CN107513196B - Method for efficiently heating high-molecular polymer by using microwaves - Google Patents
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- 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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
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- C08K7/08—Oxygen-containing compounds
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- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
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- C08J2325/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Derivatives of such polymers
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- C08J2325/04—Homopolymers or copolymers of styrene
- C08J2325/06—Polystyrene
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- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
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- C08J2371/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
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Abstract
The invention discloses a method for efficiently heating a high molecular polymer by using microwaves, which comprises the following steps: a small amount of dielectric loss ceramic materials with efficient wave-absorbing characteristics are added into high molecular polymers or monomers or oligomers thereof, so that the traditional microwave transparent high molecular polymers with low dielectric loss, which cannot be heated by microwaves, and the monomers and oligomers thereof can be rapidly heated under the action of microwaves. The device can realize the rapid, controllable and uniform heating of the high molecular polymer and the monomer and oligomer thereof, can improve the production efficiency, improve the product quality, reduce the energy consumption and increase the convenience and the easiness of automatic control. Meanwhile, as the microwave sensitive additive used in the method is a ceramic material with efficient wave-absorbing property, the addition amount is very small and is only 0.1-5% of the volume of the high-molecular polymer on the premise of meeting the requirement of rapid heating; therefore, the method has little influence on the performance of the polymer and has wide application range.
Description
Technical Field
The invention relates to a microwave heating method of a high molecular polymer, belonging to the field of high molecular materials.
Background
A general conventional method for heating a high molecular polymer is to heat the surface of the material by heating the surrounding environment, radiating heat, conducting heat or by hot air convection, and then conducting the heat to the interior of the material. The method has low efficiency, long heating time, uneven heating and large thermal stress. The microwave heating has the biggest characteristic that the microwave is generated inside a heated object, a heat source comes from the inside of the object, the heating is uniform, the phenomenon of half-cooked inside outer coke cannot be caused, the product quality is favorably improved, meanwhile, the heating time is greatly shortened due to the fact that the inside and the outside are heated simultaneously, the heating efficiency is high, and the product yield is favorably improved. The inertia of microwave heating is very small, the rapid control of temperature rise and fall can be realized, and the continuous production and the automatic control are facilitated.
Microwave is an electromagnetic wave that follows the law of relevance for electromagnetic waves and can be transmitted, absorbed or reflected by matter. Depending on the properties of the material in the microwave field, three types can be distinguished: (1) microwave transparent materials, mainly low loss insulators, such as most high molecular polymers. (2) The microwave material is totally reflected, and the microwave reflection coefficient is close to 1, such as most metals. (3) Microwave absorbing materials such as paper, wood, water, paraffin, ceramics, etc. The traditional microwave heating technology can only heat microwave absorption materials such as water, wood and the like, but most high molecular polymers such as PP, PE, PET, PS, PA, PTFE and the like generally do not generate heat in microwave, are only used as wave-transparent materials and cannot be heated by microwave.
At present, for the application of microwave heating polymer materials, the application mainly focuses on using microwave to heat free radical polymerization monomers for polymerization, or using microwave to heat epoxy resin compositions for curing; the used means mainly depends on the electric conduction loss and the magnetic loss, and realizes the absorption of the microwave by adding conductive materials such as metal powder, graphite and the like and magnetic materials such as ferrite and the like. For example: thermosetting compositions containing epoxy resin and additional steel or aluminum fibers or graphite fibers or powders, as shown in U.S. patent No. 4626642, can be cured by microwave heating. Chinese patent CN 100418740C teaches that a resin prepared by dissolving an olefin monomer capable of undergoing radical polymerization and a thermoplastic polymer soluble in the olefin monomer is used as an impregnation solution to impregnate continuous fibers, and then the continuous fibers are heated, polymerized, cured and molded by a microwave reaction chamber to prepare continuous fiber reinforced plastics. Chinese patent CN105283513A teaches that an insulating adhesive resin having a curable property can be cured by microwave heating by adding a conductive filler. Chinese patent CN 104761668A teaches that by adding fine silicon carbide powder to nonpolar monomers, bulk polymerization of the monomers can be achieved by microwave heating. CN 102027054B indicates that magnetite particles and conductive carbon material particles are added to a thermosetting epoxy resin composition, which can be cured using microwave heating.
At present, the reports of heating the high polymer by using microwaves are less, more reports only stay in the theoretical assumption stage, and the high-efficiency application is not substantial. Chinese patent CN 101932428A discloses a thermoplastic material capable of microwave heating, which is characterized in that microwave receiving additive is added into the thermoplastic material. Specific information on the added microwave receptive additive is not explicitly recited in the claims, but only that in the specific implementation method almost all substances that may absorb microwaves are listed, and that a specific substance is not specifically described; a particularly efficient microwave receptive additive is obtained without screening, preparation or modification, and no method for adding a microwave receptive additive to a polymer is specifically suggested; the microwave receiving additive as claimed in the claims is used in a wide range of amount, and a preferable ratio is not preferred. It follows that this patent mainly proposes an idea of being able to microwave heat thermoplastic materials, and is not optimized to obtain an efficient implementation. In addition, the microwave receptive additive of this patent is present in an amount of 0 to 25% by volume. Calculated according to the maximum volume content of 25 percent, the specific gravity of most polymers is 1 to 1.2, and the value is 1.1; the specific gravity of most metal oxide and other additives is 4-6, and the value is 5; the maximum weight content of the microwave receiving additive is about 60 percent, and the influence of the addition amount on the performance of the polymer is large.
Disclosure of Invention
The purpose of the invention is: the problem is solved by using a high-efficiency microwave-absorbing substance, and adding the substance into the polymer in a small amount, so that the cured products of the polymerized thermoplastic high-molecular polymer and the cured thermosetting high-molecular polymer which are difficult to be heated by microwaves can be rapidly heated by microwaves. Meanwhile, the polymer monomer and the oligomer can be polymerized to form the high polymer by microwave heating. The addition amount is small, and therefore, the influence on the properties of the polymer itself is extremely small. Thus, the method has important significance in the fields of rapid molding of thermoplastic high molecular polymers, rapid curing and post-curing of thermosetting high molecular polymers and the like.
The technical scheme for realizing the purpose of the invention is as follows: the dielectric loss ceramic material with efficient wave-absorbing property is added into the high molecular polymer, so that the high molecular polymer can be rapidly heated by microwaves.
The dielectric loss ceramic material with the efficient wave-absorbing characteristic refers to one-dimensional zinc oxide ceramic powder and comprises needle-rod-shaped, four-needle-shaped, chrysanthemum-shaped, multi-needle-shaped and network-shaped zinc oxide whiskers; the amount of the polymer is 0.01 to 5% by volume, for example, 0.01%, 1%, 1.5%, 2%, 4%, 5%, preferably 0.1 to 1%, particularly preferably 0.2 to 0.5% by volume of the polymer or monomer or oligomer.
The high polymer refers to thermoplastic high polymer including PP, PE, PET, PA, PC, PTFE, ABS, PEEK, PMMA, PVC, PS, POM, PU, phenoxy resin and thermosetting high polymer including epoxy resin, unsaturated polyester resin, polyurethane resin, vinyl ester resin, phenolic resin and cured product thereof.
For most thermoplastic high molecular polymers such as PP, PE, ABS, PVC, PS, etc., it is common practice to mix polymer powder and ceramic powder directly and uniformly. The uniformly mixed powder can be directly used or can be used after granulation.
For polymers such as phenoxy resin, which can be dissolved in a solvent but are difficult to prepare into powder, the polymer can be dissolved in the solvent, then ceramic powder is added into the solvent for uniform dispersion, and finally the solvent is removed to obtain the product.
For polymers such as PS and PMMA which can be dissolved by monomers or the monomers can be easily polymerized, ceramic powder can be added into the polymers dissolved in the monomers or directly added into the monomers, and finally the monomers are polymerized to obtain the product.
For thermosetting high molecular polymers such as epoxy resins, unsaturated polyester resins, vinyl ester resins, phenol resins, polyurethane resins, etc., ceramic powder may be dispersed in uncured resin and then cured.
The principle of the invention is as follows: the zinc oxide crystal whisker comprises a needle-rod-shaped, four-needle-shaped, chrysanthemum-shaped, multi-needle-shaped and network-shaped zinc oxide crystal whisker, and is zinc oxide ceramic powder with a certain shape prepared from common zinc oxide. The sensitivity of the zinc oxide with the specific forms to microwaves is much higher than that of common zinc oxide, and the zinc oxide is greatly superior to common microwave sensitive materials such as graphite powder, metal powder, ferrite magnetic powder, common metal oxide powder, common metal carbide powder and the like, and the high molecular polymer can be rapidly heated by the microwaves only by extremely small addition amount. The thermoplastic polymer added with the dielectric loss ceramic powder with the efficient wave-absorbing characteristic, such as polypropylene, polyethylene terephthalate, polyamide, polycarbonate, polytetrafluoroethylene, acrylonitrile-butadiene-styrene copolymer, polyether ether ketone, polyvinyl chloride, polyformaldehyde, polystyrene, polymethyl methacrylate and phenoxy resin, is softened or melted mainly by microwave heating, so that secondary molding is facilitated. For thermosetting polymers such as epoxy resins, unsaturated polyester resins, polyurethane resins, phenolic resins, and the like, uncured resins can generally be cured by microwave heating, but are not efficient. The addition of the dielectric loss ceramic material with efficient wave-absorbing property can improve the microwave heating efficiency. The thermosetting polymer cured product can not be heated by microwave generally, and can be heated by microwave after a dielectric loss ceramic material with efficient wave absorbing property is added.
Because microwave heating converts microwave energy absorbed by the high molecular polymer into kinetic energy and potential energy of molecules in the high molecular polymer, heat is generated from the inside of the high molecular polymer, and is not from other heating elements. Thus, the material is heated uniformly and integrally, and the internal thermal stress and thermal inertia of the high molecular polymer are small. Therefore, the invention realizes the rapid, controllable and uniform heating of the high molecular polymer, can improve the production efficiency, improve the product quality, reduce the energy consumption, increase the convenience of automatic control, and has important significance for the fields of rapid molding of thermoplastic high molecular polymers, rapid post-curing of thermosetting high molecular polymers and the like.
Detailed Description
The present invention will be described in further detail below with reference to examples. The "parts" described in the examples of the present invention indicate parts by mass unless otherwise specified. The zinc oxide crystal whisker is obtained from the market.
(example 1)
Adding 2 parts of tetrapod-like zinc oxide whisker into 100 parts of polyethylene powder, and mixing uniformly. Putting the powder into a vulcanizing press, heating and pressurizing to prepare a polyethylene plate capable of being heated by microwave, wherein the volume addition amount of the zinc oxide whiskers is 0.35%, and cooling to room temperature for later use.
The above polyethylene sheet capable of microwave heating was placed in a microwave oven at 25 ℃ and room temperature, heated for 2 minutes and then taken out, and it was found that the polyethylene sheet was melted.
(example 2)
To 100 parts of polyethylene powder, 1 part of needle-like zinc oxide whisker was added and mixed uniformly. Putting the powder into a vulcanizing press, heating and pressurizing to prepare a polyethylene plate capable of being heated by microwave, wherein the volume addition amount of the zinc oxide whiskers is 0.18%, and cooling to room temperature for later use.
The above polyethylene sheet capable of microwave heating was placed in a microwave oven at 25 ℃ and room temperature, heated for 2 minutes and taken out, and the surface temperature thereof was measured to be 83 ℃.
After further heating in the microwave oven for 2 minutes, the polyethylene sheet was removed and found to have melted.
(example 3)
Adding 1 part of chrysanthemum-shaped zinc oxide whisker into 100 parts of phenolic resin butanone solution with the solid content of 40%, uniformly mixing, then coating on a glass fiber checkered cloth, naturally airing, and preparing the glass fiber reinforced phenolic resin plate, wherein the volume addition amount of the zinc oxide whisker is 0.37%.
The glass fiber-reinforced phenoxy resin plate was placed in a microwave oven at 25 ℃ and room temperature, heated for 2 minutes and then taken out, and it was found that it was softened and its surface temperature was 173 ℃.
(example 4)
Adding 0.5 part of multi-needle zinc oxide whisker into 100 parts of phenolic resin butanone solution with the solid content of 40%, uniformly mixing, then coating on a glass fiber checkered cloth, naturally airing, and preparing the glass fiber reinforced phenolic resin plate, wherein the volume addition amount of the zinc oxide whisker is 0.19%.
The glass fiber-reinforced phenoxy resin sheet was placed in a microwave oven at 25 ℃ and room temperature, heated for 2 minutes and then taken out, and it was found that it was softened and tested to have a surface temperature of 142 ℃.
(example 5)
A40% polystyrene-styrene solution was prepared by adding 40 parts of a polystyrene solvent to 60 parts of styrene. Adding 1 part of dibenzoyl peroxide and 2 parts of network zinc oxide whiskers, uniformly mixing, pouring into a mold made of polytetrafluoroethylene, and putting the mold and the mold into a microwave oven at a room temperature of 25 ℃. After heating for 3 minutes by microwave, the polystyrene monomer was polymerized into polystyrene, and the liquid polystyrene-styrene solution became a polystyrene board in which the volume addition amount of zinc oxide whiskers was 0.38%.
After it had cooled to 25 c, it was again placed in the microwave oven, heated for 2 minutes and then removed, and it was found to have softened, and its surface temperature was measured to be 128 c.
(example 6)
A40% polystyrene-styrene solution was prepared by adding 40 parts of a polystyrene solvent to 60 parts of styrene. Adding 1 part of dibenzoyl peroxide and 1 part of tetrapod-like zinc oxide whisker, uniformly mixing, pouring into a mold made of polytetrafluoroethylene, and putting the mold and the mold into a microwave oven at a room temperature of 25 ℃. After heating for 3 minutes by microwave, the polystyrene monomer was polymerized into polystyrene, and the liquid polystyrene-styrene solution became a polystyrene board in which the volume addition amount of zinc oxide whiskers was 0.19%.
After it had cooled to 25 c, it was again placed in a microwave oven, heated for 2 minutes and then removed, and it was found to have softened, and its surface temperature was measured to be 105 c.
(example 7)
Adding 80 parts of methyl tetrahydrophthalic anhydride, 2 parts of promoter DMP30 and 4 parts of tetrapod-like zinc oxide whisker into 100 parts of E51 bisphenol A type epoxy resin, uniformly mixing, pouring into a mold made of polytetrafluoroethylene, and putting the mold and the mold into a microwave oven at the room temperature of 25 ℃. After microwave heating for 3 minutes, it was removed and found to have cured to form an epoxy board in which the volume addition amount of zinc oxide whiskers was 0.49%.
After cooling to 25 ℃, the shore hardness of the material was tested to be 85 using a shore durometer.
It was again placed in a microwave oven, heated for 2 minutes and then taken out, and its surface temperature was measured to be 163 ℃.
(example 8)
Adding 80 parts of methyl tetrahydrophthalic anhydride, 2 parts of accelerant DMP30 and 0.2 part of tetrapod-like zinc oxide whisker into 100 parts of E51 bisphenol A type epoxy resin, uniformly mixing, pouring into a mold made of polytetrafluoroethylene, and putting into a microwave oven at a room temperature of 25 ℃ together with the mold. After microwave heating for 3 minutes, it was removed and found to have cured to form an epoxy board in which the zinc oxide whiskers were added in an amount of 0.25% by volume.
After cooling to 25 ℃, the shore hardness of the material was tested to be 80 using a shore durometer.
It was again placed in a microwave oven, heated for 2 minutes and then taken out, and its surface temperature was measured to be 132 ℃.
Comparative example 1
A common polyethylene sheet was placed in a microwave oven at 25 ℃ at room temperature, heated for 2 minutes, and taken out, and the surface temperature thereof was measured to be 26 ℃.
Comparative example 2
And (3) coating the phenolic resin butanone solution with the solid content of 40% on a glass fiber checkered cloth, and naturally airing to prepare the glass fiber reinforced phenolic resin plate.
The glass fiber-reinforced phenoxy resin plate was placed in a microwave oven at room temperature, heated for 2 minutes, and then taken out, and the surface temperature was measured to be 28 ℃.
(comparative example 3)
A general polystyrene board was placed in a microwave oven at 25 ℃ at room temperature, heated for 2 minutes, and taken out, and the surface temperature was measured to be 27 ℃.
Comparative example 4
Adding 80 parts of methyl tetrahydrophthalic anhydride and 2 parts of accelerating agent DMP30 into 100 parts of E51 bisphenol A type epoxy resin, uniformly mixing, pouring into a mold made of polytetrafluoroethylene, and putting into a microwave oven at room temperature of 25 ℃ together with the mold. After microwave heating for 3 minutes, it was removed and found to have cured.
After cooling to 25 ℃, the shore hardness of the material was tested to be 76 using a shore durometer.
It was again placed in a microwave oven, heated for 2 minutes and then taken out, and its surface temperature was measured to be 29 ℃.
The test results of the above examples and comparative examples are shown in the following table:
as can be seen from the analysis, the test result of comparative example 1 shows that the polyethylene hardly generates heat in the microwave and the surface hardly has temperature rise; after the quadralobal zinc oxide ceramic powder is added in example 1 and example 2, the quadralobal zinc oxide ceramic powder can be rapidly heated by microwave until being melted. The phenoxy resin of comparative example 2 heated in a microwave, the test surface temperature was 28 ℃, and almost no heat was generated; and examples 3 and 4, after adding the quadralobal zinc oxide ceramic powder, it can be rapidly heated by microwave to be softened with surface temperatures of 173 ℃ and 143 ℃. The polystyrene of comparative example 3 had a surface temperature of 27 ℃ in the microwave test, and hardly emitted heat; while examples 5 and 6 added quadralobal zinc oxide ceramic powder, it could be rapidly heated by microwave to soften with surface temperatures of 128 ℃ and 105 ℃. Comparative example 4 illustrates that the uncured epoxy resin can be cured by microwave heating, the shore hardness is 76, the cured epoxy resin cannot be microwave heated, and the surface temperature is 29 ℃; in examples 7 and 8, the shore hardness of the cured product was increased after adding the quadralobal zinc oxide ceramic powder, which indicates that the curing efficiency of the epoxy resin by microwave heating was improved, and the surface temperature of the cured product after microwave heating was 163 ℃ and 132 ℃, which indicates that the cured epoxy resin could also be heated by microwave.
The invention realizes the rapid, controllable and uniform heating of the high molecular polymer, can improve the production efficiency, improve the product quality, reduce the energy consumption, increase the convenience of automatic control, and has important significance for the fields of rapid molding of thermoplastic high molecular polymers, rapid post-curing of thermosetting high molecular polymers and the like.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention, and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. A method for efficiently heating a high molecular polymer by using microwaves is characterized in that: adding dielectric loss ceramic materials with efficient wave-absorbing property into high molecular polymers or monomers or oligomers thereof, so that the high molecular polymers and the monomers and the oligomers thereof which cannot be heated by microwaves can be heated by the microwaves, or the microwave heating efficiency of the high molecular polymers and the monomers and the oligomers thereof which can be heated by the microwaves is improved; the dielectric loss ceramic material is one-dimensional zinc oxide ceramic powder; the one-dimensional zinc oxide ceramic powder comprises needle-rod-shaped, four-needle-shaped, chrysanthemum-shaped, multi-needle-shaped and network-shaped zinc oxide whiskers; the addition amount of the dielectric loss ceramic material is 0.2-0.5% of the total volume of the high molecular polymer or the monomer or the oligomer.
2. The method for efficiently heating a high molecular weight polymer using microwaves according to claim 1, wherein: the high molecular polymer comprises a thermoplastic high molecular polymer and a thermosetting high molecular polymer, wherein the thermoplastic high molecular polymer comprises PP, PE, PET, PA, PC, PTFE, ABS, PEEK, PMMA, PVC, PS, POM, PU and phenoxy resin; the thermosetting high molecular polymer comprises epoxy resin, unsaturated polyester resin, polyurethane resin, vinyl ester resin and phenolic resin.
3. The method for efficiently heating a high molecular weight polymer using microwaves according to claim 1, wherein: the method for adding the dielectric loss ceramic material into the high molecular polymer is to directly mix the high molecular polymer powder and the dielectric loss ceramic material powder.
4. The method for efficiently heating a high molecular weight polymer using microwaves according to claim 1, wherein: the method for adding the dielectric loss ceramic material into the monomer or oligomer of the high molecular polymer is to add the powder of the dielectric loss ceramic material into the monomer or oligomer for uniform dispersion and then polymerize the powder to generate the high molecular polymer.
5. The method for efficiently heating a high molecular weight polymer using microwaves according to claim 1, wherein: the method for adding the dielectric loss ceramic material into the high molecular polymer is to disperse the powder of the dielectric loss ceramic material into the high molecular polymer dissolved in the solvent and then remove the solvent.
6. The method for efficiently heating a high molecular weight polymer using microwaves according to claim 1, wherein: the dielectric loss ceramic material is added to the polymer by dispersing a powder of the dielectric loss ceramic material into the molten polymer.
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| CN1539741A (en) * | 2003-04-21 | 2004-10-27 | 中国科学院理化技术研究所 | Rod-shaped zinc oxide particles, preparation method and application thereof |
| CN101591037A (en) * | 2009-07-03 | 2009-12-02 | 北京化工大学 | A kind of one-dimensional zinc oxide nanometer material and preparation method thereof |
| CN102888114A (en) * | 2011-07-22 | 2013-01-23 | 平田株式会社 | Heating rubber |
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| CN104953070B (en) * | 2015-05-06 | 2017-07-28 | 东莞市魔方新能源科技有限公司 | A kind of lithium rechargeable battery barrier film |
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| CN1539741A (en) * | 2003-04-21 | 2004-10-27 | 中国科学院理化技术研究所 | Rod-shaped zinc oxide particles, preparation method and application thereof |
| CN101591037A (en) * | 2009-07-03 | 2009-12-02 | 北京化工大学 | A kind of one-dimensional zinc oxide nanometer material and preparation method thereof |
| CN102888114A (en) * | 2011-07-22 | 2013-01-23 | 平田株式会社 | Heating rubber |
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