CN105732976A - Phase-change-particle modified polyamide wear-resistant material and preparing method thereof - Google Patents
Phase-change-particle modified polyamide wear-resistant material and preparing method thereof Download PDFInfo
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/08—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino-carboxylic acids
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- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
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Abstract
The invention discloses a phase-change-particle modified polyamide wear-resistant material and a preparing method thereof. The phase-change-particle modified polyamide wear-resistant material is formed in the mode that reaction materials, a catalyst and an assist catalyst are catalyzed and polymerized, wherein the adding proportion of the reaction materials to the catalyst to the assist catalyst is 100 g:(0.2-0.35) g:(1.5-3.5) ml, the reaction materials comprise, by mass, 5%-10% of phase-change particle materials and 90%-95% of caprolactam, and phase-change-particle materials are porous graphene/hard paraffin phase-change materials. According to the phase-change-particle modified polyamide wear-resistant material and the preparing method thereof, the high-thermal conductivity and the high heat enthalpy of phase-change particles are used for dissipating friction heat, the tribology performance of the polyamide material is improved accordingly, particularly, the anti-wear performance of the polyamide material is greatly improved, the abrasion resistance under the low-speed and heavy-load condition is 1.3-2.7 times that of the prior art, and the abrasion resistance under the high-speed and light-load condition is 2.6-5.8 times that of the prior art; therefore prepared pieces with the wider application range are prepared with the polyamide composite material.
Description
Technical field
The present invention relates to composite abrasion resistance material technical field, a kind of phase change grains/polyamide abrasion-proof material and preparation method thereof.
Background technology
Polymer self-lubricating material is widely applied due to its light weight, the premium properties such as non-maintaining, and in order to improve the properties of antifriction and wear resistance of polymeric material further, Chinese scholars has carried out substantial amounts of research.But, owing to polymeric material is the most sensitive to temperature, therefore during fricting movement, produced frictional heat can cause operating temperature to raise, polymer can be made to occur from glassy state to elastomeric state again to the transformation of viscous state (molten state of line polymer), its modulus and hardness can significantly decline, thus reduce its maximum allowable PV value, limit its range of application.
In order to make polymeric material be applicable to more stringent fricting movement working condition, people the most i.e. start with from the heat conductivity increasing material, obtain the material that tribological property is excellent, as Chinese invention patent 102942694A discloses a kind of polyamide (nylon) material mixing the good Graphene of heat conductivity.While it is true, these materials succeeded in developing still cannot meet the requirement of some new and traditional special engineered technical fields.The PV value limit of Gonna breakthrough polymer self-lubricating material must propose brand-new research and mentality of designing according to the thermally sensitive feature of polymeric material in existing tribological material design basis, in this context, seek a kind of phase-change material comprising high-termal conductivity and high latent heat of phase change, there is the polymeric material of good wear performance, have very important significance to expanding its range.
Summary of the invention
The present invention is to solve above-mentioned technical problem, it is provided that a kind of phase change grains modified polyamide high-abrasive material and preparation method thereof, it possesses low-friction coefficient and low abrasion, can use under high PV friction condition.
The technical solution adopted in the present invention is: a kind of phase change grains modified polyamide high-abrasive material, reaction mass formed by catalyst and promoter catalytic polymerization, and wherein, reaction mass is 100g/ with catalyst, the adding proportion of promoter
(0.2-0.35) g/ (1.5-3.5) ml, reaction mass is made up of the phase change grains material of 5 ~ 10% and the caprolactam of 95 ~ 90% by mass percentage, and described phase change grains material is porous graphene/hard paraffin phase-change material.
Described catalyst is sodium hydroxide, and promoter is Toluene-2,4-diisocyanate, 4-diisocyanate.
A kind of method preparing phase change grains modified polyamide high-abrasive material:
Step one, the preparation of phase change grains material
A, weigh crystalline flake graphite, under conditions of being stirred continuously, the crystalline flake graphite weighed is joined in the mixing concentrated acid of concentrated sulphuric acid and concentrated nitric acid composition and react, control temperature and be 30-50 DEG C, mixing time is 60 min, then neutrality it is washed to, washing product is dried 12h under conditions of 105 DEG C, obtains graphite intercalation compound, standby；
B, the graphite intercalation compound of preparation in step a is placed in Muffle furnace under conditions of temperature is 850 DEG C calcining 30s, take out size-reduced, cross 200 mesh sieves after obtain porous graphene powder, standby；
C, the porous graphene powder prepared in step b add the hard paraffin accounting for its quality 2.5 times, then by mixture in the water-bath of 80 DEG C, stir speed (S.S.) be 100rpm, ultrasonic power be to mix 30min under the conditions of 180w, obtain porous graphene/hard paraffin phase change grains filler, standby；
Step 2, the preparation of modified polyamide
D, weigh in caprolactam monomer, catalyst, promoter and step c the porous graphene/wax phase change granule of preparation respectively according to the proportioning in claim 1, standby；
E, the caprolactam monomer weighed in step d is placed in flask, it is heated to molten condition the conditions of 80 DEG C, then the porous graphene weighed in step d/wax phase change granule is joined and caprolactam carries out polyreaction process, described polyreaction processes and includes with the next stage: (1) is first mechanical agitation then supersound process 30-90min, wherein stir speed (S.S.) 300-600rpm, ultrasonic power 100-300w under the conditions of 70-90 DEG C；(2) temperature be 130-150 DEG C, vacuum be 0.090-0.099MPa under conditions of reflux 30-50min；(3) adding, in the mixture after step (2) process, the catalyst weighed in step d under intense agitation, reflux under conditions of vacuum is 0.090-0.099MPa 30-50min, prepares mixture；(4) in the mixture that step (3) prepares, add in step d the promoter weighed and carry out catalytic polymerization, prepared reactant mixture is poured in the mould of (160 ± 5) DEG C, cooling and demolding after 1h, prepares product.
The grain graininess of the crystalline flake graphite used in described step one is less than 500 microns.
Crystalline flake graphite described in described step one is 3:10 with the mass ratio mixing concentrated acid, and wherein, in mixing concentrated acid, the concentration of concentrated sulphuric acid and concentrated nitric acid is respectively 98% and 65%, and mass ratio is 9:1.
The melting range of the hard paraffin used in described step one is 48 ~ 50 DEG C.
The speed being stirred vigorously in (3rd) stage of described step e is more than 600rpm.
Beneficial effects of the present invention: the present invention uses polyreaction, belong to the preparation method from molecule to material and can make Nano filling good dispersion, the present invention utilizes the high-termal conductivity of phase change grains and high enthalpy plays dissipation frictional heat so that the tribological property of polyamide material is improved, wherein wear resistance (inverse of wear rate) is greatly improved, and the abrasion resistance under low-speed heave-load is the 1.3-of prior art
2.7 times, the abrasion resistance under high speed light loading is the 2.6-5.8 times of prior art.It is thus possible to prepare the wider array of product of range of application with this polyamide compoiste material；Using hard paraffin in the present invention, there is solid-liquid phase change in hard paraffin during participating in reaction, by absorbing latent heat of phase change, it is possible to effectively dissipate frictional heat.
Detailed description of the invention
A kind of phase change grains modified polyamide high-abrasive material, is formed by catalyst and promoter catalytic polymerization by reaction mass, and wherein, reaction mass is 100g/ with catalyst, the adding proportion of promoter
(0.2-0.35) g/ (1.5-3.5) ml, reaction mass is made up of the phase change grains material of 5 ~ 10% and the caprolactam of 95 ~ 90% by mass percentage, and described phase change grains material is porous graphene/hard paraffin phase-change material.
Described catalyst is sodium hydroxide, and promoter is Toluene-2,4-diisocyanate, 4-diisocyanate.
A kind of method preparing phase change grains modified polyamide high-abrasive material, comprises the following steps:
Step one, the preparation of phase change grains material
A, weigh crystalline flake graphite, under conditions of being stirred continuously, the crystalline flake graphite weighed is joined in the mixing concentrated acid of concentrated sulphuric acid and concentrated nitric acid composition and react, control temperature and be 30-50 DEG C, mixing time is 60 min, then neutrality it is washed to, washing product is dried 12h under conditions of 105 DEG C, obtains graphite intercalation compound, standby；
B, the graphite intercalation compound of preparation in step a is placed in Muffle furnace under conditions of temperature is 850 DEG C calcining 30s, take out size-reduced, cross 200 mesh sieves after obtain porous graphene powder, standby；
C, the porous graphene powder prepared in step b add the hard paraffin accounting for its quality 2.5 times, then by mixture in the water-bath of 80 DEG C, stir speed (S.S.) be 100rpm, ultrasonic power be to mix 30min under the conditions of 180w, obtain porous graphene/hard paraffin phase change grains filler, standby；
Step 2, the preparation of modified polyamide
D, weigh in caprolactam monomer, catalyst, promoter and step c the porous graphene/wax phase change granule of preparation respectively according to the proportioning in claim 1, standby；
E, the caprolactam monomer weighed in step d is placed in flask, it is heated to molten condition the conditions of 80 DEG C, then the porous graphene weighed in step d/wax phase change granule is joined and caprolactam carries out polyreaction process, described polyreaction processes and includes with the next stage: (1) is first mechanical agitation then supersound process 30-90min, wherein stir speed (S.S.) 300-600rpm, ultrasonic power 100-300w under the conditions of 70-90 DEG C；(2) temperature be 130-150 DEG C, vacuum be 0.090-0.099MPa under conditions of reflux 30-50min；(3) adding, in the mixture after step (2) process, the catalyst weighed in step d under intense agitation, reflux under conditions of vacuum is 0.090-0.099MPa 30-50min, prepares mixture；(4) in the mixture that step (3) prepares, add in step d the promoter weighed and carry out catalytic polymerization, prepared reactant mixture is poured in the mould of (160 ± 5) DEG C, cooling and demolding after 1h, prepares product.
The grain graininess of the crystalline flake graphite used in described step one is less than 500 microns.
Crystalline flake graphite described in described step one is 3:10 with the mass ratio mixing concentrated acid, and wherein, in mixing concentrated acid, the concentration of concentrated sulphuric acid and concentrated nitric acid is respectively 98% and 65%, and mass ratio is 9:1.
The melting range of the hard paraffin used in described step one is 48 ~ 50 DEG C.
The speed being stirred vigorously in (3rd) stage of described step e is more than 600rpm.
The present invention is explained further below in conjunction with detailed description of the invention.
Embodiment 1
Using the technical scheme of phase change grains weight content 5%, concrete preparation method is as follows:
Step one, the preparation of phase change grains
By 15g crystalline flake graphite, in being stirred continuously lower addition 45g concentrated sulphuric acid (98%) and 5g concentrated nitric acid (65%) mixed solution, temperature control 50 DEG C, stirring reaction 60 min, product is washed to neutrality, at 105 DEG C of dry 12h, obtains graphite intercalation compound；Process 30s in graphite intercalation compound is placed in 850 DEG C of Muffle furnaces, through pulverizing after taking out cooling, cross 200 mesh sieves, obtain porous graphene powder；In 80 DEG C of water-baths, under the conditions of stir speed (S.S.) 100rpm, ultrasonic power 180w, dispersing cellular Graphene powder and account for its quality 2.5 times hard paraffin mixture 30min after, it is thus achieved that porous graphene/wax phase change granular filler.
The preparation of the filler modified polyamide of step 2, phase change grains
The caprolactam monomer weighing 95.0 g is placed in 250ml flask, 80 DEG C of heating, after completely melted, add phase change grains filler 5.0g and is filled with polyreaction process.Gained fills the reaction treatment process of polyreaction: first mechanical agitation then supersound process 60min under conditions of 80 DEG C, wherein stir speed (S.S.) 500rpm, ultrasonic power 200w, gained mixture refluxes 30min under the vacuum condition of 130 DEG C, vacuum is 0.095MPa, add 0.25 g sodium hydroxide with vigorous stirring, after gained mixture is carried out vacuum back-flow 30min again, vacuum is 0.095MPa, add 3.0ml promoter Toluene-2,4-diisocyanate, 4-diisocyanate, gained reaction treatment mixture pours in the mould being preheated to 165 DEG C, cooling and demolding after 60min, i.e. obtain polyamide/phase change grains composite.
Embodiment 2
Using the technical scheme of phase change grains weight content 7.5%, concrete preparation method is as follows:
Step one, the preparation of phase change grains
By 15g crystalline flake graphite, in being stirred continuously lower addition 45g concentrated sulphuric acid (98%) and 5g concentrated nitric acid (65%) mixed solution,
Temperature control 50 DEG C, stirs reaction 60
Min, product is washed to neutrality, at 105 DEG C of dry 12h, obtains graphite intercalation compound；Process 30s in graphite intercalation compound is placed in 850 DEG C of Muffle furnaces, through pulverizing after taking out cooling, cross 200 mesh sieves, obtain porous graphene powder；In 80 DEG C of water-baths, under the conditions of stir speed (S.S.) 100rpm, ultrasonic power 180w, dispersing cellular Graphene powder and account for its quality 2.5 times hard paraffin mixture 30min after, it is thus achieved that porous graphene/wax phase change granular filler.
The preparation of the filler modified polyamide of step 2, phase change grains
The caprolactam monomer weighing 92.5 g is placed in 250ml flask, 80 DEG C of heating, after completely melted, add phase change grains filler 7.5g and is filled with polyreaction process.The reaction treatment process of gained mixture is: 80 DEG C of first mechanical agitation then supersound process 60min, wherein stir speed (S.S.) 500rpm, ultrasonic power 200w, gained mixture refluxes 30min under the vacuum condition of 130 DEG C, vacuum is 0.095MPa, add 0.25 g sodium hydroxide with vigorous stirring, after gained mixture is carried out vacuum back-flow 30min again, vacuum is 0.095MPa, add 3.0ml promoter Toluene-2,4-diisocyanate, 4-diisocyanate, gained reaction treatment mixture pours in the mould being preheated to 165 DEG C, cooling and demolding after 60min, i.e. obtain polyamide/phase change grains composite.
Embodiment 3
Using the technical scheme of phase change grains weight content 10.0%, concrete preparation method is as follows:
Step one, the preparation of phase change grains
By 15g crystalline flake graphite, in being stirred continuously lower addition 45g concentrated sulphuric acid (98%) and 5g concentrated nitric acid (65%) mixed solution, temperature control 50 DEG C, stirring reaction 60 min, product is washed to neutrality, at 105 DEG C of dry 12h, obtains graphite intercalation compound；Process 30s in graphite intercalation compound is placed in 850 DEG C of Muffle furnaces, through pulverizing after taking out cooling, cross 200 mesh sieves, obtain porous graphene powder；In 80 DEG C of water-baths, under the conditions of stir speed (S.S.) 100rpm, ultrasonic power 180w, dispersing cellular Graphene powder and account for its quality 2.5 times hard paraffin mixture 30min after, it is thus achieved that porous graphene/wax phase change granular filler.
The preparation of the filler modified polyamide of step 2, phase change grains
nullThe caprolactam monomer weighing 90.0 g is placed in 250ml flask，80 DEG C of heating，After completely melted，Adding phase change grains filler 10.0g and be filled with polyreaction process. the reaction treatment process of gained mixture is: 80 DEG C of first mechanical agitation then supersound process 60min，Wherein stir speed (S.S.) 500rpm、Ultrasonic power 200w，Gained mixture refluxes 30min under the vacuum condition of 130 DEG C，Vacuum is 0.095MPa，Add 0.25 g sodium hydroxide with vigorous stirring，After gained mixture is carried out vacuum back-flow 30min again，Vacuum is 0.095MPa，Add 3.0ml promoter Toluene-2,4-diisocyanate，4-diisocyanate，Gained reaction treatment mixture pours in the mould being preheated to 165 DEG C，Cooling and demolding after 60min，I.e. obtain polyamide/phase change grains composite.
Embodiment 4
Using the technical scheme of phase change grains weight content 5%, concrete preparation method is as follows:
Step one, the preparation of phase change grains
By 15g crystalline flake graphite, in being stirred continuously lower addition 45g concentrated sulphuric acid (98%) and 5g concentrated nitric acid (65%) mixed solution, temperature control 30 DEG C, stirring reaction 60 min, product is washed to neutrality, at 105 DEG C of dry 12h, obtains graphite intercalation compound；Process 30s in graphite intercalation compound is placed in 850 DEG C of Muffle furnaces, through pulverizing after taking out cooling, cross 200 mesh sieves, obtain porous graphene powder；In 80 DEG C of water-baths, under the conditions of stir speed (S.S.) 100rpm, ultrasonic power 180w, dispersing cellular Graphene powder and account for its quality 2.5 times hard paraffin mixture 30min after, it is thus achieved that porous graphene/wax phase change granular filler.
The preparation of the filler modified polyamide of step 2, phase change grains
The caprolactam monomer weighing 95.0 g is placed in 250ml flask, 80 DEG C of heating, after completely melted, add phase change grains filler 5.0g and is filled with polyreaction process.The reaction treatment process of gained mixture is: 70 DEG C of first mechanical agitation then supersound process 30min, wherein stir speed (S.S.) 300rpm, ultrasonic power 100w, gained mixture refluxes 30min under the vacuum condition of 140 DEG C, vacuum is 0.099MPa, add 0.2 g sodium hydroxide with vigorous stirring, after gained mixture is carried out vacuum back-flow 50min again, vacuum is 0.099MPa, add 1.5ml promoter Toluene-2,4-diisocyanate, 4-diisocyanate, gained reaction treatment mixture pours in the mould being preheated to 160 DEG C, cooling and demolding after 60min, i.e. obtain polyamide/phase change grains composite.
Embodiment 5
Using the technical scheme of phase change grains weight content 10%, concrete preparation method is as follows:
Step one, the preparation of phase change grains
By 15g crystalline flake graphite, in being stirred continuously lower addition 45g concentrated sulphuric acid (98%) and 5g concentrated nitric acid (65%) mixed solution, temperature control 40 DEG C, stirring reaction 60 min, product is washed to neutrality, at 105 DEG C of dry 12h, obtains graphite intercalation compound；Process 30s in graphite intercalation compound is placed in 850 DEG C of Muffle furnaces, through pulverizing after taking out cooling, cross 200 mesh sieves, obtain porous graphene powder；In 80 DEG C of water-baths, under the conditions of stir speed (S.S.) 100rpm, ultrasonic power 180w, dispersing cellular Graphene powder and account for its quality 2.5 times hard paraffin mixture 30min after, it is thus achieved that porous graphene/wax phase change granular filler.
The preparation of the filler modified polyamide of step 2, phase change grains
The caprolactam monomer weighing 90.0 g is placed in 250ml flask, 80 DEG C of heating, after completely melted, add phase change grains filler 10g and is filled with polyreaction process.The reaction treatment process of gained mixture is: 90 DEG C of first mechanical agitation then supersound process 90min, wherein stir speed (S.S.) 600rpm, ultrasonic power 300w, gained mixture refluxes 40min under the vacuum condition of 150 DEG C, vacuum is 0.090MPa, add 0.35 g sodium hydroxide with vigorous stirring, after gained mixture is carried out vacuum back-flow 40min again, vacuum is 0.090MPa, add 3.5ml promoter Toluene-2,4-diisocyanate, 4-diisocyanate, gained reaction treatment mixture pours in the mould being preheated to 155 DEG C, cooling and demolding after 60min, i.e. obtain polyamide/phase change grains composite.
Comparative example 1
Optimal performance material disclosed in Chinese invention patent 102942694A.
Employing caprolactam: liquid paraffin: Graphene weight ratio is that the technical scheme of 100:10:0.05 is graphene-doped in caprolactam, and catalytic polymerization makes cast composite nylon material, and concrete preparation method is as follows:
100 parts of caprolactams are added with in the reactor of the Vltrasonic device under the conditions of continuously stirred, caprolactam is made to melt in temperature 120 DEG C, add 10 parts of liquid paraffin and 0.05 part of Graphene, it is 180w at ultrasonic power, frequency is 100Hz, and mechanical agitation speed is 800rpm, and temperature is 110 DEG C, disperse 30 minutes, obtain Graphene caprolactam dispersion liquid.In temperature 130 DEG C, vacuum is 0.095MPa, is dehydrated 20 minutes.Add 0.25 part of sodium hydroxide as catalyst, under vacuum is 0.095MPa, continues vacuum dehydration 30 minutes.Open valve and release vacuum, add the triphenylmethane triisocyanate of 3.0 parts, be cast to after stirring rapidly be preheated in the mould of 160 DEG C, natural cooling after being incubated 1.5 hours.Obtain liquid paraffin and Graphene modified cast mylon composite.
Embodiment 1-3 and comparative example are carried out the mensuration of coefficient of friction, wear rate.
Low-speed heave-load operating mode uses MM200 type friction wear testing machine at dry condition, loads 200N, test rate 0.43m/s, test period 60 minutes, and antithesis uses GCr15 steel loop.
High speed light loading operating mode uses MMS-1G type high temperature and high speed friction wear testing machine at dry condition, loads 20N, test rate 24m/s, frictional distance 700m, and antithesis uses GCr15 steel loop.
Concrete measurement result is as follows.
Table 1 low-speed heave-load frictional behaviour parameter list
| Test event | Example 1 | Example 2 | Example 3 | Comparative example |
| Coefficient of friction | 0.10 | 0.09 | 0.088 | 0.12 |
| Volume erosion rate (10-5mm3N-1m-1) | 0.25 | 0.16 | 0.13 | 0.35 |
Table 2 high speed light loading frictional behaviour parameter list
| Test event | Example 1 | Example 2 | Example 3 | Comparative example |
| Coefficient of friction | 0.26 | 0.21 | 0.17 | 0.35 |
| (10-5mm3N-1m-1) | 0.11 | 0.08 | 0.05 | 0.29 |
The foregoing is only several the embodiments of the present invention, be not used in the restriction present invention, present invention is also not necessarily limited to the example above.The change made under other any spirit without departing from the present invention and principle, modify, substitute, combination etc. is regarded as the substitute mode of equivalence, all should belong to scope of the presently claimed invention.
Claims (7)
1. a phase change grains modified polyamide high-abrasive material, it is characterised in that: being formed by catalyst and promoter catalytic polymerization by reaction mass, wherein, reaction mass and catalyst, the adding proportion of promoter are 100g/ (0.2-0.35) g/
(1.5-3.5) ml, reaction mass is made up of the phase change grains material of 5 ~ 10% and the caprolactam of 95 ~ 90% by mass percentage, and described phase change grains material is porous graphene/hard paraffin phase-change material.
2. a kind of phase change grains modified polyamide high-abrasive material as claimed in claim 1, it is characterised in that: described catalyst is sodium hydroxide, and promoter is Toluene-2,4-diisocyanate, 4-diisocyanate.
3. the method preparing phase change grains modified polyamide high-abrasive material as claimed in claim 1, it is characterised in that: comprise the following steps:
Step one, the preparation of phase change grains material
A, weigh crystalline flake graphite, under conditions of being stirred continuously, the crystalline flake graphite weighed is joined in the mixing concentrated acid of concentrated sulphuric acid and concentrated nitric acid composition and react, control temperature and be 30-50 DEG C, mixing time is 60 min, then neutrality it is washed to, washing product is dried 12h under conditions of 105 DEG C, obtains graphite intercalation compound, standby；
B, the graphite intercalation compound of preparation in step a is placed in Muffle furnace under conditions of temperature is 850 DEG C calcining 30s, take out size-reduced, cross 200 mesh sieves after obtain porous graphene powder, standby；
C, the porous graphene powder prepared in step b add the hard paraffin accounting for its quality 2.5 times, then by mixture in the water-bath of 80 DEG C, stir speed (S.S.) be 100rpm, ultrasonic power be to mix 30min under the conditions of 180w, obtain porous graphene/hard paraffin phase change grains filler, standby；
Step 2, the preparation of modified polyamide
D, weigh in caprolactam monomer, catalyst, promoter and step c the porous graphene/wax phase change granule of preparation respectively according to the proportioning in claim 1, standby；
E, the caprolactam monomer weighed in step d is placed in flask, it is heated to molten condition the conditions of 80 DEG C, then the porous graphene weighed in step d/wax phase change granule is joined and caprolactam carries out polyreaction process, described polyreaction processes and includes with the next stage: (1) is first mechanical agitation then supersound process 30-90min, wherein stir speed (S.S.) 300-600rpm, ultrasonic power 100-300w under the conditions of 70-90 DEG C；(2) temperature be 130-150 DEG C, vacuum be 0.090-0.099MPa under conditions of reflux 30-50min；(3) adding, in the mixture after step (2) process, the catalyst weighed in step d under intense agitation, reflux under conditions of vacuum is 0.090-0.099MPa 30-50min, prepares mixture；(4) in the mixture that step (3) prepares, add in step d the promoter weighed and carry out catalytic polymerization, prepared reactant mixture is poured in the mould of (160 ± 5) DEG C, cooling and demolding after 1h, prepares product.
The preparation method of a kind of phase change grains modified polyamide high-abrasive material the most as claimed in claim 3, it is characterised in that: the grain graininess of the crystalline flake graphite used in described step one is less than 500 microns.
The preparation method of a kind of phase change grains modified polyamide high-abrasive material the most as claimed in claim 3, it is characterized in that: crystalline flake graphite described in described step one is 3:10 with the mass ratio mixing concentrated acid, wherein, in mixing concentrated acid, the concentration of concentrated sulphuric acid and concentrated nitric acid is respectively 98% and 65%, and mass ratio is 9:1.
The preparation method of a kind of phase change grains modified polyamide high-abrasive material the most as claimed in claim 3, it is characterised in that: the melting range of the hard paraffin used in described step one is 48 ~ 50 DEG C.
A kind of preparation method preparing phase change grains modified polyamide high-abrasive material, it is characterised in that: the speed being stirred vigorously in (3rd) stage of described step e is more than 600rpm.
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| CN113717516A (en) * | 2021-07-22 | 2021-11-30 | 株洲时代新材料科技股份有限公司 | Composite material for core plate wear plate, core plate wear plate and preparation method of core plate wear plate |
| CN118530604A (en) * | 2024-07-24 | 2024-08-23 | 山东红点新材料有限公司 | Preparation method of modified asphalt and application of modified asphalt in porous graphite product |
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| CN113717516A (en) * | 2021-07-22 | 2021-11-30 | 株洲时代新材料科技股份有限公司 | Composite material for core plate wear plate, core plate wear plate and preparation method of core plate wear plate |
| CN118530604A (en) * | 2024-07-24 | 2024-08-23 | 山东红点新材料有限公司 | Preparation method of modified asphalt and application of modified asphalt in porous graphite product |
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