CN109679736A - A kind of high temperature thermal reversibility complex soap grease and preparation method thereof - Google Patents
A kind of high temperature thermal reversibility complex soap grease and preparation method thereof Download PDFInfo
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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
- C10M169/02—Mixtures of base-materials and thickeners
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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
- 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
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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
- C10M2203/00—Organic non-macromolecular hydrocarbon compounds and hydrocarbon fractions as ingredients in lubricant compositions
- C10M2203/10—Petroleum or coal fractions, e.g. tars, solvents, bitumen
- C10M2203/102—Aliphatic fractions
- C10M2203/1025—Aliphatic fractions 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
- C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
- C10M2205/02—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
- C10M2205/028—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers containing aliphatic monomers having more than four carbon atoms
- C10M2205/0285—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers containing aliphatic monomers having more than four carbon atoms 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
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/10—Carboxylix acids; Neutral salts thereof
- C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
- C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
- C10M2207/126—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids monocarboxylic
- C10M2207/1265—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids monocarboxylic used as thickening agent
-
- 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
- C10M2207/10—Carboxylix acids; Neutral salts thereof
- C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
- C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
- C10M2207/128—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids containing hydroxy groups; Ethers thereof
- C10M2207/1285—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids containing hydroxy groups; Ethers thereof used as thickening agents
-
- 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
- C10M2207/10—Carboxylix acids; Neutral salts thereof
- C10M2207/14—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings
- C10M2207/141—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings monocarboxylic
- C10M2207/1415—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings monocarboxylic used as thickening agent
-
- 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
- C10M2227/00—Organic non-macromolecular compounds containing atoms of elements not provided for in groups C10M2203/00, C10M2207/00, C10M2211/00, C10M2215/00, C10M2219/00 or C10M2223/00 as ingredients in lubricant compositions
- C10M2227/09—Complexes with metals
-
- 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
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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
- C10N2030/12—Inhibition of corrosion, e.g. anti-rust agents or anti-corrosives
-
- 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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Abstract
The present invention relates to a kind of high temperature thermal reversibility complex soap greases, raw material includes linear saturated fatty acids, aromatic acid, aluminium isopropoxide tripolymer, base oil and water, the wherein preferred stearic acid of linear saturated fatty acids, the preferred benzoic acid of aromatic acid, base oil is one or both of hydrorefined mineral oils or synthetic oil, the preferred distilled water of water.In the present invention, weigh various components, according to preparation method finished product, in preparation process, it is completely melt organic acid, guarantees that aluminium isopropoxide tripolymer is completely dissolved, water is added to promote to form stable organic acid aluminium soap, high temperature refining forms uniform fibre structure, and finished product obtained has high dropping point, thermal reversibility, excellent mechanical stability and rust-preventing characteristic.
Description
Technical field
It is especially a kind of to be rich in answering for surface active agent wastewater for degrading the invention belongs to lubricating grease manufacturing technology field
Combined bacteria agent and preparation method thereof.
Background technique
Composite aluminum base grease is the Hmp grease of generally acknowledged better performances, has the higher dropping point, excellent greater than 260 DEG C
Good colloid stability, mechanical stability, chemical stability and water-resistance especially has good pumping, is suitable for collection
The conveying and lubrication of middle lubricating system, while there is preferable cost performance.Therefore, composite aluminum base grease is in metallurgy, mechanical, change
The high temperature lubricatings such as work, food processing field has been widely used.
Composite aluminum base grease patent report starts from the early 1950s, but not having for a long time since key technology is not broken through
Obtain valuable industrial application.In recent years composite aluminum base can be made with Directly saponification in the aluminum isopropoxide (or tripolymer) found
Rouge simplifies production technology, while stable product quality, and price is relatively cheap, quickly grows over the past decade.90 years 20th century
In generation, just aluminum complex grease accounted for 7.8% or so of National Lubricating Grease total output, accounted for national lubricating grease total output in Canada
The Europe 11.8%, NLGI (National Lubricating Grease association) member state accounts for 7.6% or so, and China only accounts for lubricating grease total output
3.7% or so, far behind developed country, so, aluminum complex grease will become the main of China's lubricating grease development from now on
One of kind.
Composite aluminum base grease is to react the compound aluminium soap generated with aluminum contained compound using two or more organic acids to be
The lubricating grease of thickening agent.Or so the 1950s, people just have realized that the aluminium base two with different organic acids anion
Soap can form colloform texture in the oil, can be used for grease thickener, ink filler etc..Since higher fatty acids is water-soluble
Poor, the Al (OH) of property3It is low to be insoluble in water, reactivity, generally (such as: hard using water-soluble aluminum salt and water-soluble organic acid metallic soap
Resin acid sodium) through metathesis reaction prepare aluminium soap.However, change method does not separate that close washing difficult there is only aluminium soap, wastewater flow rate is big, environment
Seriously polluted disadvantage, and contain aluminium salt hydrolysate in the aluminium soap prepared.Jones in 1949 etc. has invented a kind of using low
The method of grade aluminium alcoholates (such as: aluminium methoxide, aluminium ethylate, aluminium isopropoxide) and organic acid reaction preparation aluminium salt；Patent USP 2,654,
710, which provide a kind of react in aqueous solution using organic acid with water-soluble aluminum salt (such as: aluminum sulfate, aluminum nitrate), prepares aluminium salt
Method, and will separation, it is dry after aluminium soap be applied to thickening polysiloxanes and prepare synthetic fat；USP 2,599,553,USP 2,
719,826, USP 2,768,138 in aqueous solution by mixing water insoluble metallic soap (such as: soda soap) containing different anions with
Water-soluble aluminum salt (such as: aluminum sulfate, aluminum nitrate) mixing co-precipitation prepares the synthetic method of compound aluminium soap, and is applied to high drop
It selects, water-resistance grease thickener.However aluminium-base grease is prepared by the method for prefabricated soap, since aluminium soap fusing point is high,
Difficulties in dispersion in base oil, need 221 DEG C at rouge temperature.To overcome the above disadvantages, patent USP 3,345,291 provide
One kind is (main with mixed organic acid using rudimentary aluminium alcoholates (mainly including aluminium ethylate, aluminium propoxide, aluminium isopropoxide etc.) in base oil
It is made of higher fatty acids and aromatic acid) reaction prepares the synthetic method of aluminium soap and composite aluminum base grease.Further, patent
USP 3,591,505 also provide one kind in base oil using aluminum alkoxide (butoxy aluminium, aluminum isopropoxide) and two kinds not
The synthetic method of composite aluminum base grease is prepared with mixture of carboxylic acids saponification, composite aluminum base grease obtained has high dropping point,
It is lubricated suitable for ball bearing.Rudimentary aluminium alcoholates prices various in early days limit aluminium-base grease production.Later, with trimerization
The large-scale industrial production of body aluminium (aluminium isopropoxide) becomes the aluminum complex grease mainly side of preparation with tripolymer aluminium soap organic acid
Method, a large amount of patents of invention (USP 3,620,975, USP 3,776,846, USP 3,843,528, USP about aluminum complex grease
4,132,658, USP 5,037,563) it is all that compound aluminium soap is prepared by tripolymer aluminium soapization.Domestic composite aluminum base grease
Research is started late, composite aluminum base grease patent report only few in number at present.Wherein, Chinese patent CN 1,900,
244A, CN 101117604 each provides one kind and synthesizes compound aluminium soap with stearic acid, benzoic acid and tripolymer aluminium, and further
The method that addition high alkaline calcium sulfonate prepares composite aluminum base grease, and find in the case where additive is not added, basic rouge has
Good water-resistance, rust-preventing characteristic, extreme pressure property, mechanical stability and high temperature colloid stability.In addition, patent USP 3,511,781
It was found that adding a certain amount of fragrant acid metal salt in aluminium-base grease can be improved its stability.
In conclusion the dropping point of complex soap grease, mechanical stability and rust-preventing characteristic etc. still can advanced optimize, warp
Retrieval is crossed, does not find patent document same as the present invention.
Summary of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide be saponified higher aliphatic using aluminium isopropoxide tripolymer
Acid and aromatic acid mixed acid and it is manufactured have high dropping point, one kind that thermal reversibility is good, mechanical stability and rust-preventing characteristic are excellent
High temperature thermal reversibility complex soap grease.
The technical solution adopted by the present invention is that:
A kind of high temperature thermal reversibility complex soap grease, it is characterised in that: following including being mixed according to weight percent
Component:
Further more, the molar ratio of organic acid total acidic group and aluminium isopropoxide tripolymer are as follows: 5~6:1.
Further more, the linear saturated fatty acids are any one in stearic acid or ten dihydroxystearic acids.
Further more, the aromatic acid is any one in benzoic acid or phthalic acid.
Further more, the molar ratio of the total acidic group of organic acid and aluminium isopropoxide tripolymer is 5.3~5.8:1, the straight chain is full
It is stearic acid with fatty acid, the aromatic acid is benzoic acid, and the water is distilled water.
It is a further object to provide a kind of preparation method of high temperature thermal reversibility complex soap grease, features
It is: the following steps are included:
(1) first part's base oil is added in the reaction vessel, heats up and linear saturated fatty acids and aromatic acid is added, to
Aluminium isopropoxide tripolymer is added after being completely melt in each component, keeps the temperature one end time；
(2) water is added after heating up, adds persistently overheating during water, second part base oil is then added, refines one after heating
The section time；
(3), in the step (2) middle modulation that remaining base oil is added and carries out consistency, preparation is completed.
Further more, the weight of step (1) first part's base oil accounts for the 60~70% of base oil total weight, it is warming up to
Linear saturated fatty acids and aromatic acid are added after 70~85 DEG C, aluminium isopropoxide tripolymer is added after stirring to complete melt in constant temperature,
Temperature keeps the temperature 20~40 minutes under conditions of being 70~90 DEG C.
Further more, (2) the water supply way is step: the product of step (1) being warming up to 125~135 DEG C, keeps 10~20
Slowly add water after minute, water is added to be to slowly warm up to 160~170 DEG C in the process.
Further more, (2) step is warming up to 190~200 DEG C after the second part base oil is added, high temperature refining 0.5~2
Hour.
Further more, step (3) after the modulation of the consistency through supercooling, shearing, homogeneous, degassing and it is filling after obtain finished product.
The advantages and positive effects of the present invention are:
In the present invention, raw material includes linear saturated fatty acids, aromatic acid, aluminium isopropoxide tripolymer, base oil and water, wherein
The preferred stearic acid of linear saturated fatty acids, the preferred benzoic acid of aromatic acid, base oil are in hydrorefined mineral oils or synthetic oil
One or two, the preferred distilled water of water.It in preparation process, is completely melt organic acid, guarantees that aluminium isopropoxide tripolymer is complete
Dissolution adds water to promote to form stable organic acid aluminium soap, and high temperature refining forms uniform fibre structure, and finished product obtained has
High dropping point, thermal reversibility, excellent mechanical stability and rust-preventing characteristic.
Specific embodiment
Below with reference to embodiment, the present invention is further described, following embodiments be it is illustrative, be not restrictive,
It cannot be limited the scope of protection of the present invention with following embodiments.
A kind of high temperature thermal reversibility complex soap grease, innovation of the invention are: including mixing according to weight percent
Following components:
Wherein, the molar ratio of organic acid total acidic group and aluminium isopropoxide tripolymer are as follows: 5~6:1.Linear saturated fatty acids are
C16-C20Any one in linear saturated fatty acids, preferably stearic acid or ten dihydroxystearic acids.Aromatic acid is benzoic acid
Or any one in phthalic acid.Base oil is the mixture of one of refined mineral oil, synthetic oil or both.
Preferred scheme is: the molar ratio of the total acidic group of organic acid and aluminium isopropoxide tripolymer is 5.3~5.8:1, straight chain
Saturated fatty acid is stearic acid, and aromatic acid is benzoic acid, and water is distilled water.
The preparation method of above-mentioned high temperature thermal reversibility complex soap grease the following steps are included:
(1) first part's base oil is added in the reaction vessel, heats up and linear saturated fatty acids and aromatic acid is added, to
Aluminium isopropoxide tripolymer is added after being completely melt in each component, keeps the temperature one end time；
(2) water is added after heating up, adds persistently overheating during water, second part base oil is then added, refines one after heating
The section time；
(3), in the step (2) middle modulation that remaining base oil is added and carries out consistency, preparation is completed.
Wherein, the weight of step (1) first part's base oil accounts for the 60~70% of base oil total weight, is warming up to
Linear saturated fatty acids and aromatic acid are added after 70~85 DEG C, aluminium isopropoxide tripolymer is added after stirring to complete melt in constant temperature,
Temperature keeps the temperature 20~40 minutes under conditions of being 70~90 DEG C.
(2) the water supply way is step: the product of step (1) being warming up to 125~135 DEG C, is kept for 10~20 minutes
Slowly add water afterwards, water is added to be to slowly warm up to 160~170 DEG C in the process.
(2) step is warming up to 190~200 DEG C after the second part base oil is added, high temperature is refined 0.5~2 hour.
Further more, (requirement of 100 DEG C of dynamic viscosities can be in 10cSt or more, according to using for the modulation of the step (3) consistency
The operating condition of lubricating grease determines viscosity) by supercooling, shearing 1~3 hour, homogeneous, degassing and it is filling after obtain finished product.
The molar ratio of linear saturated fatty acids and aromatic acid is that aromatic acid is more than fatty acid, the composite aluminum base produced in this way
Grease dropping point is high, and mechanical stability is good.Al atomic ratio organic acid total mole number is excessive in aluminium isopropoxide tripolymer, is passed through
A small amount of rock-steady structure for adding water that unreacted aluminium isopropoxide tripolymer can be made to become hydroxyl.
In the above process, C is added16-C20When linear saturated fatty acids, aromatic acid, constant temperature stirring not only guarantees that organic acid is complete
Running down, and avoid its decomposition.When aluminium isopropoxide tripolymer is added, 20~40 minutes are kept the temperature, guarantees that it is completely dissolved.Below
Be warming up to 125~135 DEG C and constant temperature 10~20 minutes, be in order to guarantee reaction carry out.Slowly plus the process of water continues 1~2
Hour, it is to guarantee that one of aluminum alkoxide of production can be slowly converting to hydroxy Al that 160~170 DEG C are warming up to after adding, this
Sample just forms stable organic acid aluminium soap.Then high temperature refining 0.5~2 hour can shape under the conditions of 190~200 DEG C of temperature
At the uniform composite aluminum base grease of fibre structure.As shown in the above, saponification is low-temperature saponification and medium temperature saponification two
Holding saponification process, (the production technology saponification temperature of general composite aluminum base grease is 100-120 DEG C, and medium temperature saponification is 160-180
DEG C, high temperature refining temperature is 200-220 DEG C).
Embodiment 1
The 350SN base oil of 1000g is added in normal pressure saponification kettle, stirring is warming up to 70 DEG C, respectively stiffened resin acid 103g,
Benzoic acid 46g, constant temperature are stirred to being completely melt.Then aluminium isopropoxide tripolymer 100g is added, temperature is maintained at 90 DEG C of half an hour,
125 DEG C are warming up to, constant temperature 15 minutes, slowly adds water 6g, slowly heats up, material retrogradation.160 DEG C were warming up to by 1.5 hours, is added
The 150BS for entering base oil 200g is heated to 200 DEG C, and high temperature is refined 1 hour.Then material is poured into reconciliation kettle, remaining base is added
The 150BS of the 350SN and 250g of plinth oil 100g carries out the modulation of consistency, cooling, shearing 2 hours, homogeneous, degassing, it is filling to get
High temperature thermal reversibility complex soap grease.
Embodiment 2
The 500N base oil of 1000g is added in normal pressure saponification kettle, stirring is warming up to 85 DEG C, respectively stiffened resin acid 103g,
Benzoic acid 46g, constant temperature are stirred to being completely melt.Then aluminium isopropoxide tripolymer 100g is added, temperature is maintained at 70 DEG C of half an hour,
135 DEG C are warming up to, constant temperature 15 minutes, slowly adds water 6g, slowly heats up, material retrogradation.170 DEG C were warming up to by 1.5 hours, is added
The 150BS for entering base oil 200g is heated to 190 DEG C, and high temperature is refined 1 hour, and material is then poured into reconciliation kettle, and remaining base is added
The 150BS of the 500N and 250g of plinth oil 100g carries out the modulation of consistency, cooling, shearing 2 hours, homogeneous, degassing, it is filling to get
High temperature thermal reversibility complex soap grease.
Embodiment 3
Normal pressure saponification kettle in be added 250g 500N and 650g 150BS base oil, stirring be warming up to 80 DEG C, respectively plus
Stearic acid 103g, fragrant acid+benzoic acid 46g, constant temperature are stirred to being completely melt.Then aluminium isopropoxide tripolymer 100g, temperature is added
80 DEG C of half an hour are maintained at, 130 DEG C is warming up to, constant temperature 15 minutes, slowly adds water 6g, slowly heat up, material retrogradation.By 1.5
Hour is warming up to 165 DEG C, and the 150BS of base oil 150g is added, and is heated to 195 DEG C, high temperature is refined 1 hour and then pours into material
Reconciling kettle, the 150BS that remaining base oil 250g is added carries out the modulation of consistency, cooling, shearing 2 hours, and it is homogeneous, degassing, filling,
Up to high temperature thermal reversibility complex soap grease.
Embodiment 4
The 150BS base oil of 850g is added in normal pressure saponification kettle, stirring is warming up to 85 DEG C, respectively stiffened resin acid 103g,
Dibenzoic acid 46g, constant temperature are stirred to being completely melt.Then aluminium isopropoxide tripolymer 100g is added, temperature is maintained at 70 DEG C half small
When, 128 DEG C are warming up to, constant temperature 15 minutes, slowly plus water 6g, slowly heating, material retrogradation were warming up to 168 by 1.5 hours
DEG C, the 150BS of base oil 150g is added, is heated to 194 DEG C, high temperature refines 1 hour and material is then poured into reconciliation kettle, is added
The 150BS of remaining base oil 250g carries out the modulation of consistency, cooling, shearing 2 hours, homogeneous, degassing, filling to get high warm
Invertibity complex soap grease.
Embodiment 5
Normal pressure saponification kettle in be added 250g 500N and 650g 150BS base oil, stirring be warming up to 82 DEG C, respectively plus
Stearic acid 120g, dibenzoic acid 64g, constant temperature are stirred to being completely melt.Then aluminium isopropoxide tripolymer 120g is added, temperature is kept
In 85 DEG C of half an hour, 131 DEG C are warming up to, constant temperature 15 minutes, slowly adds water 6g, slowly heats up, material retrogradation.By 1.5 hours
162 DEG C are warming up to, the 150BS of base oil 150g is added, is heated to 195 DEG C, high temperature refines 1 hour and material is then poured into tune
And kettle, the 150BS that remaining base oil 250g is added carry out the modulation of consistency, and it is cooling, shearing 2 hours, it is homogeneous, degassing, filling, i.e.,
Obtain high temperature thermal reversibility complex soap grease.
Embodiment 6
The PAO-10 base oil of 850g is added in normal pressure saponification kettle, stirring is warming up to 78 DEG C, respectively stiffened resin acid 120g,
Dibenzoic acid 64g, constant temperature are stirred to being completely melt.Then aluminium isopropoxide tripolymer 120g is added, temperature is maintained at 88 DEG C half small
When, 127 DEG C are warming up to, constant temperature 15 minutes, slowly plus water 6g, slowly heating, material retrogradation were warming up to 169 by 1.5 hours
DEG C, the PAO-10 of base oil 150g is added, is heated to 193 DEG C, high temperature is refined 1 hour.Then material is poured into reconciliation kettle, be added
The PAO-10 of remaining base oil 200g carries out the modulation of consistency, cooling, shearing 2 hours, homogeneous, degassing, filling to get high warm
Invertibity complex soap grease.
The present invention is prepared again in base oil by the mixed acid that aluminium isopropoxide tripolymer is saponified higher fatty acids and aromatic acid
Aluminium-base grease is closed, not additivated basic rouge has high dropping point, mechanical stability and excellent rustless property, is suitable for
Prepare high temperature resistant lubricating grease.The performance test results of composite aluminum base grease prepared by embodiment 1-6 are as shown in table 1.
Table 1: the end properties test result of embodiment 1-6 preparation
The change rate for extending work cone penetration embodies the mechanical stability of lubricating grease, and copper corrosion embodies the antirust of lubricating grease
Property.Extend within the change rate 10% of work cone penetration and illustrates that the mechanical stability of lubricating grease is superior, copper corrosion 1a, 1b explanation
Rust-preventing characteristic is preferable.
The specific implementation step of common clad aluminum is as follows:
Embodiment 7:
The 150BS base oil of 1000g is added in normal pressure saponification kettle, stirring is warming up to 60 DEG C, respectively stiffened resin acid 120g,
Benzoic acid 5g, 12- hydroxy stearic acid 70g, constant temperature are stirred to being completely melt.Sodium metaaluminate 15g is added, temperature is maintained at 105 DEG C
Saponification 2 hours is then heated to 200 DEG C, and high temperature is refined 1 hour.Material is poured into reconciliation kettle, remaining base oil is added
700g150BS carries out the modulation of consistency, cooling, shearing 2 hours, homogeneous, degassing, filling to get composite aluminum base grease.
Embodiment 8:
850g PAO-10 base oil is added in normal pressure saponification kettle, stirring is warming up to 70-85 DEG C, respectively stiffened resin acid
120g, benzoic acid 50g, constant temperature are stirred to being completely melt, aluminium isopropoxide tripolymer 110g temperature is then added and is maintained at 70-90 DEG C
Half an hour is warming up to 125-135 DEG C, and constant temperature 60 minutes, slowly plus water 6g, slowly heating, material retrogradation heated up 190-200 DEG C,
High temperature is refined 1 hour, and material is then poured into reconciliation kettle, and the modulation that residue base oil 200g PAO-10 carries out consistency is added, cold
But, shear 2.5 hours, it is homogeneous, degassing, filling to get composite aluminum base grease.
Table 2: the end properties test result of embodiment 7-8 preparation
Embodiment 7,8 is the preparation process and formula of the composite aluminum base grease of the prior art, from the property of table 1 and table 2
Can Comparative result it can be concluded that, the clad aluminum dropping point that the technique of example 1-6 is made is higher than 30-40 DEG C of prior art, before and after high temperature
The appearance of lubricating grease also changes less, illustrates that thermal reversibility is good.
Extend the change rate comparison of work cone penetration, new preparation method is also slightly better than existing preparation method, shows this theory
The lubricating grease mechanical stability of the preparation method preparation of bright book is superior, and copper corrosion is identical as prior art, copper corrosion
It as a result is all 1a, display rust-preventing characteristic is equally good.
Claims (10)
1. a kind of high temperature thermal reversibility complex soap grease, it is characterised in that: including according to weight percent mix with the following group
Point:
2. a kind of high temperature thermal reversibility complex soap grease according to claim 1, it is characterised in that: the organic acid is total
The molar ratio of acidic group and aluminium isopropoxide tripolymer are as follows: 5~6:1.
3. a kind of high temperature thermal reversibility complex soap grease according to claim 2, it is characterised in that: the linear saturation
Fatty acid is any one in stearic acid or ten dihydroxystearic acids.
4. a kind of high temperature thermal reversibility complex soap grease according to claim 3, it is characterised in that: the aromatic acid is
Any one in benzoic acid or phthalic acid.
5. a kind of high temperature thermal reversibility complex soap grease according to claim 4, it is characterised in that: the organic acid is total
The molar ratio of acidic group and aluminium isopropoxide tripolymer is 5.3~5.8:1, and the linear saturated fatty acids are stearic acid, the fragrance
Acid is benzoic acid, and the water is distilled water.
6. a kind of preparation method of the high temperature thermal reversibility complex soap grease as described in any one of Claims 1 to 5,
It is characterized in that: the following steps are included:
(1) first part's base oil is added in the reaction vessel, heats up and linear saturated fatty acids and aromatic acid is added, to each group
Divide and aluminium isopropoxide tripolymer is added after being completely melt, keeps the temperature one end time；
(2) water is added after heating up, adds persistently overheating during water, second part base oil is then added, when refining one section after heating
Between；
(3), in the step (2) middle modulation that remaining base oil is added and carries out consistency, preparation is completed.
7. a kind of high temperature thermal reversibility complex soap grease according to claim 6, it is characterised in that: step is (1) described
The weight of first part's base oil accounts for the 60~70% of base oil total weight, and linear saturation fat is added after being warming up to 70~85 DEG C
Aluminium isopropoxide tripolymer is added in acid and aromatic acid, constant temperature after stirring to complete melt, temperature is kept the temperature under conditions of being 70~90 DEG C
20~40 minutes.
8. a kind of high temperature thermal reversibility complex soap grease according to claim 6, it is characterised in that: step is (2) described
Water supply way is: the product of step (1) being warming up to 125~135 DEG C, keeps 10~after twenty minutes slowly plus water, during adding water
It is to slowly warm up to 160~170 DEG C.
9. a kind of high temperature thermal reversibility complex soap grease according to claim 6, it is characterised in that: step is (2) described
Second part base oil is warming up to 190~200 DEG C after being added, high temperature is refined 0.5~2 hour.
10. a kind of high temperature thermal reversibility complex soap grease according to claim 6, it is characterised in that: step is (3) described
After the modulation of consistency through supercooling, shearing, homogeneous, degassing and it is filling after obtain finished product.
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| WO2021217908A1 (en) * | 2020-04-28 | 2021-11-04 | 江南大学 | Food-grade lubricating grease and preparation method therefor |
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