CN111205505A - Polymer-based porous material microwave sintering forming method and prepared polymer-based porous material - Google Patents
Polymer-based porous material microwave sintering forming method and prepared polymer-based porous material Download PDFInfo
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Abstract
The invention discloses a microwave sintering forming method of a polymer-based porous material and the prepared polymer-based porous material. The method comprises the following steps: adding polymer micro powder into liquid capable of being heated by microwave, and uniformly mixing to form a fluid state; filling the mixture into a mold, and flatly paving the mixture to completely cover the mold cavity; adjusting a microwave control box, then placing the mold in the microwave control box for sintering, taking out the mold, taking out a product when the temperature is reduced to room temperature, and finishing; and (3) placing the obtained sample in deionized water, carrying out ultrasonic treatment for 3-5 hours, then placing the sample in an oven, drying the sample for 3-5 hours at the temperature of 70-80 ℃, and removing a liquid phase to obtain the required porous material. The method has the advantages of rapidness, homogeneity, selectivity and the like by utilizing microwave sintering molding, is short in molding time and high in heat energy utilization rate, and the obtained product is good in hole-opening property, high in porosity, high in mechanical property, short in molding period and simple to operate by utilizing microwave to selectively heat liquid for experiments.
Description
Technical Field
The invention belongs to the technical field of porous polymer material forming, and particularly relates to a microwave sintering forming method of a polymer-based porous material and the prepared polymer-based porous material.
Background
Because different materials and different objects have different absorption to microwaves, the objects can be selectively heated by utilizing the heat generated by the coupling of the special wave band of the microwaves and the basic fine structure of the materials, the large-area zero-gradient uniform heating of the materials is realized, and the microwave sintering has the characteristics of high temperature rise speed, high energy utilization rate, high heating efficiency, safety, environmental protection, no pollution and the like, thereby becoming a new process method for sintering the materials and being widely used for preparing stainless steel, copper-zinc alloy, tungsten-copper alloy, nickel-based high-temperature alloy, hard alloy, electronic ceramic and the like. The invention CN110375543A discloses a method and equipment for continuous microwave sintering or melting molding of dielectric materials, which utilizes the special wave band of microwave to couple with the basic fine structure of the material to generate heat, and the dielectric loss of the material makes the material integrally heated to sintering temperature or melting temperature to achieve the effect of densification, sintering or melting of products. The invention CN109837411A discloses a microwave sintering carbon nano tube reinforced copper-based composite material, which improves the hardness and the wear resistance of copper-based powder alloy and provides a new production process for preparing a high-performance carbon nano tube reinforced copper-based composite material.
At present, microwave sintering is a new research hotspot in the field of material sintering, but no corresponding research is carried out in the field of polymers. The polymer-based porous material has excellent comprehensive performance and is widely applied to various fields, but the currently adopted methods such as a powder sintering method, a thermal phase separation method, an inorganic filling method and the like have the defects of long forming period, nonuniform heating, complex operation and the like; the microwave sintering is introduced into the forming method of the polymer-based porous material, so that the production efficiency and the energy utilization rate are greatly improved, and the method is suitable for large-scale production. And the polymer matrix can be uniformly heated by utilizing the selective heating of microwave to liquid, such as glycerol, so that the polymer matrix porous material with adjustable porosity and pore diameter and uniform structure is obtained.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a microwave sintering forming method of a polymer-based porous material and the prepared polymer-based porous material. The method provided by the invention is a microwave sintering forming method for preparing the polymer-based porous material, which has the advantages of high porosity, adjustable porosity and pore size, high heating rate, high sintering speed and high production efficiency.
The purpose of the invention is realized by at least one of the following technical solutions.
The invention provides a microwave sintering forming method of a polymer-based porous material, which comprises the following steps:
(1) weighing polymer micro powder and liquid capable of being heated by microwaves, adding the polymer powder into the liquid capable of being heated by microwaves, and uniformly mixing to obtain mixed liquid (in a fluid state with certain viscosity);
(2) putting the mixed liquid obtained in the step (1) into a mould, tiling the mixed liquid to enable the mixed liquid to completely cover a mould cavity, adjusting a microwave control box, setting a required temperature, then placing the mould into the microwave control box, turning on a microwave control switch, then carrying out microwave heating sintering treatment, taking out the mould, opening the mould cavity, taking out a product, and obtaining a sintered sample;
(3) and (3) soaking the sintered sample in the step (2) in water, performing ultrasonic treatment, then putting the sample into an oven for drying, and removing a liquid phase to obtain the polymer-based porous material (the porous material).
Further, the polymer powder of the step (1) has a microscopic morphology of spherical or ellipsoidal shape and an average particle diameter of 25 to 150 μm. The polymer powder absorbs substantially no or little microwaves.
Further, the polymer in the step (1) is more than one of high density polyethylene, polypropylene, ultra-high molecular weight polyethylene, polytetrafluoroethylene, polysulfone plastic and the like. The polymer is pure powder or a polymer mixture added with an auxiliary agent.
Further, the liquid capable of being heated by microwave in the step (1) is more than one of glycerol, ethylene glycol and sulfolane. The microwavable liquid is soluble in water. The liquid capable of being heated by microwaves can absorb microwaves to different degrees, so that a heating effect is formed.
Further, the mass ratio of the polymer powder to the microwave heatable liquid in the step (1) is 6: 4-2: 8.
further, the temperature of the microwave heating sintering treatment in the step (2) is 170-200 ℃.
Further, the time of the microwave heating sintering treatment in the step (2) is 2-10 minutes.
Further, the time of the ultrasonic treatment in the step (3) is 3-5 hours.
Further, the drying temperature in the step (3) is 70-80 ℃, and the drying time is 3-5 hours.
The invention provides a polymer-based porous material prepared by the microwave sintering forming method.
The polymer-based porous material provided by the invention achieves a rapid heating effect by selectively heating liquid by microwaves, realizes bonding among polymer powder particles to obtain the required porous material, and adjusts the porosity and the pore size by changing the ratio of the liquid to the polymer powder.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the invention adopts the microwave sintering method to heat and sinter the polymer micro powder and the liquid which can be heated by microwave, and has the advantages of high heating rate, high sintering rate, high production efficiency and high porosity of the material;
(2) the invention utilizes the selective heating of microwave to the liquid, and the effect of integral heating is formed by the continuous phase formed by the liquid in the porous powder, so that the zero-gradient uniform heating of a large area in the material is realized, the material is uniformly heated, the thermal stress in the product is reduced, and the obtained product has good openness and uniform porous structure;
(3) according to the invention, the liquid is selectively heated by microwaves, the form of the polymer micro powder is basically not influenced in the heating process, the liquid phase can realize a good heating effect, the control of a heating area is realized, and the porosity and the pore size of the porous material can be regulated and controlled by adjusting different proportions of the polymer powder and the liquid;
(4) the microwave sintering forming method used by the invention is easy to control, safe, pollution-free, short in forming time, simple to operate, easy to control and suitable for large-scale production.
Drawings
FIGS. 1a and 1c are SEM images of the polymer-based porous material prepared in example 1 at different scales;
FIG. 1b is a SEM image of the microstructure of the polymer-based porous material prepared in example 2.
Detailed Description
The following examples are presented to further illustrate the practice of the invention, but the practice and protection of the invention is not limited thereto. It is noted that the processes described below, if not specifically described in detail, are all realizable or understandable by those skilled in the art with reference to the prior art. The reagents or apparatus used are not indicated to the manufacturer, and are considered to be conventional products available by commercial purchase.
Example 1
The microwave sintering forming method for the polymer-based porous material comprises the following steps:
(1) cleaning the die: and cleaning the mold cavity.
(2) Feeding: weighing by using an electronic scale, wherein the ratio is 4: 6, adding polymer powder into glycerol, and uniformly mixing the two components to form a fluid state with certain viscosity to obtain a mixture.
(3) Die filling: and (3) filling the mixture into a mold, and flatly paving the mixture to completely cover the mold cavity.
(4) Controlling the temperature: the microwave control box was adjusted and placed in the temperature range of 170 ℃ and 200 ℃ to set the required temperature, which was 200 ℃ in example 1.
(5) Microwave sintering: and (5) placing the die in a microwave control box for sintering, and timing for 2 minutes.
(6) Cooling and taking out: and after the timing is finished, the microwave sintering forming process is finished, the temperature control box is closed, the mold is taken out, and when the temperature is reduced to the room temperature, the product is taken out and trimmed.
(7) And (3) placing the obtained sample in deionized water, carrying out ultrasonic treatment for 5 hours, then placing the sample in an oven, drying the sample for 3 hours at the temperature of 70 ℃, and removing a glycerol phase to obtain the polymer-based porous material.
(8) And carrying out porosity test, micro-morphology test and mechanical property test on the obtained sample.
Example 2 (examples 1-2, in which ultra-high molecular weight polyethylene micropowder was used for microwave sintering test and brand XM220 was used, except that the ratio of ultra-high molecular weight polyethylene to glycerin was different)
The microwave sintering forming method for the polymer-based porous material comprises the following steps:
(1) cleaning the die: and cleaning the mold cavity.
(2) Feeding: weighing by using an electronic scale according to the ratio of 2: 8, adding polymer powder into glycerol, and uniformly mixing the two components to form a fluid state with certain viscosity to obtain a mixture.
(3) Die filling: the mixture is filled into a mold and laid flat so that it completely covers the mold cavity.
(4) Controlling the temperature: the microwave control box is adjusted and placed in a temperature range of 170-200 ℃, the required temperature is set, and the temperature set in the embodiment 2 is 200 ℃.
(5) Microwave sintering: and (5) placing the die in a microwave control box for sintering, and timing for 2 minutes.
(6) Cooling and taking out: and after the timing is finished, the microwave sintering forming process is finished, the temperature control box is closed, the mold is taken out, and when the temperature is reduced to the room temperature, the product is taken out and trimmed.
(7) And (3) placing the obtained sample in deionized water, carrying out ultrasonic treatment for 5 hours, then placing the sample in an oven, drying the sample for 3 hours at the temperature of 70 ℃, and removing a glycerol phase to obtain the polymer-based porous material.
(8) And carrying out porosity test, micro-morphology test and mechanical property test on the obtained sample.
Example 3
The microwave sintering forming method for the polymer-based porous material comprises the following steps:
(1) cleaning the die: and cleaning the mold cavity.
(2) Feeding: weighing by using an electronic scale, wherein the ratio is 4: 6, adding polymer powder into sulfolane, and uniformly mixing the two components to form a fluid state with certain viscosity to obtain a mixture.
(3) Die filling: the mixture is filled into a mold and laid flat so that it completely covers the mold cavity.
(4) Controlling the temperature: the microwave control box is adjusted and placed in a temperature range of 170-200 ℃, the required temperature is set, and the temperature set in the embodiment 3 is 170 ℃.
(5) Microwave sintering: and (5) placing the die in a microwave control box for sintering, and timing for 3 minutes.
(6) Cooling and taking out: and after the timing is finished, the microwave sintering forming process is finished, the temperature control box is closed, the mold is taken out, and when the temperature is reduced to the room temperature, the product is taken out and trimmed.
(7) And (3) placing the obtained sample in deionized water, carrying out ultrasonic treatment for 5 hours, then placing the sample in an oven, drying the sample for 3 hours at the temperature of 70 ℃, and removing a sulfolane phase to obtain the polymer-based porous material.
(8) And carrying out porosity test, micro-morphology test and mechanical property test on the obtained sample.
Example 4
The microwave sintering forming method for the polymer-based porous material comprises the following steps:
(1) cleaning the die: and cleaning the mold cavity.
(2) Feeding: weighing by using an electronic scale according to the ratio of 2: 8, adding polymer powder into sulfolane, and uniformly mixing the two components to form a fluid state with certain viscosity to obtain a mixture.
(3) Die filling: the mixture is filled into a mold and laid flat so that it completely covers the mold cavity.
(4) Controlling the temperature: the microwave control box was adjusted to a temperature range of 170 ℃ and 200 ℃ and the required temperature was set, example 4 was set at 180 ℃.
(5) Microwave sintering: and (5) placing the die in a microwave control box for sintering, and timing for 3 minutes.
(6) Cooling and taking out: and after the timing is finished, the microwave sintering forming process is finished, the temperature control box is closed, the mold is taken out, and when the temperature is reduced to the room temperature, the product is taken out and trimmed.
(7) And (3) placing the obtained sample in deionized water, carrying out ultrasonic treatment for 5 hours, then placing the sample in an oven, drying the sample for 3 hours at the temperature of 70 ℃, and removing a sulfolane phase to obtain the polymer-based porous material.
(8) And carrying out porosity test, micro-morphology test and mechanical property test on the obtained sample.
Comparative example 1 (comparative examples 1-2, in which ultra-high molecular weight polyethylene powder was used for the micro-powder sintering test, the brand was XM220, except that the amount of the ultra-high molecular weight polyethylene powder added was different)
(1) Cleaning the die: and cleaning the cavity of the mold, and spraying a layer of release agent.
(2) Feeding: 3g of UHMWPE (ultra-high molecular weight polyethylene, XM220) micropowder is weighed by an electronic scale, then the powder is filled into a die cavity, and after filling is finished, the die is oscillated, so that the uniformity of material filling is ensured as much as possible.
(3) Fixing the mold: and closing the female die and the male die, and connecting and fixing by using bolts.
(4) And adjusting the temperature control box to set the required sintering temperature within the temperature range of 170-200 ℃, setting the temperature set in the comparative example 1 to be 200 ℃, heating and sintering the filled forming mold after the preset sintering temperature is reached, and sintering for 10 minutes when the indication of the temperature control box reaches the specified sintering temperature and is stable.
(5) Cooling and taking out: and after the timing is finished, the sintering process is finished, the temperature control box and the circuit control system are closed, the die is taken out, the die is placed into water at 25 ℃, the die is rapidly cooled, when the temperature is reduced to the room temperature, the cooling is stopped, and the sintered product is taken out and trimmed.
(6) And drying the obtained sample at the temperature of 70 ℃ for 3 hours, and carrying out porosity test, micro-morphology test and mechanical property test.
Comparative example 2 (comparative examples 1-2 using ultra high molecular weight polyethylene powder for micro powder sintering test, brand XM220, difference is that the feeding amount of ultra high molecular weight polyethylene powder is different)
(1) Cleaning the die: and cleaning the cavity of the mold, and spraying a layer of release agent.
(2) Feeding: 4g of UHMWPE (ultra-high molecular weight polyethylene, XM220) micropowder is weighed by an electronic scale, then the powder is filled into a die cavity, and after filling is finished, the die is oscillated, so that the uniformity of material filling is ensured as much as possible.
(3) Fixing the mold: and closing the female die and the male die, and connecting and fixing by using bolts.
(4) And adjusting the temperature control box to set the required sintering temperature within the temperature range of 170-200 ℃, setting the temperature set in the comparative example 2 to be 200 ℃, heating and sintering the filled forming mold after the preset sintering temperature is reached, and sintering for 10 minutes when the indication of the temperature control box reaches the specified sintering temperature and is stable.
(5) Cooling and taking out: and after the timing is finished, the sintering process is finished, the temperature control box and the circuit control system are closed, the die is taken out, the die is placed into water at 25 ℃, the die is rapidly cooled, when the temperature is reduced to the room temperature, the cooling is stopped, and the sintered product is taken out and trimmed.
(6) And drying the obtained sample at the temperature of 70 ℃ for 3 hours, and carrying out porosity test, micro-morphology test and mechanical property test.
TABLE 1 porosity, mechanical Properties of examples and comparative examples
As can be seen from Table 1, the comparative examples 1-2 are conventional sintering processes, which have long sintering time and low porosity, and mainly because the conventional sintering processes are heated by heat conduction through the upper and lower templates, the interior of the product is heated very unevenly, the product is excessively melted at the position close to the press plate, and the core layer does not start to melt.
Embodiments 1 to 4 utilize microwave to selectively heat liquid, through to the continuous phase that liquid formed in polymer miropowder, form the effect of whole heating, realize the zero gradient of large area is heated evenly in the material, make the material heated evenly, reduce the thermal stress in the products, the porousness of the product got is good, the porous structure is even, the porosity has improved 200% -400%, mechanical properties has certain reduction, but still keep higher compression and bending strength, do not influence the actual performance of the products, can be according to the actual use requirement of the porous material. It can be intuitively found from the SEM images of fig. 1a and 1b that, when the amount of glycerol is increased, the porous structure shows more pores, i.e., the porosity of the sample is increased, and thus, the ratio of the polymer micro powder to the liquid is changed to control the porosity of the porous product. FIG. 1c is a microstructure of the porous structure of example 1 at a higher magnification, and it can be seen that the porous structure arrangement of the obtained sample is more uniform, which ensures the uniformity and stability of the product performance during use.
The above examples are only preferred embodiments of the present invention, which are intended to be illustrative and not limiting, and those skilled in the art should understand that they can make various changes, substitutions and alterations without departing from the spirit and scope of the invention.
Claims (10)
1. A microwave sintering forming method of a polymer-based porous material is characterized by comprising the following steps:
(1) adding polymer powder into a liquid capable of being heated by microwave, and uniformly mixing to obtain a mixed solution;
(2) putting the mixed solution obtained in the step (1) into a mold, then carrying out microwave heating sintering treatment, cooling to room temperature, opening the mold, and taking out a product to obtain a sintered sample;
(3) and (3) soaking the sintered sample in the step (2) in water, performing ultrasonic treatment, and drying to obtain the polymer-based porous material.
2. The microwave sintering molding method of polymer-based porous material as claimed in claim 1, wherein the microscopic morphology of the polymer powder in step (1) is spherical or ellipsoidal, and the average particle size is 25-150 μm.
3. The microwave sintering molding method of polymer-based porous material according to claim 1, wherein the polymer in step (1) is one or more of high density polyethylene, polypropylene, ultra-high molecular weight polyethylene, polytetrafluoroethylene and polysulfone plastic.
4. The microwave sintering molding method of polymer-based porous material according to claim 1, wherein the microwave-heatable liquid in step (1) is one or more of glycerol, ethylene glycol and sulfolane.
5. The microwave sintering molding method of polymer-based porous material according to claim 1, wherein the mass ratio of the polymer powder to the microwave heatable liquid in the step (1) is 6: 4-2: 8.
6. the microwave sintering and forming method of polymer-based porous material as claimed in claim 1, wherein the temperature of the microwave heating and sintering process in step (2) is 170-200 ℃.
7. The microwave sintering molding method of polymer-based porous material according to claim 1, wherein the time of the microwave heating sintering treatment in the step (2) is 2-10 minutes.
8. The microwave sintering molding method of polymer-based porous material according to claim 1, wherein the time of the ultrasonic treatment in the step (3) is 3-5 hours.
9. The microwave sintering molding method of polymer-based porous material according to claim 1, wherein the drying temperature in step (3) is 70-80 ℃ and the drying time is 3-5 hours.
10. A polymer-based porous material produced by the microwave sinter molding method as claimed in any one of claims 1 to 9.
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| JPS62124931A (en) * | 1985-11-07 | 1987-06-06 | ポ−ラス・プラスチツクス・リミテツド | Manufacture of at least partially sintered sintered product and mold therefor |
| CN1532043A (en) * | 2003-03-15 | 2004-09-29 | 1 | Method for producing three dimension object using microwave radiation |
| CN101029146A (en) * | 2006-02-27 | 2007-09-05 | 日东电工株式会社 | Method for preparing porous sheet and porous sheet obtained by the method |
| CN104057619A (en) * | 2013-03-21 | 2014-09-24 | 黑龙江彩格工业设计有限公司 | Apparatus and method for sintering high-molecular porous material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS62124931A (en) * | 1985-11-07 | 1987-06-06 | ポ−ラス・プラスチツクス・リミテツド | Manufacture of at least partially sintered sintered product and mold therefor |
| CN1532043A (en) * | 2003-03-15 | 2004-09-29 | 1 | Method for producing three dimension object using microwave radiation |
| CN101029146A (en) * | 2006-02-27 | 2007-09-05 | 日东电工株式会社 | Method for preparing porous sheet and porous sheet obtained by the method |
| CN103421207A (en) * | 2006-02-27 | 2013-12-04 | 日东电工株式会社 | Method of producing porous sheet and porous sheet obtained by the production method |
| CN104057619A (en) * | 2013-03-21 | 2014-09-24 | 黑龙江彩格工业设计有限公司 | Apparatus and method for sintering high-molecular porous material |
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