CN105585815A - Preparation method of high temperature resistance and friction resistance phenolic resin composite material - Google Patents
Preparation method of high temperature resistance and friction resistance phenolic resin composite material Download PDFInfo
- Publication number
- CN105585815A CN105585815A CN201610144391.3A CN201610144391A CN105585815A CN 105585815 A CN105585815 A CN 105585815A CN 201610144391 A CN201610144391 A CN 201610144391A CN 105585815 A CN105585815 A CN 105585815A
- Authority
- CN
- China
- Prior art keywords
- phenol
- phenolic resin
- zirconium dioxide
- flask
- add
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/04—Condensation polymers of aldehydes or ketones with phenols only of aldehydes
- C08G8/08—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ
- C08G8/10—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ with phenol
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/28—Chemically modified polycondensates
-
- C—CHEMISTRY; METALLURGY
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- C—CHEMISTRY; METALLURGY
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/149—Antislip compositions
-
- C—CHEMISTRY; METALLURGY
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2244—Oxides; Hydroxides of metals of zirconium
-
- C—CHEMISTRY; METALLURGY
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Phenolic Resins Or Amino Resins (AREA)
Abstract
The invention discloses a preparation method of a high temperature resistance and friction resistance phenolic resin composite material, and belongs to the field of composite materials. The method comprises the steps that a phenolic resin solution is prepared at first, zirconium dioxide nanometer powder is subjected to surface modification and then added into the phenolic resin solution for a reaction, and the high temperature resistance and friction resistance phenolic resin composite material is obtained. The modified nanometer zirconium dioxide is used as filler to be added into the phenolic resin solution, the compatibility between the solution and a polymer can be improved, the nanometer zirconium dioxide can be evenly added into a polymer matrix, the heat resistance of the modified phenolic resin is greatly improved, the high and stable friction coefficient is obtained and will not be lowered even being affected by rain or snow or extremely hot weather, and the application prospect is wide.
Description
Technical field
The invention discloses a kind of preparation method of high temperature resistant rub resistance phenolic resin composite, belong to composite neckTerritory.
Background technology
The structural weak link of phenolic resins is that the light base of phenol and methylene are easily oxidized, and heat resistance is affected. Along withThe development, particularly various vehicles of industry and mechanical applying working condition condition and Aeronautics and Astronautics and other national defence sophisticated technologyDevelopment, high-quality friction material has been proposed to new requirement, as higher heat decomposition temperature, good hot restorability, footEnough coefficient of friction, preferably anti-wear performance and lower noise etc. With pure phenolic resin as friction material, as senior sedan-chairThe base material of car, motorcycle brake pad and clutch disc, can't meet these requirements. The unmodified phenolic resins fragility of traditionGreatly, poor toughness, heat resistance deficiency, limited the exploitation of high-quality friction material. At present, high-quality friction material phenolic resinsMain leaning on from external import. Therefore, for adapting to the need of the high-technology fields such as automobile, electronics, Aeronautics and Astronautics and national defense industryWant, phenolic resins is carried out to modification, improve the developing direction that its toughness and heat resistance are phenolic resins.
Nano material had been used to phenol-formaldehyde resin modified in the last few years, and had obtained some achievements in research. Nano particle byLittle in size, surface area is large, surperficial non-matching atom is many, thereby strong with phenolic resins binding ability, and can be to phenolic resinsPhysical and chemical performance produces special role. Nano particle is added and in phenolic resins, can overcome conventional rigid particles and can not strengthen increasing simultaneouslyTough shortcoming, toughness, intensity and the heat resistance etc. of raising phenolic resins.
Summary of the invention
The technical problem that the present invention mainly solves:, poor toughness, resistance to large for the unmodified phenolic resins fragility of current traditionHot deficiency, has limited the exploitation of high-quality friction material, can not meet instructions for use with pure phenolic resin as friction materialProblem, provide a kind of preparation method of high temperature resistant rub resistance phenolic resin composite, the present invention first to prepare phenolic aldehyde treeLipoprotein solution, then surface modification is carried out in zirconium dioxide nanometer powder end, joined in phenol resin solution and reacted, obtainHigh temperature resistant rub resistance phenolic resin composite, the present invention is added on phenolic aldehyde tree with the nano zirconium dioxide after modification as fillerLipoprotein solution, can improve the compatibility between polymer, and nano zirconium dioxide can evenly be joined in polymeric matrix,After modification, the heat resistance of phenolic resins is very significantly improved, and has height and stable coefficient of friction, even if be subject to sleet or cruelThe impact of heat condition, coefficient of friction does not also reduce, the prospect being widely used.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is:
(1) in 1L there-necked flask, add 50~70g phenol, then add 3~8g aluminic acid, 100~120mL formaldehyde and 150~200mL mass fraction 25% NaOH is base catalyst, and flask is put into water bath with thermostatic control, and set temperature is 90~95 DEG C,Keep back flow reaction 10~12h at this temperature, reaction is cooled to room temperature after finishing, by product in bottle under 50~60Pa vacuumVacuumize and remove unnecessary water and free-phenol, obtain aluminic acid phenol-formaldehyde resin modified;
(2) above-mentioned aluminic acid phenol-formaldehyde resin modified is mixed with absolute ethyl alcohol by solid-to-liquid ratio 1:5, after mixing, add phenolic resins quality8~10% hexamethylenetetramine, obtains phenol resin solution, leaves and takes for subsequent use;
(3) take 5~10g zirconium dioxide nanometer powder end, put into baking oven, dry 4~5h at 80~90 DEG C, dry rear by solidLiquor ratio 1:10 joins in mass fraction 60% ethanolic solution, carries out ultrasonic dispersion 20~25min, and dispersion liquid is placed in to three mouthfuls of burningsIn bottle, put into water-bath, stir 30~40min at 50~60 DEG C of lower magnetic forces, after stirring, use mass fraction 15% NaOH and matterAmount mark 30% salt acid for adjusting pH value is 3~7, continues to stir 15~20min after regulating;
(4) bath temperature after above-mentioned stirring is increased to 80~90 DEG C, VTES is pressed and ethanolic solutionVolume ratio 1:3~5 are slowly added drop-wise in flask, are controlled in 25~30min and are added dropwise to complete, and stirring reaction 2~5h after dripping is anti-After should finishing, product is cooled to room temperature, then by its centrifugation, obtains sediment, sediment is joined to Soxhlet in absolute ethyl alcoholExtracting 20~22h, after extracting is placed in the solid obtaining the dry 8~10h of baking oven of 70~80 DEG C, can obtain surface modificationAfter nano zirconium dioxide powder;
(5) in phenol resin solution step (2) being made, join in flask, then add phenol resin solution gross mass 2~5% nano zirconium dioxide powder, puts into oil bath pan, at 115~120 DEG C, refluxes, and keeps stirring reaction under reflux state3~5h, reaction finishes rear cooling, and centrifugation obtains sediment, and sediment is rinsed to 2~3 with distilled water and absolute ethyl alcohol respectivelyAfter inferior, put into apparatus,Soxhlet's, with acetone extraction 5~7h, the vacuum drying oven of the solid after extracting being put into 75~85 DEG C is dryIt is dry complete.
The density of the prepared high temperature resistant rub resistance phenolic resin composite of the present invention is 1.76~1.79g/cm3Hot strengthBe 89.9~102.5MPa, impact strength is 4.26~5.03dj/cm2, coefficient of friction is 0.42~0.46, wear rate is 0.16~0.5×10-7cm3/N·m
The invention has the beneficial effects as follows:
(1) the present invention is added on phenol resin solution with the nano zirconium dioxide after modification as filler, can improve and polymerizationCompatibility between thing, can evenly join in polymeric matrix nano zirconium dioxide;
(2) after modification of the present invention, the heat resistance of phenolic resins is very significantly improved, and has height and stable coefficient of friction,Make to be subject to the impact of sleet or extremely hot condition, coefficient of friction does not also reduce;
(3) preparation method of the present invention is simple, with low cost, is with a wide range of applications.
Detailed description of the invention
First in 1L there-necked flask, add 50~70g phenol, then add 3~8g aluminic acid, 100~120mL formaldehyde and 150~200mL mass fraction 25% NaOH is base catalyst, and flask is put into water bath with thermostatic control, and set temperature is 90~95DEG C, keep back flow reaction 10~12h at this temperature, reaction is cooled to room temperature after finishing, by product in bottle in 50~60Pa vacuumUnder degree, vacuumize and remove unnecessary water and free-phenol, obtain aluminic acid phenol-formaldehyde resin modified; Aluminic acid phenol-formaldehyde resin modified is pressed solidLiquor ratio 1:5 mixes with absolute ethyl alcohol, adds the hexamethylenetetramine of phenolic resins quality 8~10% after mixing, obtains phenolic resins moltenLiquid, leaves and takes for subsequent use; Take 5~10g zirconium dioxide nanometer powder end, put into baking oven, at 80~90 DEG C, dry 4~5h, dryJoin in mass fraction 60% ethanolic solution by solid-to-liquid ratio 1:10 afterwards, carry out ultrasonic dispersion 20~25min, dispersion liquid is placed inIn there-necked flask, put into water-bath, stir 30~40min at 50~60 DEG C of lower magnetic forces, after stirring, use mass fraction 15% hydroxideSodium and mass fraction 30% salt acid for adjusting pH value are 3~7, continue to stir 15~20min after regulating; By the bath temperature after stirringBe increased to 80~90 DEG C, by VTES by being slowly added drop-wise in flask than 1:3~5 with volumes of aqueous ethanol,Be controlled in 25~30min and be added dropwise to complete, stirring reaction 2~5h after dripping, is cooled to room temperature by product after reaction finishes, then willIts centrifugation, obtains sediment, and sediment is joined to Soxhlet extracting 20~22h in absolute ethyl alcohol, after extracting by consolidating of obtainingBody is placed in the dry 8~10h of baking oven of 70~80 DEG C, can obtain the nano zirconium dioxide powder after surface modification; To makePhenol resin solution in join in flask, then add phenol resin solution gross mass 2~5% nano zirconium dioxide powder, putEnter in oil bath pan, at 115~120 DEG C, reflux, keep stirring reaction 3~5h under reflux state, reaction finishes rear cooling,Centrifugation obtains sediment, puts into apparatus,Soxhlet's after sediment is rinsed to 2~3 times with distilled water and absolute ethyl alcohol respectively,With acetone extraction 5~7h, the vacuum drying oven of the solid after extracting being put into 75~85 DEG C is completely dry.
Example 1
First in 1L there-necked flask, add 50g phenol, then add 3g aluminic acid, 100mL formaldehyde and 150mL mass fraction 25% hydrogenSodium oxide molybdena is base catalyst, and flask is put into water bath with thermostatic control, and set temperature is 90 DEG C, keeps back flow reaction at this temperature10h, is cooled to room temperature after reaction finishes, and product in bottle is vacuumized under 50Pa vacuum and remove unnecessary water and free benzenePhenol, obtains aluminic acid phenol-formaldehyde resin modified; Aluminic acid phenol-formaldehyde resin modified is mixed with absolute ethyl alcohol by solid-to-liquid ratio 1:5, after mixing, addThe hexamethylenetetramine that enters phenolic resins quality 8%, obtains phenol resin solution, leaves and takes for subsequent use; Take 5g zirconium dioxide nanometer powderEnd, puts into baking oven, and dry 4h at 80 DEG C, joins in mass fraction 60% ethanolic solution by solid-to-liquid ratio 1:10 after being dried, and entersThe ultrasonic dispersion 20min of row, is placed in there-necked flask by dispersion liquid, puts into water-bath, stirs 30min at 50 DEG C of lower magnetic forces, stirsBe 3 with mass fraction 15% NaOH and mass fraction 30% salt acid for adjusting pH value afterwards, after regulating, continue to stir 15min; To stirBath temperature after mixing is increased to 80 DEG C, by VTES by being added drop-wise to than 1:3 is slow with volumes of aqueous ethanolIn flask, be controlled in 25min and be added dropwise to complete, stirring reaction 2h after dripping, is cooled to room temperature by product after reaction finishes, then willIts centrifugation, obtains sediment, and sediment is joined to Soxhlet extracting 20h in absolute ethyl alcohol, after extracting, the solid obtaining is putIn the baking oven of 70 DEG C, dry 8h, can obtain the nano zirconium dioxide powder after surface modification; By molten the phenolic resins makingIn liquid, join in flask, then add phenol resin solution gross mass 2% nano zirconium dioxide powder, put into oil bath pan,At 115 DEG C, reflux, keep stirring reaction 3h under reflux state, reaction finishes rear cooling, and centrifugation obtains sediment, will sinkShallow lake thing is put into apparatus,Soxhlet's after rinsing 2 times with distilled water and absolute ethyl alcohol respectively, uses acetone extraction 5h, by consolidating after extractingIt is dry completely that body is put into the vacuum drying oven of 75 DEG C.
The density of the prepared high temperature resistant rub resistance phenolic resin composite of the present invention is 1.76g/cm3Hot strength is89.9MPa, impact strength is 4.26dj/cm2, coefficient of friction is 0.42, wear rate is 0.16 × 10-7cm3/N·m
Example 2
First in 1L there-necked flask, add 60g phenol, then add 5g aluminic acid, 110mL formaldehyde and 175mL mass fraction 25% hydrogenSodium oxide molybdena is base catalyst, and flask is put into water bath with thermostatic control, and set temperature is 93 DEG C, keeps back flow reaction at this temperature11h, is cooled to room temperature after reaction finishes, and product in bottle is vacuumized under 55Pa vacuum and remove unnecessary water and free benzenePhenol, obtains aluminic acid phenol-formaldehyde resin modified; Aluminic acid phenol-formaldehyde resin modified is mixed with absolute ethyl alcohol by solid-to-liquid ratio 1:5, after mixing, addThe hexamethylenetetramine that enters phenolic resins quality 9%, obtains phenol resin solution, leaves and takes for subsequent use; Take 8g zirconium dioxide nanometer powderEnd, puts into baking oven, and dry 4.5h at 85 DEG C, joins in mass fraction 60% ethanolic solution by solid-to-liquid ratio 1:10 after being dried,Carry out ultrasonic dispersion 23min, dispersion liquid is placed in to there-necked flask, put into water-bath, stir 35min at 55 DEG C of lower magnetic forces, stirMix rear with mass fraction 15% NaOH and mass fraction 30% salt acid for adjusting pH value be 5, regulate after continue stir 17min; WillBath temperature after stirring is increased to 85 DEG C, and VTES is pressed with volumes of aqueous ethanol than the slow dropping of 1:4In flask, be controlled in 27min and be added dropwise to complete, stirring reaction 3.5h after dripping, is cooled to room temperature by product after reaction finishes,By its centrifugation, obtain sediment again, sediment joined to Soxhlet extracting 21h in absolute ethyl alcohol, after extracting by consolidating of obtainingBody is placed in the dry 9h of baking oven of 75 DEG C, can obtain the nano zirconium dioxide powder after surface modification; By the phenolic aldehyde tree makingIn lipoprotein solution, join in flask, then add phenol resin solution gross mass 3% nano zirconium dioxide powder, put into oil bath pan,At 117 DEG C, reflux, keep stirring reaction 4h under reflux state, reaction finishes rear cooling, and centrifugation obtains sediment, willSediment is put into apparatus,Soxhlet's after rinsing 2 times with distilled water and absolute ethyl alcohol respectively, use acetone extraction 6h, by after extractionIt is dry completely that solid is put into the vacuum drying oven of 80 DEG C.
The density of the prepared high temperature resistant rub resistance phenolic resin composite of the present invention is 1.78g/cm3Hot strength is100.5MPa, impact strength is 4.68dj/cm2, coefficient of friction is 0.44, wear rate is 0.36 × 10-7cm3/N·m
Example 3
First in 1L there-necked flask, add 70g phenol, then add 8g aluminic acid, 120mL formaldehyde and 200mL mass fraction 25% hydrogenSodium oxide molybdena is base catalyst, and flask is put into water bath with thermostatic control, and set temperature is 95 DEG C, keeps back flow reaction at this temperature12h, is cooled to room temperature after reaction finishes, and product in bottle is vacuumized under 60Pa vacuum and remove unnecessary water and free benzenePhenol, obtains aluminic acid phenol-formaldehyde resin modified; Aluminic acid phenol-formaldehyde resin modified is mixed with absolute ethyl alcohol by solid-to-liquid ratio 1:5, after mixing, addThe hexamethylenetetramine that enters phenolic resins quality 10%, obtains phenol resin solution, leaves and takes for subsequent use; Take 10g zirconium dioxide nanometer powderEnd, puts into baking oven, and dry 5h at 90 DEG C, joins in mass fraction 60% ethanolic solution by solid-to-liquid ratio 1:10 after being dried, and entersThe ultrasonic dispersion 25min of row, is placed in there-necked flask by dispersion liquid, puts into water-bath, stirs 40min at 60 DEG C of lower magnetic forces, stirsBe 7 with mass fraction 15% NaOH and mass fraction 30% salt acid for adjusting pH value afterwards, after regulating, continue to stir 20min; To stirBath temperature after mixing is increased to 90 DEG C, by VTES by being slowly added drop-wise to burning with volumes of aqueous ethanol than 5In bottle, be controlled in 30min and be added dropwise to complete, stirring reaction 5h after dripping, is cooled to room temperature by product after reaction finishes, then by itCentrifugation, obtains sediment, and sediment is joined to Soxhlet extracting 22h in absolute ethyl alcohol, after extracting, the solid obtaining is placed inIn the baking oven of 80 DEG C, dry 10h, can obtain the nano zirconium dioxide powder after surface modification; By the phenol resin solution makingIn join in flask, then add phenol resin solution gross mass 5% nano zirconium dioxide powder, put into oil bath pan, 120At DEG C, reflux, keep stirring reaction 5h under reflux state, reaction finishes rear cooling, and centrifugation obtains sediment, will precipitateThing is put into apparatus,Soxhlet's after rinsing 3 times with distilled water and absolute ethyl alcohol respectively, uses acetone extraction 7h, by the solid after extractingThe vacuum drying oven of putting into 85 DEG C is completely dry.
The density of the prepared high temperature resistant rub resistance phenolic resin composite of the present invention is 1.79g/cm3Hot strength is102.5MPa, impact strength is 4.26~5.03dj/cm2, coefficient of friction is 0.46, wear rate is 0.5 × 10-7cm3/N·m。
Claims (1)
1. a preparation method for high temperature resistant rub resistance phenolic resin composite, is characterized in that concrete preparation method is:
(1) in 1L there-necked flask, add 50~70g phenol, then add 3~8g aluminic acid, 100~120mL formaldehyde and 150~200mL mass fraction 25% NaOH is base catalyst, and flask is put into water bath with thermostatic control, and set temperature is 90~95 DEG C,Keep back flow reaction 10~12h at this temperature, reaction is cooled to room temperature after finishing, by product in bottle under 50~60Pa vacuumVacuumize and remove unnecessary water and free-phenol, obtain aluminic acid phenol-formaldehyde resin modified;
(2) above-mentioned aluminic acid phenol-formaldehyde resin modified is mixed with absolute ethyl alcohol by solid-to-liquid ratio 1:5, after mixing, add phenolic resins quality8~10% hexamethylenetetramine, obtains phenol resin solution, leaves and takes for subsequent use;
(3) take 5~10g zirconium dioxide nanometer powder end, put into baking oven, dry 4~5h at 80~90 DEG C, dry rear by solidLiquor ratio 1:10 joins in mass fraction 60% ethanolic solution, carries out ultrasonic dispersion 20~25min, and dispersion liquid is placed in to three mouthfuls of burningsIn bottle, put into water-bath, stir 30~40min at 50~60 DEG C of lower magnetic forces, after stirring, use mass fraction 15% NaOH and matterAmount mark 30% salt acid for adjusting pH value is 3~7, continues to stir 15~20min after regulating;
(4) bath temperature after above-mentioned stirring is increased to 80~90 DEG C, VTES is pressed and ethanolic solutionVolume ratio 1:3~5 are slowly added drop-wise in flask, are controlled in 25~30min and are added dropwise to complete, and stirring reaction 2~5h after dripping is anti-After should finishing, product is cooled to room temperature, then by its centrifugation, obtains sediment, sediment is joined to Soxhlet in absolute ethyl alcoholExtracting 20~22h, after extracting is placed in the solid obtaining the dry 8~10h of baking oven of 70~80 DEG C, can obtain surface modificationAfter nano zirconium dioxide powder;
(5) in phenol resin solution step (2) being made, join in flask, then add phenol resin solution gross mass 2~5% nano zirconium dioxide powder, puts into oil bath pan, at 115~120 DEG C, refluxes, and keeps stirring reaction under reflux state3~5h, reaction finishes rear cooling, and centrifugation obtains sediment, and sediment is rinsed to 2~3 with distilled water and absolute ethyl alcohol respectivelyAfter inferior, put into apparatus,Soxhlet's, with acetone extraction 5~7h, the vacuum drying oven of the solid after extracting being put into 75~85 DEG C is dryIt is dry complete.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201610144391.3A CN105585815A (en) | 2016-03-15 | 2016-03-15 | Preparation method of high temperature resistance and friction resistance phenolic resin composite material |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201610144391.3A CN105585815A (en) | 2016-03-15 | 2016-03-15 | Preparation method of high temperature resistance and friction resistance phenolic resin composite material |
Publications (1)
Publication Number | Publication Date |
---|---|
CN105585815A true CN105585815A (en) | 2016-05-18 |
Family
ID=55925740
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201610144391.3A Withdrawn CN105585815A (en) | 2016-03-15 | 2016-03-15 | Preparation method of high temperature resistance and friction resistance phenolic resin composite material |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN105585815A (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108895102A (en) * | 2018-07-11 | 2018-11-27 | 薛向东 | A kind of preparation method of heat resistant and wear resistant type brake block |
CN114456784A (en) * | 2021-12-07 | 2022-05-10 | 中国海洋石油集团有限公司 | Long-storage phenolic resin cross-linking agent and high-temperature high-salt gel prepared from same |
-
2016
- 2016-03-15 CN CN201610144391.3A patent/CN105585815A/en not_active Withdrawn
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108895102A (en) * | 2018-07-11 | 2018-11-27 | 薛向东 | A kind of preparation method of heat resistant and wear resistant type brake block |
CN108895102B (en) * | 2018-07-11 | 2020-06-02 | 山西罗克森机械设备有限责任公司 | Preparation method of high-temperature-resistant wear-resistant brake pad |
CN114456784A (en) * | 2021-12-07 | 2022-05-10 | 中国海洋石油集团有限公司 | Long-storage phenolic resin cross-linking agent and high-temperature high-salt gel prepared from same |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN103146147B (en) | A kind of epoxy resin toughened/glass fibre prepreg and preparation method | |
CN102220062B (en) | Aqueous UV curing coating and preparation method thereof | |
CN103709346B (en) | A kind of preparation method of phenolic resin aerogel | |
CN102911308B (en) | Method for preparing fluorine contained polyacrylate/dual-sized nano SiO2 composite emulsion | |
CN104073116B (en) | Preparation method of super-amphiphobic coating | |
CN103342823B (en) | The method of hydrogel is prepared in a kind of enzymatic radical polymerization | |
CN106367031A (en) | High thermal conductivity composite phase change microcapsule and preparation method thereof | |
CN101831230A (en) | Method for preparing polyacrylate/nano-SiO2 compound coating agent by using reactive emulsifier | |
CN101812156B (en) | Water-base ambient crosslinking acrylate wood paint resin and preparation method thereof | |
CN106832757A (en) | A kind of composite of Graphene phenol-formaldehyde resin modified and preparation method thereof, application | |
CN102876297B (en) | A kind of low condensate depression phase-change material micro-capsule and preparation method thereof | |
CN103881295B (en) | A kind of modified by nano particles carbon cloth strengthens the preparation method of Wet-type friction material | |
CN108517024B (en) | Polyacrylate/nano ZnO composite leather finishing agent prepared by Pickering miniemulsion polymerization method and preparation method thereof | |
CN105585815A (en) | Preparation method of high temperature resistance and friction resistance phenolic resin composite material | |
CN108373864A (en) | A kind of High Performance Corrosion Protective Coatings and preparation method thereof | |
CN104844753A (en) | Preparation method of macromolecular composite microsphere with magnetic nanometer function | |
CN105176328A (en) | High-performance alloy-matrix anticorrosive paint and preparation method thereof | |
CN113732241B (en) | Hydrophilic nano-silica modified inorganic phosphate binder and application thereof | |
CN106147117B (en) | The preparation method of growing zinc oxide nanorod reinforced resin base frication material on carbon cloth | |
CN102786643B (en) | Preparation method and application of molecularly imprinted polymer of sulfadiazine for controlled catalytic degradation | |
CN102732148B (en) | Urushiol silicon high temperature resistant liquid anti-corrosion paint | |
CN109504216A (en) | A kind of graphene modified aqueous acrylic acid coating and preparation method thereof | |
CN102604453A (en) | Special nanometer composite seal paint for woodware and preparing method thereof | |
CN109333714A (en) | A kind of preparation method and its timber of super-hydrophobic magnetic timber | |
CN102391730B (en) | Nano functional coating |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
WW01 | Invention patent application withdrawn after publication |
Application publication date: 20160518 |
|
WW01 | Invention patent application withdrawn after publication |