CN105062643A - Boric acid and phosphoric acid containing fatty ester, preparation method thereof and minimal quantity lubricating oil prepared from boric acid and phosphoric acid containing fatty ester - Google Patents
Boric acid and phosphoric acid containing fatty ester, preparation method thereof and minimal quantity lubricating oil prepared from boric acid and phosphoric acid containing fatty ester Download PDFInfo
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Abstract
The invention relates to boric acid and phosphoric acid containing fatty ester. The boric acid and phosphoric acid containing fatty ester is characterized by being prepared from components in percentage by weight as follows: 80%-90% of fatty alcohol, 5%-10% of phosphoric acid and 5%-10% of boric acid. The invention further provides minimal quantity lubricating oil prepared from the boric acid and phosphoric acid containing fatty ester. The minimal quantity lubricating oil is characterized by being prepared from components in percentage by weight as follows: 10%-20% of the boric acid and phosphoric acid containing fatty ester, 70%-80% of synthetic ester, 5%-10% of polyester and 5%-10% of acyl sarcosine or sodium salt of acyl sarcosine. When the minimal quantity lubricating oil cooperates with a minimal quantity lubricating device for use, the use amount can be reduced to be lower than 5% of the conventional use amount, and the minimal quantity lubricating oil can have good lubricating, cooling and rust prevention effects and has obvious energy saving and emission reduction benefits and environmental protection benefits.
Description
Technical field
The invention belongs to lubrication technical field, be specifically related to a kind of boric acid phosphoric acid fatty ester and preparation method thereof and prepare micro lubricating oil with this ester.
Background technology
Traditional metal cutting process adopts mineral oil or vegetables oil or cutting fluid to carry out a large amount of shower formula lubrication and cooling, the usage quantity of lubricant is large, not only waste resource, cause the huge pollution of processing site and environment, also can have a strong impact on the healthy of operator simultaneously.Advocating today of energy-saving and emission-reduction, environment protection, green production, be badly in need of a kind of new metal cutting process technique.
Minimal Quantity Lubrication Technology is the metallic green New Machining Technology grown up in recent years, in metal cutting process, use lubricating system with trace amount by extreme pressure anti-wear exactly, micro lubricating oil that oilness is good is sprayed on process tool and finished surface carries out lubricating, cooling, solve tradition and add the problems such as machining oil in man-hour, liquid usage quantity is large, waste spillage is large.But cool owing to employing a large amount of pressurized air, business electrical amount rises, and simultaneously for meeting need of production, also will carry out the buying of air compressor machine.
Our company successfully have developed the oil-water-gas three-phase energy saving micro oiling system as CN103722447A, efficiently solves the cooling problem in Minimal quantity of lubrication oil, the air of cooling can be made to amplify more than 10 times simultaneously, reduces air compressor power consumption 70-90%.But the type of cooling of a large amount of heats is taken away owing to employing water vapor, phenomenon of getting rusty is there will be during processing ferrous metal, lubrication is carried out in the special micro lubricating agent that use is produced as oil-water-gas three-phase lubricating system with trace amount special micro lubricating agent of CN104031732A and preparation method thereof, there are 2 problems: it is cumbersome that 1.B agent adds water tank, often abandoned by workman in actual production process; 2.B agent in use may have fraction solids do not dissolve and be added in water tank, causes the problems such as the blocking of energy-conserving spray nozzle.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of boric acid phosphoric acid fatty ester is provided.
Boric acid phosphoric acid fatty ester provided by the invention, is prepared from by the component of following weight percent:
Fatty alcohol 80-90%
Phosphoric acid 5-10%
Boric acid 5-10%.
Above-mentioned fatty alcohol can be selected from fatty alcohol, and to be selected from carbonatoms be one or more mixtures in the saturated or unsaturated fatty alcohol of 6 to 24; One or more mixtures most preferably in n-hexyl alcohol, isooctyl alcohol, nonylcarbinol, lauryl alcohol, different tridecanol, oleyl alcohol, stearyl alcohol, n-Eicosanol.
The preparation method of above-mentioned boric acid phosphoric acid fatty ester is: take fatty alcohol, phosphoric acid, boric acid by weight percentage, add in reactor respectively, the air in reactor is changed out with rare gas element, be heated to 160-180 DEG C, reaction 8-12 hour, the moisture that the reaction of decompression remove portion generates, when reactor temperature drops to below 100 DEG C (, reaction generate moisture decompression and temperature-fall period in most of spontaneous evaporation), be a kind of boric acid phosphoric acid fatty ester.
Present invention also offers a kind of micro lubricating oil, be prepared from by the component of following weight percent:
Above-mentioned synthetic ester comprises one or more in polyol ester, monoesters, dibasic acid esters.
Above-mentioned polyol ester is the synthetic ester being carried out esterification synthetic gained by polyvalent alcohol and unary fatty acid, preferably from three isocaprylic acid glyceryl ester, trimethylolpropane tricaprylate, tetramethylolmethane four 2-ethylhexoate, trilaurin, trimethylolpropane trilaurate, tetramethylolmethane four laurate, triolein, trimethylolpropane tris oleic acid ester, tetramethylolmethane four oleic acid ester, tripalmitin, trimethylolpropane tris cetylate, tetramethylolmethane four cetylate etc.
Above-mentioned monoesters refers to ester prepared by monohydroxy-alcohol and unary fatty acid, the straight chain fatty acid that preferred free natural fats and oils derives and the ester that the esterification of unitary low-carbon alcohol is obtained by reacting, most preferably from Witconol 2301, Laurate methyl, Laurate ethyl, methyl stearate, Stearic ethyl stearate, Uniphat A60, ethyl palmitate, ethyl oleate, butyl oleate etc.
Above-mentioned dibasic acid esters is the product of dibasic alcohol and monoprotic acid or diprotic acid and the generation of monohydroxy-alcohol esterification, preferably from Octyl adipate, dioctyl azelate, dioctyl sebacate, DDA, two different decayl esters of azelaic acid, DI(2ETHYLHEXYL)SEBACATE, succinic acid di-isooctyl, DID Su, ethylene glycol laurate, propylene glycol oleate etc.This type of dibasic acid esters has good oilness, and kinematic viscosity is low, and low-temperature performance is good, and biodegradability is excellent.
Above-mentioned acyl group sarkosine or its sodium salt are the products that lipid acid and sarkosine carry out acylation reaction, one or more preferably in Sarkosyl L, sodium lauroyl sareosine, myristoyl-N-methylaminoacetic acid, myristoyl-N-methylaminoacetic acid sodium, cocoyl sarcosine, cocoyl sarcosine sodium etc.
Above-mentioned polyester under catalyst action, reacts esterification by diprotic acid and dibasic alcohol, and then carry out with carboxylic acid or alcohol that end-blocking is prepared from.
The concrete preparation method of above-mentioned polyester is: by dibasic alcohol and diprotic acid in molar ratio for 1:1 adds in polymeric kettle, add storng-acid cation exchange resin and carry out polyreaction as catalyzer, temperature of reaction is at 180 ~ 220 DEG C, reaction times is 8 ~ 12 hours, then adds certain proportion (dibasic alcohol: the mol ratio of monocarboxylic acid or monohydroxy-alcohol can be 1:10
-10-10
10, the amount of the actual monocarboxylic acid that adds or monohydroxy-alcohol is undertaken by the combination of polymerisate and the needs of production) monocarboxylic acid or monohydroxy-alcohol carry out end-blocking, decompression removing moisture content, obtained after removing storng-acid cation exchange resin.
Above-mentioned polyester preferably in Priolube3986, Perfad8400, SYN-ESTERGY-10, SYN-ESTERGY-59, SYN-ESTERGY-500, Hostagliss1510, Palub8646 in the mixture of one or more.
The polyester prepared by the inventive method is comparatively large due to molecular weight, can form fine and close physical protection film in the present invention, have good oilness and extreme pressure anti-wear in metallic surface, can use by chloride, sulphur, phosphorus the extreme pressure anti-wear additives of all or part of replacement.
Present invention also offers a kind of preparation method of micro lubricating oil: take above-mentioned boric acid phosphoric acid fatty ester by weight percentage; synthetic ester, polyester, acyl group sarkosine or its sodium salt to add in agitator at the temperature of 40 ~ 60 DEG C stir about 1 hour respectively, sampling observe complete transparent time.
beneficial effect of the present invention:
A kind of boric acid phosphoric acid fatty ester of the present invention, has fine extreme pressure anti-wear and oilness, high rust resistance; Synthetic ester is the good base oil of good oilness and biodegradability; Polyester is comparatively large due to molecular weight, can form fine and close physical protection film in the present invention, have good oilness and extreme pressure anti-wear in metallic surface, can use by chloride, sulphur, phosphorus the extreme pressure anti-wear additives of all or part of replacement; Acyl group sarkosine or its sodium salt are that lubricity is good, and rustless property is good; A kind of micro lubricating oil of the present invention coordinates minimum quantity lubrication device to use, and usage quantity can be reduced to original less than 5%, reaches good lubrication, cooling and rust-proof effect, and energy-saving and emission-reduction, environmental protection benefit are remarkable.
Embodiment
Below in conjunction with embodiment, the present invention is further detailed explanation:
Embodiment 1:
Take 85kg oleyl alcohol, 8kg phosphoric acid, 7kg boric acid, add in reactor respectively, change out the air in reactor with nitrogen, be heated to 170 DEG C, react 10 hours, the moisture that the reaction of decompression remove portion generates, be a kind of boric acid phosphoric acid fatty ester.
Take the 15kg boric acid phosphoric acid fatty ester of above-mentioned preparation; 71kg trimethylolpropane tris oleic acid ester, 7kg polyester (Priolube3986), 7kg sodium N-lauroyl sarcosinate to add in agitator at the temperature of 50 DEG C stir about 1 hour respectively, sampling observe complete transparent time be a kind of micro lubricating oil.
Micro lubricating oil prepared by aforesaid method, as follows through test physical and chemical index:
| Project | Master data | Experimental technique |
| Outward appearance | Yellow transparent | Range estimation |
| Kinematic viscosity40 DEG C of mm 2/s | 66 | GB/T265 |
| Pour point DEG C | -17 | GB/T3535 |
| Open flash point DEG C | 256 | GB/T3536 |
| Density2 DEG C of kg/m 3 | 923 | GB/T1884 |
| Salt mist experiment 0 grade of .h | 360 | GB/T2361 |
| Copper corrosion | 1a | GB/T5096 |
Above-mentioned micro lubricating oil is applied to gear teeth processing, hobbing machine model: YK3132; Machining gears specification: diameter 120,2.5 moduluses; Hobboing cutter: TiN coating, diameter 80, length 75.Originally 46# machinery oil carries out lubrication by oil circulation cooling, and change now KS-2107B minimum quantity lubrication device (3 nozzles, nozzle used is that our company produces energy-conserving spray nozzle) and above-mentioned micro lubricating oil into, result is as following table:
Embodiment 2:
Take 80kg stearyl alcohol, 10kg phosphoric acid, 10kg boric acid, add in reactor respectively, change out the air in reactor with nitrogen, be heated to 180 DEG C, react 8 hours, the moisture that the reaction of decompression remove portion generates, be a kind of boric acid phosphoric acid fatty ester.
Take the 20kg boric acid phosphoric acid fatty ester of above-mentioned preparation, 70kg triolein, 5kg polyester, 5kg Sodium Coco acylsarcosinate to add in agitator at the temperature of 60 DEG C stir about 1 hour respectively, sampling observe complete transparent time be a kind of micro lubricating oil.
The preparation method of above-mentioned polyester: take 1 of 90.12kg (1000mol), 4 butyleneglycols and 174.19kg (1000mol) sebacic acid add in polymeric kettle, add 1.6kg storng-acid cation exchange resin nitrogen replacement and go out air in still, in temperature at 180 DEG C, reaction times is 12 hours, then adds a certain proportion of 4kg Pentyl alcohol and carries out end-blocking, decompression removing moisture content, after removing storng-acid cation exchange resin, obtained.
Embodiment 3:
Take the different tridecanol of 84kg, 9kg phosphoric acid, 7kg boric acid, add in reactor respectively, change out the air in reactor with nitrogen, be heated to 170 DEG C, react 10 hours, the moisture that the reaction of decompression remove portion generates, be a kind of boric acid phosphoric acid fatty ester.
Take the 12kg boric acid phosphoric acid fatty ester of above-mentioned preparation; 40kg tripalmitin, 35kg succinic acid di-isooctyl, 6kg polyester (Perfad8400), 7kg lauroyl sarcosine to add in agitator at the temperature of 50 DEG C stir about 1 hour respectively, sampling observe complete transparent time be a kind of micro lubricating oil.
Embodiment 4:
Take 90kg n-Eicosanol, 5kg phosphoric acid, 5kg boric acid, add in reactor respectively, change out the air in reactor with nitrogen, be heated to 160 DEG C, react 12 hours, the moisture that the reaction of decompression remove portion generates, be a kind of boric acid phosphoric acid fatty ester.
Take the 10kg boric acid phosphoric acid fatty ester of above-mentioned preparation; 50kg tetramethylolmethane four oleic acid ester, 20kg Witconol 2301,10kg polyester (SYN-ESTERGY-59), 10kg myristoy sarcosine sodium to add in agitator at the temperature of 40 DEG C stir about 1 hour respectively, sampling observe complete transparent time be a kind of micro lubricating oil.
Embodiment 5:
Take 82kg lauryl alcohol, 9kg phosphoric acid, 9kg boric acid, add in reactor respectively, change out the air in reactor with nitrogen, be heated to 175 DEG C, react 10 hours, the moisture that the reaction of decompression remove portion generates, be a kind of boric acid phosphoric acid fatty ester.
Take the 14kg boric acid phosphoric acid fatty ester of above-mentioned preparation; 30kg tetramethylolmethane four cetylate, 45kg ethylene glycol laurate, 6kg polyester (SYN-ESTERGY-500), 5kg myristoy sarcosine to add in agitator at the temperature of 50 DEG C stir about 1 hour respectively, sampling observe complete transparent time be a kind of micro lubricating oil.
Embodiment 6:
Take 86kg nonylcarbinol, 7kg phosphoric acid, 7kg boric acid, add in reactor respectively, change out the air in reactor with nitrogen, be heated to 170 DEG C, react 10 hours, the moisture that the reaction of decompression remove portion generates, be a kind of boric acid phosphoric acid fatty ester.
Take the 16kg boric acid phosphoric acid fatty ester of above-mentioned preparation, 35kg trilaurin, 36kg oil dioctyl sebacate, 6kg polyester, 7kg cocoyl sarcosine sodium to add in agitator at the temperature of 50 DEG C stir about 1 hour respectively, sampling observe complete transparent time be a kind of micro lubricating oil.
The preparation method of above-mentioned polyester: 90.12kg (1000mol) butyleneglycol and 116.07kg (1000mol) fumaric acid are added in polymeric kettle, add 2.5kg storng-acid cation exchange resin (D001 large hole strong acid styrene system cation exchange resin) and carry out polyreaction as catalyzer, temperature of reaction is at 200 DEG C, reaction times is 10 hours, then the propyl carbinol alcohol adding 3kg carries out end-blocking, decompression removing moisture content, unreacted butyleneglycol, after removing storng-acid cation exchange resin, obtain a kind of polyester.
Embodiment 7:
Take 88kg isooctyl alcohol, 6kg phosphoric acid, 6kg boric acid, add in reactor respectively, change out the air in reactor with nitrogen, be heated to 170 DEG C, react 10 hours, the moisture that the reaction of decompression remove portion generates, be a kind of boric acid phosphoric acid fatty ester.
Take the 15kg boric acid phosphoric acid fatty ester of above-mentioned preparation; 45kg trimethylolpropane tricaprylate, 26kg butyl oleate, 8kg polyester (Hostagliss1510), 6kg myristoy sarcosine to add in agitator at the temperature of 50 DEG C stir about 1 hour respectively, sampling observe complete transparent time be a kind of micro lubricating oil.
Embodiment 8:
Take 83kg isooctyl alcohol, 8kg phosphoric acid, 9kg boric acid, add in reactor respectively, change out the air in reactor with nitrogen, be heated to 170 DEG C, react 10 hours, the moisture that the reaction of decompression remove portion generates, be a kind of boric acid phosphoric acid fatty ester.
Take the 17kg boric acid phosphoric acid fatty ester of above-mentioned preparation; 30kg ethyl palmitate, 30kg ethyl oleate, 15kg Stearic ethyl stearate, 7kg polyester (Palub8646), 8kg lauroyl sarcosine to add in agitator at the temperature of 50 DEG C stir about 1 hour respectively, sampling observe complete transparent time be a kind of micro lubricating oil.
The micro lubricating oil obtained in above-described embodiment 2-8, in the process used, all can obtain effect as similar in embodiment 1.
Claims (10)
1. a boric acid phosphoric acid fatty ester, is characterized in that, is prepared from by the component of following weight percent:
Fatty alcohol 80-90%
Phosphoric acid 5-10%
Boric acid 5-10%.
2. a kind of boric acid phosphoric acid fatty ester as claimed in claim 1, is characterized in that:
It is one or more mixtures in the saturated or unsaturated fatty alcohol of 6 to 24 that described fatty alcohol is selected from carbonatoms;
Described fatty alcohol one or more mixtures preferably in n-hexyl alcohol, isooctyl alcohol, nonylcarbinol, lauryl alcohol, different tridecanol, oleyl alcohol, stearyl alcohol, n-Eicosanol.
3. the preparation method of a kind of boric acid phosphoric acid fatty ester as claimed in claim 1 or 2, is characterized in that:
Take fatty alcohol, phosphoric acid, boric acid, add in reactor respectively, change out the air in reactor with rare gas element, be heated to 160-180 DEG C, reaction 8-12 hour, the moisture that the reaction of decompression remove portion generates, be a kind of boric acid phosphoric acid fatty ester.
4. a micro lubricating oil, is characterized in that, is prepared from by the component of following weight percent:
5. a kind of micro lubricating oil as claimed in claim 4, is characterized in that:
Described synthetic ester comprises one or more in polyol ester, monoesters, dibasic acid esters.
6. a kind of micro lubricating oil as claimed in claim 5, is characterized in that:
Described polyol ester is the synthetic ester being carried out esterification synthetic gained by polyvalent alcohol and unary fatty acid;
Described polyol ester preferably from three isocaprylic acid glyceryl ester, trimethylolpropane tricaprylate, tetramethylolmethane four 2-ethylhexoate, trilaurin, trimethylolpropane trilaurate, tetramethylolmethane four laurate, triolein, trimethylolpropane tris oleic acid ester, tetramethylolmethane four oleic acid ester, tripalmitin, trimethylolpropane tris cetylate, tetramethylolmethane four cetylate;
Described monoesters refers to ester prepared by monohydroxy-alcohol and unary fatty acid;
The straight chain fatty acid that the optional free natural fats and oils of described monoesters derives and the ester that the esterification of unitary low-carbon alcohol is obtained by reacting;
Described monoesters is preferably from Witconol 2301, Laurate methyl, Laurate ethyl, methyl stearate, Stearic ethyl stearate, Uniphat A60, ethyl palmitate, ethyl oleate, butyl oleate;
Described dibasic acid esters is the product of dibasic alcohol and monoprotic acid or diprotic acid and the generation of monohydroxy-alcohol esterification;
Described dibasic acid esters is preferably from Octyl adipate, dioctyl azelate, dioctyl sebacate, DDA, two different decayl esters of azelaic acid, DI(2ETHYLHEXYL)SEBACATE, succinic acid di-isooctyl, DID Su, ethylene glycol laurate, propylene glycol oleate.
7. a kind of micro lubricating oil as claimed in claim 4, is characterized in that:
Described acyl group sarkosine is selected from the mixture of one or more that lipid acid and sarkosine carry out in the product of acylation reaction;
Described acyl group sarkosine or its sodium salt mixture of one or more preferably in Sarkosyl L, sodium lauroyl sareosine, myristoyl-N-methylaminoacetic acid, myristoyl-N-methylaminoacetic acid sodium, cocoyl sarcosine, cocoyl sarcosine sodium.
8. a kind of micro lubricating oil as claimed in claim 4, is characterized in that:
Described polyester under catalyst action, reacts esterification by diprotic acid and dibasic alcohol, and then carry out with carboxylic acid or alcohol that end-blocking is prepared from;
The concrete preparation method of described polyester is: by dibasic alcohol and diprotic acid in molar ratio for 1:1 adds in polymeric kettle, add storng-acid cation exchange resin and carry out polyreaction as catalyzer, temperature of reaction is at 180 ~ 220 DEG C, reaction times is 8 ~ 12 hours, then monocarboxylic acid is added or monohydroxy-alcohol carries out end-blocking, decompression removing moisture content, obtained after removing storng-acid cation exchange resin.
9. a kind of micro lubricating oil as claimed in claim 4, is characterized in that:
Described polyester can be selected from Priolube3986, the mixture of one or more in Perfad8400, SYN-ESTERGY-10, SYN-ESTERGY-59, SYN-ESTERGY-500, Hostagliss1510, Palub8646.
10. a preparation method for micro lubricating oil, is characterized in that:
Boric acid phosphoric acid fatty ester, synthetic ester, polyester, acyl group sarkosine or its sodium salt to be added respectively in agitator at the temperature of 40 ~ 60 DEG C stir about 1 hour, sampling observe complete transparent time.
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| CN107603713A (en) * | 2017-10-19 | 2018-01-19 | 上海金兆节能科技有限公司 | Anti-flame hydraulic fluid composition and preparation method thereof and prepare hydraulic fluid with said composition |
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| CN108998151A (en) * | 2018-09-17 | 2018-12-14 | 佛山市禅城区诺高环保科技有限公司 | A kind of preparation method of corrosion protection abrasion resistant rolling oil additives |
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| CN105524678A (en) * | 2015-12-17 | 2016-04-27 | 上海金兆节能科技有限公司 | Intelligent repair trace lubricating oil and preparation method thereof |
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| CN107057801A (en) * | 2017-04-18 | 2017-08-18 | 上海金兆节能科技有限公司 | A kind of environmentally friendly micro cutting liquid and preparation method thereof |
| CN107603713A (en) * | 2017-10-19 | 2018-01-19 | 上海金兆节能科技有限公司 | Anti-flame hydraulic fluid composition and preparation method thereof and prepare hydraulic fluid with said composition |
| CN107699313A (en) * | 2017-10-19 | 2018-02-16 | 上海金兆节能科技有限公司 | Environmentally friendly micro cutting liquid and preparation method thereof |
| CN108998151A (en) * | 2018-09-17 | 2018-12-14 | 佛山市禅城区诺高环保科技有限公司 | A kind of preparation method of corrosion protection abrasion resistant rolling oil additives |
| CN109337733A (en) * | 2018-11-09 | 2019-02-15 | 上海金兆节能科技有限公司 | Lubricant compositions and preparation method thereof and micro cutting liquid is prepared with the composition |
| CN109337733B (en) * | 2018-11-09 | 2021-06-25 | 上海金兆节能科技有限公司 | Lubricant composition, preparation method thereof and trace cutting fluid prepared from same |
| CN109609246A (en) * | 2018-12-02 | 2019-04-12 | 上海金兆节能科技有限公司 | A kind of environmental protection micro cutting liquid and preparation method thereof |
| CN109609246B (en) * | 2018-12-02 | 2021-06-01 | 上海金兆节能科技有限公司 | Environment-friendly micro-cutting fluid and preparation method thereof |
| CN114479997A (en) * | 2021-12-17 | 2022-05-13 | 东莞市耐斯润滑科技有限公司 | Method and process for producing environment-friendly trace lubricating oil based on renewable resource material |
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