CN108912575A - A kind of preparation method of anti-ultraviolet radiation organic glass - Google Patents
A kind of preparation method of anti-ultraviolet radiation organic glass Download PDFInfo
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- CN108912575A CN108912575A CN201810464746.6A CN201810464746A CN108912575A CN 108912575 A CN108912575 A CN 108912575A CN 201810464746 A CN201810464746 A CN 201810464746A CN 108912575 A CN108912575 A CN 108912575A
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- organic glass
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L33/00—Compositions of homopolymers or copolymers 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 of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- C08L33/04—Homopolymers or copolymers of esters
- C08L33/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, which oxygen atoms are present only as part of the carboxyl radical
- C08L33/10—Homopolymers or copolymers of methacrylic acid esters
- C08L33/12—Homopolymers or copolymers of methyl methacrylate
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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
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
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Abstract
The invention discloses a kind of preparation methods of anti-ultraviolet radiation organic glass,By polymethyl methacrylate,Rice husk,Iron powder,Sodium fluoride,Maleic anhydride,Benzoyl peroxide,Nano zine oxide,Silane coupling reagent KH-570,2,2- azodiisobutyronitrile,The raw materials such as one hydronium(ion) lithia are made,The present invention introduces rice case fibre in the preparation of organic glass,Silica therein is under the catalysis of sodium fluoride and nanometer iron powder,Silicon carbide contents are generated with carbon,Improve the wearability and heat resistance of organic glass,It is modified that surface is carried out using Nano-zinc Oxide by Silane Coupling Agents on this basis,Recycle in-situ polymerization that nano zine oxide is compound with polymethyl methacrylate,The insertion of nano zine oxide is realized by simple controllable condition at a lower temperature,To which the uvioresistant performance of organic glass greatly improved,Its ultraviolet shielded rate is more than 97%,Use as uvioresistant glass is in all kinds of buildings,Equipment etc. all has preferable application prospect.
Description
Technical field
The present invention relates to technical field of polymer materials more particularly to a kind of preparation sides of anti-ultraviolet radiation organic glass
Method.
Background technique
Organic glass is abbreviated as PMMA, and chemical name is polymethyl methacrylate, is a kind of unformed heat of high transparency
Thermoplastic plastic since it has certain physical mechanical property, thus is widely used in agricultural, aviation, building, optics instrument
The fields such as device.Translucency is best in the plastic, and relative density is smaller, and anti-fragmentation performance is good, and mechanical strength and toughness are greater than silicon glass
10 times of glass or more, there is weatherability outstanding and resistance to ag(e)ing, under low temperature and higher temperature, impact strength is constant, chemistry
Performance is stablized, can general chemical corrosion resistance.But compared with other transparent plastics, organic glass also has scratch resistance poor, heat-resisting
The disadvantages of temperature is low, impact strength is low, polymerization technique is complicated, this is limited its scope of application to a certain extent.Using list
The organic glass that monomethyl methyl acrylate homopolymerization obtains often is unable to satisfy the requirement of property, and must be by organic
Glass carries out deep processing to improve the performance of organic glass.
Since the translucency of organic glass is splendid, it is seen that light transmission rate up to 92%, uv transmittance up to 73%, for
2800nm infrared light transmittance below is also preferable, this allows for being unfavorable for organic glass in the place for needing to prevent radiation
Use, the especially radiation of ultraviolet light excessively irradiates the serious health for affecting human body, if people are by this wave band purple
Skin rapid aging, skin turgor or can play blister after UV radiation, or even suffer from lupus erythematosus and skin cancer, and traditional organic glass
There is no systematic research for anti-ultraviolet radiation.
Nano zine oxide has excellent chemical stability, is a kind of cheap multifunctional inorganic filler, with anti-purple
Many performances such as external radiation, luminescence generated by light, photocatalysis, antibacterial, but since the surface of nano granular of zinc oxide can relatively high, surface
Tension enhancing is easy to reunite, and is added directly into polymeric matrix and is difficult to evenly dispersed, is unable to reach expected using effect
Fruit.Nano zine oxide is different from the polarity of polymethyl methacrylate simultaneously, and poor compatibility is easy to produce and mutually separates, and passes through letter
Often transparency is lower for obtained material in conjunction with polymethyl methacrylate by nano zine oxide for single blending method, affects reality
The property used.
Summary of the invention
The object of the invention is to remedy the disadvantages of known techniques, provides a kind of preparation of anti-ultraviolet radiation organic glass
Method.
The present invention is achieved by the following technical solutions：
A kind of preparation method of anti-ultraviolet radiation organic glass, includes the following steps：
（1）Crushed 60-80 mesh after rice husk is dried, after oxidative decoloration by it with iron powder, sodium fluoride in mass ratio（75-
78）：（0.5-1）：（1-3）Mixing is sent into calcining furnace, is warming up to 380-420 DEG C, is reacted 2-3 hours, cooling after the completion to take out
It is spare；
（2）In mass ratio by nano zine oxide, Silane coupling reagent KH-570 and 75% ethanol water（20-25）：（1-2）：
（300-350）Magnetic agitation 30-40 minutes after mixing, re-ultrasonic dispersion 20-30 minutes, mixed liquor is placed in 80-90 after the completion
It flows back 90-120 minutes in DEG C oil bath, cools down, be respectively washed 2-3 times with ethyl alcohol and clear water later, vacuum is dry at 100-110 DEG C
5-10 hours dry, ground 80-100 mesh is spare；
（3）In mass ratio by step 2 products therefrom, polymethyl methacrylate, 2,2- azodiisobutyronitrile（2-3）：（85-
95）：（6-8）It is dissolved in ethanol solution at 30-35 DEG C after mixing, hydronium(ion) oxidation is added thereto again after mixing evenly
Lithium, while it being warming up to 75-85 DEG C, return stirring reacts 120-150 minutes, after the completion by gained mixed liquor in 50-60 DEG C of air blast
It is 24-48 hours dry, it is spare to obtain nano-zinc oxide composite material；
（4）In mass ratio by step 1 products therefrom, nano-zinc oxide composite material, maleic anhydride, benzoyl peroxide（13-
16）：（6-8）：（4-5）：（0.05-0.08）It is added in reaction kettle after mixing, prepolymerization 20-40 minutes at 80-90 DEG C；
（5）By step 4 products therefrom and polymethyl methacrylate in mass ratio 1：（80-85）Twin-screw extrusion is sent into after mixing
In machine, at 220 DEG C mixing 30-40 minutes to get organic glass of the present invention.
In the step 1 in calcination process under nitrogen atmosphere protection.
The mass ratio of nano zine oxide, Silane coupling reagent KH-570 and 75% ethanol water is 24 in the step 2：
1：325.
The additional amount of a hydronium(ion) lithia is the 5-10% of nano zine oxide quality in the step 3.
The matter of step 1 products therefrom, nano-zinc oxide composite material, maleic anhydride, benzoyl peroxide in the step 4
Amount is than being 15：7：5：0.06.
The control of mixing revolving speed is 40-60 revs/min in the step 5.
It is an advantage of the invention that：
The present invention introduces rice case fibre in the preparation of organic glass, and silica therein is in sodium fluoride and nanometer iron powder
Under catalysis, silicon carbide contents are generated with carbon, improve the wearability and heat resistance of organic glass, while the active group that surface is more
Group is conducive to adsorb with matrix, so that the stability of organic glass is improved, on this basis using silane coupling agent to nano oxygen
Change zinc progress surface to be modified, reactive group is reacted with microparticle surfaces group, new chemical bond is formed, to reduce zinc oxide
The surface energy of particle, recycles in-situ polymerization that nano zine oxide is compound with polymethyl methacrylate, avoids traditional blending method
A large amount of toxic solvents and the higher defect of coating material price are consumed, it is real by simple controllable condition at a lower temperature
The insertion of existing nano zine oxide, so that the uvioresistant performance of organic glass greatly improved, thus obtained organic glass is being made
Standby upper mild condition, and there is photochemical effect and preferably cover imparted energy, ultraviolet shielded rate is more than 97%, is made
For uvioresistant glass use all kinds of buildings, in terms of all have preferable application prospect.
Specific embodiment
A kind of preparation method of anti-ultraviolet radiation organic glass, includes the following steps：
（1）It crushed 80 meshes after rice husk is dried, by itself and iron powder, sodium fluoride in mass ratio 77 after oxidative decoloration：1：2 is mixed
It closes and is sent into calcining furnace, be warming up to 400 DEG C under nitrogen atmosphere protection, react 3 hours, cooling is taken out spare after the completion；
（2）By nano zine oxide, Silane coupling reagent KH-570 and 75% ethanol water in mass ratio 24：1：Magnetic after 325 mixing
Power stirs 30 minutes, re-ultrasonic dispersion 25 minutes, mixed liquor is placed in 85 DEG C of oil baths flows back 100 minutes after the completion, Zhi Houleng
But, it is respectively washed 3 times with ethyl alcohol and clear water, is dried in vacuo 6 hours at 110 DEG C, grinding sieves with 100 mesh sieve spare；
（3）By step 2 products therefrom, polymethyl methacrylate, 2,2- azodiisobutyronitrile in mass ratio 3：90：After 7 mixing
It is dissolved in ethanol solution at 30 DEG C, a hydronium(ion) lithia is added thereto again after mixing evenly, additional amount is nano oxidized
The 8% of zinc quality, while 80 DEG C are warming up to, return stirring reacts 120 minutes, after the completion does gained mixed liquor in 55 DEG C of air blast
Dry 36 hours, it is spare to obtain nano-zinc oxide composite material；
（4）By step 1 products therefrom, nano-zinc oxide composite material, maleic anhydride, benzoyl peroxide in mass ratio 15：7：
5：It is added in reaction kettle after 0.06 mixing, prepolymerization 30 minutes at 85 DEG C；
（5）By step 4 products therefrom and polymethyl methacrylate in mass ratio 1：It is sent into double screw extruder after 85 mixing,
Mixing 30 minutes at 220 DEG C, revolving speed control is for 50 revs/min to get organic glass of the present invention.
Claims (6)
1. a kind of preparation method of anti-ultraviolet radiation organic glass, which is characterized in that include the following steps：
（1）Crushed 60-80 mesh after rice husk is dried, after oxidative decoloration by it with iron powder, sodium fluoride in mass ratio（75-
78）：（0.5-1）：（1-3）Mixing is sent into calcining furnace, is warming up to 380-420 DEG C, is reacted 2-3 hours, cooling after the completion to take out
It is spare；
（2）In mass ratio by nano zine oxide, Silane coupling reagent KH-570 and 75% ethanol water（20-25）：（1-2）：
（300-350）Magnetic agitation 30-40 minutes after mixing, re-ultrasonic dispersion 20-30 minutes, mixed liquor is placed in 80-90 after the completion
It flows back 90-120 minutes in DEG C oil bath, cools down, be respectively washed 2-3 times with ethyl alcohol and clear water later, vacuum is dry at 100-110 DEG C
5-10 hours dry, ground 80-100 mesh is spare；
（3）In mass ratio by step 2 products therefrom, polymethyl methacrylate, 2,2- azodiisobutyronitrile（2-3）：（85-
95）：（6-8）It is dissolved in ethanol solution at 30-35 DEG C after mixing, hydronium(ion) oxidation is added thereto again after mixing evenly
Lithium, while it being warming up to 75-85 DEG C, return stirring reacts 120-150 minutes, after the completion by gained mixed liquor in 50-60 DEG C of air blast
It is 24-48 hours dry, it is spare to obtain nano-zinc oxide composite material；
（4）In mass ratio by step 1 products therefrom, nano-zinc oxide composite material, maleic anhydride, benzoyl peroxide（13-
16）：（6-8）：（4-5）：（0.05-0.08）It is added in reaction kettle after mixing, prepolymerization 20-40 minutes at 80-90 DEG C；
（5）By step 4 products therefrom and polymethyl methacrylate in mass ratio 1：（80-85）Twin-screw extrusion is sent into after mixing
In machine, at 220 DEG C mixing 30-40 minutes to get organic glass of the present invention.
2. the preparation method of anti-ultraviolet radiation organic glass according to claim 1, which is characterized in that in the step 1
In calcination process under nitrogen atmosphere protection.
3. the preparation method of anti-ultraviolet radiation organic glass according to claim 1, which is characterized in that in the step 2
The mass ratio of nano zine oxide, Silane coupling reagent KH-570 and 75% ethanol water is 24：1：325.
4. the preparation method of anti-ultraviolet radiation organic glass according to claim 1, which is characterized in that in the step 3
The additional amount of one hydronium(ion) lithia is the 5-10% of nano zine oxide quality.
5. the preparation method of anti-ultraviolet radiation organic glass according to claim 1, which is characterized in that in the step 4
Step 1 products therefrom, nano-zinc oxide composite material, maleic anhydride, benzoyl peroxide mass ratio be 15：7：5：0.06.
6. the preparation method of anti-ultraviolet radiation organic glass according to claim 1, which is characterized in that in the step 5
The control of mixing revolving speed is 40-60 revs/min.
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| CN201810464746.6A CN108912575A (en) | 2018-05-16 | 2018-05-16 | A kind of preparation method of anti-ultraviolet radiation organic glass |
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| CN201810464746.6A CN108912575A (en) | 2018-05-16 | 2018-05-16 | A kind of preparation method of anti-ultraviolet radiation organic glass |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109912862A (en) * | 2019-02-25 | 2019-06-21 | 裴文韬 | A kind of composite rubber floor |
| CN112852082A (en) * | 2020-12-30 | 2021-05-28 | 郝秀花 | Zinc oxide nano-flower modified polyvinyl alcohol antibacterial material and preparation method thereof |
-
2018
- 2018-05-16 CN CN201810464746.6A patent/CN108912575A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109912862A (en) * | 2019-02-25 | 2019-06-21 | 裴文韬 | A kind of composite rubber floor |
| CN112852082A (en) * | 2020-12-30 | 2021-05-28 | 郝秀花 | Zinc oxide nano-flower modified polyvinyl alcohol antibacterial material and preparation method thereof |
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