CN113354917A - Preparation method of high-heat-resistance polymethyl methacrylate resin - Google Patents
Preparation method of high-heat-resistance polymethyl methacrylate resin Download PDFInfo
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- CN113354917A CN113354917A CN202110688504.7A CN202110688504A CN113354917A CN 113354917 A CN113354917 A CN 113354917A CN 202110688504 A CN202110688504 A CN 202110688504A CN 113354917 A CN113354917 A CN 113354917A
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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
- C08L55/00—Compositions of homopolymers or copolymers, obtained by polymerisation reactions only involving carbon-to-carbon unsaturated bonds, not provided for in groups C08L23/00 - C08L53/00
- C08L55/02—ABS [Acrylonitrile-Butadiene-Styrene] polymers
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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
- C08L2201/00—Properties
- C08L2201/10—Transparent films; Clear coatings; Transparent materials
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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
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The invention discloses a preparation method of high heat-resistant polymethyl methacrylate resin, which comprises the following steps; step one, preparing a raw material 1, putting propylene, acetone, propanediol and methyl methacrylate which have certain components into a reaction kettle, adding a compatilizer a, an initiator and a chain transfer agent which have certain components, mixing, and carrying out polymerization reaction to obtain the raw material 1; and step two, putting the raw material 1 and 50-70 parts of ABS highlight particles into a reaction kettle, heating to a molten state, adding the main antioxidant 1010 and the auxiliary antioxidant 168, and stirring and mixing at 150-180 ℃ for 60-70 min. According to the invention, polyimide PI with different components is added into the raw material 1 and ABS highlight particles, so that the heat resistance of the polymer can be improved, the PMMA resin has good performance, the conversion rate and the light transmittance are obviously increased, the heat resistance temperature of the polymethyl methacrylate resin is greatly improved, and the polymerization difficulty and the production cost are ensured.
Description
Technical Field
The invention relates to the technical field of preparation of high molecular materials, in particular to a preparation method of high heat-resistant polymethyl methacrylate resin.
Background
Polymethyl methacrylate (PMMA), a high molecular polymer, also called acrylic or organic glass, has the advantages of high transparency, low price, easy machining, etc., is a commonly used glass substitute material, and has many excellent properties, such as: high light transmission, light weight, easy processing and forming, good dimensional stability, weather resistance and electrical insulation, difficult coloring and the like; therefore, the free radical polymerization PMMA has a low glass transition temperature of only 105 ℃ and usually begins to be thermally degraded at 150 ℃, which makes the polymer easily thermally degraded not only in the production and processing process, but also easily deformed in the use process, and severely limits the application range of the PMMA, generally, a cyclic structure is introduced into a main chain and a side chain of a macromolecule, and the methyl group at alpha position is replaced by fluorine, chlorine, nitro group and cyano group, and a copolymerized organic metal salt improves the heat resistance of PMMA resin, but increases the difficulty and production cost of polymerization, and simultaneously reduces the processability and light transmittance of the polymer.
Disclosure of Invention
The invention aims to provide a preparation method of a polymethyl methacrylate resin with high heat resistance, which aims to solve the problems of increasing the heat resistance while ensuring the difficulty of polymerization and the production cost, and simultaneously reducing the processability and light transmittance of a polymer in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of polymethyl methacrylate resin with high heat resistance comprises the following steps;
step one, preparing a raw material 1, putting propylene, acetone, propanediol and methyl methacrylate which have certain components into a reaction kettle, adding a compatilizer a, an initiator and a chain transfer agent which have certain components, mixing, and carrying out polymerization reaction to obtain the raw material 1;
secondly, putting the raw material 1 and 50-70 parts of ABS highlight particles into a reaction kettle, heating to a molten state, adding the main antioxidant 1010 and the auxiliary antioxidant 168, and stirring and mixing at 150-180 ℃ for 60-70 min;
adding 5-20 parts of polyimide PI into a reaction kettle, adding 1.2-1.8 parts of compatilizer b and 2-5 parts of fixing agent, and continuing to perform polymerization reaction at 150-180 ℃ for 1-2 hours to obtain a raw material 2;
and step four, extruding and molding the raw material 2 obtained in the step three by a single-screw extruder to obtain the polymethyl methacrylate resin with high heat resistance.
Preferably, the raw material 1 consists of the following raw materials in parts by weight: 30-40 parts of propylene, 10-20 parts of acetone, 30-35 parts of propylene glycol, 20-30 parts of methyl methacrylate, 2-6 parts of compatilizer b, 10-13 parts of initiator and 10-13 parts of chain transfer agent.
Preferably, the compatilizer a and the compatilizer b are one or more of styrene grafted maleic anhydride, ethylene-methyl acrylate copolymer, maleic anhydride graft and maleic anhydride monomer.
Preferably, the initiator is any one of azobisisobutyronitrile, azobisisoheptonitrile, methyl ethyl ketone peroxide and cyclohexanone peroxide.
Preferably, the chain transfer agent is any one of n-butylmercaptan, isobutylmercaptan, n-octylmercaptan, n-dodecylmercaptan, benzoyl peroxide, tert-butyl peroxybenzoate, thiophenol of aromatic thiophenol compound, toluenethiol, and 4-tert-butyl-o-toluenethiol of thiol compound.
Preferably, the fixing agent is any one of uranium acetate, acrolein, tannic acid and potassium permanganate.
Preferably, the temperature of a charging barrel feeding area of the screw extruder is 60-80 ℃, the temperature of a first interval is 150-200 ℃, the temperature of a second interval is 180-220 ℃, the temperature of a third interval is 200-250 ℃, the temperature of a fourth interval is 200-250 ℃, and the temperature of a 5 th interval is 200-250 ℃.
Preferably, the screw rotating speed of the screw extruder is 0.3 m/s-1.2 m/s.
The preparation method of the high heat-resistant polymethyl methacrylate resin provided by the invention has the beneficial effects that:
according to the invention, polyimide PI with different components is added into the raw material 1 and ABS highlight particles, so that the heat resistance of the polymer can be improved, the polymerization reaction time can be accelerated by adding the compatilizer and the fixing agent in corresponding parts, the PMMA resin has good performance, the conversion rate and the light transmittance are obviously increased, the heat resistance temperature of the polymethyl methacrylate resin is greatly improved, and the polymerization difficulty and the production cost are ensured.
Drawings
FIG. 1 is a graph of experimental data for the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Embodiment 1, the present invention provides a technical solution: a preparation method of polymethyl methacrylate resin with high heat resistance comprises the following steps;
step one, preparing a raw material 1, namely putting 30 parts of propylene, 15 parts of acetone, 31 parts of propanediol and 22 parts of methyl methacrylate into a reaction kettle, adding 2 parts of ethylene-methyl acrylate copolymer, 12 parts of azobisisobutyronitrile and 10 parts of isobutylmercaptan, mixing, and carrying out polymerization reaction to obtain the raw material 1;
step two, putting the raw material 1 and 60 parts of ABS highlight particles into a reaction kettle, heating to a molten state, adding the main antioxidant 1010 and the auxiliary antioxidant 168, and stirring and mixing at 150 ℃ for 70 min;
step three, adding 5 parts of polyimide PI into a reaction kettle, adding 1.8 parts of maleic anhydride monomer and 3 parts of acrolein, and continuing to perform polymerization reaction at 160 ℃ for 1.2 hours to obtain a raw material 2;
and step four, extruding and molding the raw material 2 obtained in the step three by a single screw extruder, wherein the temperature of a charging barrel feeding area of the screw extruder is 60 ℃, the temperature of a first interval is 150 ℃, the temperature of a second interval is 180 ℃, the temperature of a third interval is 200 ℃, the temperature of a fourth interval is 200 ℃, the temperature of a 5 th interval is 250 ℃, and the screw rotating speed of the screw extruder is 1.2m/s, so as to obtain the polymethyl methacrylate resin with high heat resistance.
Embodiment 2, the present invention provides a technical solution: a preparation method of polymethyl methacrylate resin with high heat resistance comprises the following steps;
step one, preparing a raw material 1, namely putting 32 parts of propylene, 17 parts of acetone, 32 parts of propanediol and 23 parts of methyl methacrylate into a reaction kettle, adding 4 parts of styrene grafted maleic anhydride, 12 parts of azobisisobutyronitrile and 10 parts of isobutylmercaptan, mixing, and carrying out polymerization reaction to obtain the raw material 1;
step two, putting the raw material 1 and 65 parts of ABS highlight particles into a reaction kettle, heating to a molten state, adding the main antioxidant 1010 and the auxiliary antioxidant 168, and stirring and mixing at 150 ℃ for 60 min;
step three, adding 10 parts of polyimide PI into a reaction kettle, adding 1.5 parts of maleic anhydride monomer and 5 parts of acrolein, and continuing to perform polymerization reaction at 150 ℃ for 2 hours to obtain a raw material 2;
and step four, extruding and molding the raw material 2 obtained in the step three by a single screw extruder, wherein the temperature of a charging barrel feeding area of the screw extruder is 70 ℃, the temperature of a first interval is 150 ℃, the temperature of a second interval is 180 ℃, the temperature of a third interval is 210 ℃, the temperature of a fourth interval is 250 ℃, the temperature of a 5 th interval is 250 ℃, and the screw rotating speed of the screw extruder is 0.8m/s, so as to obtain the polymethyl methacrylate resin with high heat resistance.
Embodiment 3, the present invention provides a technical solution: a preparation method of polymethyl methacrylate resin with high heat resistance comprises the following steps;
step one, preparing a raw material 1, namely putting 30 parts of propylene, 16 parts of acetone, 32 parts of propanediol and 22 parts of methyl methacrylate into a reaction kettle, adding 3 parts of ethylene-methyl acrylate copolymer, 12 parts of azobisisobutyronitrile and 10 parts of n-octyl mercaptan, mixing, and carrying out polymerization reaction to obtain the raw material 1;
step two, putting the raw material 1 and 60 parts of ABS highlight particles into a reaction kettle, heating to a molten state, adding the main antioxidant 1010 and the auxiliary antioxidant 168, and stirring and mixing at 150 ℃ for 70 min;
step three, adding 5 parts of polyimide PI into a reaction kettle, adding 1.8 parts of maleic anhydride graft and 4 parts of uranium acetate, and continuing to perform polymerization reaction at 180 ℃ for 1 hour to obtain a raw material 2;
and step four, extruding and molding the raw material 2 obtained in the step three by a single screw extruder, wherein the temperature of a charging barrel feeding area of the screw extruder is 70 ℃, the temperature of a first interval is 150 ℃, the temperature of a second interval is 180 ℃, the temperature of a third interval is 200 ℃, the temperature of a fourth interval is 200 ℃, the temperature of a 5 th interval is 250 ℃, and the screw rotating speed of the screw extruder is 0.8m/s, so as to obtain the polymethyl methacrylate resin with high heat resistance.
Embodiment 4, the present invention provides a technical solution: a preparation method of polymethyl methacrylate resin with high heat resistance comprises the following steps;
step one, preparing a raw material 1, namely putting 30 parts of propylene, 18 parts of acetone, 30 parts of propanediol and 25 parts of methyl methacrylate into a reaction kettle, adding 2 parts of ethylene-methyl acrylate copolymer, 12 parts of methyl ethyl ketone peroxide and 10 parts of isobutyl mercaptan, mixing, and carrying out polymerization reaction to obtain the raw material 1;
step two, putting the raw material 1 and 70 parts of ABS highlight particles into a reaction kettle, heating to a molten state, adding the main antioxidant 1010 and the auxiliary antioxidant 168, and stirring and mixing at 180 ℃ for 60 min;
step three, adding 5 parts of polyimide PI into a reaction kettle, adding 1.6 parts of maleic anhydride monomer and 3 parts of acrolein, and continuing to perform polymerization reaction at 180 ℃ for 1 hour to obtain a raw material 2;
and step four, extruding and molding the raw material 2 obtained in the step three by a single screw extruder, wherein the temperature of a charging barrel feeding area of the screw extruder is 80 ℃, the temperature of a first interval is 180 ℃, the temperature of a second interval is 200 ℃, the temperature of a third interval is 220 ℃, the temperature of a fourth interval is 250 ℃, the temperature of a 5 th interval is 250 ℃, and the screw rotating speed of the screw extruder is 0.4m/s, so as to obtain the polymethyl methacrylate resin with high heat resistance.
Embodiment 5, the present invention provides a technical solution: a preparation method of polymethyl methacrylate resin with high heat resistance comprises the following steps;
step one, preparing a raw material 1, namely putting 40 parts of propylene, 10 parts of acetone, 35 parts of propanediol and 20 parts of methyl methacrylate into a reaction kettle, adding 2 parts of ethylene-methyl acrylate copolymer, 10 parts of azobisisobutyronitrile and 10 parts of n-dodecyl mercaptan, mixing, and carrying out polymerization reaction to obtain the raw material 1;
step two, putting the raw material 1 and 70 parts of ABS highlight particles into a reaction kettle, heating to a molten state, adding the main antioxidant 1010 and the auxiliary antioxidant 168, and stirring and mixing for 80min at 160 ℃;
step three, adding 20 parts of polyimide PI into a reaction kettle, adding 1.2 parts of maleic anhydride monomer and 3 parts of potassium permanganate, and continuing to perform polymerization reaction at 180 ℃ for 1.2 hours to obtain a raw material 2;
and step four, extruding and molding the raw material 2 obtained in the step three by a single screw extruder, wherein the temperature of a charging barrel feeding area of the screw extruder is 70 ℃, the temperature of a first interval is 160 ℃, the temperature of a second interval is 190 ℃, the temperature of a third interval is 210 ℃, the temperature of a fourth interval is 230 ℃, the temperature of a 5 interval is 250 ℃, and the screw rotating speed of the screw extruder is 0.5m/s, so as to obtain the polymethyl methacrylate resin with high heat resistance.
The results of the conversion, light transmittance and thermal decomposition temperature resistance of the polymethyl methacrylate resins obtained in examples 1 to 5 are shown in FIG. 1.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. A preparation method of high heat-resistant polymethyl methacrylate resin is characterized by comprising the following steps: comprises the following steps;
step one, preparing a raw material 1, putting propylene, acetone, propanediol and methyl methacrylate which have certain components into a reaction kettle, adding a compatilizer a, an initiator and a chain transfer agent which have certain components, mixing, and carrying out polymerization reaction to obtain the raw material 1;
secondly, putting the raw material 1 and 50-70 parts of ABS highlight particles into a reaction kettle, heating to a molten state, adding the main antioxidant 1010 and the auxiliary antioxidant 168, and stirring and mixing at 150-180 ℃ for 60-70 min;
adding 5-20 parts of polyimide PI into a reaction kettle, adding 1.2-1.8 parts of compatilizer b and 2-5 parts of fixing agent, and continuing to perform polymerization reaction at 150-180 ℃ for 1-2 hours to obtain a raw material 2;
and step four, extruding and molding the raw material 2 obtained in the step three by a single-screw extruder to obtain the polymethyl methacrylate resin with high heat resistance.
2. The method for preparing highly heat-resistant polymethylmethacrylate resin according to claim 1, wherein: the raw material 1 comprises the following raw materials in parts by weight: 30-40 parts of propylene, 10-20 parts of acetone, 30-35 parts of propylene glycol, 20-30 parts of methyl methacrylate, 2-6 parts of compatilizer b, 10-13 parts of initiator and 10-13 parts of chain transfer agent.
3. The method for preparing highly heat-resistant polymethylmethacrylate resin according to claim 1, wherein: the compatilizer a and the compatilizer b are one or more of styrene grafted maleic anhydride and ethylene-methyl acrylate copolymer.
4. The method for preparing highly heat-resistant polymethylmethacrylate resin according to claim 1, wherein: the initiator is any one of azodiisobutyronitrile, azodiisoheptonitrile, methyl ethyl ketone peroxide and cyclohexanone peroxide.
5. The method for preparing highly heat-resistant polymethylmethacrylate resin according to claim 1, wherein: the chain transfer agent is any one of n-butylmercaptan, isobutylmercaptan, n-octylmercaptan, n-dodecylmercaptan, benzoyl peroxide, tert-butyl peroxybenzoate of mercaptan compounds, thiophenol, toluene thiophenol and 4-tert-butyl-o-toluene thiophenol of aromatic thiophenol compounds.
6. The method for preparing highly heat-resistant polymethylmethacrylate resin according to claim 1, wherein: the fixing agent is any one of uranium acetate, acrolein, tannic acid and potassium permanganate.
7. The method for preparing highly heat-resistant polymethylmethacrylate resin according to claim 1, wherein: the temperature of a charging barrel feeding area of the screw extruder is 60-80 ℃, the temperature of a first interval is 150-200 ℃, the temperature of a second interval is 180-220 ℃, the temperature of a third interval is 200-250 ℃, the temperature of a fourth interval is 200-250 ℃, and the temperature of a 5 th interval is 200-250 ℃.
8. The method for preparing highly heat-resistant polymethylmethacrylate resin according to claim 1, wherein: the screw rotating speed of the screw extruder is 0.3-1.2 m/s.
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| CN202110688504.7A CN113354917A (en) | 2021-06-23 | 2021-06-23 | Preparation method of high-heat-resistance polymethyl methacrylate resin |
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| CN202110688504.7A CN113354917A (en) | 2021-06-23 | 2021-06-23 | Preparation method of high-heat-resistance polymethyl methacrylate resin |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0455116A1 (en) * | 1990-04-28 | 1991-11-06 | Röhm Gmbh | Thermoplastically processable polymer compositions based on polymethacrylate with addition of ABS and polycarbonate |
| CN101238177A (en) * | 2005-08-04 | 2008-08-06 | 东丽株式会社 | Resin c0mp0siti0n and m0lded article c0mprising the same |
| CN102532781A (en) * | 2010-12-07 | 2012-07-04 | 合肥杰事杰新材料股份有限公司 | High-luster scratching-resistant ABS (Acrylonitrile-Butadiene-Styrene) resin and preparation method thereof |
| CN103044848A (en) * | 2013-01-04 | 2013-04-17 | 四川长虹电器股份有限公司 | ABS/PMMA composite and preparation method thereof |
| CN106947199A (en) * | 2017-05-02 | 2017-07-14 | 湖南峰业光电有限公司 | A kind of TV high heat resistant transparent reinforcing material and its preparation method and application |
| CN111423683A (en) * | 2020-04-24 | 2020-07-17 | 聚纶材料科技（深圳）有限公司 | Optical resin for optical protective film and preparation method thereof |
-
2021
- 2021-06-23 CN CN202110688504.7A patent/CN113354917A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0455116A1 (en) * | 1990-04-28 | 1991-11-06 | Röhm Gmbh | Thermoplastically processable polymer compositions based on polymethacrylate with addition of ABS and polycarbonate |
| CN101238177A (en) * | 2005-08-04 | 2008-08-06 | 东丽株式会社 | Resin c0mp0siti0n and m0lded article c0mprising the same |
| CN102532781A (en) * | 2010-12-07 | 2012-07-04 | 合肥杰事杰新材料股份有限公司 | High-luster scratching-resistant ABS (Acrylonitrile-Butadiene-Styrene) resin and preparation method thereof |
| CN103044848A (en) * | 2013-01-04 | 2013-04-17 | 四川长虹电器股份有限公司 | ABS/PMMA composite and preparation method thereof |
| CN106947199A (en) * | 2017-05-02 | 2017-07-14 | 湖南峰业光电有限公司 | A kind of TV high heat resistant transparent reinforcing material and its preparation method and application |
| CN111423683A (en) * | 2020-04-24 | 2020-07-17 | 聚纶材料科技（深圳）有限公司 | Optical resin for optical protective film and preparation method thereof |
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Application publication date: 20210907 |