CN106589269A - Method of using styrene-acrylic ester to polymerize at surface of titanium dioxide - Google Patents
Method of using styrene-acrylic ester to polymerize at surface of titanium dioxide Download PDFInfo
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- CN106589269A CN106589269A CN201611253799.0A CN201611253799A CN106589269A CN 106589269 A CN106589269 A CN 106589269A CN 201611253799 A CN201611253799 A CN 201611253799A CN 106589269 A CN106589269 A CN 106589269A
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- 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
- C08F292/00—Macromolecular compounds obtained by polymerising monomers on to inorganic materials
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- 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
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
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- Chemical Kinetics & Catalysis (AREA)
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- Pigments, Carbon Blacks, Or Wood Stains (AREA)
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Abstract
The invention provides a method of using styrene-acrylic ester to polymerize at the surface of titanium dioxide. The method is characterized in that: first of all, a silane coupling agent is used to modify the surface of titanium dioxide; then mixed monomers that are prepared from 28 parts of styrene, 20 parts of butyl acrylate and 5 parts of Alpha-methacrylic acid, 80 parts of water, 1 part of initiator ammonium persulfate and 2 parts of emulsifier are pre-emulsified to obtain a pre-emulsified mixed monomer emulsion; 0.3 part of initiator ammonium persulfate is added into a TiO2 slurry of 80 DEG C, and after 5-min initiating reaction, the pre-emulsified mixed monomer emulsion is slowly added into the TiO2 slurry, wherein the adding time is controlled in 2-5 hours; then the reaction is kept at the constant temperature of 85 DEG C for 1 hour to obtain a TiO2 slurry coated by polystyrene-acrylic ester.
Description
Technical field
The present invention relates to a kind of method that use styrene-acrylate is polymerized in titanium dioxide surface.
Background technology
Coatings industry is the first large user of titanium dioxide, and titanium dioxide is most of to be consumed by coatings industry.Titanium dioxide
Titanium is most important pigment in coating material production, and its effect is not exclusively covered and decorated, it is often more important that can improve coating
Physical and chemical performance, strengthens chemical stability, improves covering power, reducing power, anticorrosive property, fast light and weatherability, strengthens the machine of film
Tool intensity and adhesive force, prevent from ftractureing and come off, and prevent ultraviolet and moisture from passing through, extend the service life of object.Titanium dioxide
Titanium can be divided into rutile-type, Detitanium-ore-type and plate titanium-type three types from crystal structure, wherein plate titanium-type titanium dioxide compared with
It is difficult to obtain, it is uncommon in actual applications.
In 70-100 nanometers, its particle surface contains substantial amounts of hydroxyl to the particle size range of pigmentary titanium dioxide, it is easy to send out
Raw to reunite, after reunion, the covering power of titanium dioxide can be greatly affected.So, titanium dioxide will carry out younger using before
Thin grinding, adds a certain amount of dispersant in process of lapping, it is therefore an objective to separate titanium dioxide granule, such titanium dioxide hides
Lid ability can just obtain bigger performance.In addition, titanium dioxide surface is very sensitive to environment, a small amount of impurity may be caused
Scattered granule occurs to reunite again, and the use range of titanium dioxide is widely, and use occasion varies, slightly
Will result in accidentally scattered granule to occur again to reunite, so necessary coat one layer of protection in titanium dioxide surface
Layer, titanium dioxide granule is kept apart, it is to avoid the reunion of titanium dioxide granule, makes the covering power of titanium dioxide obtain bigger
Play.
The present invention mainly coats styrene-acrylic copolymer in titanium dioxide surface, is applied in water paint.
Titanium dioxide surface polymer overmold except can reduce reunion, to greatest extent play titanium dioxide covering power in addition to, also
Some other benefits, summarize with advantages below：
（1）The reunion of titanium dioxide can be prevented so as to keep monodisperse status, strengthen its covering power, improve titanium dioxide
Utilization rate.
（2）It is easy to use, titania slurry is mixed with emulsion and adds other auxiliary agents, reduced two when using
The step of dry powder dispersion of titanium oxide is into slurry, and titanium dioxide is it may happen that reunite, it is impossible to effectively disperse.
（3）Titanium dioxide carried out transporting, used with dry powder, but carry out transporting, use with slurry, it is to avoid
The generation of titanium dioxide dust, can play the effect of environmental protection, can reduce the loss of raw material again.
（4）It is more preferable with the compatibility of emulsion after titanium dioxide surface polymer overmold, the performance of coating can be improved.
In order that polymer covering layer can be preferably combined with titanium dioxide surface, the present invention is first with the silane with double bond
Coupling agent is modified to titanium dioxide surface, and modified mechanism is：The mechanism four-step reaction of silane coupler, i.e.,（1）
3 Si-X bases being connected with silicon are hydrolyzed into Si-OH；（2）Between Si-OH, dehydrating condensation is into the oligosiloxane containing Si-OH；（3）
Si-OH in oligomer forms hydrogen bond with the OH on base material titanium dioxide surface；（4）With dehydration in heat curing process
And form covalently bonded with base material titanium dioxide.It is generally believed that on interface the silicon of silane coupler and base material titanium dioxide
Surface only one of which bonding, is left two Si-OH, or is condensed with the Si-OH in other silane, or between free state.
Titanium dioxide surface after silane coupler modified, silane coupler contain the group of unsaturated double-bond vinyl also
Titanium dioxide surface is stayed in, then is caused and styrene, acrylate copolymer with initiator ammonium persulfate, finally obtained surface
The titanium dioxide of cladding polystyrene acrylate.
The content of the invention
A kind of method that use styrene-acrylate is polymerized in titanium dioxide surface, it is characterised in that：First to TiO2Enter
Row surface is modified, by weight by 300 parts of TiO2Powder is added in 1000 parts of water, is started agitator stirring, is made TiO2Powder
It is dispersed in water, adds 1.5 parts of dispersants, by the TiO for obtaining2Slurry carries out high speed dispersion on high speed dispersor, obtains
To monodispersed TiO2Slurry；3 parts of silane couplers, plus 20 parts of dehydrated alcohol dilutions are weighed, by the second containing silane coupler
Alcoholic solution is slowly dropped to TiO2In slurry；Then the ammonia of Deca 10% adjusts the pH value of slurry to 8-9, under agitation
By TiO2Slurry is heated to 80 DEG C, and isothermal reaction 1 hour, obtains the silane coupler modified finely dispersed TiO of surface Jing2
Slurry；
By by 80 parts of 28 parts of styrene, 5 parts of mix monomers for constituting of 20 parts of butyl acrylate and α-methacrylic acid and water, initiation
1 part of agent Ammonium persulfate., 2 parts of emulsifying agent carry out pre-emulsification, obtain pre-emulsification mix monomer emulsion；
Toward 80 DEG C of above-mentioned TiO2Slurry adds 0.3 part of initiator ammonium persulfate, and initiation reaction 5 minutes is then good by pre-emulsification
Mix monomer emulsion be slowly added into above-mentioned TiO2In slurry, add time control in 2-5 hours, addition is maintained after finishing
85 DEG C of isothermal reactions 1 hour, obtain the TiO of surface Jing polystyrene acrylate claddings2Slurry；
Described silane coupler be VTES, vinyltrimethoxy silane, γ-（Methacryloxypropyl
Base）Propyl trimethoxy silicane it is therein one or more；
Described emulsifying agent is NPE ammonium sulfate；
Described TiO2Powder is anatase pigmentary TiO2；
Described dispersant is sodium acrylate.
Specific embodiment
Embodiment 1
First to TiO2Carry out surface to be modified, by 300kg anatase pigmentary TiO2Powder is added in 1000kg water, and startup is stirred
Device stirring is mixed, TiO is made2Powder is dispersed in water, adds 1.5kg dispersants, by the TiO for obtaining2Slurry is in high speed dispersor
On carry out high speed dispersion, obtain monodispersed TiO2Slurry；Weigh 3kg VTESs, plus 20kg dehydrated alcohol
Ethanol solution containing silane coupler is slowly dropped to TiO by dilution2In slurry；Then the ammonia of Deca 10% adjusts slurry
PH value to 8, under agitation by TiO2Slurry is heated to 80 DEG C, and isothermal reaction 1 hour, obtains surface Jing silane coupled
The modified finely dispersed TiO of agent2Slurry；To be made up of styrene 28kg, butyl acrylate 20kg and α-methacrylic acid 5kg
Mix monomer and water 80kg, initiator ammonium persulfate 1kg, emulsifying agent NPE ammonium sulfate 2kg carry out pre- breast
Change, obtain pre-emulsification mix monomer emulsion；Toward 80 DEG C of above-mentioned TiO2Slurry adds 0.3kg initiator ammonium persulfates, causes anti-
Answer 5 minutes, pre-emulsification good mix monomer emulsion is slowly added into into above-mentioned TiO then2In slurry, time control is added to exist
2 hours, addition maintained 85 DEG C of isothermal reactions 1 hour after finishing, and obtains the coated TiO in surface2Slurry.
Embodiment 2
First to TiO2Carry out surface to be modified, by 300kg anatase pigmentary TiO2Powder is added in 1000kg water, and startup is stirred
Device stirring is mixed, TiO is made2Powder is dispersed in water, adds 1.5kg dispersants, by the TiO for obtaining2Slurry is in high speed dispersor
On carry out high speed dispersion, obtain monodispersed TiO2Slurry；Weigh 3kg vinyltrimethoxy silanes, plus 20kg dehydrated alcohol
Ethanol solution containing silane coupler is slowly dropped to TiO by dilution2In slurry；Then the ammonia of Deca 10% adjusts slurry
PH value to 9, under agitation by TiO2Slurry is heated to 80 DEG C, and isothermal reaction 1 hour, obtains surface Jing silane coupled
The modified finely dispersed TiO of agent2Slurry；To be made up of styrene 28kg, butyl acrylate 20kg and α-methacrylic acid 5kg
Mix monomer and water 80kg, initiator ammonium persulfate 1kg, emulsifying agent NPE ammonium sulfate 2kg carry out pre- breast
Change, obtain pre-emulsification mix monomer emulsion；Toward 80 DEG C of above-mentioned TiO2Slurry adds 0.3kg initiator ammonium persulfates, causes anti-
Answer 5 minutes, pre-emulsification good mix monomer emulsion is slowly added into into above-mentioned TiO then2In slurry, time control is added to exist
5 hours, addition maintained 85 DEG C of isothermal reactions 1 hour after finishing, and obtains the coated TiO in surface2Slurry.
Embodiment 3
First to TiO2Carry out surface to be modified, by 300kg anatase pigmentary TiO2Powder is added in 1000kg water, and startup is stirred
Device stirring is mixed, TiO is made2Powder is dispersed in water, adds 1.5kg dispersants, by the TiO for obtaining2Slurry is in high speed dispersor
On carry out high speed dispersion, obtain monodispersed TiO2Slurry；Weigh 3kg γ-（Methacryloxy）Propyl trimethoxy silicon
Ethanol solution containing silane coupler is slowly dropped to TiO by alkane, plus the dilution of 20kg dehydrated alcohol2In slurry；Then Deca
10% ammonia adjusts the pH value of slurry to 8, under agitation by TiO2Slurry is heated to 80 DEG C, and isothermal reaction 1 hour,
Obtain the silane coupler modified finely dispersed TiO of surface Jing2Slurry；Will by styrene 28kg, butyl acrylate 20kg and
The mix monomer and water 80kg, initiator ammonium persulfate 1kg, emulsifying agent Nonyl pheno of α-methacrylic acid 5kg compositions
Ether ammonium sulfate 2kg carries out pre-emulsification, obtains pre-emulsification mix monomer emulsion；Toward 80 DEG C of above-mentioned TiO2Slurry adds 0.3kg to draw
Agent Ammonium persulfate. is sent out, then pre-emulsification good mix monomer emulsion is slowly added into above-mentioned TiO by initiation reaction 5 minutes2Slurry
In material, time control is added at 3 hours, addition maintains 85 DEG C of isothermal reactions 1 hour after finishing, and obtains the coated TiO in surface2
Slurry.
Embodiment 4
First to TiO2Carry out surface to be modified, by 300kg anatase pigmentary TiO2Powder is added in 1000kg water, and startup is stirred
Device stirring is mixed, TiO is made2Powder is dispersed in water, adds 1.5kg dispersants, by the TiO for obtaining2Slurry is in high speed dispersor
On carry out high speed dispersion, obtain monodispersed TiO2Slurry；Weigh 3kg VTESs, plus 20kg dehydrated alcohol
Ethanol solution containing silane coupler is slowly dropped to TiO by dilution2In slurry；Then the ammonia of Deca 10% adjusts slurry
PH value to 9, under agitation by TiO2Slurry is heated to 80 DEG C, and isothermal reaction 1 hour, obtains surface Jing silane coupled
The modified finely dispersed TiO of agent2Slurry；To be made up of styrene 28kg, butyl acrylate 20kg and α-methacrylic acid 5kg
Mix monomer and water 80kg, initiator ammonium persulfate 1kg, emulsifying agent NPE ammonium sulfate 2kg carry out pre- breast
Change, obtain pre-emulsification mix monomer emulsion；Toward 80 DEG C of above-mentioned TiO2Slurry adds 0.3kg initiator ammonium persulfates, causes anti-
Answer 5 minutes, pre-emulsification good mix monomer emulsion is slowly added into into above-mentioned TiO then2In slurry, time control is added to exist
4 hours, addition maintained 85 DEG C of isothermal reactions 1 hour after finishing, and obtains the coated TiO in surface2Slurry.
Embodiment 5
First to TiO2Carry out surface to be modified, by 300kg anatase pigmentary TiO2Powder is added in 1000kg water, and startup is stirred
Device stirring is mixed, TiO is made2Powder is dispersed in water, adds 1.5kg dispersants, by the TiO for obtaining2Slurry is in high speed dispersor
On carry out high speed dispersion, obtain monodispersed TiO2Slurry；Weigh 3kg vinyltrimethoxy silanes, plus 20kg dehydrated alcohol
Ethanol solution containing silane coupler is slowly dropped to TiO by dilution2In slurry；Then the ammonia of Deca 10% adjusts slurry
PH value to 8, under agitation by TiO2Slurry is heated to 80 DEG C, and isothermal reaction 1 hour, obtains surface Jing silane coupled
The modified finely dispersed TiO of agent2Slurry；To be made up of styrene 28kg, butyl acrylate 20kg and α-methacrylic acid 5kg
Mix monomer and water 80kg, initiator ammonium persulfate 1kg, emulsifying agent NPE ammonium sulfate 2kg carry out pre- breast
Change, obtain pre-emulsification mix monomer emulsion；Toward 80 DEG C of above-mentioned TiO2Slurry adds 0.3kg initiator ammonium persulfates, causes anti-
Answer 5 minutes, pre-emulsification good mix monomer emulsion is slowly added into into above-mentioned TiO then2In slurry, time control is added to exist
4.5 hours, addition maintained 85 DEG C of isothermal reactions 1 hour after finishing, and obtains the coated TiO in surface2Slurry.
Embodiment 6
First to TiO2Carry out surface to be modified, by 300kg anatase pigmentary TiO2Powder is added in 1000kg water, and startup is stirred
Device stirring is mixed, TiO is made2Powder is dispersed in water, adds 1.5kg dispersants, by the TiO for obtaining2Slurry is in high speed dispersor
On carry out high speed dispersion, obtain monodispersed TiO2Slurry；Weigh 3kg γ-（Methacryloxy）Propyl trimethoxy silicon
Ethanol solution containing silane coupler is slowly dropped to TiO by alkane, plus the dilution of 20kg dehydrated alcohol2In slurry；Then Deca
10% ammonia adjusts the pH value of slurry to 9, under agitation by TiO2Slurry is heated to 80 DEG C, and isothermal reaction 1 hour,
Obtain the silane coupler modified finely dispersed TiO of surface Jing2Slurry；Will by styrene 28kg, butyl acrylate 20kg and
The mix monomer and water 80kg, initiator ammonium persulfate 1kg, emulsifying agent Nonyl pheno of α-methacrylic acid 5kg compositions
Ether ammonium sulfate 2kg carries out pre-emulsification, obtains pre-emulsification mix monomer emulsion；Toward 80 DEG C of above-mentioned TiO2Slurry adds 0.3kg to draw
Agent Ammonium persulfate. is sent out, then pre-emulsification good mix monomer emulsion is slowly added into above-mentioned TiO by initiation reaction 5 minutes2Slurry
In material, time control is added at 3.5 hours, addition maintains 85 DEG C of isothermal reactions 1 hour after finishing, and obtains surface coated
TiO2Slurry.
Claims (1)
1. a kind of method that use styrene-acrylate is polymerized in titanium dioxide surface, it is characterised in that：First to TiO2Carry out table
Face is modified, by weight by 300 parts of TiO2Powder is added in 1000 parts of water, is started agitator stirring, is made TiO2Powder is uniform
It is dispersed in water, adds 1.5 parts of dispersants, by the TiO for obtaining2Slurry carries out high speed dispersion on high speed dispersor, obtains list
Scattered TiO2Slurry；3 parts of silane couplers, plus 20 parts of dehydrated alcohol dilutions are weighed, will be the ethanol containing silane coupler molten
Liquid is slowly dropped to TiO2In slurry；Then the ammonia of Deca 10% adjusts the pH value of slurry to 8-9, under agitation by TiO2
Slurry is heated to 80 DEG C, and isothermal reaction 1 hour, obtains the silane coupler modified finely dispersed TiO of surface Jing2Slurry；
By by 80 parts of 28 parts of styrene, 5 parts of mix monomers for constituting of 20 parts of butyl acrylate and α-methacrylic acid and water, initiation
1 part of agent Ammonium persulfate., 2 parts of emulsifying agent carry out pre-emulsification, obtain pre-emulsification mix monomer emulsion；
Toward 80 DEG C of above-mentioned TiO2Slurry adds 0.3 part of initiator ammonium persulfate, and initiation reaction 5 minutes is then good by pre-emulsification
Mix monomer emulsion is slowly added into above-mentioned TiO2In slurry, add time control in 2-5 hours, addition maintains 85 after finishing
DEG C isothermal reaction 1 hour, obtains the TiO of surface Jing polystyrene acrylate claddings2Slurry；
Described silane coupler be VTES, vinyltrimethoxy silane, γ-（Methacryloxypropyl
Base）Propyl trimethoxy silicane it is therein one or more；
Described emulsifying agent is NPE ammonium sulfate；
Described TiO2Powder is anatase pigmentary TiO2；
Described dispersant is sodium acrylate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611253799.0A CN106589269A (en) | 2016-12-30 | 2016-12-30 | Method of using styrene-acrylic ester to polymerize at surface of titanium dioxide |
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| CN201611253799.0A CN106589269A (en) | 2016-12-30 | 2016-12-30 | Method of using styrene-acrylic ester to polymerize at surface of titanium dioxide |
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| CN106589269A true CN106589269A (en) | 2017-04-26 |
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| CN201611253799.0A Pending CN106589269A (en) | 2016-12-30 | 2016-12-30 | Method of using styrene-acrylic ester to polymerize at surface of titanium dioxide |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107383291A (en) * | 2017-08-02 | 2017-11-24 | 四川省蓝扬科技有限公司 | It is a kind of to stablize environment-friendly water-based pigment and preparation method thereof |
| CN108130721A (en) * | 2017-12-20 | 2018-06-08 | 彭裕民 | Weight reducing health care women's dress and preparation method thereof |
| CN113583503A (en) * | 2021-08-27 | 2021-11-02 | 河南佰利联新材料有限公司 | Hybrid slurry, preparation method thereof and coating |
| CN114410131A (en) * | 2021-12-14 | 2022-04-29 | 河南河大纳米材料工程研究中心有限公司 | Water-phase instant titanium dioxide material and preparation method and application thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108130721B (en) * | 2017-12-20 | 2020-06-16 | 湖北赛尚服饰集团有限公司 | Slimming health-care women's dress and preparation method thereof |
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| CN113583503B (en) * | 2021-08-27 | 2022-12-30 | 河南佰利联新材料有限公司 | Hybrid slurry, preparation method thereof and coating |
| CN114410131A (en) * | 2021-12-14 | 2022-04-29 | 河南河大纳米材料工程研究中心有限公司 | Water-phase instant titanium dioxide material and preparation method and application thereof |
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