CN102533417B - Method for preparing nano-attapulgite lubricating grease - Google Patents
Method for preparing nano-attapulgite lubricating grease Download PDFInfo
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- CN102533417B CN102533417B CN201110397390.7A CN201110397390A CN102533417B CN 102533417 B CN102533417 B CN 102533417B CN 201110397390 A CN201110397390 A CN 201110397390A CN 102533417 B CN102533417 B CN 102533417B
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Abstract
The invention discloses a method for preparing nano-attapulgite lubricating grease, belonging to the technical field of the preparation of the lubricating grease. The lubricating grease is formed by the following ingredients in part by weight: 10-70 parts of surface-modified attapulgite, 0-15 parts of lubricating grease additive, 4-40 parts of polarity dispersant and 25-85 parts of base oil. The nano-attapulgite lubricating grease prepared by the method disclosed by the invention has the advantages of stable performance, excellent abrasion resistance and capability of meeting the working requirements on the lubricating grease for mechanisms of mechanical equipment, such as gears, bearings, instruments and meters and the like under harsh conditions. The method disclosed by the invention is simple in operation, and the prepared nano-attapulgite lubricating grease is transparent in appearance and has excellent high-temperature performance and excellent wear-resisting and bearing capability, so that an application basis for the application of attapulgite in the lubrication industry is pioneered.
Description
Technical field
The invention belongs to lubricating grease preparing technical field, be specifically related to a kind of nano-attapulgite preparation of greases method.
Background technology
Lubricating grease has plurality of advantages and widespread use in metallurgy, mine and production obtain friction pair, progress along with industrial technology, make mechanical means towards long lifetime future development, make the mechanical means under severe condition (high temperature, at a high speed, the direction such as high loading) more and more higher to the performance of lubricating grease and life requirements.From plain mineral oil type lubricating grease to synthetic oil future development, high-performance synthetic grease is the trend of the development of lubricating grease.Up to the present, yet there are no the report of making grease thickener about attapulgite.
Non-saponification lubricating grease be take bentone grease as representative, the advantage such as bentone grease has that high dropping point, thick warm nature are good, humidity, chemically stable are good, and there is good biodegradability, so bentone grease is widely used.Attapulgite is a kind of clay mineral that attapulgite is main component of take, Attapulgite crystal is bar-shaped, fibrous form, diameter 20～40nm, length 0.5～1 μ m, is a kind of natural nano material, a kind of ore deposit soil of natural environmental-protective, containing heavy metal and toxicant, environment-friendly degradable, is a kind of starting material that can widespread use.China's attapulgite clay is mainly distributed in the ground such as Xuyi in China Jiangsu, and it is formed in the basalt of the new Tr.Area, Xuyi attapulgite clay is of high grade, reserves are large, high-quality attapulgite clay reserves have been verified more than 6,700 ten thousand tons in area, Xuyi, useful clay total amount reaches more than 500,000,000 tons, account for the 65-70% of China's reserves, due to special physicochemical property and the processing performance that attapulgite clay has, it is used widely at aspects such as oil, chemical industry, building materials, papermaking, medicine, agriculturals.Domestic current consumption maximum be coating, drilling mud, edible oil decolouring etc.We study discovery, the structure of attapulgite and bentonitic structural similitude, and after organic decoration, can make grease thickener, prepare lubricating grease.
Summary of the invention
The object of the present invention is to provide a kind of nano-attapulgite preparation of greases method.
A preparation of greases method, carry out in accordance with the following steps:
(1) attapulgite is carried out to finishing with organic ammonium salt, the consumption of organic ammonium salt is the 30-70% of attapulgite quality;
(2) in reaction vessel, add base oil, the attapulgite through finishing is slowly added in reaction vessel, stir 30-120min, mix;
(3) add polarity dispersion aids, mix and blend 60-120min, mixes;
(4) be heated to 60-120 ℃, insulation 120-180min;
(5) be cooled to 50-80 ℃, add additive and base oil, stir and be incubated 60-120min, coolingly by grinding, obtain nano-attapulgite lubricating grease.
The weight of nano-attapulgite lubricating grease of take is benchmark, and base oil content is 25-85%, and the content of the attapulgite of finishing is 10-70%, and the content of polarity dispersion agent is 4-40%, and the content of grease additive is 0-15%.
Described organic ammonium salt is cetyl trimethylammonium bromide, Cetyltrimethylammonium bromide, the two decyl ammonium chloride of dimethyl or dimethyl stearyl benzyl ammonium chloride.
Described base oil is mineral oil, synthetic oil or vegetable and animals oils.
Described polarity dispersion agent is ethanol, acetone, sherwood oil or water.
Described grease additive is one or more in oxidation inhibitor, extreme pressure agent, anti-wear agent.
Described oxidation inhibitor is one or more in alkyl zinc dithiophosphate, pentanoic, 2,6 ditertbutylparacresols; Described extreme pressure agent is one or more in alkylphosphonic acid carboxylic acid amine, alkoxyl group phosphamide, nano-calcium carbonate; Described anti-wear agent is one or more in molybdenumdisulphide, molybdenum dialkyldithiocarbamacompositions, alkyl zinc dithiophosphate.
Beneficial effect of the present invention: nano-attapulgite PERFORMANCE OF GREASES of the present invention is stable, resistance to abrasion is good, can meet mechanical means under severe condition, as the job requirement of mechanism's lubricating grease such as gear, bearing, instrument and instrument.Method of the present invention provides nano-attapulgite preparation of greases method, not only simple to operate, and the nano-attapulgite lubricating grease appearance transparent of preparation, there is good high temperature resistant property and excellent wear-resistant and supporting capacity, for attapulgite has been opened up application foundation in lubricated industrial application.
Embodiment
With specific embodiment, the present invention will be further described below.
Embodiment 1
Nano-attapulgite preparation of greases method, carry out in accordance with the following steps:
(1) 18g attapulgite is carried out to finishing with 6g cetyl trimethylammonium bromide, make the attapulgite of 24g finishing;
(2) get the polyalphaolefin 140g that 100 ℃ of viscosity are 40cSt and join in container, the attapulgite through finishing is slowly added in reaction vessel, stir 30min, mix;
(3) add 12g acetone, mix and blend 60min, mixes;
(4) be heated to 100 ℃, insulation 120min;
(5) be cooled to 60 ℃, add polyalphaolefin and the 10g molybdenum disulfide powder of 36g surplus, 2g 2,6 ditertbutylparacresols, stir and are incubated 60min, and cooling rear use three roller shredders grind three times repeatedly, obtain nano-attapulgite lubricating grease.
The product main performance index making is as table 1:
The dropping point of table 1 nano-attapulgite lubricating grease and cone penetration value
| Test item | Detection method | |
| Dropping point/℃ | 322 | GB/T 3498 |
| Cone penetration | 328 | GB/T 269 |
The result of fine motion rub(bing)test:
The contact of some face, and mating material: GCr15 (hardness: 700HRC, to dual diameter: 10mm, load: 200N, time 30min.
Embodiment 2
Nano-attapulgite preparation of greases method, carry out in accordance with the following steps:
(1) 20g attapulgite is carried out to finishing with 10g cetyl trimethylammonium bromide, make the attapulgite of 30g finishing;
(2) get the polyalphaolefin 80g that 100 ℃ of viscosity are 40cSt and join in container, the attapulgite through finishing is slowly added in reaction vessel, stir 60min, mix;
(3) add 8g sherwood oil, mix and blend 40min, mixes;
(4) be heated to 100 ℃, insulation 150min;
(5) be cooled to 50 ℃, add polyalphaolefin and the 6g alkylphosphonic acid carboxylic acid amine of 80g surplus, stir and be incubated 80min, cooling rear use three roller shredders grind three times repeatedly, obtain nano-attapulgite lubricating grease.
The product main performance index making is as table 2:
The dropping point of table 2 nano-attapulgite lubricating grease and cone penetration value
| Test item | Detection method | |
| Dropping point/℃ | 328 | GB/T 3498 |
| Cone penetration | 256 | GB/T 269 |
The result of fine motion rub(bing)test:
The contact of some face, and mating material: GCr15 (hardness: 700HRC, to dual diameter: 10mm, load: 200N, time 30min.
Embodiment 3
Nano-attapulgite preparation of greases method, carry out in accordance with the following steps:
(1) 18g attapulgite is carried out to finishing with 6g Cetyltrimethylammonium bromide, make the attapulgite of 24g finishing;
(2) get the paraffin base mineral oil 60g that 100 ℃ of viscosity are 40cSt and join in container, the attapulgite through finishing is slowly added in reaction vessel, stir 80min, mix;
(3) add 10g ethanol, mix and blend 100min, mixes;
(4) be heated to 100 ℃, insulation 100min;
(5) be cooled to 50 ℃, add paraffin base mineral oil and 6g molybdenum disulfide powder and the 4g alkoxyl group phosphamide of 80g surplus, stir and be incubated 180min, cooling rear use three roller shredders grind three times repeatedly, obtain nano-attapulgite lubricating grease.
The product main performance index making is as table 3:
The dropping point of table 3 nano-attapulgite lubricating grease and cone penetration value
| Test item | Detection method | |
| Dropping point/℃ | 303 | GB/T 3498 |
| Cone penetration | 287 | GB/T 269 |
The result of fine motion rub(bing)test:
The contact of some face, and mating material: GCr15 (hardness: 700HRC, to dual diameter: 10mm, load: 200N, time 30min.
Embodiment 4
Nano-attapulgite preparation of greases method, carry out in accordance with the following steps:
(1) 20g attapulgite is carried out to finishing with the two decyl ammonium chloride of 10g dimethyl, make the attapulgite of 30g finishing;
(2) get the polyethers 50g that 100 ℃ of viscosity are 40cSt and join in container, the attapulgite through finishing is slowly added in reaction vessel, stir 120min, mix;
(3) add 20g water, mix and blend 180min, mixes;
(4) be heated to 120 ℃, insulation 180min;
(5) be cooled to 70 ℃, add polyethers and the 4g nano-calcium carbonate of 80g surplus, 2g pentanoic stirs and is incubated 180min, and cooling rear use three roller shredders grind three times repeatedly, obtain nano-attapulgite lubricating grease.
The product main performance index making is as table 4:
The dropping point of table 4 nano-attapulgite lubricating grease and cone penetration value
| Test item | Detection method | |
| Dropping point/℃ | 331 | GB/T 3498 |
| Cone penetration | 302 | GB/T 269 |
The result of fine motion rub(bing)test:
The contact of some face, and mating material: GCr15 (hardness: 700HRC, to dual diameter: 10mm, load: 200N, time 30min.
Embodiment 5
Nano-attapulgite preparation of greases method, carry out in accordance with the following steps:
(1) 12g attapulgite is carried out to finishing with the two decyl ammonium chloride of 6g dimethyl, make the attapulgite of 18g finishing;
(2) get the silicone oil 50g that 100 ℃ of viscosity are 40cSt and join in container, the attapulgite through finishing is slowly added in reaction vessel, stir 90min, mix;
(3) add 10g sherwood oil, mix and blend 150min, mixes;
(4) be heated to 100 ℃, insulation 180min;
(5) be cooled to 60 ℃, add silicone oil and 2g molybdenum dialkyldithiocarbamacompositions and the 6g alkyl zinc dithiophosphate of 75g surplus, stir and be incubated 180min, cooling rear use three roller shredders grind three times repeatedly, obtain nano-attapulgite lubricating grease.
The product main performance index making is as table 5:
The dropping point of table 5 nano-attapulgite lubricating grease and cone penetration value
| Test item | Detection method | |
| Dropping point/℃ | 318 | GB/T 3498 |
| Cone penetration | 278 | GB/T 269 |
The result of fine motion rub(bing)test:
The contact of some face, and mating material: GCr15 (hardness: 700HRC, to dual diameter: 10mm, load: 200N, time 30min.
Claims (6)
1. a nano-attapulgite preparation of greases method, is characterized in that, carries out in accordance with the following steps:
(1) attapulgite is carried out to finishing with organic ammonium salt, the consumption of organic ammonium salt is the 30-70% of attapulgite quality;
(2) in reaction vessel, add base oil, the attapulgite through finishing is slowly added in reaction vessel, stir 30-120min, mix;
(3) add polarity dispersion aids, mix and blend 60-120min, mixes;
(4) be heated to 60-120 ℃, insulation 120-180min;
(5) be cooled to 50-80 ℃, add grease additive and base oil, stir and be incubated 60-120min, coolingly by grinding, obtain nano-attapulgite lubricating grease;
Described organic ammonium salt is cetyl trimethylammonium bromide, Cetyltrimethylammonium bromide, the two decyl ammonium chloride of dimethyl or dimethyl stearyl benzyl ammonium chloride.
2. a kind of nano-attapulgite preparation of greases method according to claim 1, it is characterized in that, the weight of nano-attapulgite lubricating grease of take is benchmark, base oil content is 25-85%, the content of the attapulgite of finishing is 10-70%, the content of polarity dispersion agent is 4-40%, and the content of grease additive is 0-15%.
3. a kind of nano-attapulgite preparation of greases method according to claim 1, is characterized in that, described base oil is mineral oil, synthetic oil or vegetable and animals oils.
4. a kind of nano-attapulgite preparation of greases method according to claim 1, is characterized in that, described polarity dispersion agent is ethanol, acetone, sherwood oil or water.
5. a kind of nano-attapulgite preparation of greases method according to claim 1, is characterized in that, described grease additive is one or more in oxidation inhibitor, extreme pressure agent, anti-wear agent.
6. a kind of nano-attapulgite preparation of greases method according to claim 5, is characterized in that, described oxidation inhibitor is one or more in alkyl zinc dithiophosphate, pentanoic, 2,6 ditertbutylparacresols; Described extreme pressure agent is one or more in alkylphosphonic acid carboxylic acid amine, alkoxyl group phosphamide, nano-calcium carbonate; Described anti-wear agent is one or more in molybdenumdisulphide, molybdenum dialkyldithiocarbamacompositions, alkyl zinc dithiophosphate.
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| CN201110397390.7A CN102533417B (en) | 2011-12-02 | 2011-12-02 | Method for preparing nano-attapulgite lubricating grease |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108059998A (en) * | 2018-01-30 | 2018-05-22 | 中国科学院宁波材料技术与工程研究所 | A kind of extreme pressure high temperature attapulgite lubricant composition, its preparation method and application |
| CN108410543A (en) * | 2018-04-19 | 2018-08-17 | 翟琳 | A kind of fire-retardant preparation of greases method of concave convex rod soil matrix |
| CN112646640B (en) * | 2020-12-23 | 2022-04-08 | 中国科学院兰州化学物理研究所 | Modified composite calcium sulfonate-based lubricating grease and preparation method thereof |
| CN114045185B (en) * | 2021-10-18 | 2022-08-19 | 安徽中天石化股份有限公司 | Perfluoropolyether lubricating grease and preparation method thereof |
| CN115418259B (en) * | 2022-09-20 | 2023-06-27 | 西南交通大学 | Grease thickening agent and preparation method thereof, and grease and preparation method thereof |
| CN115851339B (en) * | 2022-10-24 | 2024-02-06 | 佛山科学技术学院 | Online repair type lubricating grease and preparation method and application thereof |
Citations (1)
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|---|---|---|---|---|
| CN1566295A (en) * | 2003-06-30 | 2005-01-19 | 中国石油化工股份有限公司 | Process for producing water based lubricating liquid |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1566295A (en) * | 2003-06-30 | 2005-01-19 | 中国石油化工股份有限公司 | Process for producing water based lubricating liquid |
Non-Patent Citations (4)
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| 丁旭等.纳米坡缕石的表面修饰及摩擦学性能研究.《润滑与密封》.2010,(第10期),39-41. |
| 凹凸棒土有机改性的研究;张良等;《涂料工业》;20071101(第11期);41-43 * |
| 张良等.凹凸棒土有机改性的研究.《涂料工业》.2007,(第11期), |
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