CN114316550A - Resin and preparation method thereof - Google Patents
Resin and preparation method thereof Download PDFInfo
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- CN114316550A CN114316550A CN202210112004.3A CN202210112004A CN114316550A CN 114316550 A CN114316550 A CN 114316550A CN 202210112004 A CN202210112004 A CN 202210112004A CN 114316550 A CN114316550 A CN 114316550A
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- 229920005989 resin Polymers 0.000 title claims abstract description 102
- 239000011347 resin Substances 0.000 title claims abstract description 102
- 238000002360 preparation method Methods 0.000 title abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 59
- 238000000465 moulding Methods 0.000 claims abstract description 28
- 239000000203 mixture Substances 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 25
- 238000005086 pumping Methods 0.000 claims abstract description 20
- 238000003756 stirring Methods 0.000 claims abstract description 20
- 239000000945 filler Substances 0.000 claims abstract description 19
- 229920001187 thermosetting polymer Polymers 0.000 claims abstract description 15
- 238000011049 filling Methods 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 12
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 10
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- 239000004917 carbon fiber Substances 0.000 claims description 10
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 10
- 239000003365 glass fiber Substances 0.000 claims description 9
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 5
- 239000006229 carbon black Substances 0.000 claims description 5
- 239000004927 clay Substances 0.000 claims description 5
- 239000000835 fiber Substances 0.000 claims description 5
- 239000000377 silicon dioxide Substances 0.000 claims description 5
- 229920006337 unsaturated polyester resin Polymers 0.000 claims description 5
- 239000005995 Aluminium silicate Substances 0.000 claims description 4
- 229910052582 BN Inorganic materials 0.000 claims description 4
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 4
- 229920001807 Urea-formaldehyde Polymers 0.000 claims description 4
- 235000012211 aluminium silicate Nutrition 0.000 claims description 4
- 239000010425 asbestos Substances 0.000 claims description 4
- GBAOBIBJACZTNA-UHFFFAOYSA-L calcium sulfite Chemical compound [Ca+2].[O-]S([O-])=O GBAOBIBJACZTNA-UHFFFAOYSA-L 0.000 claims description 4
- 235000010261 calcium sulphite Nutrition 0.000 claims description 4
- 239000002041 carbon nanotube Substances 0.000 claims description 4
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 4
- 239000003822 epoxy resin Substances 0.000 claims description 4
- 229910021389 graphene Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- 239000010445 mica Substances 0.000 claims description 4
- 229910052618 mica group Inorganic materials 0.000 claims description 4
- 239000003094 microcapsule Substances 0.000 claims description 4
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims description 4
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims description 4
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 4
- 239000005011 phenolic resin Substances 0.000 claims description 4
- 229920000647 polyepoxide Polymers 0.000 claims description 4
- -1 polytetrafluoroethylene Polymers 0.000 claims description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 4
- 229910052895 riebeckite Inorganic materials 0.000 claims description 4
- 235000012239 silicon dioxide Nutrition 0.000 claims description 4
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 4
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 3
- 229920000877 Melamine resin Polymers 0.000 claims description 3
- 239000004642 Polyimide Substances 0.000 claims description 3
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 3
- 229920001568 phenolic resin Polymers 0.000 claims description 3
- 229920001721 polyimide Polymers 0.000 claims description 3
- 239000004814 polyurethane Substances 0.000 claims description 3
- 229920002635 polyurethane Polymers 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims 1
- 230000007547 defect Effects 0.000 abstract description 24
- 239000000463 material Substances 0.000 description 26
- 238000009489 vacuum treatment Methods 0.000 description 10
- 239000003795 chemical substances by application Substances 0.000 description 7
- 238000001132 ultrasonic dispersion Methods 0.000 description 6
- 238000006073 displacement reaction Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 239000003999 initiator Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000002131 composite material Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 229920002430 Fibre-reinforced plastic Polymers 0.000 description 1
- GZCGUPFRVQAUEE-SLPGGIOYSA-N aldehydo-D-glucose Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O GZCGUPFRVQAUEE-SLPGGIOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000805 composite resin Substances 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000011151 fibre-reinforced plastic Substances 0.000 description 1
- 238000009787 hand lay-up Methods 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000009740 moulding (composite fabrication) Methods 0.000 description 1
- 229920005749 polyurethane resin Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 235000012222 talc Nutrition 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
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Abstract
The invention provides a resin and a preparation method thereof. The method for preparing the resin comprises the following steps: mixing thermosetting resin and modified filler and fully stirring to obtain a mixed raw material; carrying out first vacuum-pumping treatment on the mixed raw materials to obtain a pretreated raw material mixture; pouring the pretreated raw material mixture into a forming space, and filling the forming space; and performing alternate treatment of centrifugal treatment and second vacuumizing treatment on the molding space filled with the pretreatment raw material mixture, and curing to obtain the resin. Therefore, the resin prepared by the method is dense, has no defects such as cavities and the like, and improves the mechanical property of the resin. In particular, the mechanical properties such as strength, toughness and the like of the resin which works in a narrow working space can be ensured.
Description
Technical Field
The invention relates to the technical field of materials, in particular to resin and a preparation method thereof.
Background
Thermosetting resin (thermosetting resin) refers to a resin which undergoes chemical change after being heated, gradually hardens and forms, is not softened after being heated, and cannot be dissolved. The thermosetting resin has a molecular structure of a body type, has the advantages of high heat resistance, difficult deformation under pressure and poor mechanical properties. The thermosetting resin-based composite material is also called fiber reinforced plastic, is a multiphase material consisting of thermoplastic resin matrix, fiber reinforced material and other fillers, has superior performance compared with a single material, effectively overcomes the defects of poor mechanical performance and the like of the single resin matrix, and is a composite material which is mature in the prior art and most widely applied. The thermosetting composite material forming method includes hand lay-up forming, compression molding, lamination forming, winding forming, extrusion forming and the like, and is widely used for various resin products. However, when the molding space of the resin is small, for example, the molding space is a gap smaller than 1mm, the traditional molding method is difficult to be developed, and the resin is poured into the space only by the fluidity of the material, so that a plurality of product defects such as air pockets, holes, cracks and the like are generated, and the mechanical property of the material is seriously influenced.
Disclosure of Invention
The present invention is directed to solving, at least to some extent, one of the technical problems in the related art. Therefore, an object of the present invention is to provide a method for preparing a resin, which can solve the problem of poor mechanical properties of a resin material after molding in a narrow space.
In one aspect of the invention, a method of making a resin is provided. According to an embodiment of the present invention, a method of preparing a resin includes: mixing thermosetting resin and modified filler and fully stirring to obtain a mixed raw material; carrying out first vacuum-pumping treatment on the mixed raw materials to obtain a pretreated raw material mixture; pouring the pretreated raw material mixture into a forming space, and filling the forming space; and performing alternate treatment of centrifugal treatment and second vacuumizing treatment on the molding space filled with the pretreatment raw material mixture, and curing to obtain the resin. Therefore, the resin prepared by the method is dense, has no defects such as cavities and the like, and improves the mechanical property of the resin. In particular, the mechanical properties such as strength, toughness and the like of the resin which works in a narrow working space can be ensured.
According to an embodiment of the present invention, at least one of the following conditions is satisfied: the thermosetting resin is at least one selected from epoxy resin, phenolic resin, unsaturated polyester resin, melamine-formaldehyde resin, urea resin, polyurethane and polyimide; the modified filler is selected from at least one of microcapsule, calcium carbonate, clay, kaolin, talcum powder, asbestos, mica, carbon black, calcium sulfate, calcium sulfite, metal powder, carbon fiber, glass fiber, silicon dioxide, graphene, carbon nano tube, polytetrafluoroethylene powder/fiber, graphite, molybdenum disulfide, boron nitride and zirconium oxide.
According to an embodiment of the invention, the width of the molding space is 0.1mm to 10 mm.
According to the embodiment of the invention, based on the mixed raw materials, the mass percentage of the modified filler is 0.1-99%, preferably 10-90%.
According to the embodiment of the invention, the stirring speed is 10-500 r/min, preferably 200-300 r/min.
According to the embodiment of the invention, the vacuum degree after the first vacuum pumping treatment is-0.09 to-0.1 MPa.
According to the embodiment of the invention, the rotation speed of the centrifugal treatment is 50-3000 r/min, and preferably 200-2000 r/min.
According to the embodiment of the invention, after the alternating treatment, the vacuum degree of the forming space is-0.09 to-0.1 MPa.
According to the embodiment of the invention, the temperature of the curing treatment is 40-200 ℃, and preferably 60-140 ℃.
In another aspect of the invention, the invention provides a resin. According to an embodiment of the invention, the resin is prepared by the method described above. Therefore, the resin structure is compact, and the defects such as cavities and the like do not exist, so that the mechanical property of the resin can be greatly improved.
Drawings
The above and/or additional aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
FIG. 1 is a flow chart of a method of making a resin in one embodiment of the present invention.
FIG. 2 is a photograph of a surface of a defect-free resin prepared in example 1;
FIG. 3 is a pressure-displacement graph of a defect-free resin prepared in example 1;
FIG. 4 is a photograph of the surface of the resin prepared in comparative example 1;
FIG. 5 is a pressure-displacement graph of the resin prepared in comparative example 1.
Detailed Description
The scheme of the invention will be explained with reference to the examples. It will be appreciated by those skilled in the art that the following examples are illustrative of the invention only and should not be taken as limiting the scope of the invention. The examples, where specific techniques or conditions are not indicated, are to be construed according to the techniques or conditions described in the literature in the art or according to the product specifications. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
The invention will now be described with reference to specific examples, which are intended to be illustrative only and not to be limiting in any way.
In one aspect of the invention, a method of making a resin is provided. According to an embodiment of the present invention, referring to fig. 1, a method of preparing a resin includes:
s100: and mixing the thermosetting resin and the modified filler, and fully stirring to obtain a mixed raw material.
According to an embodiment of the present invention, the thermosetting resin is selected from at least one of epoxy resin, phenol resin, unsaturated polyester resin, melamine-formaldehyde resin, urea resin, polyurethane, and polyimide. The thermosetting resin can be used for preparing dense resin materials without cavity defects by adopting the method, so that the method can be applied to most of thermosetting resins and has a wider application range.
According to an embodiment of the present invention, the modified filler is selected from at least one of microcapsules, calcium carbonate, clay, kaolin, talc, asbestos, mica, carbon black, calcium sulfate, calcium sulfite, metal powder, carbon fiber, glass fiber, silica, graphene, carbon nanotube, polytetrafluoroethylene powder/fiber, graphite, molybdenum disulfide, boron nitride, and zirconium oxide. The filler may contribute to the strength, toughness and wear resistance of the resin. Specifically, if the modified filler is selected from at least one of microcapsules, talcum powder, asbestos, mica, carbon black, calcium sulfate, calcium sulfite, metal powder, molybdenum disulfide, boron nitride, zirconium oxide and polytetrafluoroethylene powder/fiber, the wear resistance of the resin can be well improved, and if the modified filler is selected from at least one of calcium carbonate, clay, kaolin, carbon fiber, glass fiber, silicon dioxide, graphene and carbon nano tube, the strength and toughness of the resin can be well improved, so that the performance and reliability of the resin are improved.
According to the embodiment of the invention, the mass ratio of the modified filler is 0.1-99% (for example, the mass ratio of the modified filler is 0.1%, 1%, 5%, 10%, 15%, 20%, 30%, 40%, 50%, 60%, 70%, 80%, 90% or 99%) by mass percentage based on the mixed raw materials. Therefore, the technical personnel in the field can flexibly set the mass ratio of the modified filler according to the requirements on the strength and the toughness of the resin, the specific material of the modified filler and other practical conditions, and only the good service performance of the resin is ensured. In some embodiments, the modified filler is 10-90% by mass.
According to the embodiment of the invention, the stirring speed is 10-500 r/min (10r/min, 50r/min, 100r/min, 150r/min, 200r/min, 250r/min, 300r/min, 350r/min, 400r/min, 450r/min, 500 r/min). Therefore, under the condition of the stirring speed, the thermosetting resin and the modified filler can be quickly and uniformly mixed. In some embodiments, the stirring rate is 200 to 300 r/min. Wherein, the mixed raw materials can be subjected to ultrasonic dispersion for a certain time after being fully stirred, so that the gas and the water can be removed in the subsequent first vacuumizing treatment.
In some embodiments, the mixing material may further include at least one of an initiator and a curing agent. Thus, the performance of the prepared resin is improved.
S200: and carrying out first vacuum-pumping treatment on the mixed raw materials to obtain a pretreated raw material mixture. Therefore, through the first vacuum-pumping treatment, gas and water molecules in the mixed raw material can be removed, so that the preparation of the resin material without cavities is facilitated, and the pouring amount can be improved to the maximum extent in the limited forming space when the resin material is poured into the forming space subsequently.
According to the embodiment of the present invention, the degree of vacuum after the first vacuum process is-0.09 to-0.1 MPa (for example, -0.09MPa, -0.05MPa, -0.03MPa, -0.01MPa, 0MPa, 0.02MPa, 0.04MPa, 0.05MPa, 0.07MPa, 0.09MPa, 0.1 MPa). Thereby, the gas and water molecules in the mixed raw material can be removed to the maximum extent.
The time of the first vacuum-pumping treatment is not particularly required, as long as the vacuum degree after the first vacuum-pumping treatment is-0.09 to-0.1 Mpa, which is not limited herein.
S300: pouring the pretreated raw material mixture into the forming space and filling the forming space.
According to the embodiment of the present invention, the width of the molding space is 0.1mm to 10mm (for example, the width of the molding space is 0.1mm, 0.5mm, 1.0mm, 2mm, 3mm, 4mm, 5mm, 6mm, 7mm, 8mm, 9mm, 10 mm). Therefore, the forming space is narrow, the resin which works in a narrow working space (a gap with the width less than 1 mm) can be prepared, the prepared resin has no defect problems such as cavities, and the like, and the mechanical properties such as the strength of the resin can be greatly improved.
S400: and performing alternate treatment of centrifugal treatment and second vacuumizing treatment on the molding space filled with the pretreatment raw material mixture, and curing to obtain the resin. Therefore, the defects such as cavities in the resin are continuously reduced in the alternate treatment until the defects such as cavities disappear, the prepared resin is dense and has no defects such as cavities, and the mechanical property of the resin is improved.
The times of the centrifugal treatment and the second vacuum-pumping treatment are not particularly required, as long as the required vacuum degree can be achieved. In addition, the sequence of the centrifugal treatment and the second vacuumizing treatment in the alternate treatment of the centrifugal treatment and the second vacuumizing treatment has no special requirement, and a person skilled in the art can flexibly set the sequence according to actual requirements.
According to the embodiment of the invention, the rotation speed of the centrifugal treatment is 50-3000 r/min, for example, the rotation speed of the centrifugal treatment is 50r/min, 100r/min, 300r/min, 500r/min, 800r/min, 1000r/min, 1300r/min, 1500r/min, 1800r/min, 2000r/min, 2300r/min, 2500r/min, 2800r/min and 3000 r/min. In some embodiments, the rotation speed of the centrifugal treatment is 200-2000 r/min. According to the embodiment of the invention, after the alternating treatment, the vacuum degree of the forming space is-0.09 to-0.1 Mpa, such as-0.09 Mpa, -0.05Mpa, -0.03Mpa, -0.01Mpa, 0Mpa, 0.02Mpa, 0.04Mpa, 0.05Mpa, 0.07Mpa, 0.09Mpa and 0.1 Mpa. Thus, by performing the centrifugal treatment and the second vacuum-pumping treatment under the above-mentioned addition, the gas in the resin can be removed more favorably until a resin free from void defects is obtained.
According to the embodiment of the present invention, the curing temperature is 40-200 ℃, such as 40 ℃, 60 ℃, 80 ℃, 100 ℃, 120 ℃, 140 ℃, 160 ℃, 180 ℃, 200 ℃. In some embodiments, the curing temperature may be 60 to 140 ℃. Thereby, the cured resin can be obtained quickly and efficiently in the above temperature range.
In another aspect of the invention, the invention provides a resin. According to an embodiment of the invention, the resin is prepared by the method described above. From this, the resin structure is closely knit, and does not have defects such as cavity in, can promote the mechanical properties of resin greatly, can be fine moreover be applied to in narrow and small working space. It will be understood by those skilled in the art that the resin has all the features and advantages of the method for preparing the resin described above, and will not be described in excessive detail herein.
Examples
Example 1
Adding 100g of unsaturated polyester resin, 10g of carbon fiber, 10g of glass fiber and 5g of silicon dioxide into a 250ml beaker, fully stirring, performing ultrasonic dispersion for 10min, adding 0.3g of initiator and 2g of curing agent, and uniformly stirring to obtain a mixed raw material;
putting the mixed raw materials into a vacuum environment, and removing air and moisture dissolved in the mixed raw materials through first vacuum treatment to obtain a pretreated raw material mixture, wherein the vacuum degree after the first vacuum treatment is-0.99 MPa;
pouring the pretreated raw material mixture into the molding space and filling the molding space;
and carrying out second vacuum-pumping treatment on the molding space filled with the pretreated raw material mixture for 10min, then carrying out centrifugal treatment on the resin, wherein the centrifugal rate is 1500r/min, continuously reducing the defects such as cavities in the resin until the defects disappear by adopting a centrifugal and vacuum-pumping alternative treatment mode, and then placing the resin material at the temperature of 80 ℃ for curing treatment to obtain the compacted defect-free resin material. The surface of the prepared resin can be seen in fig. 2, the pressure-displacement curve can be seen in fig. 3, and as can be seen from fig. 2, the surface of the resin is smooth, and defects such as air pockets and holes are basically eliminated; as can be seen from FIG. 3, the resin has good pressure-bearing capacity, and the pressure-bearing capacity can reach about 18 kN.
Example 2
Adding 100g of epoxy resin, 11g of carbon fiber, 11g of glass fiber and 5g of graphite into a 250ml beaker, fully stirring, performing ultrasonic dispersion for 10min, adding 50g of curing agent, and uniformly stirring to obtain a mixed raw material;
putting the mixed raw materials into a vacuum environment, and removing air and moisture dissolved in the mixed raw materials through first vacuum treatment to obtain a pretreated raw material mixture, wherein the vacuum degree after the first vacuum treatment is-0.99 MPa;
pouring the pretreated raw material mixture into the molding space and filling the molding space;
and carrying out second vacuum-pumping treatment on the molding space filled with the pretreated raw material mixture for 10min, then carrying out centrifugal treatment on the resin, wherein the centrifugal rate is 1600r/min, continuously reducing the defects such as cavities in the resin until the defects disappear by adopting a centrifugal and vacuum-pumping alternative treatment mode, and then placing the resin material at the temperature of 120 ℃ for curing treatment to obtain the compacted defect-free resin material.
Example 3
Adding 100g of phenolic resin, 8g of carbon fiber, 12g of glass fiber and 5g of calcium carbonate into a 250ml beaker, fully stirring, performing ultrasonic dispersion for 10min, adding 6g of curing agent, and uniformly stirring to obtain a mixed raw material;
putting the mixed raw materials into a vacuum environment, and removing air and moisture dissolved in the mixed raw materials through first vacuum treatment to obtain a pretreated raw material mixture, wherein the vacuum degree after the first vacuum treatment is-0.99 MPa;
pouring the pretreated raw material mixture into the molding space and filling the molding space;
and carrying out second vacuum-pumping treatment for 10min on the molding space filled with the pretreated raw material mixture, then carrying out centrifugal treatment on the resin at a centrifugal rate of 1000r/min, continuously reducing defects such as cavities in the resin until the defects disappear by adopting a centrifugal and vacuum-pumping alternative treatment mode, and then placing the resin material at the temperature of 150 ℃ for curing treatment to obtain the compacted defect-free resin material.
Example 4
Adding 100g of urea-formaldehyde resin, 13g of carbon fiber, 10g of glass fiber and 5g of clay into a 250ml beaker, fully stirring, performing ultrasonic dispersion for 10min, adding 1g of curing agent, and uniformly stirring to obtain a mixed raw material;
putting the mixed raw materials into a vacuum environment, and removing air and moisture dissolved in the mixed raw materials through first vacuum treatment to obtain a pretreated raw material mixture, wherein the vacuum degree after the first vacuum treatment is-0.99 MPa;
pouring the pretreated raw material mixture into the molding space and filling the molding space;
and carrying out second vacuum-pumping treatment on the molding space filled with the pretreated raw material mixture for 12min, then carrying out centrifugal treatment on the resin at a centrifugal rate of 1800r/min, continuously reducing defects such as cavities in the resin until the defects disappear by adopting a centrifugal and vacuum-pumping alternative treatment mode, and then placing the resin material at a temperature of 50 ℃ for curing treatment to obtain the compacted defect-free resin material.
Example 5
Adding 100g of polyurethane resin, 10g of carbon fiber, 9g of glass fiber and 5g of carbon black into a 250ml beaker, fully stirring, performing ultrasonic dispersion for 10min, adding 1g of curing agent, and uniformly stirring to obtain a mixed raw material;
putting the mixed raw materials into a vacuum environment, and removing air and moisture dissolved in the mixed raw materials through first vacuum treatment to obtain a pretreated raw material mixture, wherein the vacuum degree after the first vacuum treatment is-0.99 MPa;
pouring the pretreated raw material mixture into the molding space and filling the molding space;
and carrying out second vacuum-pumping treatment on the molding space filled with the pretreated raw material mixture for 10min, then carrying out centrifugal treatment on the resin, wherein the centrifugal rate is 1600r/min, continuously reducing the defects such as cavities in the resin until the defects disappear by adopting a centrifugal and vacuum-pumping alternative treatment mode, and then placing the resin material at the temperature of 50 ℃ for curing treatment to obtain the compacted defect-free resin material.
Comparative example 1
Adding 100g of unsaturated polyester resin, 10g of carbon fiber, 0.3g of initiator and 2g of curing agent into a 250ml beaker, uniformly stirring to obtain a mixed raw material, pouring the mixed raw material into a molding space, filling the molding space, and then placing the mixed raw material at the temperature of 80 ℃ for curing treatment to obtain the pouring molded resin material. The surface of the prepared resin can be seen in fig. 4, the pressure-displacement curve can be seen in fig. 5, and as can be seen in fig. 4, the surface of the resin is filled with a large number of product defects such as air pockets, holes and the like; as can be seen from FIG. 5, the pressure-bearing capacity of the resin is poor and is only about 10 kN.
The terms "first" and "second" are used herein for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present application, "a plurality" means two or more unless specifically limited otherwise.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (10)
1. A method of making a resin, comprising:
mixing thermosetting resin and modified filler and fully stirring to obtain a mixed raw material;
carrying out first vacuum-pumping treatment on the mixed raw materials to obtain a pretreated raw material mixture;
pouring the pretreated raw material mixture into a forming space, and filling the forming space;
and performing alternate treatment of centrifugal treatment and second vacuumizing treatment on the molding space filled with the pretreatment raw material mixture, and curing to obtain the resin.
2. The method of claim 1, wherein at least one of the following conditions is satisfied:
the thermosetting resin is at least one selected from epoxy resin, phenolic resin, unsaturated polyester resin, melamine-formaldehyde resin, urea resin, polyurethane and polyimide;
the modified filler is selected from at least one of microcapsule, calcium carbonate, clay, kaolin, talcum powder, asbestos, mica, carbon black, calcium sulfate, calcium sulfite, metal powder, carbon fiber, glass fiber, silicon dioxide, graphene, carbon nano tube, polytetrafluoroethylene powder/fiber, graphite, molybdenum disulfide, boron nitride and zirconium oxide.
3. The method of claim 1, wherein the forming space has a width of 0.1mm to 10 mm.
4. The method according to claim 1, wherein the mass percentage of the modified filler is 0.1-99%, preferably 10-90%, based on the mixed raw materials.
5. The method according to claim 1, wherein the stirring is performed at a rate of 10 to 500r/min, preferably 200 to 300 r/min.
6. The method according to claim 1, wherein the degree of vacuum after the first vacuuming is-0.09 to-0.1 Mpa.
7. A method according to any one of claims 1 to 6, wherein the rotational speed of the centrifugation is 50 to 3000r/min, preferably 200 to 2000 r/min.
8. The method according to any one of claims 1 to 6, wherein the vacuum degree of the forming space after the alternating treatment is-0.09 to-0.1 MPa.
9. A method according to any one of claims 1 to 6, wherein the temperature of the curing treatment is 40 to 200 ℃, preferably 60 to 140 ℃.
10. A resin produced by the method according to any one of claims 1 to 9.
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