CN109021177A - A kind of preparation method of transparent wear organic glass - Google Patents
A kind of preparation method of transparent wear organic glass Download PDFInfo
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- CN109021177A CN109021177A CN201810769039.8A CN201810769039A CN109021177A CN 109021177 A CN109021177 A CN 109021177A CN 201810769039 A CN201810769039 A CN 201810769039A CN 109021177 A CN109021177 A CN 109021177A
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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
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/006—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polymers provided for in C08G18/00
- C08F283/008—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polymers provided for in C08G18/00 on to unsaturated polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4825—Polyethers containing two hydroxy groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4833—Polyethers containing oxyethylene units
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/08—Ingredients agglomerated by treatment with a binding agent
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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
- C08K2003/2244—Oxides; Hydroxides of metals of zirconium
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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)
- Polyurethanes Or Polyureas (AREA)
Abstract
The invention discloses a kind of preparation methods of transparent wear organic glass, include the following steps: that acrylonitrile, divinylbenzene, modified Nano zirconium oxide, dibutyl tin dilaurate, fire retardant, benzoyl peroxide are added in methyl methacrylate and are mixed, 70-80 DEG C of heating, insulated and stirred 30-40min, it is cooled to 30-35 DEG C, it places 2-3 days, is warming up to 90-100 DEG C, heat preservation 2-3h obtains transparent wear organic glass.The organic glass that the present invention is prepared has good wearability and the transparency.
Description
Technical field
The present invention relates to organic glass technical field more particularly to a kind of preparation methods of transparent wear organic glass
Background technique
Polymethyl methacrylate is also known as organic glass, has a preferable transparency, chemical stability, mechanical property and resistance to
The advantages that Hou Xing, easy dyeing, easy processing, attractive appearance, therefore be used widely.But organic glass is not wear-resisting, Ren Menchang
Increase the wearability of organic glass by adding specific filler, but often will be greatly reduced the transparency of organic glass, limits
The development of organic glass uses.
Summary of the invention
Technical problems based on background technology, the invention proposes a kind of preparation sides of transparent wear organic glass
Method, the organic glass that the present invention is prepared has good wearability and the transparency, and shock resistance is preferable.
A kind of preparation method of transparent wear organic glass proposed by the present invention, includes the following steps: acrylonitrile, diethyl
Methyl methacrylate is added in alkenyl benzene, modified Nano zirconium oxide, dibutyl tin dilaurate, fire retardant, benzoyl peroxide
Middle mixing heats up 70-80 DEG C, insulated and stirred 30-40min, is cooled to 30-35 DEG C, places 2-3 days, is warming up to 90-100 DEG C, protects
Warm 2-3h obtains transparent wear organic glass.
Preferably, in the preparation process of modified Nano zirconium oxide, in nitrogen atmosphere, by nano zircite and different Fo Er
Ketone diisocyanate mixes, and it is mixed that polyethylene glycol 2000, n,N-Dimethylaniline, toluene and dibutyl tin dilaurate is then added
Even, heating, insulated and stirred obtains prepolymer solution；Four amylalcohol triacrylate of season is added into polyurethane prepolymer solution, adjusts
Temperature is saved, insulated and stirred is in neutrality with pH is adjusted, and removing toluene is evaporated under reduced pressure and obtains modified Nano zirconium oxide.
Preferably, in the preparation process of modified Nano zirconium oxide, in nitrogen atmosphere, by nano zircite and different Fo Er
Ketone diisocyanate mixes, and it is mixed that polyethylene glycol 2000, n,N-Dimethylaniline, toluene and dibutyl tin dilaurate is then added
It is even, it is warming up to 75-80 DEG C, insulated and stirred 1-2h obtains prepolymer solution；Four amylalcohol of season is added into polyurethane prepolymer solution
Triacrylate adjusts the temperature to 60-65 DEG C, insulated and stirred 4-5h, adjusts pH with triethylamine and is in neutrality, is evaporated under reduced pressure and removes first
Benzene obtains modified Nano zirconium oxide.
Preferably, acrylonitrile, divinylbenzene, modified Nano zirconium oxide, dibutyl tin dilaurate, fire retardant, peroxide
Change benzoyl, the weight ratio of methyl methacrylate is 10-15:10-15:25-35:0.1-0.2:10-15:2-3:100.
Preferably, in the preparation process of modified Nano zirconium oxide, nano zircite, gathers at isophorone diisocyanate
Ethylene glycol 2000, N, the weight ratio of accelerine are 8-12:20-25:30-33:5-7.
Preferably, in the preparation process of modified Nano zirconium oxide, isophorone diisocyanate, di lauric dibutyl
Tin, four amylalcohol triacrylate of season, toluene weight ratio be 20-25:0.1-0.2:7-9:80-100.
Preferably, fire retardant is organic silicon fibre retardant FS2030C and organic silicon fibre retardant FS2050C.
The present invention mixes nano zircite and isophorone diisocyanate, then with polyethylene glycol 2000, N, N- bis-
Pet reaction occurs for methylaniline, and nano zircite surface contains great amount of hydroxy group, can react, make with isophorone diisocyanate
It obtains nano zircite to be grafted on polyurethane, then is reacted with four amylalcohol triacrylate of season and introduce multiple carbon at the both ends of polyurethane
Carbon double bond, then with acrylonitrile, divinylbenzene, methyl methacrylate in dibutyl tin dilaurate, benzoyl peroxide
The lower copolymerization of effect, which forms complex network and wears, to be connect, and nano zircite is uniformly distributed therein, and nano zircite and polyurethane have
There are good hardness, wearability, shock resistance, the hardness of organic glass can be improved, greatly increases the wear-resisting of organic glass
Property and shock resistance, and the modified Nano zirconium oxide of appropriate amount is added, the transparency of organic glass can be kept；It is added third
Alkene nitrile, divinylbenzene introduce the polar group and phenyl group of appropriate level in organic glass, further increase of the invention
Hardness, wearability；Acrylonitrile, divinylbenzene and the methyl methacrylate copolymer of Optimum Contents, can keep organic glass
The transparency；Organic silicon fibre retardant FS2030C and organic silicon fibre retardant FS2050C cooperates, and can greatly increase the present invention
Anti-flammability, and the transparency of the invention will not be reduced；The present invention is cooperated by each object, so that the present invention was prepared
Organic glass has good wearability and keeps higher transparency, and shock resistance is preferable.
Specific embodiment
In the following, technical solution of the present invention is described in detail by specific embodiment.
Embodiment 1
A kind of preparation method of transparent wear organic glass, includes the following steps: acrylonitrile, divinylbenzene, modification
Nano zircite, dibutyl tin dilaurate, fire retardant, benzoyl peroxide are added in methyl methacrylate and mix, and heat up
75 DEG C, insulated and stirred 35min, 32.5 DEG C are cooled to, is placed 2.5 days, is warming up to 95 DEG C, it is organic that heat preservation 2.5h obtains transparent wear
Glass.
Embodiment 2
A kind of preparation method of transparent wear organic glass, includes the following steps: acrylonitrile, divinylbenzene, modification
Nano zircite, dibutyl tin dilaurate, fire retardant, benzoyl peroxide are added in methyl methacrylate and mix, and heat up
70 DEG C, insulated and stirred 40min, 30 DEG C are cooled to, is placed 3 days, is warming up to 90 DEG C, heat preservation 3h obtains transparent wear organic glass；
Wherein, in the preparation process of modified Nano zirconium oxide, in nitrogen atmosphere, by nano zircite and isophorone
Diisocyanate mixes, and it is mixed that polyethylene glycol 2000, n,N-Dimethylaniline, toluene and dibutyl tin dilaurate is then added
It is even, 75 DEG C are warming up to, insulated and stirred 2h obtains prepolymer solution；Four amylalcohol of season, three propylene is added into polyurethane prepolymer solution
Acid esters adjusts the temperature to 60 DEG C, insulated and stirred 5h, adjusts pH with triethylamine and is in neutrality, and removing toluene is evaporated under reduced pressure and is modified
Nano zircite.
Embodiment 3
A kind of preparation method of transparent wear organic glass, includes the following steps: acrylonitrile, divinylbenzene, modification
Nano zircite, dibutyl tin dilaurate, fire retardant, benzoyl peroxide are added in methyl methacrylate and mix, and heat up
80 DEG C, insulated and stirred 30min, 35 DEG C are cooled to, is placed 2 days, is warming up to 100 DEG C, heat preservation 2h obtains transparent wear organic glass；
Wherein, in the preparation process of modified Nano zirconium oxide, in nitrogen atmosphere, by nano zircite and isophorone
Diisocyanate mixes, and it is mixed that polyethylene glycol 2000, n,N-Dimethylaniline, toluene and dibutyl tin dilaurate is then added
It is even, 80 DEG C are warming up to, insulated and stirred 1h obtains prepolymer solution；Four amylalcohol of season, three propylene is added into polyurethane prepolymer solution
Acid esters adjusts the temperature to 65 DEG C, insulated and stirred 4h, adjusts pH with triethylamine and is in neutrality, and removing toluene is evaporated under reduced pressure and is modified
Nano zircite, wherein nano zircite, isophorone diisocyanate, polyethylene glycol 2000, n,N-Dimethylaniline weight
Amount is than being 12:20:33:5 isophorone diisocyanate, dibutyl tin dilaurate, four amylalcohol triacrylate of season, toluene
Weight ratio is 25:0.1:9:80.
Embodiment 4
A kind of preparation method of transparent wear organic glass, includes the following steps: acrylonitrile, divinylbenzene, modification
Nano zircite, dibutyl tin dilaurate, fire retardant, benzoyl peroxide are added in methyl methacrylate and mix, and heat up
72 DEG C, insulated and stirred 37min, 32 DEG C are cooled to, is placed 3 days, is warming up to 92 DEG C, heat preservation 2.7h obtains the organic glass of transparent wear
Glass；
Wherein, in the preparation process of modified Nano zirconium oxide, in nitrogen atmosphere, by nano zircite and isophorone
Diisocyanate mixes, and it is mixed that polyethylene glycol 2000, n,N-Dimethylaniline, toluene and dibutyl tin dilaurate is then added
It is even, 76 DEG C are warming up to, insulated and stirred 1.8h obtains prepolymer solution；Four amylalcohol 3 third of season is added into polyurethane prepolymer solution
Olefin(e) acid ester adjusts the temperature to 61 DEG C, insulated and stirred 4.7h, adjusts pH with triethylamine and is in neutrality, and removing toluene is evaporated under reduced pressure and obtains
Modified Nano zirconium oxide, wherein nano zircite, isophorone diisocyanate, polyethylene glycol 2000, n,N-Dimethylaniline
Weight ratio be 8:25:30:7, isophorone diisocyanate, dibutyl tin dilaurate, four amylalcohol triacrylate of season, first
The weight ratio of benzene is 20:0.2:7:100；
Acrylonitrile, divinylbenzene, modified Nano zirconium oxide, dibutyl tin dilaurate, fire retardant, benzoyl peroxide first
Acyl, methyl methacrylate weight ratio be 10:15:25:0.2:10:3:100.
Embodiment 5
A kind of preparation method of transparent wear organic glass, includes the following steps: acrylonitrile, divinylbenzene, modification
Nano zircite, dibutyl tin dilaurate, fire retardant, benzoyl peroxide are added in methyl methacrylate and mix, and heat up
78 DEG C, insulated and stirred 33min, 33 DEG C are cooled to, is placed 2 days, is warming up to 98 DEG C, heat preservation 2.3h obtains the organic glass of transparent wear
Glass；
Wherein, in the preparation process of modified Nano zirconium oxide, in nitrogen atmosphere, by nano zircite and isophorone
Diisocyanate mixes, and it is mixed that polyethylene glycol 2000, n,N-Dimethylaniline, toluene and dibutyl tin dilaurate is then added
It is even, 78 DEG C are warming up to, insulated and stirred 1.2h obtains prepolymer solution；Four amylalcohol 3 third of season is added into polyurethane prepolymer solution
Olefin(e) acid ester adjusts the temperature to 63 DEG C, insulated and stirred 4.3h, adjusts pH with triethylamine and is in neutrality, and removing toluene is evaporated under reduced pressure and obtains
Modified Nano zirconium oxide, wherein nano zircite, isophorone diisocyanate, polyethylene glycol 2000, n,N-Dimethylaniline
Weight ratio be 10:22:32:6, isophorone diisocyanate, dibutyl tin dilaurate, four amylalcohol triacrylate of season,
The weight ratio of toluene is 22:0.12:8:90；
Acrylonitrile, divinylbenzene, modified Nano zirconium oxide, dibutyl tin dilaurate, fire retardant, benzoyl peroxide first
Acyl, methyl methacrylate weight ratio be 15:10:35:0.1:15:2:100；
Fire retardant is organic silicon fibre retardant FS2030C and organic silicon fibre retardant FS2050C.
Test example 1
Embodiment 5 is tested for the property, and using common organic glass as control group, as a result as follows:
It is good that organic glass wearability is prepared in the present invention as can be seen from the above table, transparent good, anti-flammability and shock resistance
Better performances.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (7)
1. a kind of preparation method of transparent wear organic glass, which comprises the steps of: by acrylonitrile, divinyl
Base benzene, modified Nano zirconium oxide, dibutyl tin dilaurate, fire retardant, benzoyl peroxide are added in methyl methacrylate
It mixes, heats up 70-80 DEG C, insulated and stirred 30-40min, be cooled to 30-35 DEG C, place 2-3 days, be warming up to 90-100 DEG C, heat preservation
2-3h obtains transparent wear organic glass.
2. the preparation method of transparent wear organic glass according to claim 1, which is characterized in that in modified Nano zirconium oxide
Preparation process in, in nitrogen atmospheres, nano zircite and isophorone diisocyanate are mixed, poly- second two is then added
Alcohol 2000, n,N-Dimethylaniline, toluene and dibutyl tin dilaurate mix, and heating, insulated and stirred obtains prepolymer solution；
Four amylalcohol triacrylate of season is added into polyurethane prepolymer solution, adjusts temperature, insulated and stirred is in neutrality with pH is adjusted,
Removing toluene is evaporated under reduced pressure and obtains modified Nano zirconium oxide.
3. the preparation method of transparent wear organic glass according to claim 1 or claim 2, which is characterized in that in modified Nano oxygen
In the preparation process for changing zirconium, in nitrogen atmosphere, nano zircite and isophorone diisocyanate are mixed, are then added poly-
Ethylene glycol 2000, n,N-Dimethylaniline, toluene and dibutyl tin dilaurate mix, and are warming up to 75-80 DEG C, insulated and stirred 1-
2h obtains prepolymer solution；Four amylalcohol triacrylate of season is added into polyurethane prepolymer solution, adjusts the temperature to 60-65
DEG C, insulated and stirred 4-5h adjusts pH with triethylamine and is in neutrality, and removing toluene is evaporated under reduced pressure and obtains modified Nano zirconium oxide.
4. the preparation method of any one of -3 transparent wear organic glasses according to claim 1, which is characterized in that acrylonitrile,
Divinylbenzene, modified Nano zirconium oxide, dibutyl tin dilaurate, fire retardant, benzoyl peroxide, methyl methacrylate
Weight ratio be 10-15:10-15:25-35:0.1-0.2:10-15:2-3:100.
5. the preparation method of transparent wear organic glass according to Claims 2 or 3, which is characterized in that in modified Nano oxygen
In the preparation process for changing zirconium, nano zircite, isophorone diisocyanate, polyethylene glycol 2000, n,N-Dimethylaniline
Weight ratio is 8-12:20-25:30-33:5-7.
6. the preparation method of transparent wear organic glass according to Claims 2 or 3, which is characterized in that in modified Nano oxygen
In the preparation process for changing zirconium, isophorone diisocyanate, dibutyl tin dilaurate, four amylalcohol triacrylate of season, toluene
Weight ratio be 20-25:0.1-0.2:7-9:80-100.
7. the preparation method of any one of -6 transparent wear organic glasses according to claim 1, which is characterized in that fire retardant is
Organic silicon fibre retardant FS2030C and organic silicon fibre retardant FS2050C.
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| CN201810769039.8A CN109021177A (en) | 2018-07-13 | 2018-07-13 | A kind of preparation method of transparent wear organic glass |
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