CN1216027C - Preparation method of ultrahigh-alkalinity calcium naphthenate - Google Patents
Preparation method of ultrahigh-alkalinity calcium naphthenate Download PDFInfo
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- CN1216027C CN1216027C CN 02123780 CN02123780A CN1216027C CN 1216027 C CN1216027 C CN 1216027C CN 02123780 CN02123780 CN 02123780 CN 02123780 A CN02123780 A CN 02123780A CN 1216027 C CN1216027 C CN 1216027C
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- calcium
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- NKFIBMOQAPEKNZ-UHFFFAOYSA-N 5-amino-1h-indole-2-carboxylic acid Chemical compound NC1=CC=C2NC(C(O)=O)=CC2=C1 NKFIBMOQAPEKNZ-UHFFFAOYSA-N 0.000 title claims abstract description 11
- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 49
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims abstract description 30
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 21
- HNNQYHFROJDYHQ-UHFFFAOYSA-N 3-(4-ethylcyclohexyl)propanoic acid 3-(3-ethylcyclopentyl)propanoic acid Chemical compound CCC1CCC(CCC(O)=O)C1.CCC1CCC(CCC(O)=O)CC1 HNNQYHFROJDYHQ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000000920 calcium hydroxide Substances 0.000 claims abstract description 10
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims abstract description 10
- 239000002904 solvent Substances 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims abstract description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 18
- 238000006386 neutralization reaction Methods 0.000 claims description 13
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical class CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 10
- 238000004821 distillation Methods 0.000 claims description 10
- 230000003311 flocculating effect Effects 0.000 claims description 9
- 238000010792 warming Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 8
- 238000011085 pressure filtration Methods 0.000 claims description 7
- 239000008096 xylene Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 claims description 4
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 claims description 4
- 239000001569 carbon dioxide Substances 0.000 claims description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 claims description 2
- 239000002893 slag Substances 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims 1
- 229910052799 carbon Inorganic materials 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 2
- 235000011116 calcium hydroxide Nutrition 0.000 description 26
- 235000011089 carbon dioxide Nutrition 0.000 description 21
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 12
- 239000000047 product Substances 0.000 description 12
- 239000002253 acid Substances 0.000 description 11
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 7
- 229910052791 calcium Inorganic materials 0.000 description 7
- 239000011575 calcium Substances 0.000 description 7
- 229910000019 calcium carbonate Inorganic materials 0.000 description 6
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical class OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 description 5
- 238000009833 condensation Methods 0.000 description 5
- 230000005494 condensation Effects 0.000 description 5
- 239000000706 filtrate Substances 0.000 description 5
- 238000010025 steaming Methods 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 4
- 239000010687 lubricating oil Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- -1 for example Substances 0.000 description 2
- 238000012356 Product development Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000010727 cylinder oil Substances 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000010688 mineral lubricating oil Substances 0.000 description 1
- 125000005609 naphthenate group Chemical group 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a preparation method of ultrahigh alkaline calcium naphthenate, said method uses naphthenic acid and calcium hydroxide as raw material, and under the existance of methyl alcohol and auxiliary accelerator, the ultrahigh alkaline calcium naphthenate whose base value is greater than 400mgKOH/g is synthesized, and the end point of carbonation reaction is controlled by pH value of reaction liquor, after the reaction is completed, the filter aid is added, and the filter aid is pressurized, filtered and deslagged, and the solvent is evaporated so as to obtain the required product. The ultrahigh-base-number calcium naphthenate synthesized by the method has the advantages of high base number, low turbidity, stable performance and the like.
Description
Technical field
The present invention relates to a kind of peace and quiet dispersing additive that is used for internal combustion (IC) engine lubricating oil and preparation method thereof, belong to the lubricating oil field, specifically, is process for preparing ultrahigh basicity calcium naphthenate.
Background technology
Highly basic calcium naphthenate has detergent-dispersant performance preferably, and good acid neutralization capacity has excellent diffustivity, thereby is mainly used in the production marine cylinder oil.1991 the 4th phases of " refining of petroleum " magazine have reported that base number is the calcium naphthenate product development method of 250mgKOH/g, use methyl alcohol as promotor, the calcium naphthenate product of preparation base number 250mgKOH/g.
Summary of the invention
The objective of the invention is to provide a kind of naphthenate with superhigh base number calcium preparation method, a kind of peace and quiet dispersing additive of excellent property is provided for lubricating oil, under the identical condition of lubricating oil base number, can reduce the dosage of the quiet dispersion agent of metal, have favorable economic benefit and social benefit.
The method for preparing ultrahigh basicity calcium naphthenate of the present invention is as follows:
Naphthenic acid, solvent and the calcium hydroxide of metering are mixed stirring and is warming up to 40 ℃ in container; Drop into water, keep temperature of reaction between 50～65 ℃, neutralization reaction 1 hour; Drop into methyl alcohol and accelerant A, neutralization reaction 1～2 hour; Divide and drop into the calcium hydroxide of residual content 2～4 times, the back that stirs feeds carbon dioxide, carries out carbonation reaction, keeps the carbonation reaction temperature at 50～60 ℃, is 8～11 up to the pH of reaction solution value, stops carbonation reaction; Be warming up to more than 120 ℃, promotor and water are removed in distillation; Add flocculating aids, remove solid slag through pressure filtration; Underpressure distillation removes to desolvate and obtains product.
Said neutralization reaction of the present invention and carbonation reaction, the proportion scale of each component is: in 100 parts of naphthenic acid, calcium hydroxide is 40～70 parts, methyl alcohol is 10～50 parts, accelerant A is 5～20 parts, and water is 0.5～10 part, and solvent is 50～200 parts, flocculating aids is 3～50 parts, and carbonic acid gas ventilation speed is 30mL/min.
The mixture that the said reaction raw materials naphthenic acid of the present invention is naphthenic acid, mineral lubricating oils etc., naphthenic acid content is preferably between 30～50% (weights) between 20～70% (weights).
The acidic components of the said naphthenic acid of the present invention for from the fraction oil that crude distillation obtains, extracting, structural formula is:
Wherein, n=7～36, (CH2)
nIn also may comprise 1～4 five-ring or six-ring, R is the alkyl chain of C3～20;
The temperature of said neutralization reaction of the present invention and carbonation reaction is controlled at 30～70 ℃, is preferably between 50～65 ℃.
The said carbon dioxide feeding of the present invention speed is 10～200 milliliters/min of per 100 gram naphthenic acid per minutes, is preferably 30～50 milliliters/min.
The terminal point of the said carbonation reaction of the present invention is with the pH value control of reaction solution, and the general pH value is controlled between 8～12, is preferably 9～11.
The said accelerant A of the present invention is C
4-8Low mass molecule alcohol or its mixture, for example, the mixture of butanols, amylalcohol, hexanol, enanthol and octanol, add-on is 5～20 parts, is preferably 8～15 parts.
The said solvent of the present invention can be hydro carbons or aromatic hydrocarbon solvent, for example, gasoline, dimethylbenzene, add-on is 50～300 parts, is preferably 70～200 parts.
The said flocculating aids of the present invention can be diatomite or light calcium carbonate, and add-on is 3～50 parts, is preferably 8～15 parts.
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 parts in neutralization reaction, drops into the calcium hydroxide of residual content in carbonation reaction.
Embodiment
The following examples will be made further supplementary notes to the present invention.
The analytical procedure of every index in the embodiment of the invention:
1, total basicnumber analytical procedure: SH/T0251.
2, viscosity analytical procedure: GB/T265.
3, calcium contents analytical procedure: SH/T0297
Embodiment 1:
In having 2000 milliliters of there-necked flasks of electronic stirring, condensation water trap, drop into 300 gram naphthenic acid (pure acid number 115.8mgKOH/g, acid content 45%) and 300 the gram dimethylbenzene, add 15.0 gram calcium hydroxides (purity 98.12%) and 6.0 gram water, holding temperature was carried out neutralization reaction 1 hour about 60 ℃; Add 45 gram methyl alcohol, 33.0 gram n-hexyl alcohols and 45.0 gram calcium hydroxides, feeding flow velocity is the carbonic acid gas of 100 ml/min, carries out carbonation reaction, to the pH value of reaction solution be 11.0; Stop carbonic acid gas, add 45.0 gram calcium hydroxides, feed carbonic acid gas, continue carbonation reaction, to the pH value of reaction solution be 11.0; Stop carbonic acid gas, add 40.0 gram calcium hydroxides, to the pH value of reaction solution be 10.0, stop carbonation reaction.Be warming up to 120 ℃ of steaming engaging benzenemethanols and water, add the light calcium carbonate flocculating aidss of 45 grams, pressure filtration, filtrate is removed removal xylene and butanols gets product through underpressure distillation.Product calcium contents 14.5%, base number 408.2mgKOH/g.
Embodiment 2:
In having 2000 milliliters of there-necked flasks of electronic stirring, condensation water trap, drop into 300 gram naphthenic acid (pure acid number 115.8mgKOH/g, acid content 45%) and 300 the gram dimethylbenzene, add 15.0 gram calcium hydroxides (purity 98.12%) and 6.0 gram water, holding temperature was carried out neutralization reaction 1 hour about 60 ℃; Add 33.0 gram butanols and 45.0 gram calcium hydroxides, feeding flow velocity is the carbonic acid gas of 100 ml/min, carries out carbonation reaction, to the pH value of reaction solution be 11.0; Stop carbonic acid gas, add 45.0 gram calcium hydroxides, feed carbonic acid gas, continue carbonation reaction, to the pH value of reaction solution be 11.0; Stop carbonic acid gas, add 40.0 gram calcium hydroxides, to the pH value of reaction solution be 10.0, stop carbonation reaction.Be warming up to 120 ℃ of steaming engaging benzenemethanols and water, add the light calcium carbonate flocculating aidss of 45 grams, pressure filtration, filtrate is removed removal xylene and butanols gets product through underpressure distillation.Product calcium contents 14.6%, base number 406.8mgKOH/g.
Embodiment 3:
In having 2000 milliliters of there-necked flasks of electronic stirring, condensation water trap, drop into 300 gram naphthenic acid (pure acid number 115.8mgKOH/g, acid content 45%) and 300 the gram dimethylbenzene, add 15.0 gram calcium hydroxides (purity 99%) and 6.0 gram water, holding temperature was carried out neutralization reaction 1 hour about 60 ℃; Add 33.0 industrial octanols of gram and 45.0 gram calcium hydroxides, feeding flow velocity is the carbonic acid gas of 100 ml/min, carries out carbonation reaction, to the pH value of reaction solution be 11.0; Stop carbonic acid gas, add 45.0 gram calcium hydroxides, feed carbonic acid gas, continue carbonation reaction, to the pH value of reaction solution be 11.0; Stop carbonic acid gas, add 40.0 gram calcium hydroxides, to the pH value of reaction solution be 10.0, stop carbonation reaction.Be warming up to 120 ℃ of steaming engaging benzenemethanols and water, add the light calcium carbonate flocculating aidss of 45 grams, pressure filtration, filtrate is removed removal xylene and butanols gets product through underpressure distillation.Product calcium contents 14.6%, base number 418.6mgKOH/g.
Embodiment 4:
In having 2000 milliliters of there-necked flasks of electronic stirring, condensation water trap, drop into 300 gram naphthenic acid (pure acid number 155.8mgKOH/g, acid content 45%) and 300 the gram dimethylbenzene, add 15.0 gram calcium hydroxides (purity 99%) and 6.0 gram water, holding temperature was carried out neutralization reaction 1 hour about 60 ℃; Add 33.0 gram butanols and 45.0 gram calcium hydroxides, feeding flow velocity is the carbonic acid gas of 100 ml/min, carries out carbonation reaction, to the pH value of reaction solution be 11.0; Stop carbonic acid gas, add 45.0 gram calcium hydroxides, feed carbonic acid gas, continue carbonation reaction, to the pH value of reaction solution be 11.0; Stop carbonic acid gas, add 40.0 gram calcium hydroxides, to the pH value of reaction solution be 10.0, stop carbonation reaction.Be warming up to 120 ℃ of steaming engaging benzenemethanols and water, add the light calcium carbonate flocculating aidss of 45 grams, pressure filtration, filtrate is removed removal xylene and butanols gets product through underpressure distillation.Product calcium contents 13.9%, base number 434.1mgKOH/g.
Embodiment 5:
In having 2000 milliliters of there-necked flasks of electronic stirring, condensation water trap, drop into 300 gram naphthenic acid (pure acid number 198.7mgKOH/g, acid content 45%) and 300 the gram dimethylbenzene, add 15.7 gram calcium hydroxides (purity 99%) and 6.0 gram water, holding temperature was carried out neutralization reaction 1 hour about 60 ℃; Add 33.0 gram butanols and 45.0 gram calcium hydroxides, feeding flow velocity is the carbonic acid gas of 100 ml/min, carries out carbonation reaction, to the pH value of reaction solution be 11.0; Stop carbonic acid gas, add 45.0 gram calcium hydroxides, feed carbonic acid gas, continue carbonation reaction, to the pH value of reaction solution be 11.0; Stop carbonic acid gas, add 40.0 gram calcium hydroxides, to the pH value of reaction solution be 10.0, stop carbonation reaction.Be warming up to 120 ℃ of steaming engaging benzenemethanols and water, add the light calcium carbonate flocculating aidss of 45 grams, pressure filtration, filtrate is removed removal xylene and butanols gets product through underpressure distillation.Product calcium contents 15.4%, base number 438mgKOH/g.
Claims (2)
1, a kind of product base number is characterized in that in above ultrahigh basicity calcium naphthenate product of 350mgKOH/g and preparation method:
(1) naphthenic acid, solvent xylene or gasoline and the calcium hydroxide with metering mixes stirring and is warming up to 30～60 ℃ in container;
(2) drop into water, keep temperature of reaction between 30～70 ℃, neutralization reaction 0.5～3 hour;
(3) drop into methyl alcohol and accelerant A then, accelerant A is that carbon number is 4～8 low mass molecule alcohol or their mixture, neutralization reaction 0.5～3 hour;
(4) branch drops into the calcium hydroxide of residual contentes 2～4 times, feeds carbon dioxide, carries out carbonation reaction, keeps the carbonation reaction temperature at 30～70 ℃, is 8～11 up to the pH of reaction solution value, stops carbonation reaction;
(5) be warming up to more than 120 ℃ distillation for removing methanol, water and part accelerant A; Add flocculating aids, remove solid slag through pressure filtration; Underpressure distillation removes to desolvate and remain accelerant A and obtains product; In 100 parts of naphthenic acid, calcium hydroxide is 40～70 parts; Accelerant A is 5～20 parts.
2, method according to claim 1 is characterized in that: described accelerant A is selected from butanols, amylalcohol, hexanol, enanthol, octanol, or their mixture.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02123780 CN1216027C (en) | 2002-06-28 | 2002-06-28 | Preparation method of ultrahigh-alkalinity calcium naphthenate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02123780 CN1216027C (en) | 2002-06-28 | 2002-06-28 | Preparation method of ultrahigh-alkalinity calcium naphthenate |
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| Publication Number | Publication Date |
|---|---|
| CN1465560A CN1465560A (en) | 2004-01-07 |
| CN1216027C true CN1216027C (en) | 2005-08-24 |
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| CN 02123780 Expired - Fee Related CN1216027C (en) | 2002-06-28 | 2002-06-28 | Preparation method of ultrahigh-alkalinity calcium naphthenate |
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Families Citing this family (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101885677B (en) * | 2009-05-14 | 2013-09-04 | 中国石油化工股份有限公司 | Preparation method for high-alkaline calcium naphthenate |
| 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 |
| CN102071085B (en) * | 2009-11-19 | 2013-01-30 | 中国石油化工股份有限公司 | High-base number metal detergent and preparation method thereof |
| CN103666647B (en) * | 2012-09-25 | 2015-07-01 | 中国石油化工股份有限公司 | High-base-number naphthenic acid composite calcium-magnesium detergent, preparation method thereof and lubricating oil composition |
| CN103666641B (en) * | 2012-09-25 | 2015-09-23 | 中国石油化工股份有限公司 | High base number sodium napthionate purification agent, its preparation method and lubricating oil composition |
| CN103666642B (en) * | 2012-09-25 | 2016-03-23 | 中国石油化工股份有限公司 | High base number naphthenic acid lithium, its preparation method and lubricating oil composition |
| CN104276945B (en) * | 2013-07-02 | 2016-01-13 | 中国科学院兰州化学物理研究所 | A kind of preparation method of boronation overbased calcium alkyl-salicylate |
| CN104293450B (en) * | 2013-07-17 | 2017-02-08 | 中国石油化工股份有限公司 | Composite calcium naphthenate-based tetra-polyurea lubricating grease and preparation method thereof |
| CN104449956B (en) * | 2013-09-13 | 2017-07-25 | 中国石油化工股份有限公司 | A kind of high base number composite calcium-base polyurea grease and preparation method thereof |
| CN104449961B (en) * | 2013-09-13 | 2017-07-25 | 中国石油化工股份有限公司 | A kind of sulfoacid calcium calcium naphthenate-based hexapolyurea lubricating grease and preparation method thereof |
| CN106977393B (en) * | 2017-05-27 | 2019-04-23 | 西安石油大学 | The technique of continuous production calcium naphthenate |
| CN111849587A (en) * | 2020-08-14 | 2020-10-30 | 德杰(浙江)润滑科技有限公司 | Preparation method and process of lubricating oil 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 |
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- 2002-06-28 CN CN 02123780 patent/CN1216027C/en not_active Expired - Fee Related
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