CN107828478A - A kind of Composite calcium naphthenate base lubricant composition and preparation method thereof - Google Patents
A kind of Composite calcium naphthenate base lubricant composition and preparation method thereof Download PDFInfo
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- CN107828478A CN107828478A CN201710975739.8A CN201710975739A CN107828478A CN 107828478 A CN107828478 A CN 107828478A CN 201710975739 A CN201710975739 A CN 201710975739A CN 107828478 A CN107828478 A CN 107828478A
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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
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- 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
- C10M2201/08—Inorganic acids or salts thereof
- C10M2201/084—Inorganic acids or salts thereof containing sulfur, selenium or tellurium
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- 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
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- 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
- C10M2201/087—Boron oxides, acids or salts
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- 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
- C10M2203/1006—Petroleum or coal fractions, e.g. tars, solvents, bitumen used as base material
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- 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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- 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
- C10M2207/121—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms
- C10M2207/122—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms monocarboxylic
- C10M2207/1225—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms monocarboxylic used as thickening agent
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- 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
- C10M2207/121—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms
- C10M2207/123—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms polycarboxylic
- C10M2207/1236—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms polycarboxylic used as thickening agent
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- 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
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- 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
- C10M2207/142—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings polycarboxylic
- C10M2207/1426—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings polycarboxylic used as thickening agent
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- 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
- C10M2207/144—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings containing hydroxy groups
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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
- C10M2207/16—Naphthenic acids
- C10M2207/166—Naphthenic acids used as thickening agents
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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
- C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
- C10M2219/04—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
- C10M2219/044—Sulfonic acids, Derivatives thereof, e.g. neutral salts
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- 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
- 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 Composite calcium naphthenate base lubricant composition and preparation method thereof；Use the formula and its preparation technology for main stock thickener into the Composite calcium naphthenate base lubricant composition of fat such as basicity calcium naphthenate, Aromatic carboxylic calcium and alkyl benzene calcium sulfonate, small molecule fatty acid calcium or inorganic acid calcium, including following components (by percentage to the quality)：(1) content for the overbased calcium alkyl-salicylate that base number is 300~420mgKOH/g is 30~60%；(2) content of Aromatic carboxylic calcium is 1~10%；(3) content of alkyl benzene calcium sulfonate is 1~10%；(4) content of small molecule fatty acid calcium or inorganic acid calcium is 1~10%；(5) lubricating base oil, surplus.The lubricating grease high comprehensive performance prepared using the present invention, mainly has prominent heat-resisting quantity, excellent extreme pressure anti-wear and water-resistance etc., the lubrication available for the more wetting system positions of high-temperature high-load.
Description
Technical field
The invention belongs to technical field of lubricating grease, it is more particularly to a kind of using basicity calcium naphthenate, Aromatic carboxylic calcium and
Alkyl benzene calcium sulfonate, small molecule fatty acid calcium or inorganic acid calcium etc. are composition of the main stock thickener into fat.
Background technology
It is similar with the naming method of complex calcium sulfonate grease, using basicity calcium naphthenate and other organic acids or inorganic
The lubricating grease that sour calcium is combined is referred to as Composite calcium naphthenate base lubricating grease.Complex calcium sulfonate grease is with alkaline sulfoacid
Calcium is primary raw material, and Composite calcium naphthenate base lubricating grease is using basicity calcium naphthenate as primary raw material.Basicity calcium naphthenate is also
A kind of detergent for lubricating oil, typically pass through aphthenic acids (also known as petroleum acids) warp and Ca (OH)2React, be carbonated contour alkalization technology
And be made, aphthenic acids is the accessory substance of petroleum refining, and raw material is easy to get.
Patent CN104293449, CN103695137 and CN103627496 mention a kind of Composite calcium naphthenate base lubrication
Oil/fat composition and preparation method thereof, but higher fatty acid calcium is all included in its formula, highest refining temperature in its preparation technology
For 180~230 DEG C, product of the present invention is related to one kind and uses basicity calcium naphthenate, Aromatic carboxylic calcium and alkyl benzene sulphonate
Calcium, small molecule fatty acid calcium or inorganic acid calcium etc. are composition of the main stock thickener into fat, not comprising higher fatty acid calcium, and
The highest refining temperature of preparation technology is 220~250 DEG C.
The present invention is led to for the lubrication occasion of the more water of high-temperature high-load such as metallurgy, cement, ceramics, textile and paper industry
Cross the suitable formula of screening and technique, develop it is a kind of using basicity calcium naphthenate, Aromatic carboxylic calcium and alkyl benzene calcium sulfonate,
Small molecule fatty acid calcium or inorganic acid calcium etc. are that new the having of main stock thickener into fat protrudes heat-resisting quantity, excellent extreme pressure resists
The Composite calcium naphthenate base lubricant composition of mill property and water-resistance grade high performance.
The content of the invention
It is an object of the invention to provide a kind of new having to protrude heat-resisting quantity, excellent extreme pressure anti-wear and water-resistance etc.
The formula and preparation method of high performance Composite calcium naphthenate base lubricating grease.The present invention passes through lot of experiments screening formula and technique
A kind of new lubricant composition is made, meets the requirement of high temperature, high load capacity and more water lubrication occasions.
The technology of the present invention is as follows：
A kind of Composite calcium naphthenate base lubricant composition, its component and weight/mass percentage composition are as follows：
(1) content for the overbased calcium alkyl-salicylate that base number is 300~420mgKOH/g is 30~60%；
(2) content of Aromatic carboxylic calcium is 1~10%；
(3) content of alkyl benzene calcium sulfonate is 1~10%.
(4) content of small molecule fatty acid calcium or inorganic acid calcium is 1~10%.
(5) lubricating base oil, surplus.
The Composite calcium naphthenate base preparation of greases technique is as follows：
(1) overbased calcium alkyl-salicylate and 35~65% base oil are mixed, transforming agent is added after stirring, it is warming up to 75~
105 DEG C, preferably 80~100 DEG C, 40~120min is kept, to material retrogradation.Determined with Fourier infrared spectrograph
In 855cm-1There is the absworption peak of vaterite-type calcium carbonate left and right.
(2) calcium hydroxide will be first added in the material obtained by (1) step, then adds Aromatic carboxylic, benzene sulfonamide
Acid, small molecule aliphatic acid or inorganic acid are reacted, and heating dehydration is to more than 200 DEG C after reaction, in temperature-rise period
Can
It is suitably added 10~30% base oil；
(3) material of (2) step is continuously heating to 220 DEG C~250 DEG C, preferably 230~240 DEG C, constant temperature stirs 5~20 points
Clock, after material retrogradation, cool down and add remaining base oil in formula, finally homogenizing etc. produces required product.
Commercially available overbased calcium alkyl-salicylate belongs to Newtonian fluid, wherein containing amorphous calcium carbonate, passes through infrared spectrum
It is 860cm to determine its characteristic peak-1Left and right.In the presence of transforming agent, amorphous calcium carbonate is changed into crystal habit presence, passes through
Infrared spectrum measurement obtains characteristic peak in 855cm-1Left and right, predominantly aragonite calcium carbonate crystal, now material is by newton body turn
Turn to non-newtonian fluid.And to the end finished product when, also still for aragonitic crystallize.
The transforming agent includes C1~C5 aliphatic acid, fatty alcohol etc. and C8~C15 alkyl benzene sulphonate and water etc., its
Reclaimed water adds simultaneously as the diluent of acid with acid, and transforming agent comprises at least a kind of acids and a kind of alcohols, acids are excellent
Select formic acid, acetic acid, propionic acid, DBSA etc., alcohols preferred alcohol, isopropanol, normal propyl alcohol, n-butanol etc..Transforming agent
It is to add the conversion for promoting calcium carbonate crystal formation in early stage conversion process, is largely overflow in last handling process from system
Go out, therefore be not included in component.
The base number of the overbased calcium alkyl-salicylate is 300~420mgKOH/g, preferably 350~420mgKOH/g, quality hundred
It is 30~60%, preferably 30~50% to divide content.
The Aromatic carboxylic is the carboxylic acid that at least 1 carboxyl is joined directly together with aromatic ring, on aromatic ring can with substituted base,
Its substituent can be alkyl, aryl, hydroxyl etc..Such as：Phthalic acid, terephthalic acid (TPA), salicylic acid etc..
The alkyl benzene sulphonate refers to C8-C15 alkyl benzene sulphonates, preferably DBSA.
The molecular weight of the small molecule aliphatic acid or inorganic acid is less than or equal to 150.Wherein, small molecule aliphatic acid can be selected from
One kind in acetic acid, ethanedioic acid, propionic acid, malonic acid, butyric acid, succinic acid etc., preferably acetic acid；Small molecule inorganic acid can be selected from
One kind in boric acid, phosphoric acid, sulfuric acid etc., preferably boric acid.
The lubricating base oil can be mineral oil, olefin oil or the mixture of the two, 100 DEG C of kinematic viscosity 10~
60mm2/ s, open flash point are more than 240 DEG C.
Embodiment
In order to screen suitable formula and technique, repeatedly failure case is experienced in laboratory, selects several successes herein
Example has carried out the evaluation of heat-resisting quantity and extreme pressure anti-wear.
The effect of the present invention is further illustrated by the following examples.However, it should be understood that the following examples are not limitations
The scope of the present invention, any change without departing from present inventive concept and scope, it is within the scope of the present invention.
Embodiment 1：
1. the overbased calcium alkyl-salicylate that 200g base numbers are 410mgKOH/g is added in 100g mineral oil, 50 are heated with stirring to
~60 DEG C, 10g n-butanols and 20g acetic acid (being diluted with suitable quantity of water) are added, continues heating stirring to 80~90 DEG C, constant temperature 60min
Material retrogradation afterwards, infrared detection have 855cm-1Absworption peak.2. calcium hydroxide 25g will be added in the material of retrogradation, then add
Phthalic acid 20g, DBSA 20g and boric acid 20g, stirring reaction 30 minutes, stirring heating draining is then proceeded to,
40g mineral oil is added after being heated to 200 DEG C.3. then, being further heated with stirring to 225~235 DEG C, the gradual retrogradation of material is permanent
After 5~10min of temperature, the stirring cooling of 60g mineral oil is added, continues homogenizing finished product lubricating grease after being cooled to less than 100 DEG C.Profit
Consistent lubricant mass percent forms：Overbased calcium alkyl-salicylate 42.2%, Aromatic carboxylic calcium 5.4%, alkyl benzene calcium sulfonate
4.5%, small molecule inorganic acid calcium 5.7%, base oil 42.2%.Obtained PERFORMANCE OF GREASES is listed in table 1.
Embodiment 2：
1. the overbased calcium alkyl-salicylate that 150g base numbers are 300mgKOH/g is added in 70g mineral oil, 50 are heated with stirring to
~60 DEG C, 10g isopropanols and 20g propionic acid (being diluted with suitable quantity of water) are added, continues heating stirring to 85~95 DEG C, constant temperature 120min
Material retrogradation afterwards, infrared detection have 855cm-1Absworption peak.2. calcium hydroxide 51g will be added in the material of retrogradation, then add
Terephthalic acid (TPA) 40.7g, DBSA 47.2g and acetic acid 37.9g, stirring reaction 30 minutes, then proceed to stirring and rise
Warm water discharge, 60g mineral oil is added after being heated to 200 DEG C.3. then, being further heated with stirring to 230~240 DEG C, material is gradual
Retrogradation, after 10~20min of constant temperature, the stirring cooling of 70g mineral oil is added, continues to be homogenized finished products after being cooled to less than 100 DEG C
Lubricating grease.Lubricating grease mass percent forms：Overbased calcium alkyl-salicylate 30%, Aromatic carboxylic calcium 10%, alkyl benzene sulphonate
Calcium 10%, small molecule inorganic acid calcium 10%, base oil 40%.Obtained PERFORMANCE OF GREASES is listed in table 1.
Embodiment 3：
1. the overbased calcium alkyl-salicylate that 300g base numbers are 420mgKOH/g is added in 120g olefin oils, agitating and heating
To 50~60 DEG C, 8g ethanol and 15g formic acid (being diluted with suitable quantity of water) are added, continues heating stirring to 75~80 DEG C, constant temperature 40min
Material retrogradation afterwards, infrared detection have 855cm-1Absworption peak.2. calcium hydroxide 4.4g will be added in the material of retrogradation, then add
Salicylic acid 4.4g, DBSA 4.7g and boric acid 3.8g, stirring reaction 30 minutes, stirring heating draining is then proceeded to,
18.5g olefin oils are added after being heated to 200 DEG C.3. then, being further heated with stirring to 240~250 DEG C, material gradually becomes
It is thick, after 5~10min of constant temperature, the stirring cooling of 46.5g olefin oils is added, continues homogenizing after being cooled to less than 100 DEG C and is made into
Product lubricating grease.Lubricating grease mass percent forms：Overbased calcium alkyl-salicylate 60%, Aromatic carboxylic calcium 1%, alkyl benzene sulphonate
Calcium 1%, small molecule inorganic acid calcium 1%, base oil 37%.Obtained PERFORMANCE OF GREASES is listed in table 1.
Embodiment 4：
1. the overbased calcium alkyl-salicylate that 240g base numbers are 400mgKOH/g is added in 80g olefin oils, agitating and heating
To 50~60 DEG C, add 10g normal propyl alcohols and 30g DBSAs (being diluted with suitable quantity of water), continue heating stirring to 95~
105 DEG C, material retrogradation after constant temperature 70min, infrared detection has 855cm-1Absworption peak.2. hydroxide will be added in the material of retrogradation
Calcium 34.2g, then add phthalic acid 27.3g, DBSA 31.7g and acetic acid 25.5g, stirring reaction 30 and divide
Clock, stirring heating draining is then proceeded to, 20g mineral oil is added after being heated to 200 DEG C.3. then, further it is heated with stirring to 220
~230 DEG C, the gradual retrogradation of material, after 10~20min of constant temperature, add the stirring cooling of 39g mineral oil, continue to be cooled to 100 DEG C with
Finished product lubricating grease is homogenized after lower.Lubricating grease mass percent forms：Overbased calcium alkyl-salicylate 50%, Aromatic carboxylic calcium
7%, alkyl benzene calcium sulfonate 7%, small molecule inorganic acid calcium 7%, base oil 29%.Obtained PERFORMANCE OF GREASES is listed in table 1.
Embodiment 5：
1. the overbased calcium alkyl-salicylate that 275g base numbers are 350mgKOH/g is added in 100g mineral oil, 50 are heated with stirring to
~60 DEG C, 10g normal propyl alcohols and 20g acetic acid (being diluted with suitable quantity of water) are added, continues heating stirring to 80~90 DEG C, constant temperature 100min
Material retrogradation afterwards, infrared detection have 855cm-1Absworption peak.2. calcium hydroxide 12.8g, Ran Houjia will be added in the material of retrogradation
Enter phthalic acid 12.2g, DBSA 14.1g and boric acid 7.5g, stirring reaction 30 minutes, then proceed to stirring and rise
Warm water discharge, 30g olefin oils are added after being heated to 200 DEG C.3. 230~240 DEG C then, are further heated with stirring to, material
Gradual retrogradation, after 5~10min of constant temperature, the stirring cooling of 55g olefin oils is added, continue homogenizing after being cooled to less than 100 DEG C and make
Obtain finished product lubricating grease.Lubricating grease mass percent forms：Overbased calcium alkyl-salicylate 55%, Aromatic carboxylic calcium 3%, alkylbenzene
Sulfoacid calcium 3%, small molecule inorganic acid calcium 2%, base oil 37%.Obtained PERFORMANCE OF GREASES is listed in table 1.
Embodiment 6：
The overbased calcium alkyl-salicylate that 225g base numbers are 400mgKOH/g is added in 100g olefin oils, is heated with stirring to
50~60 DEG C, 10g n-butanols and 20g acetic acid (being diluted with suitable quantity of water) are added, continues heating stirring to 80~90 DEG C, constant temperature
Material retrogradation after 60min, infrared detection have 855cm-1Absworption peak.2. calcium hydroxide 14.4g will be added in the material of retrogradation, so
Phthalic acid 12.2g, DBSA 28.2g and boric acid 7.5g are added afterwards, stirring reaction 30 minutes, then proceed to stir
Heating draining is mixed, 50g olefin oils are added after being heated to 200 DEG C.3. 230~240 DEG C then, are further heated with stirring to,
The gradual retrogradation of material, after 5~10min of constant temperature, the stirring cooling of 70g olefin oils is added, is continued equal after being cooled to less than 100 DEG C
Change finished product lubricating grease.Lubricating grease mass percent forms：Overbased calcium alkyl-salicylate 45%, Aromatic carboxylic calcium 3%, alkane
Base benzene sulfonic acid calcium 6%, small molecule inorganic acid calcium 2%, base oil 44%.Obtained PERFORMANCE OF GREASES is listed in table 1.
Embodiment analytical control result is as shown in table 1.
The gained PERFORMANCE OF GREASES evaluation result of 1 embodiment of table 1~6
The dropping point of general high temperature resistant lubricating grease is typically larger than 260 DEG C, and the PB values of general extreme-pressure lubricating grease are not less than 686N,
PD values are not less than 2452N, and in general water-resistant oleosol adds the cone penetration difference of water roller 1/4 to be usually more than 10.And by data in table 1
Understand, the dropping point of lubricant composition of the invention is more than 300 DEG C, and PB values are more than 834N, and PD values are not less than 3089N, add water to roll
Cylinder data be less than 5, therefore the present invention use basicity calcium naphthenate and calcium of organic acid and inorganic acid calcium etc. to be made for primary raw material
Composite calcium naphthenate grease of calcium composition, there is prominent heat-resisting quantity, excellent extreme pressure anti-wear and water-resistance etc., can expire
The lubricating requirement at the sufficient more wetting system positions of high-temperature high-load.
Claims (10)
1. Composite calcium naphthenate base lubricant composition, its component and weight/mass percentage composition are as follows：
(1) content for the overbased calcium alkyl-salicylate that base number is 300~420mgKOH/g is 30~60%；
(2) content of Aromatic carboxylic calcium is 1~10%；
(3) content of alkyl benzene calcium sulfonate is 1~10%；
(4) content of small molecule fatty acid calcium or inorganic acid calcium is 1~10%；
(5) lubricating base oil, surplus.
2. lubricant composition as claimed in claim 1, it is characterised in that the base number of overbased calcium alkyl-salicylate be 300~
420mgKOH/g, its weight/mass percentage composition are 30~60%.
3. lubricant composition as claimed in claim 1, it is characterised in that Aromatic carboxylic is at least 1 carboxyl and aromatic ring
The carboxylic acid being joined directly together, substituted base on aromatic ring, its substituent is alkyl, aryl or hydroxyl.
4. lubricant composition as claimed in claim 3, its feature is sour phthalic acid, terephthaldehyde in aromatic radical carboxylic
Acid, salicylic acid, its weight/mass percentage composition are 1~10%.
5. lubricant composition as claimed in claim 1, it is characterised in that alkyl benzene sulphonate refers to C8-C15 alkyl benzene sulphonates,
Its weight/mass percentage composition is 1~10%.
6. lubricant composition as claimed in claim 1, it is characterised in that the molecular weight of small molecule aliphatic acid or inorganic acid is small
In equal to 150；Wherein, small molecule aliphatic acid can be in acetic acid, ethanedioic acid, propionic acid, malonic acid, butyric acid, succinic acid etc.
It is a kind of；Small molecule inorganic acid can be selected from one kind in boric acid, phosphoric acid, sulfuric acid etc.；Its weight/mass percentage composition is 1~10%.
7. lubricant composition as claimed in claim 1, it is characterised in that lubricating base oil be mineral oil, olefin oil or
Its mixture, 100 DEG C of 10~60mm of kinematic viscosity2/ s, open flash point are more than 240 DEG C.
8. the preparation method of lubricant composition as claimed in claim 1, it is characterised in that by overbased calcium alkyl-salicylate and 35
~65% base oil mixing, adds transforming agent after stirring, is warming up to 75~105 DEG C, keep 40~120min；To material retrogradation
Calcium hydroxide is first added afterwards, is then added Aromatic carboxylic, alkyl benzene sulphonate, small molecule aliphatic acid or inorganic acid and is reacted,
Heating dehydration can be suitably added 10~30% base oil to more than 200 DEG C, in temperature-rise period after reaction；Material is continuously heating to
220 DEG C~250 DEG C, constant temperature stirs 5~20 minutes, after material retrogradation, cools down and adds remaining base oil in formula, finally
Homogenizing etc. produces required product.
9. preparation method as claimed in claim 8, it is characterised in that transforming agent is selected from C1~C5 aliphatic acid, fatty alcohol and C8
~C15 alkyl benzene sulphonate and water.
10. preparation method as claimed in claim 8, it is characterised in that diluent and acid of the transforming agent reclaimed water as acid
Add simultaneously, transforming agent comprises at least a kind of acids and a kind of alcohols；Acids is formic acid, acetic acid, propionic acid, detergent alkylate sulphur
Acid；Alcohols is ethanol, isopropanol, normal propyl alcohol or n-butanol.
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| CN201710975739.8A CN107828478A (en) | 2017-10-19 | 2017-10-19 | A kind of Composite calcium naphthenate base lubricant composition and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116064185A (en) * | 2021-10-29 | 2023-05-05 | 中国石油化工股份有限公司 | Method for preparing lubricating grease and application thereof |
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| CN101935578A (en) * | 2010-10-11 | 2011-01-05 | 长沙众城石油化工有限责任公司 | Calcium sulfonate complex grease and preparation method thereof |
| CN103627496A (en) * | 2012-08-28 | 2014-03-12 | 中国石油化工股份有限公司 | Composite calcium naphthenate-based lubricating grease and preparation method therefor |
| CN103695137A (en) * | 2012-09-27 | 2014-04-02 | 中国石油化工股份有限公司 | Composite calcium naphthenate lubricating grease and preparation method thereof |
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2017
- 2017-10-19 CN CN201710975739.8A patent/CN107828478A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101935578A (en) * | 2010-10-11 | 2011-01-05 | 长沙众城石油化工有限责任公司 | Calcium sulfonate complex grease and preparation method thereof |
| CN103627496A (en) * | 2012-08-28 | 2014-03-12 | 中国石油化工股份有限公司 | Composite calcium naphthenate-based lubricating grease and preparation method therefor |
| CN103695137A (en) * | 2012-09-27 | 2014-04-02 | 中国石油化工股份有限公司 | Composite calcium naphthenate lubricating grease and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116064185A (en) * | 2021-10-29 | 2023-05-05 | 中国石油化工股份有限公司 | Method for preparing lubricating grease and application thereof |
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