min, then adding 455g of purified water, 0.2g of potassium trichlorovinyl platinum (II) and 1g of efficient microemulsion and 0.09g of zinc undecylenate, stirring and mixing at a high speed for 25min, then carrying out ultrasonic dispersion for 18min to form a microemulsion, heating to 50 ℃, reacting for 180min, adding 50g of ammonia water after the reaction is finished, heating to 69 ℃, and continuing to react for 40 min; after the reaction is finished, centrifugal sedimentation, filtration and drying are carried out, and the copolymerized organic silicon resin microsphere can be obtained.
The high-efficiency microemulsion is prepared by the following steps:
stirring and mixing 18g of nonenyl succinic anhydride and 12g of fatty alcohol-polyoxyethylene ether uniformly, controlling the temperature to be between 40 and 60 ℃, and controlling the temperature to be between 200 ℃ and 300 mu W/cm2Under the irradiation of ultraviolet light, the reaction lasts for 80 min; then adding 5g of polyoxyethylene sorbitan monostearate, 3g of sorbitan oleate, 1.4g of spiro quaternary ammonium tetrafluoroborate, 0.5g of terpene styrene, 5g of sodium carbonate and 1.4g of ammonium persulfate into a reactor, stirring and mixing uniformly, and then controlling the temperature to be 220 ℃ under the protection of nitrogen and reacting for 80 min; after the reaction is finished, the temperature is reduced to 60 ℃, 1.2g of cross-linking agent is added, and the mixture is stirred for 30-60min, so that the high-efficiency microemulsion can be obtained.
The cross-linking agent is triethylene tetramine.
The ultrasonic dispersion adopts the frequency of 20KHz and the power of 3200W.
The homopolymerization organic silicon resin microsphere is used as an excellent light diffusant.
The average grain diameter of the organic silicon resin microspheres prepared by the experiment is 690nm, and the grain diameter polydispersity index is 1.86; SEM shows that the spherical structure of the product has no defect and has yellowing phenomenon by visual inspection.
Comparative example 2
A preparation method of copolymerized organic silicon resin microspheres comprises the following operation steps:
adding 45g of vinyl tri (dimethylsiloxane) silane into a reactor, stirring and mixing uniformly, adding 11g of 1,1,3, 3-tetramethyldisiloxane, heating to 50 ℃, stirring and mixing for 67min, then adding 455g of purified water, 0.2g of potassium trichlorovinyl platinum (II) and 1g of efficient microemulsion, stirring and mixing 1g of 1, 4-dibromoacetoxy-2-butene at a high speed for 25min, performing ultrasonic dispersion for 18min to form microemulsion, heating to 50 ℃, reacting for 180min, adding 50g of ammonia water after the reaction is finished, heating to 69 ℃, and continuing to react for 40 min; after the reaction is finished, centrifugal sedimentation, filtration and drying are carried out, and the copolymerized organic silicon resin microsphere can be obtained.
The high-efficiency microemulsion is prepared by the following steps:
stirring and mixing 18g of nonenyl succinic anhydride and 12g of fatty alcohol-polyoxyethylene ether uniformly, controlling the temperature to be between 40 and 60 ℃, and controlling the temperature to be between 200 ℃ and 300 mu W/cm2Under the irradiation of ultraviolet light, the reaction lasts for 80 min; then adding 5g of polyoxyethylene sorbitan monostearate, 3g of sorbitan oleate, 1.4g of spiro quaternary ammonium tetrafluoroborate, 0.5g of terpene styrene, 5g of sodium carbonate and 1.4g of ammonium persulfate into a reactor, stirring and mixing uniformly, and then controlling the temperature to be 220 ℃ under the protection of nitrogen and reacting for 80 min; after the reaction is finished, the temperature is reduced to 60 ℃, 1.2g of cross-linking agent is added, and the mixture is stirred for 30-60min, so that the high-efficiency microemulsion can be obtained.
The cross-linking agent is triethylene tetramine.
The ultrasonic dispersion adopts the frequency of 20KHz and the power of 3200W.
The homopolymerization organic silicon resin microsphere is used as an excellent light diffusant.
The average grain diameter of the organic silicon resin microspheres prepared by the experiment is 720nm, and the grain diameter polydispersity index is 1.96; SEM shows that the spherical structure of the product has no defect and has yellowing phenomenon by visual inspection.
Comparative example 3
A preparation method of copolymerized organic silicon resin microspheres comprises the following operation steps:
adding 45g of vinyl tri (dimethylsiloxane) silane into a reactor, stirring and mixing uniformly, adding 11g of 1,1,3, 3-tetramethyldisiloxane, heating to 50 ℃, stirring and mixing for 67min, adding 455g of purified water, 0.2g of potassium trichlorovinyl platinum (II) and 1g of efficient microemulsion, 1g of 1, 4-dibromoacetoxy-2-butene and 0.09g of zinc undecylenate, stirring and mixing at a high speed for 25min, performing ultrasonic dispersion for 18min to form microemulsion, heating to 50 ℃, reacting for 180min, adding 50g of ammonia water after the reaction is finished, heating to 69 ℃, and continuing to react for 40 min; after the reaction is finished, centrifugal sedimentation, filtration and drying are carried out, and the copolymerized organic silicon resin microsphere can be obtained.
The high-efficiency microemulsion is prepared by the following steps:
stirring and mixing 18g of nonenyl succinic anhydride and 12g of fatty alcohol-polyoxyethylene ether uniformly, controlling the temperature to be between 40 and 60 ℃, and controlling the temperature to be between 200 ℃ and 300 mu W/cm2Under the irradiation of ultraviolet light, the reaction lasts for 80 min; then adding 5g of polyoxyethylene sorbitan monostearate, 3g of sorbitan oleate, 0.5g of terpene styrene, 5g of sodium carbonate and 1.4g of ammonium persulfate into a reactor, stirring and mixing uniformly, and then controlling the temperature to be 220 ℃ under the protection of nitrogen to react for 80 min; after the reaction is finished, the temperature is reduced to 60 ℃, 1.2g of cross-linking agent is added, and the mixture is stirred for 30-60min, so that the high-efficiency microemulsion can be obtained.
The cross-linking agent is triethylene tetramine.
The ultrasonic dispersion adopts the frequency of 20KHz and the power of 3200W.
The homopolymerization organic silicon resin microsphere is used as an excellent light diffusant.
The average particle size of the organic silicon resin microspheres prepared in the experiment is 740nm, and the polydispersity index of the particle size is 2.647; the spherical structure of the product has individual defects, and the visual inspection does not have the yellowing phenomenon.
Reference 4
A preparation method of copolymerized organic silicon resin microspheres comprises the following operation steps:
adding 45g of vinyl tri (dimethylsiloxane) silane into a reactor, stirring and mixing uniformly, adding 11g of 1,1,3, 3-tetramethyldisiloxane, heating to 50 ℃, stirring and mixing for 67min, adding 455g of purified water, 0.2g of potassium trichlorovinyl platinum (II), 1g of OP-10, 1g of 1, 4-dibromoacetoxy-2-butene and 0.09g of zinc undecylenate, stirring and mixing at a high speed for 25min, performing ultrasonic dispersion for 18min to form a microemulsion, heating to 50 ℃, reacting for 180min, adding 50g of ammonia water after the reaction is finished, heating to 69 ℃, and continuing to react for 40 min; after the reaction is finished, centrifugal sedimentation, filtration and drying are carried out, and the copolymerized organic silicon resin microsphere can be obtained.
The cross-linking agent is triethylene tetramine.
The ultrasonic dispersion adopts the frequency of 20KHz and the power of 3200W.
The homopolymerization organic silicon resin microsphere is used as an excellent light diffusant.
The average grain diameter of the organic silicon resin microspheres prepared in the experiment is 810nm, and the grain diameter polydispersity index is 3.712; SEM shows that the spherical structure of the product has more defects. No yellowing phenomenon is observed visually.
Claims (5)
1. A preparation method of copolymerized organic silicon resin microspheres comprises the following operation steps:
adding 40-68 parts of vinyl tri (dimethylsiloxane) silane into a reactor according to the mass parts, stirring and mixing uniformly, adding 8-19 parts of 1,1,3, 3-tetramethyldisiloxane, heating to 40-60 ℃, stirring and mixing for 60-90min, then adding 400-700 parts of purified water, 0.1-0.5 part of potassium trichlorovinyl platinum (II), 0.5-3 parts of high-efficiency microemulsion, 0.5-2.3 parts of 1, 4-dibromoacetoxyl-2-butene and 0.03-0.6 part of zinc undecylenate, stirring and mixing at a high speed for 20-30min, then ultrasonically dispersing for 10-30min to form a microemulsion, heating to 40-60 ℃, reacting for 120min, adding 30-70 parts of ammonia water after the reaction is completed, heating to 65-85 ℃, continuously reacting for 30-60 min; after the reaction is finished, centrifugal sedimentation, filtration and drying are carried out, and the copolymerized organic silicon resin microsphere can be obtained.
2. The preparation method of the copolymerized silicone resin microsphere according to claim 1, wherein: the high-efficiency microemulsion is prepared by the following steps:
according to the mass portion, 10-24 portions of nonenyl succinic anhydride and 8-16 portions of fatty alcohol polyStirring and mixing the ethylene oxide with the uniform mixing, controlling the temperature at 40-60 ℃, and controlling the temperature at 200-2Under the irradiation of ultraviolet light, the reaction lasts for 30-120 min; then adding 3-8 parts of polyoxyethylene sorbitan monostearate, 1-5 parts of sorbitan oleate, 0.5-1.8 parts of spiro quaternary ammonium tetrafluoroborate, 0.1-0.9 part of terpene styrene, 2-7 parts of sodium carbonate and 0.8-2.6 parts of ammonium persulfate into a reactor, stirring and mixing uniformly, controlling the temperature to be 180-260 ℃ under the protection of nitrogen, and reacting for 40-120 min; after the reaction is finished, the temperature is reduced to 50-80 ℃, 0.6-1.4 parts of cross-linking agent is added, and the high-efficiency micro-emulsifier can be obtained after stirring for 30-60 min.
3. The preparation method of the copolymerized silicone resin microsphere according to claim 2, wherein: the cross-linking agent is ethylenediamine, triethylenetetramine, 1,4,7,10, 10-hexamethyltriethylenetetramine or diethylaminopropylamine.
4. The preparation method of the copolymerized silicone resin microsphere according to claim 1, wherein: the ultrasonic dispersion adopts the frequency of 20KHz and the power of 2000-4200W.
5. The preparation method of the copolymerized silicone resin microsphere according to claim 1, wherein: the homopolymerization organic silicon resin microsphere is used as a light diffusant.
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