CN1403435A - Prepn process of magnesium naphthenate with superhigh base number - Google Patents
Prepn process of magnesium naphthenate with superhigh base number Download PDFInfo
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- CN1403435A CN1403435A CN 01130770 CN01130770A CN1403435A CN 1403435 A CN1403435 A CN 1403435A CN 01130770 CN01130770 CN 01130770 CN 01130770 A CN01130770 A CN 01130770A CN 1403435 A CN1403435 A CN 1403435A
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Abstract
The preparation process of magnesium naphthenate with superhigh base number includes the following steps: mixing naphthenic acid, solvent and magnesia in a reactor, heating to 25-60 deg.c for 0.5-4.0 hr; reaction at 40-60 deg.c for 2.0-4.0 hr while adding water, methyl and amine promoter; carbonating for 2.0-4.5 hr while introducing CO2 gas in certain amount; heating to 110 deg.c to eliminate alcohol and water; centrifugating or filtering while adding filter aid and depressing distillation to eliminate solvent. The present invention can provide excellent detergent for petroleum product and has simple preparation process and low production cost.
Description
The present invention relates to a kind of preparation method of magnesium naphthenate with superhigh base number, belong to super base number magnesium carboxylates, be used as the petroleum oil product purification agent.
In recent years, along with the fast development of engine oil, engine itself develops to little, the high-power direction of volume in addition, and is more and more harsher to the requirement of oil product high-temperature behavior.This just requires oil dope to have higher cleansing performance, antioxidant property, rustless property, and the corrosive acid in the comprehensive sulfurous fuels, and the high base number purification agent is the unique additive that can realize all these indispensable performances.U.S. Pat 4293429 " MgO dispersion system ", a kind of method stable, mobile dispersion MgO system for preparing is disclosed, in relatively stable, non-volatile process, be heated to above 230 ℃ MgO particle and be less than the carboxylic acid of this MgO proportioning number, formation is the above-mentioned MgO system of the decomposition of fixed point with the carboxylic acid, and described carboxylic acid mainly is meant acetic acid.Super its base number of base number magnesium carboxylates that adopts this method to prepare can reach 400KOH/g, and good fluidity, is the comparatively good petroleum oil product purification agent of a kind of performance.Existing problem is: because the particle size distribution of product is bigger, can only adopt centrifugation to separate; The high-temperature processing technology that must adopt temperature to be higher than 230 ℃ before separation is handled, so that its viscosity reduces.But high-temperature processing technology is difficult for realizing on device, has increased the complicacy of preparation and treatment process and the cost of product.
The preparation method who the purpose of this invention is to provide a kind of magnesium naphthenate with superhigh base number, this method have simple preparation and treatment process, can reduce production costs effectively when providing the purification agent of excellent property for petroleum oil product.
The objective of the invention is to realize by following technical solution.
A kind of preparation method of magnesium naphthenate with superhigh base number, at room temperature add naphthenic acid, solvent and the magnesium oxide of metering in the reactor, mix to stir and be warming up to 25 ℃-60 ℃, mixing process keeps 0.5h-4.0h, add entry and methyl alcohol, amine type accelerator then, 40 ℃-60 ℃ reactions 2.0-4.0 hour, then feed a certain amount of carbon dioxide, carried out carbonation reaction 2.0-4.5 hour, intensification dealcoholysis water to 110 ℃, centrifugal or adding flocculating aids filters, and underpressure distillation is sloughed solvent and obtained product.
Above-mentioned amine type accelerator is a purity greater than 65% trolamine, magnesium oxide is activated magnesia, the composition proportion scope of various component materials is: when the add-on of the naphthenic acid that contains sour 35-60% (weight) is 100 grams, add activated magnesia 18-30 gram, solvent 70-160 gram, water 8-25 gram, methyl alcohol 21-42 gram, trolamine 1.8-10 gram, carbonic acid gas 12-30 gram.Solvent can be that boiling range is 40 ℃-180 ℃ a straight-run spirit, also can be toluene or dimethylbenzene.The structural formula of naphthenic acid is:
Wherein: n=7-36, (CH
2)
nIn can comprise 1-4 five-ring or six-ring, R is C
3-20Alkyl chain.
The scope of quantity of methyl alcohol/(quantity of methyl alcohol+water yield) is between 45%-75% (weight), and the purity of methyl alcohol is greater than 98%.Flocculating aids is light calcium carbonate or diatomite, and when the add-on of the naphthenic acid that contains sour 35-60% (weight) was 100 grams, the add-on of flocculating aids was the 3-50 gram.
The magnesium naphthenate product of the present invention that adopts the inventive method to prepare, adopt SH/T0251 total basicnumber analytical standard to measure, its total basicnumber is 350-500mgKOH/g, and the ability of the corrosive acid in the extremely strong comprehensive sulfurous fuels is arranged, and has good cleansing performance, antioxidant property and rustless property.Compared with prior art, the reasonable distribution of the inventive method preparation adopts GB/T265 viscosity analytical standard to measure, and its 100 ℃ of kinematic viscosity are 80-300mm
2/ s can adopt filter type to separate; In the product preparation process, must not adopt high-temperature processing technology to handle, be easy on device realize that preparation and treatment process process are simple, reduce the cost of product.
Below in conjunction with embodiment the present invention is discussed in detail.
Embodiment 1
In having the there-necked flask that stirs and reflux, add the naphthenic acid 330g, magnesium oxide 78g, the straight-run spirit 450g of activity-60 that contain acid 45% (weight), mix to stir and be warming up to 50 ℃ of * 2h, add trolamine 25g, water 56g, methyl alcohol 80g, 50 ℃ of following aminations 2 hours, the carbonic acid gas that feeds 145ml/min carried out carbonation reaction 4 hours, was warming up to 110 ℃ and removed alcohol, water, add flocculating aids light calcium carbonate 50g, filtration, underpressure distillation obtain product of the present invention.The filtering rate of its product is 336Kg/m
2H, base number are 434.1mgKOH/g, and 100 ℃ of kinematic viscosity are 172.0mm
2/ s.
Embodiment 2
Amination in the example 1 was become 3.0 hours in 2.0 hours, and all the other are constant, and the filtering rate of the product of the present invention that obtains is 810Kg/m
2H, base number are 428.0mgKOH/g, and 100 ℃ of kinematic viscosity are 212.0mm
2/ s.
Embodiment 3
In having the there-necked flask that stirs and reflux, add the naphthenic acid 330g, magnesium oxide 78g, the straight-run spirit 450g of activity-40 that contain acid 45% (weight), mix to stir and be warming up to 50 ℃ of * 3h, add trolamine 25g, water 66g, methyl alcohol 88g, 50 ℃ of following aminations 3.0 hours, the carbonic acid gas that feeds 195ml/min carried out carbonation reaction 3.0 hours, was warming up to 110 ℃ and removed alcohol, water, add flocculating aids light calcium carbonate 50g, filtration, underpressure distillation obtain product of the present invention.The filtering rate of its product is 710Kg/m
2H, base number are 434.1mgKOH/g, and 100 ℃ of kinematic viscosity are 182.0mm
2/ s.
Embodiment 4
In having the there-necked flask that stirs and reflux, add the naphthenic acid 330g, magnesium oxide 65g, the straight-run spirit 330g of activity-40 that contain acid 40% (weight), mix to stir and be warming up to 50 ℃ of * 1h, add trolamine 8.0g, water 32g, methyl alcohol 120g, 50 ℃ of following aminations 3.0 hours, the carbonic acid gas that feeds 160ml/min carried out carbonation reaction 3.0 hours, was warming up to 110 ℃ and removed alcohol, water, add flocculating aids light calcium carbonate 50g, filtration, underpressure distillation obtain product of the present invention.The filtering rate of its product is 336Kg/m
2H, base number are 354.1mgKOH/g, and 100 ℃ of kinematic viscosity are 238.0mm
2/ s.
Embodiment 5
In having the there-necked flask that stirs and reflux, add the naphthenic acid 330g, magnesium oxide 85g, the straight-run spirit 450g of activity-80 that contain acid 40% (weight), mix and be warming up to 55 ℃ of * 3h, add trolamine 30.0g, water 73g, methyl alcohol 120g, 55 ℃ of following aminations 3.0 hours, the carbonic acid gas that feeds 140ml/min carried out carbonation reaction 5.0 hours, was warming up to 110 ℃ and removed alcohol, water, add flocculating aids light calcium carbonate 60g, filtration, underpressure distillation obtain product of the present invention.The filtering rate of its product is 377Kg/m
2H, base number are 464.1mgKOH/g, and 100 ℃ of kinematic viscosity are 205.2mm
2/ s.
Embodiment 6
Flocculating aids light calcium carbonate among the embodiment 5 is changed to diatomite 33 grams, and all the other are constant, and the filtering rate of the product of the present invention that obtains is 358Kg/m
2H, base number are 460.0mgKOH/g, and 100 ℃ of kinematic viscosity are 202.0mm
2/ s.
Embodiment 7
In having the there-necked flask that stirs and reflux, add the naphthenic acid 330g, magnesium oxide 75g, the dimethylbenzene 250g of activity-40 that contain acid 40% (weight), mix to stir and be warming up to 55 ℃ of * 3h, add trolamine 20.0g, water 67g, methyl alcohol 88g, 55 ℃ of following aminations 2.0 hours, the carbonic acid gas that feeds 140ml/min carried out carbonation reaction 4.0 hours, was warming up to 110 ℃ and removed alcohol, water, add flocculating aids light calcium carbonate 60g, filtration, underpressure distillation obtain product of the present invention.The filtering rate of this product is 412Kg/m
2H, base number are 411.1mgKOH/g, and 100 ℃ of kinematic viscosity are 189.2mm
2/ s.
Embodiment 8
Dimethylbenzene among the embodiment 6 is changed to toluene, and all the other are constant, and the filtering rate of the product of the present invention that obtains is 386Kg/m
2H, base number are 407.0mgKOH/g, and 100 ℃ of kinematic viscosity are 180.4mm
2/ s.
Each product that obtains by the foregoing description is made a service test, and its result is:
1. adopt the SH/T0269 standard to carry out the detergency test: detergency is not more than 2.0 grades;
2. adopt the SH/T0299 standard to carry out the oxidation stability test: oxidation stability is not more than 5.0:
3. adopt GB/T1134 standard (synthetic sea water) to carry out corrosion test: no liquid phase corrosion.
Add the process of flocculating aids product separation in the foregoing description, all can finish by the mode of centrifugation.
The inventive method also can be used for the preparation of carboxylic acid, sulfonic acid and salicylic super base number magnesium salts.
Claims (7)
1. the preparation method of a magnesium naphthenate with superhigh base number, it is characterized in that: at room temperature add naphthenic acid, solvent and the magnesium oxide of metering in the reactor, mix to stir and be warming up to 25 ℃-60 ℃, mixing process keeps 0.5h-4.0h, add entry and methyl alcohol, amine type accelerator then, 40 ℃-60 ℃ reactions 2.0-4.0 hour, then feed a certain amount of carbon dioxide, carried out carbonation reaction 2.0-4.5 hour, intensification dealcoholysis water to 110 ℃, centrifugal or adding flocculating aids filters, and underpressure distillation is sloughed solvent and obtained product.
2. method according to claim 1, it is characterized in that: described amine type accelerator is a purity greater than 65% trolamine, magnesium oxide is activated magnesia, the composition proportion scope of various component materials is: when the add-on of the naphthenic acid that contains sour 35-60% (weight) is 100 grams, add activated magnesia 18-30 gram, solvent 70-160 gram, water 8-25 gram, methyl alcohol 21-42 gram, trolamine 1.8-10 gram, carbonic acid gas 12-30 gram.
3. method according to claim 1 is characterized in that: described solvent can be that boiling range is 40 ℃-180 ℃ a straight-run spirit, also can be toluene or dimethylbenzene.
4. method according to claim 1 is characterized in that: the structural formula of described naphthenic acid is
Wherein: n=7-36, (CH
2)
nIn can comprise 1-4 five-ring or six-ring, R is C
3-20Alkyl chain.
5. method according to claim 1 is characterized in that: the scope of described quantity of methyl alcohol/(quantity of methyl alcohol+water yield) is between 45%-75% (weight).
6. method according to claim 1 is characterized in that: the purity of described methyl alcohol is greater than 98%.
7. method according to claim 1 is characterized in that: described flocculating aids is light calcium carbonate or diatomite, and when the add-on of the naphthenic acid that contains sour 35-60% (weight) was 100 grams, the add-on of flocculating aids was the 3-50 gram.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011307706A CN1164556C (en) | 2001-08-24 | 2001-08-24 | Prepn process of magnesium naphthenate with superhigh base number |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011307706A CN1164556C (en) | 2001-08-24 | 2001-08-24 | Prepn process of magnesium naphthenate with superhigh base number |
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| CN1403435A true CN1403435A (en) | 2003-03-19 |
| CN1164556C CN1164556C (en) | 2004-09-01 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103131520A (en) * | 2011-11-25 | 2013-06-05 | 中国石油天然气股份有限公司 | Metal detergent accelerant, preparation and applications thereof |
| CN103666641A (en) * | 2012-09-25 | 2014-03-26 | 中国石油化工股份有限公司 | High base number sodium napthionate clearing agent, and preparation method and lubricating oil composition thereof |
| CN103666642A (en) * | 2012-09-25 | 2014-03-26 | 中国石油化工股份有限公司 | High-base-number lithium naphthenate and preparation method thereof as well as lubricating oil composition |
| CN107502412A (en) * | 2017-08-30 | 2017-12-22 | 黄山学院 | A kind of high temperature resistant type magnesium salts detergent for lubricating oil and preparation method thereof |
-
2001
- 2001-08-24 CN CNB011307706A patent/CN1164556C/en not_active Expired - Lifetime
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103131520A (en) * | 2011-11-25 | 2013-06-05 | 中国石油天然气股份有限公司 | Metal detergent accelerant, preparation and applications thereof |
| CN103666641A (en) * | 2012-09-25 | 2014-03-26 | 中国石油化工股份有限公司 | High base number sodium napthionate clearing agent, and preparation method and lubricating oil composition thereof |
| CN103666642A (en) * | 2012-09-25 | 2014-03-26 | 中国石油化工股份有限公司 | High-base-number lithium naphthenate and preparation method thereof as well as 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 |
| CN107502412A (en) * | 2017-08-30 | 2017-12-22 | 黄山学院 | A kind of high temperature resistant type magnesium salts detergent for lubricating oil and preparation method thereof |
| CN107502412B (en) * | 2017-08-30 | 2020-02-14 | 黄山学院 | High-temperature-resistant magnesium salt lubricating oil detergent and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN1164556C (en) | 2004-09-01 |
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Granted publication date: 20040901 |