CN1080715C - Process for preparing alkaline alkyl sodium salicylate - Google Patents
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- CN1080715C CN1080715C CN97111390A CN97111390A CN1080715C CN 1080715 C CN1080715 C CN 1080715C CN 97111390 A CN97111390 A CN 97111390A CN 97111390 A CN97111390 A CN 97111390A CN 1080715 C CN1080715 C CN 1080715C
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Abstract
The present invention relates to a method for preparing alkaline alkyl sodium salicylate. In the method, alkyl salicylic acid and calcium hydroxide are used as raw materials, and the materials can be respectively combined into different kinds of alkyl sodium salicylate with super-high, high, medium or low alkali numbers in a low molecular alcohol accelerator by different mixing ratios; the terminal point of carbonation is controlled by the pH value of reacting liquid; when the action is over, the needed product is obtained by the steps of filter aid addition, pressure filtration, deslagging and solvent removal by steaming. The synthesized product of the present invention has the advantages of low viscosity, low turbidity, steady performance, etc.
Description
The present invention relates to a kind of peace and quiet dispersing additive that is used for internal combustion (IC) engine lubricating oil, particularly a kind of is to contain the preparation method that the oxygen on-macromolecular organic compound is the lubricating composition of feature with additive.
Alkaline alkyl sodium salicylate is better as a class intrinsic detergency, neutralising capacity is strong, high temperature is down stable and have the purification agent of certain anti-oxidant, corrosion resistance, has obtained using comparatively widely in especially all kinds of diesel engine oils of modern engine oil.The 11st the 3rd phase of volume of " lubricating oil " magazine has been reported alkylsalicylate development of series product method.The preparation technology of low alkali value alkyl sodium salicylate, adopt calcium chloride solution and sodium salicylate in the presence of gasoline and methyl alcohol, carry out replacement(metathesis)reaction, obtain product through centrifugation, distillation for removing methanol and gasoline then, double decomposition prepares the technical process of low alkali value alkyl sodium salicylate referring to Fig. 1.The synthesis technique of calcium alkyl salicylate with high base number, referring to Fig. 2, at first be that calcium oxide and water carry out slaking reaction in the presence of gasoline, this reaction product and Whitfield's ointment carry out neutralization reaction in the presence of methyl alcohol, then feed carbonic acid gas and carry out high quaternization, reaction product is sloughed the first alcohol and water through distillation, add gasoline dilution then, carry out centrifugation, remove solid slag after, slough gasoline through distillation, obtain product and be calcium alkyl salicylate with high base number.Above-mentioned preparation method, technical process is complicated, long processing time, the alkyl sodium salicylate of making different base numbers will adopt two kinds of different raw materials, two kinds of technologies, when the feeding carbonic acid gas carries out high quaternization, generally weigh the carbonation reaction terminal point with the time, can't judge the end of a period opportunity of high quaternization, often cause the not enough or excessive of carbonation reaction, cause the colloidal particle that forms greater particle size, though centrifugation can be removed the solid slag of greater particle size (mainly being lime carbonate and unreacted calcium hydroxide), can't Ex-all, separate out thereby cause product precipitation after leaving standstill for some time, to occur, the phenomenon that base number descends.In addition, carbonation reaction excessively also makes product viscosity and turbidity increase.
The objective of the invention is to simplify preparation technology, just can produce the alkyl sodium salicylate series product of different base numbers with a kind of processing method; Use easy and practical new to determine the terminal point of carbonation reaction,, prevent to produce the colloidal particle of greater particle size to avoid the not enough of carbonation reaction or excessively; Adopt new separating technology, guarantee that solid slag can more fully separate, make product be steady state in accumulating or use midium or long term, avoid precipitation occurring, viscosity is low, turbidity is little, the alkyl sodium salicylate of the various different base numbers of stable performance thereby produce.
Method provided by the invention is that alkyl salicylate, solvent and promotor are mixed stirring, heating in reaction vessel, input calcium hydroxide, water carry out neutralization reaction, the calcium hydroxide that adds residual content then, feed carbonic acid gas, carry out carbonation reaction, judge reaction end with pH value, after reaction finishes, add thermal distillation and remove promotor and water, add thinner and flocculating aids, solid slag is removed in pressure filtration, and underpressure distillation removes solvent and thinner more at last, thereby makes the alkaline alkyl sodium salicylate lubricating oil additive.Concrete steps are as follows:
1, alkyl salicylate, solvent and promotor are mixed stirring in container, and heat temperature raising is to 30-60 ℃:
2, drop into calcium hydroxide, water, continue to stir, keeping temperature is 30-70 ℃, neutralization reaction 0.5-3 hour;
3, the calcium hydroxide that adds residual content feeds carbon dioxide, continues to stir, and carries out carbonation reaction, maintains the temperature at 30-70 ℃, is 7-12 up to the pH value of reaction solution, stops carbonation reaction;
4, be warming up to more than 80 ℃, promotor, water are removed in distillation;
5, add thinner and flocculating aids, remove solid slag through pressure filtration;
6, the heating underpressure distillation removes and desolvates and thinner.
Said neutralization reaction of the present invention and carbonation reaction, the proportion scale of each component is: in 100 parts of (weight) alkyl salicylates, calcium hydroxide is 4-40 part (weight), promotor is 0.5-100 part (weight), water is 0.5-30 part (weight), and carbonic acid gas is 0.5-30 part (weight), and solvent is 30-500 part, thinner is 0-300 part, and flocculating aids is 3-50 part.
The mixture that the said reaction raw materials alkyl salicylate of the present invention is alkyl salicylate, alkylphenol, mineral lubricating oils etc., the alkylated salicylamide acid content is preferably between the 30-50% (weight) between 20-70% (weight).
The structure of the said alkyl salicylate of the present invention is R-C
6H
3(OH) COOH or R (R ')-C
6H
2(OH)-and COOH or its mixture, wherein R, R ' they are C
8-30Alkyl chain.
The temperature of said neutralization reaction of the present invention and carbonation reaction is controlled at 30-70 ℃, is preferably between 40-65 ℃.
The said carbon dioxide feeding of the present invention speed is per 100 gram alkyl salicylate per minute 5-300 milliliters, is preferably the 20-100 milliliter.
The terminal point of the said carbonation reaction of the present invention is with the pH value control of reaction solution, and general pH value is controlled between the 7-12, is preferably 8-11.
The said promotor of the present invention can be C
1-8Low mass molecule alcohol or its mixture, for example, the mixture of methyl alcohol, ethanol, methyl alcohol and butanols, add-on is 0.5-100 part (weight), is preferably 10-40 part (weight).
The said solvent of the present invention can be hydro carbons or aromatic hydrocarbon solvent, for example, gasoline, dimethylbenzene, add-on is 30-500 part (weight), is preferably 50-200 part (weight).
The said thinner of the present invention can be hydro carbons or aromatic hydrocarbon solvent, for example, gasoline, dimethylbenzene, add-on is 0-300 part (weight), is preferably 0-100 part (weight).
The said flocculating aids of the present invention can be diatomite or light calcium carbonate, and add-on is 3-50 part (weight), is preferably 6-30 part (weight).
The purity of the said calcium hydroxide of the present invention is not less than 95%.The add-on of calcium hydroxide is 3-10 part (weight) in neutralization reaction, drops into the calcium hydroxide of residual content in carbonation reaction.When preparation superelevation, height, in or during the low alkali value alkyl sodium salicylate, total consumption of calcium hydroxide is respectively 25-40 part (weight), 18-30 part (weight), 10-22 part (weight), 4-10 part (weight).
Advantage of the present invention is to have simplified preparation technology, removed the slaking reaction process from, saved preparation time, directly adopt calcium hydroxide and alkyl salicylate to carry out neutralization reaction, utilize the different ratios of calcium hydroxide and alkyl salicylate, can directly prepare overbased, high base number, middle base number or low alkali value alkyl sodium salicylate; In the carbonation reaction process, control reaction end with the pH value of reaction solution, can in time grasp reaction progress degree like this, accurately control reaction end, avoid the not enough or excessive of carbonation reaction, make the additive colloidal solid tiny evenly, product filters easily; Use pressure and filter aid filtration technology, solid slag more fully can be removed by filter, can in product, not precipitate and separate out.The additive of this method preparation, turbidity is little, viscosity is low, stable performance, and its lime carbonate colloidal particle are many below 20nm, are steady state in accumulating and use midium or long term.
Description of drawings:
Fig. 1 double decomposition prepares low alkali value alkyl sodium salicylate process flow sheet
Fig. 2 high base number calcium salicylate synthesis process flow diagram
Fig. 3 alkaline alkyl sodium salicylate synthesis process flow diagram of the present invention
The following examples will be made further supplementary notes to the present invention.
Embodiment 1:
In having 2000 milliliters of there-necked flasks of electronic stirring, condensation water trap, drop into 400 gram alkyl salicylate (acid number 58.24mgKOH/g, acid content 40%) and 454 milliliters of gasoline and 95 ml methanol, stirring is warming up to 30 ℃, add 15.7 gram calcium hydroxides (purity 98.12%) and 11.2 gram water, holding temperature was carried out neutralization reaction 1 hour about 60 ℃.Add 116.8 gram calcium hydroxides then, and feed flow velocity be the carbonic acid gas of 135 milliliters of per minutes to carry out carbonation reaction be 8.1 until the pH value of reaction solution, stop carbonation reaction.Be warming up to 120 ℃ of steaming engaging benzenemethanols and water, add 7300 milliliters of gasoline dilutions, add the super-cell of 60 grams again, pressure filtration, filtrate is removed gasoline through underpressure distillation and is got product.Per hour 1120 liters every square metre of filtration times 6 minutes, filtration velocity.
Resultant metal is than 7.28, base number 319.5mgKOH/g, 100 ℃ of kinematic viscosity 43.26mm
2/ s, turbidity 5.60JTu.Add this routine synthetic product 3% and ZDDP oxidation inhibitor 0.5% in the MVI500 base oil, carry out L-1 coke test (stopped 45 seconds, opened 15 seconds), Jiao weighs 43.6 milligrams.
Embodiment 2:
In having 2000 milliliters of there-necked flasks of electronic stirring, condensation water trap, drop into 400 gram alkyl salicylate (acid number 58.24mgKOH/g, acid content 40%) and 454 milliliters of gasoline and 74 ml methanol, stirring is warming up to 30 ℃, add 1 5.7 gram calcium hydroxides (purity 98.12%) and 11.2 gram water, holding temperature was carried out neutralization reaction 1 hour about 60 ℃.Add 76.9 gram calcium hydroxides then, and feed flow velocity be the carbonic acid gas of 135 milliliters of per minutes to carry out carbonation reaction be 8.9 until the pH value of reaction solution, stop carbonation reaction.Be warming up to 120 ℃ of steaming engaging benzenemethanols and water, add 250 milliliters of gasoline dilutions, add the super-cell of 77 grams again, pressure filtration, filtrate is removed gasoline through underpressure distillation and is got product.Per hour 1380 liters every square metre of filtration times 4 minutes, filtration velocity.
Resultant metal is than 5.07, base number 243.5mgKOH/g, 100 ℃ of kinematic viscosity 21.73mm
2/ s, turbidity 23.66JTu.Add this routine synthetic product 3% and ZDDP oxidation inhibitor 0.5% in the MVI500 base oil, carry out L-1 coke test (stopped 45 seconds, opened 15 seconds), Jiao weighs 38.9 milligrams.
Embodiment 3:
In having 2000 milliliters of there-necked flasks of electronic stirring, condensation water trap, drop into 400 gram alkyl salicylate (acid number 58.24mgKOH/g, acid content 40%) and 454 milliliters of gasoline and 84 ml methanol, stirring is warming up to 30 ℃, add 15.7 gram calcium hydroxides (purity 98.12%) and 11.2 gram water, holding temperature was carried out neutralization reaction 1 hour about 60 ℃.Add 46.9 gram calcium hydroxides then, and feed flow velocity be the carbonic acid gas of 135 milliliters of per minutes to carry out carbonation reaction be 8.5 until the pH value of reaction solution, stop carbonation reaction.Be warming up to 120 ℃ of steaming engaging benzenemethanols and water, add 250 milliliters of gasoline dilutions, add the super-cell of 70 grams again, pressure filtration, filtrate is removed gasoline through underpressure distillation and is got product.Per hour 1104 liters every square metre of filtration times 5 minutes, filtration velocity.
Resultant metal is than 3.43, base number 177.4mgKOH/g, 100 ℃ of kinematic viscosity 19.10mm
2/ s, turbidity 19.46JTu.Add this routine synthetic product 3% and ZDDP oxidation inhibitor 0.5% in the MVI500 base oil, carry out L-1 coke test (stopped 45 seconds, opened 15 seconds), Jiao weighs 32.6 milligrams.
Embodiment 4:
In having 2000 milliliters of there-necked flasks of electronic stirring, condensation water trap, drop into 400 gram alkyl salicylate (acid number 58.24mgKOH/g, acid content 40%) and 454 milliliters of gasoline and 11 ml methanol, stirring is warming up to 30 ℃, add 15.7 gram calcium hydroxides (purity 98.12%) and 11.2 gram water, holding temperature was carried out neutralization reaction 1 hour about 60 ℃.Add 10.0 gram calcium hydroxides then, and feed flow velocity be the carbonic acid gas of 100 milliliters of per minutes to carry out carbonation reaction be 8.3 until the pH value of reaction solution, stop carbonation reaction.Be warming up to 120 ℃ of steaming engaging benzenemethanols and water, add 150 milliliters of gasoline dilutions, add the super-cell of 40 grams again, pressure filtration, filtrate is removed gasoline through underpressure distillation and is got product.Per hour 4760 liters every square metre of filtration times 1 minute, filtration velocity.
Resultant metal is than 1.47, base number 61.7mgKOH/g, 100 ℃ of kinematic viscosity 17.98mm
2/ s, turbidity 3.53JTu.Add this routine synthetic product 3% and ZDDP oxidation inhibitor 0.5% in the MVI500 base oil, carry out L-1 coke test (stopped 45 seconds, opened 15 seconds), Jiao weighs 25.4 milligrams.
Embodiment 5:
In having 2000 milliliters of there-necked flasks of electronic stirring, condensation water trap, drop into 400 gram alkyl salicylate (acid number 34.95mgKOH/g, acid content 24%) and 357 gram dimethylbenzene and 74 ml methanol, stirring is warming up to 35 ℃, add 15.7 gram calcium hydroxides (purity 98.12%) and 11.2 gram water, holding temperature was carried out neutralization reaction 1 hour about 60 ℃.Add 76.9 gram calcium hydroxides then, and feed flow velocity be the carbonic acid gas of 150 milliliters of per minutes to carry out carbonation reaction be 8.7 until the pH value of reaction solution, stop carbonation reaction.Be warming up to 120 ℃ of steaming engaging benzenemethanols and water, add 150 gram dimethylbenzene, add the light calcium carbonate flocculating aids of 70 grams again, pressure filtration, filtrate is removed removal xylene through underpressure distillation and is got product.Per hour 1837 liters every square metre of filtration times 3 minutes, filtration velocity.
Resultant metal is than 7.21, base number 212.5mgKOH/g, 100 ℃ of kinematic viscosity 10.66mm
2/ s, turbidity 8.46JTu.Add this routine synthetic product 3% and ZDDP oxidation inhibitor 0.5% in the MVI500 base oil, carry out L-1 coke test (stopped 45 seconds, opened 15 seconds), Jiao weighs 28.6 milligrams.
Embodiment 6:
In having 2000 milliliters of there-necked flasks of electronic stirring, condensation water trap, drop into 400 gram alkyl salicylate (acid number 34.95mgKOH/g, acid content 24%) and 275 gram gasoline and 34 milliliters of ethanol, stirring is warming up to 40 ℃, add 15.7 gram calcium hydroxides (purity 98.12%) and 10 gram water, holding temperature was carried out neutralization reaction 1 hour about 60 ℃.Add 42.6 gram calcium hydroxides then, and feed flow velocity be the carbonic acid gas of 120 milliliters of per minutes to carry out carbonation reaction be 9.2 until the pH value of reaction solution, stop carbonation reaction.Be warming up to 120 ℃ of steamings and take off ethanol and water, add 150 gram gasoline, add the light calcium carbonate flocculating aids of 70 grams again, pressure filtration, filtrate is removed gasoline through underpressure distillation and is got product.Per hour 1237 liters every square metre of filtration times 4 minutes, filtration velocity.
Resultant metal is than 4.81, base number 151.1mgKOH/g, 100 ℃ of kinematic viscosity 8.37mm
2/ s, turbidity 5.32JTu.Add this routine synthetic product 3% and ZDDP oxidation inhibitor 0.5% in the MVI500 base oil, carry out L-1 coke test (stopped 45 seconds, opened 15 seconds), Jiao weighs 34.3 milligrams.
Embodiment 7:
In having 2000 milliliters of there-necked flasks of electronic stirring, condensation water trap, drop into 400 gram alkyl salicylate (acid number 58.24mgKOH/g, acid content 40%) and 357 gram dimethylbenzene and 84 ml methanol, 18 milliliters of butanols, stirring is warming up to 30 ℃, add 15.7 gram calcium hydroxides (purity 98.12%) and 12 gram water, holding temperature was carried out neutralization reaction 1 hour about 60 ℃.Add 46.9 gram calcium hydroxides then, and feed flow velocity be the carbonic acid gas of 145 milliliters of per minutes to carry out carbonation reaction be 8.9 until the pH value of reaction solution, stop carbonation reaction.Be warming up to 120 ℃ of steaming engaging benzenemethanols, butanols and water, add 150 gram dimethylbenzene dilutions, add the light calcium carbonate flocculating aids of 60 grams again, pressure filtration, filtrate is removed removal xylene through underpressure distillation and is got product.Per hour 1224 liters every square metre of filtration times 4 minutes, filtration velocity.
Resultant metal is than 3.53, base number 181.6mgKOH/g, 100 ℃ of kinematic viscosity 17.83mm
2/ s, turbidity 10.34JTu.Add this routine synthetic product 3% and ZDDP oxidation inhibitor 0.5% in the MVI500 base oil, carry out L-1 coke test (stopped 45 seconds, opened 15 seconds), Jiao weighs 34.4 milligrams.
Claims (26)
1, a kind of preparation method of alkaline alkyl sodium salicylate is characterized in that:
(1), alkyl salicylate, solvent and promotor are mixed stirring in container and be warming up to 30-60 ℃;
(2), drop into calcium hydroxide and water, continue to stir, maintain the temperature between 30-70 ℃ neutralization reaction 0.5-3 hour;
(3), drop into the calcium hydroxide of residual content, feed carbon dioxide, carry out carbonation reaction, holding temperature is at 3070 ℃, is 7-12 up to the pH value of reaction solution, stops carbonation reaction;
(4), be warming up to more than 80 ℃, promotor and water are removed in distillation;
(5), add thinner and flocculating aids, remove solid slag through pressure filtration;
(6), heat underpressure distillation, except that desolvating and thinner.
With respect to the alkyl salicylate of 100 weight parts, the total consumption of calcium hydroxide is the 4-40 weight part, and wherein the input amount of step (2) is the 3-10 weight part.
2, method according to claim 1, it is characterized in that: the proportion scale that participates in the each component of neutralization reaction and carbonation reaction is, alkyl salicylate with respect to 100 weight parts, calcium hydroxide is the 4-40 weight part, and promotor is the 0.5-100 weight part, and water is the 0.5-30 weight part, carbonic acid gas is the 0.5-30 weight part, solvent is the 30-500 weight part, and thinner is the 0-300 weight part, and flocculating aids is the 3-50 weight part.
3, method according to claim 1 and 2 is characterized in that: the reaction raw materials alkyl salicylate is the mixture of alkyl salicylate, alkylphenol, mineral lubricating oils, and wherein the alkylated salicylamide acid content is a 20-70% weight.
4, according to claim 1 or 2 or 3 described methods, it is characterized in that: described alkyl salicylate is R-C
6H
3(OH)-COOH, R (R ')-C
6H
2(OH)-and COOH or its mixture, wherein R, R ' they are C
8-30Alkyl chain.
5, method according to claim 1 is characterized in that the temperature control of neutralization reaction and carbonation reaction is 40-65 ℃.
6, method according to claim 1 is characterized in that: it is per 100 gram alkyl salicylate per minute 5-300 milliliters that carbon dioxide leads to speed.
7, method according to claim 1 is characterized in that, the terminal point of carbonation reaction is with the pH value control of reaction solution, and general pH value is controlled at 8-11.
8, method according to claim 1 and 2 is characterized in that: described promotor is alcohol or its mixture of C1-8.
9, method according to claim 1 is characterized in that: described solvent is alkyl hydro carbons or aromatic hydrocarbon solvent.
10, method according to claim 1 is characterized in that: described thinner is the fragrant hydrocarbon solvent of alkanes or aromatic hydrocarbons.
11, method according to claim 1 is characterized in that: described flocculating aids is diatomite or light calcium carbonate.
12, method according to claim 3 is characterized in that: the content of described alkyl salicylate is 30-50% weight.
13, method according to claim 6 is characterized in that: described carbon dioxide feeding speed is per minute 20-100 milliliter.
14, method according to claim 8 is characterized in that: described promotor is the mixture of methyl alcohol, ethanol or methyl alcohol and propyl alcohol, methyl alcohol and butanols.
15, method according to claim 9 is characterized in that: described solvent is gasoline or dimethylbenzene.
16, method according to claim 10 is characterized in that: described thinner is gasoline or dimethylbenzene.
17, according to Claim 8 or 14 described methods, it is characterized in that: described promotor add-on is the 0.5-100 weight part.
18, according to claim 9 or 15 described methods, it is characterized in that: described solvent adding amount is the 30-500 weight part.
19, according to claim 10 or 16 described methods, it is characterized in that: described thinner add-on is the 0-300 weight part.
20, method according to claim 11 is characterized in that: described flocculating aids add-on is the 3-50 weight part.
21, method according to claim 17 is characterized in that: described promotor add-on is the 10-40 weight part.
22, method according to claim 1 and 2 is characterized in that: described calcium hydroxide purity is more than 95%.
23, method according to claim 1 and 2 is characterized in that: the total consumption of described calcium hydroxide is the 25-40 weight part, is used to prepare overbased alkyl salicylate.
24, method according to claim 1 and 2 is characterized in that: the total consumption of described calcium hydroxide is the 18-30 weight part, is used to prepare the alkyl sodium salicylate of high base number.
25, method according to claim 1 and 2 is characterized in that: the total consumption of described calcium hydroxide is the 10-22 weight part, is used for preparing the alkyl sodium salicylate of base number.
26, method according to claim 1 and 2 is characterized in that: the total consumption of described calcium hydroxide is the 4-10 weight part, is used to prepare the alkyl sodium salicylate of low alkali value.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97111390A CN1080715C (en) | 1997-06-13 | 1997-06-13 | Process for preparing alkaline alkyl sodium salicylate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97111390A CN1080715C (en) | 1997-06-13 | 1997-06-13 | Process for preparing alkaline alkyl sodium salicylate |
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| CN1202479A CN1202479A (en) | 1998-12-23 |
| CN1080715C true CN1080715C (en) | 2002-03-13 |
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| CN97111390A Expired - Fee Related CN1080715C (en) | 1997-06-13 | 1997-06-13 | Process for preparing alkaline alkyl sodium salicylate |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102276450A (en) * | 2011-05-16 | 2011-12-14 | 锦州康泰润滑油添加剂有限公司 | Preparation process for alkaline calcium alkylsalicylate |
| CN102702376A (en) * | 2012-05-24 | 2012-10-03 | 河北科技师范学院 | Process for extracting chestnut polysaccharide by pressurized solvent extraction method |
| CN111170850A (en) * | 2019-12-26 | 2020-05-19 | 山东源根石油化工有限公司 | Additive, preparation method and lubricating oil using additive |
| CN113549481B (en) * | 2021-07-29 | 2023-03-31 | 新乡市瑞丰新材料股份有限公司 | Preparation process of ultrahigh-base-number calcium alkyl salicylate |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2019561C1 (en) * | 1992-07-13 | 1994-09-15 | Дрогобычский опытный завод | Process for preparing alkylsalicylate additive to lubricating oils |
| CN1144216A (en) * | 1995-09-01 | 1997-03-05 | 中国石化兰州炼油化工总厂 | Method for preparation of calcium alkyl salicylate with high base number |
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1997
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2019561C1 (en) * | 1992-07-13 | 1994-09-15 | Дрогобычский опытный завод | Process for preparing alkylsalicylate additive to lubricating oils |
| CN1144216A (en) * | 1995-09-01 | 1997-03-05 | 中国石化兰州炼油化工总厂 | Method for preparation of calcium alkyl salicylate with high base number |
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