CN104031718B - A kind of boronation aliphatic amide ester lubricating additive and preparation method thereof - Google Patents
A kind of boronation aliphatic amide ester lubricating additive and preparation method thereof Download PDFInfo
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- CN104031718B CN104031718B CN201410276225.XA CN201410276225A CN104031718B CN 104031718 B CN104031718 B CN 104031718B CN 201410276225 A CN201410276225 A CN 201410276225A CN 104031718 B CN104031718 B CN 104031718B
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- aliphatic amide
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- -1 aliphatic amide ester Chemical class 0.000 title claims abstract description 71
- 239000000654 additive Substances 0.000 title claims abstract description 35
- 230000000996 additive effect Effects 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 230000001050 lubricating effect Effects 0.000 title claims abstract description 26
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims abstract description 58
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 36
- 150000001412 amines Chemical class 0.000 claims abstract description 31
- 229960003742 phenol Drugs 0.000 claims abstract description 29
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 18
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims abstract description 16
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical compound CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 claims abstract description 16
- QYDYPVFESGNLHU-KHPPLWFESA-N methyl oleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC QYDYPVFESGNLHU-KHPPLWFESA-N 0.000 claims abstract description 16
- CYQAYERJWZKYML-UHFFFAOYSA-N phosphorus pentasulfide Chemical compound S1P(S2)(=S)SP3(=S)SP1(=S)SP2(=S)S3 CYQAYERJWZKYML-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229960004418 trolamine Drugs 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims abstract description 13
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims abstract description 13
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims abstract description 13
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000005642 Oleic acid Substances 0.000 claims abstract description 13
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000004327 boric acid Substances 0.000 claims abstract description 13
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims abstract description 13
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 5
- 230000015572 biosynthetic process Effects 0.000 claims description 18
- 238000003786 synthesis reaction Methods 0.000 claims description 18
- 238000001816 cooling Methods 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 3
- 229910052717 sulfur Inorganic materials 0.000 abstract description 8
- 239000011593 sulfur Substances 0.000 abstract description 7
- TZHYBRCGYCPGBQ-UHFFFAOYSA-N [B].[N] Chemical group [B].[N] TZHYBRCGYCPGBQ-UHFFFAOYSA-N 0.000 abstract description 3
- 230000003078 antioxidant effect Effects 0.000 abstract description 3
- 230000006837 decompression Effects 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 239000010687 lubricating oil Substances 0.000 description 15
- 239000003921 oil Substances 0.000 description 10
- 231100000241 scar Toxicity 0.000 description 7
- 229910000831 Steel Inorganic materials 0.000 description 6
- 239000010959 steel Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 230000007613 environmental effect Effects 0.000 description 3
- 238000011835 investigation Methods 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical group N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012208 gear oil Substances 0.000 description 2
- 239000010720 hydraulic oil Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 239000002199 base oil Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000002283 diesel fuel Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 230000010534 mechanism of action Effects 0.000 description 1
- 239000010705 motor oil Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
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Abstract
The invention discloses a kind of boronation aliphatic amide ester lubricating additive and preparation method thereof, Witconol 2301 and trolamine are placed in container, react 4 ~ 5 hours under the condition of temperature 90 DEG C, pressure 80mmHg, then add oleic acid and react again, obtain amine hydroxybenzene; Mixed with thiophosphoric anhydride and lauryl alcohol by amine hydroxybenzene, high pressure uninterruptedly circulates and passes into ammonia, temperature 170 DEG C ~ 180 DEG C, reacts 4 ~ 5 hours, obtains aliphatic amide ester cpds.Aliphatic amide ester and boric acid are mixed, temperature 100 DEG C, pressure 230mmHg, reaction 4-5 hour, then decompression is to 30mmHg, then reacts, then lower the temperature, filter, obtain boronation aliphatic amide ester lubricating additive.The present invention is uninterruptedly circulated by three-step reaction and passes into ammonia and two steps decompression method and make a kind of novel novel boronation aliphatic amide ester lubricating additive with low-sulfur, low-phosphorous, efficient, nitrogen boron structure, preparing product there is excellent wear-resistant, antifriction and antioxidant property, production method is simple, cost is low, and product structure is stablized.
Description
Technical field
The present invention relates to a kind of lubricating oil additive and preparation method thereof, relate in particular to a kind of boronation aliphatic amide ester lubricating additive and preparation method thereof.
Background technology
In order to increase the antifriction antiwear effect of lubricating oil, usually in lubricating oil, a small amount of lubricating oil additive is added, traditional lubricating oil additive is high-sulfur, high phosphorus or containing chlorine type anti-wear agent, this kind of additive has corrodibility and selectivity to friction pair material, and not environmentally.For the novel antiwear and antifriction mechanism of action, as far back as middle 1960s, people just start to study with different laboratory apparatuss, analysis means.Boronation aliphatic amide ester containing B, S, P, N in molecular structure, be applied in lubricating oil, greatly can improve oil product antiwear and antifriction function, ashless, increase lubrication and dispersing property and thermo-oxidative stability, be applied in especially in two, three class base oils and full synthetic oil, have splendid oil soluble and efficient oilness.
With the compatibility of other lubricating oil additives in, shown by a large amount of four balls long mill experiments, boronation aliphatic amide ester additive and multiple additives have outstanding wear-resistant synergy, significantly can heighten the extreme pressure value of system, lower frictional coefficient, reduce wear scar diameter, strengthen oxidation stability and thermostability, this has great importance to development low-sulfur, low-phosphorous engine oil.Meanwhile, be applied in gear oil, due to containing BN, greatly can improve the weld load of system, due to low-sulfur, low-phosphorous, ashless, nitrogen boron structure, so boronation aliphatic amide ester is again a kind of environment-friendly lubricating oil additive of great potential.
Boronation aliphatic amide ester, as a kind of novel lubricating oil additive, has low-sulfur, low-phosphorous, efficient characteristic of environmental protection; Due to containing boron nitride structure, there is again effective compatibility of amine, so have excellent wear-resistant, antifriction and anti-oxidant feature, be widely applied in petrol and diesel oil, gear oil, antiwear hydraulic oil, ashless anti-wear hydraulic oil, ashless high pressureturbine oil, effectively can improve long mill, improve PB value, improve the oil soluble in two, three class oil and full synthetic oil.
Summary of the invention
The invention provides and a kind of there is low-sulfur, low-phosphorous, efficient characteristic of environmental protection, the boronation aliphatic amide ester lubricating additive again with effective compatibility of boron nitride structure and amine and preparation method thereof.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is: a kind of preparation method of boronation aliphatic amide ester lubricating additive, react with Witconol 2301 and trolamine and generate amine hydroxybenzene, mix with thiophosphoric anhydride and lauryl alcohol again, high pressure uninterruptedly circulates and passes into ammonia generation aliphatic amide ester, last and acid reaction two step reduces pressure method, makes boronation aliphatic amide ester lubricating additive.
Specifically, the preparation method of described boronation aliphatic amide ester lubricating additive, comprises the steps:
1) synthesis of amine hydroxybenzene
Witconol 2301 and trolamine are placed in container, react 4 ~ 5 hours under the condition of temperature 80 DEG C-90 DEG C, pressure 160mmHg-180mmHg, add oleic acid adjusted to ph and reach 9-10, then under pressure 40mmHg-50mmHg condition, temperature continues reaction 2 ~ 4 hours for 100 DEG C-110, obtains amine hydroxybenzene;
2) synthesis of aliphatic amide ester
The amine hydroxybenzene of preparation is mixed with thiophosphoric anhydride and lauryl alcohol, pressure 0.2MPa-0.25MPa uninterruptedly circulates and passes into ammonia, temperature 170 DEG C ~ 180 DEG C, react 4 ~ 5 hours, then temperature is transferred to 110 DEG C ~ 120 DEG C, stop passing into ammonia, pressure 20mmHg-30mmHg reacts 2 ~ 3 hours again, obtains aliphatic amide ester cpds;
3) synthesis of boronation aliphatic amide ester
The aliphatic amide ester of preparation and boric acid are mixed, temperature 100 DEG C-110 DEG C, pressure 210mmHg-230mmHg, reaction 4-5 hour, then cool to 70 DEG C-80 DEG C, pressure 20mmHg-30mmHg, then react 2-3 hour, cooling, filters, obtains boronation aliphatic amide ester lubricating additive.
Described step 1) in Witconol 2301 and trolamine, oleic acid weight ratio be 100-120:60-70:20-24.
Described step 2) in amine hydroxybenzene and thiophosphoric anhydride, lauryl alcohol weight ratio be 100-120:20-26:12-14.
Described step 3) in aliphatic amide ester and boric acid weight ratio be 100-120:15-18.
Preferably, the weight ratio of described Witconol 2301 and trolamine, oleic acid is 100:60:20; The weight ratio of amine hydroxybenzene and thiophosphoric anhydride, lauryl alcohol is 100:20:12; Aliphatic amide ester and boric acid weight ratio are 100:15.
Boronation aliphatic amide ester lubricating additive prepared by above-mentioned preparation method.
The invention has the beneficial effects as follows: uninterruptedly being circulated by three-step reaction is passed into ammonia and two steps decompression method and make a kind of novel novel boronation aliphatic amide ester lubricating additive with low-sulfur, low-phosphorous, efficient, nitrogen boron structure, product has excellent wear-resistant, antifriction and antioxidant property, there is excellent dispersing property, efficient, environmental protection.To friction pair material, not there is corrodibility and selectivity.
Embodiment
The preparation method of boronation aliphatic amide ester lubricating additive of the present invention, react with Witconol 2301 and trolamine and generate amine hydroxybenzene, mix with thiophosphoric anhydride and lauryl alcohol again, high pressure uninterruptedly circulates and passes into ammonia generation aliphatic amide ester, last and acid reaction two step reduces pressure method, makes boronation aliphatic amide ester lubricating additive.
Specifically, the preparation method of described boronation aliphatic amide ester lubricating additive, comprises the steps:
1) synthesis of amine hydroxybenzene
Witconol 2301 and trolamine are placed in container, react 4 ~ 5 hours under the condition of temperature 80 DEG C-90 DEG C, pressure 160mmHg-180mmHg, add oleic acid adjusted to ph and reach 9-10, then under pressure 40mmHg-50mmHg condition, temperature continues reaction 2 ~ 4 hours for 100 DEG C-110, obtains amine hydroxybenzene;
2) synthesis of aliphatic amide ester
The amine hydroxybenzene of preparation is mixed with thiophosphoric anhydride and lauryl alcohol, pressure 0.2MPa-0.25MPa uninterruptedly circulates and passes into ammonia, temperature 170 DEG C ~ 180 DEG C, react 4 ~ 5 hours, then temperature is transferred to 110 DEG C ~ 120 DEG C, stop passing into ammonia, pressure 20mmHg-30mmHg reacts 2 ~ 3 hours again, obtains aliphatic amide ester cpds;
3) synthesis of boronation aliphatic amide ester
The aliphatic amide ester of preparation and boric acid are mixed, temperature 100 DEG C-110 DEG C, pressure 210mmHg-230mmHg, reaction 4-5 hour, then cool to 70 DEG C-80 DEG C, pressure 20mmHg-30mmHg, then react 2-3 hour, cooling, filters, obtains boronation aliphatic amide ester lubricating additive.
Described step 1) in Witconol 2301 and trolamine, oleic acid weight ratio be 100-120:60-70:20-24.
Described step 2) in amine hydroxybenzene and thiophosphoric anhydride, lauryl alcohol weight ratio be 100-120:20-26:12-14.
Described step 3) in aliphatic amide ester and boric acid weight ratio be 100-120:15-18.
Preferably, the weight ratio of described Witconol 2301 and trolamine, oleic acid is 100:60:20; The weight ratio of amine hydroxybenzene and thiophosphoric anhydride, lauryl alcohol is 100:20:12; Aliphatic amide ester and boric acid weight ratio are 100:15.
Boronation aliphatic amide ester lubricating additive prepared by above-mentioned preparation method.
Below in conjunction with embodiment, the present invention is described in further detail:
Embodiment 1
1, the synthesis of amine hydroxybenzene
Witconol 2301 100 grams and trolamine 60 grams are placed in container, temperature 90 DEG C, react 4 hours under the condition of pressure 180mmHg, add oleic acid 20 grams of adjusted to ph and reach about 10, then, under pressure 40mmHg condition, temperature 100 DEG C continues reaction 2 hours, obtains amine hydroxybenzene.
2, the synthesis of aliphatic amide ester
In the 300ml there-necked flask that mechanical stirrer, thermometer and still head are housed, the amine hydroxybenzene 100 grams getting above-mentioned preparation mixes with thiophosphoric anhydride 20 grams and lauryl alcohol 12 grams, high pressure uninterruptedly circulates and passes into ammonia, temperature about 170 DEG C, react 5 hours, then temperature regulating is low to 120 DEG C, stops passing into ammonia, vacuum reacts 3 hours again, obtains aliphatic amide ester cpds.
3, the synthesis of boronation aliphatic amide ester
The aliphatic amide ester 100 grams of preparation and boric acid 15 grams are mixed, temperature 100 DEG C, pressure 230mmHg, reacts 5 hours, then cool to 80 DEG C, pressure 30mmHg, then react 3 hours, cooling, filter, obtain faint yellow boronation aliphatic amide ester lubricating additive, productive rate 90.5%.
The antifriction antiwear of product and the investigation of supporting capacity: utilize four-ball tester to measure, setting load (temperature 20 DEG C, load 392N, speed 1450R/min, time 30min) under extreme pressure and anti-wear and wear-resistant performance, four-ball test steel ball used is the GCR steel ball of diameter 12.7mm, and test shows that product has good extreme pressure and anti-wear and wear-resistant performance.By contrast, directly adopt lubricating oil, wear scar diameter reaches 0.8mm, maximumly reaches 30KG without seizing PB.Add product 1% prepared by the present embodiment in lubricating oil, wear scar diameter reaches 0.42mm, maximumly reaches 90KG without seizing PB.Measure oil soluble energy: the 500N 1, getting 100 grams adds the boronation aliphatic amide ester of 1 gram, clear, after 60 days, clear.2, the PA06 getting 100 grams adds the boronation aliphatic amide ester of 1 gram, clear, after 60 days, and clear.
Embodiment 2
1, the synthesis of amine hydroxybenzene
Witconol 2301 120 grams and trolamine 70 grams are placed in container, temperature 90 DEG C, reacts 4 hours under the condition of pressure 180mmHg, adds oleic acid 24 grams of adjusted to ph and reach about 9, then under vacuum 40mmHg high condition, temperature 100 DEG C continues reaction 4 hours, obtains amine hydroxybenzene.
2, the synthesis of aliphatic amide ester
In the 500ml there-necked flask that mechanical stirrer, thermometer and still head are housed, the amine hydroxybenzene 200 grams getting above-mentioned preparation mixes with thiophosphoric anhydride 45 grams and lauryl alcohol 25 grams, high pressure uninterruptedly circulates and passes into ammonia, temperature about 180 DEG C, react 4 hours, then temperature regulating is low to 110 DEG C, stops passing into ammonia, and vacuum reacts 2 hours again.Obtain aliphatic amide ester cpds.
The synthesis of 3 boronation aliphatic amide esters
The aliphatic amide ester 200 grams of preparation and boric acid 35 grams are mixed, temperature 105 DEG C, pressure 230mmHg, reacts 4 hours, then cool to 85 DEG C, pressure 30mmHg, then react 2 hours, cooling, filter, obtain faint yellow boronation aliphatic amide ester lubricating additive, productive rate 92.5%.
The antifriction antiwear of product and the investigation of supporting capacity: utilize four-ball tester to measure, setting load (temperature 20 DEG C, load 392N, speed 1450R/min, time 30min) under extreme pressure and anti-wear and wear-resistant performance, four-ball test steel ball used is the GCR steel ball of diameter 12.7mm, and test shows that product has good extreme pressure and anti-wear and wear-resistant performance.By contrast, directly adopt lubricating oil, wear scar diameter reaches 0.8mm, maximumly reaches 30KG without seizing PB.Add product 1% prepared by the present embodiment in lubricating oil, wear scar diameter reaches 0.40mm, maximumly reaches 90KG without seizing PB.Measure oil soluble energy: the 500N 1, getting 100 grams adds the boronation aliphatic amide ester of 1 gram, clear, after 60 days, clear.2, the PA06 getting 100 grams adds the boronation aliphatic amide ester of 1 gram, clear, after 60 days, and clear.
Embodiment 3
1, the synthesis of amine hydroxybenzene
Witconol 2301 110 grams and trolamine 65 grams are placed in container, temperature 90 DEG C, reacts 5 hours under the condition of pressure 180mmHg, adds oleic acid 22 adjusted to ph and reach about 9.5, then under vacuum 40mmHg condition, temperature 100 DEG C continues reaction 3 hours, obtains amine hydroxybenzene.
2, the synthesis of aliphatic amide ester
In the 500ml there-necked flask that mechanical stirrer, thermometer and still head are housed, the amine hydroxybenzene 300 grams getting above-mentioned preparation mixes with thiophosphoric anhydride 55 grams and lauryl alcohol 30 grams, high pressure uninterruptedly circulates and passes into ammonia, temperature about 170 DEG C, react 4.5 hours, then temperature regulating is low to 120 DEG C, stops passing into ammonia, and vacuum reacts 2.5 hours again.Obtain aliphatic amide ester cpds.
The synthesis of 3 boronation aliphatic amide esters
The aliphatic amide ester 400 grams of preparation and boric acid 55 grams are mixed, temperature 100 DEG C, pressure 230mmHg, reacts 4.5 hours, then cool to 80 DEG C, pressure 30mmHg, then react 2.5 hours, cooling, filter, obtain faint yellow boronation aliphatic amide ester lubricating additive, productive rate 88.5%.
The antifriction antiwear of product and the investigation of supporting capacity: utilize four-ball tester to measure, setting load (temperature 20 DEG C, load 392N, speed 1450R/min, time 30min) under extreme pressure and anti-wear and wear-resistant performance, four-ball test steel ball used is the GCR steel ball of diameter 12.7mm, and test shows that product has good extreme pressure and anti-wear and wear-resistant performance.By contrast, directly adopt lubricating oil, wear scar diameter reaches 0.8mm, maximumly reaches 30KG without seizing PB.Add product 1% prepared by the present embodiment in lubricating oil, wear scar diameter reaches 0.39mm, maximumly reaches 90KG without seizing PB.Measure oil soluble energy: the 500N 1, getting 100 grams adds the boronation aliphatic amide ester of 1 gram, clear, after 60 days, clear.2, the PA06 getting 100 grams adds the boronation aliphatic amide ester of 1 gram, clear, after 60 days, and clear.
In sum, content of the present invention is not limited in the above-described embodiment, and the knowledgeable people in same area can propose other embodiment easily within technical director's thought of the present invention, but this embodiment all comprises within the scope of the present invention.
Claims (3)
1. the preparation method of a boronation aliphatic amide ester lubricating additive, it is characterized in that, react with Witconol 2301 and trolamine and generate amine hydroxybenzene, mix with thiophosphoric anhydride and lauryl alcohol again, high pressure uninterruptedly circulates and passes into ammonia generation aliphatic amide ester, last and acid reaction two step reduces pressure method, makes boronation aliphatic amide ester lubricating additive, comprises the steps:
1) synthesis of amine hydroxybenzene
Witconol 2301 and trolamine are placed in container, react 4 ~ 5 hours under the condition of temperature 80 DEG C-90 DEG C, pressure 160mmHg-180mmHg, add oleic acid adjusted to ph and reach 9-10, then under pressure 40mmHg-50mmHg condition, temperature 100 DEG C-110 DEG C continues reaction 2 ~ 4 hours, obtain amine hydroxybenzene, the weight ratio of Witconol 2301 and trolamine, oleic acid is 100-120:60-70:20-24;
2) synthesis of aliphatic amide ester
The amine hydroxybenzene of preparation is mixed with thiophosphoric anhydride and lauryl alcohol, pressure 0.2MPa-0.25MPa uninterruptedly circulates and passes into ammonia, temperature 170 DEG C ~ 180 DEG C, react 4 ~ 5 hours, then temperature is transferred to 110 DEG C ~ 120 DEG C, stop passing into ammonia, pressure 20mmHg-30mmHg reacts 2 ~ 3 hours again, obtain aliphatic amide ester cpds, the weight ratio of amine hydroxybenzene and thiophosphoric anhydride, lauryl alcohol is 100-120:20-26:12-14;
3) synthesis of boronation aliphatic amide ester
The aliphatic amide ester of preparation and boric acid are mixed, temperature 100 DEG C-110 DEG C, pressure 210mmHg-230mmHg, reaction 4-5 hour, then cools to 70 DEG C-80 DEG C, pressure 20mmHg-30mmHg, react 2-3 hour again, cooling, filter, obtain boronation aliphatic amide ester lubricating additive, aliphatic amide ester and boric acid weight ratio are 100-120:15-18.
2. the preparation method of boronation aliphatic amide ester lubricating additive according to claim 1, is characterized in that, the weight ratio of described Witconol 2301 and trolamine, oleic acid is 100:60:20; The weight ratio of amine hydroxybenzene and thiophosphoric anhydride, lauryl alcohol is 100:20:12; Aliphatic amide ester and boric acid weight ratio are 100:15.
3. boronation aliphatic amide ester lubricating additive prepared by the preparation method as described in any one of claim 1-2.
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| CN104611090A (en) * | 2014-12-09 | 2015-05-13 | 大庆劲普化工有限公司 | Magnetic boronized phosphonate amine ester lubricating oil additive |
| CN107011971B (en) * | 2017-04-19 | 2020-05-05 | 纳米克斯（辽宁）能源有限公司 | Sulfur-phosphorus-nitrogen lubricating oil additive and preparation method thereof |
| CN109536250B (en) * | 2018-11-02 | 2021-09-14 | 欧陆宝(天津)新材料科技有限公司 | Environment-friendly degradable aluminum and aluminum alloy drawing process lubricant and preparation method thereof |
| CN109679752B (en) * | 2019-01-29 | 2021-10-15 | 汉能（青岛）润滑科技有限公司 | Degradable lubricating oil adopting permeation layer technology and preparation method thereof |
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| CN1931980A (en) * | 2006-09-29 | 2007-03-21 | 陈必昌 | Process of preparing lubricant for hardware production |
| CN101037638A (en) * | 2006-03-15 | 2007-09-19 | 中国石油化工股份有限公司 | Phosphamide ester extreme pressure anti-wear additives and preparation and application thereof |
| CN102453916A (en) * | 2010-10-21 | 2012-05-16 | 王严绪 | Non-sulfur and non-phosphorus water-soluble organic boron additive |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101037638A (en) * | 2006-03-15 | 2007-09-19 | 中国石油化工股份有限公司 | Phosphamide ester extreme pressure anti-wear additives and preparation and application thereof |
| CN1931980A (en) * | 2006-09-29 | 2007-03-21 | 陈必昌 | Process of preparing lubricant for hardware production |
| CN102453916A (en) * | 2010-10-21 | 2012-05-16 | 王严绪 | Non-sulfur and non-phosphorus water-soluble organic boron additive |
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Effective date of registration: 20160121 Address after: Lanyuan road 300384 Tianjin city Nankai District Huayuan Industrial Park No. 2 (No. II) 2 No. 1602 Patentee after: Wang Yanxu Address before: 300384 Tianjin City, Nankai District Huayuan Industrial Park orchid Road No. 2 Patentee before: Tianjin Shun Neng chemical company limited |