CN103524646B - The preparation method of a kind of high refractive index polystyrene and a kind of high refractive index silica gel - Google Patents
The preparation method of a kind of high refractive index polystyrene and a kind of high refractive index silica gel Download PDFInfo
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- CN103524646B CN103524646B CN201310541929.0A CN201310541929A CN103524646B CN 103524646 B CN103524646 B CN 103524646B CN 201310541929 A CN201310541929 A CN 201310541929A CN 103524646 B CN103524646 B CN 103524646B
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Abstract
The present invention relates to the preparation method of a kind of polystyrene, also relate to the method for the silica gel preparing high refractive index with this polystyrene as weighting material. The present invention has synthesized the polystyrene of a kind of high refractive index, and in this, as weighting material, with the vinyl silicone oil of common low-refraction as carrier, prepare the high refractive index silica gel that specific refractory power is greater than 1.54, can be used for the embedding of LED, it is the preparation method of a kind of cheap high refractive index silica gel.
Description
Technical field
The present invention relates to the preparation method of a kind of polystyrene, also relate to the method for the silica gel preparing high refractive index with this polystyrene as weighting material.
Background technology
At present, LED embedding generally adopts the silica gel that specific refractory power is greater than 1.40, in order to improve light extraction efficiency, it is more preferable to scheme be take the silica gel of high refractive index, numerous producer and university concentrate one's energy the silica gel developing high refractive index. As CN101974157A discloses the synthetic method of a kind of phenyl hydrogen-containing silicon oil, it is taking Diphenylsilanediol and methyl hydrogen dichlorosilane as raw material, connect under acid agent effect de-except hydrogenchloride, then balanced reaction under strongly acidic conditions, obtains finally by decolouring, filtration, desolventizing and low-boiling-point substance. It is an advantage of the invention that raw material is easy to get, reaction conditions is gentle, simple for process. The phenyl hydrogen-containing silicon oil adopting the inventive method obtained, its viscosity is 200��500mm2/ s, specific refractory power is 1.50��1.53. the silicon-ketone composition of addition-curable described in CN101891959A comprises A: the diorganopolysiloxanecompositions with the structure represented by formula (1): (wherein R1 represents unsaturated group of aliphatic series to nSi (R2) 2 (R1) to (R1) (R2) 2SiO ((Ar) 2SiO), R2 represents identical or different, that do not replace or replace univalence hydrocarbyl, Ar represent can comprise or can not comprise heteroatomic identical or different, that do not replace or replace aryl, and n represents the integer of 1 or bigger), B: every molecule comprises at least two hydrogen atoms with silicon atom bonding and do not comprise the silicoorganic compound of unsaturated group of aliphatic series, present in an amount at least sufficient under the existence of following hydrosilylation catalysts, solidify described composition, and C: based on the hydrosilylation catalysts of platinum metals. this solidifying product has heigh clarity, high refractive index (being greater than 1.54) and favourable intensive property. the high refractive index organopolysiloxane composition that CN1694925 provides comprises: (A) each molecule has the straight chain organopolysiloxane of at least two alkenyls being bonded with silicon and at least one aryl being bonded with silicon, (B) there is the side chain organopolysiloxane of the siloxane unit that following general formula represents: RSiO3/2, wherein R is substituted or unsubstituted univalence hydrocarbyl, wherein component (B) each molecule has at least one alkenyl being bonded with silicon and at least one aryl being bonded with silicon, (C) each molecule has the organopolysiloxane of the hydrogen atom that at least two are bonded with silicon, and (D) hydrosilylation catalysts. in CN102643627A 1) polysiloxane A, at least containing the polysiloxane of an alkylene being connected with silicon and aromatic base in every molecule, structural formula is as follows:
(R1R22SiO1/2) a (R12SiO2/2) b (R1R2SiO2/2) c (R3SiO2/2) d (R3SiO3/2) e wherein R1 be alkyl, R2 is alkylene, R3 is aromatic base, described a+b+c+d+e=100, a=1 ~ 20, b=10 ~ 20, c=10 ~ 20, d=0 ~ 10, e=30 ~ 60; 2) polysiloxane B, at least containing the oxygen base silane of two hydrogen atoms being connected with silicon and aromatic base in every molecule, structural formula is as follows:
(R1R4SiO1/2) o (R12SiO2/2) p (R1R4SiO2/2) q (R3SiO2/2) r (R3SiO3/2) s wherein R1 be alkyl, R3 is aromatic base, R4 is H atom or alkyl, described o+p+q+r+s=100, o=1 ~ 20, p=10 ~ 20, q=0 ~ 20, r=0 ~ 10, s=30 ~ 60.
Going up incomplete statistics according to this, Si?H addition reaction mechanism generally taked by high refractive index silica gel, and by the platinum of complexing as catalyzer, main component is vinyl-terminated silicone oil and end hydrogen silicone oil, and must containing a large amount of aromatic groups such as phenyl or naphthyl on main chain. Silicon monomer containing phenyl or naphthyl not easily obtains, and requires very high to purity, so price is very expensive, finding a kind of cheap high refractive index silica gel is a kind of meaningful exploration.
Summary of the invention
First technical problem to be solved by this invention is to provide the preparation method of a kind of polystyrene, and the method can prepare the polystyrene that specific refractory power reaches 1.59.
2nd technical problem to be solved by this invention is to provide a kind of method preparing high refractive index silica gel with this polystyrene as weighting material.
Technical problem to be solved by this invention is achieved by the following technical programs:
The preparation method of a kind of high refractive index polystyrene is, by the styrene monomer of 1-10g, 1-10g polyvinylpyrrolidone is dissolved in 5-10g water and 50-500g ethanol or methyl alcohol or propyl alcohol, then the Diisopropyl azodicarboxylate of the 0.1-0.5% accounting for styrene monomer weight is added, it is warmed up to 72 ~ 78 DEG C, high-speed stirring, reacts 3-5 hour, obtaining the polymerized emulsion of vinylbenzene, it is the granules of polystyrene of 1.59 that this emulsion high speed centrifugation under 15000rpm makes polystyrene depart from system acquisition specific refractory power.
The preparation method of a kind of high refractive index silica gel is:
(1) the granules of polystyrene 30-80 DEG C of drying under vacuum above-mentioned preparation method prepared, obtains Polystyrene powder;
(2) by Polystyrene powder ultrasonic disperse to, in ethanol or methyl alcohol or propanol solution, then adding in vinyl silicone oil while stirring and go, revolve after mixing to steam and dry ethanol or methyl alcohol or propyl alcohol are extracted out from system, obtain the silicone oil of polystyrene good distribution;
The add-on of polystyrene accounts for the 40-80% of vinyl silicone oil weight;
(3) silicone oil of polystyrene good distribution is added linking agent and catalyzer solidification, obtained high refractive index silica gel.
Further, described vinyl silicone oil is the vinyl silicone oil of a kind of general formula having in following two kinds of general formulas:
(1) ViR2SiO(SiR2O)nSiR2Vi;
(2) (Vi)3SiO[Si(R)(Vi)O]m[Si(R)2O]nSi(Vi)3;
Described R is methyl or ethyl or propyl group.
Further, linking agent described in step 3 is general formula is Me3SiO(MeHSiO)nSiMe3Linking agent, add-on is the amount making Si-H/Vi=1.02.
Further, described catalyzer is platinum catalyst, and add-on is 2-100ppm.
Further, condition of cure is 150 DEG C of 2h that are heating and curing.
The present invention has following useful effect:
The present invention has synthesized the polystyrene that a kind of specific refractory power reaches the high refractive index of 1.59, and in this, as weighting material, with the vinyl silicone oil of common low-refraction as carrier, prepare the high refractive index silica gel that specific refractory power is greater than 1.54, can be used for the embedding of LED, it is the preparation method of a kind of cheap high refractive index silica gel.
Embodiment
Below in conjunction with embodiment, the present invention will be described in detail, and embodiment is only the preferred embodiment of the present invention, is not limitation of the invention.
Embodiment 1
By the styrene monomer of 5g, 2g polyvinylpyrrolidone (PVP) is dissolved in 10g water and 100g ethanol, then the Diisopropyl azodicarboxylate (AIBN) of 0.01g is added, it is warmed up to 75 DEG C, high-speed stirring, reacting 5 hours, obtain the polymerized emulsion of vinylbenzene, it is the granules of polystyrene of 1.59 that this emulsion high speed centrifugation under 15000rpm makes polystyrene depart from system acquisition specific refractory power.
Above-mentioned granules of polystyrene is 60 DEG C of dryings under vacuum, obtain Polystyrene powder, then by its ultrasonic disperse to, in ethanolic soln, then adding vinyl silicone oil ViMe while stirring2SiO(SiR2O)20SiMe2Going in Vi (R is methyl), revolve steaming drying and extracted out from system by ethanol, obtain the vinyl silicone oil mixture of polystyrene good distribution after mixing, the add-on of polystyrene accounts for the 50% of silicone oil weight. Then with this mixture and linking agent Me3SiO(MeHSiO)50SiMe3Mixing by vacuum stirring deaeration all-in-one (model MT-300) of Shenzhen Mai Lixi Science and Technology Ltd., make Si-H/Vi=1.02, add the platinum catalyst of 5ppm simultaneously, 150 DEG C of 2h that are heating and curing, testing its specific refractory power after solidification is 1.57.
Embodiment 2
By the styrene monomer of 10g, 2g polyvinylpyrrolidone (PVP) is dissolved in 5g water and 200g ethanol, then the Diisopropyl azodicarboxylate (AIBN) of 0.05g is added, it is warmed up to 75 DEG C, high-speed stirring, reacting 4 hours, obtain the polymerized emulsion of vinylbenzene, it is the granules of polystyrene of 1.59 that this emulsion high speed centrifugation under 15000rpm makes polystyrene depart from system acquisition specific refractory power.
Above-mentioned granules of polystyrene is 60 DEG C of dryings under vacuum, obtain Polystyrene powder, then by its ultrasonic disperse to, in ethanolic soln, then adding vinyl silicone oil ViMe while stirring2SiO(SiR2O)20SiMe2Going in Vi (R is methyl), revolve steaming drying and extracted out from system by ethanol, obtain the vinyl silicone oil mixture of polystyrene good distribution after mixing, the add-on of polystyrene accounts for the 80% of silicone oil weight. Then with this mixture and linking agent Me3SiO(MeHSiO)50SiMe3Mixing by vacuum stirring deaeration all-in-one (model MT-300) of Shenzhen Mai Lixi Science and Technology Ltd., make Si-H/Vi=1.04, add the platinum catalyst of 6ppm simultaneously, 150 DEG C of 2h that are heating and curing, testing its specific refractory power after solidification is 1.58.
Embodiment 3
By the styrene monomer of 1g, 10g polyvinylpyrrolidone (PVP) is dissolved in 10g water and 500g ethanol, then the Diisopropyl azodicarboxylate (AIBN) of 0.005g is added, it is warmed up to 75 DEG C, high-speed stirring, reacting 3 hours, obtain the polymerized emulsion of vinylbenzene, it is the granules of polystyrene of 1.59 that this emulsion high speed centrifugation under 15000rpm makes polystyrene depart from system acquisition specific refractory power.
Above-mentioned granules of polystyrene is 60 DEG C of dryings under vacuum, obtain Polystyrene powder, then by its ultrasonic disperse to, in ethanolic soln, then adding vinyl silicone oil ViMe while stirring2SiO(SiR2O)20SiMe2Going in Vi (R is methyl), revolve steaming drying and extracted out from system by ethanol, obtain the vinyl silicone oil mixture of polystyrene good distribution after mixing, the add-on of polystyrene accounts for the 40% of silicone oil weight. Then with this mixture and linking agent Me3SiO(MeHSiO)50SiMe3Mixing by vacuum stirring deaeration all-in-one (model MT-300) of Shenzhen Mai Lixi Science and Technology Ltd., make Si-H/Vi=1.04, add simultaneously, the platinum catalyst of 4ppm, 150 DEG C of 2h that are heating and curing, testing its specific refractory power after solidification is 1.56.
Claims (5)
1. the preparation method of a high refractive index silica gel, it is characterised in that:
(1) by granules of polystyrene 30-80 DEG C of drying under vacuum, Polystyrene powder is obtained; The preparation method of described granules of polystyrene is: by the styrene monomer of 1-10g, 1-10g polyvinylpyrrolidone is dissolved in 5-10g water and 50-500g ethanol or methyl alcohol or propyl alcohol, then the Diisopropyl azodicarboxylate of the 0.1-0.5% accounting for styrene monomer weight is added, it is warmed up to 72 ~ 78 DEG C, high-speed stirring, reacting 3-5 hour, obtain the polymerized emulsion of vinylbenzene, it is the granules of polystyrene of 1.59 that this emulsion high speed centrifugation under 15000rpm makes polystyrene depart from system acquisition specific refractory power;
(2) by Polystyrene powder ultrasonic disperse to, in ethanol or methyl alcohol or propanol solution, then adding in vinyl silicone oil while stirring and go, revolve after mixing to steam and dry ethanol or methyl alcohol or propyl alcohol are extracted out from system, obtain the silicone oil of polystyrene good distribution;
The add-on of polystyrene accounts for the 40-80% of vinyl silicone oil weight;
(3) silicone oil of polystyrene good distribution is added linking agent and catalyzer solidification, obtained high refractive index silica gel.
2. the preparation method of high refractive index silica gel according to claim 1, it is characterised in that: described vinyl silicone oil is the vinyl silicone oil of a kind of general formula having in following two kinds of general formulas:
ViR2SiO(SiR2O)nSiR2Vi;
(Vi)3SiO[Si(R)(Vi)O]m[Si(R)2O]nSi(Vi)3;
Described R is methyl or ethyl or propyl group.
3. the preparation method of high refractive index silica gel according to claim 1, it is characterised in that: linking agent described in step 3 is general formula is Me3SiO(MeHSiO)nSiMe3Linking agent, add-on is the amount making Si-H/Vi=1.02.
4. the preparation method of high refractive index silica gel according to claim 3, it is characterised in that: described catalyzer is platinum catalyst, and add-on is 2-100ppm.
5. the preparation method of high refractive index silica gel according to claim 4, it is characterised in that: condition of cure is 150 DEG C of 2h that are heating and curing.
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