CN1089747C - Process for prepared boronized high-basicity magnesium alkylsalicylate as additive of lubricating oil - Google Patents
Process for prepared boronized high-basicity magnesium alkylsalicylate as additive of lubricating oil Download PDFInfo
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- CN1089747C CN1089747C CN99100369A CN99100369A CN1089747C CN 1089747 C CN1089747 C CN 1089747C CN 99100369 A CN99100369 A CN 99100369A CN 99100369 A CN99100369 A CN 99100369A CN 1089747 C CN1089747 C CN 1089747C
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- reaction
- warming
- methyl alcohol
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- additive
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- 239000011777 magnesium Substances 0.000 title claims abstract description 17
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims abstract description 13
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 13
- 238000000034 method Methods 0.000 title claims abstract description 6
- 239000000654 additive Substances 0.000 title claims abstract description 5
- 230000000996 additive effect Effects 0.000 title claims abstract description 5
- 239000010687 lubricating oil Substances 0.000 title abstract description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 36
- 238000006243 chemical reaction Methods 0.000 claims description 22
- 238000010792 warming Methods 0.000 claims description 18
- 239000002904 solvent Substances 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 13
- 238000010025 steaming Methods 0.000 claims description 10
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 claims description 9
- 229960004217 benzyl alcohol Drugs 0.000 claims description 9
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 9
- 239000004327 boric acid Substances 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 9
- 238000002360 preparation method Methods 0.000 claims description 7
- -1 alkyl salicylate Chemical compound 0.000 claims description 6
- 239000003879 lubricant additive Substances 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- 239000003153 chemical reaction reagent Substances 0.000 claims description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 4
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 4
- 235000011089 carbon dioxide Nutrition 0.000 claims description 4
- 238000010790 dilution Methods 0.000 claims description 3
- 239000012895 dilution Substances 0.000 claims description 3
- 238000009835 boiling Methods 0.000 claims description 2
- 238000006386 neutralization reaction Methods 0.000 claims description 2
- 229960001860 salicylate Drugs 0.000 claims description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims 1
- 238000005271 boronizing Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 9
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 239000002585 base Substances 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 5
- 239000003599 detergent Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 229910052796 boron Inorganic materials 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- 238000009833 condensation Methods 0.000 description 3
- 230000005494 condensation Effects 0.000 description 3
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 description 2
- 235000012245 magnesium oxide Nutrition 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 238000009423 ventilation Methods 0.000 description 2
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000007810 chemical reaction solvent Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000006184 cosolvent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 235000011837 pasties Nutrition 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
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- Lubricants (AREA)
Abstract
The present invention relates to a method for preparing boronized high-basicity magnesium alkylsalicylate as additive of lubricating oil, which is synthesized in a two-step method of preparing and boronizing high-basicity magnesium alkylsalicylate.
Description
The present invention relates to a kind of high-basicity magnesium alkylaslicylate as lubricant additive of boronation, belong to the lubricating oil field.
The mistakes basicity component of tradition purification agent is that the form with carbonate exists, thereby the mistakes basicity metal detergent of this carbonating can quicken the oxidation of oil under exacting terms the metallic surface appearance is worn and torn.The beginning of the nineties at the end of the eighties, external each major oil companies develop and have developed with the boride metal purification agent of borate as the alkali storehouse, as U.S.4,965,004,3,4830,548 etc., domestic also do not have a relevant patent report, and this novel boride metal purification agent not only has the effect of purification agent, and good oxidative stability arranged, excellent friction resistant polishing machine etc.
Patent 4,965,004 has described a kind of preparation method of metal detergent of boronation.It is in the presence of a kind of proton type solvent and a kind of hydrocarbon cosolvent, and boronation reagent is joined in a kind of high alkaline metal detergent, stirs, and reacts 0.25-5.0 hour, and steaming desolventizes, and after the filtration, obtains a kind of metal detergent of boronation.
Patent 3,480,548 it be with a kind of high base number metal detergent (150-175 ℃) and boric acid or other boronation reagent react under very high temperature, it carries out in the presence of the solvent not having.This just causes CO
2Overflow fast, cause serious bubble-related issues.
The process of boronation of the present invention is (30-70 ℃) that carries out under lower temperature, and begins to prepare from untreated high base number magnesium alkylsalicylate, and the boron amount is improved.
The present invention seeks to provide a kind of high-basicity magnesium alkylaslicylate as lubricant additive of boronation, thereby a kind of new additive agent of excellent property is provided for top-grade lubricating oil.
Boronation high-basicity magnesium alkylaslicylate as lubricant additive of the present invention prepares with following method: 1, the preparation of high base number magnesium alkylsalicylate.The preparation method of high base number magnesium alkylsalicylate is existing narration in patent ZL94101431.2 and ZL94101432.0.2, the methyl alcohol and the solvent that in the reaction mixture of the first step, add metering, stirring is warming up between 30～70 ℃, adds the boric acid of metering, reacts 0.5～4 hour, reaction is warming up to 110 ℃ after finishing, steaming engaging benzenemethanol and water, solubilizing agent dilution, the cooling back is centrifugal, steams desolventizing at last, gets product.
A kind of preparation method of high-basicity magnesium alkylaslicylate as lubricant additive of boronation, it is characterized in that: reactions steps is carried out in two steps: the reaction of the first step high basicity, solvent and methyl alcohol are put into reactor, stirring also is warming up to 30～60 ℃, drop into light magnesium oxide, add entry and ammoniacal liquor simultaneously, continue to stir, kept 10-13 minute, add alkyl salicylate then, and keep temperature of reaction between 30～60 ℃, carry out neutralization reaction 1 hour, and fed carbonic acid gas then and carry out high basicity reaction 2 hours, be warming up to 110 ℃, steaming engaging benzenemethanol and water, cooling.The boronation reaction of second step, the boronation temperature of reaction maintains between 30～70 ℃, and the boronation reaction times is 0.5～4 hour, and reaction is warming up to 110 ℃ after finishing, steaming engaging benzenemethanol and water, the solubilizing agent dilution, the cooling back is centrifugal, steams desolventizing at last and gets product.Add 5～45 parts of methyl alcohol in 100 parts of alkyl salicylates, 10～100 parts of solvents, 20～50 parts of boric acid, methyl alcohol must be purity greater than 95% chemical reagent or industrial goods, the reaction solvent for use is that dimethylbenzene or boiling range are 60～160 ℃ straight-run spirit, and the boric acid of reaction usefulness can be that SILVER REAGENT also can be a technical grade product.
Embodiment 1
Add 200 milliliters in gasoline in having 500 milliliters of there-necked flasks of electric mixer and condensation water trap, 90 milliliters of methyl alcohol stir, and are warming up to about 50 ℃; Drop into 16.0 gram light magnesium oxides, stir, water and ammonia water mixture (3～4 parts of water add 1 part of ammoniacal liquor) are added in the mixture for about 65 milliliters, react after 20～30 minutes, mixture becomes pasty state, adds 100.0 gram alkyl salicylates, stirs, control reaction temperature is 50～55 ℃, reacts 1 hour.After reaction is finished, feed carbonic acid gas, Ventilation Rate is 200～250 ml/min, about 120 minutes; Reaction is warming up to 110 ℃ after finishing, steaming engaging benzenemethanol and water, and 14 milliliters of methyl alcohol are added in cooling, stir, and are warming up to 50～55 ℃ then, add boric acid 24.7 grams, react about 90 minutes, carry out the boronation reaction.Reaction is warming up to 110 ℃, steaming engaging benzenemethanol and water after finishing; Cooling, the gasoline that adds twice dilutes.Reaction product under 3600 rev/mins of rotating speeds centrifugal 30 minutes removes solvent under reduced pressure after removing slag and gets product.Product Mg:5.43m%, B:1.67m%, TBN:249mgKOH/g.
Comparative example 1
Add 81 milliliters in gasoline in having 1000 milliliters of there-necked flasks of electric mixer and condensation water trap, 14 milliliters of methyl alcohol stir, and are warming up to 64 ℃; (TBN=281mgKOH/g Mg=6.45m%), and adds 16.6 gram boric acid to the magnesium alkylsalicylate of input 100.0 gram high base numbers, reacts 1.5 hours.Reaction is warming up to 110 ℃, steaming engaging benzenemethanol and water after finishing; Cooling, the gasoline that adds twice dilutes, and is centrifugal, removes solvent under reduced pressure and get product.Product Mg:5.41m%, B:0.62m%, TBN:244mgKOH/g.
Embodiment 2
Add 400 milliliters in gasoline in having 1000 milliliters of there-necked flasks of electric mixer and condensation water trap, 180 milliliters of methyl alcohol stir, and are warming up to 50～60 ℃; Drop into 32.0 gram light magnesium oxides, stir, water and ammonia water mixture are added in the mixture for about 130 milliliters, react after 20～30 minutes, add 200 gram alkyl salicylates, keeping temperature of reaction is 50～55 ℃, reacts 1 hour; Feed carbonic acid gas then, Ventilation Rate is 400～450 milliliters, is warming up to 50～60 ℃ then; Add boric acid 49.4 grams, reacted about 90 minutes, carry out boronation and react, reaction is warming up to 110 ℃ after finishing, steaming engaging benzenemethanol and water, and cooling, the gasoline that adds twice dilutes, and is centrifugal, removes solvent under reduced pressure and get product.Product Mg:5.81m%, B:3.2m%, TBN:313mgKOH/g.
Claims (2)
1, a kind of preparation method of high-basicity magnesium alkylaslicylate as lubricant additive of boronation is characterized in that this additive prepares by the following method:
Solvent and methyl alcohol are put into reactor, stir and be warming up to 30～60 ℃, drop into light magnesium oxide, add entry and ammoniacal liquor simultaneously, continue to stir, kept 10-13 minute, add alkyl salicylate then, and keep temperature of reaction between 30～60 ℃, carried out neutralization reaction 1 hour, feed carbonic acid gas then and carry out high basicity reaction 2 hours, be warming up to 110 ℃, steaming engaging benzenemethanol and water, cooling, add solvent and methyl alcohol, be warming up between 30～70 ℃, add boric acid, reacted 0.5～4 hour, reaction is warming up to 110 ℃, steaming engaging benzenemethanol and water after finishing, the solubilizing agent dilution, the cooling back is centrifugal, steams desolventizing at last and gets product, in the boronation reaction, per 100 parts of alkyl salicylates are added 5～45 parts of methyl alcohol, 10～100 parts of solvents, 20～50 parts of boric acid, reaction is that dimethylbenzene or boiling range are 60～160 ℃ straight-run spirit with solvent.
2, the preparation method of additive according to claim 1 is characterized in that: methyl alcohol must be purity greater than 95% chemical reagent or industrial goods.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99100369A CN1089747C (en) | 1999-01-26 | 1999-01-26 | Process for prepared boronized high-basicity magnesium alkylsalicylate as additive of lubricating oil |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99100369A CN1089747C (en) | 1999-01-26 | 1999-01-26 | Process for prepared boronized high-basicity magnesium alkylsalicylate as additive of lubricating oil |
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| Publication Number | Publication Date |
|---|---|
| CN1262266A CN1262266A (en) | 2000-08-09 |
| CN1089747C true CN1089747C (en) | 2002-08-28 |
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| CN99100369A Expired - Fee Related CN1089747C (en) | 1999-01-26 | 1999-01-26 | Process for prepared boronized high-basicity magnesium alkylsalicylate as additive of lubricating oil |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110295079A (en) * | 2019-07-19 | 2019-10-01 | 中国科学院兰州化学物理研究所 | A kind of preparation and application of low-temperature lubrication oil additive |
| CN113234517A (en) * | 2021-05-07 | 2021-08-10 | 新乡市瑞丰新材料股份有限公司 | Preparation method of nano-grade high-boron-content composite magnesium detergent |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4965004A (en) * | 1989-04-21 | 1990-10-23 | Texaco Inc. | Process for a borated detergent additive |
| CN1107461A (en) * | 1994-02-23 | 1995-08-30 | 中国石化兰州炼油化工总厂 | Process for preparing high-basicity magnesium alkylsalicylate |
-
1999
- 1999-01-26 CN CN99100369A patent/CN1089747C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4965004A (en) * | 1989-04-21 | 1990-10-23 | Texaco Inc. | Process for a borated detergent additive |
| CN1107461A (en) * | 1994-02-23 | 1995-08-30 | 中国石化兰州炼油化工总厂 | Process for preparing high-basicity magnesium alkylsalicylate |
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| Publication number | Publication date |
|---|---|
| CN1262266A (en) | 2000-08-09 |
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