CN102492522A - Composite aluminum soap grease and preparation method thereof - Google Patents
Composite aluminum soap grease and preparation method thereof Download PDFInfo
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- CN102492522A CN102492522A CN2011103564873A CN201110356487A CN102492522A CN 102492522 A CN102492522 A CN 102492522A CN 2011103564873 A CN2011103564873 A CN 2011103564873A CN 201110356487 A CN201110356487 A CN 201110356487A CN 102492522 A CN102492522 A CN 102492522A
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Abstract
The invention provides composite aluminum soap grease and a preparation method thereof, and belongs to the technical field of lubricating grease preparation. The lubricating grease comprises the following constituents by weight: 5 to 9 percent of C12 to C18 saturated straight-chain fatty acid, 0 to 4 percent of C12 to C18 saturated hydroxy fatty acid, 0.25 to 3 percent of aromatic acid, 0.5 to 1.5 percent of sodium metaaluminate, and 83 to 92 percent of base oil. The preparation method comprises the following steps: adding part of the base oil into a normal-pressure esterifying kettle; stirring; adding the aromatic acid, the C12 to C18 saturated straight-chain fatty acid and the saturated hydroxy fatty acid when the temperature reaches 60 to 80 DEG C; stirring at a constant temperature till the aromatic acid, the C12 to C18 saturated straight-chain fatty acid and the saturated hydroxy fatty acid are dissolved completely; adding the sodium metaaluminate when the temperature reaches 100 to 120 DEG C; saponifying at a low temperature for 1 to 4 hours; saponifying for 1 to 3 hours when the temperature reaches 160 to 180 DEG C; refining for 0.5 to 2 hours when the temperature reaches 200 to 200 DEG C; adding the rest base oil; stirring; cooling; grinding; and degassing to obtain the composite aluminum soap grease. The composite aluminum soap grease prepared by the invention has the advantages of high drop point, favorable mechanical stability and excellent rustproof performance.
Description
Technical field
The invention belongs to the railway grease preparing technical field, be specifically related to a kind of composite aluminum base grease and preparation method thereof.
Background technology
Aluminum complex grease has the advantage of dropping point height, good in oxidation resistance, is applicable to that the high temperature services such as steel-making, steel rolling and sintering of metallurgy industry are lubricated, is a kind of high temperature resistant railway grease of excellent property.Simultaneously, aluminium soap grease also has excellent high-temperature and reversible property, and pumping is good, is particularly suitable for the needs of centrallubrication.In addition, aluminium soap grease also has good water resisting property and certain wear-resistant and lubricity.Therefore, aluminum complex grease has a good application prospect in high temperature lubricating fields such as metallurgy, machinery, chemical industry.
The aluminum complex grease patent report starts from early 1950s, because crucial technology of preparing does not break through, does not obtain valuable industrial application for a long time.Up to find aluminum isopropoxide (or tripolymer) directly saponification make aluminum complex grease, production technique is simplified, constant product quality simultaneously, price is relatively cheap, develops very rapid closely during the last ten years.Early 1990s; Aluminum complex grease accounts for about 7.8 % of U.S.'s railway grease ultimate production; Account for 11.8 % of national railway grease ultimate production in Canada; The European member states of NLGI (U.S.'s grease institute) accounts for about 7.6 %, and China only accounts for about 3.7 % of railway grease ultimate production, lags far behind developed country.So aluminum complex grease will become one of principal item of China's railway grease development from now on.
The railway grease that the compound aluminium soap that composite aluminum base grease refers to utilize organic acid and the aluminum contained compound reaction more than two kinds to generate makes for viscosifying agent.Before and after the 1950's, people just have realized that having anionic aluminium base two soaps of different organic acids can form colloidal structure in oil, can be used for grease thickener, printing ink weighting agent etc.Since the higher fatty acid poorly water-soluble, Al (OH)
3Be insoluble in water, reactive behavior is low, general using water-soluble aluminum salt and water-soluble organic acid metallic soap (as: StNa) prepare aluminium soap through replacement(metathesis)reaction.Yet this method not only exists aluminium soap to separate and the washing difficulty, and wastewater flow rate is big, environmental pollution is serious, and contains aluminium salt hydrolysis product in the preparation aluminium soap.Jones in 1949 etc. have invented a kind of method of utilizing rudimentary aluminium alcoholates (as: aluminum methylate, aluminum ethylate, aluminum isopropylate etc.) and organic acid reaction to prepare aluminium soap; Patent USP 2,654, and 710 provide a kind of preparation method who in the aqueous solution, utilizes the synthetic aluminium soap of organic acid and water-soluble aluminum salt (as: Tai-Ace S 150, aluminum nitrate etc.) reaction, and will separate, dried aluminium soap is applied to the multiviscosisty ZGK 5 and prepares synthetic fat.USP 2; 599,553, USP 2,719; 826, USP 2; 768, the 138 mixing water insoluble metallic soap (as: soda soap) through containing different anions and water-soluble aluminum salt (as: Tai-Ace S 150, aluminum nitrate etc.) are mixed the compound aluminium soap of prepared by co-precipitation in the aqueous solution compound methods, and be applied to high dropping point, water resisting property grease thickener.Yet, prepare aluminium soap grease through the method for prefabricated soap, because the aluminium soap fusing point is high, difficulties in dispersion in base oil needs very high 221 ℃ of one-tenth fat temperature (430 ℉).In order to overcome above-mentioned shortcoming; Patent USP 3; 345,291 provide a kind of compound method of in base oil, utilizing rudimentary aluminium alcoholates (mainly comprising aluminum ethylate, Tripropoxyaluminum, aluminum isopropylate and aluminium butoxide) and mixed organic acid (mainly being made up of higher fatty acid and aromatic acid) prepared in reaction aluminium soap and composite aluminum base grease.Further; Patent USP 3; 591; 505 also provide a kind of compound method of in base oil, utilizing aluminum alkoxide (butoxy aluminium, aluminum isopropoxide) and the saponification of two kinds of different carboxylic acids mixtures to prepare composite aluminum base grease, and the aluminum complex grease that makes has high dropping point, are applicable to that spot contact bearing is lubricated.Early stage various rudimentary aluminium alcoholates expensive have limited aluminium soap grease production.Afterwards, along with the large-scale industrial production of tripolymer aluminium (aluminum isopropylate), become the aluminum complex grease main preparation methods with tripolymer aluminium soap organic acid, (USP 3 about a large amount of patents of invention of aluminum complex grease; 620,975, USP 3,776, and 846, USP 3; 843,528, USP 4,132; 658, USP 5,037, and 563) all be to prepare compound aluminium soap through the tripolymer aluminium soapization.The research of domestic composite aluminum base grease is started late, and composite aluminum base grease patent report few in number is only arranged at present.Wherein, Chinese patent CN 1; 900,244A, CN 101117604) provide a kind of respectively with the synthetic compound aluminium soap of Triple Pressed Stearic Acid, phenylformic acid and tripolymer aluminium, and further add the method that high alkaline calcium sulfonate prepares composite aluminum base grease; And find that basic fat has good water resisting property, rust-preventing characteristic, extreme pressure property, mechanical stability and high temperature colloid stability under the not additivated situation.In addition, patent USP3,511,781 find in aluminium soap grease, to add a certain amount of aromatic acid an alkali metal salt can improve its stability.
At present, be equipped with the high shortcoming of composite aluminum base grease production technique ubiquity cost by the tripolymer aluminum.With respect to tripolymer aluminium, the sodium metaaluminate price is low.The present invention has prepared aluminum complex grease with sodium metaaluminate saponification higher fatty acid and aromatic acid mixed carboxylic acid in a certain amount of base oil, the prepared composite aluminium soap grease has high dropping point, favorable mechanical stability and rust-preventing characteristic.
Summary of the invention
The present invention is directed to technological single, the cost high-technology problem that exist in the existing aluminium soap synthetic technology, a kind of composite aluminum base grease and preparation method thereof is provided, this preparation method prepares composite aluminum base grease with the sodium metaaluminate saponification of cheapness.
The composition and the weight percent of composite aluminum base grease provided by the present invention are:
C
12-C
18Saturated straight chain lipid acid 5-9%; C
12-C
18Saturated hydroxy-fatty acid 0-4%; Aromatic acid 0.25-3 %; Sodium metaaluminate 0.5-1.5%; Base oil 83-92%.
The mol ratio of total acidic group of the organic acid in the said composition and sodium metaaluminate is: (2.5-3.5): 1, preferred (3-3.5): 1.
Said C
12-C
18Saturated straight chain lipid acid is Triple Pressed Stearic Acid.
Said C
12-C
18Saturated hydroxy-fatty acid is the 12-oxystearic acid.
Said aromatic acid is phenylformic acid or phthalic acid, preferred phthalic acid.
Said base oil is a kind of or both mixtures in hydrorefined mineral oils, the synthetic oil.
Preparing method's concrete steps of composite aluminum base grease provided by the present invention are following:
In the normal pressure esterification still, add the base oil of 50-60%, stir and be warming up to 60-80 ℃, add aromatic acid, C respectively
12-C
18Linear saturated fatty acids, C
12-C
18Saturated hydroxy-fatty acid, constant temperature are stirred to fully dissolving, be warming up to 100-120 ℃ after; Add sodium metaaluminate,, slowly be warming up to again in 160-180 ℃ warm saponification 1-3 hour in 100-120 ℃ of low-temperature saponification 1-4 hour; Then; Continue to be warming up to 200-220 ℃ of high temperature and refine after 0.5-2 hour, add remaining 40-50% base oil and stir, cool off, and promptly get composite aluminum base grease after the processing of grinding, outgas.
Among the present invention, lipid acid and aromatic acid are compound produces compound aluminium soap with the sodium metaaluminate saponification, improve the thickening ability and the mechanical stability of compound aluminium soap, and aromatic acid acidity helps by force and the sodium metaaluminate saponification; Adding a certain amount of hydroxy fatty acid can generate a certain amount of hydrogen bond action between the soap fiber, can further improve its stability and become the fat performance.Though every moles, of aluminum per mole of titanium metal can with 3 equimolar acid saponification salifies, not exclusively contain structure and the performance that small amount of hydroxyl groups helps improving its thickening ability and aluminium soap grease on the saponified aluminium atom.Simultaneously, during said sodium metaaluminate saponification,, comprise that also sodium and organic acid saponification generate soda soap except aluminium and the organic acid saponification.So the mol ratio of total acidic group of organic acid such as lipid acid according to the invention, hydroxy fatty acid and aromatic acid and sodium metaaluminate is (2.5-3.5): 1.
In the inventive method, in 60-80 ℃ of base oil, add organic acid, not only can promote the organic acid dissolving, and can avoid its decomposition; Lipid acid dissolves fully; Being warming up to 100-120 ℃ of adding sodium metaaluminate after mixing carried out low-temperature saponification 1-4 hour; Help that sodium metaaluminate is uniformly dispersed, the sodium ion saponification in the sodium metaaluminate and the generation of meta-aluminic acid and aluminic acid, said temperature can be avoided nascent state meta-aluminic acid and aluminic acid dehydration formation aluminum oxide simultaneously; After the low-temperature saponification, slowly being warming up in 160-180 ℃ warm saponification 1-3 hour mainly is to promote nascent state aluminic acid and meta-aluminic acid and organic acid further to react generation organic acid aluminium soap; After the saponification fully, through the aluminum complex grease of 200-220 ℃ of high temperature refining can formation in 0.5-2 hour aluminium soap and the compound multiviscosisty of soda soap.So sodium metaaluminate saponification organic acid according to the invention is made up of for two sections low-temperature saponification and middle temperature saponification.
Beneficial effect of the present invention is following:
The invention provides a kind of sodium metaaluminate with cheapness is the aluminium source, preparation composite aluminum base grease and preparation method.The mixed organic acid of forming by lipid acid, hydroxy fatty acid and phenylformic acid with depart from sour soda soapization, can make have high dropping point, the composite aluminum base grease of good stability and excellent rustless property; The aluminium soap preparation technology who forms with low-temperature saponification and middle temperature saponification can overcome the low shortcoming of sodium metaaluminate reactive behavior, replaces the tripolymer aluminum to be equipped with aluminium soap grease, has the low advantage of cost.
Embodiment
Embodiment 1: in the normal pressure esterification still, add 100g 150BS base oil, stir and be warming up to 60 ℃, add 0.5g phenylformic acid, 12g Triple Pressed Stearic Acid, 7g 12-oxystearic acid respectively, constant temperature is stirred to dissolving fully.Be warming up to 100 ℃, add the 1.5g sodium metaaluminate,, slowly be warming up in 170 ℃ warm saponification again 2 hours in 105 ℃ of low-temperature saponification 2 hours.Then, continue to be warming up to 200 ℃ of high temperature refinings 1 hour.At last, adding 79g 150BS base oil stirs, cools off, and the processing of grinding, outgas promptly gets composite aluminum base grease.
Embodiment 2: in the normal pressure esterification still, add 100g PAO-20 (polyalphaolefin) base oil, stir and be warming up to 60 ℃, add 3g phenylformic acid, 16g Triple Pressed Stearic Acid respectively, constant temperature is stirred to dissolving fully.Be warming up to 100 ℃, add the 2g sodium metaaluminate,, slowly be warming up in 170 ℃ warm saponification again 2 hours in 105 ℃ of low-temperature saponification 2 hours.Then, continue to be warming up to 200 ℃ of high temperature refinings 1 hour.At last, add 79 g PAO-20 base oils, stir, cool off, and the processing of grinding, outgas promptly gets composite aluminum base grease.
Embodiment 3: in the normal pressure esterification still, add 100g 150BS base oil, stir and be warming up to 60 ℃, add 6g phenylformic acid, 12g Triple Pressed Stearic Acid respectively, constant temperature is stirred to dissolving fully.Be warming up to 110 ℃, add 3 g sodium metaaluminates,, slowly be warming up in 160 ℃ warm saponification again 2 hours in 120 ℃ of low-temperature saponification 2 hours.Then, continue to be warming up to 210 ℃ of high temperature refinings 1 hour.At last, adding 79g 150BS base oil stirs, cools off, and the processing of grinding, outgas promptly gets composite aluminum base grease.
Embodiment 4: in the normal pressure esterification still, add 100g 150BS base oil, stir and be warming up to 70 ℃, add 2g phenylformic acid, 14g Triple Pressed Stearic Acid, 3g 12-oxystearic acid respectively, constant temperature is stirred to dissolving fully.Be warming up to 120 ℃, add the 2g sodium metaaluminate,, slowly be warming up in 180 ℃ warm saponification again 2 hours in 120 ℃ of low-temperature saponification 2 hours.Then, continue to be warming up to 210 ℃ of high temperature refinings 1 hour.At last, add 79 g 150BS base oils, stir, cool off, and the processing of grinding, outgas promptly gets composite aluminum base grease.
Embodiment 5: in the normal pressure esterification still, add 100g 150BS base oil, stir and be warming up to 80 ℃, add 3g phenylformic acid, 13g Triple Pressed Stearic Acid, 3g 12-oxystearic acid respectively, constant temperature is stirred to dissolving fully.Be warming up to 120 ℃, add the 2g sodium metaaluminate,, slowly be warming up in 170 ℃ warm saponification again 2 hours in 110 ℃ of low-temperature saponification 2 hours.Then, continue to be warming up to 220 ℃ of high temperature refinings 1 hour.At last, add 79 g 150BS base oils, stir, cool off, and the processing of grinding, outgas promptly gets composite aluminum base grease.
Embodiment 6: in the normal pressure esterification still, add 100g 150BS base oil, stir and be warming up to 65 ℃, add 3g phenylformic acid, 13g Triple Pressed Stearic Acid, 3g 12-oxystearic acid respectively, constant temperature is stirred to dissolving fully.Be warming up to 120 ℃, add the 2g sodium metaaluminate,, slowly be warming up in 170 ℃ warm saponification again 1 hour in 110 ℃ of low-temperature saponification 3 hours.Then, continue to be warming up to 220 ℃ of high temperature refinings 1 hour.At last, adding 79g 150BS base oil stirs, cools off, and the processing of grinding, outgas promptly gets composite aluminum base grease.
Embodiment 7: in the normal pressure esterification still, add 100g 150BS base oil, stir and be warming up to 65 ℃, add 3g phenylformic acid, 13g Triple Pressed Stearic Acid, 3g 12-oxystearic acid respectively, constant temperature is stirred to dissolving fully.Be warming up to 120 ℃, add the 2g sodium metaaluminate,, slowly be warming up in 170 ℃ warm saponification again 3 hours in 110 ℃ of low-temperature saponification 1 hour.Then, continue to be warming up to 220 ℃ of high temperature refinings 2 hours.At last, add 79 g 150BS base oils, stir, cool off, and the processing of grinding, outgas promptly gets composite aluminum base grease.
Embodiment 8: in the normal pressure esterification still, add 100g 150BS base oil, stir and be warming up to 65 ℃, add 3g phenylformic acid, 13g Triple Pressed Stearic Acid, 3g 12-oxystearic acid respectively, constant temperature is stirred to dissolving fully.Be warming up to 120 ℃, add the 2g sodium metaaluminate,, slowly be warming up in 170 ℃ warm saponification again 1 hour in 110 ℃ of low-temperature saponification 4 hours.Then, continue to be warming up to 220 ℃ of high temperature refinings 0.5 hour.At last, adding 79g 150BS base oil stirs, cools off, and the processing of grinding, outgas promptly gets composite aluminum base grease.
Aluminium base lubricated performance measurement result is as shown in table 1 for embodiment 1-8 prepared composite.The result shows, the preparation method of a kind of composite aluminum base grease of the present invention can be in base oil prepares composite aluminum base basis fat by the mixed carboxylic acid of direct saponification higher fatty acid of sodium metaaluminate and aromatic acid.Not additivated basic fat has high dropping point, stability and excellent rustless property, is applicable to the high temperature resistant railway grease of preparation.
Table 1 instance 1-8 prepares composite aluminum base basis fat salient features and measures the result
Claims (6)
1. composite aluminum base grease, it is characterized in that: the composition and the weight percent of this railway grease are:
C
12-C
18Saturated straight chain lipid acid 5-9 %, C
12-C
18Saturated hydroxy-fatty acid 0-4%, aromatic acid 0.25-3%, sodium metaaluminate 0.5-1.5%, base oil 83-92%; The mol ratio of total acidic group of the organic acid in the said composition and sodium metaaluminate is: (2.5-3.5): 1, preferred (3-3.5): 1.
2. the preparation method of a kind of composite aluminum base grease as claimed in claim 1 is characterized in that this preparation method is specific as follows:
In the normal pressure esterification still, add the base oil of 50-60wt%, stir and be warming up to 60-80 ℃, add aromatic acid, C respectively
12-C
18Linear saturated fatty acids, C
12-C
18Saturated hydroxy-fatty acid, constant temperature are stirred to fully dissolving, be warming up to 100-120 ℃ after; Add sodium metaaluminate,, slowly be warming up to again in 160-180 ℃ warm saponification 1-3 hour in 100-120 ℃ of low-temperature saponification 1-4 hour; Then; Continue to be warming up to 200-220 ℃ of high temperature and refine after 0.5-2 hour, add remaining 40-50wt% base oil and stir, cool off, and promptly get said composite aluminum base grease after the processing of grinding, outgas.
3. a kind of composite aluminum base grease according to claim 1 is characterized in that said C
12-C
18Saturated straight chain lipid acid is Triple Pressed Stearic Acid.
4. a kind of composite aluminum base grease according to claim 1 is characterized in that said C
12-C
18Saturated hydroxy-fatty acid is the 12-oxystearic acid.
5. a kind of composite aluminum base grease according to claim 1 is characterized in that said aromatic acid is phenylformic acid or phthalic acid, preferred phthalic acid.
6. a kind of composite aluminum base grease according to claim 1 is characterized in that said base oil is a kind of or both mixtures in hydrorefined mineral oils, the synthetic oil.
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| CN201110356487.3A CN102492522B (en) | 2011-11-11 | 2011-11-11 | Composite aluminum soap grease and preparation method thereof |
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|---|---|---|---|
| CN201110356487.3A CN102492522B (en) | 2011-11-11 | 2011-11-11 | Composite aluminum soap grease and preparation method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103980979A (en) * | 2014-05-26 | 2014-08-13 | 苏州惠丰润滑油有限公司 | Complex aluminum-titanium-based grease composition and preparation method thereof |
| CN105586136A (en) * | 2014-10-23 | 2016-05-18 | 中国石油化工股份有限公司 | Complex aluminum-based lubricating grease composition with excellent antifriction property and preparation method therefor |
| CN106278289A (en) * | 2016-08-16 | 2017-01-04 | 佛山市彩贵新型材料有限公司 | A kind of ceramic hardness assistant composition |
| CN106278156A (en) * | 2016-08-16 | 2017-01-04 | 佛山市彩贵新型材料有限公司 | A kind of reinforcing aids compositions |
| CN106348763A (en) * | 2016-08-16 | 2017-01-25 | 佛山市彩贵新型材料有限公司 | Additive for enhancing color-penetrated tile hardness and preparation method thereof |
| CN106365687A (en) * | 2016-08-16 | 2017-02-01 | 佛山市彩贵新型材料有限公司 | Auxiliary agent capable of improving wear resistance of tile and application method thereof |
| CN108485769A (en) * | 2018-05-07 | 2018-09-04 | 东莞市蓝鲸化工科技有限公司 | A kind of high temperature resistant luboil fat and preparation method thereof |
| CN109679736A (en) * | 2018-12-25 | 2019-04-26 | 泰伦特生物工程股份有限公司 | A kind of high temperature thermal reversibility complex soap grease and preparation method thereof |
| CN110408459A (en) * | 2019-07-22 | 2019-11-05 | 纳拓润滑技术（上海）有限公司 | A kind of high-performance composite aluminum base bentonite grease and preparation method thereof |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103980979A (en) * | 2014-05-26 | 2014-08-13 | 苏州惠丰润滑油有限公司 | Complex aluminum-titanium-based grease composition and preparation method thereof |
| CN103980979B (en) * | 2014-05-26 | 2016-08-17 | 江苏惠丰润滑材料股份有限公司 | Aluminum-titanium compositing yl grease compositions and preparation method |
| CN105586136A (en) * | 2014-10-23 | 2016-05-18 | 中国石油化工股份有限公司 | Complex aluminum-based lubricating grease composition with excellent antifriction property and preparation method therefor |
| CN105586136B (en) * | 2014-10-23 | 2018-05-25 | 中国石油化工股份有限公司 | Excellent composite aluminum base grease composition of a kind of Wear vesistance and preparation method thereof |
| CN106278289A (en) * | 2016-08-16 | 2017-01-04 | 佛山市彩贵新型材料有限公司 | A kind of ceramic hardness assistant composition |
| CN106278156A (en) * | 2016-08-16 | 2017-01-04 | 佛山市彩贵新型材料有限公司 | A kind of reinforcing aids compositions |
| CN106348763A (en) * | 2016-08-16 | 2017-01-25 | 佛山市彩贵新型材料有限公司 | Additive for enhancing color-penetrated tile hardness and preparation method thereof |
| CN106365687A (en) * | 2016-08-16 | 2017-02-01 | 佛山市彩贵新型材料有限公司 | Auxiliary agent capable of improving wear resistance of tile and application method thereof |
| CN108485769A (en) * | 2018-05-07 | 2018-09-04 | 东莞市蓝鲸化工科技有限公司 | A kind of high temperature resistant luboil fat and preparation method thereof |
| CN109679736A (en) * | 2018-12-25 | 2019-04-26 | 泰伦特生物工程股份有限公司 | A kind of high temperature thermal reversibility complex soap grease and preparation method thereof |
| CN110408459A (en) * | 2019-07-22 | 2019-11-05 | 纳拓润滑技术（上海）有限公司 | A kind of high-performance composite aluminum base bentonite grease and preparation method thereof |
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