CN107497484A - A kind of hydrophobic type polyvinyl alcohol sustained-release micro-spheres of supported catalyst and preparation method thereof - Google Patents
A kind of hydrophobic type polyvinyl alcohol sustained-release micro-spheres of supported catalyst and preparation method thereof Download PDFInfo
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- CN107497484A CN107497484A CN201710565792.0A CN201710565792A CN107497484A CN 107497484 A CN107497484 A CN 107497484A CN 201710565792 A CN201710565792 A CN 201710565792A CN 107497484 A CN107497484 A CN 107497484A
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- 239000004005 microsphere Substances 0.000 title claims abstract description 32
- 239000004372 Polyvinyl alcohol Substances 0.000 title claims abstract description 30
- 229920002451 polyvinyl alcohol Polymers 0.000 title claims abstract description 30
- 238000013268 sustained release Methods 0.000 title claims abstract description 30
- 239000012730 sustained-release form Substances 0.000 title claims abstract description 30
- 239000003054 catalyst Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 230000002209 hydrophobic effect Effects 0.000 title claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 36
- 235000019422 polyvinyl alcohol Nutrition 0.000 claims abstract description 29
- 229940068984 polyvinyl alcohol Drugs 0.000 claims abstract description 29
- 239000000839 emulsion Substances 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000000243 solution Substances 0.000 claims abstract description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000012153 distilled water Substances 0.000 claims abstract description 8
- 239000008236 heating water Substances 0.000 claims abstract description 8
- 238000004078 waterproofing Methods 0.000 claims abstract description 8
- 238000004132 cross linking Methods 0.000 claims abstract description 6
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 6
- 239000011259 mixed solution Substances 0.000 claims abstract description 6
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims abstract description 6
- 235000019394 potassium persulphate Nutrition 0.000 claims abstract description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 235000015112 vegetable and seed oil Nutrition 0.000 claims abstract description 6
- 239000008158 vegetable oil Substances 0.000 claims abstract description 6
- 239000012188 paraffin wax Substances 0.000 claims abstract description 5
- 238000001556 precipitation Methods 0.000 claims abstract description 5
- HVUMOYIDDBPOLL-UHFFFAOYSA-N 2-(3,4-Dihydroxyoxolan-2-yl)-2-hydroxyethyl octadecanoate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(O)C1OCC(O)C1O HVUMOYIDDBPOLL-UHFFFAOYSA-N 0.000 claims abstract description 4
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 claims abstract description 4
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 claims abstract description 3
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims abstract description 3
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims abstract 4
- 229920001214 Polysorbate 60 Polymers 0.000 claims abstract 2
- 230000018044 dehydration Effects 0.000 claims abstract 2
- 238000006297 dehydration reaction Methods 0.000 claims abstract 2
- 230000002045 lasting effect Effects 0.000 claims abstract 2
- 235000010989 polyoxyethylene sorbitan monostearate Nutrition 0.000 claims abstract 2
- 239000001818 polyoxyethylene sorbitan monostearate Substances 0.000 claims abstract 2
- 229940113124 polysorbate 60 Drugs 0.000 claims abstract 2
- 238000005406 washing Methods 0.000 claims abstract 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 18
- 239000004698 Polyethylene Substances 0.000 claims description 6
- -1 polyethylene Polymers 0.000 claims description 6
- 229920000573 polyethylene Polymers 0.000 claims description 6
- 238000013019 agitation Methods 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 239000004094 surface-active agent Substances 0.000 claims description 4
- ZNZYKNKBJPZETN-WELNAUFTSA-N Dialdehyde 11678 Chemical compound N1C2=CC=CC=C2C2=C1[C@H](C[C@H](/C(=C/O)C(=O)OC)[C@@H](C=C)C=O)NCC2 ZNZYKNKBJPZETN-WELNAUFTSA-N 0.000 claims description 3
- 230000001476 alcoholic effect Effects 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 150000002148 esters Chemical class 0.000 claims description 3
- 235000019441 ethanol Nutrition 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 239000004816 latex Substances 0.000 claims description 3
- 229920000126 latex Polymers 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 230000001804 emulsifying effect Effects 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims 1
- 238000000926 separation method Methods 0.000 claims 1
- 239000010883 coal ash Substances 0.000 description 10
- 239000000835 fiber Substances 0.000 description 8
- 238000000034 method Methods 0.000 description 5
- 239000011094 fiberboard Substances 0.000 description 4
- 239000003921 oil Substances 0.000 description 3
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 239000008346 aqueous phase Substances 0.000 description 2
- 239000003995 emulsifying agent Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 235000019198 oils Nutrition 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000007720 emulsion polymerization reaction Methods 0.000 description 1
- 239000010881 fly ash Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000000123 paper Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000001993 wax Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/38—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of titanium, zirconium or hafnium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/06—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing polymers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/51—Spheres
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/04—Mixing
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F120/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
- C08F120/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F120/10—Esters
- C08F120/12—Esters of monohydric alcohols or phenols
- C08F120/14—Methyl esters, e.g. methyl (meth)acrylate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/32—Polymerisation in water-in-oil emulsions
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Inorganic Chemistry (AREA)
- Medicinal Preparation (AREA)
- Catalysts (AREA)
- Manufacturing Of Micro-Capsules (AREA)
Abstract
The invention discloses hydrophobic type polyvinyl alcohol sustained-release micro-spheres of a kind of supported catalyst and preparation method thereof, it is characterised in that adds distilled water into polyvinyl alcohol, dissolves to obtain poly-vinyl alcohol solution；Poly-vinyl alcohol solution is added drop-wise in vegetable oil, adds Span80, emulsion reaction, crosslinking agent glutaraldehyde is added dropwise, after stirring, adds hydrochloric, after continuing stirring crosslinking reaction, precipitation is centrifuged, washing, acetone dehydration, dries at room temperature, obtain sustained-release micro-spheres；Paraffin heating water bath is melted, adds polysorbate60, sorbester p18, stirs, methylate methyl acrylate, potassium peroxydisulfate, emulsion reaction, filters to obtain complex emulsions waterproofing agent；Butyl titanate is well mixed with absolute ethyl alcohol, is slowly added under stirring in mixed solution, lasting stirring, obtains TiO2Colloidal sol, it is well mixed with complex emulsions waterproofing agent, sustained-release micro-spheres are immersed, be dried in vacuo, obtain the sustained-release micro-spheres of supported catalyst.
Description
Technical field
The present invention relates to sustained-release micro-spheres field, and in particular to a kind of hydrophobic type polyvinyl alcohol sustained-release micro-spheres of supported catalyst
And preparation method thereof.
Background technology
Coal ash fiber is flyash gets rid of the ultra-fine inorganic mineral fibres that a fiber-forming process produces by melting, at present
Research for coal ash fiber both at home and abroad and production are still at an early stage, most of research still rest on fiber copy paper with
And fiberboard preparation etc..
Wang Cheng is far away from its master thesis《The preparation and water resistance research of coal ash fiberboard》In, using wet method system
Plate technology utilization coal ash fiber prepares sheet material, and coal ash fiber is loosened except Slag treatment by water conservancy stirring means, ground
The factors such as adhesive polyethylene alcohol, coal ash fiber slurry agitation jitter time, coal ash fiber concentration, additive have been studied carefully to powder
The influence of coal ash fiberboard mechanical property, improved by modified coal ash fiber, modified adhesive and using waterproof coating
The water resistance of coal ash fiberboard.But combination property, water resistance deficiency be present.
The content of the invention
The present invention solves the technical problem of provide a kind of hydrophobic type polyvinyl alcohol sustained-release micro-spheres of supported catalyst
And preparation method thereof, the sustained-release micro-spheres prepared according to the technique possess good sustained release performance and hydrophobic performance.
The technical problems to be solved by the invention are realized using following technical scheme：
The preparation method of the hydrophobic type polyvinyl alcohol sustained-release micro-spheres of a kind of supported catalyst, it is characterised in that enter according to the following steps
OK：
A. into 40-50 weight account polyethylene alcohol 1:15-20 adds distilled water, is warming up to 80-90 DEG C of heating water bath stirring 1-
2h, it is completely dissolved, obtains transparent polyethylene alcoholic solution；
B. under magnetic agitation, by gained poly-vinyl alcohol solution 1 in a:1-2 is added drop-wise in vegetable oil, adds 0.1-0.2 parts by weight
Surfactant Span80,40-60 DEG C of emulsified 30-40min, homogeneous latex emulsion system is formed, 1-2 parts by weight of crosslinking agent penta is added dropwise
Dialdehyde, after stirring 10-20min, 0.2-0.5 part by weight of catalyst hydrochloric acid is added, after continuing stirring crosslinking reaction 1-2h, centrifugation point
From precipitation, wash 3-5 times, acetone is dehydrated 2-3 times, is dried at room temperature, is obtained sustained-release micro-spheres；
C. by 6-10 parts by weight paraffin, heating water bath, stirring fusing are slow to add 2-3 parts by weight polysorbate60,1-2 at 85-95 DEG C
Parts by weight sorbester p18, stirs, and 1:3-5 adds distilled water, continues constant temperature stirring 1-2h, adds 5-8 weight parts of methacrylic acid first
Ester, 0.1-0.2 parts by weight potassium peroxydisulfates, 3-4h is reacted in 70-80 DEG C of stirring and emulsifying, room temperature is cooled to, with 100-200 eye mesh screens
Filtering and discharging, obtain complex emulsions waterproofing agent；
D. by 5-10 parts by weight butyl titanate and absolute ethyl alcohol 3-2:1 is well mixed, stirring lower 1:2-4 is slowly added to mix molten
In liquid, 2-3h is persistently stirred, obtains TiO2Colloidal sol, it is well mixed with material in c, thus obtained microsphere in b is immersed 8-
10h, 85-95 DEG C of vacuum drying 4-6h, obtain the sustained-release micro-spheres of supported catalyst.
Wherein, concentration of hydrochloric acid described in step b is 0.5-1mol/L；Emulsion reaction mixing speed is described in step c
1000-1100rpm；Mixed solution described in step d is hydrochloric acid and deionized water 1:30-40 is mixed.
The present invention reaction mechanism and have the beneficial effect that：
Polyvinyl alcohol (PVA) microballoon is prepared using emulsion-crosslinking method, mixed aqueous phase with oil phase using emulsifying agent, forms Water-In-Oil
(W/O) reaction system, PVA contain substantial amounts of hydroxyl, in acid condition can with crosslinking agent glutaraldehyde occur aldolisation, penta
After dialdehyde addition system, it can be well mixed in a manner of scattering and permeating with PVA solution, under the catalysis of hydrochloric acid, the two is handed over
Connection reaction, solidifies balling-up, using the PVA aqueous solution as aqueous phase, using vegetable oil as oil phase, using Span80 as surfactant, is prepared into
To PVA sustained-release micro-spheres；Using sorbester p18 as emulsifying agent, using potassium peroxydisulfate as initiator, using methyl methacrylate as monomer, with stone
Wax emulsion carries out emulsion polymerization, obtains complex emulsions waterproofing agent, available for the hydrophobicity and dimensional stability for improving PVA microballoons；It is logical
Cross sol-gal process and be prepared for TiO2The hydrosol, it is well mixed with complex emulsions waterproofing agent, PVA sustained-release micro-spheres are immersed it
In, obtain the sustained-release micro-spheres of supported catalyst.
Embodiment
In order that the technical means, the inventive features, the objects and the advantages of the present invention are easy to understand, tie below
Specific embodiment is closed, the present invention is expanded on further.
Embodiment
The preparation method of the hydrophobic type polyvinyl alcohol sustained-release micro-spheres of a kind of supported catalyst, it is characterised in that by following step
It is rapid to carry out：
A. into 40kg polyvinyl alcohol 1:15 add distilled water, are warming up to 80-90 DEG C of heating water bath stirring 2h, are completely dissolved, obtain
Transparent polyethylene alcoholic solution；
B. under magnetic agitation, by gained poly-vinyl alcohol solution 1 in a:2 are added drop-wise in vegetable oil, add 0.2kg surfactants
Span80,40-60 DEG C of emulsified 35min, homogeneous latex emulsion system is formed, 1kg crosslinking agent glutaraldehydes are added dropwise, after stirring 15min, added
Enter 0.5kg hydrochlorics, after continuing stirring crosslinking reaction 2h, centrifuge precipitation, wash 3 times, acetone is dehydrated 3 times, room temperature
Under dry, obtain sustained-release micro-spheres；
C. by 6kg paraffin, heating water bath, stirring fusing, slow plus 2kg polysorbate60s, 1kg sorbester p18s, stirring are equal at 85-95 DEG C
It is even, 1:5 add distilled water, continue constant temperature stirring 2h, add 5kg methyl methacrylates, 0.1kg potassium peroxydisulfates, in 70-80 DEG C of stirring
Emulsion reaction 3h, is cooled to room temperature, with 100 eye mesh screen filtering and dischargings, obtains complex emulsions waterproofing agent；
D. by 5kg butyl titanates and absolute ethyl alcohol 2:1 is well mixed, stirring lower 1:4 are slowly added in mixed solution, persistently stir
3h is mixed, obtains TiO2Colloidal sol, it is well mixed with material in c, thus obtained microsphere in b is immersed into 10h, 85-95 DEG C of vacuum is done
Dry 6h, obtain the sustained-release micro-spheres of supported catalyst.
Wherein, concentration of hydrochloric acid described in step b is 1mol/L；Emulsion reaction mixing speed is described in step c
1100rpm；Mixed solution described in step d is hydrochloric acid and deionized water 1:35 mixing.
Claims (5)
- A kind of 1. preparation method of the hydrophobic type polyvinyl alcohol sustained-release micro-spheres of supported catalyst, it is characterised in that：Add distilled water into polyvinyl alcohol, dissolve to obtain poly-vinyl alcohol solution；Poly-vinyl alcohol solution is added drop-wise in vegetable oil, added Span80, emulsion reaction, crosslinking agent glutaraldehyde is added dropwise, after stirring, adds hydrochloric, after continuing stirring crosslinking reaction, centrifugation Precipitation and separation, washing, acetone dehydration, dry at room temperature, obtain sustained-release micro-spheres；Paraffin heating water bath is melted, adds polysorbate60, sapn 60, stir, methylate methyl acrylate, potassium peroxydisulfate, emulsion reaction, filter to obtain complex emulsions waterproofing agent；By metatitanic acid fourth Ester is well mixed with absolute ethyl alcohol, is slowly added under stirring in mixed solution, lasting stirring, obtains TiO2Colloidal sol, by its with it is compound Emulsion water-proof agent is well mixed, and sustained-release micro-spheres are immersed, vacuum drying, obtains the sustained-release micro-spheres of supported catalyst.
- A kind of 2. preparation method of the hydrophobic type polyvinyl alcohol sustained-release micro-spheres of supported catalyst, it is characterised in that：A. into 40-50 weight account polyethylene alcohol 1:15-20 adds distilled water, is warming up to 80-90 DEG C of heating water bath stirring 1- 2h, it is completely dissolved, obtains transparent polyethylene alcoholic solution；B. under magnetic agitation, by gained poly-vinyl alcohol solution 1 in a:1-2 is added drop-wise in vegetable oil, adds 0.1-0.2 parts by weight Surfactant Span80,40-60 DEG C of emulsified 30-40min, homogeneous latex emulsion system is formed, 1-2 parts by weight of crosslinking agent penta is added dropwise Dialdehyde, after stirring 10-20min, 0.2-0.5 part by weight of catalyst hydrochloric acid is added, after continuing stirring crosslinking reaction 1-2h, centrifugation point From precipitation, wash 3-5 times, acetone is dehydrated 2-3 times, is dried at room temperature, is obtained sustained-release micro-spheres；C. by 6-10 parts by weight paraffin, heating water bath, stirring fusing are slow to add 2-3 parts by weight polysorbate60,1-2 at 85-95 DEG C Parts by weight sorbester p18, stirs, and 1:3-5 adds distilled water, continues constant temperature stirring 1-2h, adds 5-8 weight parts of methacrylic acid first Ester, 0.1-0.2 parts by weight potassium peroxydisulfates, 3-4h is reacted in 70-80 DEG C of stirring and emulsifying, room temperature is cooled to, with 100-200 eye mesh screens Filtering and discharging, obtain complex emulsions waterproofing agent；D. by 5-10 parts by weight butyl titanate and absolute ethyl alcohol 3-2:1 is well mixed, stirring lower 1:2-4 is slowly added to mix molten In liquid, 2-3h is persistently stirred, obtains TiO2Colloidal sol, it is well mixed with material in c, thus obtained microsphere in b is immersed 8- 10h, 85-95 DEG C of vacuum drying 4-6h, obtain the sustained-release micro-spheres of supported catalyst.
- 3. a kind of preparation method of the hydrophobic type polyvinyl alcohol sustained-release micro-spheres of supported catalyst according to claim 2, its It is characterised by, concentration of hydrochloric acid described in step b is 0.5-1mol/L.
- 4. a kind of preparation method of the hydrophobic type polyvinyl alcohol sustained-release micro-spheres of supported catalyst according to claim 2, its It is characterised by, emulsion reaction mixing speed described in step c is 1000-1100rpm.
- 5. a kind of preparation method of the hydrophobic type polyvinyl alcohol sustained-release micro-spheres of supported catalyst according to claim 2, its It is characterised by, mixed solution described in step d is hydrochloric acid and deionized water 1:30-40 is mixed.
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| CN111097522A (en) * | 2019-12-31 | 2020-05-05 | 江南大学 | Preparation method of controllable slow-release catalyst |
| CN111205614A (en) * | 2019-07-29 | 2020-05-29 | 杭州金州高分子科技有限公司 | Flame-retardant antibacterial PC alloy material for intelligent closestool and preparation method thereof |
| CN111229139A (en) * | 2020-01-15 | 2020-06-05 | 四川大学华西医院 | Iodine 131-loaded collagen-polyvinyl alcohol embolism microsphere and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108744020A (en) * | 2018-06-12 | 2018-11-06 | 杭州艾力康医药科技有限公司 | A kind of preparation method of ion-exchange type polyvinyl alcohol microparticles |
| CN111205614A (en) * | 2019-07-29 | 2020-05-29 | 杭州金州高分子科技有限公司 | Flame-retardant antibacterial PC alloy material for intelligent closestool and preparation method thereof |
| CN111205614B (en) * | 2019-07-29 | 2021-12-28 | 杭州金州高分子科技有限公司 | Flame-retardant antibacterial PC alloy material for intelligent closestool and preparation method thereof |
| CN111097522A (en) * | 2019-12-31 | 2020-05-05 | 江南大学 | Preparation method of controllable slow-release catalyst |
| CN111097522B (en) * | 2019-12-31 | 2023-09-01 | 江南大学 | Preparation method of controllable slow-release catalyst |
| CN111229139A (en) * | 2020-01-15 | 2020-06-05 | 四川大学华西医院 | Iodine 131-loaded collagen-polyvinyl alcohol embolism microsphere and preparation method thereof |
| CN111229139B (en) * | 2020-01-15 | 2020-11-24 | 四川大学华西医院 | Iodine 131-loaded collagen-polyvinyl alcohol embolism microsphere and preparation method thereof |
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