CN104496786A - Synthesis method of calcium-magnesium salicylate composite detergent - Google Patents
Synthesis method of calcium-magnesium salicylate composite detergent Download PDFInfo
- Publication number
- CN104496786A CN104496786A CN201410755481.7A CN201410755481A CN104496786A CN 104496786 A CN104496786 A CN 104496786A CN 201410755481 A CN201410755481 A CN 201410755481A CN 104496786 A CN104496786 A CN 104496786A
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- temperature
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- secondary accelerator
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M129/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen
- C10M129/02—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen having a carbon chain of less than 30 atoms
- C10M129/26—Carboxylic acids; Salts thereof
- C10M129/48—Carboxylic acids; Salts thereof having carboxyl groups bound to a carbon atom of a six-membered aromatic ring
- C10M129/54—Carboxylic acids; Salts thereof having carboxyl groups bound to a carbon atom of a six-membered aromatic ring containing hydroxy groups
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/26—Overbased carboxylic acid salts
- C10M2207/262—Overbased carboxylic acid salts derived from hydroxy substituted aromatic acids, e.g. salicylates
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/04—Detergent property or dispersant property
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/10—Inhibition of oxidation, e.g. anti-oxidants
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/12—Inhibition of corrosion, e.g. anti-rust agents or anti-corrosives
Abstract
The invention discloses a synthesis method of a calcium-magnesium salicylate composite detergent in the field of lubricant additives. The method comprises the following steps: adding alkyl salicylic acid and solvent xylene in a reaction container, adding calcium oxide, accelerant, auxiliary promoter and the like in a stirring state, and carrying out a neutralization reaction when a reaction temperature rises to the temperature needed by the neutralization reaction; after the neutralization reaction is ended, adding magnesium oxide, water, ammonia water, auxiliary promoter and the like, charging carbon dioxide and carrying out a carbonation reaction; after the carbonation reaction is ended, carrying out product post-treatment to obtain a lubricant detergent product. The method disclosed by the invention achieves the following beneficial effects: the alkali number of the calcium-magnesium salicylate composite detergent prepared by the method is greater than 400mg KOH/g, the thermal oxidation stability and the high-temperature detergency of lubricant oil are obviously improved, the dispersibility and the wear resistance of the lubricant oil are improved to a certain extent, and the product stability is great.
Description
Technical field
The invention belongs to lubricating oil additive field, be specifically related to a kind of synthetic method of calcium salicylate magnesium complex detergents.
background
detergent for lubricating oil is one of the large additive of modern lubricating oil five (purification agent, dispersion agent, oxidation inhibitor, extreme pressure anti-wear additives, viscosity index improver), grow up with the technical progress of oil engine, along with engine is to high-power, superpower development, and the requirement of user to the drain period extends day by day, thus the use properties of lubricating oil is had higher requirement.In order to meet these service requirementss of lubricating oil, just need in lubricant base, add various dissimilar additive.Detergent for lubricating oil is exactly acid neutralization capacity in order to improve lubricating oil and peace and quiet divergent function and a kind of additive grown up.
Salicylate is the important lubricant oil metal detergent of a class, in recent years, the magnesium salts purification agent that base number is high, ash content is low, acid neutralization capacity is strong obtains and develops fast, with the composite use of various calcium salt, there is good synergy, therefore, in actual application, both are normal adopts composite form to use.Salicylate is compared with other metal detergents (sulfonate, alkyl phenate), has excellent acid neutralization capacity, high temperature detergency, anti-oxidative stability and hydrolysis stability; Sulfonate raw material is easy to get, and is to use maximum class purification agents at present, and adopt composite form to use although salicylate and sulfonate are normal in actual application, different purification agent there will be coprecipitation phenomena in harmonic process.
Summary of the invention
in order to overcome the above problems, the invention provides a kind of synthetic method of calcium salicylate magnesium complex detergents.
A synthetic method for calcium salicylate magnesium complex detergents, said method comprising the steps of:
(1) alkyl salicylate, solvent xylene are added in the there-necked flask with agitator, reflux condensing tube, water trap and thermometer, calcium oxide, methyl alcohol, secondary accelerator urea is added under whipped state, treat that temperature is increased to 68 ~ 78 DEG C, carry out normal salt building-up reactions 1 hour;
(2) after positive reactant salt terminates, reduce temperature to 60 DEG C, add magnesium oxide and mix 20min, when temperature of reaction is down to 40 DEG C, add water, ammoniacal liquor and secondary accelerator volatile salt, wherein water and ammoniacal liquor evenly add in 20min, are that the speed of 120mLmin-1 passes into carbonic acid gas with speed simultaneously, carry out carbonation reaction 3 hours, in carbonation, temperature of reaction remains on 40 ~ 50 DEG C;
(3) carbonation reaction terminates rear intensification methanol removal, water and secondary accelerator etc., and treat that temperature is down to room temperature, adding dimethylbenzene dilutes and carry out centrifugal slagging-off, and the solution after slagging-off, by distilling the solvent xylene sloughed wherein, can obtain purification agent product.
Further, the components by weight percent adding each reactant in step (1) is alkyl salicylate 60-85 part, calcium oxide 3-10 part, dimethylbenzene 180-200 part, methyl alcohol 15-25 part.
Further, the magnesium oxide 1-25 part added in step (1), distilled water 10-15 part, ammoniacal liquor 5-10 part.
Further, the components by weight percent of the secondary accelerator urea added in step (1) is 2-10 part.
Further, the components by weight percent of the secondary accelerator volatile salt added in step (2) is 2-10 part.
The beneficial effect that the present invention reaches is:
(1) by calcium salicylate magnesium complex detergents that above method is obtained, there is excellent thermotolerance, high temperature detergency, good acid neutralization capacity, antioxygen corrosion resistance, extreme pressure anti-wear, and have certain low temperature dispersity concurrently, having good synergy with other additives, is the comprehensive lubricating oil additive of a kind of performance.The calcium salicylate magnesium complex detergents base number obtained by described method is greater than 400 mgKOHg-1, adds the use properties that lubricating oil can well improve lubricating oil.
(2) the best synthetic technological condition obtained has repeatability well, the result of the performance test of purification agent illustrates that product improves obviously to the thermal oxidation stability of lubricating oil and high temperature detergency, improve to the dispersiveness of lubricating oil and resistance to abrasion, the stability of product is fine.
Embodiment
Embodiment 1
A synthetic method for calcium salicylate magnesium complex detergents, said method comprising the steps of:
(1) alkyl salicylate 60 parts, solvent xylene 180 parts are added in the there-necked flask with agitator, reflux condensing tube, water trap and thermometer, 3 parts, calcium oxide, methyl alcohol 15 parts, 2 parts, secondary accelerator urea is added under whipped state, treat that temperature is increased to 68 ~ 78 DEG C, carry out normal salt building-up reactions 1 hour;
(2) after positive reactant salt terminates, reduce temperature to 60 DEG C, add magnesium oxide 1-25 part and mix 20min, when temperature of reaction is down to 40 DEG C, add distilled water 10 parts, ammoniacal liquor 5 parts and secondary accelerator volatile salt 2 parts, wherein water and ammoniacal liquor evenly add in 20min, are that the speed of 120mLmin-1 passes into carbonic acid gas with speed simultaneously, carry out carbonation reaction 3 hours, in carbonation, temperature of reaction remains on 40 ~ 50 DEG C;
(3) carbonation reaction terminates rear intensification methanol removal, water and secondary accelerator etc., and treat that temperature is down to room temperature, adding dimethylbenzene dilutes and carry out centrifugal slagging-off, and the solution after slagging-off, by distilling the solvent xylene sloughed wherein, can obtain purification agent product.
Embodiment 2
A synthetic method for calcium salicylate magnesium complex detergents, said method comprising the steps of:
(1) alkyl salicylate 85 parts, solvent xylene 200 parts are added in the there-necked flask with agitator, reflux condensing tube, water trap and thermometer, 10 parts, calcium oxide, methyl alcohol 25 parts, 10 parts, secondary accelerator urea is added under whipped state, treat that temperature is increased to 68 ~ 78 DEG C, carry out normal salt building-up reactions 1 hour;
(2) after positive reactant salt terminates, reduce temperature to 60 DEG C, add magnesium oxide 1-25 part and mix 20min, when temperature of reaction is down to 40 DEG C, add distilled water 15 parts, ammoniacal liquor 10 parts and secondary accelerator volatile salt 10 parts, wherein water and ammoniacal liquor evenly add in 20min, are that the speed of 120mLmin-1 passes into carbonic acid gas with speed simultaneously, carry out carbonation reaction 3 hours, in carbonation, temperature of reaction remains on 40 ~ 50 DEG C;
(3) carbonation reaction terminates rear intensification methanol removal, water and secondary accelerator etc., and treat that temperature is down to room temperature, adding dimethylbenzene dilutes and carry out centrifugal slagging-off, and the solution after slagging-off, by distilling the solvent xylene sloughed wherein, can obtain purification agent product.
Embodiment 3
A synthetic method for calcium salicylate magnesium complex detergents, said method comprising the steps of:
(1) alkyl salicylate 75 parts, solvent xylene 190 parts are added in the there-necked flask with agitator, reflux condensing tube, water trap and thermometer, 8 parts, calcium oxide, methyl alcohol 20 parts, 8 parts, secondary accelerator urea is added under whipped state, treat that temperature is increased to 68 ~ 78 DEG C, carry out normal salt building-up reactions 1 hour;
(2) after positive reactant salt terminates, reduce temperature to 60 DEG C, add magnesium oxide 1-25 part and mix 20min, when temperature of reaction is down to 40 DEG C, add distilled water 12 parts, ammoniacal liquor 8 parts and secondary accelerator volatile salt 2-10 part, wherein water and ammoniacal liquor evenly add in 20min, are that the speed of 120mLmin-1 passes into carbonic acid gas with speed simultaneously, carry out carbonation reaction 3 hours, in carbonation, temperature of reaction remains on 40 ~ 50 DEG C;
(3) carbonation reaction terminates rear intensification methanol removal, water and secondary accelerator etc., and treat that temperature is down to room temperature, adding dimethylbenzene dilutes and carry out centrifugal slagging-off, and the solution after slagging-off, by distilling the solvent xylene sloughed wherein, can obtain purification agent product.
Claims (5)
1. a synthetic method for calcium salicylate magnesium complex detergents, is characterized in that, said method comprising the steps of:
Alkyl salicylate, solvent xylene are added in the there-necked flask with agitator, reflux condensing tube, water trap and thermometer, calcium oxide, methyl alcohol, secondary accelerator urea is added under whipped state, treat that temperature is increased to 68 ~ 78 DEG C, carry out normal salt building-up reactions 1 hour;
After positive reactant salt terminates, reduce temperature to 60 DEG C, add magnesium oxide and mix 20min, when temperature of reaction is down to 40 DEG C, add water, ammoniacal liquor and secondary accelerator volatile salt, wherein water and ammoniacal liquor evenly add in 20min, are that the speed of 120mLmin-1 passes into carbonic acid gas with speed simultaneously, carry out carbonation reaction 3 hours, in carbonation, temperature of reaction remains on 40 ~ 50 DEG C;
Carbonation reaction terminates rear intensification methanol removal, water and secondary accelerator etc., and treat that temperature is down to room temperature, adding dimethylbenzene dilutes and carry out centrifugal slagging-off, and the solution after slagging-off, by distilling the solvent xylene sloughed wherein, can obtain purification agent product.
2. the synthetic method of calcium salicylate magnesium complex detergents according to claim 1, it is characterized in that, the components by weight percent adding each reactant in step (1) is alkyl salicylate 60-85 part, calcium oxide 3-10 part, dimethylbenzene 180-200 part, methyl alcohol 15-25 part.
3. the synthetic method of calcium salicylate magnesium complex detergents according to claim 1, is characterized in that, the magnesium oxide 1-25 part added in step (1), distilled water 10-15 part, ammoniacal liquor 5-10 part.
4. the synthetic method of calcium salicylate magnesium complex detergents according to claim 1, is characterized in that, the components by weight percent of the secondary accelerator urea added in step (1) is 2-10 part.
5. the synthetic method of calcium salicylate magnesium complex detergents according to claim 1, is characterized in that, the components by weight percent of the secondary accelerator volatile salt added in step (2) is 2-10 part.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201410755481.7A CN104496786A (en) | 2014-12-11 | 2014-12-11 | Synthesis method of calcium-magnesium salicylate composite detergent |
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| CN201410755481.7A CN104496786A (en) | 2014-12-11 | 2014-12-11 | Synthesis method of calcium-magnesium salicylate composite detergent |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2017071776A (en) * | 2015-10-08 | 2017-04-13 | インフィニューム インターナショナル リミテッド | Lubricating oil composition |
| CN107118824A (en) * | 2017-05-05 | 2017-09-01 | 西安石油大学 | A kind of mixed-matrix lubricating oil magnesium salts detersive and preparation method thereof |
| CN107201260A (en) * | 2017-05-14 | 2017-09-26 | 谢新昇 | A kind of preparation method of detergent for lubricating oil |
| CN107987920A (en) * | 2016-10-26 | 2018-05-04 | 中国石油化工股份有限公司 | A kind of method of lubricant oil composite and raising lubricating oil detergency |
| CN107987926A (en) * | 2016-10-26 | 2018-05-04 | 中国石油化工股份有限公司 | Lubricant composition for internal combustion engines and the method for improving IC engine lubricating oil detergency |
| CN107987918A (en) * | 2016-10-26 | 2018-05-04 | 中国石油化工股份有限公司 | Lubricant composition for internal combustion engines and the method for improving IC engine lubricating oil detergency |
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| CN104098466A (en) * | 2013-04-03 | 2014-10-15 | 中国石油天然气股份有限公司 | Preparation method of alkyl salicylate |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2017071776A (en) * | 2015-10-08 | 2017-04-13 | インフィニューム インターナショナル リミテッド | Lubricating oil composition |
| CN106566596A (en) * | 2015-10-08 | 2017-04-19 | 英菲诺姆国际有限公司 | Lubricating oil composition |
| CN106566596B (en) * | 2015-10-08 | 2021-04-09 | 英菲诺姆国际有限公司 | Lubricating oil composition |
| CN107987920A (en) * | 2016-10-26 | 2018-05-04 | 中国石油化工股份有限公司 | A kind of method of lubricant oil composite and raising lubricating oil detergency |
| CN107987926A (en) * | 2016-10-26 | 2018-05-04 | 中国石油化工股份有限公司 | Lubricant composition for internal combustion engines and the method for improving IC engine lubricating oil detergency |
| CN107987918A (en) * | 2016-10-26 | 2018-05-04 | 中国石油化工股份有限公司 | Lubricant composition for internal combustion engines and the method for improving IC engine lubricating oil detergency |
| CN107987926B (en) * | 2016-10-26 | 2022-04-12 | 中国石油化工股份有限公司 | Internal combustion engine lubricating oil composition and method for improving detergency of internal combustion engine lubricating oil |
| CN107987920B (en) * | 2016-10-26 | 2022-04-12 | 中国石油化工股份有限公司 | Lubricating oil composition and method for improving detergency of lubricating oil |
| CN107987918B (en) * | 2016-10-26 | 2022-09-23 | 中国石油化工股份有限公司 | Internal combustion engine lubricating oil composition and method for improving detergency of internal combustion engine lubricating oil |
| CN107118824A (en) * | 2017-05-05 | 2017-09-01 | 西安石油大学 | A kind of mixed-matrix lubricating oil magnesium salts detersive and preparation method thereof |
| CN107201260A (en) * | 2017-05-14 | 2017-09-26 | 谢新昇 | A kind of preparation method of detergent for lubricating oil |
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Application publication date: 20150408 |