CN102634400A - High-performance calcium sulfonate complex grease and preparation method thereof - Google Patents
High-performance calcium sulfonate complex grease and preparation method thereof Download PDFInfo
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- CN102634400A CN102634400A CN201210095354XA CN201210095354A CN102634400A CN 102634400 A CN102634400 A CN 102634400A CN 201210095354X A CN201210095354X A CN 201210095354XA CN 201210095354 A CN201210095354 A CN 201210095354A CN 102634400 A CN102634400 A CN 102634400A
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Abstract
The invention relates to grease and a preparation method thereof, in particular to calcium sulfonate complex grease and a preparation method thereof, which belong to the field of chemical technology. A formula of the calcium sulfonate complex grease includes, in weight percentage, 23.5-35.5% of base oil, 32.0-45.4% of high alkalinity calcium sulfonate, 5-15% of calcium carbonate, 1.1-1.5% of alkyl benzene sulfonic acid, 2.5-3.5% of isopropanol, 3-6% of water, 1.9-2.7% of calcium hydroxide, 2-4% of 12-hydroxystearic acid, 1.75-2.25% of inorganic acid, 0.5-3.5% of thickening agent, and 0.1-5% of antioxidant. The calcium sulfonate complex grease has the advantages of high dropping point, fine rust and corrosion resistance, extreme pressure and wear resistance, fine mechanical stability, no hardening in long-term storage and long service life.
Description
Technical field
The present invention relates to a kind of railway grease and preparation method thereof, especially a kind of calcium sulfonate grease and preparation method thereof that meets belongs to technical field of chemistry.
Background technology
Complex calcium sulfonate grease is a type high temp multipurpose grease; This railway grease does not add any additives and just has excellent extreme pressure and antiwear behavior, water repelling property, salt fog resistance performance, protection against corrosion and rust-preventing characteristic; Also has good high temperature performance simultaneously; Mechanical stability, colloid stability and oxidation stability are called as " the efficient railway grease of a new generation ".Abroad just begin to prepare railway grease with calcium sulphonate as viscosifying agent the 1950's, but because its thickening ability is low, oil soluble newton body calcium sulphonate solution thickening ability is very little, so fail effectively to be promoted.After the seventies, the improvement of people through p-sulfonic acid calcium, and further with the overbasic complex calcium sulfonate greases of compound preparation such as lipid acid and borate; Overcome original product characteristic gradually, very big improvement has been arranged on performance, and had the patented technology of some overbased Calcium Sulfonate Complex Grease to deliver; Like US4597800, US4834584, US5126062; US5308514, US5338467.Wherein, although the railway grease for preparing among the US4597800 is had outstanding performance at aspects such as high thermal resistance, shear stabilities, its shortcoming is that viscosifying agent content is high, causes temperature pumping property poor, has hindered the wide range of industrial applications of this fat; It is that the calcium sulphonate of 400 mgKOH/g prepares overbased Calcium Sulfonate Complex Grease that US4834584, US5126062 and US5308514 have proposed to adopt total basicnumber, but the railway grease that they are prepared is shorter work-ing life; And US5338467 adopts alcohols, ethers, and after having transformed, transforming agent directly is discharged in the atmosphere, causes environmental pollution, and exists conversion not thorough, problems such as conversion process instability.Since the nineties, complex calcium sulfonate grease formally put goods on the market; Its Application Areas has expanded to industries such as iron and steel, metallurgy, paper pulp, fresh water and seawater transportation, railway, generating, automobile production, building, food machinery; Caused the extensive concern of domestic and international railway grease industry, its output abroad especially Canada, the U.S. is with 15% speed increment every year on average.But the industrial application of calcium sulfonate complex grease still is in the starting stage at home; Though there are indivedual producers to form small-scale industrial production; But also not as big series products widespread use popularization in industry, a lot of comparatively harsh lubricated operating mode occasions are gone back the dependence on import calcium sulfonate grease.The applicant understands the back and finds: though domestic have TP to describe this type preparation of greases method, and like CN1718700A, CN1414076; CN1872968A, CN101153239A, but also have certain defective; Wherein, CN1718700A is in order to reduce preparation cost, and adopting base number is the calcium alkylbenzenesulfonate of 300 mgKOH/g; Consumption is higher, and cost is also corresponding have been improved; And contain organic carbamide compound among the preparation technology of CN1414076A, and enhance product performance through in overbased Calcium Sulfonate Complex Grease, adding organic carbamide compound, the production technique more complicated, technology controlling and process point is many, and the PT is long, and raw material is poisonous.Adopting base number among the CN1872968A is the main raw material of the calcium sulphonate of 250-320mgKOH/g as complex calcium sulfonate grease; And consumption is up to 60% (weight percentage); And along with total basicnumber goes on the market greater than the ultrahigh basicity calcium sulphonate of 380mgKOH/g is low-cost, developing more, the complex calcium sulfonate grease of best performance has been imperative.Although adopted the calcium sulphonate of overbased (TBN400) among the CN101153239A, cost is still higher, and the package stability of product is relatively poor, and work-ing life is shorter.In addition, also have some patents, the technical scheme that provides like CN101935578A exists conversion not thorough, and transforms less stable; The preparation technology that CN102268323A provides can not guarantee CaCO
3In fat, fully disperse, the fat dropping point of preparation is on the low side, and bearing runs off bigger; CN101824357A then can not effectively solve complex calcium sulfonate and the case-hardened problem of railway grease.All adopt boric acid as mineral acid in these patents, not only the bearing wastage is bigger, exists to transform thoroughly not reach the conversion poor stability, technology controlling and process is required more high shortcoming, and cost is higher.
The viscosifying agent system of calcium sulfonate complex grease is mainly with the non-newtonian fluid high alkaline calcium sulfonate, and wherein lime carbonate exists with the form of calcite crystal formation, the performance decisive role of p-sulfonic acid calcium grease.If lime carbonate contain quantity not sufficient or lime carbonate wherein from the unformed calcite crystal formation that is not converted into fully, then railway grease can be soft partially, high-temperature behavior is not good, the sintering load of railway grease is on the low side.Therefore; The key of preparation complex calcium sulfonate grease is the conversion of newton's height alkaline sulfoacid calcium, and it is more complete that high alkaline calcium sulfonate is transformed, and reduces the consumption of high alkaline calcium sulfonate; Thereby effectively reduce cost and enhance product performance, become the technological focus that these those skilled in the art pay close attention to.In addition, good compound prescription and preparation technology have the supplementary function that is highly profitable to the grease of calcium sulfonic acid after changing mutually, but these all to be prior art be short of.
Summary of the invention
The objective of the invention is the defective to the prior art existence, a kind of high-performance complex calcium sulfonate grease of proposition has high dropping point; Good antirust and non-corrosibility; Extreme pressure anti-wear and good mechanical stability, and place for a long time non-sclerous, the characteristics of long service life.
The present invention is through following technical scheme technical solution problem: a kind of complex calcium sulfonate grease comprises following raw materials in percentage by weight:
Base oil 23.5-35.5%
High alkaline calcium sulfonate 32.0-45.4%
Lime carbonate 5-15%
Alkyl benzene sulphonate(ABS) 1.1-1.5%
Virahol 2.5-3.5%
Water 3-6%
Calcium hydroxide 1.9-2.7%
12-oxystearic acid 2-4%
Mineral acid 1.75-2.25%
Tackifier 0.5-3.5%
Oxidation inhibitor 0.1-5%.
Wherein, said base oil is at least a in MO, the synthetic oil, and 40 ℃ kinematic viscosity is 60-1500mm
2/ s.
Said high alkaline calcium sulfonate is that base number is high alkalinity calcium mahogany sulfonate or the high alkalinity calcium alkylbenzenesulfonate of 380-500mgKOH/g.
The maximum particle diameter of said lime carbonate is 20 μ m, and the massfraction in the lime carbonate is less than 0.05%.
Said alkyl benzene sulphonate(ABS) is a kind of in the LABS of C10-C18.
Said mineral acid is a kind of in phosphoric acid, sulfuric acid or the nitric acid.
Said tackifier are a kind of in polyisobutene, polymethylmethacrylate or the PS-isoprene.
Said oxidation inhibitor is pentanoic or PA.
The present invention adopts above-mentioned raw materials to prepare complex calcium sulfonate grease, and the preparation method may further comprise the steps:
Step 1, base oil, high alkaline calcium sulfonate and lime carbonate are placed reaction kettle, be heated to 60-90 ℃;
Step 2, Virahol, water and alkyl benzene sulphonate(ABS) are joined in the said mixture, reheat is to 100-110 ℃, and remains on and continue stirring reaction 30-90min under this temperature, to forming gel;
When step 3, formation gel, add calcium hydroxide, be warming up to 115-120 ℃; Speed with 3kg/min-10kg/min adds the 12-oxystearic acid then; Behind the reaction 15-30min, the speed with 2kg/min-6kg/min adds mineral acid again, reaction 15-30min;
Step 4, treat that above-mentioned reaction is accomplished after, temperature is risen to 125-150 ℃, add tackifier, continue the reactant system temperature is risen to 160-180 ℃ high temperature refining 60-90min;
Step 5, the temperature of reaction product is reduced to 80-90 ℃, adds oxidation inhibitor, and mixed grinding 45-60min, through filter, must finished product after the degassing.
Preparing method of the present invention can also be chosen in the said step 3, adds before the 12-oxystearic acid, in reaction system, adds the Glacial acetic acid min. 99.5 of 0.15-0.40%, and stirring reaction 15-30min.The effect that adds Glacial acetic acid min. 99.5 is in order further to improve transformation efficiency, to make conversion more thorough.
The complex calcium sulfonate grease that adopts above-mentioned raw materials and method to prepare gained has the following advantages:
1. have good high thermal resistance, favorable mechanical stability and excellent extreme pressure anti-wear, product structure is stable, the characteristics of long service life;
2. in traditional wheel bearing test, the bearing wastage of complex calcium sulfonate grease of the present invention is starkly lower than the bearing wastage (8%) of the high alkaline calcium sulfonate base fat that adopts the lime borate modification less than 3%;
3. in compounded technology, adopt alkyl benzene sulphonate(ABS) and mineral acid to improve the technology of complex calcium sulfonate grease jointly; Promoted the efficient that newton's height alkaline sulfoacid calcium changes into the non-newtonian fluid calcium sulphonate greatly; And transform comparatively thoroughly, solved the surface hardening problem of complex calcium sulfonate grease.
Embodiment
Used high alkaline calcium sulfonate among the following embodiment derives from Jinzhou, Liaoning petroleum additive company, and other raw material is market and purchases conventional raw material like no specified otherwise.
Embodiment one
Present embodiment prepares complex calcium sulfonate grease according to the following steps with raw material:
Step 1, the 150BS base oil with 32.08%, 38.25% 380TBN calcium mahogany sulfonate and 10.5% lime carbonate place the opening reaction kettle that has steam jacket, two moving blades to mix, and are heated to 75 ℃;
Step 2, the Virahol with 2.58%, 3.52% water and 1.25% hexadecyl Phenylsulfonic acid join in the said mixture, reheat to 102 ℃, and remain on and continue stirring reaction 45min under this temperature, to forming gel;
Step 3, when forming gel, add 2.5% calcium hydroxide, and be warming up to 115 ℃, add 1.85% 12-oxystearic acid then with the speed of 4kg/min, behind the stirring reaction 15min, add 2.15% sulfuric acid again with 3kg/min, continue stirring reaction 30min;
Step 4, the temperature of reaction system is risen to 126 ℃, add 3.12% polyisobutene, continue the reactant system temperature is risen to 175 ℃ high temperature refining 60min;
Step 5, the temperature of reaction product is reduced to 85 ℃, adds 2.2% pentanoic, and mixed grinding 60min, through filter, must finished product after the degassing.
The physical and chemical performance analysis result of preparation gained finished product sees table 1.
Embodiment two
Present embodiment prepares complex calcium sulfonate grease according to the following steps with raw material:
Step 1, the intermediate base base oil with 30.71%, 41.44% 400TBN calcium alkylbenzenesulfonate and 7.89% lime carbonate place the opening reaction kettle that has steam jacket, two moving blades to mix, and are heated to 66 ℃;
Step 2, the Virahol with 3.16%, 4.74% water and 1.3% Witco 1298 Soft Acid join in the said mixture, reheat to 107 ℃, and remain on and continue stirring reaction 60min under this temperature, to forming gel;
When step 3, formation gel, add 2.29% calcium hydroxide, and be warming up to 116 ℃; Glacial acetic acid min. 99.5 with 0.31% joins in the reaction system; And react 20min, add 2.96% 12-oxystearic acid then with 6kg/min, behind the stirring reaction 20min; Add 1.97% phosphoric acid again with the speed of 2kg/min, continue stirring reaction 20min;
Step 4, the temperature of reaction system is risen to 130 ℃, add 1.26% PS-isobutyl diene polymer, continue the reactant system temperature is risen to 163 ℃ high temperature refining 75min;
Step 5, the temperature of reaction product is reduced to 90 ℃, adds 1.97% PA, and mixed grinding 60min, through filter, must finished product after the degassing.
The physical and chemical performance analysis result of preparation gained finished product sees table 1.
Embodiment three
Present embodiment prepares complex calcium sulfonate grease according to the following steps with raw material:
Step 1, the poly-alpha olefins with 31.46%, 32.86% 400TBN calcium alkylbenzenesulfonate and 12.28% lime carbonate place the opening reaction kettle that has steam jacket, two moving blades to mix, and are heated to 85 ℃;
Step 2, the Virahol with 3.43%, 5.21% water and 1.42% octadecyl Phenylsulfonic acid join in the said mixture, reheat to 110 ℃, and remain on and continue stirring reaction 90min under this temperature, to forming gel;
When step 3, formation gel, add 1.98% calcium hydroxide, and be warming up to 120 ℃; Glacial acetic acid min. 99.5 with 0.18% joins in the reaction system; And reaction 25min, add 3.32% 12-oxystearic acid then with the speed of 8kg/min, behind the stirring reaction 20min; Add 2.13% nitric acid again with the speed of 5kg/min, continue stirring reaction 30min;
Step 4, the temperature of reaction system is risen to 145 ℃, add 2.48% polymethylmethacrylate, continue the reactant system temperature is risen to 180 ℃ high temperature refining 90min;
Step 5, the temperature of reaction product is reduced to 88 ℃, adds 3.25% PA, and mixed grinding 45min, through filter, must finished product after the degassing.
The physical and chemical performance analysis result of preparation gained finished product sees table 1.
The physicochemical property check data of each embodiment railway grease of table 1
Can find out from the data of table 1; The complex calcium sulfonate grease that the prescription of choose reasonable and the compatibility gained of the present invention through transforming agent makes; Have high dropping point, good resistance to elevated temperatures and outstanding extreme pressure and antiwear behavior, and all obviously be superior to the prepared product of prior art in the bearing wastage with on work-ing life.
Except that above-mentioned enforcement, the present invention can also have other embodiments.All employings are equal to the technical scheme of replacement or equivalent transformation formation, all drop on the protection domain of requirement of the present invention.
Claims (10)
1. complex calcium sulfonate grease comprises following raw materials in percentage by weight:
Base oil 23.5-35.5%
High alkaline calcium sulfonate 32.0-45.4%
Lime carbonate 5-15%
Alkyl benzene sulphonate(ABS) 1.1-1.5%
Virahol 2.5-3.5%
Water 3-6%
Calcium hydroxide 1.9-2.7%
12-oxystearic acid 2-4%
Mineral acid 1.75-2.25%
Tackifier 0.5-3.5%
Oxidation inhibitor 0.1-5%.
2. complex calcium sulfonate grease according to claim 1 is characterized in that: said base oil is at least a in MO, the synthetic oil.
3. complex calcium sulfonate grease according to claim 1 is characterized in that: said high alkaline calcium sulfonate is that base number is high alkalinity calcium mahogany sulfonate or the high alkalinity calcium alkylbenzenesulfonate of 380-500mgKOH/g.
4. complex calcium sulfonate grease according to claim 1 is characterized in that: the maximum particle diameter of said lime carbonate is 20 μ m, and massfraction quartzy in the lime carbonate is less than 0.05%.
5. complex calcium sulfonate grease according to claim 1 is characterized in that: said alkyl benzene sulphonate(ABS) is a kind of in the LABS of C10-C18.
6. high-performance complex calcium sulfonate grease according to claim 1 is characterized in that: said mineral acid is a kind of in phosphoric acid, sulfuric acid or the nitric acid.
7. high-performance complex calcium sulfonate grease according to claim 1 is characterized in that: said tackifier are a kind of in polyisobutene, polymethylmethacrylate or the PS-isoprene.
8. high-performance complex calcium sulfonate grease according to claim 1 is characterized in that: said oxidation inhibitor is pentanoic or PA.
9. the preparation method of complex calcium sulfonate grease according to claim 1 may further comprise the steps:
Step 1, base oil, high alkaline calcium sulfonate and lime carbonate are placed reaction kettle, be heated to 60-90 ℃;
Step 2, Virahol, water and alkyl benzene sulphonate(ABS) are joined in the said mixture, reheat is to 100-110 ℃, and remains on and continue stirring reaction 30-90min under this temperature, to forming gel;
When step 3, formation gel, add calcium hydroxide, be warming up to 115-120 ℃; Speed with 3kg/min-10kg/min adds the 12-oxystearic acid then; Behind the reaction 15-30min, the speed with 2kg/min-6kg/min adds mineral acid again, reaction 15-30min;
Step 4, treat that above-mentioned reaction is accomplished after, temperature is risen to 125-150 ℃, add tackifier, continue temperature is risen to 160-180 ℃ high temperature refining 60-90min;
Step 5, the temperature of reaction product is reduced to 80-90 ℃, adds oxidation inhibitor, and mixed grinding 45-60min, through filter, must finished product after the degassing.
10. according to the preparation method of the said high-performance complex calcium sulfonate grease of claim 9, it is characterized in that: in the said step 3, before adding the 12-oxystearic acid, add the Glacial acetic acid min. 99.5 of 0.15-0.40%, and stirring reaction 15-30min.
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