CN108314753B - Transparent antistatic PMMA and preparation method thereof - Google Patents
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—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 a salt, anhydride ester, amide, imide or nitrile thereof
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- 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
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- 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
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Abstract
The invention relates to a high scoreThe field of sub-materials, in particular to transparent antistatic PMMA and a preparation method thereof; the transparent antistatic PMMA is prepared from the following components: methyl methacrylate; an initiator; an intermediate monomer; sulfonate monomers. The invention selects an intermediate monomer which has good compatibility with methyl methacrylate and sulfonate respectively, the sulfonate contains hydrophilic groups to increase the moisture absorption of the surface of the product, and a monomolecular conductive film is formed on the surface of the PMMA product, so that the PMMA achieves the antistatic effect. The preparation method has simple operation steps and easy implementation, and the surface resistance of the PMMA obtained by polymerization is lower than 1012Omega, can reach permanent antistatic effect, does not influence the transparency of PMMA on the basis of improving the antistatic performance of PMMA, and has the light transmittance of over 90 percent, which is equivalent to that of pure PMMA.
Description
Technical Field
The invention relates to the field of high polymer materials, in particular to transparent antistatic PMMA and a preparation method thereof.
Background
Polymethyl methacrylate (PMMA), also known as acrylic or organic glass, is a transparent polymer material polymerized from methyl methacrylate monomers, and is widely used in lighting parts in the fields of aviation, construction, agriculture, and the like due to its good optical transparency. In addition, the organic glass also has good electrical insulation performance, so that the organic glass also has wide application in the aspects of instruments, instrument parts, automobile parts, electrical appliance insulation materials and the like. However, the excellent electrical insulation of PMMA products also causes some problems, such as static electricity easily generated on the surface of PMMA products after friction, and static charge accumulation, dust in the air easily adsorbed during the processing or final use of PMMA products, electric shock, and even fire and explosion accidents. Thus, the antistatic modification of PMMA is of great significance.
The invention discloses a preparation method of an antistatic organic glass film (application number: CN 201310241383.7). firstly, a silane coupling agent, ethanol and acetic acid are used for preparing sol, then fullerene alcohol solid is prepared by fullerene, the sol and the fullerene alcohol solid are added into a polymethyl methacrylate prepolymer, the sol and the fullerene alcohol solid are mixed uniformly to obtain a coating liquid, and finally, the coating liquid is coated on a substrate and is solidified to obtain the antistatic organic glass film. The invention can make PMMA reach the antistatic grade, but the fullerene in the method is expensive, is not suitable for industrialized production, and has larger influence on the transparency of PMMA.
The synthesis of zirconium oxide (ZrO) by hydrolytic condensation of zirconium n-propoxide (ZNP) and 1-propanol in the presence of Methacrylic Acid (MA) was performed by Chao-Ching Chang et al (Preparation of zirconia loaded poly (acrylate) optically doped coatings on PMMA substrates J. APPL. POLYM. SCI.2015, DOI: 10.1002)2) Nano particles, chemically modifying the formed nano particles by using an ultraviolet light curing coupling agent 3- (trimethoxysilyl) propyl methacrylate (MSMA), then crosslinking the chemically modified nano particles with a monomer dipentaerythritol hexaacrylate (DPHA) to prepare a coating sol, and coating the coating sol on a PMMA substrate to generate a transparent antistatic hard coating, so that the surface resistance of the PMMA can be reduced to 1012Omega. However, the antistatic coating is easy to fall off in the use process of PMMA, the antistatic performance of the PMMA product is gradually reduced along with the prolonging of the use time of the PMMA product, and the permanent antistatic effect cannot be achieved.
Therefore, how to effectively prepare the PMMA composite material having permanent antistatic effect and maintaining its transparency is a technical problem to be solved at present.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a transparent antistatic PMMA copolymer with permanent antistatic performance and transparency.
Another object of the present invention is to provide a novel process for preparing transparent antistatic PMMA copolymer which can achieve permanent antistatic properties of PMMA while maintaining its transparency.
In order to achieve the purpose, the invention adopts the following technical scheme:
the transparent antistatic PMMA is prepared from the following components in parts by weight: 68.00-99.00 parts of methyl methacrylate; 0.03-0.20 part of an initiator; 1.00-30.00 parts of intermediate monomer; 0-2.00 parts of sulfonate monomer.
In the technical scheme, the intermediate monomer is selected and has good compatibility with Methyl Methacrylate (MMA) and sulfonate respectively, the sulfonate contains hydrophilic groups to increase the moisture absorption of the surface of the PMMA product, and a monomolecular conductive film is formed on the surface of the PMMA product, so that the PMMA achieves an antistatic effect. The selected intermediate monomer can be mutually soluble with MMA in any proportion, and sulfonate can be dissolved at the same time, so that three monomers are mixed to obtain a homogeneous system, and the transparent antistatic PMMA copolymer is obtained by thermal polymerization. The method is simple and easy to operate and implement, and the surface resistance of the PMMA obtained by polymerization is lower than 1012Omega, can reach permanent antistatic effect, does not influence the transparency of PMMA on the basis of improving the antistatic performance of PMMA, and has the light transmittance of over 90 percent, which is equivalent to that of pure PMMA.
Preferably, the initiator is an azo-based or peroxide-based initiator.
Preferably, the sulfonate monomer is one or more of L-butyl-3-methylimidazole methanesulfonate, L-tyrosine benzyl ester p-toluenesulfonate, 6-amidino-2-naphthol methanesulfonate and 3-sulfopropyl methacrylate potassium salt.
Preferably, the intermediate monomer is a monomer containing both a hydrophilic group, a hydrophobic group and a double bond.
Preferably, the intermediate monomer is one of hydroxyethyl methacrylate, hydroxypropyl acrylate and 1, 4-butanediol dimethacrylate.
A preparation method of transparent antistatic PMMA comprises the following steps:
(1) dissolving an initiator in MMA, and uniformly mixing to form a solution A;
(2) dissolving sulfonate monomers in intermediate monomers, and uniformly mixing by ultrasonic waves to form a solution B;
(3) putting the solution A obtained in the step (1) and the solution B obtained in the step (2) into a flask, and uniformly mixing by ultrasonic waves;
(4) placing the flask in an oil bath pan for prepolymerization, and removing bubbles and dissolved air after the prepolymerization is finished to degas a prepolymerization solution;
(5) treating a common glass plate purchased from the market with a silane coupling agent to make the surface hydrophobic;
(6) and (3) injecting the pre-polymerization solution obtained in the step (4) into the glass mold pretreated by the silane coupling agent in the step (5), placing the glass mold in a water bath for reaction and curing, and then performing secondary curing molding in a forced air oven to obtain the transparent antistatic PMMA.
Preferably, the ultrasonic temperature in the step (3) is 80-90 ℃, and the ultrasonic time is 60 min.
Preferably, the temperature of the oil bath in the step (4) is 80-90 ℃, preferably 80 ℃; the method for judging the prepolymerization end point comprises the following steps: the end point of the prepolymerization is 10s after a large amount of bubbles in the flask emerge.
Preferably, the specific method for treating the commercially available glass plate with the silane coupling agent in the step (5) is as follows: after washing and drying a commercially available glass plate with ethanol and deionized water, the surface of the glass plate was subjected to a hydrophobic treatment by immersing the plate in an acetone solution (100.00g) containing 1.50g of Hexadecyltrimethoxysilane (HTEOS) for 10 seconds.
Preferably, the specification of the glass plate mould in the step (6) is 15cm multiplied by 4 mm; the method for injecting the pre-polymerization liquid comprises the following steps: placing the rubber ring on a glass plate treated by a silane coupling agent, covering the rubber ring with another glass plate treated by the silane coupling agent, sealing the rubber ring by using a clamp to leave a gap, injecting a pre-polymerization solution into the gap, and well sealing the two glass plates by using the clamp; the temperature of the water bath kettle is 60-75 ℃, and the reaction time is 180 min; the temperature of the blast oven is 100-110 ℃, and the curing treatment time in the blast oven is 60 min.
The invention has the beneficial effects that:
(1) the invention can be prepared by utilizing a mature PMMA preparation process, the operation is simple and convenient, the implementation is easy, and the surface resistance of the antistatic PMMA reaches 1012Below omega, the antistatic effect is obvious, and the permanent antistatic property is realized without influencing the transparency of PMMA;
(2) the reagent adopted by the invention is safe and low in price, and is beneficial to popularization and application.
Detailed Description
The technical solution of the present invention is further specifically described below by way of examples, but the scope of the present invention is not limited thereto.
Example 1
(1) 97.95 parts MMA and 0.05 part ABVN (initiator) and 2.00 parts hydroxyethyl methacrylate (HEMA) were mixed well in a 250mL flask;
(2) placing the flask in an oil bath kettle at 80 ℃ for prepolymerization, connecting a spherical condenser and a thermometer (PID) in the flask to control the temperature, keeping the system at 80 ℃ for 20min, taking out the flask after about 10s of a large amount of bubbles in the flask emerge, placing the flask in an ice-water bath until the wall of the flask becomes cold, and degassing the prepolymer by applying vacuum (650mmHg) to remove the bubbles and dissolved air;
(3) commercially available glass plates were washed three times with ethanol and deionized water, respectively, dried, and then the glass plates were immersed for 10s in an acetone solution (100.00g) containing 1.50g of Hexadecyltrimethoxysilane (HTEOS) to make the surfaces hydrophobic. After pretreatment, drying at room temperature for 60 min;
(4) and (3) injecting the prepolymer solution into a glass mold (the specification of the mold is 15cm multiplied by 4mm) pretreated by a silane coupling agent, carrying out water bath reaction at 60 ℃ for 180min, taking out, and treating in a blast oven at 100 ℃ for 60min to solidify and mold to obtain a finished product.
Example 2
(1) 97.95 parts MMA and 0.05 part ABVN and 5.00 parts HEMA were mixed well in a 250mL flask;
(2) placing the flask in an oil bath kettle at 80 ℃ for prepolymerization, connecting a spherical condenser and a thermometer (PID) in the flask to control the temperature, keeping the system at 80 ℃ for 20min, taking out the flask after 10s of a large amount of bubbles in the flask emerge, placing the flask in an ice-water bath until the wall of the flask is cooled, and degassing the prepolymer by applying vacuum (650mmHg) to remove the bubbles and dissolved air;
(3) commercially available glass plates were washed three times with ethanol and deionized water, respectively, dried, and then the glass plates were immersed for 10s in an acetone solution (100.00g) containing 1.50g of Hexadecyltrimethoxysilane (HTEOS) to make the surfaces hydrophobic. After pretreatment, drying at room temperature for 60 min;
(4) and (3) injecting the prepolymer solution into a glass mold (the specification of the mold is 15cm multiplied by 4mm) pretreated by a silane coupling agent, carrying out water bath reaction at 60 ℃ for 180min, taking out, and treating in a blast oven at 100 ℃ for 60min to solidify and mold to obtain a finished product.
Example 3
(1) 97.95 parts MMA and 0.05 part ABVN and 10.00 parts HEMA were mixed well in a 250mL flask;
(2) placing the flask in an oil bath kettle at 80 ℃ for prepolymerization, connecting a spherical condenser and a thermometer (PID) in the flask to control the temperature, keeping the system at 80 ℃ for 20min, taking out the flask after 10s of a large amount of bubbles in the flask emerge, placing the flask in an ice-water bath until the wall of the flask is cooled, and degassing the prepolymer by applying vacuum (650mmHg) to remove the bubbles and dissolved air;
(3) commercially available glass plates were washed three times with ethanol and deionized water, respectively, dried, and then the glass plates were immersed for 10s in an acetone solution (100.00g) containing 1.50g of Hexadecyltrimethoxysilane (HTEOS) to make the surfaces hydrophobic. After pretreatment, drying at room temperature for 60 min;
(4) and (3) injecting the prepolymer solution into a glass mold (the specification of the mold is 15cm multiplied by 4mm) pretreated by a silane coupling agent, carrying out water bath reaction at 60 ℃ for 180min, taking out, and treating in a blast oven at 100 ℃ for 60min to solidify and mold to obtain a finished product.
Example 4
(1) 97.95 parts MMA and 0.05 part ABVN and 15.00 parts HEMA were mixed well in a 250mL flask;
(2) placing the flask in an oil bath kettle at 80 ℃ for prepolymerization, connecting a spherical condenser and a thermometer (PID) in the flask to control the temperature, keeping the system at 80 ℃ for 20min, taking out the flask after 10s of a large amount of bubbles in the flask emerge, placing the flask in an ice-water bath until the wall of the flask is cooled, and degassing the prepolymer by applying vacuum (650mmHg) to remove the bubbles and dissolved air;
(3) commercially available glass plates were washed three times with ethanol and deionized water, respectively, dried, and then the glass plates were immersed for 10s in an acetone solution (100.00g) containing 1.50g of Hexadecyltrimethoxysilane (HTEOS) to make the surfaces hydrophobic. After pretreatment, drying at room temperature for 60 min;
(4) and (3) injecting the prepolymer solution into a glass mold (the specification of the mold is 15cm multiplied by 4mm) pretreated by a silane coupling agent, carrying out water bath reaction at 60 ℃ for 180min, taking out, and treating in a blast oven at 100 ℃ for 60min to solidify and mold to obtain a finished product.
Example 5
(1) 97.95 parts MMA and 0.05 part ABVN and 20.00 parts HEMA were mixed well in a 250mL flask;
(2) placing the flask in an oil bath kettle at 80 ℃ for prepolymerization, connecting a spherical condenser and a thermometer (PID) in the flask to control the temperature, keeping the system at 80 ℃ for 20min, taking out the flask after 10s of a large amount of bubbles in the flask emerge, placing the flask in an ice-water bath until the wall of the flask is cooled, and degassing the prepolymer by applying vacuum (650mmHg) to remove the bubbles and dissolved air;
(3) commercially available glass plates were washed three times with ethanol and deionized water, respectively, dried, and then the glass plates were immersed for 10s in an acetone solution (100.00g) containing 1.50g of Hexadecyltrimethoxysilane (HTEOS) to make the surfaces hydrophobic. After pretreatment, drying at room temperature for 60 min;
(4) and (3) injecting the prepolymer solution into a glass mold (the specification of the mold is 15cm multiplied by 4mm) pretreated by a silane coupling agent, carrying out water bath reaction at 60 ℃ for 180min, taking out, and treating in a blast oven at 100 ℃ for 60min to solidify and mold to obtain a finished product.
Example 6
(1) 89.45 parts MMA and 0.05 part ABVN were mixed well in a beaker;
(2) adding 10.00 parts of HEMA and 0.50 part of 3-ethoxyanilide mesylate into a beaker, and carrying out ultrasonic treatment for 30min to uniformly mix the materials;
(3) putting the uniformly mixed solution in the (1) and the (2) into a 250mL flask, and performing ultrasonic treatment for 180min to uniformly mix the solution;
(4) placing the flask in an oil bath kettle at 80 ℃ for prepolymerization, uniformly dispersing sulfonate by magnetic stirring, connecting a spherical condenser and a thermometer (PID) in the flask to control the temperature, maintaining the system at 80 ℃ for 20min, taking out the flask after 10s of a large amount of bubbles in the flask emerge, placing the flask into an ice-water bath, keeping the magnetic stirring until the wall of the flask is cooled, and degassing the prepolymer by applying vacuum (650mmHg) to remove the bubbles and dissolved air;
(5) commercially available glass plates were washed three times with ethanol and deionized water, respectively, dried, and then the glass plates were immersed for 10s in an acetone solution (100.00g) containing 1.50g of Hexadecyltrimethoxysilane (HTEOS) to make the surfaces hydrophobic. After pretreatment, drying at room temperature for 60 min;
(6) and (3) injecting the prepolymer into a glass mold (the specification of the mold is 15cm multiplied by 4mm) pretreated by a silane coupling agent, carrying out water bath reaction for 180min at 70 ℃, taking out, and treating for 60min in a blast oven at 100 ℃ to solidify and mold to obtain a finished product.
Example 7
(1) 89.35 parts MMA and 0.05 part ABVN were mixed well in a beaker;
(2) adding 10.00 parts of HEMA and 0.60 part of 3-ethoxyanilide mesylate into a beaker, and carrying out ultrasonic treatment for 30min to uniformly mix the materials;
(3) putting the uniformly mixed solution in the (1) and the (2) into a 250mL flask, and performing ultrasonic treatment for 180min to uniformly mix the solution;
(4) placing the flask in an oil bath kettle at 80 ℃ for prepolymerization, uniformly dispersing sulfonate by magnetic stirring, connecting a spherical condenser and a thermometer (PID) in the flask to control the temperature, keeping the system at 80 ℃ for 20min, taking out the flask and placing the flask in an ice-water bath after the prepolymerization is finished after a large amount of bubbles in the flask emerge, keeping the magnetic stirring until the wall of the flask is cooled, and degassing the prepolymer by applying vacuum (650mmHg) to remove the bubbles and dissolved air;
(5) commercially available glass plates were washed three times with ethanol and deionized water, respectively, dried, and then the glass plates were immersed for 10s in an acetone solution (100.00g) containing 1.50g of Hexadecyltrimethoxysilane (HTEOS) to make the surfaces hydrophobic. After pretreatment, drying at room temperature for 60 min;
(6) and (3) injecting the prepolymer solution into a glass mold (the specification of the mold is 15cm multiplied by 4mm) pretreated by a silane coupling agent, carrying out water bath reaction at 60 ℃ for 180min, taking out, and treating in a blast oven at 100 ℃ for 60min to solidify and mold to obtain a finished product.
Example 8
(1) 89.25 parts MMA and 0.05 part ABVN were mixed well in a beaker;
(2) adding 10.00 parts of HEMA and 0.70 part of 3-ethoxyanilide mesylate into a beaker, and carrying out ultrasonic treatment for 30min to uniformly mix the materials;
(3) putting the uniformly mixed solution in the (1) and the (2) into a 250mL flask, and performing ultrasonic treatment for 180min to uniformly mix the solution;
(4) placing the flask in an oil bath kettle at 80 ℃ for prepolymerization, uniformly dispersing sulfonate by magnetic stirring, connecting a spherical condenser and a thermometer (PID) in the flask to control the temperature, keeping the system at 80 ℃ for 20min, taking out the flask and placing the flask in an ice-water bath after the prepolymerization is finished after a large amount of bubbles in the flask emerge, keeping the magnetic stirring until the wall of the flask is cooled, and degassing the prepolymer by applying vacuum (650mmHg) to remove the bubbles and dissolved air;
(5) commercially available glass plates were washed three times with ethanol and deionized water, respectively, dried, and then the glass plates were immersed for 10s in an acetone solution (100.00g) containing 1.50g of Hexadecyltrimethoxysilane (HTEOS) to make the surfaces hydrophobic. After pretreatment, drying at room temperature for 60 min;
(6) and (3) injecting the prepolymer solution into a glass mold (the specification of the mold is 15cm multiplied by 4mm) pretreated by a silane coupling agent, carrying out water bath reaction at 60 ℃ for 180min, taking out, and treating in a blast oven at 100 ℃ for 60min to solidify and mold to obtain a finished product.
Example 9
(1) 89.77 parts MMA and 0.05 part ABVN were mixed well in a beaker;
(2) adding 10.00 parts and 0.80 part of 3-ethoxyanilide mesylate into a beaker, and carrying out ultrasonic treatment for 30min to uniformly mix the materials;
(3) putting the uniformly mixed solution in the (1) and the (2) into a 250mL flask, and performing ultrasonic treatment for 180min to uniformly mix the solution;
(4) placing the flask in an oil bath kettle at 80 ℃ for prepolymerization, uniformly dispersing sulfonate by magnetic stirring, connecting a spherical condenser and a thermometer (PID) in the flask to control the temperature, keeping the system at 80 ℃ for 20min, taking out the flask and placing the flask in an ice-water bath after the prepolymerization is finished after a large amount of bubbles in the flask emerge, keeping the magnetic stirring until the wall of the flask is cooled, and degassing the prepolymer by applying vacuum (650mmHg) to remove the bubbles and dissolved air;
(5) commercially available glass plates were washed three times with ethanol and deionized water, respectively, dried, and then the glass plates were immersed for 10s in an acetone solution (100.00g) containing 1.50g of Hexadecyltrimethoxysilane (HTEOS) to make the surfaces hydrophobic. After pretreatment, drying at room temperature for 60 min;
(6) and (3) injecting the prepolymer solution into a glass mold (the specification of the mold is 15cm multiplied by 4mm) pretreated by a silane coupling agent, carrying out water bath reaction at 60 ℃ for 180min, taking out, and treating in a blast oven at 100 ℃ for 60min to solidify and mold to obtain a finished product.
Example 10
(1) 89.05 parts MMA and 0.05 part ABVN were mixed well in a beaker;
(2) adding 10.00 parts of HEMA and 0.09 part of 3-ethoxyanilide mesylate into a beaker, and carrying out ultrasonic treatment for 30min to uniformly mix the materials;
(3) putting the uniformly mixed solution in the (1) and the (2) into a 250mL flask, and performing ultrasonic treatment for 180min to uniformly mix the solution;
(4) placing the flask in an oil bath kettle at 80 ℃ for prepolymerization, uniformly dispersing sulfonate by magnetic stirring, connecting a spherical condenser and a thermometer (PID) in the flask to control the temperature, keeping the system at 80 ℃ for 20min, taking out the flask and placing the flask in an ice-water bath after the prepolymerization is finished after a large amount of bubbles in the flask emerge, keeping the magnetic stirring until the wall of the flask is cooled, and degassing the prepolymer by applying vacuum (650mmHg) to remove the bubbles and dissolved air;
(5) commercially available glass plates were washed three times with ethanol and deionized water, respectively, dried, and then the glass plates were immersed for 10s in an acetone solution (100.00g) containing 1.50g of Hexadecyltrimethoxysilane (HTEOS) to make the surfaces hydrophobic. After pretreatment, drying at room temperature for 60 min;
(6) and (3) injecting the prepolymer solution into a glass mold (the specification of the mold is 15cm multiplied by 4mm) pretreated by a silane coupling agent, carrying out water bath reaction at 60 ℃ for 180min, taking out, and treating in a blast oven at 100 ℃ for 60min to solidify and mold to obtain a finished product.
TABLE 1 Effect of different intermediate monomer contents on the surface resistance and light transmittance of PMMA Final products
| Numbering | MMA parts (parts) | HEMA parts (parts) | Surface resistance (omega) | Light transmittance (%) |
| Example 1 | 97.95 | 2.00 | 1012～1014 | 93.8 |
| Example 2 | 94.95 | 5.00 | 1012～1014 | 91.2 |
| Example 3 | 89.95 | 10.00 | 1012～1013 | 91.3 |
| Example 4 | 84.95 | 15.00 | 1012～1013 | 90.8 |
| Example 5 | 79.95 | 20.00 | 1012～1013 | 90.5 |
TABLE 2 Effect of different sulfonate contents on surface resistance and light transmittance of PMMA Final
| Numbering | MMA parts (parts) | HEMA parts (parts) | Surface resistance (omega) | Light transmittance (%) |
| Example 6 | 89.45 | 0.50 | ＜1012 | 92.6 |
| Example 7 | 89.35 | 0.60 | ＜1012 | 92.2 |
| Example 8 | 89.25 | 0.70 | ＜1012 | 91.8 |
| Example 9 | 89.77 | 0.80 | ＜1012 | 90.5 |
| Example 10 | 89.05 | 0.90 | ＜1012 | 88.8 |
The amounts of ABVN added in tables 1 and 2 were 0.05 parts, and HEMA added in table 2 was 10.00 parts. It can be seen from the above table 1 that the transmittance of the PMMA finished product does not change much with the increase of the content of the intermediate monomer, and from table 2 that the transmittance of PMMA decreases with the increase of the sulfonate content.
The above embodiments are merely representative examples of the present invention. It is obvious that the technical solution of the present invention is not limited to the above-described embodiments, and many variations are possible. Variations that would be directly derivable by a person of ordinary skill in the art from the present disclosure are to be considered within the scope of the present invention.
Claims (7)
1. The transparent antistatic PMMA is characterized by being prepared from the following components in parts by weight: 68.00-99.00 parts of methyl methacrylate; 0.03-0.20 part of an initiator; 2.00-20.00 parts of intermediate monomer; 0.5-0.9 part of sulfonate monomer;
the intermediate monomer is one of hydroxyethyl methacrylate and hydroxypropyl acrylate;
the sulfonate monomer is 3-ethoxyanilide mesylate.
2. The transparent antistatic PMMA according to claim 1, characterized in that the initiator is azo or peroxide initiator.
3. A method for preparing transparent antistatic PMMA according to claim 1, wherein the method comprises the following steps:
(1) dissolving an initiator in MMA, and uniformly mixing to form a solution A;
(2) dissolving sulfonate monomers in intermediate monomers, and uniformly mixing by ultrasonic waves to form a solution B;
(3) putting the solution A obtained in the step (1) and the solution B obtained in the step (2) into a flask, and uniformly mixing by ultrasonic waves;
(4) placing the flask in an oil bath pan for prepolymerization, and removing bubbles and dissolved air after the prepolymerization is finished to degas a prepolymerization solution;
(5) treating a common glass plate purchased from the market with a silane coupling agent to make the surface hydrophobic;
(6) and (3) injecting the pre-polymerization solution obtained in the step (4) into the glass mold pretreated by the silane coupling agent in the step (5), placing the glass mold in a water bath for reaction and curing, and then performing secondary curing molding in a forced air oven to obtain the transparent antistatic PMMA.
4. The preparation method of the transparent antistatic PMMA according to claim 3, wherein the ultrasonic temperature in the step (3) is 80-90 ℃, and the ultrasonic time is 60 min.
5. The method for preparing transparent antistatic PMMA according to the claim 3, characterized in that the temperature of the oil bath in the step (4) is 80 ℃ to 90 ℃; the method for judging the prepolymerization end point comprises the following steps: the end point of the prepolymerization is 10s after a large amount of bubbles in the flask emerge.
6. The method for preparing transparent antistatic PMMA according to the claim 3, characterized in that the concrete method of treating the commercial glass plate with silane coupling agent in the step (5) is: after washing and drying a commercially available glass plate with ethanol and deionized water, the surface of the glass plate was subjected to a hydrophobic treatment by immersing the plate in an acetone solution containing 1.50g of hexadecyltrimethoxysilane HTEOS for 10 seconds.
7. The method for preparing transparent antistatic PMMA according to the claim 3 or 4 or 5 or 6, characterized in that the glass plate mold size in the step (6) is 15cm x 4 mm; the method for injecting the pre-polymerization liquid comprises the following steps: placing the rubber ring on a glass plate treated by a silane coupling agent, covering the rubber ring with another glass plate treated by the silane coupling agent, sealing the rubber ring by using a clamp to leave a gap, injecting a pre-polymerization solution into the gap, and well sealing the two glass plates by using the clamp; the temperature of the water bath is 60-75 ℃, and the reaction time is 180 min; the temperature of the air-blowing oven is 100-110 ℃, and the curing treatment time in the air-blowing oven is 60 min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810138873.7A CN108314753B (en) | 2018-02-10 | 2018-02-10 | Transparent antistatic PMMA and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810138873.7A CN108314753B (en) | 2018-02-10 | 2018-02-10 | Transparent antistatic PMMA and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108314753A CN108314753A (en) | 2018-07-24 |
| CN108314753B true CN108314753B (en) | 2021-03-09 |
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| CN109369843A (en) * | 2018-11-14 | 2019-02-22 | 安徽新涛光电科技有限公司 | A kind of preparation process of antistatic organic glass |
| CN110373122B (en) * | 2019-05-07 | 2021-07-30 | 浙江工业大学 | Interlayer glass intermediate film and preparation method thereof |
| CN111499795A (en) * | 2020-05-07 | 2020-08-07 | 浙江展宇新材料有限公司 | Production process of PMMA monomer copolymerized organic glass |
| CN112666770B (en) * | 2021-01-12 | 2022-09-23 | 浙江工业大学 | Electrochromic flexible device based on P (SPMA-MMA) hydrogel electrolyte and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS4934587Y1 (en) * | 1970-08-11 | 1974-09-19 | ||
| US5086106A (en) * | 1986-09-08 | 1992-02-04 | Mitsubishi Rayon Company Ltd. | Methacrylic resin cast plate having excellent antistatic property |
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| JPS5423395B2 (en) * | 1972-07-31 | 1979-08-13 | ||
| JPS5974150A (en) * | 1982-10-20 | 1984-04-26 | Takemoto Oil & Fat Co Ltd | Method for destaticizing methyl methacrylate resin molding |
| JPH06329730A (en) * | 1993-05-25 | 1994-11-29 | Nippon Niyuukazai Kk | Antistatic composition |
| CN103590249B (en) * | 2013-11-20 | 2015-05-13 | 上海天伟纺织质量技术服务有限公司 | Preparation method of water-repellent and oil-repellent antistatic finishing agent |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS4934587Y1 (en) * | 1970-08-11 | 1974-09-19 | ||
| US5086106A (en) * | 1986-09-08 | 1992-02-04 | Mitsubishi Rayon Company Ltd. | Methacrylic resin cast plate having excellent antistatic property |
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