CN103214674B - Method for efficiently producing an organic silicone resin microsphere - Google Patents
Method for efficiently producing an organic silicone resin microsphere Download PDFInfo
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- CN103214674B CN103214674B CN201210226121.9A CN201210226121A CN103214674B CN 103214674 B CN103214674 B CN 103214674B CN 201210226121 A CN201210226121 A CN 201210226121A CN 103214674 B CN103214674 B CN 103214674B
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- 229920002050 silicone resin Polymers 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 25
- 239000004005 microsphere Substances 0.000 title abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 36
- 238000006243 chemical reaction Methods 0.000 claims abstract description 25
- 238000003756 stirring Methods 0.000 claims abstract description 20
- 238000007599 discharging Methods 0.000 claims abstract description 16
- 238000006068 polycondensation reaction Methods 0.000 claims abstract description 14
- 238000009835 boiling Methods 0.000 claims abstract description 11
- 238000004519 manufacturing process Methods 0.000 claims abstract description 11
- 239000000725 suspension Substances 0.000 claims abstract description 5
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 239000003513 alkali Substances 0.000 claims abstract description 3
- 230000001105 regulatory effect Effects 0.000 claims abstract description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 28
- 229910000077 silane Inorganic materials 0.000 claims description 28
- 125000003545 alkoxy group Chemical group 0.000 claims description 7
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical group CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 4
- JCVQKRGIASEUKR-UHFFFAOYSA-N triethoxy(phenyl)silane Chemical group CCO[Si](OCC)(OCC)C1=CC=CC=C1 JCVQKRGIASEUKR-UHFFFAOYSA-N 0.000 claims description 3
- 125000003118 aryl group Chemical group 0.000 claims description 2
- 239000002585 base Substances 0.000 claims description 2
- 125000005395 methacrylic acid group Chemical group 0.000 claims description 2
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 18
- 239000007789 gas Substances 0.000 abstract description 10
- 238000009413 insulation Methods 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 2
- 239000011261 inert gas Substances 0.000 abstract 1
- 239000000376 reactant Substances 0.000 abstract 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 18
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 18
- 230000007062 hydrolysis Effects 0.000 description 16
- 239000000843 powder Substances 0.000 description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 8
- 238000013019 agitation Methods 0.000 description 5
- 229910052786 argon Inorganic materials 0.000 description 5
- 238000010792 warming Methods 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- FVIWBCXKBVGTGV-UHFFFAOYSA-N CO[SiH](OC)OC.C[Si](OCC)(CCCOC(C=C)=O)CCC Chemical compound CO[SiH](OC)OC.C[Si](OCC)(CCCOC(C=C)=O)CCC FVIWBCXKBVGTGV-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 150000001282 organosilanes Chemical class 0.000 description 3
- 239000004033 plastic Substances 0.000 description 3
- 229920003023 plastic Polymers 0.000 description 3
- -1 polysiloxane Polymers 0.000 description 3
- 239000005060 rubber Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 229910002808 Si–O–Si Inorganic materials 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 description 2
- 239000000413 hydrolysate Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 125000000962 organic group Chemical group 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 238000009941 weaving Methods 0.000 description 2
- QDHHCQZDFGDHMP-UHFFFAOYSA-N Chloramine Chemical group ClN QDHHCQZDFGDHMP-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229940040145 liniment Drugs 0.000 description 1
- 239000000865 liniment Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012946 outsourcing Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 125000004149 thio group Chemical group *S* 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N urea group Chemical group NC(=O)N XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 238000006886 vinylation reaction Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Abstract
The invention relates to a method for efficiently producing an organic silicone resin microspheres, comprising: adding silicanes with three or four hydrolysable groups into a high temperature and high pressure reaction vessel, adding water, and stirring; (2) introducing an inert gas into the reaction vessel, to make gas pressure intensity in the reaction vessel be 760*1-7600*10 mmHg; (3) heating the reaction vessel, until the temperature is in a range from a water boiling point -10 DEG C under a relative pressure intensity to a water boiling point under a relative pressure intensity, to perform hydrolysis reaction; (4) in a condition of heat insulation and pressure maintaining, adding alkali, to regulating pH value of reactants in the reaction vessel to be 7-14, and carrying out polycondensation and balling reaction; and (5) reducing temperature and pressure until normal temperature and normal pressure, discharging materials to obtain an waterborne suspension of organic silicone resin microspheres. The method can raise productivity of the organic silicone resin, and simplifies production operations.
Description
Technical field
The present invention relates to silicone resin, be specifically related to the method for producing silicone resin microballoon.
Background technology
Organosilicon is that a veriety is various, excellent property, novel high polymer material that security is good, due to the performance of its excellence, is widely used in every profession and trade in recent years as type material, the industries such as such as coating, plastics, rubber, medicine, hair care articles, weaving.
It is main chain that silicone resin refers to Si-O-Si, Siliciumatom is connected with the electrodeless superpolymer of cross-linking type half of organic group.Silicone resin had both had Si-O-Si inorganic component, had organic group again, therefore had inorganic and organism dual structure feature concurrently.Silicone resin is compared with general polysiloxane, there is better thermotolerance, lower surface energy, excellent thermo-oxidative stability, winter hardiness, weathering resistance, electrical insulating property, hydrophobic nature, oilness, application are more extensive, be particularly useful for the industries such as coating, plastics, rubber.
Silicone resin generally uses with microballoon or particle form.The method of current production organosilicon microballoon mainly comprises emulsion method, utilize inorganic powder to make legal and mechanical disintegration method of sieving of the organic silicon process of carrier outsourcing, silane hydrolyzate retrude etc., but there are production process complexity, cycle long (a general production cycle needs more than 8 hours), the shortcomings such as efficiency is low.
Such as, Chinese patent application 2005100343835 discloses a kind of manufacture method of organic silicon resin ball-shaped micro powder, and the method comprises: water, alcoholic solvent and basic catalyst mix by (1), then at 28-35 DEG C, drip three-functionality-degree silane; (2) less than 15 DEG C termination reactions are cooled to.
Chinese patent application 2006100203618 discloses a kind of synthetic method of silicone resin, the method comprises selects at least one alkyl trialkoxy silane as starting raw material, then water, solvent and hydrochloric acid is added, backflow 1-6 hour, add hexamethyldisilazane again, slaking, obtains transparent silicone resin.
Chinese patent application 2007100356321 discloses a kind of preparation method for organic silicon resin, between the washing and filter progress of the hydrolysis condensation reaction technique of routine, increase and have conventional vacuum to distill oily water separation operation, carry out underpressure distillation oily water separation operation before filtration, remove by underpressure distillation oily water separation operation the micro-moisture remained in organosilicon toluene layer.
Chinese patent application 2007101320524 discloses a kind of preparation technology of organic silicon resin for high temperature resisting powder paint, comprise by organosilane monomer and extraordinary organosilane monomer mixing after add boiling point lower than 100 DEG C with the immiscible organic solvent of water, then sharp alcohols, ethers or esters solvent and water, in the Water Under solution of temperature lower than 25 DEG C, after polycondensation and Active Regulation, steam solvent, obtain solid phase prod.
Chinese patent application 2011100747105 discloses a kind of sand screen silicone resin containing vinyl and preparation method thereof, and it is hydrolyzed under condition of ice bath, room temperature cure, after steaming organic solvent, obtains silicone resin.
Aforesaid method is all be hydrolyzed under normal temperature or low temperature, and hydrolysis rate is slow, and complex procedures.In order to improve the productivity of silicone resin, simplifying production process, needing to improve the preparation technology of silicone resin powder.
Summary of the invention
In order to overcome above-mentioned deficiency, present inventor has performed and study with keen determination, found that: when carrying out hydrolysis and the polycondensation of organosilane at high temperature under high pressure, energy is Reaction time shorten significantly, hydrolysate can directly be reunited at high temperature under high pressure for silicone resin microballoon, thus in very short time, obtain the silicone resin microballoon of excellent performance, thus completes the present invention.
The object of the present invention is to provide a kind of method of high efficiency production silicone resin microballoon, the method comprises:
(1) in high-temperature high-pressure reaction kettle, add the silane with three or four hydrolysable group, and drop into water, the weight ratio of the silane and water wherein with three or four hydrolysable group is 1:1-1:20;
(2) in reactor, be filled with rare gas element, make gas pressure intensity in reactor be 760 × 1-7600 × 10mmHg;
(3) reacting by heating still, until in the scope of the water boiling point of temperature under (water boiling point under corresponding pressure-10 DEG C) to corresponding pressure, be hydrolyzed reaction;
(4) under constant temperature, pressure, add alkali, the pH regulating reaction kettle for reaction thing is 7-14, carries out polycondensation, balling-up reaction;
(5) lower the temperature, be depressurized to normal temperature, normal pressure, discharging obtains silicone resin microballoon waterborne suspension.
By method provided by the invention, can in the very short time being no more than 2 hours high efficiency production silicone resin microballoon, High Temperature High Pressure is conducive to the quick and complete hydrolysis of silane, and be conducive to the product polycondensation balling-up after complete hydrolysis, particularly in the basic conditions, polycondensation balling-up speed is accelerated further, and efficiency is 3 to 4 times that carry out reacting at normal pressure, low temperature are as 10-60 DEG C.In addition, the method is " still " formula method, and reaction process is all carried out in same reactor, and without the need to stopping or carrying out the operations such as separation and purification between the reaction period, reaction process is simple.
Embodiment
The present invention is described in detail below, and illustrated by these, the features and advantages of the invention will become more clear, clear and definite.
In the present invention, silane used is the silane with three or four hydrolysable group, can form microballoon after its complete hydrolysis.For the silane with three or four hydrolysable group, the organoalkoxysilane with three or four alkoxyl groups can be used, for the organoalkoxysilane with three alkoxyl groups, except three hydrolyzable alkoxy groups groups, other group can also be had, such as chloropropyl, aromatic base, amino, chlorine atom, methacrylic acid group, sulfydryl, urea groups, thio group or epoxy group(ing).
As for the alkoxyl group in trialkoxy silane and tetraalkoxysilane, being not particularly limited, can be methoxyl group, oxyethyl group etc. independently of one another.
As the specific examples of trialkoxy silane and tetraalkoxysilane, mention such as propyl-triethoxysilicane, propyl trimethoxy silicane, phenyl triethoxysilane, tetraethoxysilane, methyl-propyl acryloxypropylethoxysilane Trimethoxy silane.
In the present invention, can use above-mentioned any one that have in the organoalkoxysilane of three or four alkoxyl groups, or use wherein arbitrarily two or more combination.Preferably, as hydrolyzable silane, be made up of trialkoxy silane and tetraalkoxysilane, and the weight ratio of trialkoxy silane and tetraalkoxysilane is preferably 1:2-1:5, the all processes of now hydrolysis, polycondensation, balling-up reaction can complete in 2 hours, and gained silicone resin microballoon excellent quality, in product, solid impurity content is no more than 1000ppm.
In the present invention, in order to promote silane hydrolyzate, the amount ratio of the silane and water with three or four hydrolysable group is 1:1-1:20, and preferred 1:2-1:10, based on weight.If the amount ratio of silane and water is higher than 1: 1, then hydrolysis can be caused complete not because the water yield is too low; Otherwise, if the amount ratio of silane and water is lower than 1: 20, then can cause complicated operation because the water yield is too high.
The present inventor finds through research, when reacting when being hydrolyzed in airtight autoclave, when by heating temperatures to (water boiling point under corresponding pressure-10 DEG C) to the scope of the water boiling point under corresponding pressure time, be generally 80 DEG C-180 DEG C, now water is in state at a simmer, under such High Temperature High Pressure, silane is hydrolyzed rapidly.Experiment finds, in such a situa-tion, hydrolysis reaction carries out 10-20 minute silane and gets final product complete hydrolysis.
The rare gas element that the present invention is used, is mainly used to make pressure in still be raised to required degree, ensures that gas itself does not participate in reaction simultaneously.
The present inventor finds through great many of experiments, after silane complete hydrolysis, when the polycondensation that is hydrolyzed in airtight autoclave, balling-up reaction, time in the scope of the water boiling point of temperature under (water boiling point under corresponding pressure-10 DEG C) to corresponding pressure, be generally 80 DEG C-180 DEG C, namely under heat-insulation pressure keeping condition, polycondensation is obviously accelerated, the balling-up and polycondensation product is reunited fast, especially, when system pH is adjusted to alkalescence, as pH be 7-14 time, when particularly pH is 8-10, is easier to polycondensation product reunion and forms ball and ball growth.In such a situa-tion, experiment finds, 1 hours hydrolysate can polycondensation completely, form silicone resin microballoon.
Lower the temperature, be depressurized to normal temperature, normal pressure, discharging obtains silicone resin microballoon waterborne suspension.For this silicone resin microballoon waterborne suspension, can aftertreatment be carried out, as with acid neutralization, filtration, oven dry, obtain silicone resin microsphere powder.
According to the organosilicon microballoon resin that the present invention obtains, there is excellent character, the sliding hand feeling agent of fire retardant, light diffusing agent, surperficial antifriction liniment or silk etc. can be used as, for industries such as coating, plastics, rubber, medicine, hair care articles, weavings.
Embodiment
Embodiment 1
100g tetraethoxysilane, 400g propyl trimethoxy silicane and 3L water is dropped in autoclave, in autoclave, be under agitation filled with argon gas to pressure is 760 × 2mmHg, be warming up to system temperature to 110 DEG C, stir at this temperature and complete hydrolysis in 15 minutes, the sodium hydroxide solution of 10% is added by feeding device in autoclave, regulation system pH is 7, stop after stirring stirring, heat-insulation pressure keeping step-down after 1 hour, be cooled to room temperature, discharging, neutralize with acetic acid, filter, dry to obtain silicone resin microsphere powder.From be fed to discharging only the used time less than 2 hours.
Embodiment 2
100g phenyl triethoxysilane, 400g propyl trimethoxy silicane and 3L water is dropped in autoclave, in autoclave, be under agitation filled with argon gas to pressure is 760 × 5mmHg, be warming up to system temperature to 140 DEG C, stir at this temperature and complete hydrolysis in 15 minutes, the sodium hydroxide solution of 10% is added by feeding device in autoclave, regulation system pH is 8, stop after stirring stirring, heat-insulation pressure keeping step-down after 1 hour, be cooled to room temperature, discharging, neutralize with acetic acid, filter, dry to obtain silicone resin microsphere powder.From be fed to discharging only the used time less than 2 hours.
Embodiment 3
100g methyl-propyl acryloxypropylethoxysilane Trimethoxy silane, 400g propyl-triethoxysilicane and 2L water is dropped in autoclave, in autoclave, be under agitation filled with argon gas to pressure is 760 × 4mmHg, be warming up to system temperature to 130 DEG C, stir at this temperature and complete hydrolysis in 30 minutes, the sodium hydroxide solution of 10% is added by feeding device in autoclave, regulation system pH is 10, stop after stirring stirring, heat-insulation pressure keeping step-down after 1 hour, be cooled to room temperature, discharging, neutralize with acetic acid, filter, dry to obtain silicone resin microsphere powder.From be fed to discharging only the used time less than 2 hours.
Embodiment 4
In autoclave, drop into 500g propyl trimethoxy silicane and 2L water, in autoclave, be under agitation filled with argon gas is 760 × 4mmHg to pressure, is warming up to system temperature to 130 DEG C, stir at this temperature and complete hydrolysis in 20 minutes, added the sodium hydroxide solution of 10% by feeding device in autoclave, regulation system pH is 8, stops stirring after stirring, heat-insulation pressure keeping step-down after 1 hour, be cooled to room temperature, discharging, neutralize with acetic acid, filter, dry to obtain silicone resin microsphere powder.From be fed to discharging only the used time less than 2 hours.
Embodiment 5
In autoclave, drop into 100g tetraethoxysilane and 3L water, in autoclave, be under agitation filled with argon gas is 760 × 2mmHg to pressure, is warming up to system temperature to 110 DEG C, stir at this temperature and complete hydrolysis in 15 minutes, added the sodium hydroxide solution of 10% by feeding device in autoclave, regulation system pH is 10, stops stirring after stirring, heat-insulation pressure keeping step-down after 1 hour, be cooled to room temperature, discharging, neutralize with acetic acid, filter, dry to obtain silicone resin microsphere powder.From be fed to discharging only the used time less than 2 hours.
Comparative example 1
At room temperature, in reactor, drop into 100g methyl-propyl acryloxypropylethoxysilane Trimethoxy silane, 400g propyl-triethoxysilicane and 2L water, stir at 50-60 DEG C and complete hydrolysis in 3 hours, add the sodium hydroxide solution of 10%, regulation system p H is 10, stop after stirring stirring, at 60 DEG C, be incubated 5-6 hour, be cooled to room temperature, discharging, with acetic acid neutralization, filter, dry to obtain silicone resin microsphere powder.From being fed to about 10 hours discharging used times.
Above by exemplary embodiment and embodiment to invention has been detailed description, but, these embodiments and embodiment are only illustrative, do not form any restriction to scope of the present invention.It will be appreciated by those skilled in the art that when not exceeding spirit and scope of the invention, can carry out multiple equivalencing, modification and improvement to technical solutions and their implementation methods of the present invention, these all should fall within the scope of protection of the present invention.
The all documents mentioned in literary composition, which is hereby incorporated by reference.
Claims (4)
1. a method for high efficiency production silicone resin microballoon, the method comprises:
(1) in high-temperature high-pressure reaction kettle, add the silane with three or four hydrolysable group, and drop into water, stir, the weight ratio of the silane and water wherein with three or four hydrolysable group is 1:1-1:20;
(2) in reactor, be pressed into rare gas element, make gas pressure intensity in reactor be 760 × 1-7600 × 10mmHg;
(3) reacting by heating still, until in the scope of the water boiling point of temperature under (water boiling point under corresponding pressure-10 DEG C) to corresponding pressure, be hydrolyzed reaction, the time of the reaction that is hydrolyzed is 10-20 minute;
(4) under constant temperature, pressure, add alkali, the pH regulating reaction kettle for reaction thing is 8-10, carries out polycondensation, balling-up reaction, carries out polycondensation, the time of balling-up reaction is 1 hour;
(5) lower the temperature, be depressurized to normal temperature, normal pressure, discharging obtains silicone resin microballoon waterborne suspension;
The silane wherein with three or four hydrolysable group is the organoalkoxysilane with three or four alkoxyl groups,
Wherein, for the organoalkoxysilane with three alkoxyl groups, other group on silane is aromatic base, methacrylic acid group.
2. method according to claim 1, wherein the weight ratio of trialkoxy silane and tetraalkoxysilane is 1:2-1:5.
3. method according to claim 1 and 2, wherein trialkoxy silane is phenyl triethoxysilane;
Tetraalkoxysilane is tetraethoxysilane.
4. method according to claim 1, wherein in step (1), the amount ratio of the silane and water with three or four hydrolysable group is 1:2-1:10.
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| CN104610545A (en) * | 2015-02-11 | 2015-05-13 | 广州市晶硅新材料有限公司 | Preparation method of colored organosilicon powder |
| CN109608996B (en) * | 2018-11-29 | 2021-01-26 | 佛山市顺德区蓝天实业有限公司 | High-reflection powder coating suitable for LED lampshade and preparation method thereof |
| CN111927800A (en) * | 2020-08-13 | 2020-11-13 | 马宁疆 | Aromatic dustproof material for fan and preparation method thereof |
| CN112646186B (en) * | 2020-12-16 | 2021-10-12 | 上海大学 | Method for preparing organic silicon resin coating by utilizing hydrolytic polymerization of organic silane |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000186148A (en) * | 1998-12-21 | 2000-07-04 | Ge Toshiba Silicones Co Ltd | Production of spherical polymethylsilsesquioxane particle |
| CN101676023A (en) * | 2008-09-17 | 2010-03-24 | 中国科学院化学研究所 | Method for preparing poly-organic silsesquioxane microsphere |
| CN101809068A (en) * | 2007-04-24 | 2010-08-18 | 莫门蒂夫性能材料股份有限公司 | Method of applying an anti-corrosion and/or adhesion promoting coating to a metal and resulting coated metal |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000186148A (en) * | 1998-12-21 | 2000-07-04 | Ge Toshiba Silicones Co Ltd | Production of spherical polymethylsilsesquioxane particle |
| CN101809068A (en) * | 2007-04-24 | 2010-08-18 | 莫门蒂夫性能材料股份有限公司 | Method of applying an anti-corrosion and/or adhesion promoting coating to a metal and resulting coated metal |
| CN101676023A (en) * | 2008-09-17 | 2010-03-24 | 中国科学院化学研究所 | Method for preparing poly-organic silsesquioxane microsphere |
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