CN106633574A - Preparation method of special titanium dioxide for organic glass - Google Patents
Preparation method of special titanium dioxide for organic glass Download PDFInfo
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- CN106633574A CN106633574A CN201611253560.3A CN201611253560A CN106633574A CN 106633574 A CN106633574 A CN 106633574A CN 201611253560 A CN201611253560 A CN 201611253560A CN 106633574 A CN106633574 A CN 106633574A
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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
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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
- 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
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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
- 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
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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
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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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
- 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 preparation method of special titanium dioxide for organic glass is characterized in that firstly, TiO2 is subjected to surface modification with a cationic monomer, then a mixed monomer consisting of 60 parts of methyl methacrylate and 10 parts of ethylene glycol dimethacrylate, 80 parts of water, 1 part of an initiator, namely, ammonium persulfate and 2 parts of an emulsifier are pre-emulsified, and a pre-emulsified mixed monomer emulsion is obtained; 0.3 parts of the initiator, namely, ammonium persulfate is added to TiO2 slurry at 80 DEG C for an initiation reaction for 5 min, then the pre-emulsified mixed monomer emulsion is slowly added to the TiO2 slurry for 2-5 h, the mixture reacts at the constant temperature of 85 DEG C for 1 h after addition, and TiO2 slurry with the surface coated with polymethyl methacrylate is obtained, and dry powder of titanium dioxide for organic glass is obtained after the slurry is filtered and dried.
Description
Technical field
The present invention relates to a kind of preparation method of the special titanium dioxide of lucite.
Background technology
Polymethyl methacrylate is commonly referred to lucite, english abbreviation PMMA, with the high grade of transparency, low price, easily
It is usually commonly used glass alternative materials the advantages of machining.Lucite is to develop a kind of important heat earlier
Thermoplastic plastic, with the transparency, stability and weatherability, easy dyeing, easy processing, attractive appearance, has extensively in building industry
Application.1. heigh clarity.Lucite is macromolecule transparent material most excellent at present, and light transmittance reaches lucite
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 does, this is because quartzy energy
Completely through ultraviolet.Simple glass can only pass through 0.6% ultraviolet, but lucite can pass through 73%.2. mechanical strength
It is high.The relative molecular mass of lucite is about 2,000,000, is the macromolecular compound of long-chain, and forms the chain of molecule very
Softness, therefore, the intensity of lucite is higher, and stretch-proof and shock proof ability are higher than simple glass 7-18 times.There is one kind
Through heating and the lucite of stretch processing, molecule segment therein arranges to obtain unusual orderliness, and making the toughness of material has
Significantly improve.Followed closely into this lucite with nail, even if nail breaks through, also do not cracked on lucite.It is this to have
Machine glass quilt attack equally will not go to pieces after wearing.Therefore, the lucite of stretch processing can be used as bulletproof glass, also use
Make the canopy on military aircraft.3. it is lightweight.The density of lucite is 1.18g/cm3;, an equal amount of material, its is heavy
Amount only has the half of simple glass, metallic aluminium（Belong to light metal）43%.4. it is easy to process.Lucite can not only use lathe
Cut, drilling machine is drilled, and variously-shaped utensil can be bonded to acetone, chloroform etc., also can be with blowing, note
The method of the plastic shaping such as penetrating, extrude is processed into greatly to canopy, little to the panoramic product such as artificial tooth and denture fixing device.
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, the covering power of titanium dioxide can be greatly affected after reunion.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 particle is reunited again, and the use range of titanium dioxide is widely, and use occasion varies, slightly
Will result in scattered particle accidentally to reunite again, 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, and the covering power for making titanium dioxide obtains bigger
Play.
A kind of preparation method of the special titanium dioxide of lucite of the present invention, a kind of special titanium dioxide of lucite.For
The weatherability and opacity of lucite are improved, generally requires that titanium dioxide is added in lucite, due to organic
The particularity of process of glass, and common titanium dioxide may not apply to lucite at all, the present invention is in titanium dioxide
The polymethyl methacrylate of Surface coating crosslinking, the polymethyl methacrylate of crosslinking will not be by organic hyaline monomer destruction
Can be well dispersed in lucite.
In order that polymer covering layer can preferably be combined with titanium dioxide surface, the present invention first with the sun with double bond from
Sub- monomer is modified to titanium dioxide surface, and modified mechanism is：Titanium dioxide surface is per se with substantial amounts of negative electrical charge, band
Cationic monomer one end of double bond carries positive charge, and by charge effect titanium dioxide surface is adsorbed onto, and 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,
GDMA copolymer, finally obtained the titanium dioxide of Surface coating polymethyl methacrylate.
The content of the invention
A kind of preparation method of the special titanium dioxide of lucite, it is characterised in that：First to TiO2Carry out surface to be modified,
By weight by 300 parts of TiO2Powder is added in 1000 parts of water, starts agitator stirring, makes TiO2Powder is dispersed in
In water, 1.5 parts of dispersants are added, by the TiO for obtaining2Slurry carries out high speed dispersion on high speed dispersor, obtains monodispersed
TiO2Slurry；3 parts of cationic monomers, plus 20 parts of absolute ethyl alcohol dilutions are weighed, the ethanol solution containing cationic monomer is slow
It is added drop-wise to TiO2In slurry, stir 30 minutes, obtain the modifies finely dispersed TiO of surface Jing cation monos2Slurry；
By by 80 parts of 60 parts of methyl methacrylate, 10 parts of mix monomers for constituting of GDMA and water, draw
Sending out 1 part of agent ammonium persulfate, 2 parts of emulsifying agent carries out pre-emulsification, obtains pre-emulsification mix monomer emulsion；
By above-mentioned TiO2Slurry is heated to 80 DEG C, adds 0.3 part of initiator ammonium persulfate, and initiation reaction 5 minutes then will be pre-
The mix monomer emulsion for having emulsified is slowly added into above-mentioned TiO2In slurry, add time control in 2-5 hours, addition is finished
85 DEG C of maintenance isothermal reaction 1 hour afterwards, obtains the TiO of surface Jing polymethyl methacrylate claddings2Slurry, by slurries filtration,
It is dried to obtain the titanium dioxide dry powder that can be used for lucite；
Described cationic monomer be MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, acrylyl oxy-ethyl-trimethyl salmiac,
Acrylic acid N, N- dimethylamino ethyl ester it is therein one or more；
Described emulsifying agent is NPE ammonium sulfate；
Described TiO2Powder is anatase pigmentary TiO2；
Described dispersant is PAA.
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, 1.5kg dispersants is added, by the TiO for obtaining2Slurry is in high speed dispersor
On carry out high speed dispersion, obtain monodispersed TiO2Slurry；3kg MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chlorides are weighed, plus
20kg absolute ethyl alcohols dilute, and the ethanol solution containing cationic monomer is slowly dropped to into TiO2In slurry, stir 30 minutes, obtain
To the modifies finely dispersed TiO of surface Jing cation monos2Slurry；Will be by the kg of methyl methacrylate 60, dimethyl allene
The mix monomer and water 80kg, initiator ammonium persulfate 1kg, emulsifying agent Nonyl pheno of the kg of sour glycol ester 10 compositions
Ether ammonium sulfate 2kg carries out pre-emulsification, obtains pre-emulsification mix monomer emulsion；By above-mentioned TiO2Slurry is heated to 80 DEG C, adds
Then 0.3kg initiator ammonium persulfates, initiation reaction 5 minutes is slowly added into the good mix monomer emulsion of pre-emulsification above-mentioned
TiO2In slurry, time control is added at 2 hours, add 85 DEG C of maintenance isothermal reaction 1 hour after finishing, obtain surface Jing and gather
The TiO of methyl methacrylate cladding2Slurry, slurries filtration, 105 DEG C are dried to obtain the titanium dioxide that can be used for lucite
Dry powder.
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, 1.5kg dispersants is added, by the TiO for obtaining2Slurry is in high speed dispersor
On carry out high speed dispersion, obtain monodispersed TiO2Slurry；Weigh 3kg acrylyl oxy-ethyl-trimethyl salmiacs, plus 20kg without
Water-ethanol dilutes, and the ethanol solution containing cationic monomer is slowly dropped to into TiO2In slurry, stir 30 minutes, obtain surface
The modifies finely dispersed TiO of Jing cation monos2Slurry；Will be by the kg of methyl methacrylate 60, dimethacrylate second two
The mix monomer and water 80kg, initiator ammonium persulfate 1kg, emulsifying agent NPE sulfuric acid of the kg of alcohol ester 10 compositions
Ammonium 2kg carries out pre-emulsification, obtains pre-emulsification mix monomer emulsion；By above-mentioned TiO2Slurry is heated to 80 DEG C, adds 0.3kg to draw
Agent ammonium persulfate is sent out, then the good mix monomer emulsion of pre-emulsification is slowly added into above-mentioned TiO by initiation reaction 5 minutes2Slurry
In material, time control is added at 5 hours, add 85 DEG C of maintenance isothermal reaction 1 hour after finishing, obtain surface Jing polymethyls
The TiO of sour methyl esters cladding2Slurry, slurries filtration, 105 DEG C are dried to obtain the titanium dioxide dry powder that can be used for lucite.
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, 1.5kg dispersants is added, by the TiO for obtaining2Slurry is in high speed dispersor
On carry out high speed dispersion, obtain monodispersed TiO2Slurry；Weigh 3kg acrylic acid N, N- dimethylamino ethyl esters, plus 20kg without
Water-ethanol dilutes, and the ethanol solution containing cationic monomer is slowly dropped to into TiO2In slurry, stir 30 minutes, obtain surface
The modifies finely dispersed TiO of Jing cation monos2Slurry；Will be by the kg of methyl methacrylate 60, dimethacrylate second two
The mix monomer and water 80kg, initiator ammonium persulfate 1kg, emulsifying agent NPE sulfuric acid of the kg of alcohol ester 10 compositions
Ammonium 2kg carries out pre-emulsification, obtains pre-emulsification mix monomer emulsion；By above-mentioned TiO2Slurry is heated to 80 DEG C, adds 0.3kg to draw
Agent ammonium persulfate is sent out, then the good mix monomer emulsion of pre-emulsification is slowly added into above-mentioned TiO by initiation reaction 5 minutes2Slurry
In material, time control is added at 3 hours, add 85 DEG C of maintenance isothermal reaction 1 hour after finishing, obtain surface Jing polymethyls
The TiO of sour methyl esters cladding2Slurry, slurries filtration, 105 DEG C are dried to obtain the titanium dioxide dry powder that can be used for lucite.
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, 1.5kg dispersants is added, by the TiO for obtaining2Slurry is in high speed dispersor
On carry out high speed dispersion, obtain monodispersed TiO2Slurry；3kg MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chlorides are weighed, plus
20kg absolute ethyl alcohols dilute, and the ethanol solution containing cationic monomer is slowly dropped to into TiO2In slurry, stir 30 minutes, obtain
To the modifies finely dispersed TiO of surface Jing cation monos2Slurry；Will be by the kg of methyl methacrylate 60, dimethyl allene
The mix monomer and water 80kg, initiator ammonium persulfate 1kg, emulsifying agent Nonyl pheno of the kg of sour glycol ester 10 compositions
Ether ammonium sulfate 2kg carries out pre-emulsification, obtains pre-emulsification mix monomer emulsion；By above-mentioned TiO2Slurry is heated to 80 DEG C, adds
Then 0.3kg initiator ammonium persulfates, initiation reaction 5 minutes is slowly added into the good mix monomer emulsion of pre-emulsification above-mentioned
TiO2In slurry, time control is added at 4 hours, add 85 DEG C of maintenance isothermal reaction 1 hour after finishing, obtain surface Jing and gather
The TiO of methyl methacrylate cladding2Slurry, slurries filtration, 105 DEG C are dried to obtain the titanium dioxide that can be used for lucite
Dry powder.
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, 1.5kg dispersants is added, by the TiO for obtaining2Slurry is in high speed dispersor
On carry out high speed dispersion, obtain monodispersed TiO2Slurry；Weigh 3kg acrylyl oxy-ethyl-trimethyl salmiacs, plus 20kg without
Water-ethanol dilutes, and the ethanol solution containing cationic monomer is slowly dropped to into TiO2In slurry, stir 30 minutes, obtain surface
The modifies finely dispersed TiO of Jing cation monos2Slurry；Will be by the kg of methyl methacrylate 60, dimethacrylate second two
The mix monomer and water 80kg, initiator ammonium persulfate 1kg, emulsifying agent NPE sulfuric acid of the kg of alcohol ester 10 compositions
Ammonium 2kg carries out pre-emulsification, obtains pre-emulsification mix monomer emulsion；By above-mentioned TiO2Slurry is heated to 80 DEG C, adds 0.3kg to draw
Agent ammonium persulfate is sent out, then the good mix monomer emulsion of pre-emulsification is slowly added into above-mentioned TiO by initiation reaction 5 minutes2Slurry
In material, time control is added at 4.5 hours, add 85 DEG C of maintenance isothermal reaction 1 hour after finishing, obtain the poly- methyl-props of surface Jing
The TiO of e pioic acid methyl ester cladding2Slurry, slurries filtration, 105 DEG C are dried to obtain the titanium dioxide dry powder that can be used for lucite.
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, 1.5kg dispersants is added, by the TiO for obtaining2Slurry is in high speed dispersor
On carry out high speed dispersion, obtain monodispersed TiO2Slurry；Weigh 3kg acrylic acid N, N- dimethylamino ethyl esters, plus 20kg without
Water-ethanol dilutes, and the ethanol solution containing cationic monomer is slowly dropped to into TiO2In slurry, stir 30 minutes, obtain surface
The modifies finely dispersed TiO of Jing cation monos2Slurry；Will be by the kg of methyl methacrylate 60, dimethacrylate second two
The mix monomer and water 80kg, initiator ammonium persulfate 1kg, emulsifying agent NPE sulfuric acid of the kg of alcohol ester 10 compositions
Ammonium 2kg carries out pre-emulsification, obtains pre-emulsification mix monomer emulsion；By above-mentioned TiO2Slurry is heated to 80 DEG C, adds 0.3kg to draw
Agent ammonium persulfate is sent out, then the good mix monomer emulsion of pre-emulsification is slowly added into above-mentioned TiO by initiation reaction 5 minutes2Slurry
In material, time control is added at 3.5 hours, add 85 DEG C of maintenance isothermal reaction 1 hour after finishing, obtain the poly- methyl-props of surface Jing
The TiO of e pioic acid methyl ester cladding2Slurry, slurries filtration, 105 DEG C are dried to obtain the titanium dioxide dry powder that can be used for lucite.
Claims (1)
1. the preparation method of the special titanium dioxide of a kind of lucite, it is characterised in that：First to TiO2Carry out surface to be modified, press
Weight portion meter is by 300 parts of TiO2Powder is added in 1000 parts of water, starts agitator stirring, makes TiO2Powder is dispersed in water
In, 1.5 parts of dispersants are added, by the TiO for obtaining2Slurry carries out high speed dispersion on high speed dispersor, obtains monodispersed TiO2
Slurry；3 parts of cationic monomers, plus 20 parts of absolute ethyl alcohol dilutions are weighed, the ethanol solution containing cationic monomer is slowly added dropwise
To TiO2In slurry, stir 30 minutes, obtain the modifies finely dispersed TiO of surface Jing cation monos2Slurry；
By by 80 parts of 60 parts of methyl methacrylate, 10 parts of mix monomers for constituting of GDMA and water, draw
Sending out 1 part of agent ammonium persulfate, 2 parts of emulsifying agent carries out pre-emulsification, obtains pre-emulsification mix monomer emulsion；
By above-mentioned TiO2Slurry is heated to 80 DEG C, adds 0.3 part of initiator ammonium persulfate, and initiation reaction 5 minutes then will be pre-
The mix monomer emulsion for having emulsified is slowly added into above-mentioned TiO2In slurry, add time control in 2-5 hours, addition is finished
85 DEG C of maintenance isothermal reaction 1 hour afterwards, obtains the TiO of surface Jing polymethyl methacrylate claddings2Slurry, by slurries filtration,
It is dried to obtain the titanium dioxide dry powder that can be used for lucite；
Described cationic monomer be MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, acrylyl oxy-ethyl-trimethyl salmiac,
Acrylic acid N, N- dimethylamino ethyl ester it is therein one or more；
Described emulsifying agent is NPE ammonium sulfate；
Described TiO2Powder is anatase pigmentary TiO2；
Described dispersant is PAA.
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| CN201611253560.3A CN106633574B (en) | 2016-12-30 | 2016-12-30 | A kind of preparation method of the special titanium dioxide of organic glass |
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| CN201611253560.3A CN106633574B (en) | 2016-12-30 | 2016-12-30 | A kind of preparation method of the special titanium dioxide of organic glass |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107815051A (en) * | 2017-11-11 | 2018-03-20 | 蚌埠承永玻璃制品有限公司 | A kind of processing method for improving lucite quality |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1955218A (en) * | 2006-10-27 | 2007-05-02 | 四川大学 | Preparation method of ultraviolet light stabilizer |
| WO2009110848A1 (en) * | 2008-03-04 | 2009-09-11 | Agency For Science, Technology And Research | Low shrinkage multifunctional ssq resins |
| WO2009141057A1 (en) * | 2008-05-23 | 2009-11-26 | Merck Patent Gmbh | Polymerisation method for producing core-shell particles |
| CN102558412A (en) * | 2012-02-10 | 2012-07-11 | 北京理工大学 | Preparation method of high-strength titanium dioxide nano-grade composite hydrogel |
-
2016
- 2016-12-30 CN CN201611253560.3A patent/CN106633574B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1955218A (en) * | 2006-10-27 | 2007-05-02 | 四川大学 | Preparation method of ultraviolet light stabilizer |
| WO2009110848A1 (en) * | 2008-03-04 | 2009-09-11 | Agency For Science, Technology And Research | Low shrinkage multifunctional ssq resins |
| WO2009141057A1 (en) * | 2008-05-23 | 2009-11-26 | Merck Patent Gmbh | Polymerisation method for producing core-shell particles |
| CN102558412A (en) * | 2012-02-10 | 2012-07-11 | 北京理工大学 | Preparation method of high-strength titanium dioxide nano-grade composite hydrogel |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107815051A (en) * | 2017-11-11 | 2018-03-20 | 蚌埠承永玻璃制品有限公司 | A kind of processing method for improving lucite quality |
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