CN117430834A - Preparation method of organomagnesium doped polysilsesquioxane microsphere - Google Patents
Preparation method of organomagnesium doped polysilsesquioxane microsphere Download PDFInfo
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- CN117430834A CN117430834A CN202311458013.9A CN202311458013A CN117430834A CN 117430834 A CN117430834 A CN 117430834A CN 202311458013 A CN202311458013 A CN 202311458013A CN 117430834 A CN117430834 A CN 117430834A
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- polysilsesquioxane
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- 239000004005 microsphere Substances 0.000 title claims abstract description 45
- 229920000734 polysilsesquioxane polymer Polymers 0.000 title claims abstract description 37
- 125000002734 organomagnesium group Chemical group 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 31
- 239000011777 magnesium Substances 0.000 claims abstract description 31
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 24
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims abstract description 24
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 12
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 12
- DCQBZYNUSLHVJC-UHFFFAOYSA-N 3-triethoxysilylpropane-1-thiol Chemical compound CCO[Si](OCC)(OCC)CCCS DCQBZYNUSLHVJC-UHFFFAOYSA-N 0.000 claims abstract description 11
- JAUWOQLHLFMTON-UHFFFAOYSA-M magnesium;but-1-ene;bromide Chemical compound [Mg+2].[Br-].[CH2-]CC=C JAUWOQLHLFMTON-UHFFFAOYSA-M 0.000 claims abstract description 10
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 58
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical group CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 30
- 238000006243 chemical reaction Methods 0.000 claims description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 26
- 238000003756 stirring Methods 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 17
- 238000003760 magnetic stirring Methods 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- 239000000376 reactant Substances 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 6
- 239000003054 catalyst Substances 0.000 claims description 5
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 4
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 125000003944 tolyl group Chemical group 0.000 claims description 2
- 239000008096 xylene Substances 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 abstract 1
- -1 polysiloxane Polymers 0.000 description 12
- 239000002245 particle Substances 0.000 description 9
- 238000000149 argon plasma sintering Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 230000007935 neutral effect Effects 0.000 description 4
- 229920001296 polysiloxane Polymers 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 229920003217 poly(methylsilsesquioxane) Polymers 0.000 description 2
- 238000006068 polycondensation reaction Methods 0.000 description 2
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- WBIQQQGBSDOWNP-UHFFFAOYSA-N 2-dodecylbenzenesulfonic acid Chemical compound CCCCCCCCCCCCC1=CC=CC=C1S(O)(=O)=O WBIQQQGBSDOWNP-UHFFFAOYSA-N 0.000 description 1
- UNIYDALVXFPINL-UHFFFAOYSA-N 3-(2-methylprop-2-enoyloxy)propylsilicon Chemical compound CC(=C)C(=O)OCCC[Si] UNIYDALVXFPINL-UHFFFAOYSA-N 0.000 description 1
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 229940060296 dodecylbenzenesulfonic acid Drugs 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/12—Powdering or granulating
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
- C08J2383/08—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen, and oxygen
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Silicon Polymers (AREA)
Abstract
The invention relates to the technical field of polysilsesquioxane microspheres, in particular to a preparation method of an organomagnesium doped polysilsesquioxane microsphere; the invention provides a preparation method of an organomagnesium doped polysilsesquioxane microsphere, which is characterized in that mercaptopropyl triethoxysilane, 3-butenyl magnesium bromide and tetraallyl silicate are used for preparing magnesium-based siloxane, then the magnesium-based siloxane is stirred and reacted with hydrochloric acid and ammonia water, and the organomagnesium modified polysilsesquioxane microsphere is obtained after drying.
Description
Technical Field
The invention relates to the technical field of polysilsesquioxane microspheres, in particular to a preparation method of an organomagnesium doped polysilsesquioxane microsphere.
Background
Polysilsesquioxane microspheres are typically prepared from alkoxysilane and deionized water by hydrolysis-polycondensation. The common silicone resin microsphere is mainly polysilsesquioxane and takes trimethoxysilane as a raw material. The trifunctional silane has a density smaller than that of water and is in two mutually incompatible phases, so that hydrolysis reaction is carried out on the interface to generate silanol which is soluble in water, and the silanol is subjected to polycondensation reaction under the action of a base catalyst to generate polysilsesquioxane.
CN201410132209.3 relates to a polysiloxane microsphere with core-shell structure and its preparation method. The polysiloxane microsphere comprises a core and a shell layer wrapping the core, wherein the absolute value of the refractive index difference between the core and the shell layer is 0.01-0.12; the particle size of the microsphere is 0.1-50 mu m, and the particle size of the core is 20-70% of the particle size of the polysiloxane microsphere. The polysiloxane microsphere disclosed by the invention can be used as a light dispersing agent to be applied to diffusion materials such as LED illumination and LCD backlight sources, and has high light transmittance and good diffusion effect.
CN201410146936.5 discloses a preparation method of polymethylsilsesquioxane light scattering microsphere. The invention evenly mixes methyltrialkoxysilane, methacryloxypropyl silane and dodecylbenzene sulfonic acid, and then drops the mixture into water for reaction at 20-40 ℃; adding an alkaline solution to adjust the pH to 8.5-9.5, heating to 60-80 ℃, adding methyl methacrylate, swelling, dripping an initiator aqueous solution, reacting, cooling to room temperature, stirring, dripping ethanol until precipitation is separated out, filtering the obtained mixed solution, washing filter residues with water, and drying the filter residues at 70-90 ℃ to obtain the polymethylsilsesquioxane light scattering microspheres; the microsphere is added into transparent resin PC, has light scattering effect, has good compatibility with PC matrix, and does not affect other excellent impact toughness of PC basically while playing the light scattering effect. The preparation method adopts water as a solvent, is environment-friendly, has low cost and has extremely strong development potential.
The existing literature has complicated operation, easy environmental pollution and less reports on how to control the particle size of polysilsesquioxane microspheres, and the particle size is uneven, the pore size is not adjustable, and the chemical stability and the mechanical strength are poor based on the fact that the particle size needs to be further optimized.
Disclosure of Invention
The invention discloses a preparation method of an organomagnesium doped polysilsesquioxane microsphere, and belongs to the technical field of polysilsesquioxane microspheres. The modified polysilsesquioxane microsphere prepared by the invention has uniform particle size, adjustable pore diameter, high chemical stability and high mechanical strength.
The preparation process of organic magnesium doped polysilsesquioxane microsphere includes the following steps:
1000-1500 parts of deionized water, 1-5 parts of hydrochloric acid are added into a reaction kettle to adjust the pH, stirring is started after cooling, 15-25 parts of magnesium-based siloxane is added to react for 1-4 hours, 3-10 parts of ammonia water is added to adjust the pH, stirring is performed for 7-12 hours, then reactants are centrifuged, water washing is performed to neutrality, and drying is performed to obtain the organomagnesium modified polysilsesquioxane microsphere.
Further, the concentration of the hydrochloric acid is 5-12%, and the pH value is adjusted to be 4.8-6.0;
further, the temperature is reduced to 5-20 ℃;
further, the stirring is magnetic stirring, and the stirring speed is 180-300r/min;
further, the preparation method of the magnesium-based siloxane comprises the following steps:
adding 10-25 parts of mercaptopropyl triethoxysilane, 0.1-0.7 part of 3-butenyl magnesium bromide, 5-16 parts of tetra-allyl silicate, 1-5 parts of catalyst and 100-200 parts of organic solvent into a reaction kettle, stirring for reaction, and distilling under reduced pressure to remove toluene to obtain magnesium-based siloxane;
further, the catalyst is triethylamine;
further, the organic solvent is toluene, xylene or chloroform;
further, the reaction temperature is 80-90 ℃ and the reaction time is 4-8 hours;
further, the concentration of the ammonia water is 8-16%, and the pH is adjusted to 7.8-10.8.
The technical effects are as follows:
the modified polysilsesquioxane microsphere prepared by the method has the excellent performances of uniform particle size, adjustable pore diameter, high chemical stability and high mechanical strength.
Drawings
FIG. 1 is a scanning electron micrograph of an organomagnesium doped polysilsesquioxane microsphere.
Detailed Description
The invention is further illustrated by the following examples:
example 1
10g of mercaptopropyl triethoxysilane, 0.1g of 3-butenyl magnesium bromide, 5g of tetra allyl silicate, 1g of triethylamine and 100g of toluene are added into a reaction kettle to react for 6 hours under stirring at 80 ℃, and toluene is distilled off under reduced pressure to obtain magnesium-based siloxane.
1000g of deionized water is added into a reaction kettle, hydrochloric acid is added to adjust the pH to 5.5, the temperature is reduced to 15 ℃, magnetic stirring is started, the rotating speed is 200r/min, 15g of magnesium-based siloxane is added to react for 2 hours, ammonia water is added to adjust the pH to 7.8, magnetic stirring is performed, the reaction is performed for 7 hours, the reactants are centrifuged, water washing is performed to neutrality, and the organic magnesium modified polysilsesquioxane microsphere is obtained after drying.
Example 2
12g of mercaptopropyl triethoxysilane, 0.3g of 3-butenyl magnesium bromide, 8g of tetra allyl silicate, 2g of triethylamine and 120g of toluene are added into a reaction kettle to react for 8 hours under stirring at 80 ℃, and toluene is distilled off under reduced pressure to obtain magnesium-based siloxane.
1000g of deionized water is added into a reaction kettle, hydrochloric acid is added to adjust the pH to 5.5, the temperature is reduced to 12 ℃, magnetic stirring is started, the rotating speed is 200r/min, 18g of magnesium-based siloxane is added to react for 3 hours, ammonia water is added to adjust the pH to 8.5, magnetic stirring is performed, the reaction is performed for 9 hours, the reactants are centrifuged, water washing is performed to neutrality, and the organic magnesium modified polysilsesquioxane microsphere is obtained after drying.
Example 3
16g of mercaptopropyl triethoxysilane, 0.5g of 3-butenyl magnesium bromide, 12g of tetra allyl silicate, 3g of triethylamine and 150g of toluene are added into a reaction kettle to react for 4 hours under stirring at 85 ℃, and toluene is distilled off under reduced pressure to obtain magnesium-based siloxane.
1000g of deionized water is added into a reaction kettle, hydrochloric acid is added to adjust the pH to 5.0, the temperature is reduced to 10 ℃, magnetic stirring is started, the rotating speed is 200r/min, 20g of magnesium-based siloxane is added to react for 3 hours, ammonia water is added to adjust the pH to 8.9, magnetic stirring is performed, the reaction is performed for 8 hours, the reactants are centrifuged, water washing is performed to neutrality, and the organic magnesium modified polysilsesquioxane microsphere is obtained after drying.
Example 4
20g of mercaptopropyl triethoxysilane, 0.5g of 3-butenyl magnesium bromide, 12g of tetra allyl silicate, 3g of triethylamine and 160g of toluene are added into a reaction kettle to react for 6 hours under stirring at 85 ℃, and toluene is distilled off under reduced pressure to obtain magnesium-based siloxane.
Adding 1200g of deionized water into a reaction kettle, adding hydrochloric acid to adjust the pH to 4.8, cooling to 10 ℃, opening magnetic stirring at the rotating speed of 300r/min, adding 15g of magnesium-based siloxane, reacting for 2 hours, adding ammonia water to adjust the pH to 7.8, magnetically stirring, reacting for 10 hours, centrifuging the reactant, washing with water to be neutral, and drying to obtain the organomagnesium modified polysilsesquioxane microsphere.
Example 5
24g of mercaptopropyl triethoxysilane, 0.6g of 3-butenyl magnesium bromide, 14g of tetra allyl silicate, 4g of triethylamine and 180g of toluene are added into a reaction kettle to react for 6 hours under stirring at 90 ℃, and toluene is distilled off under reduced pressure to obtain magnesium-based siloxane.
Adding 1500g of deionized water into a reaction kettle, adding hydrochloric acid to adjust the pH to 4.8, cooling to 8 ℃, opening magnetic stirring at the rotating speed of 300r/min, adding 22g of magnesium-based siloxane, reacting for 4 hours, adding ammonia water to adjust the pH to 9.8, magnetically stirring, reacting for 12 hours, centrifuging the reactant, washing with water to be neutral, and drying to obtain the organomagnesium modified polysilsesquioxane microsphere.
Example 6
25g of mercaptopropyl triethoxysilane, 0.7g of 3-butenyl magnesium bromide, 16g of tetra allyl silicate, 5g of triethylamine and 200g of toluene are added into a reaction kettle to react for 8 hours under stirring at 90 ℃, and toluene is distilled off under reduced pressure to obtain magnesium-based siloxane.
Adding 1500g of deionized water into a reaction kettle, adding hydrochloric acid to adjust the pH to 4.8, cooling to 5 ℃, opening magnetic stirring at the rotating speed of 300r/min, adding 15g of magnesium-based siloxane, reacting for 4 hours, adding ammonia water to adjust the pH to 10.8, reacting for 10 hours at the stirring speed, centrifuging the reactant, washing with water to be neutral, and drying to obtain the organomagnesium modified polysilsesquioxane microsphere.
Comparative example 1
10g of mercaptopropyl triethoxysilane, 0.1g of 3-butenyl magnesium bromide, 5g of tetra allyl silicate, 1g of triethylamine and 100g of toluene are added into a reaction kettle to react for 6 hours under stirring at 80 ℃, and toluene is distilled off under reduced pressure to obtain magnesium-based siloxane.
1000g of deionized water is added into a reaction kettle, magnetic stirring is started, the rotating speed is 200r/min, 15g of magnesium-based siloxane is added, the reaction is carried out for 2 hours, the reactants are centrifuged, water is washed to be neutral, and the organic magnesium modified polysilsesquioxane microsphere is obtained after drying.
Comparative example 2
10g of mercaptopropyl triethoxysilane, 5g of tetra allyl silicate, 1g of triethylamine and 100g of toluene are added into a reaction kettle to react for 6 hours under stirring at 80 ℃, and toluene is distilled off under reduced pressure to obtain magnesium-based siloxane.
1000g of deionized water is added into a reaction kettle, hydrochloric acid is added to adjust the pH to 5.5, the temperature is reduced to 15 ℃, magnetic stirring is started, the rotating speed is 200r/min, 15g of magnesium-based siloxane is added to react for 2 hours, ammonia water is added to adjust the pH to 7.8, magnetic stirring is performed, the reaction is performed for 7 hours, the reactants are centrifuged, water washing is performed to neutrality, and the organic magnesium modified polysilsesquioxane microsphere is obtained after drying.
Observing the shape and the particle size of the microspheres by SEM; performing a cantilever beam notch impact strength test according to GB/T1843-2002; tensile property testing was performed with reference to GB/T1040-1992;
the results of the performance tests for all of the above examples and comparative examples are shown in the following table:
Claims (9)
1. the preparation process of organic magnesium doped polysilsesquioxane microsphere includes the following steps:
1000-1500 parts of deionized water, 1-5 parts of hydrochloric acid are added into a reaction kettle to adjust the pH, stirring is started after cooling, 15-25 parts of magnesium-based siloxane is added to react for 1-4 hours, 3-10 parts of ammonia water is added to adjust the pH, stirring is performed for 7-12 hours, then reactants are centrifuged, water washing is performed to neutrality, and drying is performed to obtain the organomagnesium modified polysilsesquioxane microsphere.
2. The method for preparing the organomagnesium doped polysilsesquioxane microsphere according to claim 1, wherein the method comprises the following steps: the concentration of the hydrochloric acid is 5-12%, and the pH value is adjusted to be 4.8-6.0.
3. The method for preparing the organomagnesium doped polysilsesquioxane microsphere according to claim 1, wherein the method comprises the following steps: the temperature is reduced to 5-20 ℃.
4. The method for preparing the organomagnesium doped polysilsesquioxane microsphere according to claim 1, wherein the method comprises the following steps: the stirring is magnetic stirring, and the stirring rotating speed is 180-300r/min.
5. The method for preparing the organomagnesium doped polysilsesquioxane microsphere according to claim 1, wherein the method comprises the following steps: the preparation method of the magnesium-based siloxane comprises the following steps:
10-25 parts of mercaptopropyl triethoxysilane, 0.1-0.7 part of 3-butenyl magnesium bromide, 5-16 parts of tetra-allyl silicate, 1-5 parts of catalyst and 100-200 parts of organic solvent are added into a reaction kettle according to parts by weight, stirred for reaction, and toluene is distilled off under reduced pressure to obtain the magnesium-based siloxane.
6. The method for preparing the organomagnesium doped polysilsesquioxane microsphere according to claim 5, wherein the method comprises the following steps: the catalyst is triethylamine.
7. The method for preparing the organomagnesium doped polysilsesquioxane microsphere according to claim 5, wherein the method comprises the following steps: the organic solvent is toluene, xylene or chloroform.
8. The method for preparing the organomagnesium doped polysilsesquioxane microsphere according to claim 5, wherein the method comprises the following steps: the reaction temperature is 80-90 ℃ and the reaction time is 4-8 hours.
9. The method for preparing the organomagnesium doped polysilsesquioxane microsphere according to claim 1, wherein the method comprises the following steps: the concentration of the ammonia water is 8-16%, and the pH value is regulated to 7.8-10.8.
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