CN106633574B - A kind of preparation method of the special titanium dioxide of organic glass - Google Patents

A kind of preparation method of the special titanium dioxide of organic glass Download PDF

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CN106633574B
CN106633574B CN201611253560.3A CN201611253560A CN106633574B CN 106633574 B CN106633574 B CN 106633574B CN 201611253560 A CN201611253560 A CN 201611253560A CN 106633574 B CN106633574 B CN 106633574B
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tio
slurry
parts
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titanium dioxide
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CN106633574A (en
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王彦华
陈建定
章圣苗
夏浙安
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East China University of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/10—Encapsulated ingredients
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2237—Oxides; Hydroxides of metals of titanium
    • C08K2003/2241—Titanium dioxide
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/002—Physical properties
    • C08K2201/003—Additives being defined by their diameter
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives

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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)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Cosmetics (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

A kind of preparation method of the special titanium dioxide of organic glass, it is characterised in that：First with cationic monomer to TiO2Surface modification is carried out, then by by 2 parts of 80 parts of 60 parts of methyl methacrylate, 10 parts of mix monomers formed of ethylene glycol dimethacrylate and water, 1 part of initiator ammonium persulfate, emulsifier progress pre-emulsifications, obtains pre-emulsification mix monomer lotion；Toward 80 DEG C of TiO20.3 part of initiator ammonium persulfate is added in slurry, then the good mix monomer lotion of pre-emulsification is slowly added into above-mentioned TiO by initiation reaction 5 minutes2In slurry, time control is added at 25 hours, 85 DEG C of maintenance isothermal reaction 1 hour, obtains the TiO that surface is coated through polymethyl methacrylate after addition2Slurry by slurries filtration, is dried to obtain and can be used for the titanium dioxide dry powder of organic glass.

Description

A kind of preparation method of the special titanium dioxide of organic glass
Technical field
The present invention relates to a kind of preparation methods of the special titanium dioxide of organic glass.
Background technology
Polymethyl methacrylate is commonly referred to organic glass, english abbreviation PMMA, has a high grade of transparency, low price, easily In mechanical processing the advantages that, be the glass alternative materials being commonly used usually.Organic glass is to develop a kind of important heat earlier Thermoplastic plastic has the transparency, stability and weatherability, easy dyeing, easy processing, attractive appearance, has in construction industry extensively Application.1. heigh clarity.Organic glass is current most excellent macromolecule transparent material, and light transmittance reaches organic glass 92%, it is higher than the light transmittance of glass.The fluorescent tube for being referred to as the sunlamp of artificial minisun is that quartz is done, this is because quartzy energy Completely through ultraviolet light.Simple glass can only penetrate 0.6% ultraviolet light, but organic glass can penetrate 73%.2. mechanical strength It is high.The relative molecular mass of organic glass is about 2,000,000, is the high-molecular compound of long-chain, and forms the chain of molecule very Softness, therefore, the intensity of organic glass are relatively high, and stretch-proof and shock proof ability ratio simple glass are 7-18 times high.There is one kind By heating and the organic glass of stretch processing, molecule segment therein arrange to obtain unusual orderliness, the toughness of material made to have It significantly improves.It is followed closely into this organic glass with nail, even if not cracked if nail is broken through on organic glass.It is this to have Machine glass quilt attack will not equally go to pieces after wearing.Therefore, the organic glass of stretch processing can be used as bulletproof glass, also use Make the canopy on military aircraft.3. light-weight.The density of organic glass is 1.18g/cm3;, an equal amount of material is heavy Amount only has the half of simple glass, metallic aluminium（Belong to light metal）43%.4. easy to process.Organic glass can not only use lathe It is cut, drilling machine drills, and variously-shaped utensil can be bonded to acetone, chloroform etc., can also use blowing, note The method of the plastic shapings such as penetrating, squeeze out is processed into and arrives canopy greatly, small to panoramic products such as artificial tooth and denture fixing devices.
For the particle size range of pigmentary titanium dioxide at 70-100 nanometers, particle surface contains a large amount of hydroxyl, it is easy to send out Raw to reunite, the covering power of titanium dioxide can be greatly affected after reunion.So to be carried out before titanium dioxide use younger A certain amount of dispersant is added in process of lapping in thin grinding, it is therefore an objective to so that titanium dioxide granule is separated, such titanium dioxide hides Lid ability can just obtain the performance of bigger.In addition, titanium dioxide surface is very sensitive to environment, a small amount of impurity may cause Scattered particle is reunited again, and the use scope of titanium dioxide is very extensive, and use occasion is multifarious, slightly It will result in scattered particle accidentally again to reunite, so it is necessary to coating one layer of protection in titanium dioxide surface Layer, titanium dioxide granule is kept apart, the reunion of titanium dioxide granule is avoided, the covering power of titanium dioxide is made to obtain bigger It plays.
A kind of preparation method of the special titanium dioxide of organic glass of the present invention, a kind of special titanium dioxide of organic glass.For The weatherability and opacity for improving organic glass, generally require titanium dioxide being added in organic glass, due to organic The particularity of process of glass, and common titanium dioxide may not apply to organic glass at all, the present invention is in titanium dioxide Surface coats crosslinked polymethyl methacrylate, crosslinked polymethyl methacrylate will not be destroyed by organic hyaline monomer and It can be well dispersed in organic glass.
In order to enable polymer covering layer preferably to be combined with titanium dioxide surface, the present invention first with double bond sun from Sub- monomer is modified titanium dioxide surface, and modified mechanism is：Titanium dioxide surface is per se with a large amount of negative electrical charge, band Cationic monomer one end of double bond carries positive charge, is adsorbed onto titanium dioxide surface by charge effect, the other end contains insatiable hunger Also stay in titanium dioxide surface with the group of double bond vinyl, then with initiator ammonium persulfate cause with methyl methacrylate, Ethylene glycol dimethacrylate copolymer finally obtained the titanium dioxide of surface cladding polymethyl methacrylate.
Invention content
A kind of preparation method of the special titanium dioxide of organic glass, it is characterised in that：First to TiO2Surface modification is carried out, By weight by 300 parts of TiO2Powder is added in 1000 parts of water, is started blender stirring, is made TiO2Powder is dispersed in In water, 1.5 parts of dispersants, the TiO that will be obtained is added2Slurry carries out high speed dispersion on high speed dispersor, obtains monodispersed TiO2Slurry；3 parts of cationic monomers are weighed, 20 parts of absolute ethyl alcohol dilutions are added, the ethanol solution containing cationic monomer is slow It is added drop-wise to TiO2In slurry, stirs 30 minutes, obtain surface through the modifies finely dispersed TiO of cation mono2Slurry；
It will be by 60 parts of methyl methacrylate, 10 parts of mix monomers formed of ethylene glycol dimethacrylate and water 80 2 parts of part, 1 part of initiator ammonium persulfate, emulsifier progress pre-emulsifications, obtain pre-emulsification mix monomer lotion；
By above-mentioned TiO2Slurry is heated to 80 DEG C, is added 0.3 part of initiator ammonium persulfate, initiation reaction 5 minutes, then The good mix monomer lotion of pre-emulsification is slowly added into above-mentioned TiO2In slurry, time control is added at 2-5 hours, is added After maintain 85 DEG C of isothermal reactions 1 hour, obtain the TiO that surface is coated through polymethyl methacrylate2Slurry, by slurry mistake It filters, be dried to obtain the titanium dioxide dry powder that can be used for organic glass；
The cationic monomer is MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, acrylyl oxy-ethyl-trimethyl chlorination Ammonium, acrylic acid N, N- dimethylamino ethyl ester are one such or two or more；
The emulsifier is nonylphenol polyoxyethylene ether ammonium sulfate；
The TiO2Powder is anatase pigmentary TiO2；
The dispersant is sodium acrylate.
Specific implementation mode
Embodiment 1
First to TiO2Surface modification is carried out, by 300kg anatase pigmentaries TiO2Powder is added in 1000kg water, is opened Dynamic blender stirring, makes TiO2Powder is evenly dispersed in water, and 1.5kg dispersants, the TiO that will be obtained is added2Slurry is in high speed point It dissipates and carries out high speed dispersion on machine, obtain monodispersed TiO2Slurry；3kg MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chlorides are weighed, Add 20kg absolute ethyl alcohols to dilute, the ethanol solution containing cationic monomer is slowly dropped to TiO2In slurry, stir 30 minutes, Surface is obtained through the modifies finely dispersed TiO of cation mono2Slurry；It will be by 60 kg of methyl methacrylate, dimethyl propylene The mix monomer and water 80kg, initiator ammonium persulfate 1kg, emulsifier polyoxyethylene nonyl phenyl second of olefin(e) acid glycol ester 10 kg compositions Alkene ether ammonium sulfate 2kg carries out pre-emulsification, obtains pre-emulsification mix monomer lotion；By above-mentioned TiO2Slurry is heated to 80 DEG C, adds Enter 0.3kg initiator ammonium persulfates, then the good mix monomer lotion of pre-emulsification is slowly added by initiation reaction 5 minutes The TiO stated2In slurry, time control is added at 2 hours, 85 DEG C of maintenance isothermal reaction 1 hour after addition obtains surface warp The TiO of polymethyl methacrylate cladding2Slurries filtration, 105 DEG C are dried to obtain the titanium dioxide that can be used for organic glass by slurry Titanium dry powder.
Embodiment 2
First to TiO2Surface modification is carried out, by 300kg anatase pigmentaries TiO2Powder is added in 1000kg water, is opened Dynamic blender stirring, makes TiO2Powder is evenly dispersed in water, and 1.5kg dispersants, the TiO that will be obtained is added2Slurry is in high speed point It dissipates and carries out high speed dispersion on machine, obtain monodispersed TiO2Slurry；3kg acrylyl oxy-ethyl-trimethyl salmiacs are weighed, are added 20kg absolute ethyl alcohols dilute, and the ethanol solution containing cationic monomer is slowly dropped to TiO2In slurry, stirs 30 minutes, obtain To surface through the modifies finely dispersed TiO of cation mono2Slurry；It will be by 60 kg of methyl methacrylate, dimethyl allene The mix monomer and water 80kg, initiator ammonium persulfate 1kg, emulsifier Nonyl pheno of sour glycol ester 10 kg compositions Ether ammonium sulfate 2kg carries out pre-emulsification, obtains pre-emulsification mix monomer lotion；By above-mentioned TiO2Slurry is heated to 80 DEG C, is added Then the good mix monomer lotion of pre-emulsification is slowly added into above-mentioned by 0.3kg initiator ammonium persulfates, initiation reaction 5 minutes TiO2In slurry, time control is added at 5 hours, 85 DEG C of maintenance isothermal reaction 1 hour after addition obtains surface through poly- The TiO of methyl methacrylate cladding2Slurries filtration, 105 DEG C are dried to obtain the titanium dioxide that can be used for organic glass by slurry Dry powder.
Embodiment 3
First to TiO2Surface modification is carried out, by 300kg anatase pigmentaries TiO2Powder is added in 1000kg water, is opened Dynamic blender stirring, makes TiO2Powder is evenly dispersed in water, and 1.5kg dispersants, the TiO that will be obtained is added2Slurry is in high speed point It dissipates and carries out high speed dispersion on machine, obtain monodispersed TiO2Slurry；3kg acrylic acid N, N- dimethylamino ethyl ester is weighed, is added 20kg absolute ethyl alcohols dilute, and the ethanol solution containing cationic monomer is slowly dropped to TiO2In slurry, stirs 30 minutes, obtain To surface through the modifies finely dispersed TiO of cation mono2Slurry；It will be by 60 kg of methyl methacrylate, dimethyl allene The mix monomer and water 80kg, initiator ammonium persulfate 1kg, emulsifier Nonyl pheno of sour glycol ester 10 kg compositions Ether ammonium sulfate 2kg carries out pre-emulsification, obtains pre-emulsification mix monomer lotion；By above-mentioned TiO2Slurry is heated to 80 DEG C, is added Then the good mix monomer lotion of pre-emulsification is slowly added into above-mentioned by 0.3kg initiator ammonium persulfates, initiation reaction 5 minutes TiO2In slurry, time control is added at 3 hours, 85 DEG C of maintenance isothermal reaction 1 hour after addition obtains surface through poly- The TiO of methyl methacrylate cladding2Slurries filtration, 105 DEG C are dried to obtain the titanium dioxide that can be used for organic glass by slurry Dry powder.
Embodiment 4
First to TiO2Surface modification is carried out, by 300kg anatase pigmentaries TiO2Powder is added in 1000kg water, is opened Dynamic blender stirring, makes TiO2Powder is evenly dispersed in water, and 1.5kg dispersants, the TiO that will be obtained is added2Slurry is in high speed point It dissipates and carries out high speed dispersion on machine, obtain monodispersed TiO2Slurry；3kg MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chlorides are weighed, Add 20kg absolute ethyl alcohols to dilute, the ethanol solution containing cationic monomer is slowly dropped to TiO2In slurry, stir 30 minutes, Surface is obtained through the modifies finely dispersed TiO of cation mono2Slurry；It will be by 60 kg of methyl methacrylate, dimethyl propylene The mix monomer and water 80kg, initiator ammonium persulfate 1kg, emulsifier polyoxyethylene nonyl phenyl second of olefin(e) acid glycol ester 10 kg compositions Alkene ether ammonium sulfate 2kg carries out pre-emulsification, obtains pre-emulsification mix monomer lotion；By above-mentioned TiO2Slurry is heated to 80 DEG C, adds Enter 0.3kg initiator ammonium persulfates, then the good mix monomer lotion of pre-emulsification is slowly added by initiation reaction 5 minutes The TiO stated2In slurry, time control is added at 4 hours, 85 DEG C of maintenance isothermal reaction 1 hour after addition obtains surface warp The TiO of polymethyl methacrylate cladding2Slurries filtration, 105 DEG C are dried to obtain the titanium dioxide that can be used for organic glass by slurry Titanium dry powder.
Embodiment 5
First to TiO2Surface modification is carried out, by 300kg anatase pigmentaries TiO2Powder is added in 1000kg water, is opened Dynamic blender stirring, makes TiO2Powder is evenly dispersed in water, and 1.5kg dispersants, the TiO that will be obtained is added2Slurry is in high speed point It dissipates and carries out high speed dispersion on machine, obtain monodispersed TiO2Slurry；3kg acrylyl oxy-ethyl-trimethyl salmiacs are weighed, are added 20kg absolute ethyl alcohols dilute, and the ethanol solution containing cationic monomer is slowly dropped to TiO2In slurry, stirs 30 minutes, obtain To surface through the modifies finely dispersed TiO of cation mono2Slurry；It will be by 60 kg of methyl methacrylate, dimethyl allene The mix monomer and water 80kg, initiator ammonium persulfate 1kg, emulsifier Nonyl pheno of sour glycol ester 10 kg compositions Ether ammonium sulfate 2kg carries out pre-emulsification, obtains pre-emulsification mix monomer lotion；By above-mentioned TiO2Slurry is heated to 80 DEG C, is added Then the good mix monomer lotion of pre-emulsification is slowly added into above-mentioned by 0.3kg initiator ammonium persulfates, initiation reaction 5 minutes TiO2In slurry, time control is added at 4.5 hours, 85 DEG C of maintenance isothermal reaction 1 hour after addition obtains surface warp The TiO of polymethyl methacrylate cladding2Slurries filtration, 105 DEG C are dried to obtain the titanium dioxide that can be used for organic glass by slurry Titanium dry powder.
Embodiment 6
First to TiO2Surface modification is carried out, by 300kg anatase pigmentaries TiO2Powder is added in 1000kg water, is opened Dynamic blender stirring, makes TiO2Powder is evenly dispersed in water, and 1.5kg dispersants, the TiO that will be obtained is added2Slurry is in high speed point It dissipates and carries out high speed dispersion on machine, obtain monodispersed TiO2Slurry；3kg acrylic acid N, N- dimethylamino ethyl ester is weighed, is added 20kg absolute ethyl alcohols dilute, and the ethanol solution containing cationic monomer is slowly dropped to TiO2In slurry, stirs 30 minutes, obtain To surface through the modifies finely dispersed TiO of cation mono2Slurry；It will be by 60 kg of methyl methacrylate, dimethyl allene The mix monomer and water 80kg, initiator ammonium persulfate 1kg, emulsifier Nonyl pheno of sour glycol ester 10 kg compositions Ether ammonium sulfate 2kg carries out pre-emulsification, obtains pre-emulsification mix monomer lotion；By above-mentioned TiO2Slurry is heated to 80 DEG C, is added Then the good mix monomer lotion of pre-emulsification is slowly added into above-mentioned by 0.3kg initiator ammonium persulfates, initiation reaction 5 minutes TiO2In slurry, time control is added at 3.5 hours, 85 DEG C of maintenance isothermal reaction 1 hour after addition obtains surface warp The TiO of polymethyl methacrylate cladding2Slurries filtration, 105 DEG C are dried to obtain the titanium dioxide that can be used for organic glass by slurry Titanium dry powder.

Claims (1)

1. a kind of preparation method of the special titanium dioxide of organic glass, it is characterised in that：First to TiO2Surface modification is carried out, is pressed Parts by weight meter is by 300 parts of TiO2Powder is added in 1000 parts of water, is started blender stirring, is made TiO2Powder is dispersed in water In, 1.5 parts of dispersants, the TiO that will be obtained is added2Slurry carries out high speed dispersion on high speed dispersor, obtains monodispersed TiO2 Slurry；3 parts of cationic monomers are weighed, adds 20 parts of absolute ethyl alcohol dilutions, the ethanol solution containing cationic monomer is slowly added dropwise To TiO2In slurry, stirs 30 minutes, obtain surface through the modifies finely dispersed TiO of cation mono2Slurry；
By by 80 parts of 60 parts of methyl methacrylate, 10 parts of mix monomers formed of ethylene glycol dimethacrylate and water, draw 2 parts of 1 part of agent ammonium persulfate, emulsifier progress pre-emulsifications are sent out, pre-emulsification mix monomer lotion is obtained；
By above-mentioned TiO2Slurry is heated to 80 DEG C, 0.3 part of initiator ammonium persulfate is added, initiation reaction 5 minutes then will be pre- The mix monomer lotion emulsified is slowly added into above-mentioned TiO2In slurry, time control is added at 2-5 hours, addition finishes 85 DEG C of maintenance isothermal reaction 1 hour afterwards, obtains the TiO that surface is coated through polymethyl methacrylate2Slurry, by slurries filtration, It is dried to obtain the titanium dioxide dry powder that can be used for organic glass；
The cationic monomer be MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, acrylyl oxy-ethyl-trimethyl salmiac, Acrylic acid N, N- dimethylamino ethyl ester is one such or two or more；
The emulsifier is nonylphenol polyoxyethylene ether ammonium sulfate；
The TiO2Powder is anatase pigmentary TiO2；
The dispersant is Sodium Polyacrylate.
CN201611253560.3A 2016-12-30 2016-12-30 A kind of preparation method of the special titanium dioxide of organic glass Active CN106633574B (en)

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