CN103965478A - Method for preparing attapulgite-based MQ organic silicon resin - Google Patents
Method for preparing attapulgite-based MQ organic silicon resin Download PDFInfo
- Publication number
- CN103965478A CN103965478A CN201410196378.3A CN201410196378A CN103965478A CN 103965478 A CN103965478 A CN 103965478A CN 201410196378 A CN201410196378 A CN 201410196378A CN 103965478 A CN103965478 A CN 103965478A
- Authority
- CN
- China
- Prior art keywords
- recessed soil
- silicone resin
- preparation
- soil matrix
- alkali lye
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 229960000892 attapulgite Drugs 0.000 title abstract description 10
- 229910052625 palygorskite Inorganic materials 0.000 title abstract description 10
- 238000000034 method Methods 0.000 title abstract description 8
- 229920005989 resin Polymers 0.000 title abstract description 7
- 239000011347 resin Substances 0.000 title abstract description 7
- 229910052710 silicon Inorganic materials 0.000 title abstract description 6
- 239000010703 silicon Substances 0.000 title abstract description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title abstract 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 52
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 23
- 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
- 239000002689 soil Substances 0.000 claims description 62
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 59
- 229920002050 silicone resin Polymers 0.000 claims description 49
- 239000011159 matrix material Substances 0.000 claims description 39
- 238000002360 preparation method Methods 0.000 claims description 28
- 239000000377 silicon dioxide Substances 0.000 claims description 25
- 235000012239 silicon dioxide Nutrition 0.000 claims description 25
- 229960001866 silicon dioxide Drugs 0.000 claims description 25
- 235000019353 potassium silicate Nutrition 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- -1 octadecyloxy phenyl TMOS Chemical compound 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
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 230000001105 regulatory effect Effects 0.000 claims description 8
- 230000007062 hydrolysis Effects 0.000 claims description 7
- 238000006460 hydrolysis reaction Methods 0.000 claims description 7
- 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
- 229910000077 silane Inorganic materials 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
- 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
- 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
- 239000002253 acid Substances 0.000 abstract description 3
- 230000003014 reinforcing effect Effects 0.000 abstract description 3
- 238000005282 brightening Methods 0.000 abstract description 2
- 239000006229 carbon black Substances 0.000 abstract description 2
- 239000000835 fiber Substances 0.000 abstract description 2
- 239000004115 Sodium Silicate Substances 0.000 abstract 1
- 239000003153 chemical reaction reagent Substances 0.000 abstract 1
- 239000005543 nano-size silicon particle Substances 0.000 abstract 1
- 239000012779 reinforcing material Substances 0.000 abstract 1
- 229910052911 sodium silicate Inorganic materials 0.000 abstract 1
- 239000004094 surface-active agent Substances 0.000 abstract 1
- 230000002195 synergetic effect Effects 0.000 abstract 1
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 description 6
- 239000003921 oil Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 3
- 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
- 239000000463 material Substances 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
- 239000011258 core-shell material Substances 0.000 description 1
- 239000013530 defoamer Substances 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
- 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
- 239000012756 surface treatment agent Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a method for preparing an attapulgite-based MQ organic silicon resin. The resin is prepared by the following steps of firstly, preparing the attapulgite into a mixture of fiber nanosilicon dioxide and sodium silicate in the presence of alkali, subsequently, in the presence of acid and M chain link organic silicon end-capping reagent, forming a dispersion liquid of the attapulgite-based MQ organic silicon resin, and treating to obtain a product. The resin has a synergic reinforcing effect on white carbon black and the MQ organic silicon resin, is relatively good in dispersity, large in specific surface area, good in thermal resistance and low in cost, and can be widely applied to fields such as surfactants, reinforcing materials, tackifiers, demolding agents, anti-sticking agents, brightening agents, scratch resisting agents and the like.
Description
Technical field
The present invention relates to the preparing technical field of silicone resin, relate in particular 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 that has four functionality siloxanes polycondensation chain links (Q) and single functionality siloxane unit (M) to form, its molar mass is generally 1000～8000, character and the range of application of the when structures shape resin of the amount of M chain link and Q chain link in molecular structure.MQ silicone resin is mainly used in following field: the one, and surface treatment agent, as bonding in organic pressure-sensitive gel, mobile phone key glue, epoxies adhesive surface etc.; The 2nd, supporting material, is applied in the joint sealant of RTV glue, HTV glue, add-on type liquid silicon rubber, hot sulfurization rubber, semiconductor element etc.; The 3rd, tackifier, for seal gum and silicone resin coating; The 4th, 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 silicon ester method 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 make low M/Q product, obtained paying close attention to widely.
Recessed soil is the abbreviation of attapulgite, also claims 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 in 20nm left and right, and length can reach several microns, has flourishing specific surface area, abundant at China's reserves, cheap.Recessed soil is under alkali effect, can form the mixture of fibrous nano silicon-dioxide and water glass, then under the effect of acid and the agent of M chain link organosilicon end capping, form MQ silicone resin (the being recessed soil matrix MQ silicone resin) dispersion liquid that is evenly being coated 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 ofly 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 preparation method's of recessed soil matrix MQ silicone resin of the present invention concrete steps are as follows:
(1) preparation of fibrous nano silicon-dioxide and waterglass mixture: recessed soil is distributed in alkali lye, at 20-100 DEG C, stir 0.5-24h, make 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, the fibrous nano silicon-dioxide and the waterglass mixture that in concentrated hydrochloric acid, add step (1) to prepare, regulating pH value is 0.5-5, hydrolysis 1-60min, then add the alcoholic solution of M chain link organosilicon end capping agent, cohydrolysis 1-120min, the agent of M chain link organosilicon end capping is 0.01-1 with adding the mass ratio of recessed soil at first: 1, cohydrolysis temperature is controlled at 20-100 DEG C, makes recessed soil matrix MQ silicone resin dispersion liquid;
(3) aftertreatment: extract with extraction agent, get upper strata oil reservoir, wash to dry at 60-120 DEG C after neutrality, obtain 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), preferably the concentration of 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, octadecyloxy phenyl TMOS, vinyl alkoxy silane, methyl alkoxy silane, aminoalkoxy silane, hydrogen base organoalkoxysilane, sulfonic group organoalkoxysilane.Alcoholic solution is the one in methyl alcohol, ethanol.
In step (2), preferably regulating pH value is 3.
In step (2), selective hydrolysis 30min, then adds the alcoholic solution of M chain link organosilicon end capping agent, cohydrolysis 90min, and cohydrolysis temperature is controlled at 70 DEG C.
In step (2), the agent of M chain link organosilicon end capping with add the mass ratio of recessed soil to be preferably 0.5: 1 at first.
10, the preparation method of recessed soil matrix MQ silicone resin as claimed in claim 1, 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 has taking fibrous nano silicon-dioxide as core, MQ silicone resin is the nanostructure of shell, has the collaborative reinforcing effect of white carbon black and MQ silicone resin.
2, the core-shell nano structure that the present invention has, 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, thereby has larger surface energy and stronger absorption property.
4, in stratum nucleare of the present invention, fibrous nano silicon-dioxide has given product higher resistance toheat;
5, the present invention is taking cheap recessed soil as raw material, and stratum nucleare is fibrous nano silicon-dioxide, has significant cost advantage.
Brief description of the drawings
Fig. 1 is scanning electron microscope (SEM) figure that does not add recessed soil matrix MQ silicone resin.
Fig. 2 is scanning electron microscope (SEM) figure of the recessed soil matrix MQ silicone resin prepared of the embodiment of the present invention 3.
Embodiment
The following examples are to 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, at 100 DEG C, stir 24h, make 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, in concentrated hydrochloric acid, add fibrous nano silicon-dioxide and waterglass mixture, regulating pH value is 0.5, hydrolysis 1min, then add the ethanolic soln of hexamethyldisiloxane, cohydrolysis 120min, hexamethyldisiloxane is 1: 1 with adding the mass ratio of recessed soil at first, cohydrolysis temperature is controlled at 100 DEG C, makes recessed soil matrix MQ silicone resin dispersion liquid;
3, aftertreatment: extract with toluene, get upper strata oil reservoir, wash to dry at 120 DEG C after neutrality, obtain 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, at 20 DEG C, stir 0.5h, make 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, in concentrated hydrochloric acid, add fibrous nano silicon-dioxide and waterglass mixture, regulating pH value is 5, hydrolysis 60min, then add the methanol solution of trimethylchlorosilane, cohydrolysis 1min, trimethylchlorosilane is 0.01: 1 with adding the mass ratio of recessed soil at first, cohydrolysis temperature is controlled at 20 DEG C, makes recessed soil matrix MQ silicone resin dispersion liquid;
3, aftertreatment: extract with dimethylbenzene, get upper strata oil reservoir, wash to dry at 60 DEG C after neutrality, obtain 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, at 80 DEG C, stir 4h, make 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, in concentrated hydrochloric acid, add fibrous nano silicon-dioxide and waterglass mixture, regulating pH value is 2, hydrolysis 15min, then add the ethanol solution of γ-aminopropyl triethoxysilane, cohydrolysis 60min, γ-aminopropyl triethoxysilane is 0.1: 1 with adding the mass ratio of recessed soil at first, cohydrolysis temperature is controlled at 80 DEG C, makes recessed soil matrix MQ silicone resin dispersion liquid;
3, aftertreatment: extract with silicone oil, get upper strata oil reservoir, wash to dry at 80 DEG C after neutrality, obtain 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, at 90 DEG C, stir 4h, make 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, in concentrated hydrochloric acid, add fibrous nano silicon-dioxide and waterglass mixture, regulating pH value is 1, hydrolysis 30min, then add the ethanol solution of vinyltrimethoxy silane, cohydrolysis 30min, vinyltrimethoxy silane is 0.25: 1 with adding the mass ratio of recessed soil at first, cohydrolysis temperature is controlled at 60 DEG C, makes recessed soil matrix MQ silicone resin dispersion liquid;
3, aftertreatment: extract with dimethyl silicone oil, get upper strata oil reservoir, wash to dry at 80 DEG C after neutrality, obtain 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 successively in two roller mills mixing even taking-up sizing material by said sequence.Sheet under thin-pass 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 be 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.In embodiment 3, saved step 1, directly fibrous nano silicon-dioxide and waterglass mixture have been 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 prepared recessed soil matrix MQ silicone resin of the present invention is larger as can be seen from Table 1, and thermotolerance is larger, silicon rubber is possessed to stronger reinforcing property simultaneously, increases tensile strength, the tear strength of silicon rubber.
Although illustrated and described embodiments of the invention, for the ordinary skill in the art, be appreciated that without departing from the principles and spirit of the present invention and can carry out multiple variation, amendment, replacement and modification to these embodiment, scope of the present invention is limited by claims and equivalent thereof.
Claims (10)
1. a preparation method for recessed soil matrix MQ silicone resin, is characterized in that: described preparation method's concrete steps are as follows:
(1) preparation of fibrous nano silicon-dioxide and waterglass mixture: recessed soil is distributed in alkali lye, at 20-100 DEG C, stir 0.5-24h, make 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, the fibrous nano silicon-dioxide and the waterglass mixture that in concentrated hydrochloric acid, add step (1) to prepare, regulating pH value is 0.5-5, hydrolysis 1-60min, then add the alcoholic solution of M chain link organosilicon end capping agent, cohydrolysis 1-120min, the agent of M chain link organosilicon end capping is 0.01-1 with adding the mass ratio of recessed soil at first: 1, cohydrolysis temperature is controlled at 20-100 DEG C, makes recessed soil matrix MQ silicone resin dispersion liquid;
(3) aftertreatment: extract with extraction agent, get upper strata oil reservoir, wash to dry at 60-120 DEG C after neutrality, obtain recessed soil matrix MQ silicone resin.
2. the preparation method of recessed soil matrix MQ silicone resin as claimed in claim 1, 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), recessed soil is distributed in alkali lye, at 60 DEG C, stirs 12h.
4. the preparation method of recessed soil matrix MQ silicone resin as claimed in claim 1, is characterized in that: in step (1), 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, octadecyloxy phenyl TMOS, vinyl alkoxy silane, methyl alkoxy silane, aminoalkoxy silane, hydrogen base organoalkoxysilane, sulfonic group organoalkoxysilane.
6. the preparation method of recessed soil matrix MQ silicone resin as claimed in claim 1, 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, is characterized in that: in step (2), regulating pH value 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), is hydrolyzed 30min, then adds the alcoholic solution of M chain link organosilicon end capping agent, and cohydrolysis 90min, cohydrolysis temperature is controlled 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), the agent of M chain link organosilicon end capping is 0.5: 1 with adding the mass ratio of recessed soil at first.
10. the preparation method of recessed soil matrix MQ silicone resin as claimed in claim 1, is characterized in that: in step (3), extraction agent is the one in benzene,toluene,xylene, silicone oil, dimethyl silicone oil.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410196378.3A CN103965478B (en) | 2014-05-12 | 2014-05-12 | A kind of preparation method of recessed soil matrix MQ silicone resin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410196378.3A CN103965478B (en) | 2014-05-12 | 2014-05-12 | A kind of preparation method of recessed soil matrix MQ silicone resin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103965478A true CN103965478A (en) | 2014-08-06 |
| CN103965478B CN103965478B (en) | 2016-04-27 |
Family
ID=51235510
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410196378.3A Active CN103965478B (en) | 2014-05-12 | 2014-05-12 | A kind of preparation method of recessed soil matrix MQ silicone resin |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103965478B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107189442A (en) * | 2017-06-27 | 2017-09-22 | 淮阴工学院 | A kind of modifying methylphenyl silicone resin based on nano concave earth 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 |
| CN108239427A (en) * | 2017-12-19 | 2018-07-03 | 成英 | A kind of recessed native nano-fluid base geological polymer fluorescent paint and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101323667A (en) * | 2008-06-24 | 2008-12-17 | 杭州师范大学 | Preparation of methyl vinyl MQ resin for LED encapsulated strengthening |
| CN101899157A (en) * | 2010-07-22 | 2010-12-01 | 南昌大学 | Method for preparing MQ silicone resins |
| CN102875811A (en) * | 2011-07-12 | 2013-01-16 | 常州化学研究所 | Preparation method for phenyl vinyl MQ silicone resin |
| CN103436035A (en) * | 2013-08-19 | 2013-12-11 | 深圳市华创威实业有限公司 | Novel silicon resin |
-
2014
- 2014-05-12 CN CN201410196378.3A patent/CN103965478B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101323667A (en) * | 2008-06-24 | 2008-12-17 | 杭州师范大学 | Preparation of methyl vinyl MQ resin for LED encapsulated strengthening |
| CN101899157A (en) * | 2010-07-22 | 2010-12-01 | 南昌大学 | Method for preparing MQ silicone resins |
| CN102875811A (en) * | 2011-07-12 | 2013-01-16 | 常州化学研究所 | Preparation method for phenyl vinyl MQ silicone resin |
| CN103436035A (en) * | 2013-08-19 | 2013-12-11 | 深圳市华创威实业有限公司 | Novel silicon resin |
Non-Patent Citations (1)
| Title |
|---|
| 王国建，谢晶: "《水玻璃有机化法制备MQ硅树脂的研究》", 《建筑材料学报》, vol. 7, no. 3, 30 September 2004 (2004-09-30), pages 299 - 305 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107189442A (en) * | 2017-06-27 | 2017-09-22 | 淮阴工学院 | A kind of modifying methylphenyl silicone resin based on nano concave earth 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 |
| CN108239427A (en) * | 2017-12-19 | 2018-07-03 | 成英 | A kind of recessed native nano-fluid base geological polymer fluorescent paint 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103965478B (en) | 2016-04-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108658576B (en) | Preparation method of composite silica aerogel felt | |
| CN104017534B (en) | A kind of transparent organic silicon LED lamp bar joint sealant and preparation method thereof | |
| CN106336469B (en) | A kind of synthetic method of the selfreparing elastomeric material based on gutta-percha | |
| CN103965478B (en) | A kind of preparation method of recessed soil matrix MQ silicone resin | |
| CN103160129B (en) | Mold rubber and preparation method thereof | |
| CN104892942A (en) | Tackifier for addition-type organic silicon rubber and preparation method thereof | |
| CN104017519B (en) | Glued board tackiness agent and preparation method thereof | |
| CN103044683A (en) | Modified MQ silicone resin and preparation method thereof | |
| CN104194562B (en) | A kind of normal temperature cure monocomponent nanocomposite composite aqueous paint preparation method | |
| CN103897398A (en) | Silica sol reinforced water-based organic silicone elastomer as well as preparation method and application thereof | |
| CN106700657A (en) | Surface treatment method of high-temperature-resistant nano calcium carbonate for silicone adhesives | |
| CN103173178B (en) | Organic silicon modified polyether adhesive and preparation method thereof | |
| CN103865474A (en) | Preparation method of transparent pasty alcohol type organosilicone sealant | |
| CN106634770A (en) | A transparent type one-component silane-modified polyether sealant and a preparing method thereof | |
| CN105297542A (en) | Method for irradiating and curing release paper isolation layer for leather | |
| CN107987311A (en) | A kind of preparation method of hydrophobicity melamine sponge enhancing polysilsesquioxane composite aerogel | |
| CN107523259A (en) | A kind of preparation of organosilicon sealant coupling agent modified α 570 | |
| CN103173182B (en) | Organic silicon modified polyurethane sealant and preparation method thereof | |
| CN106047276A (en) | High-hardness high-adhesion modified high-heat conduction LED organosilicon package glue and preparation method thereof | |
| CN104449353A (en) | Ceramic paint for decoration walls of subway stations and preparation method of ceramic paint | |
| CN104130738A (en) | Acidic silicone sealant with good bonding performance on stainless steel, and preparation method thereof | |
| CN103788660A (en) | Glass fiber/ epoxy resin hybrid modified silicone rubber mold rubber and preparation method thereof | |
| CN110283426B (en) | Bio-based degradable starch filled epoxy resin composite material and preparation method thereof | |
| CN107573507A (en) | A kind of preparation method of big particle diameter polysiloxanes microballoon | |
| CN105348958B (en) | A kind of water-based dumb light coating varnish of two-component organic inorganic hybridization and preparation method thereof and construction method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C53 | Correction of patent of invention or patent application | ||
| CB02 | Change of applicant information |
Address after: High tech Zone Guang River Road 272400 Shandong Jining City 16, Jining city quality inspection by quality inspection center of Shandong Applicant after: Zhang Guoqing Address before: 272401 Shandong city of Jining province Jiaxiang county Zhang Xiang Zhang Tun Yueguan No. 132 Applicant before: Zhang Guoqing |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| CB03 | Change of inventor or designer information |
Inventor after: Zhang Guihua Inventor after: Yang Anjing Inventor after: Kang Jiaojiao Inventor after: Lv Guizhi Inventor after: Liu Yuanyuan Inventor after: Zhang Guoqing Inventor before: Zhang Yali Inventor before: Yin Zhenyan Inventor before: Zhang Guoqing Inventor before: Zeng Yongbin Inventor before: Zhang Qingjie |
|
| COR | Change of bibliographic data | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20160303 Address after: 272400 junction of Torch Road and electromechanical two road, Jining hi tech Zone, Shandong Applicant after: SHANDONG CAYON TESTING TECHNOLOGY Co.,Ltd. Address before: High tech Zone Guang River Road 272400 Shandong Jining City 16, Jining city quality inspection by quality inspection center of Shandong Applicant before: Zhang Guoqing |
|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| DD01 | Delivery of document by public notice | ||
| DD01 | Delivery of document by public notice |
Addressee: SHANDONG CAYON TESTING TECHNOLOGY Co.,Ltd. Document name: Notification to Pay the Fees |
|
| CP03 | Change of name, title or address | ||
| CP03 | Change of name, title or address |
Address after: No. 18, Taibailou West Road, Rencheng District, Jining City, Shandong Province, 2007 Patentee after: Shandong Jiayuan Testing Technology Co.,Ltd. Address before: 272400 north of the intersection of Huoju road and electromechanical Second Road, high tech Zone, Jining City, Shandong Province Patentee before: SHANDONG CAYON TESTING TECHNOLOGY Co.,Ltd. |