CN101993767B - Nano calcium carbonate-containing calcium sulfonate complex grease and production method thereof - Google Patents
Nano calcium carbonate-containing calcium sulfonate complex grease and production method thereof Download PDFInfo
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- CN101993767B CN101993767B CN201010537753.8A CN201010537753A CN101993767B CN 101993767 B CN101993767 B CN 101993767B CN 201010537753 A CN201010537753 A CN 201010537753A CN 101993767 B CN101993767 B CN 101993767B
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Abstract
The invention relates to nano calcium carbonate-containing calcium sulfonate complex grease and a production method thereof. The grease comprises the following components in percentage by weight: 10 to 40 percent of high base-value calcium alkylbenzenesulfonate, 50 to 85 percent of base oil, 1 to 10 percent of nano calcium carbonate, 0.5 to 5 percent of boric acid, 0.5 to 5 percent of saturated fatty acid with 12 to 22 carbon atoms, 0.1 to 5 percent of anti-oxidant additive and 1 to 5 percent of composite transformation accelerator HBS. The grease and the production method have the advantages that: a nano calcium carbonate material is added into the formula of the calcium sulfonate complex grease for the first time, so that the thermal stability and extreme pressure wearing resistance of the ordinary calcium sulfonate complex grease are enhanced and a preparation and operation process is simplified. Simultaneously, the composite transformation accelerator is adopted, so that transformation speed and transformation rate are increased and production cost is lowered.
Description
Technical field
The present invention relates to field of lubricant, particularly, relate to a kind of composite calcium sulfonate grease lubricant and production method thereof.
Background technology
Since the eighties in 20th century, composite calcium sulfonate grease lubricant is studied much abroad and applies, and has formed many patented technologies.As US4,560,489, US4,824,584, US5,126,062, US5,308,514, US5,338,476 etc.Although domestic research aspect composite calcium sulfonate grease lubricant is more late, develop also comparatively rapid, constantly have patented technology produce.As the patent disclosing or authorize has: CN02130820.9, CN200510047000.8, CN200510073101.2, CN200710131339.5, CN200810063176.6, CN200810101182.6, CN201010105181.6, CN201010188808.9 etc.
The viscosifying agent of composite calcium sulfonate grease lubricant is mainly calcium sulfonate with high base number (for the indispensable detergent additive of engine oil), and calcium carbonate is wherein unformed carbonic acid calcium.And in composite calcium sulfonate grease lubricant, what play densification and heat stabilization is the calcium carbonate of calcite crystal formation.Therefore,, in composite calcium sulfonate grease lubricant production process, the completeness that unformed carbonic acid calcium is converted into the calcium carbonate of calcite crystal formation directly has influence on the performance of composite calcium sulfonate grease lubricant.Common composite calcium sulfonate grease lubricant technique and formula are difficult to reach good transforming degree, and the lubricating grease thermal stability of production is bad, and transformation time is long and production technique is unstable, finally causes quality product bad, and production cost is high.
Object of the present invention is intended to adopt up-to-date nanosecond science and technology achievement, provides that a kind of composite calcium sulfonate grease lubricant containing nano material is newly filled a prescription, novel process.Due to the introducing of nano material, improve the bad problem of poor heat stability, extreme pressure and antiwear behavior of composite calcium sulfonate grease lubricant.Meanwhile, improve conversion rate and transformation efficiency, reduced product cost.
Summary of the invention
The object of this invention is to provide a kind of composite calcium sulfonate grease lubricant and production method thereof containing nano-calcium carbonate, the poor heat stability of existing like product and the shortcoming of extreme pressure and antiwear behavior deficiency have been overcome, simplify preparation manipulation technique, overcome the problem of conversion rate and low conversion rate simultaneously.
The technical scheme that realizes above-mentioned purpose is as follows:
Containing the composite calcium sulfonate grease lubricant of nano-calcium carbonate, comprise following component:
Mineral base oil, its weight percentage is 50～85% of raw material for lubricating grease total amount; High base number calcium alkylbenzenesulfonate: its weight percentage is 10～40% of raw material for lubricating grease total amount; Nano-calcium carbonate: its weight percentage is 1～10% of raw material for lubricating grease total amount; Boric acid: its weight percentage is 0.5～5% of raw material for lubricating grease total amount; C
12～C
22saturated fatty acid: its weight percentage is 0.5～5% of raw material for lubricating grease total amount; The compound inversion accelerating agent of HBS: its weight percentage is 1.0～5% of raw material for lubricating grease total amount; Antioxidant addn: its weight percentage is 0.1～5% of raw material for lubricating grease total amount.
Further, described mineral base oil can be mixture a kind of, two or more different viscosity grade base oil, as: MVI150, MVI500, HVI150, HVI200, HVI500,120BS, 150BS, No. 100 machinery oil or SUPER500, kinematic viscosity is 30～500mm
2/ s.
Described high base number calcium alkylbenzenesulfonate total basicnumber is 250～500mgKOH/g.For commercially available prod.
The compound inversion accelerating agent of described HBS is commercially available prod.
Described antioxidant is amine type high-temperature anti-oxidant.
Described high-temperature anti-oxidant is the mixture of di-iso-octyldiphenylamine, N-phenyl-a-naphthylamine, N-Phenyl beta naphthylamine and two or more amine type high-temperature anti-oxidant.
The particle diameter of described nano-calcium carbonate is 5～100 nanometers.
Described boric acid is commercially available prod, and content is greater than 90%.
Described C
12～C
22saturated fatty acid is the lipid acid of hydroxyl preferably.As: 12-oxystearic acid.
Composite calcium sulfonate grease lubricant containing nano-calcium carbonate provided by the invention is to produce with step by the following method:
(1) 20～50% and high base number calcium alkylbenzenesulfonate of base oil gross weight are added in reactor, stirring reaction is heated to 60 ± 5 ℃, then add water (1～10% of the raw material for lubricating grease total amount measuring, additional) and the compound inversion accelerating agent of HBS, stir and be warmed up to 80～95 ℃ of conversion reactions to transforming completely (with infrared spectroscopy monitor).
(2) add nano-calcium carbonate to stir, then order adds hot solution (boric acid is mixed with water, be heated to 95 ℃, become the solution of homogeneous transparent), the C of boric acid and water (ratio of boric acid and water is 1:2～5, and water is additional)
12～C
22saturated fatty acid, stirs and dewaters and add part excess oil (base oil gross weight 30～65%), is warmed up to 180 ℃, constant temperature 10 minutes.Stop heating, add antioxidant and all remain base oil, stir and be cooled to below 100 ℃.
(3) the degassed rear finished product of homogenizing.
The invention has the beneficial effects as follows:
First, Nano-Calcium Carbonate is introduced in composite calcium sulfonate grease lubricant formula, improved thermostability and the extreme pressure and antiwear behavior of common composite calcium sulfonate grease lubricant, simplified preparation manipulation technique.Meanwhile, owing to having adopted compound inversion accelerating agent, improve conversion rate and transformation efficiency, reduced production cost.
Embodiment
Below the preferred embodiments of the present invention are described, should be appreciated that preferred embodiment described herein, only for description and interpretation the present invention, is not intended to limit the present invention.
embodiment 1
In the reactor with agitator, add 200 kilograms of HVI500(40 ℃ of kinematic viscosity to be: 97mm
2/ s, account for base oil gross weight 37.8%) and 400 kilograms of total basicnumbers calcium alkylbenzenesulfonate that is 250mgKOH/g (for raw material for lubricating grease total amount 40%), stirring heating is warmed up to 60 ℃, add 50 kg of water and 50 kilograms of HBS(be raw material for lubricating grease total amount 5%), stirring is warmed up to 80～95 ℃ of constant temperature conversion reactions, until transform completely, (uses the unformed carbonic acid calcium of infrared spectroscopy monitor at 862cm
-1the charateristic avsorption band at place disappears, and approximately reacts 0.5 hour to 1 hour).Add 10 kilograms of nano-calcium carbonates (for raw material for lubricating grease total amount 1%), stir 5 minutes, then order add 5 kilograms of boric acid (for raw material for lubricating grease total amount 0.5%) with the hot solution of 25 kg of water, 5 kilograms of 12-oxystearic acids (be raw material for lubricating grease total amount 0.5%), stir dewater and add 200 kilograms of HVI500(account for base oil gross weight 37.8%), continue dehydration and be warmed up to 180 ℃, constant temperature stops heating after 10 minutes, add 1 kilogram of di-iso-octyldiphenylamine (for raw material for lubricating grease total amount 0.1%), 129 kilograms of HVI500, stirring is cooled to lower than 100 ℃, through homogenizer homogenizing and degassed after finished product.The present embodiment base oil dosage is 52.9% of raw material for lubricating grease total amount.Salient features is in Table 1.
embodiment 2
In the reactor with agitator, add the calcium alkylbenzenesulfonate that 200 kilograms of 150BS base oils (account for base oil gross weight 30.3%) and 100 kilograms of total basicnumbers are 400mgKOH/g (for raw material for lubricating grease total amount 10%), stirring heating is warmed up to 60 ℃, add 50 kg of water and 10 kilograms of HBS(be raw material for lubricating grease total amount 1%), stirring is warmed up to 80～95 ℃ of constant temperature conversion reactions, until transform completely, (uses the unformed carbonic acid calcium of infrared spectroscopy monitor at 862cm
-1the charateristic avsorption band at place disappears, and approximately reacts 0.5 hour to 1 hour).Add 100 kilograms of nano-calcium carbonates (for raw material for lubricating grease total amount 10%), stir 5 minutes, then order add 30 kilograms of boric acid (for raw material for lubricating grease total amount 3%) with the hot solution of 90 kg of water, 50 kilograms of 12-oxystearic acids (be raw material for lubricating grease total amount 5%), stir and dewater and add 329 kilograms of 150BS base oils (account for base oil gross weight 49.8%), continue dehydration and be warmed up to 180 ℃, constant temperature stops heating after 10 minutes, add 50 kilograms of N-phenyl-a-naphthylamine (for raw material for lubricating grease total amount 5%) and 131 kilograms of 150BS base oils, stirring is cooled to lower than 100 ℃, after homogenizer homogenizing is degassed, obtain finished product.The present embodiment base oil dosage is 66% of raw material for lubricating grease total amount.Salient features is in Table 1.
embodiment 3
In the reactor with agitator, add 150 kilograms of 150BS(account for base oil total amount 30%) and 350 kilograms of total basicnumbers calcium alkylbenzenesulfonate that is 300mgKOH/g (for raw material for lubricating grease total amount 35%), stirring heating is warmed up to 60 ℃, add 50 kg of water and 30 kilograms of HBS(be raw material for lubricating grease total amount 3%), stirring is warmed up to 80～95 ℃ of constant temperature conversion reactions, until transform completely, (uses the unformed carbonic acid calcium of infrared spectroscopy monitor at 862cm
-1the charateristic avsorption band at place disappears, and approximately reacts 0.5 hour to 1 hour).Add 50 kilograms of nano-calcium carbonates (for raw material for lubricating grease total amount 5%), stir 5 minutes, then order add 10 kilograms of boric acid (for raw material for lubricating grease total amount 1%) with the hot solution of 50 kg of water, 30 kilograms of 12-oxystearic acids (be raw material for lubricating grease total amount 3%), stir dewater and add 250 kilograms of HVI150(be raw material for lubricating grease total amount 50%), continue dehydration and be warmed up to 180 ℃, constant temperature stops heating after 10 minutes, add 30 kilograms of N-Phenyl beta naphthylamine (for raw material for lubricating grease total amount 3%), 100 kilograms of 150BS, stirring is cooled to lower than 100 ℃, after homogenizer homogenizing is degassed, obtain finished product.The present embodiment base oil dosage is 50% of raw material for lubricating grease total amount.Salient features is in Table 1.
embodiment 4
In the reactor with agitator, add 170 kilograms of 150BS(be base oil total amount 20%) and 100 kilograms of total basicnumbers calcium alkylbenzenesulfonate that is 400mgKOH/g (for raw material for lubricating grease total amount 10%), stirring heating is warmed up to 60 ℃, add 50 kg of water and 10 kilograms of HBS(be raw material for lubricating grease total amount 1%), stirring is warmed up to 80～95 ℃ of constant temperature conversion reactions, until transform completely, (uses the unformed carbonic acid calcium of infrared spectroscopy monitor at 862cm
-1the charateristic avsorption band at place disappears, and approximately reacts 0.5 hour to 1 hour).Add 10 kilograms of nano-calcium carbonates (for raw material for lubricating grease total amount 1%), stir 5 minutes, then order add 5 kilograms of boric acid (for raw material for lubricating grease total amount 0.5%) with the hot solution of 20 kg of water, 5 kilograms of 12-oxystearic acids (be raw material for lubricating grease total amount 0.5%), stir dewater and add 300 kilograms of HVI500(be base oil total amount 35.3%) and 100 kilograms of HVI150(be base oil total amount 11.7%), continue dehydration and be warmed up to 180 ℃, constant temperature stops heating after 10 minutes, add 15 kilograms of N-Phenyl beta naphthylamine (for raw material for lubricating grease total amount 1.5%), 5 kilograms of N-Phenyl beta naphthylamine (be raw material for lubricating grease total amount 0.5%) and 280 kilograms of 150BS, stirring is cooled to lower than 100 ℃, after homogenizer homogenizing is degassed, obtain finished product.The present embodiment base oil dosage is 85% of raw material for lubricating grease total amount.Salient features is in Table 1.
embodiment 5
In the reactor with agitator, add 240 kilograms of 150BS(be base oil total amount 37.5%) and 200 kilograms of total basicnumbers calcium alkylbenzenesulfonate that is 300mgKOH/g (for raw material for lubricating grease total amount 20%), stirring heating is warmed up to 60 ℃, add 50 kg of water and 20 kilograms of HBS(be raw material for lubricating grease total amount 2%), stirring is warmed up to 80～95 ℃ of constant temperature conversion reactions, until transform completely, (uses the unformed carbonic acid calcium of infrared spectroscopy monitor at 862cm
-1the charateristic avsorption band at place disappears, and approximately reacts 0.5 hour to 1 hour).Add 50 kilograms of nano-calcium carbonates (for raw material for lubricating grease total amount 5%), stir 5 minutes, then order add 30 kilograms of boric acid (for raw material for lubricating grease total amount 3%) with the hot solution of 100 kg of water, 40 kilograms of 12-oxystearic acids (be raw material for lubricating grease total amount 4%), stir dewater and add 300 kilograms of HVI500(be base oil total amount 46.9%), continue dehydration and be warmed up to 180 ℃, constant temperature stops heating after 10 minutes, add 10 kilograms of N-Phenyl beta naphthylamine (for raw material for lubricating grease total amount 1%), 10 kilograms of di-iso-octyldiphenylamines (be raw material for lubricating grease total amount 1%) and 100 kilograms of HVI500, stirring is cooled to lower than 100 ℃, after homogenizer homogenizing is degassed, obtain finished product.The present embodiment base oil dosage is 64% of raw material for lubricating grease total amount.Salient features is in Table 1.
The each embodiment performance analysis data of table 1
Note is 1.: lubricating grease is placed in to watch-glass, then puts into constant temperature in the baking oven of 180 ℃ 3 hours, observe the softening situation of lubricating grease.
By analysis, thermal stability and the extreme pressure and antiwear behavior of the composite calcium sulfonate grease lubricant containing nano-calcium carbonate of embodiment 1-5 gained are better than common composite calcium sulfonate grease lubricant.Its transformation time also shortens dramatically.
Finally it should be noted that: the foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, although the present invention is had been described in detail with reference to previous embodiment, for a person skilled in the art, its technical scheme that still can record aforementioned each embodiment is modified, or part technical characterictic is wherein equal to replacement.Within the spirit and principles in the present invention all, any modification of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (3)
1. containing a composite calcium sulfonate grease lubricant for nano-calcium carbonate, it is characterized in that the feed composition that comprises following weight percentage:
Mineral base oil, 50-85%;
High base number calcium alkylbenzenesulfonate, 10-40%;
Nano-calcium carbonate, 1-10%;
Boric acid, 0.5-5%;
C
12-C
22saturated fatty acid, 0.5-5%;
The compound inversion accelerating agent of HBS, 1-5%;
Antioxidant, 0.1-5%,
Wherein,
Described high base number calcium alkylbenzenesulfonate total basicnumber is 250-400mgKOH/g;
Described antioxidant is amine type high-temperature antioxidant;
The particle diameter of described nano-calcium carbonate is 5-100 nanometer;
Described C
12-C
22saturated fatty acid is the lipid acid of hydroxyl;
40 ℃ of kinematic viscosity of described mineral base oil are 30-500mm
2/ s, described mineral base oil is MVI150, MVI500, HVI150, HVI200, HVI500,150BS, 120BS or No. 100 machinery oil, or any two or more mixture wherein;
The described composite calcium sulfonate grease lubricant containing nano-calcium carbonate makes as follows:
The 20-50% of mineral base oil gross weight and high base number calcium alkylbenzenesulfonate are added in reactor, stirring reaction is heated to 60 ± 5 ℃, then add water and the compound inversion accelerating agent of HBS of raw material for lubricating grease total amount 1-10%, stir and be warmed up to 80-95 ℃, conversion reaction is complete;
In the reaction solution of step (1), add nano-calcium carbonate, stir, then to add part by weight be the boric acid of 1:2-5 and the hot solution of water, C to order
12-C
22saturated fatty acid, stirs the 30-65% that dewaters and add mineral base oil gross weight, is warmed up to 180 ℃, reacts 10 minutes; Stop heating, add antioxidant and residue mineral base oil, stir and be cooled to below 100 ℃;
By degassed step (2) gained mixture homogenization, obtain finished product.
2. the composite calcium sulfonate grease lubricant containing nano-calcium carbonate according to claim 1, is characterized in that, described antioxidant is di-iso-octyldiphenylamine, N-phenyl-a-naphthylamine or N-Phenyl beta naphthylamine, or two or more mixture arbitrarily wherein.
3. the composite calcium sulfonate grease lubricant containing nano-calcium carbonate according to claim 1, is characterized in that, described boric acid is commercially available boric acid, and the content of boric acid is greater than 90%.
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| US10519393B2 (en) | 2016-05-18 | 2019-12-31 | Nch Corporation | Composition and method of manufacturing calcium magnesium sulfonate greases |
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| CN107090343A (en) * | 2017-05-25 | 2017-08-25 | 曹平 | A kind of high energy conductive lubricating cream |
| CN108192696B (en) * | 2017-12-29 | 2020-09-01 | 上海峰竺复合新材料科技有限公司 | Calcium carbonate whisker modified composite calcium sulfonate lubricating grease and preparation method thereof |
| CN109627805B (en) * | 2019-01-15 | 2021-04-30 | 广西大学 | Preparation method and application of modified nano calcium carbonate |
| CN109762632B (en) * | 2019-01-15 | 2021-12-10 | 广西碳酸钙产业化工程院有限公司 | High-performance composite calcium sulfonate-based lubricating grease containing calcium carbonate and preparation method thereof |
| US11661563B2 (en) | 2020-02-11 | 2023-05-30 | Nch Corporation | Composition and method of manufacturing and using extremely rheopectic sulfonate-based greases |
| CN114958469B (en) * | 2022-06-30 | 2023-02-21 | 南京科润工业介质股份有限公司 | Trace lubricating oil containing nano calcium sulfonate |
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