CN102839036A - Water base extreme pressure wear resistance multifunctional additive and preparation method thereof, and water base lubricating liquid composition - Google Patents
Water base extreme pressure wear resistance multifunctional additive and preparation method thereof, and water base lubricating liquid composition Download PDFInfo
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- CN102839036A CN102839036A CN2011101702718A CN201110170271A CN102839036A CN 102839036 A CN102839036 A CN 102839036A CN 2011101702718 A CN2011101702718 A CN 2011101702718A CN 201110170271 A CN201110170271 A CN 201110170271A CN 102839036 A CN102839036 A CN 102839036A
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Abstract
The present invention provides a water base sulfur-phosphorous type extreme pressure wear resistance multifunctional additive and a preparation method thereof, and a water base lubricating liquid composition containing the additive. The additive is prepared by the following steps: (1) carrying out a reaction of fatty acid amide containing at least a hydroxyl group and P2S5 for 1-8 h at a temperature of 80-120 DEG C to generate sulfuric phosphoric acid; and (2) carrying out a reaction of the sulfuric phosphoric acid generated in the step (1) and alcohol amine for 1-6 h at a temperature of 50-90 DEG C to prepare the finished product. The water base sulfur-phosphorous type extreme pressure wear resistance multifunctional additive has characteristics of excellent extreme pressure wear resistance, good corrosion resistance, good rust resistance, and good solubility in a water base lubricating liquid.
Description
Technical field
The present invention relates to a kind of extreme-pressure anti-wear multifunction additive, relate in particular to a kind of water base sulphur phosphorus type extreme-pressure anti-wear multifunction additive.
Background technology
Over nearly 20 years, water-based lubricating liquid is owing to have good economy, cooling property and security, and helps energy-conservation and environmental protection, has been widely used in difficult combustion water-base hydraulic fluid and the metal processing treatment liquid, thereby constantly developed.Water-based lubricating liquid is the important factor that the water-based lubricating liquid quality improves with wear preventive additive, so water-based lubricating liquid is one of research emphasis of this area with the research of wear preventive additive.The used wear preventive additive of traditional water-based lubricating liquid generally all is oil-soluble; With tensio-active agent it is distributed in the water, these oil-soluble wear preventive additives generally are divided into oiliness improver and extreme pressure agent again, and the former mainly works under underload; Be generally long carbochain ester and carboxylic acid; They are adsorbed in the metallic surface and form what is called " oil film ", help the slip between the metallic contact face and play antifriction function, but " oil film " break and lose efficacy under high loading; The latter is worked under high loading, contains sulphur, phosphorus, boron isoreactivity element usually, forms iron sulphide in the metallic surface, iron phosphate membrane and working.Another kind of new water base anti-wear agent is the synthesizing water-solubility anti-wear agent, it overcome the oil soluble anti-wear agent unstable in water, be subject to water quality impact, disperse characteristics uneven, that be difficult to each position of effectively lubricating metal.The group that plays water-soluble effect in the water-soluble anti-wear agent is generally polyglycol chain, carboxyl, ammonium ion etc., contains long carbochain simultaneously and plays " oiliness improver " effect, introduces the suitable active element again and just has oiliness improver and extreme pressure agent dual-use function.The multiple function of synthesizing water-solubility anti-wear agent makes that the water-based lubricating liquid composition that forms is comparatively simple, and available tap water preparation is not only stable, energy-conservation, also is beneficial to the performance of anti-wear agent abrasion resistance.
The article " oilness of malonate derivative " that is published in " Hunan University's journal " in October, 1996 has disclosed the technical scheme that ZDTP is modified as thiophosphatephosphorothioate monocarboxylic acid verivate; The author introduces the propanedioic acid group in the thiophosphoric acid ester molecular structure; Thereby synthesized novel water-soluble anti-wear agent, had the water-soluble lubricant additive of extreme pressure agent and oiliness improver double effects through the anti-wear agent of modification simultaneously.Synthesized a kind of water-soluble oleic acid diethylolamine molybdenum among the patent CN00134326, this agent has good extreme pressure, wear-resistant, antifriction performance.
Summary of the invention
The object of the present invention is to provide a kind of water base extreme-pressure anti-wear multifunction additive and preparation method thereof, this additive has excellent extreme pressure and antiwear behavior, has good anticorrosive, rustless property simultaneously, in water-based lubricating liquid, has the good solubility ability.
The present invention also provides a kind of water based lubrication fluid composition.
A kind of water base extreme-pressure anti-wear multifunction additive, its preparation method may further comprise the steps:
(1) will contain the fatty acid amide and the P of a hydroxyl at least
2S
5Between 80 ℃～120 ℃, react 1h～8h and generate sulphur phosphoric acid;
(2) the sulphur phosphoric acid and the hydramine that step (1) are generated prepare at 50 ℃～90 ℃ reaction 1h～6h.
At the fatty acid amide described in the step (1) is the condensation product that the N-acylation reaction takes place for lipid acid and hydramine; Said lipid acid contains the saturated or undersaturated alkyl between C10～C20, the alkyl between preferred C12～C18, the most preferably unsaturated alkyl between C12～C18; Said hydramine is selected from primary amine and/or the secondary amine that contains a hydroxyl at least; The primary amine and/or the secondary amine that preferably contain 1-5 hydroxyl, most preferred ethanol amine and/or diethylolamine, said fatty acid amide and said P
2S
5Mol ratio between 1: 1 and 8: 1, preferably between 2: 1 and 4: 1, preferably between 90 ℃～110 ℃, the reaction times is preferably between 2h～6h for temperature of reaction.
Be selected from primary amine, secondary amine and the tertiary amine that contains at least one hydroxyl one or more at the described hydramine of step (2); Preferably contain in primary amine, secondary amine and the tertiary amine of 1-5 hydroxyl one or more; In most preferred ethanol amine, diethylolamine and the trolamine one or more, the mol ratio of said sulphur phosphoric acid and said hydramine are between 0.25: 1 and 4: 1, preferably between 0.5: 1 and 2: 1; Preferred 60 ℃～80 ℃ of temperature of reaction, preferred 1h～4h of reaction times.
In the water base extreme-pressure anti-wear multifunction additive of the present invention the massfraction of sulphur content between 5%～10%, the massfraction of phosphorus content between 2%～8%, the massfraction of nitrogen content is between 3%～10%.
A kind of method for preparing above-mentioned water base extreme-pressure anti-wear multifunction additive comprises:
(1) will contain the fatty acid amide and the P of a hydroxyl at least
2S
5Between 80 ℃～120 ℃, react 1h～8h and generate sulphur phosphoric acid;
(2) the sulphur phosphoric acid and the hydramine that step (1) are generated react 1h～6h at 50 ℃～90 ℃, collect product.
The present invention also provides a kind of water based lubrication fluid composition; Contain above-mentioned water base extreme-pressure anti-wear multifunction additive and water based lubrication basal liquid in the said composition; Said water base extreme-pressure anti-wear multifunction additive accounts for 0.1%～5% of compsn total mass, preferably between 0.2%～2%.Said water based lubrication basal liquid is water and/or terepthaloyl moietie.The slip additive that can also contain other kind in this lubricating fluid compsn is like in oxidation inhibitor, dispersion agent and the rust-preventive agent one or more.
Water base extreme-pressure anti-wear multifunction additive of the present invention has excellent extreme pressure, wear-resistant and anticorrosive, rustless property, in water-based lubricating liquid, has the good solubility ability.
Water based lubrication fluid composition of the present invention has excellent extreme pressure and antiwear behavior and anticorrosive, rustless property.
Embodiment
Except that special declaration, various content are all represented with massfraction in the present invention.
The mensuration of sulphur, phosphorus content adopts ASTM D5185 method in the additive of the present invention, and the mensuration of nitrogen content adopts SH/T 0224 method, and the mensuration of carbon content adopts SH/T 0656 method.
Instance 1
In the there-necked flask that electronic stirring, return line, TM are housed; 0.4mol oleic acid diethylolamine and 0.1mol thiophosphoric anhydride are heated to 90 ℃, and reaction 6h reduces to then and adds the 0.2mol trolamine behind the normal temperature; Be heated to 70 ℃ of reaction 1.5h, thereby make product A.The sulphur content of product A is 6.21%, phosphorus content is 5.98%, nitrogen content is 5.13%, carbon content is 68.14%.
Additive of the present invention comprises the reaction product of multiple structure, has listed the example equation formula of main reaction in the instance 1 below:
Step (1):
The fatty acid amide of being selected for use in the formula is the oleic acid diethylolamine, i.e. the condensation product of oleic acid and diethylolamine.
Step (2):
Instance 2
In the there-necked flask that electronic stirring, return line, TM are housed; 0.4mo l laurostearic acid diethylolamine and 0.1mol thiophosphoric anhydride are heated to 110 ℃, and reaction 6h reduces to then and adds the 0.2mol trolamine behind the normal temperature; Be heated to 80 ℃ of reaction 1.5h, thereby make product B.The sulphur content of product B is 8.30%, phosphorus content is 3.41%, nitrogen content is 6.11%, carbon content is 55.89%.
Instance 3
In the there-necked flask that electronic stirring, return line, TM are housed; 0.4mol lauroleic acid diethylolamine and 0.1mol thiophosphoric anhydride are heated to 100 ℃, and reaction 4h reduces to then and adds the 0.2mol trolamine behind the normal temperature; Be heated to 60 ℃ of reaction 1.5h, thereby make products C.The sulphur content of products C is 7.97%, phosphorus content is 4.0%, nitrogen content is 5.66%, carbon content is 54.50%.
Instance 4
Respectively product A, product B, products C and common water base anti-wear agent dimeracid, oleic acid, triethanolamine oleate are added to concoct in the water-ethylene glycol lubrication base liquid and be the water based lubrication fluid composition; Difference called after embodiment 1～4 and Comparative Examples 1～3; These additives account for the massfraction of compsn total mass and see table 1; Evaluate solubility property and the abrasion resistance of these additives in the water based lubrication basal liquid respectively, the result is with seeing table 1.
Water base anti-wear agent dimeracid and oleic acid all derive from Mudanjiang detergents and cosmetic factory, and triethanolamine oleate derives from Shanghai Gaoqiao petrochemical corporation (complex).
Mass ratio in the water-ethylene glycol lubrication base liquid between water and the terepthaloyl moietie is 1: 1.
Endurance check adopts tetra-ball machine test GB/T3142 method, and test conditions is 1200r/min, 294N, 30min; Liquid-phase corrosion test adopts the GB/T11143 method; GB/T 5096 methods are adopted in copper strip test, and test conditions is 50 ℃, 3h.
Table 1
Can find out that from table 1 the water base extreme-pressure anti-wear multifunction additive of the present invention has good extreme pressure and antiwear behavior, and has good resistance to corrosion and antirust ability concurrently, in water-based lubricating liquid, has the good solubility ability.
Claims (19)
1. water base extreme-pressure anti-wear multifunction additive, its preparation method may further comprise the steps:
(1) will contain the fatty acid amide and the P of a hydroxyl at least
2S
5Between 80 ℃～120 ℃, react 1h～8h and generate sulphur phosphoric acid;
(2) the sulphur phosphoric acid and the hydramine that step (1) are generated react 1h～6h at 50 ℃～90 ℃, collect product.
2. according to the described additive of claim 1; It is characterized in that; Said fatty acid amide is the condensation product that the N-acylation reaction takes place for lipid acid and hydramine; Wherein said lipid acid contains the saturated or undersaturated alkyl between C10～C20, and said hydramine is selected from primary amine and/or the secondary amine that contains a hydroxyl at least.
3. according to the described additive of claim 2, it is characterized in that wherein said lipid acid contains the alkyl between C12～C18, said hydramine is selected from primary amine and/or the secondary amine that contains 1-5 hydroxyl.
4. according to the described additive of claim 2, it is characterized in that wherein said lipid acid contains the unsaturated alkyl between C12～C18, said hydramine is selected from thanomin and/or diethylolamine.
5. according to the described additive of claim 1, it is characterized in that fatty acid amide and said P described in the step (1)
2S
5Mol ratio between 1: 1 and 8: 1.
6. according to the described additive of claim 1, it is characterized in that fatty acid amide and said P described in the step (1)
2S
5Mol ratio between 2: 1 and 4: 1.
7. according to the described additive of claim 1, it is characterized in that temperature of reaction is between 90 ℃～110 ℃ in the step (1).
8. according to the described additive of claim 1, it is characterized in that the reaction times is between 2h-6h in the step (1).
9. according to the described additive of claim 1, it is characterized in that hydramine is selected from one or more in primary amine, secondary amine and the tertiary amine that contains at least one hydroxyl described in the step (2).
10. according to the described additive of claim 1, it is characterized in that hydramine is selected from one or more in primary amine, secondary amine and the tertiary amine that contains 1-5 hydroxyl described in the step (2).
11., it is characterized in that hydramine is selected from one or more in thanomin, diethylolamine and the trolamine described in the step (2) according to the described additive of claim 1.
12. according to the described additive of claim 1, the mol ratio that it is characterized in that sulphur phosphoric acid described in the step (2) and said hydramine is between 0.25: 1 and 4: 1.
13. according to the described additive of claim 1, the mol ratio that it is characterized in that sulphur phosphoric acid described in the step (2) and said hydramine is between 0.5: 1 and 2: 1.
14., it is characterized in that temperature of reaction is between 60 ℃～80 ℃ in the step (2) according to the described additive of claim 1.
15., it is characterized in that preferred 1h～4h of reaction times in the step (2) according to the described additive of claim 1.
16. according to the described additive of claim 1, the massfraction that it is characterized in that sulphur content in the said additive between 5%～10%, the massfraction of phosphorus content between 2%～8%, the massfraction of nitrogen content is between 3%～10%.
17. the preparation method of a water base extreme-pressure anti-wear multifunction additive comprises:
(1) will contain the fatty acid amide and the P of a hydroxyl at least
2S
5Between 80 ℃～120 ℃, react 1h～8h and generate sulphur phosphoric acid;
(2) the sulphur phosphoric acid and the hydramine that step (1) are generated react 1h～6h at 50 ℃～90 ℃, collect product.
18. a water based lubrication fluid composition contains water base extreme-pressure anti-wear multifunction additive and the water based lubrication basal liquid of one of claim 1-16 in the said composition, said water base extreme-pressure anti-wear multifunction additive accounts for 0.1%～5% of compsn total mass.
19., it is characterized in that said water based lubrication basal liquid is water and/or terepthaloyl moietie according to the described water based lubrication fluid composition of claim 18.
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| CN201110170271.8A CN102839036B (en) | 2011-06-23 | 2011-06-23 | Water base extreme pressure wear resistance multifunctional additive and preparation method thereof, and water base lubricating liquid composition |
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|---|---|---|---|
| CN201110170271.8A CN102839036B (en) | 2011-06-23 | 2011-06-23 | Water base extreme pressure wear resistance multifunctional additive and preparation method thereof, and water base lubricating liquid composition |
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| CN102839036A true CN102839036A (en) | 2012-12-26 |
| CN102839036B CN102839036B (en) | 2014-08-20 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110343562A (en) * | 2019-07-09 | 2019-10-18 | 广州市君禾实业有限公司 | A kind of water base extraordinary fatty amine highly-efficient lubricant |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1139151A (en) * | 1994-06-22 | 1997-01-01 | 唐山工程技术学院 | Prepn of efficient antirusting water-base cutting fluid |
| US20020128159A1 (en) * | 2001-01-08 | 2002-09-12 | Swami Krishan Kumar | Process of preparing multi-functional additive for lubricant composition form saturated cashew nut shell liquid |
| CN1673322A (en) * | 2004-03-24 | 2005-09-28 | 中国石油天然气股份有限公司 | Prepn of nitrogen sulfate phosphate type phosphorus-containing agent |
-
2011
- 2011-06-23 CN CN201110170271.8A patent/CN102839036B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1139151A (en) * | 1994-06-22 | 1997-01-01 | 唐山工程技术学院 | Prepn of efficient antirusting water-base cutting fluid |
| US20020128159A1 (en) * | 2001-01-08 | 2002-09-12 | Swami Krishan Kumar | Process of preparing multi-functional additive for lubricant composition form saturated cashew nut shell liquid |
| CN1673322A (en) * | 2004-03-24 | 2005-09-28 | 中国石油天然气股份有限公司 | Prepn of nitrogen sulfate phosphate type phosphorus-containing agent |
Non-Patent Citations (2)
| Title |
|---|
| 《润滑与密封》 19940815 易伦等 "水溶性抗磨添加剂的研究" 第6-10、34页 1-19 , * |
| 易伦等: ""水溶性抗磨添加剂的研究"", 《润滑与密封》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110343562A (en) * | 2019-07-09 | 2019-10-18 | 广州市君禾实业有限公司 | A kind of water base extraordinary fatty amine highly-efficient lubricant |
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| CN102839036B (en) | 2014-08-20 |
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