CN103214674A - 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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- CN103214674A CN103214674A CN2012102261219A CN201210226121A CN103214674A CN 103214674 A CN103214674 A CN 103214674A CN 2012102261219 A CN2012102261219 A CN 2012102261219A CN 201210226121 A CN201210226121 A CN 201210226121A CN 103214674 A CN103214674 A CN 103214674A
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- silicone resin
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- silane
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- 229920002050 silicone resin Polymers 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 32
- 239000004005 microsphere Substances 0.000 title abstract 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 34
- 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 9
- 239000000725 suspension Substances 0.000 claims abstract description 5
- 239000000376 reactant Substances 0.000 claims abstract description 4
- 239000003513 alkali Substances 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 30
- 229910000077 silane Inorganic materials 0.000 claims description 28
- 125000003545 alkoxy group Chemical group 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- -1 chloropropyl Chemical group 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 5
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 4
- 230000001143 conditioned effect Effects 0.000 claims description 3
- JCVQKRGIASEUKR-UHFFFAOYSA-N triethoxy(phenyl)silane Chemical compound CCO[Si](OCC)(OCC)C1=CC=CC=C1 JCVQKRGIASEUKR-UHFFFAOYSA-N 0.000 claims description 3
- QDHHCQZDFGDHMP-UHFFFAOYSA-N Chloramine Chemical group ClN QDHHCQZDFGDHMP-UHFFFAOYSA-N 0.000 claims description 2
- 125000003118 aryl group Chemical group 0.000 claims description 2
- 239000002585 base Substances 0.000 claims description 2
- 125000003700 epoxy group Chemical group 0.000 claims description 2
- 239000003063 flame retardant Substances 0.000 claims description 2
- 229940040145 liniment Drugs 0.000 claims description 2
- 239000000865 liniment Substances 0.000 claims description 2
- 125000005395 methacrylic acid group Chemical group 0.000 claims description 2
- 125000004149 thio group Chemical group *S* 0.000 claims description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N urea group Chemical group NC(=O)N XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 2
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 20
- 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
- 230000001105 regulatory effect Effects 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 18
- 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 10
- 238000013019 agitation Methods 0.000 description 5
- 229910052786 argon Inorganic materials 0.000 description 5
- 238000010792 warming Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 239000000047 product Substances 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
- 239000002904 solvent Substances 0.000 description 4
- 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
- 238000004821 distillation 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
- 239000005060 rubber Substances 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon 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
- 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
- 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
- 230000015572 biosynthetic process Effects 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
- 150000002148 esters Chemical class 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 239000012535 impurity Substances 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
- 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
- 238000010189 synthetic method Methods 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
Landscapes
- Silicon Polymers (AREA)
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 produce the method for silicone resin microballoon.
Background technology
Organosilicon is that a veriety is various, excellent property, novel high polymer material that security is good, because its excellent performance has been widely used in every profession and trade as type material, for example industries such as coating, plastics, rubber, medicine, hair care articles, weaving in recent years.
It is main chain that silicone resin is meant with Si-O-Si, is connected with the cross-linking type half electrodeless superpolymer of organic group on the Siliciumatom.Silicone resin had both had the Si-O-Si inorganic component, had organic group again, therefore had concurrently inorganic and organism dual structure characteristics.Silicone resin is compared with general polysiloxane, have better thermotolerance, lower surface energy, excellent thermo-oxidative stability, winter hardiness, weathering resistance, electrical insulating property, hydrophobic nature, oilness, application is more extensive, is particularly useful for industries such as coating, plastics, rubber.
Silicone resin generally uses with microballoon or particle form.The method of producing the organosilicon microballoon at present mainly comprises emulsion method, utilizes inorganic powder to make carrier outsourcing organosilicon method, silane hydrolyzate after method and mechanical disintegration method of sieving etc., but production process complexity, cycle long (a general production cycle needs more than 8 hours) are all arranged, shortcoming such as efficient is low.
For example, Chinese patent application 2005100343835 discloses a kind of manufacture method of organic silicon resin ball-shaped micro powder, and this method comprises: (1) mixes water, alcoholic solvent and basic catalyst, drips three-functionality-degree silane down at 28-35 ℃ then; (2) be cooled to 15 ℃ of following termination reactions.
Chinese patent application 2006100203618 discloses a kind of synthetic method of silicone resin, this method comprises selects at least a alkyl trialkoxy silane as starting raw material, add entry, solvent and hydrochloric acid then, 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, in the washing of the hydrolysis condensation reaction technology of routine and filter between the operation, increasing has conventional underpressure distillation oily water separation operation, before filtering, carry out underpressure distillation oily water separation operation, remove the micro-moisture that remains in the organosilicon toluene layer by underpressure distillation oily water separation operation.
Chinese patent application 2007101320524 discloses a kind of preparation technology of organic silicon resin for high temperature resisting powder paint, comprise with organosilane monomer and extraordinary organosilane monomer mix the back add boiling point be lower than 100 ℃ with the immiscible organic solvent of water in, sharp then alcohols, ethers or esters solvent and water, be lower than hydrolysis under 25 ℃ the condition in temperature, after polycondensation and active the adjusting, steam solvent, obtain solid phase prod.
Chinese patent application 2011100747105 discloses a kind of sand screen with containing silicone resin of vinyl and preparation method thereof, and it is hydrolyzed under condition of ice bath, room temperature cure, steam organic solvent after, obtain silicone resin.
Aforesaid method all is to 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, simplify production process, need the preparation technology of silicone resin powder be improved.
Summary of the invention
In order to overcome above-mentioned deficiency, the inventor has carried out research with keen determination, found that: when hydrolysis and the polycondensation of under High Temperature High Pressure, carrying out organosilane, can significantly shorten the reaction times, hydrolysate can directly be reunited under High Temperature High Pressure and is the silicone resin microballoon, thereby obtains the silicone resin microballoon of excellent performance in the short period of time at the utmost point, thereby finishes the present invention.
The object of the present invention is to provide a kind of method of high efficiency production silicone resin microballoon, this method comprises:
(1) add the silane with three or four hydrolysable group in high-temperature high-pressure reaction kettle, and drop into water, wherein having the silane of three or four hydrolysable group and the weight ratio of water is 1:1-1:20;
(2) in reactor, charge into rare gas element, make that gas pressure intensity is 760 * 1-7600 * 10mmHg in the reactor;
(3) reacting by heating still, in the scope of (water boiling point under the corresponding pressure-10 ℃) water boiling point to the corresponding pressure, reaction is hydrolyzed until temperature;
(4) under constant temperature, pressure, add alkali, the pH of reactant is 7-14 in the conditioned reaction still, 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 be at the utmost point that is no more than 2 hours high efficiency production silicone resin microballoon in the short period of time, High Temperature High Pressure helps the quick and complete hydrolysis of silane, and help product polycondensation balling-up after the complete hydrolysis, particularly under alkaline condition, polycondensation balling-up speed is further accelerated, and efficient is 3 to 4 times that react under normal pressure, low temperature such as 10-60 ℃.In addition, this method is " still " formula method, and reaction process is all carried out in same reactor, and, need not between the reaction period to end or carry out operation such as separation and purification, reaction process is simple.
Embodiment
Below the present invention is described in detail, by these explanations, it is more clear, clear and definite that characteristics of the present invention and advantage will become.
In the present invention, used silane is the silane with three or four hydrolysable group, so that can form microballoon after its complete hydrolysis.For silane with three or four hydrolysable group, can use organoalkoxysilane with three or four alkoxyl groups, for organoalkoxysilane with three alkoxyl groups, except three hydrolyzable alkoxy grps, can also have other group, for example chloropropyl, aromatic base, amino, chlorine atom, methacrylic acid group, sulfydryl, urea groups, thio group or epoxy group(ing).
Alkoxyl group as in trialkoxy silane and the tetraalkoxysilane is not particularly limited, and can be methoxyl group, oxyethyl group etc. independently of one another.
As the specific examples of trialkoxy silane and tetraalkoxysilane, mention for example propyl-triethoxysilicane, propyl trimethoxy silicane, phenyl triethoxysilane, tetraethoxysilane, methyl-propyl acyloxy propyl trimethoxy silicane.
In the present invention, can use in the above-mentioned organoalkoxysilane with three or four alkoxyl groups any, perhaps use wherein the combination of two or more arbitrarily.Preferably, as hydrolyzable silane, constitute by trialkoxy silane and tetraalkoxysilane, and the weight ratio of trialkoxy silane and tetraalkoxysilane is preferably 1:2-1:5, the all processes of hydrolysis this moment, polycondensation, balling-up reaction can be finished in 2 hours, and gained silicone resin microballoon excellent quality, solid impurity content is no more than 1000ppm in the product.
In the present invention, in order to promote silane hydrolyzate, having the silane of three or four hydrolysable group and the amount ratio of water is 1:1-1:20, and preferred 1:2-1:10 is based on weight.If the amount ratio of silane and water is higher than 1: 1, then can cause hydrolysis complete inadequately owing to the water yield is low excessively; Otherwise,, then can cause complicated operation owing to the water yield is too high if the amount ratio of silane and water is lower than 1: 20.
The inventor is through discovering, when in enclosed autoclave, being hydrolyzed reaction, when in the scope that temperature is heated to (water boiling point under the corresponding pressure-10 ℃) water boiling point to the corresponding pressure, be generally 80 ℃-180 ℃, this moment, water was in state at a simmer, under such High Temperature High Pressure, the rapid hydrolysis of silane.Experiment finds that under such condition, 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 the interior pressure of still to be raised to required degree, guarantees that simultaneously gas itself does not participate in reaction.
The inventor finds through a large amount of experiments, after the silane complete hydrolysis, when the polycondensation that in enclosed autoclave, is hydrolyzed, balling-up reaction, temperature is in the scope of (water boiling point under the corresponding pressure-10 ℃) water boiling point to the corresponding pressure the time, be generally 80 ℃-180 ℃, be under the heat-insulation pressure keeping condition, polycondensation is obviously accelerated, and the polycondensation product balling-up of reuniting fast, especially, when system pH is adjusted to alkalescence, when being 7-14 as pH, when particularly pH is 8-10, is easier to the polycondensation product reunion and forms ball and ball growth.Under such condition, experiment finds that hydrolysate can complete, the formation silicone resin microballoon of polycondensation about 1 hour.
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 carry out aftertreatment, as with acid neutralization, filtration, oven dry, obtain silicone resin microballoon powder.
The organosilicon microballoon resin that obtains according to the present invention has excellent character, can be used as fire retardant, light diffusing agent, surperficial antifriction liniment or the sliding hand feeling agent of silk etc., is used for industries such as coating, plastics, rubber, medicine, hair care articles, weaving.
Embodiment
Embodiment 1
In autoclave, drop into 100g tetraethoxysilane, 400g propyl trimethoxy silicane and 3L water, under agitation charging into argon gas to pressure in autoclave is 760 * 2mmHg, be warming up to system temperature to 110 ℃, under this temperature, stir and finished hydrolysis in 15 minutes, sodium hydroxide solution by feeding device adding 10% in the 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 neutralizes with acetic acid, filter, dry silicone resin microballoon powder.From be fed to discharging only the time spent less than 2 hours.
Embodiment 2
In autoclave, drop into 100g phenyl triethoxysilane, 400g propyl trimethoxy silicane and 3L water, under agitation charging into argon gas to pressure in autoclave is 760 * 5mmHg, be warming up to system temperature to 140 ℃, under this temperature, stir and finished hydrolysis in 15 minutes, sodium hydroxide solution by feeding device adding 10% in the 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 neutralizes with acetic acid, filter, dry silicone resin microballoon powder.From be fed to discharging only the time spent less than 2 hours.
Embodiment 3
In autoclave, drop into 100g methyl-propyl acyloxy propyl trimethoxy silicane, 400g propyl-triethoxysilicane and 2L water, under agitation charging into argon gas to pressure in autoclave is 760 * 4mmHg, be warming up to system temperature to 130 ℃, under this temperature, stir and finished hydrolysis in 30 minutes, sodium hydroxide solution by feeding device adding 10% in the 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 neutralizes with acetic acid, filter, dry silicone resin microballoon powder.From be fed to discharging only the time spent less than 2 hours.
Embodiment 4
Drop into 500g propyl trimethoxy silicane and 2L water in autoclave, under agitation charging into argon gas to pressure in autoclave is 760 * 4mmHg, is warming up to system temperature to 130 ℃, under this temperature, stir and finished hydrolysis in 20 minutes, by the sodium hydroxide solution of feeding device adding 10% in the autoclave, regulation system pH is 8, stops after stirring stirring, heat-insulation pressure keeping step-down after 1 hour, be cooled to room temperature, discharging neutralizes with acetic acid, filter, dry silicone resin microballoon powder.From be fed to discharging only the time spent less than 2 hours.
Embodiment 5
Drop into 100g tetraethoxysilane and 3L water in autoclave, under agitation charging into argon gas to pressure in autoclave is 760 * 2mmHg, is warming up to system temperature to 110 ℃, under this temperature, stir and finished hydrolysis in 15 minutes, by the sodium hydroxide solution of feeding device adding 10% in the autoclave, regulation system pH is 10, stops after stirring stirring, heat-insulation pressure keeping step-down after 1 hour, be cooled to room temperature, discharging neutralizes with acetic acid, filter, dry silicone resin microballoon powder.From be fed to discharging only the time spent less than 2 hours.
Comparative Examples 1
At room temperature, in reactor, drop into 100g methyl-propyl acyloxy propyl trimethoxy silicane, 400g propyl-triethoxysilicane and 2L water, stir down at 50-60 ℃ and finished hydrolysis in 3 hours, add 10% sodium hydroxide solution, regulation system p H is 10, stop after stirring stirring, be incubated 5-6 hour down, be cooled to room temperature at 60 ℃, discharging, with acetic acid neutralization, filter, dry silicone resin microballoon powder.From being fed to about 10 hours of discharging time spent.
More than by exemplary embodiment and embodiment the present invention is had been described in detail, but, these embodiments and embodiment only are illustrative, scope of the present invention are not constituted any restriction.It will be appreciated by those skilled in the art that under the situation that does not exceed spirit and scope of the invention can carry out multiple replacement of equal value, modify and improve technical solutions and their implementation methods of the present invention, these all should fall within the scope of protection of the present invention.
All documents of mentioning in the literary composition are incorporated herein by reference in full at this.
Claims (10)
1. the method for a high efficiency production silicone resin microballoon, this method comprises:
(1) add the silane with three or four hydrolysable group in high-temperature high-pressure reaction kettle, and drop into water, stir, wherein having the silane of three or four hydrolysable group and the weight ratio of water is 1:1-1:20;
(2) in reactor, be pressed into rare gas element, make that gas pressure intensity is 760 * 1-7600 * 10mmHg in the reactor;
(3) reacting by heating still, in the scope of (water boiling point under the corresponding pressure-10 ℃) water boiling point to the corresponding pressure, reaction is hydrolyzed until temperature;
(4) under constant temperature, pressure, add alkali, the pH of reactant is 7-14 in the conditioned reaction still, carries out polycondensation, balling-up reaction;
(5) lower the temperature, be depressurized to normal temperature, normal pressure, discharging obtains silicone resin microballoon waterborne suspension.
2. method according to claim 1, the silane that wherein has three or four hydrolysable group is the organoalkoxysilane with three or four alkoxyl groups.
3. method according to claim 2, wherein, for the organoalkoxysilane with three alkoxyl groups, other group on the silane is chloropropyl, aromatic base, amino, chlorine atom, methacrylic acid group, sulfydryl, urea groups, thio group or epoxy group(ing).
4. according to claim 2 or 3 described methods, wherein the weight ratio of trialkoxy silane and tetraalkoxysilane is preferably 1:2-1:5.
5. according to claim 2 or 3 described methods, wherein trialkoxy silane is propyl-triethoxysilicane, propyl trimethoxy silicane, phenyl triethoxysilane, methyl-propyl acyloxy propyl trimethoxy silicane;
Tetraalkoxysilane is a tetraethoxysilane.
6. method according to claim 1, wherein in the step (1), having the silane of three or four hydrolysable group and the amount ratio of water is 1:2-1:10.
7. method according to claim 1, wherein in the step (3), the time of the reaction that is hydrolyzed is 10-20 minute.
8. method according to claim 1, wherein in the step (4), the pH of reactant is 8-10 in the conditioned reaction still.
9. method according to claim 1, wherein in the step (4), the time of carrying out polycondensation, balling-up reaction is 1 hour.
According to the silicone resin of each described method preparation among the claim 1-9 as fire retardant, light diffusing agent, releasing agent, the purposes of surperficial antifriction liniment or the sliding hand feeling agent of silk.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN109608996A (en) * | 2018-11-29 | 2019-04-12 | 佛山市顺德区蓝天实业有限公司 | A kind of high reflection powdery paints and preparation method thereof suitable for LED lamp cover |
| CN111927800A (en) * | 2020-08-13 | 2020-11-13 | 马宁疆 | Aromatic dustproof material for fan and preparation method thereof |
| CN112646186A (en) * | 2020-12-16 | 2021-04-13 | 上海大学 | Method for preparing organic silicon resin coating by utilizing hydrolytic polymerization of organic silane |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN109608996A (en) * | 2018-11-29 | 2019-04-12 | 佛山市顺德区蓝天实业有限公司 | A kind of high reflection powdery paints and preparation method thereof suitable for LED lamp cover |
| CN111927800A (en) * | 2020-08-13 | 2020-11-13 | 马宁疆 | Aromatic dustproof material for fan and preparation method thereof |
| CN112646186A (en) * | 2020-12-16 | 2021-04-13 | 上海大学 | Method for preparing organic silicon resin coating by utilizing hydrolytic polymerization of organic silane |
| 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 |
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