CN105176632A - High-temperature lubrication grease antifriction and anti-wear additive and preparation method thereof - Google Patents
High-temperature lubrication grease antifriction and anti-wear additive and preparation method thereof Download PDFInfo
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- CN105176632A CN105176632A CN201410270713.XA CN201410270713A CN105176632A CN 105176632 A CN105176632 A CN 105176632A CN 201410270713 A CN201410270713 A CN 201410270713A CN 105176632 A CN105176632 A CN 105176632A
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Abstract
The invention discloses a high-temperature lubrication grease antifriction and anti-wear additive and a preparation method thereof. The additive is a castor oil phenyl phosphate compound. A reactant adopted in the invention is green and renewable plant oil, that is castor oil, and the prepared castor oil phenyl phosphate has a large molecular weight and a stable structure, can be used as a high-temperature antifriction and anti-wear additive, and also has very high thermal stability and very good friction characteristic. The additive has good antifriction and anti-wear performances at 200DEG C when the additive is added to lithium base grease.
Description
Technical field
The present invention relates to a kind of high temperature resistant lubricating grease antiwear and friction-reducing additive and preparation method thereof.
Background technology
Lubricating grease is the colloidal dispersion of thickening material in lubricating fluid, and it normally two components is heated together until thickening material expands and is attached together with oil and formed.Due to lubricating grease there is low frictional coefficient, be easy to control, for a long time work-ing life and cheap cost, make it be preferentially use as lubricant at specific area.But, along with the fast development of spacecraft, turbine, automobile, farm machinery, railway apparatus and industrial machine etc., more and more can be competent in the urgent need to lubricating grease and use under high loading, high speed and high-temperature.Can at high temperature so develop, such as 149-232 ° of C, or under higher temperature, the lubricating grease of sufficient lubrication becomes more and more important.In order to address these problems, the lubricating grease used under much high temperature, such as composite calcium-base fat, aluminum complex grease, lithium saponify, polyurea grease and silicone grease etc. are developed to meet high temperature demands.But only have little high temperature lubricating additive particularly antifriction, wear preventive additive is commercially used, these all limit the development of high temperature grease.
Set up the common recognition that environmentally friendly and conservation-minded society has been the world today, along with the exhaustion of the day by day harsh of environmental requirement and petroleum resources, renewable new forms of energy progressively earn widespread respect in the applied research of lubricating area.Viscotrol C derives from non-grain bioenergy-castor-oil plant, not only has the general characteristic of vegetables oil, and it has incomparable " do not strive grain with people, do not strive ground with the grain " advantage of rape seed oil, peanut oil, soybean wet goods vegetables oil.Viscotrol C has more excellent oilness and anti-oxidative stability energy than other vegetables oil, the suitable base oil as Biodegradable lubricant and slip additive.At home and abroad, the existing a large amount of report of the research work of this respect.(the KarP. such as Prasenjit, AsthanaP., LiangH.Formationandcharacterizationoftribofilm.Journalof Tribology.2008,130,4201) friction film of Viscotrol C and other three kinds of base oils is analyzed and researched, result shows that the Viscotrol C of strong polarity is easier forms transfer layer at steel friction surface, effectively prevents the problems such as the abrasive dust adhesion of metal hardening and metallic surface.(the Zhang Naiqing such as Zhang Naiqing, Zhang Guanghui, Zhang Tianpeng, Qi Xinran, Meng Xiangbing. gather ricinoleate ester phosphoric acid ester and preparation method thereof and prepare biodegradable micro cutting oil with this ester. application number 201310354862.X) describe the preparation of poly-ricinoleate ester phosphoric acid ester and the application in biodegradable micro cutting oil thereof.Superfine (the Wu Chao of Wu, Jia Xiaoming, Zhang Haoqiang. the preparation and property of the cruel water base lubricant of Viscotrol C boric acid. Institutes Of Technology Of Hebei's journal (natural science edition) .2007,29,53) utilize Viscotrol C, organic alcohol amine and boric acid synthesize a kind of environment-friendly water-based lubricant.(the square Jian Hua such as Fang Jianhua, Chen Boshui, Dong Ling. phthalein amine type modified castor oil lubricating additive is on the impact of steel one steel-steel pair and steel one aluminium friction pair tribological property. petroleum journal .2009,25,78) chemical modification introducing boron, nitrogen element has been carried out to Viscotrol C, and have studied the tribological property of modified product in steel/steel and steel/aluminum-system.(the Li Changjin such as Li Changjin, Tu Zhengwen, Xu Wangsheng. the synthesis of phosphorous nitride castor oil lubricating additive and tribological property thereof. Wuhan Engineering Univ's journal, 2009,31,22) induce one phosphorus and nitrogen in Viscotrol C, synthesized a kind of phosphorous nitride modified castor oil additive, this new modified Viscotrol C additive has excellent extreme pressure, antiwear and friction reduction property.(the DrownD.C such as Drown, HarperK., FrameE.Screeningvegetableoilalcoholestersasfuellubricity enhancers.JournaloftheAmericanOilChemists ' Society.2001,78,579) research finds, Viscotrol C has more excellent lubricity compared with the vegetables oil of other equal carbon chain lengths, can be used as fuel lubrication additive.In addition, China is Semen Ricini big producing country, and annual production more than 20 ten thousand tons, is only second to India and Brazil, carries out Viscotrol C and has important practical significance in the applied research of lubricating area.
Summary of the invention
The object of the invention is to provide a kind of high temperature grease antiwear and friction-reducing additive and preparation method thereof.
The present invention is achieved by the following measures:
We have prepared a kind of at high temperature excellent lubricating properties, antifriction antiwear lubricating grease additive that preparation method is easy, and additive is Viscotrol C phosphenylic acid ester cpds.
A kind of high temperature grease antifriction wear preventive additive, is characterized in that additive is for such as formula the Viscotrol C phenyl phosphate ester shown in I,
Wherein, L represents the esterified Viscotrol C in 12-position, and n is the integer of 1 to 3.
Viscotrol C phenyl phosphate ester shown in formula I of the present invention, when n is 3, compound is Viscotrol C three (diphenyl phosphoester), and molecular weight is 1629.
Viscotrol C phenyl phosphate ester shown in formula I of the present invention, when n is 2, compound is Viscotrol C two (diphenyl phosphoester), and molecular weight is 1397.
Viscotrol C phenyl phosphate ester shown in formula I of the present invention, when n is 1, compound is Viscotrol C diphenyl phosphoester, and molecular weight is 1165.
High temperature grease antifriction wear preventive additive of the present invention is a kind of white powder.
A preparation method for high temperature grease antifriction wear preventive additive, is characterized in that the method comprises following two steps:
Step 1) uses phosphorus chloride diphenyl phthalate and Viscotrol C according to mol ratio 1:1 ~ 3:1 reaction, under catalyzer Aluminum chloride anhydrous or Magnesium Chloride Anhydrous catalysis, in 90 ~ 140 DEG C of back flow reaction 10 ~ 20 hours, the Viscotrol C phenyl phosphate ester of production I, whole process passes into nitrogen protection;
Step 2) reaction carries out filtering after terminating and dry, namely uses acetonitrile, water washing, dry at 110 DEG C, obtains white powdery solids product.
Method of the present invention, the consumption of catalyzer is 1% ~ 2% of reactant total mass.
The reactant that the present invention adopts is green, reproducible vegetables oil and Viscotrol C, the Viscotrol C phenyl phosphate ester (formula I) prepared, and molecular weight is large, and Stability Analysis of Structures, can use as high-temperature antifriction wear preventive additive.
Formula I of the present invention is added in 12-hydroxy lithium stearate base fat, can obtain excellent antifriction, abrasion resistance at 200 DEG C.
Formula I of the present invention is added in 12-hydroxy lithium stearate base fat, and at 200 DEG C, its anti-wear and wear-resistant performance is better than traditional wear preventive additive zinc dialkyl dithiophosphate (ZDDP).
Formula I of the present invention is added in compositing lithio ester, can obtain excellent antifriction, abrasion resistance at 200 DEG C.
Formula I of the present invention is added in compositing lithio ester, and at 200 DEG C, their anti-wear and wear-resistant performance is better than traditional wear preventive additive zinc dialkyl dithiophosphate (ZDDP).
Formula I of the present invention as high-temperature antifriction anti-wear lubricating additive add to the addition in 12-hydroxy lithium stearate base fat and compositing lithio ester be 1% ~ 4%.
Formula I of the present invention is added in 12-hydroxy lithium stearate base fat, changes frequency when being increased to 40Hz from 15Hz, and adding the frictional coefficient after 3%ZDDP and 3% formula I and mill spot all has improvement clearly.Comparatively speaking, the anti-wear and wear-resistant performance of formula I is better than ZDDP.
Formula I of the present invention is added in compositing lithio ester, changes frequency when being increased to 40Hz from 15Hz, and adding the frictional coefficient after 3%ZDDP and 3% formula I and mill spot all has improvement clearly.Comparatively speaking, the anti-wear and wear-resistant performance of formula I is better than ZDDP.
Accompanying drawing explanation
Fig. 1 is the pyrolysis temperature curve of embodiment 1 product (when formula I, n=3, being denoted as BMY-P).
Fig. 2 is that concentration is respectively 0%, 1%, 2%, embodiment 1 product of 3%, 4% is (when formula I, n=3, be denoted as BMY-P) add 12-hydroxy lithium stearate base fat (being called for short single lithium) on the micro-vibration friction abrasion testing machine of SRV-IV in 200 DEG C, frequency 25Hz, load 100N, the time dependent relation curve of frictional coefficient under the operating mode of amplitude 1mm.
Fig. 3 is concentration 0%, 3% example 1 product (formula I, during n=3, be denoted as BMY-P) and 3%ZDDP add 12-hydroxy lithium stearate base fat (being called for short single lithium) at the micro-vibration friction abrasion testing machine of SRV-IV in 200 DEG C, frequency 25Hz, the time dependent relation curve of frictional coefficient under load 100N, amplitude 1mm operating mode.
Fig. 4 is concentration is 0%, 1%, 2%, 3%, embodiment 1 product (when formula I, n=3, being denoted as BMY-P) of 4% adds compositing lithio ester at the micro-vibration friction abrasion testing machine of SRV-IV in 200 DEG C, frequency 25Hz, load 100N, the time dependent relation curve of frictional coefficient under amplitude 1mm operating mode.
Fig. 5 is concentration 0%, and 3% example 1 product is (when formula I, n=3, be denoted as BMY-P) and 3%ZDDP add compositing lithio ester at the micro-vibration friction abrasion testing machine of SRV-IV in 200 DEG C, frequency 25Hz, load 100N, the time dependent relation curve of frictional coefficient under amplitude 1mm operating mode.
Fig. 6 is that concentration is respectively 0%, 1%, embodiment 1 product (the formula I of 2%, 3%, 4%, during n=3, be denoted as BMY-P) join 12-hydroxy lithium stearate base fat (being called for short single lithium) and compositing lithio ester in 200 DEG C on the micro-vibration friction abrasion testing machine of SRV-IV, frequency 25Hz, load 100N, amplitude 1mm, grinds the wear volume of spot under long mill 30min operating mode.
Fig. 7 is concentration 0%, 3% example 1 product (formula I, during n=3, be denoted as BMY-P) and 3%ZDDP add 12-hydroxy lithium stearate base fat (being called for short single lithium) at the micro-vibration friction abrasion testing machine of SRV-IV in 200 DEG C, load 100N, amplitude 1mm, when frequency is increased to 40Hz from 15Hz and the relation curve of the friction coefficient change of frequency.
Fig. 8 is concentration 0%, and 3% example 1 product is (when formula I, n=3, be denoted as BMY-P) and 3%ZDDP add compositing lithio ester at the micro-vibration friction abrasion testing machine of SRV-IV in 200 DEG C, load 100N, amplitude 1mm, the relation curve of the friction coefficient frequency when frequency is increased to 40Hz from 15Hz.
Fig. 9 is that concentration is respectively 0%, 3% example 1 product (formula I, during n=3, be denoted as BMY-P), 3%ZDDP adds 12-hydroxy lithium stearate base fat (being called for short single lithium) and compositing lithio ester on the micro-vibration friction abrasion testing machine of SRV-IV in 200 DEG C, load 100N, amplitude 1mm, grinds the wear volume of spot when frequency is increased to 40Hz from 15Hz.
Embodiment
Embodiment 1
5.0g(5.36mmol is added in 100mL there-necked flask) Viscotrol C, 4.463g(16.6mmol) phosphorus chloride diphenyl phthalate, 0.1g Aluminum chloride anhydrous.Add 50mL toluene afterwards.There-necked flask connects prolong respectively, thermometer and bilateral piston (being connected nitrogen access equipment).Pass into nitrogen protection, be warming up to 100
oc reacts 14h.Filter out solid after having reacted, wash 2 times with water, acetonitrile wash 2 times.110
odry 2h under C.Obtain 7.16g white powder product, i.e. Viscotrol C three (diphenyl phosphoester) (when formula I, n=3), molecular weight is 1629, productive rate 82%.
Embodiment 2
5.0g(5.36mmol is added in 100mL there-necked flask) Viscotrol C, 2.88g(10.72mmol) phosphorus chloride diphenyl phthalate, 0.1g Aluminum chloride anhydrous.Add 50mL toluene afterwards.There-necked flask connects prolong respectively, thermometer and bilateral piston (being connected nitrogen access equipment).Pass into nitrogen protection, be warming up to 100
oc reacts 14h.Filter out solid after having reacted, wash 2 times with water, acetonitrile wash 2 times.110
odry 2h under C.Obtain 6.37g white powder product, i.e. Viscotrol C two (diphenyl phosphoester) (when formula I, n=2), molecular weight is 1397, productive rate 86%.
Embodiment 3
5.0g(5.36mmol is added in 100mL there-necked flask) Viscotrol C, 1.436g(5.36mmol) phosphorus chloride diphenyl phthalate, 0.1g Aluminum chloride anhydrous.Add 50mL toluene afterwards.There-necked flask connects prolong respectively, thermometer and bilateral piston (being connected nitrogen access equipment).Pass into nitrogen protection, be warming up to 100
oc reacts 14h.Filter out solid after having reacted, wash 2 times with water, acetonitrile wash 2 times.110
odry 2h under C.Obtain 5.4g white powder product, i.e. Viscotrol C diphenyl phosphoester (when formula I, n=1), molecular weight is 1165, productive rate 89%.
Evaluation of Thermal Stability
Thermostability is measured by STA449CJupitersimultaneousTG-DSC.Viscotrol C three (diphenyl phosphoester) (being denoted as BMY-P) 5mg embodiment 1 prepared puts into sample pool, and probe temperature is from 20-800
oC, temperature increase rate is 10
oC/ min, measures under air ambient.Result as shown in Figure 1.The heat decomposition temperature of BMY-P (
t d) be 295
oC.Show that this material has extraordinary thermal stability.
The tribological property evaluation of product:
Viscotrol C three (diphenyl phosphoester) (being denoted as BMY-P) of embodiment 1 being prepared adds in 12-hydroxy lithium stearate base fat and compositing lithio ester, and on three-roll grinder, evenly, being mixed with concentration is 1% in grinding, 2%, 3%, 4% lubricating grease, its tribological property of comprehensive evaluation:
1. the micro-vibration friction abrasion testing machine test concentrations of SRV-IV adopting German Optimol grease company to produce is respectively 0%, 1%, embodiment 1 product (being denoted as BMY-P) of 2%, 3%, 4% joins in 12-hydroxy lithium stearate base fat, at 200 DEG C, frequency 25Hz, the frictional coefficient f under the operating mode of amplitude 1mm, load 100N during long mill 30min, test the GCr15 bearing steel that steel ball used is Φ=10mm, lower sample is the GCr15 bloom of Φ 24 × 7.9mm.The results are shown in accompanying drawing 2 and 3.As seen from the figure, under 200 DEG C of high temperature, this compound well can lubricate steel-steel frictional pair as additive, and frictional coefficient significantly reduces, and friction reducing effect is very obvious.Further, the antifriction effect of BMY-P in 12-hydroxy lithium stearate base fat is better than ZDDP.
2. the micro-vibration friction abrasion testing machine test concentrations of SRV-IV adopting German Optimol grease company to produce is respectively 0%, 1%, embodiment 1 product (BMY-P) of 2%, 3%, 4% joins in compositing lithio ester, at 200 DEG C, frequency 25Hz, the frictional coefficient f under the operating mode of amplitude 1mm, load 100N during long mill 30min, test the GCr15 bearing steel that steel ball used is Φ=10mm, lower sample is the GCr15 bloom of Φ 24 × 7.9mm.The results are shown in attached Figure 4 and 5.As seen from the figure, under 200 DEG C of high temperature, this compound has lubricant effect as additive to steel-steel frictional pair, and frictional coefficient obviously reduces.Further, the friction reducing effect of BMY-P in compositing lithio ester is better than ZDDP.
3. adopt the non-contacting Surface Tester test concentrations of MicroXAM3D to be respectively 0%, 1%, 2%, 3%, embodiment 1 product (being designated as BMY-P) of 4% joins in 12-hydroxy lithium stearate base fat and compositing lithio ester, at 200 DEG C, and frequency 25Hz, wear volume under the operating mode of amplitude 1mm, load 100N after long mill 30min.As shown in Figure 6, after adding this additive, the wear volume of mill spot obviously reduces test result.Show that this additive has good anti-wear effect.
4. the micro-vibration friction abrasion testing machine test concentrations of SRV-IV adopting German Optimol grease company to produce be respectively 0% and 3% embodiment 1 product (being denoted as BMY-P) and 3%ZDDP add 12-hydroxy lithium stearate base fat and compositing lithio ester at 200 DEG C, frequency 15-40Hz, under the operating mode of amplitude 1mm, frictional coefficient f is with the relation curve of change of frequency, test the GCr15 bearing steel that steel ball used is Φ=10mm, lower sample is the GCr15 bloom of Φ 24 × 7.9mm.The results are shown in accompanying drawing 7 and 8.As seen from the figure, when frequency is increased to 40Hz from 15Hz, the frictional coefficient of ZDDP and embodiment 1 product (BMY-P) all has reduction, and it is the most obvious that BMY-P reduces.Show that the anti-wear and wear-resistant performance of example 1 product is very outstanding, and be better than the ZDDP of same amount.
5. adopt MicroXAM3D non-contacting Surface Tester test concentrations be respectively 0% and 3% embodiment 1 product (being denoted as BMY-P) and 3%ZDDP add 12-hydroxy lithium stearate base fat and compositing lithio ester at 200 DEG C, load 100N, wear volume under amplitude 1mm, frequency 15-40Hz operating mode.As shown in Figure 9, after adding this additive, the wear volume of mill spot obviously reduces test result.Show that this additive has good anti-wear effect.
Claims (6)
1. a high temperature grease antifriction wear preventive additive, is characterized in that additive is for such as formula the Viscotrol C phenyl phosphate ester shown in I,
Wherein, L represents the esterified Viscotrol C in 12-position, and n is the integer of 1 to 3.
2. additive as claimed in claim 1, it is characterized in that the Viscotrol C phenyl phosphate ester shown in described formula I, when n is 3, compound is Viscotrol C three (diphenyl phosphoester), and molecular weight is 1629.
3. additive as claimed in claim 1, it is characterized in that the Viscotrol C phenyl phosphate ester shown in described formula I, when n is 2, compound is Viscotrol C two (diphenyl phosphoester), and molecular weight is 1397.
4. additive as claimed in claim 1, it is characterized in that the Viscotrol C phenyl phosphate ester shown in described formula I, when n is 1, compound is Viscotrol C diphenyl phosphoester, and molecular weight is 1165.
5. the preparation method of a kind of high temperature grease antifriction wear preventive additive as described in Claims 1-4, is characterized in that the method comprises following two steps:
Step 1) uses phosphorus chloride diphenyl phthalate and Viscotrol C according to mol ratio 1:1 ~ 3:1 reaction, under catalyzer Aluminum chloride anhydrous or Magnesium Chloride Anhydrous catalysis, in 90 ~ 140 DEG C of back flow reaction 10 ~ 20 hours, the Viscotrol C phenyl phosphate ester of production I, whole process passes into nitrogen protection;
Step 2) reaction carries out filtering after terminating and dry, namely uses acetonitrile, water washing, dry at 110 DEG C, obtains white powdery solids product.
6. method as claimed in claim 5, is characterized in that the consumption of catalyzer is 1% ~ 2% of reactant total mass.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08134486A (en) * | 1994-11-15 | 1996-05-28 | Matsushita Electric Ind Co Ltd | Additive for refrigerator oil and refrigerator oil |
| CN103450255A (en) * | 2013-08-14 | 2013-12-18 | 菏泽茂坤环保科技有限公司 | Polyricinoleate phosphate and preparation method thereof, and application of polyricinoleate phosphate in preparing biodegradable trace cutting oil |
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2014
- 2014-06-17 CN CN201410270713.XA patent/CN105176632B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08134486A (en) * | 1994-11-15 | 1996-05-28 | Matsushita Electric Ind Co Ltd | Additive for refrigerator oil and refrigerator oil |
| CN103450255A (en) * | 2013-08-14 | 2013-12-18 | 菏泽茂坤环保科技有限公司 | Polyricinoleate phosphate and preparation method thereof, and application of polyricinoleate phosphate in preparing biodegradable trace cutting oil |
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