CN1147578C - Process for preparing compound metal type lubricating oil cleaning agent - Google Patents
Process for preparing compound metal type lubricating oil cleaning agentInfo
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- CN1147578C CN1147578C CNB021043922A CN02104392A CN1147578C CN 1147578 C CN1147578 C CN 1147578C CN B021043922 A CNB021043922 A CN B021043922A CN 02104392 A CN02104392 A CN 02104392A CN 1147578 C CN1147578 C CN 1147578C
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Abstract
The present invention relates to a composite metal type lubricating oil detergent with high alkalinity and a preparation method thereof. In the technological method, composite metal type detergents with high alkalinity are synthesized by introducing different kinds of metals, accelerants, activating accelerators, surfactants, etc. The method takes alkyl salicylate, etc. as raw materials, and the composite metal type detergents with high alkalinity (as high as 350 mg KOH/g) are synthesized according to certain proportional mixture ratio under the condition that methanol and an ammoniacal compound are used as accelerants. Besides the favorable property of purification at high temperature, the synthetic product of the present invention also has favorable colloid stability, definite resistance to oxidation and corrosion and good extreme-pressure wearing resistance, is especially suitable for hydrogenized base oil and is a kind of lubricating oil additive with superior performance.
Description
The present invention relates to a kind of preparation method of high basicity lube oil additive, the preparation method that the high basicity of especially a kind of compound metal type is peace and quiet dose belongs to the lubricating oil field.
Metal detergent plays an important role in modern communication as the host of internal combustion engine oil. Generally can be divided into barium salt, calcium salt, magnesium salt etc. by different metal types, wherein the purposes with calcium salt is the most general.
In recent years along with the pay attention to day by day to environmental protection; barium salt with certain toxicity progressively withdraws from historical stage; and the calcium salt product of environment-friendly type has worldwide obtained everybody approval, and the magnesium product salt without toxicity, low ash content, high base number has also obtained tremendous development simultaneously. According to latest report, at present both at home and abroad research institution the Devoting Major Efforts To Developing oxidation corrosion resistance can be good the good zinc salt of sodium salt, sylvite, mantoquita product and extreme pressure and antiwear behavior, molybdenum product salt, sulfuration, the modified product of boronation. No matter but the exploitation of which kind of metal product salt all concentrates on take alkylbenzene sulfonic acid as matrix, namely form the different metal salt of alkylbenzene sulfonic acid. Alkyl salicylate salt is with its good high temperature detergent performance and deacidification, also has that certain low temperature disperses simultaneously, anti-oxidant anticorrosive a, extreme pressure and antiwear behavior and have the good characteristics such as synergism with other agent, and extremely people pay attention to. The salicylic acid product salt only has calcium salt, magnesium salt both at home and abroad at present, wherein the alkali value mostly is the magnesium product salt greater than the additive of 300mgKOH/g, and this can not satisfy the superior requirement of oil product far away. Along with the fast development of high-grade internal combustion engine oil, in the oil product peace and quiet dose of the different metal type compound, be widely used, developing of peace and quiet dose of the compound metal type that forms but different metal is compound in initial reaction stage then seldom is seen in report. Developing of peace and quiet dose of compound metal type, can successfully solve the various problems that peace and quiet dose of compound tense of different metal salt occurs, the ratio that makes different metal is controlled and can arbitrarily regulate in initial reaction stage, thereby satisfies the needs of lubricating oil and fuel oil development.
The objective of the invention is to provide a kind of take alkyl salicylate as main, under the condition of introducing kicker and surfactant, prepare peace and quiet dose of the high basicity of compound metal type by certain metallization process, this product not only contains a certain amount of alkyl salicylate salt (calcium, magnesium, sodium etc.), alkylbenzene sulfonic acid salt, but also contain a small amount of alkyl phenates, thereby except the every performance with traditional high basicity alkyl salicylate salt, also give its some unique characteristic, thereby can be the new additive agent that contains different metal that lubricating oil provides a kind of stability, favorable dispersibility.
The preparation method that the high basicity of a kind of compound metal type of the present invention is peace and quiet dose, namely introduce surfactant and carry out the different metal metallization processes as follows: the dilution solvent (gasoline, dimethylbenzene, cyclohexane etc.), specific surfactant and the promoter methyl alcohol (industrial goods) that in there-necked flask, drop into metering, be warming up to 30-60 ℃, drop into industrial magnesium oxide (purity is more than 93%) or magnesia and the calcium oxide mixture of metering, the water and the ammoniacal liquor that add simultaneously metering, behind about 30 minutes of the stirring reaction, the alkyl salicylate that adds metering, stirring reaction, keep reaction temperature 40-60 ℃, reaction 1 hour neutralizes. Thereafter look final product during the second step metallization reaction and form different calcium oxide or NaOH or the two mixture that add metering, under 40-60 ℃, keep reaction 30 minutes, then lead to into a certain amount of carbon dioxide, carry out high basicity and reacted about 2 hours. Reaction is warming up to 110 ℃ after finishing, and steaming engaging benzenemethanol and water dilute centrifugal rear decompression steaming and takes off solvent, get product. Promoter is used methyl alcohol, and kicker uses ammonia and ammonium salt, and surfactant is alkylbenzene sulfonic acid or aphthenic acids, and the batching of each component is than certain ratio is arranged. In 90 parts of (weight) alkyl salicylates (oil-containing 40%), surfactant is 1-10 part, magnesia is 1-20 part, and calcium oxide is 1-15 part, NaOH 1-10 part, methyl alcohol is 30-150 part, water is 5.0-80.0 part, and the Ammonia kicker is 1.0-20.0 part, and solvent is 40-200 part, carbon dioxide is 20-100 part, and reaction temperature is controlled between 40-60 ℃.
The present invention is when peace and quiet dose of preparation calcium, magnesium bimetallic, and the second step metallization reaction adds calcium oxide separately; Preparation contains peace and quiet dose of metal sodium namely during three metal detergents, one or both metallic compounds that add when reacting with the first step are corresponding, the second step metallization reaction adds remaining two kinds or a kind of metallic compound, be that NaOH adds with calcium oxide or NaOH adds separately, contain peace and quiet dose of the compound metal type of three kinds of metals with formation.
This reaction system can be fit to calcium oxide, the magnesia of different stage, surfactant is two alkyl or monoalkyl benzene sulfonic acid, aphthenic acids, reaction can be that boiling range is 60-160 ℃ direct steaming gasoline with solvent, also can be that boiling point is higher than 120 ℃ material, such as dimethylbenzene. The structure of reacting used primary raw material alkyl salicylate is:
Wherein R is C8-30The alkyl chain.
Methyl alcohol must be purity greater than 95% chemical reagent or industrial goods, and kicker can be the Ammonia products such as ammoniacal liquor, ammonium carbonate or carbonic hydroammonium, preferably selects ammoniacal liquor. Surfactant, methyl alcohol, the water yield and kicker are the principal elements that affects product alkali value and viscosity. Suitable dosage of surfactant is 5.0-10.0 gram/90 gram alkyl salicylates, and methanol usage is 30-60 gram/90 gram alkyl salicylates; The consumption of suitable water is 30.0-60.0 gram/90.0 gram alkyl salicylates. Synthetic product has excellent anti-oxidant anticorrosive, heat endurance and detergent-dispersant performance energy.
In the synthetic reaction process of peace and quiet dose of product of the high basicity of compound metal type of the present invention:
The effect of methyl alcohol: methyl alcohol is as inorganic phase and organic carrier mutually, can make in the reactant mixture the ternary and oily solution of gas, liquid, solid and aqueous solution two-phase evenly mixed, simultaneously, methyl alcohol has the surface energy that reduces the alkaline-earth metal oxide thing, wetting surface promotes the slaking reaction to carry out slowly and steadily. At last, methyl alcohol also can promote the formation of colloid particle as carrier.
The effect of water in reaction: water is a kind of reaction reagent, slaking reaction needs just can carry out having under the condition of water, and only under the condition that guarantees the water yield, hydroxide magnesium, the calcium hydroxide of generation are evenly disperseed, original position generates the less carbonate lattice of particle diameter, and participating in into the glue reaction, synthetic product viscosity is also less like this.
The effect of kicker: the introducing of kicker, can improve the reactivity of methyl alcohol, impel the hydroxide of generation evenly to disperse, original position generates the less carbonate lattice of particle diameter, guarantees that course of reaction is steady, and participates in into the glue reaction.
The effect of surfactant: the present invention makes reaction medium that great variety occur owing to having introduced surfactant alkylbenzene sulfonic acid, alkylbenzene sulfonic acid is as a kind of reaction reagent, it can stop the carbonate particle of generation and alkyl salicylate salt micella to assemble growth, and impel it to generate rapidly load glue group and be scattered in the oily solution stablely, simultaneously, alkylbenzene sulfonic acid can generate the less mixing micella that is more evenly distributed of particle diameter with alkyl salicylate, and participates in into the glue reaction.
The investigation result of Surfactant and kicker is as follows:
Table one, surfactant and kicker are on the impact of reaction
| Surfactant adding amount g | Alkyl salicylate g | Kicker g | TBN mgKOH/g | Remarks | |
| 1 | 0.0 | 100.0 | 0.0 | / | Jelly |
| 2 | 0.0 | 100.0 | 15.0 | 349 | |
| 3 | 5.0 | 95.0 | 15.0 | 340 | |
| 4 | 10.0 | 90.0 | 15.0 | 370 | |
| 5 | 15.0 | 85.0 | 15.0 | 391 | |
| 6 | 20.0 | 80.0 | 15.0 | / | Jelly during dehydration |
From table one result as can be known, the adding amount of surfactant and kicker has important impact to the alkali value of product.
In the experiment heat endurance of compound high basicity metal detergent, anti-oxidant property, high temperature detergency etc. are evaluated, be the results are shown in Table two.
The assessment of performance result of table two, the high basicity product of compound metal type
| Project | 1407-003 | 1407-027 | High basicity magnesium salt | Overbased calcium salt | Test method |
| Surfactant g | 10.0 | 10.0 | 10.0 | / | |
| Alkali value mgKOh/g | 380 | 352 | 429 | 361 | SH/T0251 |
| Ca％ | 5.08 | 6.01 | / | 12.54 | SH/T0297 |
| Mg％ | 5.09 | 4.12 | 9.95 | / | SH/T0027 |
| Na％ | / | 0.88 | / | / | |
| The heat pipe oxidation (320 ℃ * 4h) level | 2.0 | 2.0 | 3.0 | 4.5 | SH/T0645 |
| (320 ℃ * 3h) mg of coking amounts | 160.6 | 188.0 | 177.0 | 122.7 | SH018。0235 |
| Oxidation stability TFOUT min | 167 | 105 | / | 98 | SH/T0193 |
| (100 ℃ * 4d) v% of colloid-stabilised property | 0.00 | 0.00 | 0.00 | 0.00 | Q/ZLJS3005 |
| Pb N | 509.6 | 509.6 | 441.0 | 558.0 | GB3142-82 |
| Wear scar diameter (196N * 60min) | 0.27 | 0.32 | 0.30 | 0.24 | Q/SH018.0114- 89 |
Annotate: call in 2.0% dosage and carry out assessment of performance among the 98.0%HVIM H500.
The result shows, peace and quiet dose of the high basicity of compound metal type has preferably Practical Performance.
Peace and quiet dose of the high basicity of compound metal type of the inventive method preparation, under identical alkali value requires, can reduce the adding amount of additive in oil product, particularly suitable is in hydrogenated base oil, because the comprehensive performance such as its good high temperature detergency, anti-oxidant property and heat endurance, can be common in gasoline machine oil and the diesel engine oil, will produce preferably social benefit and economic benefit. In addition, this agent and other additive compound use can guarantee that engine oil has multiple performance, with ability significance are arranged to improving in the lubricated oleic acid.
The following examples are to further explanation of the present invention, rather than limit the invention, and spirit of the present invention and protection domain are listed as in the claim book.
Embodiment 1: add 150 milliliters in gasoline, 60 milliliters of methyl alcohol (analyzing pure) in 500 milliliters of there-necked flasks with electric mixer and condensation dehydration device, alkylbenzene sulfonic acid 10.0 grams, stir, be warming up to 30-50 ℃, drop into 15.0 gram industrial magnesium oxides (production of chemical plant, Dunhuang, Shanghai), 45.0 gram water, 15.0 gram ammoniacal liquor stirs, at this moment visible mixture retrogradation, and be attended by the temperature rise phenomenon, after about 30 minutes, add 90.0 gram alkyl salicylates, stir, the control reaction temperature is 45-60 ℃, reacts 1 hour, and reaction neutralizes. After reaction is finished, add 10.0 gram calcium oxide again, carry out the second metallization reaction under 45-60 ℃, lead to into carbon dioxide after 30 minutes, ventilation speed is the 200-300 ml/min, and keeping reaction temperature is 45-60 ℃, carries out high basicity and reacts about 2 hours. After reaction finishes, be warming up to 110 ℃, steaming engaging benzenemethanol and water add gasoline dilution, cooling, centrifugally go behind the slag decompression to steam to take off solvent to get product. The product calcium content is 5.08%, magnesium content 5.09%, and the alkali value is 380mgKOH/g, kinematic viscosity (100 ℃) is 203.51mm2/s。
Embodiment 2: add 150 milliliters in gasoline, 60 milliliters of methyl alcohol (analyzing pure) in 500 milliliters of there-necked flasks with electric mixer and condensation dehydration device, alkylbenzene sulfonic acid 10.0 grams, stir, be warming up to 30-50 ℃, drop into 10.0 gram industrial magnesium oxides (production of chemical plant, Dunhuang, Shanghai), 10.0 gram calcium oxide, 45.0 gram water, at this moment visible mixture retrogradation, and be attended by the temperature rise phenomenon, after about 30 minutes, add 90.0 gram alkyl salicylates, the control reaction temperature is 45-60 ℃, reacts 1 hour, and reaction neutralizes. After reaction is finished, add 5.0 gram NaOH again, carry out the second metallization reaction under 45-60 ℃, lead to into carbon dioxide after 30 minutes, ventilation speed is the 200-300 ml/min, and keeping reaction temperature is 45-60 ℃, carries out high basicity and reacts about 2 hours. After reaction finishes, be warming up to 110 ℃, steaming engaging benzenemethanol and water add gasoline dilution, cooling, centrifugally go behind the slag decompression to steam to take off solvent to get product. The product calcium content is 5.25%, magnesium content 3.56%, and sodium content 2.58%, the alkali value is 402mgKOH/g, kinematic viscosity (100 ℃) is 100.1mm2/s。
Embodiment 3: add 150 milliliters in gasoline, 45 milliliters of methyl alcohol (analyzing pure) in 500 milliliters of there-necked flasks with electric mixer and condensation dehydration device, alkylbenzene sulfonic acid 10.0 grams, stir, be warming up to 30-50 ℃, drop into 15.0 gram industrial magnesium oxides (production of chemical plant, Dunhuang, Shanghai), 5.0 gram calcium oxide, 35.0 gram water, 20.0 gram ammoniacal liquor stirs, at this moment visible mixture retrogradation, and be attended by the temperature rise phenomenon, after about 30 minutes, add 90.0 gram alkyl salicylates, stir, the control reaction temperature is 45-60 ℃, reacts 1 hour, and reaction neutralizes. After reaction is finished, add 5.0 gram calcium oxide again, carry out the second metallization reaction under 45-60 ℃, lead to into carbon dioxide after 30 minutes, ventilation speed is the 200-300 ml/min, and keeping reaction temperature is 45-60 ℃, carries out high basicity and reacts about 2 hours. After reaction finishes, be warming up to 110 ℃, steaming engaging benzenemethanol and water add gasoline dilution, cooling, centrifugally go behind the slag decompression to steam to take off solvent to get product. The product calcium content is 3.60%, magnesium content 5.05%, and the alkali value is 370mgKOH/g.
Embodiment 4: add 150 milliliters in gasoline, 60 milliliters of methyl alcohol (analyzing pure) in 500 milliliters of there-necked flasks with electric mixer and condensation dehydration device, alkylbenzene sulfonic acid 10.0 grams, stir, be warming up to 30-50 ℃, drop into 10.0 gram industrial magnesium oxides (production of chemical plant, Dunhuang, Shanghai), 45.0 gram water, at this moment visible mixture retrogradation, and be attended by the temperature rise phenomenon, after about 30 minutes, add 90.0 gram alkyl salicylates, the control reaction temperature is 45-60 ℃, reacts 1 hour, and reaction neutralizes. After reaction is finished, add again 10.0 gram calcium oxide, 2.0 gram NaOH, under 45-60 ℃, carry out the second metallization reaction, lead to into carbon dioxide after 30 minutes, ventilation speed is the 200-300 ml/min, and keeping reaction temperature is 45-60 ℃, carries out high basicity and reacts about 2 hours. After reaction finishes, be warming up to 110 ℃, steaming engaging benzenemethanol and water add gasoline dilution, cooling, centrifugally go behind the slag decompression to steam to take off solvent to get product. The product calcium content is 6.01%, magnesium content 4.17%, and sodium content 0.88%, the alkali value is 352mgKOH/g, kinematic viscosity (100 ℃) is 98.4mm2/s。
Claims (6)
1, the preparation method of peace and quiet dose of product of the high basicity of a kind of compound metal type, it is characterized in that: the dilution solvent that in reaction vessel, drops into metering, surfactant, promoter methyl alcohol, be warming up to 30-60 ℃, drop into industrial magnesium oxide or magnesia and the calcium oxide mixture of metering, the water and the ammoniacal liquor that add simultaneously metering, behind the stirring reaction 30 minutes, the alkyl salicylate that adds metering, stir, keep reaction temperature 40-60 ℃, reaction 1 hour neutralizes, look final product during thereafter second step metallization and form different calcium oxide or NaOH or the two mixture that add metering, under 40-60 ℃, keep reaction 30 minutes, then lead to into a certain amount of carbon dioxide, carry out high basicity reaction 2 hours, after reaction finishes, be warming up to 110 ℃, steaming engaging benzenemethanol and water, dilute centrifugal rear decompression steaming and take off solvent, get product, in 90 parts of alkyl salicylates of oil-containing 40%, surfactant is 1-10 part, and magnesia is 1-20 part, calcium oxide is 1-15 part, NaOH 1-10 part, methyl alcohol are 30-150 part, and water is 5.0-80.0 part, kicker is 1.0-20.0 part, solvent is 40-200 part, and carbon dioxide is 20-100 part, and above umber is the weight umber that each material accounts for whole material.
2, the preparation method of peace and quiet dose of product of the high basicity of compound metal type according to claim 1 is characterized in that: peace and quiet dose of preparation calcium, magnesium bimetallic, when the second step metallization reaction, calcium oxide adds separately.
3, the preparation method of peace and quiet dose of product of the high basicity of compound metal type according to claim 1, it is characterized in that: preparation contains metal sodium, calcium, magnesium peace and quiet dose, when the second step metallization reaction, one or both metallic compounds that add when reacting with the first step are corresponding, the second step reaction adds remaining two kinds or a kind of metallic compound, be that NaOH adds with calcium oxide or NaOH adds separately, contain peace and quiet dose of the compound metal type of three kinds of metals with formation.
4, the preparation method of peace and quiet dose of product of the high basicity of compound metal type according to claim 1 is characterized in that: kicker is ammoniacal liquor or ammonium carbonate or carbonic hydroammonium.
5, the preparation method of peace and quiet dose of product of the high basicity of compound metal type according to claim 1 is characterized in that: surfactant is alkylbenzene sulfonic acid or aphthenic acids, molecular weight 300-500.
6, the preparation method of peace and quiet dose of product of the high basicity of compound metal type according to claim 1 is characterized in that: reaction is that boiling range is 60-160 ℃ direct steaming gasoline or dimethylbenzene with solvent.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB021043922A CN1147578C (en) | 2002-03-07 | 2002-03-07 | Process for preparing compound metal type lubricating oil cleaning agent |
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| CNB021043922A CN1147578C (en) | 2002-03-07 | 2002-03-07 | Process for preparing compound metal type lubricating oil cleaning agent |
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| CN1147578C true CN1147578C (en) | 2004-04-28 |
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| CNB021043922A Expired - Fee Related CN1147578C (en) | 2002-03-07 | 2002-03-07 | Process for preparing compound metal type lubricating oil cleaning agent |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101195785B (en) * | 2006-12-07 | 2010-05-19 | 中国石油天然气股份有限公司 | Production method for alkyl sodium salicylate metallic detersive |
| CN101886013B (en) * | 2009-05-14 | 2013-01-30 | 中国石油化工股份有限公司 | Method for preparing mixed-matrix metal cleaner |
| CN104283280A (en) * | 2014-10-16 | 2015-01-14 | 昆山市圣光新能源科技有限公司 | Novel anti-skid two-cable automotive emergency ignition power source with charging and Bluetooth functions |
| CN106566596B (en) * | 2015-10-08 | 2021-04-09 | 英菲诺姆国际有限公司 | Lubricating oil composition |
| CN107201260A (en) * | 2017-05-14 | 2017-09-26 | 谢新昇 | A kind of preparation method of detergent for lubricating oil |
| CN107446661B (en) * | 2017-08-30 | 2020-07-03 | 黄山学院 | Metal magnesium salt lubricating oil detergent with high dispersing capacity and preparation method thereof |
| CN116515543B (en) * | 2023-04-12 | 2024-04-02 | 湖南鸿福实业有限公司 | High-dispersion stable lubricating oil metal detergent and preparation method thereof |
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2002
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