CN101633740B - Method for preparing transparent heat-resistant polymethyl methacrylate nano-composite membrane - Google Patents
Method for preparing transparent heat-resistant polymethyl methacrylate nano-composite membrane Download PDFInfo
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- CN101633740B CN101633740B CN2008100408405A CN200810040840A CN101633740B CN 101633740 B CN101633740 B CN 101633740B CN 2008100408405 A CN2008100408405 A CN 2008100408405A CN 200810040840 A CN200810040840 A CN 200810040840A CN 101633740 B CN101633740 B CN 101633740B
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Abstract
The invention relates to a method for preparing a transparent heat-resistant polymethyl methacrylate nano-composite membrane. The method comprises the following steps: dispersing montmorillonite into deionized water, and stirring the mixture at a temperature of 50 to 90 DEG C for 2 to 6 hours to obtain a montmorillonite suspension for standby; dissolving polymethyl methacrylate into solvent to prepare polymethyl methacrylate solution; and mixing the montmorillonite suspension and the polymethyl methacrylate solution uniformly, casting the mixture at a temperature lower than 150 DEG C, and volatilizing the solvent to prepare the transparent heat-resistant polymethyl methacrylate nano-composite membrane. The content of the montmorillonite in the membrane is more than 0 weight percent and less than or equal to 10 weight percent. Compared with the prior art, the method for preparing the transparent heat-resistant polymethyl methacrylate nano-composite membrane has reasonable process and simple operation; and the nano-composite membrane cast from the polymethyl methacrylate and the montmorillonite by a solvent blending method has the advantages of convenient shaping, adjustable thickness, high transparency, good heat resistance, high use temperature and the like, and can be widely used in the industries such as external decoration materials, optical materials and the like.
Description
Technical field
The present invention relates to macromolecular material, relate in particular to a kind of preparation method of transparent heat-resistant polymethyl methacrylate nano-composite membrane.
Background technology
Polymethylmethacrylate (PMMA is commonly called as synthetic glass) is a kind of transparent good macromolecular material of widespread use, has beautiful texture and preeminent weathering resistance.Its transmittance is higher more than 10% than simple glass, and light weight is tough and tensile, be easy to forming process, can also frustrate and secondary processing such as cut, thereby be widely used in fields such as aviation, automobile, boats and ships, illumination, electronic instrument, opticinstrument, medicine equipment, building materials and cultural goods.Though synthetic glass possesses above-mentioned plurality of advantages, the drawbacks limit that its use temperature is lower, thermotolerance is relatively poor its range of application.Therefore, to synthetic glass in addition modification be very important work to improve its thermotolerance.
Filling inorganic rigid particle is to improve the stable on heating effective ways of synthetic glass, and this method not only can be improved its thermotolerance, improves use temperature, can also improve its surface hardness, improves wear resistance.The inorganic particulate of big scale can influence the transparency of material, thereby utilizes nanometer composite technology to prepare the popular research topic that high heat resistance PMMA becomes the Materials science worker.
At present, existing a large amount of bibliographical information PMMA/ Nano composite material of montmorillonite, yet these reports organo montmorillonites that use more, as quaternary ammonium salt, alkylammonium salt, comonomer or high-activity compound modified montmorillonoid.There are problems such as complicated component, complex operation in these preparation methods, and micromolecular adding has reduced the thermostability of material.
Summary of the invention
Purpose of the present invention is exactly to provide in order to overcome the defective that above-mentioned prior art exists that a kind of technology is reasonable, easy to operate, the preparation method of the simple transparent heat-resistant polymethyl methacrylate nano-composite membrane of composition.
Purpose of the present invention can be achieved through the following technical solutions:
A kind of preparation method of transparent heat-resistant polymethyl methacrylate nano-composite membrane is characterized in that, this method may further comprise the steps:
(1) polynite is scattered in the deionized water, stirred 2～6 hours, obtain montmorillonite suspension liquid at 50～90 ℃, standby;
(2) polymethylmethacrylate is dissolved in makes polymethyl methacrylate solution in the solvent;
(3) above-mentioned montmorillonite suspension liquid and polymethyl methacrylate solution are mixed, cast, solvent flashing make transparent heat-resistant polymethyl methacrylate nano-composite membrane down to be lower than 150 ℃ in temperature, polynite content is greater than 0wt%, smaller or equal to 10wt% in this film.
The concentration of described montmorillonite suspension liquid is 0.01wt%～5wt%.
The concentration of described polymethyl methacrylate solution is 0.01wt%～20wt%.
Described polynite comprises that cation exchange capacity (CEC) is greater than 45mequiv100g
-1Original soil.
Described polymethylmethacrylate comprises the technical grade polymethylmethacrylate.
Described solvent comprises acetone, tetrahydrofuran (THF), N, dinethylformamide or N,N-dimethylacetamide.
Compared with prior art, technology of the present invention is reasonable, simple to operate, utilize solution blended process that polymethylmethacrylate and polynite blend are cast into nano compound film, this film forming is convenient, thickness is adjustable, has transparency height, good heat resistance, use temperature advantages of higher, can be widely used in industries such as outer exterior material and optical material.
Embodiment
The invention will be further described below in conjunction with specific embodiment.
Embodiment 1
A kind of preparation method of transparent heat-resistant polymethyl methacrylate nano-composite membrane, this method may further comprise the steps:
(1) (cation exchange capacity (CEC) is 85mequiv100g with polynite
-1) be scattered in the deionized water, concentration equals 2wt%, stirs 4 hours at 70 ℃;
(2) polymethylmethacrylate (PMMA) is dissolved in N, makes concentration in the dinethylformamide and equal 5wt% solution;
(3) above-mentioned PMMA solution and montmorillonite suspension liquid were pressed mass ratio (100: 0; 97.5: 2.5; 95: 5; 91: 9; 82: 18; 78: 22) mix, cast under temperature is lower than 120 ℃, solvent flashing make transparent heat-resistant polymethyl methacrylate nano-composite membrane (thickness 0.2mm), and polynite content is 0wt% in the film, 1wt%, 2wt%, 4wt%, 8wt% and 10wt%.
With polynite content is that 0wt% compares, and the polymethyl methacrylate nano-composite membrane transmittance is kept preferably, and thermotolerance and use temperature all have raising by a relatively large margin, and performance is as shown in table 1:
The performance of the polymethyl methacrylate nano-composite membrane of table 1. embodiment 1
Annotate: T
D5%And T
D5%Represent the heat decomposition temperature when thermal weight loss is 5wt% and 10wt% under the nitrogen atmosphere respectively, T
gBe second-order transition temperature, numerical value heats up by 10 ℃/min of DSC and is surveyed, down together.
Embodiment 2
A kind of preparation method of transparent heat-resistant polymethyl methacrylate nano-composite membrane, this method may further comprise the steps:
(1) (cation exchange capacity (CEC) is 100mequiv100g with original montmorillonoid soil
-1) be scattered in the deionized water, concentration equals 4wt%, stirs 6 hours at 50 ℃;
(2) technical grade polymethylmethacrylate (PMMA) is dissolved in makes concentration in the acetone and equal 10wt% solution;
(3) above-mentioned PMMA solution and montmorillonite suspension liquid were pressed mass ratio (100: 0; 97.5: 2.5; 95: 5; 91: 9; 82: 18; 78: 22) mix, make transparent heat-resistant polymethyl methacrylate nano-composite membrane (thickness 0.1mm) at temperature 25 ℃ of following cast, solvent flashings, polynite content is 0wt% in the film, 1wt%, 2wt%, 4wt%, 8wt% and 10wt%.
With polynite content is that 0wt% compares, and the polymethyl methacrylate nano-composite membrane transmittance is kept preferably, and thermotolerance and use temperature all have raising by a relatively large margin, and performance is as shown in table 2:
The performance of the polymethyl methacrylate nano-composite membrane of table 2. embodiment 2
Embodiment 3
A kind of preparation method of transparent heat-resistant polymethyl methacrylate nano-composite membrane, this method may further comprise the steps:
(1) (cation exchange capacity (CEC) is 120mequiv100g with original montmorillonoid soil
-1) be scattered in the deionized water, concentration equals 5wt%, stirs 2 hours at 90 ℃;
(2) technical grade polymethylmethacrylate (PMMA) is dissolved in makes concentration in the tetrahydrofuran (THF) and equal 20wt% solution;
(3) above-mentioned PMMA solution and montmorillonite suspension liquid were pressed mass ratio (100: 0; 96: 4; 92.5: 7.5; 85.7: 14.3; 74: 26; 69: 31) mix, make transparent heat-resistant polymethyl methacrylate nano-composite membrane (thickness 0.2mm) at temperature 40 ℃ of following cast, solvent flashings, polynite content is 0wt% in the film, 1wt%, 2wt%, 4wt%, 8wt% and 10wt%.
With polynite content is that 0wt% compares, and the polymethyl methacrylate nano-composite membrane transmittance is kept preferably, and thermotolerance and use temperature all have raising by a relatively large margin, and performance is as shown in table 3:
The performance of the polymethyl methacrylate nano-composite membrane of table 3. embodiment 3
Embodiment 4
A kind of preparation method of transparent heat-resistant polymethyl methacrylate nano-composite membrane, this method may further comprise the steps:
(1) (cation exchange capacity (CEC) is greater than 45mequiv100g with original montmorillonoid soil
-1) be scattered in the deionized water, concentration equals 3wt%, stirs 4 hours at 70 ℃;
(2) polymethylmethacrylate (PMMA) is dissolved in makes concentration in the N,N-dimethylacetamide and equal 15wt% solution;
(3) above-mentioned PMMA solution and montmorillonite suspension liquid were pressed mass ratio (100: 0; 95: 5; 91: 9; 83: 7; 70: 30; 65: 35) mix, make transparent heat-resistant polymethyl methacrylate nano-composite membrane (thickness 0.2mm) at temperature 140 ℃ of following cast, solvent flashings, polynite content is 0wt% in the film, 1wt%, 2wt%, 4wt%, 8wt% and 10wt%.
With polynite content is that 0wt% compares, and the polymethyl methacrylate nano-composite membrane transmittance is kept preferably, and thermotolerance and use temperature all have raising by a relatively large margin, and performance is as shown in table 4:
The performance of the polymethyl methacrylate nano-composite membrane of table 4. embodiment 4
Embodiment 5
A kind of preparation method of transparent heat-resistant polymethyl methacrylate nano-composite membrane, this method may further comprise the steps:
(1) (cation exchange capacity (CEC) is 85mequiv100g with polynite
-1) be scattered in the deionized water, concentration equals 0.01wt%, stirs 4 hours at 70 ℃;
(2) polymethylmethacrylate (PMMA) is dissolved in N, makes concentration in the dinethylformamide and equal 5wt% solution;
(3) above-mentioned PMMA solution and montmorillonite suspension liquid were mixed by 1: 5, cast under temperature is lower than 120 ℃, solvent flashing make transparent heat-resistant polymethyl methacrylate nano-composite membrane (thickness 0.2mm), and polynite content is 1wt%. in the film
With polynite content is that 0wt% compares, and the polymethyl methacrylate nano-composite membrane transmittance is kept preferably, and thermotolerance and use temperature all have raising by a relatively large margin.
Embodiment 6
A kind of preparation method of transparent heat-resistant polymethyl methacrylate nano-composite membrane, this method may further comprise the steps:
(1) (cation exchange capacity (CEC) is 100mequiv100g with original montmorillonoid soil
-1) be scattered in the deionized water, concentration equals 4wt%, stirs 6 hours at 50 ℃;
(2) technical grade polymethylmethacrylate (PMMA) is dissolved in makes concentration in the acetone and equal 0.01wt% solution;
(3) above-mentioned PMMA solution and montmorillonite suspension liquid were mixed by 3600: 1, make transparent heat-resistant polymethyl methacrylate nano-composite membrane (thickness 0.1mm) at temperature 25 ℃ of following cast, solvent flashings, polynite content is 10wt% in the film.
With polynite content is that 0wt% compares, and the polymethyl methacrylate nano-composite membrane transmittance is kept preferably, and thermotolerance and use temperature all have raising by a relatively large margin.
Claims (5)
1. the preparation method of a transparent heat-resistant polymethyl methacrylate nano-composite membrane is characterized in that, this method is made up of following steps:
(1) polynite is scattered in the deionized water, stirred 2～6 hours, obtain montmorillonite suspension liquid at 50～90 ℃, standby;
(2) polymethylmethacrylate is dissolved in makes polymethyl methacrylate solution in the solvent;
(3) above-mentioned montmorillonite suspension liquid and polymethyl methacrylate solution are mixed, cast, solvent flashing make transparent heat-resistant polymethyl methacrylate nano-composite membrane down to be lower than 150 ℃ in temperature, polynite content is greater than 0wt%, smaller or equal to 10wt% in this film;
Described polynite comprises that cation exchange capacity (CEC) is greater than 45mequiv100g
-1Original soil.
2. the preparation method of transparent heat-resistant polymethyl methacrylate nano-composite membrane according to claim 1 is characterized in that, the concentration of described montmorillonite suspension liquid is 0.01wt%～5wt%.
3. the preparation method of transparent heat-resistant polymethyl methacrylate nano-composite membrane according to claim 1 is characterized in that, the concentration of described polymethyl methacrylate solution is 0.01wt%～20wt%.
4. the preparation method of transparent heat-resistant polymethyl methacrylate nano-composite membrane according to claim 1 is characterized in that, described polymethylmethacrylate comprises the technical grade polymethylmethacrylate.
5. the preparation method of transparent heat-resistant polymethyl methacrylate nano-composite membrane according to claim 1 is characterized in that, described solvent comprises acetone, tetrahydrofuran (THF), N, dinethylformamide or N,N-dimethylacetamide.
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| CN105419204A (en) * | 2015-12-22 | 2016-03-23 | 安徽省春谷3D打印智能装备产业技术研究院有限公司 | Kaolin-modified 3D-printer window glass material and preparation method thereof |
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| CN105440537A (en) * | 2015-12-22 | 2016-03-30 | 安徽省春谷3D打印智能装备产业技术研究院有限公司 | 3D printer window glass material based on bentonite modification, and preparation method thereof |
| CN105440536A (en) * | 2015-12-22 | 2016-03-30 | 安徽省春谷3D打印智能装备产业技术研究院有限公司 | 3D printer window glass material based on magnesia modification, and preparation method thereof |
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| CN105482336A (en) * | 2015-12-22 | 2016-04-13 | 安徽省春谷3D打印智能装备产业技术研究院有限公司 | Expanded vermiculite modified 3D (three dimensional) printer window glass material and preparation method thereof |
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| CN105838011A (en) * | 2016-04-12 | 2016-08-10 | 苏州甫众塑胶有限公司 | A poly(methyl methacrylate) composite plastic material and a preparing method thereof |
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