CN103965478B - A kind of preparation method of recessed soil matrix MQ silicone resin - Google Patents
A kind of preparation method of recessed soil matrix MQ silicone resin Download PDFInfo
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- 239000002689 soil Substances 0.000 title claims abstract description 66
- 229920002050 silicone resin Polymers 0.000 title claims abstract description 53
- 239000011159 matrix material Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 54
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 27
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 26
- 229960001866 silicon dioxide Drugs 0.000 claims abstract description 26
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 26
- 235000019353 potassium silicate Nutrition 0.000 claims abstract description 25
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 24
- 239000000203 mixture Substances 0.000 claims abstract description 21
- 239000003513 alkali Substances 0.000 claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 15
- 239000006185 dispersion Substances 0.000 claims abstract description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 59
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 9
- -1 aminoalkoxysilane Chemical compound 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 230000007062 hydrolysis Effects 0.000 claims description 8
- 238000006460 hydrolysis reaction Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 6
- 230000001476 alcoholic effect Effects 0.000 claims description 6
- 229920002545 silicone oil Polymers 0.000 claims description 6
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 4
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 4
- 125000003545 alkoxy group Chemical group 0.000 claims description 4
- 238000000605 extraction Methods 0.000 claims description 4
- 229910000077 silane Inorganic materials 0.000 claims description 4
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- 239000002585 base Substances 0.000 claims description 2
- DMZWVCJEOLBQCZ-UHFFFAOYSA-N chloro(ethenyl)silane Chemical compound Cl[SiH2]C=C DMZWVCJEOLBQCZ-UHFFFAOYSA-N 0.000 claims description 2
- YGZSVWMBUCGDCV-UHFFFAOYSA-N chloro(methyl)silane Chemical compound C[SiH2]Cl YGZSVWMBUCGDCV-UHFFFAOYSA-N 0.000 claims description 2
- GTPDFCLBTFKHNH-UHFFFAOYSA-N chloro(phenyl)silicon Chemical compound Cl[Si]C1=CC=CC=C1 GTPDFCLBTFKHNH-UHFFFAOYSA-N 0.000 claims description 2
- VPZDAHBNTYZYHC-UHFFFAOYSA-N chlorosilylamine Chemical compound N[SiH2]Cl VPZDAHBNTYZYHC-UHFFFAOYSA-N 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 2
- 229920002554 vinyl polymer Polymers 0.000 claims description 2
- 239000008096 xylene Substances 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 5
- 239000002253 acid Substances 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 3
- 230000003014 reinforcing effect Effects 0.000 abstract description 3
- 229920005989 resin Polymers 0.000 abstract description 3
- 239000011347 resin Substances 0.000 abstract description 3
- 238000005282 brightening Methods 0.000 abstract description 2
- 239000006229 carbon black Substances 0.000 abstract description 2
- 239000013530 defoamer Substances 0.000 abstract description 2
- 239000012756 surface treatment agent Substances 0.000 abstract description 2
- 229960000892 attapulgite Drugs 0.000 description 6
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 239000003921 oil Substances 0.000 description 6
- 229910052625 palygorskite Inorganic materials 0.000 description 6
- 239000003292 glue Substances 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 229920002379 silicone rubber Polymers 0.000 description 3
- 239000005051 trimethylchlorosilane Substances 0.000 description 3
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 description 2
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000002734 clay mineral Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- XQSFXFQDJCDXDT-UHFFFAOYSA-N hydroxysilicon Chemical compound [Si]O XQSFXFQDJCDXDT-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 239000000565 sealant Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 238000005987 sulfurization reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Abstract
The invention discloses a kind of preparation method of recessed soil matrix MQ silicone resin, recessed soil is first prepared into the mixture of fibrous nano silicon-dioxide and water glass by this resin in alkali effect, then under acid and M chain link organosilicon end capping agent effect, form the dispersion liquid of recessed soil matrix MQ silicone resin, and obtain product through aftertreatment.This resin has the collaborative reinforcing effect of white carbon black and MQ silicone resin, and dispersiveness is better, specific surface area is large, resistance toheat is good, with low cost, can be widely used in fields such as surface treatment agent, supporting material, tackifier, releasing agent, defoamer, release agent, brightening agent, damage resistant agent.
Description
Technical field
The present invention relates to the preparing technical field of silicone resin, particularly relate to a kind of preparation method of recessed soil matrix MQ silicone resin.
Background technology
MQ silicone resin is the very unique siloxanes of a class, it is the silicone resin having four functionality siloxane polycondensation chain links (Q) and single functionality siloxane unit (M) to form, its molar mass is generally 1000 ~ 8000, the character of the when structures shape resin of the amount of M chain link and Q chain link and range of application in molecular structure.MQ silicone resin is mainly used in following field: one is surface treatment agent, as bonding in organic pressure-sensitive gel, mobile phone key glue, epoxies adhesive surface etc.; Two is supporting materials, is applied in the joint sealant etc. of RTV glue, HTV glue, add-on type liquid silicon rubber, hot sulfurization rubber, semiconductor element; Three is tackifier, for seal gum and silicone resin coating; Four is other additives, as releasing agent, defoamer, release agent, brightening agent, damage resistant agent etc.The method for making of MQ silicone resin, is mainly divided into water glass (water glass) method and silicic acid ester process by Q chain link raw material sources, and M chain link source is mainly trimethylchlorosilane.Soluble glass method technique is simple, raw material is easy to get, with low cost, be easy to obtained low M/Q product, obtain and pay close attention to widely.
Recessed soil is the abbreviation of attapulgite, and also claiming attapulgite or polygorskite, is a kind of rich zeopan clay mineral with natural one dimension Nano structure, the brilliant diameter of its single fiber is at about 20nm, and length can reach several micron, has flourishing specific surface area, at China's rich reserves, cheap.Recessed soil is under alkali effect, the mixture of fibrous nano silicon-dioxide and water glass can be formed, then acid and the agent of M chain link organosilicon end capping effect under, form MQ silicone resin (the i.e. recessed soil matrix MQ silicone resin) dispersion liquid being evenly coated with fibrous nano silicon-dioxide, and obtain recessed soil matrix MQ silicone resin through aftertreatment.At present, the method has no bibliographical information.
Summary of the invention
The object of this invention is to provide a kind of there is fibrous nano nucleocapsid structure, the preparation method of dispersing property is good, absorption property is good, resistance toheat is good, with low cost recessed soil matrix MQ silicone resin.
The technical scheme that the present invention takes is:
The concrete steps of the preparation method of recessed soil matrix MQ silicone resin of the present invention are as follows:
(1) preparation of fibrous nano silicon-dioxide and waterglass mixture: recessed soil is distributed in alkali lye, 0.5-24h is stirred at 20-100 DEG C, obtained fibrous nano silicon-dioxide and waterglass mixture, wherein the concentration of alkali lye is 0.5-20mol/L, and the mass ratio of recessed soil and alkali lye is 0.05-0.25: 1;
(2) preparation of recessed soil matrix MQ silicone resin dispersion liquid: under constantly stirring, fibrous nano silicon-dioxide and waterglass mixture prepared by step (1) is added in concentrated hydrochloric acid, adjust ph is 0.5-5, hydrolysis 1-60min, then the alcoholic solution of M chain link organosilicon end capping agent is added, cohydrolysis 1-120min, the agent of M chain link organosilicon end capping is 0.01-1: 1 with the mass ratio adding recessed soil at first, cohydrolysis temperature controls at 20-100 DEG C, obtained recessed soil matrix MQ silicone resin dispersion liquid;
(3) aftertreatment: extract with extraction agent, gets upper strata oil reservoir, washs to neutrality dry at 60-120 DEG C, obtains recessed soil matrix MQ silicone resin.
In step (1), alkali lye is the one in sodium hydroxide, potassium hydroxide.
In step (1), preferably recessed soil is distributed in alkali lye, at 60 DEG C, stirs 12h.
In step (1), the concentration of preferred alkali lye is 10mol/L, and the mass ratio of recessed soil and alkali lye is 0.15: 1.
In step (2), the agent of M chain link organosilicon end capping is the one in methyl chlorosilane, phenyl chlorosilane, vinyl chlorosilane, amino chlorosilane, phenyl alkoxysilane, vinyl alkoxy silane, methyl alkoxy silane, aminoalkoxysilane, hydrogen base organoalkoxysilane, sulfonic group organoalkoxysilane.Alcoholic solution is the one in methyl alcohol, ethanol.
In step (2), preferred adjust ph is 3.
In step (2), selective hydrolysis 30min, then add the alcoholic solution of M chain link organosilicon end capping agent, cohydrolysis 90min, cohydrolysis temperature controls at 70 DEG C.
In step (2), the agent of M chain link organosilicon end capping is preferably 0.5: 1 with the mass ratio adding recessed soil at first.
10, the preparation method of recessed soil matrix MQ silicone resin as claimed in claim 1, it is characterized in that: in step (3), extraction agent is the one in benzene,toluene,xylene, silicone oil, dimethyl silicone oil.
Positively effect of the present invention is as follows:
1, the present invention have with fibrous nano silicon-dioxide be core, the MQ silicone resin nanostructure that is shell, there is the collaborative reinforcing effect of white carbon black and MQ silicone resin.
2, the nanometer nuclear shell nano-structure that has of the present invention, makes its dispersiveness better.
3, in stratum nucleare of the present invention, fibrous nano silicon-dioxide activates through soda acid, has higher specific surface area, thus has larger surface energy and stronger absorption property.
4, in stratum nucleare of the present invention, fibrous nano silicon-dioxide imparts the higher resistance toheat of product;
5, the present invention is with cheap recessed soil for raw material, and stratum nucleare is fibrous nano silicon-dioxide, has significant cost advantage.
Accompanying drawing explanation
Fig. 1 is scanning electron microscope (SEM) figure not adding recessed soil matrix MQ silicone resin.
Fig. 2 is scanning electron microscope (SEM) figure of recessed soil matrix MQ silicone resin prepared by the embodiment of the present invention 3.
Embodiment
The following examples describe in further detail of the present invention.
Embodiment 1:
1, the preparation of fibrous nano silicon-dioxide and waterglass mixture: recessed soil is distributed in sodium hydroxide solution, 24h is stirred at 100 DEG C, obtained fibrous nano silicon-dioxide and waterglass mixture, wherein the concentration of sodium hydroxide solution is 20mol/L, and the mass ratio of attapulgite and sodium hydroxide solution is 0.05: 1;
2, the preparation of recessed soil matrix MQ silicone resin dispersion liquid: under constantly stirring, fibrous nano silicon-dioxide and waterglass mixture is added in concentrated hydrochloric acid, adjust ph is 0.5, hydrolysis 1min, then add the ethanolic soln of hexamethyldisiloxane, cohydrolysis 120min, hexamethyldisiloxane is 1: 1 with the mass ratio adding recessed soil at first, cohydrolysis temperature controls at 100 DEG C, obtained recessed soil matrix MQ silicone resin dispersion liquid;
3, aftertreatment: extract with toluene, gets upper strata oil reservoir, washs to neutrality dry at 120 DEG C, obtains recessed soil matrix MQ silicone resin.
Embodiment 2:
1, the preparation of fibrous nano silicon-dioxide and waterglass mixture: recessed soil is distributed in potassium hydroxide solution, 0.5h is stirred at 20 DEG C, obtained fibrous nano silicon-dioxide and waterglass mixture, wherein the concentration of potassium hydroxide solution is 0.5mol/L, and the mass ratio of attapulgite and potassium hydroxide solution is 0.25: 1;
2, the preparation of recessed soil matrix MQ silicone resin dispersion liquid: under constantly stirring, fibrous nano silicon-dioxide and waterglass mixture is added in concentrated hydrochloric acid, adjust ph is 5, hydrolysis 60min, then add the methanol solution of trimethylchlorosilane, cohydrolysis 1min, trimethylchlorosilane is 0.01: 1 with the mass ratio adding recessed soil at first, cohydrolysis temperature controls at 20 DEG C, obtained recessed soil matrix MQ silicone resin dispersion liquid;
3, aftertreatment: extract with dimethylbenzene, gets upper strata oil reservoir, washs to neutrality dry at 60 DEG C, obtains recessed soil matrix MQ silicone resin.
Embodiment 3:
1, the preparation of fibrous nano silicon-dioxide and waterglass mixture: recessed soil is distributed in sodium hydroxide, 4h is stirred at 80 DEG C, obtained fibrous nano silicon-dioxide and waterglass mixture, wherein the concentration of sodium hydroxide solution is 10mol/L, and the mass ratio of attapulgite and alkali lye is 0.1: 1;
2, the preparation of recessed soil matrix MQ silicone resin dispersion liquid: under constantly stirring, fibrous nano silicon-dioxide and waterglass mixture is added in concentrated hydrochloric acid, adjust ph is 2, hydrolysis 15min, then add the ethanol solution of γ-aminopropyl triethoxysilane, cohydrolysis 60min, γ-aminopropyl triethoxysilane is 0.1: 1 with the mass ratio adding recessed soil at first, cohydrolysis temperature controls at 80 DEG C, obtained recessed soil matrix MQ silicone resin dispersion liquid;
3, aftertreatment: extract with silicone oil, gets upper strata oil reservoir, washs to neutrality dry at 80 DEG C, obtains recessed soil matrix MQ silicone resin.
Embodiment 4:
1, the preparation of fibrous nano silicon-dioxide and waterglass mixture: recessed soil is distributed in sodium hydroxide, 4h is stirred at 90 DEG C, obtained fibrous nano silicon-dioxide and waterglass mixture, wherein the concentration of sodium hydroxide solution is 15mol/L, and the mass ratio of attapulgite and alkali lye is 0.2: 1;
2, the preparation of recessed soil matrix MQ silicone resin dispersion liquid: under constantly stirring, fibrous nano silicon-dioxide and waterglass mixture is added in concentrated hydrochloric acid, adjust ph is 1, hydrolysis 30min, then add the ethanol solution of vinyltrimethoxy silane, cohydrolysis 30min, vinyltrimethoxy silane is 0.25: 1 with the mass ratio adding recessed soil at first, cohydrolysis temperature controls at 60 DEG C, obtained recessed soil matrix MQ silicone resin dispersion liquid;
3, aftertreatment: extract with dimethyl silicone oil, gets upper strata oil reservoir, washs to neutrality dry at 80 DEG C, obtains recessed soil matrix MQ silicone resin.
The performance of embodiment 5 recessed soil matrix MQ silicone resin of the present invention
Experiment basic recipe (part) is as follows: MVQ110-2,100; Filler, 50; A-151,2.5; Hydroxy silicon oil, 4; Two 25,1.5.Add in two roller mill successively by said sequence, mixing even taking-up sizing material.Thin-pass bottom sheet after back mixing evenly, pressing mold enters 25t vulcanizing press, carries out one step cure 10min at 170 DEG C, and pressure is 10Mpa, then 150 DEG C of maintenance 1h in baking oven, then is warming up to 200 DEG C of maintenance 2h.Then gained film is cut into standard sample of photo on sheet-punching machine, carries out performance test according to national standard.
Comparative example 1: MQ silicone resin prepared by water glass.Namely eliminate step 1 in embodiment 3, directly fibrous nano silicon-dioxide and waterglass mixture are changed to water glass, other are all identical with embodiment 3.
Test result is as shown in table 1:
Table 1 performance test results
The specific surface area of the recessed soil matrix MQ silicone resin as can be seen from Table 1 prepared by the present invention is comparatively large, and thermotolerance is comparatively large, possesses stronger reinforcing property to silicon rubber simultaneously, increases tensile strength, the tear strength of silicon rubber.
Although illustrate and describe embodiments of the invention, for the ordinary skill in the art, be appreciated that and can carry out multiple change, amendment, replacement and modification to these embodiments without departing from the principles and spirit of the present invention, scope of the present invention is by claims and equivalents thereof.
Claims (10)
1. a preparation method for recessed soil matrix MQ silicone resin, is characterized in that: the concrete steps of described preparation method are as follows:
(1) preparation of fibrous nano silicon-dioxide and waterglass mixture: recessed soil is distributed in alkali lye, 0.5-24h is stirred at 20-100 DEG C, obtained fibrous nano silicon-dioxide and waterglass mixture, wherein the concentration of alkali lye is 0.5-20mol/L, and the mass ratio of recessed soil and alkali lye is 0.05-0.25: 1;
(2) preparation of recessed soil matrix MQ silicone resin dispersion liquid: under constantly stirring, fibrous nano silicon-dioxide and waterglass mixture prepared by step (1) is added in concentrated hydrochloric acid, adjust ph is 0.5-5, hydrolysis 1-60min, then the alcoholic solution of M chain link organosilicon end capping agent is added, cohydrolysis 1-120min, the agent of M chain link organosilicon end capping is 0.01-1: 1 with the mass ratio adding recessed soil at first, cohydrolysis temperature controls at 20-100 DEG C, obtained recessed soil matrix MQ silicone resin dispersion liquid;
(3) aftertreatment: extract with extraction agent, gets upper strata oil reservoir, washs to neutrality dry at 60-120 DEG C, obtains recessed soil matrix MQ silicone resin.
2. the preparation method of recessed soil matrix MQ silicone resin as claimed in claim 1, it is characterized in that: in step (1), alkali lye is the one in sodium hydroxide, potassium hydroxide.
3. the preparation method of recessed soil matrix MQ silicone resin as claimed in claim 1, is characterized in that: in step (1), be distributed in alkali lye by recessed soil, at 60 DEG C, stir 12h.
4. the preparation method of recessed soil matrix MQ silicone resin as claimed in claim 1, is characterized in that: in step (1), and the concentration of alkali lye is 10mol/L, and the mass ratio of recessed soil and alkali lye is 0.15: 1.
5. the preparation method of recessed soil matrix MQ silicone resin as claimed in claim 1, it is characterized in that: in step (2), the agent of M chain link organosilicon end capping is the one in methyl chlorosilane, phenyl chlorosilane, vinyl chlorosilane, amino chlorosilane, phenyl alkoxysilane, vinyl alkoxy silane, methyl alkoxy silane, aminoalkoxysilane, hydrogen base organoalkoxysilane, sulfonic group organoalkoxysilane.
6. the preparation method of recessed soil matrix MQ silicone resin as claimed in claim 1, it is characterized in that: in step (2), alcoholic solution is the one in methyl alcohol, ethanol.
7. the preparation method of recessed soil matrix MQ silicone resin as claimed in claim 1, it is characterized in that: in step (2), adjust ph is 3.
8. the preparation method of recessed soil matrix MQ silicone resin as claimed in claim 1, is characterized in that: in step (2), and hydrolysis 30min, then add the alcoholic solution of M chain link organosilicon end capping agent, cohydrolysis 90min, cohydrolysis temperature controls at 70 DEG C.
9. the preparation method of recessed soil matrix MQ silicone resin as claimed in claim 1, is characterized in that: in step (2), and the agent of M chain link organosilicon end capping is 0.5: 1 with the mass ratio adding recessed soil at first.
10. the preparation method of recessed soil matrix MQ silicone resin as claimed in claim 1, it is characterized in that: in step (3), extraction agent is the one in benzene,toluene,xylene, silicone oil, dimethyl silicone oil.
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| CN107189442B (en) * | 2017-06-27 | 2020-05-19 | 淮阴工学院 | Modified methyl phenyl silicone resin based on nano attapulgite and preparation method thereof |
| CN108046839A (en) * | 2017-12-19 | 2018-05-18 | 罗洪梅 | A kind of recessed soil matrix porous ceramics of chemical modification and preparation method thereof |
| CN108239427B (en) * | 2017-12-19 | 2020-04-17 | 青岛海源实业有限公司 | Attapulgite nano-fluid based geopolymer fluorescent paint and preparation method thereof |
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| CN102875811A (en) * | 2011-07-12 | 2013-01-16 | 常州化学研究所 | Preparation method for phenyl vinyl MQ silicone resin |
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