CN108531248A - A kind of wear-resisting anti-hardening preparation of greases method - Google Patents
A kind of wear-resisting anti-hardening preparation of greases method Download PDFInfo
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- CN108531248A CN108531248A CN201810569825.3A CN201810569825A CN108531248A CN 108531248 A CN108531248 A CN 108531248A CN 201810569825 A CN201810569825 A CN 201810569825A CN 108531248 A CN108531248 A CN 108531248A
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M159/00—Lubricating compositions characterised by the additive being of unknown or incompletely defined constitution
- C10M159/12—Reaction products
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
- C10M169/04—Mixtures of base-materials and additives
- C10M169/048—Mixtures of base-materials and additives the additives being a mixture of compounds of unknown or incompletely defined constitution, non-macromolecular and macromolecular compounds
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M177/00—Special methods of preparation of lubricating compositions; Chemical modification by after-treatment of components or of the whole of a lubricating composition, not covered by other classes
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/04—Elements
- C10M2201/041—Carbon; Graphite; Carbon black
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/04—Elements
- C10M2201/05—Metals; Alloys
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/06—Metal compounds
- C10M2201/062—Oxides; Hydroxides; Carbonates or bicarbonates
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/085—Phosphorus oxides, acids or salts
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/28—Esters
- C10M2207/30—Complex esters, i.e. compounds containing at leasst three esterified carboxyl groups and derived from the combination of at least three different types of the following five types of compounds: monohydroxyl compounds, polyhydroxy xompounds, monocarboxylic acids, polycarboxylic acids or hydroxy carboxylic acids
- C10M2207/301—Complex esters, i.e. compounds containing at leasst three esterified carboxyl groups and derived from the combination of at least three different types of the following five types of compounds: monohydroxyl compounds, polyhydroxy xompounds, monocarboxylic acids, polycarboxylic acids or hydroxy carboxylic acids used as base material
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2221/00—Organic macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/08—Resistance to extreme temperature
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/10—Inhibition of oxidation, e.g. anti-oxidants
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/26—Waterproofing or water resistance
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2050/00—Form in which the lubricant is applied to the material being lubricated
- C10N2050/10—Semi-solids; greasy
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Lubricants (AREA)
Abstract
The present invention relates to lubricating grease preparing technical fields, and in particular to a kind of wear-resisting anti-hardening preparation of greases method.The present invention will make xerogel by oneself,Oleic acid,Heisuojin is configured to explosive by a certain percentage,Carbon coating copper nano particles are obtained through detonation,By microbial grease,Ethyl palmitate,Esterification products are obtained by the reaction in lithium amide etc.,It places it in centrifugation layering and obtains biological lubricant crude product,Processing finally is distilled to it and obtains biological lubricant,With vegetable seed oleic acid,Azelaic acid,Neopentyl glycol is that raw material is esterified to obtain mixed ester,Mix carbon coating copper nano particles,Obtain wear-resisting anti-hardening lubricating grease,Copper is under friction surface micro-bulge or rough peak strong collision and frictional heat energy effect,Play surface modifying function,To play friction-reducing and antiwear action,Improve the high temperature resistance and sintering load of lubricating grease,Carbon coating copper nano particles can Composite calcium-sulfonate-batetrapolyurea,Reduce the consumption of lubricating grease small particles,Avoid the Surface hardened layer phenomenon of lubricating grease,It has a extensive future.
Description
Technical field
The present invention relates to lubricating grease preparing technical fields, and in particular to a kind of wear-resisting anti-hardening preparation of greases method.
Background technology
The essence of friction process is the consumption of energy and the loss process of material, it was reported that generation is had lost due to friction
The 50%~70% of boundary's energy, 80% machine failure is caused by the abrasion of parts.Lubrication is the most effective of antifriction antiwear
One of approach.
Lubricating grease is that thickening agent is scattered in base oil（Fluid lubricant）Formed in it is a kind of half with plasticity solid
Body shape product.The additive or filler for being intended to improve certain characteristic can be added in this product, mainly by mineral oil（Or synthesis profit
Lubricating oil）It is modulated with thickening agent.Lubricating grease mainly plays reduction mechanical friction, prevents the effect of mechanical wear while also simultaneous
Prevent protective effect and the sealing and dustproof effect of metal erosion.There are some lubricating grease to be mainly used to prevent metal rusting or corrosion,
Referred to as protect lubricating grease.Such as industrial vaseline etc. has a small number of lubricating grease to be specially used as sealing use, referred to as packing grease, such as screw thread
Fat.Lubricating grease is the substance of semi-solid mostly, has unique mobility.
The rapid development of the modern industry, the requirement to lubricating grease is higher and higher, and the lubricating grease of high-quality multiple-effect is its development
Direction.Complex calcium sulfonate grease is current one of high-performance multipurpose grease few in number, it has good resistance to height
Warm nature, extreme pressure anti-wear, shear stability, low temperature pumpmg quality, rust-preventing characteristic and water-resistance, and raw material is easy to get, cost is relatively low, more
The foreground of being widely applied is suffered from the various bad working environments environment such as dirt, more water, high load capacity.The lubricating grease is without heavy metal and right
The harmful functional additive of environment is a kind of environment-friendly type lubricating grease.Such lubricating grease is especially suitable for steel mill's conticaster, tandem mill
The lubrication of equipment under group and conditions of similarity is conducive to simplify lubricating grease kind, facilitates with oil management, is referred to as " high-efficiency lubricating
Fat " causes the extensive concern of domestic and international lubricating grease industry.
The performance of calcium sulfonate complex grease depends greatly on will be unformed in newton body calcium sulfonate with high base number
CaCO3It is converted into the transformation of crystal process of the non-newtonian fluid sulfoacid calcium of calcite crystal form.If the content of calcium carbonate is insufficient or it
In calcium carbonate be not fully converted to calcite crystal form from unformed, then lubricating grease can be partially soft, and high-temperature behavior is bad, lubricating grease
Sintering load it is relatively low.In addition, that there is also stability is poor, extreme pressure is anti-for complex calcium sulfonate grease in the prior art lubrication
Poor, poor fire the defect of mill property.
Invention content
Present invention mainly solves the technical issues of, for lubricating grease in the prior art extreme pressure and antiwear behavior need into
One step is promoted, and properties of product are unstable, and existing composite sulfoacid calcium-soap grease production technology is more complicated, compound at present
In calcium sulfonate grease in newton body calcium sulfonate with high base number unformed calcium carbonate be converted into during calcite crystal form transforming degree compared with
Small, lubricating grease can be partially soft, and high-temperature behavior is bad, and in addition complex calcium sulfonate grease can have grain due to particle diameter distribution unevenness
The trend that sub- phase total surface area reduces, makes small particles gradually be consumed, big particle is gradually grown up, to accelerate such lubricating grease
Case-hardened defect, provide a kind of wear-resisting anti-hardening preparation of greases method.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
A kind of wear-resisting anti-hardening preparation of greases method, it is characterised in that specifically preparation process is：
（1）It counts in parts by weight, 30~40 parts of citric acid solutions is mixed with 20~25 parts of nitrate trihydrate copper and are placed in beaker, it will
Beaker is placed in water-bath, heat temperature raising, stirs to get copper citrate gel, and copper citrate gel is placed in baking oven, heating
Heating, is dried to obtain copper citrate xerogel, is put into hermetic bag and preserves；
（2）It takes 15~18g copper citrates xerogel, 32~35g oleic acid, 50~55g heisuojin to be mixed to get explosive, explosive is filled
Enter in sealed plastic bag, sealed plastic bag connects a lead, and it is that 50~60L is close that sealed plastic bag is suspended on volume with lead
Container center is closed, nitrogen and argon gas are filled with into closed container, ignition charge is stood, and collection obtains carbon coating copper nano particles；
（3）Yeast dry powder is mixed with organic extract liquid, is put into separatory funnel, is stood, subnatant is removed, upper liquid is taken to be put into
In distilling apparatus, heat temperature raising, distillation obtains microbial grease；
（4）Microbial grease, ethyl palmitate, diphenylamines, lithium amide are mixed and be put into reaction kettle, heating water bath heating is protected
Temperature reaction, obtains esterification products, esterification products is put into supercentrifuge and are centrifuged, and stratification removes supernatant liquid, obtains
Lower layer's biological lubricant crude product, biological lubricant crude product is placed in distilling apparatus, heat temperature raising, and distillation is to there is no liquid steamings
Go out, obtains biological lubricant；
（5）Wooden calcium sulfonate 20~30min of solid abrasive is obtained into lignosulfonic acid calcium powder, lignosulfonic acid calcium powder is configured to
After 400~450mL wooden calcium sulfonates aqueous solution, be added to blender, dropping funel three-necked flask in, to three-necked flask
After logical nitrogen excludes air, potassium hydroxide solution adjusting pH is added into three-necked flask, stirs to get alkaline solution；
（6）Count in parts by weight, into the four-hole boiling flask with reflux and blender be added 40~50 parts of azelaic acids, 60~
65 parts of neopentyl glycols, 30~35 parts of biological lubricants, 20~25 parts of above-mentioned alkaline solutions start blender under nitrogen protection, with
The rotating speed of 200~230r/min is stirred, and to four-hole boiling flask heat temperature raising, insulated and stirred reaction is until reflux no longer goes out
Water removes reflux, 20~25 parts of carbon coating copper nano particles, 10~20 parts of calcium phosphate is added to four-hole boiling flask, heat preservation is stirred
It mixes, discharging obtains wear-resisting anti-hardening lubricating grease.
Step（1）The mass fraction of the citric acid solution is 20%, and temperature is 80~90 DEG C after heat temperature raising, stirring
Time is 40~50min, and temperature is 100~110 DEG C after heat temperature raising, and drying time is 6~7h.
Step（2）The volume ratio of the nitrogen and argon gas is 3 ︰ 1, and time of repose is 10~15min.
Step（3）The yeast dry powder is 1 ︰ 10 with organic extract liquid mixing quality ratio, and organic extract liquid is by chloroform, first
Alcohol, water are that 2 ︰, 1 ︰ 2 are mixed by volume, and time of repose is 20~30min, and temperature is 90~100 DEG C after heat temperature raising, is steamed
It is 4~5h to evaporate the time.
Step（4）The microbial grease, ethyl palmitate, diphenylamines, lithium amide mixing quality ratio are 2 ︰, 5 ︰, 3 ︰ 1,
Temperature is 60~70 DEG C after heating water bath heating, and the insulation reaction time is 2~3h, and supercentrifuge rotating speed is 2000~2200r/
Min, rotating speed centrifugation time are 15~20min, and temperature is 70~80 DEG C after heat temperature raising.
Step（5）The mass fraction of wooden calcium sulfonate's aqueous solution is 30%, and the mass fraction of potassium hydroxide solution is
40%, it is 8~9 to adjust pH, and mixing time is 10~15min.
Step（6）Temperature is 80~85 DEG C after the heat temperature raising, and the insulated and stirred time is 40~50min.
The beneficial effects of the invention are as follows：
（1）Copper citrate xerogel is prepared in citric acid and nitrate trihydrate copper Hybrid Heating, drying by the present invention, will be dry solidifying
Glue, oleic acid, heisuojin are configured to explosive by a certain percentage, and carbon coating copper nano particles are obtained through detonation,
Yeast dry powder is placed in organic extract liquid, subnatant is obtained by extraction, subnatant is distilled to obtain microbial grease, it will be micro-
Esterification products are obtained by the reaction in the mixing such as bio-oil, ethyl palmitate, lithium amide, diphenylamines, heating and thermal insulation, and esterification products are set
It is layered in centrifugation, obtains lower layer's biological lubricant crude product, finally biological lubricant crude product distillation is handled to obtain biological lubricant,
It is esterified to obtain mixed ester using vegetable seed oleic acid, azelaic acid, neopentyl glycol as raw material, mixes carbon coating copper nano particles, be prepared
Wear-resisting anti-hardening lubricating grease, in lubricating oil after incorporation carbon coating copper nano particles, copper is micro- in friction surface as soft metal particle
Under convex body or rough peak strong collision and frictional heat energy effect, participate in local metallurgical reaction, change the substance of friction surface at
Point, surface modifying function is played, there is friction portion fresh surface chemism and catalytic action metal nanoparticle can be made negative
Monocrystalline is reduced under the reduction of electronics, the localized hyperthermia for the generation that rubs in addition makes crystallite simple substance in friction subtabulation
Face forms the molten alloy film with wear-compensating effect, to play friction-reducing and antiwear action；
（2）The lube base oil of the present invention is bio-oil, and thickening agent is carbon coating copper nano particles and wooden calcium sulfonate's group
At mixture, have preferable Efficient Adhesive Promotion, the wooden calcium sulfonate of alkalization can be enable to play fabulous dispersion effect, and energy
It is enough that the fat of thickening is separated into smaller particle, since the performance of calcium sulfonate complex grease is depended greatly on newton
Unformed calcium carbonate is converted into the transformation of crystal process of the non-newtonian fluid sulfoacid calcium of calcite crystal form in body calcium sulfonate with high base number, this
Invention forms the conversion ratio of calcite crystal form by the unformed calcium carbonate of highly polar raising of biological lubricant, improves lubricating grease
High temperature resistance and sintering load, in addition, conversion after calcite crystal form calcium carbonate grain size and particle diameter distribution from
Ostwald, which is cured, theoretically also can largely influence the hardening of calcium sulfonate complex grease, lubricating grease during storage,
Due to particle diameter distribution unevenness, can exist particle phase total surface area reduction trend, but the present invention carbon coating copper nano particles
Can Composite calcium-sulfonate-batetrapolyurea, reduce lubricating grease small particles consumption, improve lubricating grease small particles dispersibility, avoid the table of lubricating grease
Face hardening phenomenon, and under the factors effect such as the high temperature of friction generation and oxygen oxidation reaction life occurs for microorganism lubricating oil
At high-temperature oxidation resistant group, have a extensive future.
Specific implementation mode
It counts in parts by weight, citric acid solution and 20~25 parts of nitrate trihydrate copper by 30~40 parts of mass fractions for 20%
Mixing is placed in beaker, and beaker is placed in water-bath, is heated to 80~90 DEG C, is stirred 40~50min, is obtained citric acid
Copper citrate gel is placed in baking oven by copper gel, is heated to 100~110 DEG C, and it is dry to obtain copper citrate by dry 6~7h
Gel is put into hermetic bag and preserves；15~18g copper citrates xerogel, 32~35g oleic acid, 50~55g heisuojin is taken to mix
To explosive, explosive is fitted into sealed plastic bag, sealed plastic bag connects a lead, and sealed plastic bag is suspended on lead
Volume is 50~60L closed containers center, and the nitrogen and argon gas that volume ratio is 3 ︰ 1 are filled with into closed container, and ignition charge is quiet
10~15min is set, collection obtains carbon coating copper nano particles；Yeast dry powder is mixed for 1 ︰ 10 in mass ratio with organic extract liquid
It closes, wherein organic extract liquid is that 2 ︰, 1 ︰ 2 are mixed by volume by chloroform, methanol, water, is put into separatory funnel, stands 20
~30min removes subnatant, upper liquid is taken to be put into distilling apparatus, is heated to 90~100 DEG C, distills 4~5h, obtains
Microbial grease；It is that 2 ︰, 5 ︰, 3 ︰ 1 mixing is put into reaction in mass ratio by microbial grease, ethyl palmitate, diphenylamines, lithium amide
In kettle, heating water bath is warming up to 60~70 DEG C, 2~3h of insulation reaction, obtains esterification products, and esterification products are put into high speed centrifugation
15~20min is centrifuged with the rotating speed of 2000~2200r/min in machine, stratification removes supernatant liquid, obtains lower layer's biology profit
Biological lubricant crude product is placed in distilling apparatus by lubricating oil crude product, is heated to 70~80 DEG C, distillation is to there is no liquid steamings
Go out, obtains biological lubricant；Wooden calcium sulfonate 20~30min of solid abrasive is obtained into lignosulfonic acid calcium powder, by lignosulfonic acid
Calcium powder is configured to 400~450mL mass fractions after 30% wooden calcium sulfonate's aqueous solution, to be added to blender, dropping liquid leakage
In the three-necked flask of bucket, after leading to nitrogen exclusion air to three-necked flask, the hydrogen-oxygen that mass fraction is 40% is added into three-necked flask
It is 8~9 to change potassium solution to adjust pH, stirs 10~15min, obtains alkaline solution；It counts in parts by weight, to reflux and stirring
It mixes and 40~50 parts of azelaic acids, 60~65 parts of neopentyl glycols, 30~35 parts of biological lubricants, 20~25 is added in the four-hole boiling flask of device
The above-mentioned alkaline solution of part is started blender, is stirred with the rotating speed of 200~230r/min, to four-hole boiling flask under nitrogen protection
Be heated to 80~85 DEG C, insulated and stirred reaction removes reflux until reflux is no longer discharged, to four-hole boiling flask plus
Enter 20~25 parts of carbon coating copper nano particles, 10~20 parts of calcium phosphate, 40~50min of insulated and stirred, discharging obtains wear-resisting anti-hard
Change lubricating grease.
It counts in parts by weight, the citric acid solution that 30 parts of mass fractions are 20% is mixed with 20 parts of nitrate trihydrate copper and is placed in
In beaker, beaker is placed in water-bath, is heated to 80 DEG C, 40min is stirred, copper citrate gel is obtained, by citric acid
Copper gel is placed in baking oven, is heated to 100 DEG C, and dry 6h obtains copper citrate xerogel, is put into hermetic bag and preserves；
It takes 15g copper citrates xerogel, 32g oleic acid, 50g heisuojin to be mixed to get explosive, explosive is fitted into sealed plastic bag, seal
Polybag connects a lead, and it is 50L closed containers center that sealed plastic bag is suspended on volume with lead, into closed container
It is filled with the nitrogen and argon gas that volume ratio is 3 ︰ 1, ignition charge stands 10min, and collection obtains carbon coating copper nano particles；By ferment
Female dry powder is that 1 ︰ 10 is mixed in mass ratio with organic extract liquid, and wherein organic extract liquid is 2 ︰ by volume by chloroform, methanol, water
1 ︰ 2 is mixed, and is put into separatory funnel, and 20min is stood, and removes subnatant, upper liquid is taken to be put into distilling apparatus, and heating rises
Temperature distills 4h, obtains microbial grease to 90 DEG C；In mass ratio by microbial grease, ethyl palmitate, diphenylamines, lithium amide
It is put into reaction kettle for 2 ︰, 5 ︰, 3 ︰ 1 mixing, heating water bath is warming up to 60 DEG C, and insulation reaction 2h obtains esterification products, and esterification is produced
Object is put into supercentrifuge the centrifugation 15min of the rotating speed with 2000r/min, and stratification removes supernatant liquid, obtains lower layer's life
Object lubricating oil crude product, biological lubricant crude product is placed in distilling apparatus, is heated to 70 DEG C, distillation is to there is no liquid steamings
Go out, obtains biological lubricant；Wooden calcium sulfonate solid abrasive 20min is obtained into lignosulfonic acid calcium powder, by lignosulfonic acid calcium powder
End is configured to after 400mL mass fractions are 30% wooden calcium sulfonate's aqueous solution, be added to blender, three mouthfuls of dropping funel
In flask, after leading to nitrogen exclusion air to three-necked flask, the potassium hydroxide solution that mass fraction is 40% is added into three-necked flask
It is 8 to adjust pH, stirs 10min, obtains alkaline solution；It counts in parts by weight, to the four-hole boiling flask with reflux and blender
40 parts of azelaic acids of middle addition, 60 parts of neopentyl glycols, 30 parts of biological lubricants, 20 parts of above-mentioned alkaline solutions start under nitrogen protection
Blender is stirred with the rotating speed of 200r/min, is heated to 80 DEG C to four-hole boiling flask, insulated and stirred reaction is until reflux
Device is no longer discharged, and removes reflux, and 20 parts of carbon coating copper nano particles, 10 parts of calcium phosphate, heat preservation is added to four-hole boiling flask
40min is stirred, discharging obtains wear-resisting anti-hardening lubricating grease.
It counts in parts by weight, the citric acid solution that 35 parts of mass fractions are 20% is mixed with 23 parts of nitrate trihydrate copper and is placed in
In beaker, beaker is placed in water-bath, is heated to 85 DEG C, 45min is stirred, copper citrate gel is obtained, by citric acid
Copper gel is placed in baking oven, is heated to 105 DEG C, and dry 6h obtains copper citrate xerogel, is put into hermetic bag and preserves；
It takes 17g copper citrates xerogel, 33g oleic acid, 53g heisuojin to be mixed to get explosive, explosive is fitted into sealed plastic bag, seal
Polybag connects a lead, and it is 55L closed containers center that sealed plastic bag is suspended on volume with lead, into closed container
It is filled with the nitrogen and argon gas that volume ratio is 3 ︰ 1, ignition charge stands 13min, and collection obtains carbon coating copper nano particles；By ferment
Female dry powder is that 1 ︰ 10 is mixed in mass ratio with organic extract liquid, and wherein organic extract liquid is 2 ︰ by volume by chloroform, methanol, water
1 ︰ 2 is mixed, and is put into separatory funnel, and 25min is stood, and removes subnatant, upper liquid is taken to be put into distilling apparatus, and heating rises
Temperature distills 4h, obtains microbial grease to 95 DEG C；In mass ratio by microbial grease, ethyl palmitate, diphenylamines, lithium amide
It is put into reaction kettle for 2 ︰, 5 ︰, 3 ︰ 1 mixing, heating water bath is warming up to 65 DEG C, and insulation reaction 2h obtains esterification products, and esterification is produced
Object is put into supercentrifuge the centrifugation 17min of the rotating speed with 2100r/min, and stratification removes supernatant liquid, obtains lower layer's life
Object lubricating oil crude product, biological lubricant crude product is placed in distilling apparatus, is heated to 75 DEG C, distillation is to there is no liquid steamings
Go out, obtains biological lubricant；Wooden calcium sulfonate solid abrasive 25min is obtained into lignosulfonic acid calcium powder, by lignosulfonic acid calcium powder
End is configured to after 425mL mass fractions are 30% wooden calcium sulfonate's aqueous solution, be added to blender, three mouthfuls of dropping funel
In flask, after leading to nitrogen exclusion air to three-necked flask, the potassium hydroxide solution that mass fraction is 40% is added into three-necked flask
It is 8 to adjust pH, stirs 13min, obtains alkaline solution；It counts in parts by weight, to the four-hole boiling flask with reflux and blender
45 parts of azelaic acids of middle addition, 63 parts of neopentyl glycols, 33 parts of biological lubricants, 23 parts of above-mentioned alkaline solutions start under nitrogen protection
Blender is stirred with the rotating speed of 225r/min, is heated to 83 DEG C to four-hole boiling flask, insulated and stirred reaction is until reflux
Device is no longer discharged, and removes reflux, and 23 parts of carbon coating copper nano particles, 15 parts of calcium phosphate, heat preservation is added to four-hole boiling flask
45min is stirred, discharging obtains wear-resisting anti-hardening lubricating grease.
It counts in parts by weight, the citric acid solution that 40 parts of mass fractions are 20% is mixed with 25 parts of nitrate trihydrate copper and is placed in
In beaker, beaker is placed in water-bath, is heated to 90 DEG C, 50min is stirred, copper citrate gel is obtained, by citric acid
Copper gel is placed in baking oven, is heated to 110 DEG C, and dry 7h obtains copper citrate xerogel, is put into hermetic bag and preserves；
It takes 18g copper citrates xerogel, 35g oleic acid, 55g heisuojin to be mixed to get explosive, explosive is fitted into sealed plastic bag, seal
Polybag connects a lead, and it is 60L closed containers center that sealed plastic bag is suspended on volume with lead, into closed container
It is filled with the nitrogen and argon gas that volume ratio is 3 ︰ 1, ignition charge stands 15min, and collection obtains carbon coating copper nano particles；By ferment
Female dry powder is that 1 ︰ 10 is mixed in mass ratio with organic extract liquid, and wherein organic extract liquid is 2 ︰ by volume by chloroform, methanol, water
1 ︰ 2 is mixed, and is put into separatory funnel, and 30min is stood, and removes subnatant, upper liquid is taken to be put into distilling apparatus, and heating rises
Temperature distills 5h, obtains microbial grease to 100 DEG C；In mass ratio by microbial grease, ethyl palmitate, diphenylamines, lithium amide
It is put into reaction kettle for 2 ︰, 5 ︰, 3 ︰ 1 mixing, heating water bath is warming up to 70 DEG C, and insulation reaction 3h obtains esterification products, and esterification is produced
Object is put into supercentrifuge the centrifugation 20min of the rotating speed with 2200r/min, and stratification removes supernatant liquid, obtains lower layer's life
Object lubricating oil crude product, biological lubricant crude product is placed in distilling apparatus, is heated to 80 DEG C, distillation is to there is no liquid steamings
Go out, obtains biological lubricant；Wooden calcium sulfonate solid abrasive 30min is obtained into lignosulfonic acid calcium powder, by lignosulfonic acid calcium powder
End is configured to after 450mL mass fractions are 30% wooden calcium sulfonate's aqueous solution, be added to blender, three mouthfuls of dropping funel
In flask, after leading to nitrogen exclusion air to three-necked flask, the potassium hydroxide solution that mass fraction is 40% is added into three-necked flask
It is 9 to adjust pH, stirs 15min, obtains alkaline solution；It counts in parts by weight, to the four-hole boiling flask with reflux and blender
50 parts of azelaic acids of middle addition, 65 parts of neopentyl glycols, 35 parts of biological lubricants, 25 parts of above-mentioned alkaline solutions start under nitrogen protection
Blender is stirred with the rotating speed of 230r/min, is heated to 85 DEG C to four-hole boiling flask, insulated and stirred reaction is until reflux
Device is no longer discharged, and removes reflux, and 25 parts of carbon coating copper nano particles, 20 parts of calcium phosphate, heat preservation is added to four-hole boiling flask
50min is stirred, discharging obtains wear-resisting anti-hardening lubricating grease.
The lubricating grease that comparative example is produced with Yangzhou company is as a comparison case to wear-resisting anti-hardening produced by the present invention
Lubricating grease in lubricating grease and comparative example is detected, and testing result is as shown in table 1：
Dropping point is tested
Reference standard GB/T3498-2008 is tested.
Work cone penetration test reference standard GB/T269 is tested.The cone penetration that works is smaller, shows grease thickener
Thickening performance it is better.
Oxidation stability test reference standard SH/T0325 is tested.Oxidation stability is smaller, shows the anti-of lubricating grease
Oxidation susceptibility is better.
Stencil oil-dividing test reference standard SH/T0324 is tested.Stencil oil-dividing value is smaller, shows the colloid of lubricating grease
Stability is better.
Anticorrosive property test reference standard GB/T5018-2008 is tested.
Water leaching number of dropouts test reference standard SH/T0109 is tested.Water leaching number of dropouts is smaller, shows the anti-of lubricating grease
It is aqueous can be better.
1 performance measurement result of table
According to data in table 1 it is found that wear-resisting anti-hardening lubricating grease produced by the present invention, have splendid inoxidizability, extreme pressure property,
Wearability, colloid stability and water proofing property etc. can be competent in the harsh working condition such as high temperature, high speed, high load capacity, more water, should
Lubricant grease is with good economic efficiency and social benefit.
Claims (7)
1. a kind of wear-resisting anti-hardening preparation of greases method, it is characterised in that specifically preparation process is：
（1）It counts in parts by weight, 30~40 parts of citric acid solutions is mixed with 20~25 parts of nitrate trihydrate copper and are placed in beaker, it will
Beaker is placed in water-bath, heat temperature raising, stirs to get copper citrate gel, and copper citrate gel is placed in baking oven, heating
Heating, is dried to obtain copper citrate xerogel, is put into hermetic bag and preserves；
（2）It takes 15~18g copper citrates xerogel, 32~35g oleic acid, 50~55g heisuojin to be mixed to get explosive, explosive is filled
Enter in sealed plastic bag, sealed plastic bag connects a lead, and it is that 50~60L is close that sealed plastic bag is suspended on volume with lead
Container center is closed, nitrogen and argon gas are filled with into closed container, ignition charge is stood, and collection obtains carbon coating copper nano particles；
（3）Yeast dry powder is mixed with organic extract liquid, is put into separatory funnel, is stood, subnatant is removed, upper liquid is taken to be put into
In distilling apparatus, heat temperature raising, distillation obtains microbial grease；
（4）Microbial grease, ethyl palmitate, diphenylamines, lithium amide are mixed and be put into reaction kettle, heating water bath heating is protected
Temperature reaction, obtains esterification products, esterification products is put into supercentrifuge and are centrifuged, and stratification removes supernatant liquid, obtains
Lower layer's biological lubricant crude product, biological lubricant crude product is placed in distilling apparatus, heat temperature raising, and distillation is to there is no liquid steamings
Go out, obtains biological lubricant；
（5）Wooden calcium sulfonate 20~30min of solid abrasive is obtained into lignosulfonic acid calcium powder, lignosulfonic acid calcium powder is configured to
After 400~450mL wooden calcium sulfonates aqueous solution, be added to blender, dropping funel three-necked flask in, to three-necked flask
After logical nitrogen excludes air, potassium hydroxide solution adjusting pH is added into three-necked flask, stirs to get alkaline solution；
（6）Count in parts by weight, into the four-hole boiling flask with reflux and blender be added 40~50 parts of azelaic acids, 60~
65 parts of neopentyl glycols, 30~35 parts of biological lubricants, 20~25 parts of above-mentioned alkaline solutions start blender under nitrogen protection, with
The rotating speed of 200~230r/min is stirred, and to four-hole boiling flask heat temperature raising, insulated and stirred reaction is until reflux no longer goes out
Water removes reflux, 20~25 parts of carbon coating copper nano particles, 10~20 parts of calcium phosphate is added to four-hole boiling flask, heat preservation is stirred
It mixes, discharging obtains wear-resisting anti-hardening lubricating grease.
2. the wear-resisting anti-hardening preparation of greases method of one kind according to claim 1, it is characterised in that：Step（1）Institute
The mass fraction for the citric acid solution stated is 20%, and temperature is 80~90 DEG C after heat temperature raising, and mixing time is 40~50min, is added
Temperature is 100~110 DEG C after heat heating, and drying time is 6~7h.
3. the wear-resisting anti-hardening preparation of greases method of one kind according to claim 1, it is characterised in that：Step（2）Institute
The volume ratio of the nitrogen and argon gas stated is 3 ︰ 1, and time of repose is 10~15min.
4. the wear-resisting anti-hardening preparation of greases method of one kind according to claim 1, it is characterised in that：Step（3）Institute
The yeast dry powder stated is 1 ︰ 10 with organic extract liquid mixing quality ratio, and organic extract liquid is 2 ︰ by volume by chloroform, methanol, water
1 ︰ 2 is mixed, and time of repose is 20~30min, and temperature is 90~100 DEG C after heat temperature raising, and distillation time is 4~5h.
5. the wear-resisting anti-hardening preparation of greases method of one kind according to claim 1, it is characterised in that：Step（4）Institute
Microbial grease, ethyl palmitate, diphenylamines, the lithium amide mixing quality ratio stated are 2 ︰, 5 ︰, 3 ︰ 1, temperature after heating water bath heating
It it is 60~70 DEG C, the insulation reaction time is 2~3h, and supercentrifuge rotating speed is 2000~2200r/min, and rotating speed centrifugation time is
15~20min, temperature is 70~80 DEG C after heat temperature raising.
6. the wear-resisting anti-hardening preparation of greases method of one kind according to claim 1, it is characterised in that：Step（5）Institute
The mass fraction for the wooden calcium sulfonate's aqueous solution stated is 30%, and the mass fraction of potassium hydroxide solution is 40%, and it is 8~9 to adjust pH,
Mixing time is 10~15min.
7. the wear-resisting anti-hardening preparation of greases method of one kind according to claim 1, it is characterised in that：Step（6）Institute
Temperature is 80~85 DEG C after the heat temperature raising stated, and the insulated and stirred time is 40~50min.
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| CN110453265A (en) * | 2019-07-25 | 2019-11-15 | 刘军伟 | A kind of preparation method of aluminium alloy anode oxide film hole sealing agent |
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