CN105062643B - Boric acid phosphoric acid fatty ester and preparation method thereof and prepare micro lubricating oil with the ester - Google Patents
Boric acid phosphoric acid fatty ester and preparation method thereof and prepare micro lubricating oil with the ester Download PDFInfo
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Abstract
The present invention relates to a kind of boric acid phosphoric acid fatty ester, it is characterised in that is prepared from by following components in percentage by weight：Fatty alcohol 80 90%；Phosphoric acid 5 10%；Boric acid 5 10%.Present invention also offers the micro lubricating oil prepared with the ester, it is characterised in that is prepared from by following components in percentage by weight：Boric acid phosphoric acid fatty ester 10 20%；Synthetic ester 70~80%；Polyester 5~10%；Acyl group methyl amimoacetic acid or its sodium salt 5~10%.The micro lubricating oil coordinates minimum quantity lubrication device to use, and usage amount can be reduced to original less than 5%, reach good lubrication, cooling and rust-proof effect, and energy-saving and emission-reduction, environmental protection benefit are notable.
Description
Technical field
The invention belongs to lubrication technical field, and in particular to a kind of boric acid phosphoric acid fatty ester and preparation method thereof and use the ester
Prepare micro lubricating oil.
Background technology
Traditional metal cutting process carries out a large amount of shower formula lubrications using mineral oil or vegetable oil or cutting fluid and cooled down,
The usage amount of lubricant is big, and not only waste of resource, causes the huge pollution of processing site and environment, while can also have a strong impact on behaviour
Make the healthy of workman.Advocate energy-saving and emission-reduction, environmental protection, green production today, be badly in need of a kind of new metal cutting
Processing technology.
Minimal Quantity Lubrication Technology is the metallic green New Machining Technology grown up in recent years, is exactly in metal cutting process mistake
The good micro lubricating oil of extreme pressure anti-wear, lubricity is sprayed on process tool and finished surface using lubricating system with trace amount in journey
It is lubricated, cools down, cutting oil, liquid usage amount is big when solving traditional processing, waste the problems such as leakage rate is big.But due to using
Substantial amounts of compressed air is cooled down, and business electrical amount rises, while to meet production needs, also to carry out adopting for air compressor machine
Purchase.
Our company successfully have developed the oil-water-gas three-phase energy saving micro lubricating system such as CN103722447A, efficiently solve
Cooling problem in Minimal quantity of lubrication oil, while the air of cooling can be made to amplify more than 10 times, reduces air compressor
Electricity 70-90%.But it is due to the type of cooling for having used water vapor to take away substantial amounts of heat, occurs during processing ferrous metal
Get rusty phenomenon, use special micro lubricating agent of such as CN104031732A oil-water-gas three-phase lubricating system with trace amount and preparation method thereof
The special micro lubricating agent of production is lubricated cooling, 2 problems occurs：1.B agent addition water tank is cumbersome, actual production
Often abandoned in journey by workman；2.B agent may have fraction solids not dissolve and be added into water tank in use, cause
The problems such as blocking of energy-conserving spray nozzle.
The content of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of boric acid phosphoric acid fatty ester.
The boric acid phosphoric acid fatty ester that the present invention is provided, is prepared from by following components in percentage by weight：
Fatty alcohol 80-90%
Phosphoric acid 5-10%
Boric acid 5-10%.
It is one kind in 6 to 24 saturation or unsaturated fatty alcohol that above-mentioned fatty alcohol, which may be selected from fatty alcohol selected from carbon number,
Or several mixtures；Most preferably from n-hexyl alcohol, isooctanol, Decanol, laruyl alcohol, different tridecanol, oleyl alcohol, stearyl alcohol, arachidic alcohol
In one or more of mixtures.
The preparation method of above-mentioned boric acid phosphoric acid fatty ester is：Fatty alcohol, phosphoric acid, boric acid, difference are weighed by weight percentage
Add in reactor, the air in reactor is changed out with inert gas, be heated to 160-180 DEG C, react 8-12 hours, decompression
The moisture of partial reaction generation is removed, (i.e., the moisture of reaction generation is in decompression when reactor temperature is dropped to below 100 DEG C
With most of natural evaporation in temperature-fall period), as a kind of boric acid phosphoric acid fatty ester.
Present invention also offers a kind of micro lubricating oil, it is prepared from by following components in percentage by weight：
Above-mentioned synthetic ester includes the one or more in polyol ester, monoesters, dibasic acid esters.
Above-mentioned polyol ester is the synthetic ester that the artificial synthesized gained of esterification is carried out by polyalcohol and unary fatty acid, excellent
Selected from three isooctyl acid glyceride, trimethylolpropane tricaprylate, the tricaprylate of pentaerythrite four, laurin,
Trimethylolpropane trilaurate, the laurate of pentaerythrite four, olein, trimethylolpropane tris oleate,
The oleate of pentaerythrite four, tripalmitin, trimethylolpropane tris palmitate, the palmitate of pentaerythrite four etc..
Above-mentioned monoesters refers to ester prepared by monohydric alcohol and unary fatty acid, preferably is selected from the straight chain fatty as derived from natural oil
The ester that acid and unitary low-carbon alcohols esterification are obtained, most preferably from methyl oleate, methyl laurate, ethyl laurate, stearic acid
Methyl esters, ethyl stearte, methyl hexadecanoate, ethyl palmitate, ethyl oleate, butyl oleate etc..
Above-mentioned dibasic acid esters is the product of dihydric alcohol and monoacid or binary acid and the generation of monohydric alcohol esterification, preferably oneself
Adipate, dioctyl azelate, di-n-octyl sebacate, dichenyl adipate, two different decayl esters of azelaic acid, the isodecyl of decanedioic acid two
Ester, succinic acid di-isooctyl, DID Su, ethylene glycol laurate, propylene glycol oleate etc..Such dibasic acid esters has good
Good lubricity, kinematic viscosity is low, and low temperature performance well, biodegradability is excellent.
Above-mentioned acyl group methyl amimoacetic acid or its sodium salt are the products that aliphatic acid and methyl amimoacetic acid carry out acylation reaction, preferably are selected from lauroyl
Methyl amimoacetic acid, sodium lauroyl sarcosine, myristoyl-N-methylaminoacetic acid, myristoyl-N-methylaminoacetic acid sodium, cocoyl sarcosine, cocounut oil acyl flesh ammonia
One or more in sour sodium etc..
Above-mentioned polyester is that esterification is reacted under catalyst action by binary acid and dihydric alcohol, and carboxylic acid or alcohol are then used again
Carry out what end-blocking was prepared from.
The specific preparation method of above-mentioned polyester is：It is 1 in molar ratio by dihydric alcohol and binary acid：1 adds in polymeric kettle, plus
Enter storng-acid cation exchange resin as catalyst and carry out polymerisation, reaction temperature is at 180~220 DEG C, and the reaction time is 8
~12 hours, then add certain proportion (dihydric alcohol：The mol ratio of monocarboxylic acid or monohydric alcohol can be 1：10-10-1010, it is real
Carried out the need for combination and production of the amount by polymerizate of monocarboxylic acid or monohydric alcohol that border is added) monocarboxylic acid or unitary
Alcohol is blocked, and moisture content is removed under reduced pressure, and is removed and is made after storng-acid cation exchange resin.
Above-mentioned polyester preferably is selected from Priolube 3986, Perfad 8400, SYN-ESTER GY-10, SYN-ESTER GY-
One or more of mixtures in 59, SYN-ESTER GY-500, Hostagliss 1510, Palub 8646.
The polyester prepared by the inventive method can form densification because molecular weight is larger, in the present invention in metal surface
Physical protection film, with good lubricity and extreme pressure anti-wear, can completely or partially replace the extreme-pressure anti-wear of chloride, sulphur, phosphorus
Agent is used.
Present invention also offers a kind of preparation method of micro lubricating oil：Above-mentioned boric acid phosphoric acid is weighed by weight percentage
Fatty ester, synthetic ester, polyester, acyl group methyl amimoacetic acid or its sodium salt are separately added into agitator the stir about at a temperature of 40~60 DEG C
1 hour, when sampling observation is fully transparent.
Beneficial effects of the present invention：
A kind of boric acid phosphoric acid fatty ester of the present invention, with fine extreme pressure anti-wear and lubricity, high rust resistance；Close
It is good lubricity and the good base oil of biodegradability into ester；Polyester is larger due to molecular weight, in the present invention may be used
The physical protection film of densification is formed in metal surface, with good lubricity and extreme pressure anti-wear, can completely or partially be replaced
Chloride, sulphur, the extreme pressure anti-wear additives of phosphorus are used；Acyl group methyl amimoacetic acid or its sodium salt are that greasy property is good, and rustless property is good；The present invention
A kind of micro lubricating oil coordinate minimum quantity lubrication device use, usage amount can be reduced to original less than 5%, reached good
Lubrication, cooling and rust-proof effect, energy-saving and emission-reduction, environmental protection benefit are notable.
Embodiment
With reference to embodiment, the present invention is further detailed explanation：
Embodiment 1：
Weigh 85kg oleyl alcohol, 8kg phosphoric acid, 7kg boric acid, be separately added into reactor, changed out with nitrogen in reactor
Air, is heated to 170 DEG C, reacts 10 hours, and the moisture of partial reaction generation is removed under reduced pressure, as a kind of boric acid phosphoric acid fat
Ester.
Weigh the 15kg boric acid phosphoric acid fatty esters of above-mentioned preparation, 71kg trimethylolpropane tris oleate, 7kg polyester
(Priolube 3986), 7kg sodium N-lauroyl sarcosinates are separately added into agitator stir about 1 hour at a temperature of 50 DEG C,
Sampling observation is a kind of micro lubricating oil when fully transparent.
Micro lubricating oil prepared by the above method, it is as follows through testing physical and chemical index：
| Project | Master data | Experimental method |
| Outward appearance | Yellow transparent | Range estimation |
| 40 DEG C of mm of kinematic viscosity@2/s | 66 | GB/T265 |
| Pour point DEG C | -17 | GB/T3535 |
| Open flash point DEG C | 256 | GB/T3536 |
| 2 DEG C of kg/m of density@3 | 923 | GB/T1884 |
| 0 grade of .h of salt mist experiment | 360 | GB/T2361 |
| Copper corrosion | 1a | GB/T5096 |
Above-mentioned micro lubricating oil is processed applied to gear teeth, gear-hobbing machine model：YK3132；Process gear set specifications：Diameter
120,2.5 moduluses；Hobboing cutter：TiN coatings, diameter 80, length 75.Circulation lubrication originally is carried out with 46# machinery oil, is changed now
For KS-2107B minimum quantity lubrication devices (3 nozzles, nozzle used is that our company produces energy-conserving spray nozzle) and above-mentioned micro lubricating oil, knot
Fruit such as following table：
Embodiment 2：
Weigh 80kg stearyl alcohols, 10kg phosphoric acid, 10kg boric acid, be separately added into reactor, reactor is changed out with nitrogen
In air, be heated to 180 DEG C, react 8 hours, the moisture of partial reaction generation, as a kind of boric acid phosphate ester is removed under reduced pressure
Fat ester.
Weigh the 20kg boric acid phosphoric acid fatty esters of above-mentioned preparation, 70kg oleins, 5kg polyester, 5kg cocoyls
Sodium sarcosinate is separately added into agitator stir about 1 hour at a temperature of 60 DEG C, and sampling observation is one kind when fully transparent
Micro lubricating oil.
The preparation method of above-mentioned polyester：Weigh 90.12kg (1000mol) 1,4 butanediols and 174.19kg (1000mol)
Decanedioic acid is added in polymeric kettle, is added 1.6kg storng-acid cation exchange resin nitrogen displacements and is gone out air in kettle, exists in temperature
180 DEG C, the reaction time is 12 hours, then adds a certain proportion of 4kg n-amyl alcohols and is blocked, moisture content is removed under reduced pressure, and is removed
After storng-acid cation exchange resin, it is made.
Embodiment 3：
Weigh the different tridecanols of 84kg, 9kg phosphoric acid, 7kg boric acid, be separately added into reactor, reactor is changed out with nitrogen
In air, be heated to 170 DEG C, react 10 hours, the moisture of partial reaction generation, as a kind of boric acid phosphate ester is removed under reduced pressure
Fat ester.
The 12kg boric acid phosphoric acid fatty esters of above-mentioned preparation are weighed, 40kg tripalmitins, 35kg succinic acid two are different pungent
Ester, 6kg polyester (Perfad 8400), 7kg lauroyl sarcosines are separately added into agitator the stir about at a temperature of 50 DEG C
1 hour, sampling observation was a kind of micro lubricating oil when fully transparent.
Embodiment 4：
Weigh 90kg arachidic alcohols, 5kg phosphoric acid, 5kg boric acid, be separately added into reactor, changed out with nitrogen in reactor
Air, be heated to 160 DEG C, react 12 hours, the moisture of partial reaction generation is removed under reduced pressure, as a kind of boric acid phosphoric acid fat
Ester.
Weigh the 10kg boric acid phosphoric acid fatty esters of above-mentioned preparation, the oleate of 50kg pentaerythrites four, 20kg methyl oleates,
10kg polyester (SYN-ESTER GY-59), 10kg myristoy sarcosine sodium are separately added into agitator in 40 DEG C of temperature
Lower stir about 1 hour, sampling observation is a kind of micro lubricating oil when fully transparent.
Embodiment 5：
Weigh 82kg laruyl alcohols, 9kg phosphoric acid, 9kg boric acid, be separately added into reactor, changed out with nitrogen in reactor
Air, be heated to 175 DEG C, react 10 hours, the moisture of partial reaction generation is removed under reduced pressure, as a kind of boric acid phosphoric acid fat
Ester.
Weigh the 14kg boric acid phosphoric acid fatty esters of above-mentioned preparation, the palmitate of 30kg pentaerythrites four, 45kg ethylene glycol month
Cinnamic acid ester, 6kg polyester (SYN-ESTER GY-500), 5kg myristoy sarcosines are separately added into agitator at 50 DEG C
At a temperature of stir about 1 hour, sampling observation is a kind of micro lubricating oil when fully transparent.
Embodiment 6：
Weigh 86kg Decanols, 7kg phosphoric acid, 7kg boric acid, be separately added into reactor, changed out with nitrogen in reactor
Air, be heated to 170 DEG C, react 10 hours, the moisture of partial reaction generation is removed under reduced pressure, as a kind of boric acid phosphoric acid fat
Ester.
The 16kg boric acid phosphoric acid fatty esters of above-mentioned preparation are weighed, the oily decanedioic acid two of 35kg laurins, 36kg is pungent
Ester, 6kg polyester, 7kg cocoyl sarcosine sodium are separately added into agitator stir about 1 hour at a temperature of 50 DEG C, and sampling is seen
It is a kind of micro lubricating oil when examining fully transparent.
The preparation method of above-mentioned polyester：By 90.12kg (1000mol) butanediols and 116.07kg (1000mol) fumaric acid
Add in polymeric kettle, add 2.5kg storng-acid cation exchange resin (D001 macropore strong acid polystyrene cation exchange trees
Fat) as catalyst progress polymerisation, reaction temperature is at 200 DEG C, and the reaction time is 10 hours, then adds 3kg positive fourth
Alcohol alcohol is blocked, and moisture content, unreacted butanediol is removed under reduced pressure, and is removed after storng-acid cation exchange resin, is produced one kind
Polyester.
Embodiment 7：
Weigh 88kg isooctanol, 6kg phosphoric acid, 6kg boric acid, be separately added into reactor, changed out with nitrogen in reactor
Air, be heated to 170 DEG C, react 10 hours, the moisture of partial reaction generation is removed under reduced pressure, as a kind of boric acid phosphoric acid fat
Ester.
Weigh the 15kg boric acid phosphoric acid fatty esters of above-mentioned preparation, 45kg trimethylolpropane tricaprylates, 26kg oleic acid
Butyl ester, 8kg polyester (Hostagliss 1510), 6kg myristoy sarcosines are separately added into agitator in 50 DEG C of temperature
Lower stir about 1 hour, sampling observation is a kind of micro lubricating oil when fully transparent.
Embodiment 8：
Weigh 83kg isooctanol, 8kg phosphoric acid, 9kg boric acid, be separately added into reactor, changed out with nitrogen in reactor
Air, be heated to 170 DEG C, react 10 hours, the moisture of partial reaction generation is removed under reduced pressure, as a kind of boric acid phosphoric acid fat
Ester.
The 17kg boric acid phosphoric acid fatty esters of above-mentioned preparation are weighed, 30kg ethyl palmitates, 30kg ethyl oleates, 15kg are stearic
Acetoacetic ester, 7kg polyester (Palub 8646), 8kg lauroyl sarcosines are separately added into agitator and stirred at a temperature of 50 DEG C
Mix about 1 hour, sampling observation is a kind of micro lubricating oil when fully transparent.
The micro lubricating oil obtained in above-described embodiment 2-8, during use, can be obtained as embodiment 1 is similar
Effect.
Claims (6)
1. a kind of micro lubricating oil, it is characterised in that be prepared from by following components in percentage by weight：
Described boric acid phosphoric acid fatty ester, is prepared from by following components in percentage by weight：
Fatty alcohol 80-90%
Phosphoric acid 5-10%
Boric acid 5-10%；
The preparation method of the boric acid phosphoric acid fatty ester：
Fatty alcohol, phosphoric acid, boric acid are weighed, is separately added into reactor, the air in reactor is changed out with inert gas, is heated
To 160-180 DEG C, react 8-12 hours, the moisture of partial reaction generation, as a kind of boric acid phosphoric acid fatty ester is removed under reduced pressure；
One kind in n-hexyl alcohol, isooctanol, Decanol, different tridecanol, oleyl alcohol, stearyl alcohol, arachidic alcohol of the fatty alcohol or
Several mixtures；
The one or more that the synthetic ester is selected in polyol ester, monoesters；
The polyester is selected from Priolube 3986, Perfad 8400, SYN-ESTER GY-10,
One or more in SYN-ESTER GY-59, SYN-ESTER GY-500, Hostagliss 1510, Palub 8646
Mixture；
The sarcosinate salt is in sodium lauroyl sarcosine, myristoyl-N-methylaminoacetic acid sodium, cocoyl sarcosine sodium
One or more of mixtures.
2. a kind of micro lubricating oil as claimed in claim 1, it is characterised in that：
The polyol ester is the synthetic ester that the artificial synthesized gained of esterification is carried out by polyalcohol and unary fatty acid；
The monoesters refers to ester prepared by monohydric alcohol and unary fatty acid.
3. a kind of micro lubricating oil as claimed in claim 1, it is characterised in that：
The polyol ester is selected from three isooctyl acid glyceride, trimethylolpropane tricaprylate, the tricaprylate of pentaerythrite four,
Laurin, trimethylolpropane trilaurate, the laurate of pentaerythrite four, olein, three hydroxyl first
Base propane trioleate, the oleate of pentaerythrite four, tripalmitin, trimethylolpropane tris palmitate, Ji Wusi
The palmitate of alcohol four.
4. a kind of micro lubricating oil as claimed in claim 1, it is characterised in that：
The monoesters is selected from methyl oleate, methyl laurate, ethyl laurate, methyl stearate, ethyl stearte, palmitic acid first
Ester, ethyl palmitate, ethyl oleate, butyl oleate.
5. a kind of micro lubricating oil as claimed in claim 1, it is characterised in that：
The monoesters is selected from the ester that straight chain fatty acid and unitary low-carbon alcohols esterification as derived from natural oil are obtained.
6. a kind of preparation method of micro lubricating oil as described in claim 1-5 is any, it is characterised in that：
Boric acid phosphoric acid fatty ester, synthetic ester, polyester, sarcosinate salt are separately added into agitator in 40~60 DEG C of temperature
The lower stir about of degree 1 hour, when sampling observation is fully transparent.
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| CN105524678B (en) * | 2015-12-17 | 2018-05-25 | 上海金兆节能科技有限公司 | Intelligence repairs micro lubricating oil and preparation method thereof |
| 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 |
| 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 |
| 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 |
| 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 |
| 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 |
| 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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| CN101654636A (en) * | 2009-09-14 | 2010-02-24 | 上海金兆节能科技有限公司 | Biological type micro lubricating oil and preparation method and application thereof |
| CN102899154B (en) * | 2012-10-19 | 2014-04-02 | 宋小林 | Fully synthetic cutting solution |
| CN104263476B (en) * | 2014-09-16 | 2016-08-10 | 上海金兆节能科技有限公司 | Biodegradable micro lubricating oil and preparation method thereof |
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Effective date of registration: 20200628 Address after: 528300 2 Daliang Road, five Sha Road, Shunde District, Foshan, Guangdong. Patentee after: Guangdong Fu Yansheng Science and Technology Ltd. s Address before: 200436 room 299, Lane 4-103, West Road, Baoshan District, Shanghai Patentee before: SHANGHAI JINZHAO ENERGY-SAVING TECHNOLOGY Co.,Ltd. |