CN109536266B - Treatment method for reducing acid value of lubricating oil - Google Patents
Treatment method for reducing acid value of lubricating oil Download PDFInfo
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- CN109536266B CN109536266B CN201710857325.5A CN201710857325A CN109536266B CN 109536266 B CN109536266 B CN 109536266B CN 201710857325 A CN201710857325 A CN 201710857325A CN 109536266 B CN109536266 B CN 109536266B
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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
- C10M177/00—Special methods of preparation of lubricating compositions; Chemical modification by after-treatment of components or of the whole of a lubricating composition, not covered by other classes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/14—Methyl esters, e.g. methyl (meth)acrylate
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F226/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen
- C08F226/06—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen by a heterocyclic ring containing nitrogen
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1804—C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate
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- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Lubricants (AREA)
Abstract
The invention discloses a treatment method for reducing the acid value of lubricating oil. The method comprises the following steps: the used treating agent is a polymer containing ethylene monomer structural units and acrylate structural units; the vinyl monomer structural unit has a structure represented by formula (1):
Description
Technical Field
The invention relates to the technical field of lubricating oil treatment, in particular to a treatment method for reducing the acid value of lubricating oil.
Background
Lubricating oils are a very important class of petroleum products. Lubricating oils are available in many varieties, but they are mainly composed of base oils and appropriate amounts of various additives. For the lubricant base oil produced from crude oil, the quality standards thereof are classified into paraffin-based base oil series, intermediate-based base oil series, and naphthenic-based base oil series according to the crude oil category.
Besides a certain viscosity, the lubricating oil also needs to have better viscosity-temperature property and anti-oxidation stability, and lower carbon residue value. In order to meet the above requirements, most of the polycyclic short side chain aromatics and gums must be removed from the lubricating oil feedstock to improve the quality of the lubricating oil, a process known as lube oil refining. The commonly used purification methods are: acid and alkali refining, solvent refining, adsorption refining, hydrorefining and the like.
In the prior art, the treating agents adopted by solvent refining are usually ethylene oxide, light hydrocarbon, surfactant and the like, and the solvent refining has the advantages of good refining effect, wide range of applicable raw materials, easy production, low price and the like, but also has the defects of low refining yield, poor deacidification selectivity and the like. In addition, with the enlargement of the development scale of heavy crude oil in recent years, the quality of the distillate oil of the lubricating oil is reduced, and the shortage of solvent refining of the lubricating oil is more remarkable.
The acid number of the lubricating oil is a quality index representing the total content of organic acids in the lubricating oil, and the acid number is the number of milligrams of potassium hydroxide required for neutralizing 1 gram of petroleum product. The magnitude of the change in acid number is often used to measure the oxidation stability of a lubricating oil. The high acid value of the lubricating oil indicates that the lubricating oil has high organic acid content and may cause corrosion to mechanical parts, and particularly, the corrosion effect may be more obvious in the presence of water.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a treatment method for reducing the acid value of lubricating oil. Can effectively reduce the acid value of the lubricating oil and has small oil product loss.
One of the objects of the present invention is to provide a treatment method for reducing the acid value of a lubricating oil.
The method comprises the following steps:
the used treating agent is a polymer containing ethylene monomer structural units and acrylate structural units;
the vinyl monomer structural unit has a structure represented by formula (1):
wherein n is 1 or 2, and R1 and R2 are each independently H or C1-C20 alkanyl.
Among them, preferred are:
r1 and R2 are each independently H, CH3, C2H5 or C4H 9.
Based on the total weight of the polymer, the content of the ethylene structural unit (1) is 0.1-99.9 wt%, and the content of the acrylate structural unit is 0.1-99.9 wt%; more preferably, the content of the ethylene structural unit (1) is 10 to 30 wt% and the content of the acrylate structural unit is 70 to 90 wt%, based on the total weight of the polymer.
The molecular weight of the polymer is between 500 and 100000, the molecular weight distribution is 1.0-8.0, preferably 100 and 35000, and the molecular weight distribution is 1.5-5.0.
The method comprises the following steps:
dissolving the treating agent in a solvent, and refining the lubricating oil sample by the solvent; standing after refining;
the weight percentage of the lubricating oil sample to the treating agent is (85-99%): (0.1-15%); preferably (90-95%): (4-10%).
The purification reaction time is preferably 0.1 to 1 hour; the purification reaction temperature is preferably 90 to 130 ℃.
The standing time is 0.5-1.5 hours.
The refining time refers to the time required for refining the lubricating oil sample by shaking or the like after the solvent and the lubricating oil sample are mixed.
The standing time is the time required for the sample of lubricating oil to stand still, i.e., the phase separation time.
The lubricating oil sample is preferably a naphthenic oil;
the solvent is preferably furfural or NMP.
The invention can adopt the following technical scheme:
the method comprises the following steps: the invention provides an acid treating agent which can effectively reduce the acid value of lubricating oil.
The treating agent provided by the invention is a polymer containing ethylene monomer structural units and acrylate structural units;
the vinyl monomer structural unit has a structure represented by formula (1):
wherein n is 1 or 2, and R1 and R2 are each independently H or C1-C20 alkanyl.
R1 and R2 are each independently H or C1-C20 alkanyl, preferably H, CH3, C2H5, C4H9
The acrylate is acrylate with alkyl side chain, the alkyl side chain is C1-C20 linear alkyl or branched alkyl side chain, and preferably CH3, C2H5, C4H9 and C12H25.
The copolymer can be a random copolymer, a block copolymer, an alternating copolymer or a graft copolymerization.
According to a preferred embodiment of the present invention, in order to improve the acid removal performance of the polymer of the present invention, the polymer may further contain an acrylamide structural monomer.
The monomer of the acrylamide structure may be a monomer commonly used in the art, and is preferably one or more selected from the group consisting of 2-acrylamido-2-methylpropanesulfonic acid, N-vinylpyrrolidone, dimethylaminoethyl acrylate, diethylaminoethyl acrylate, dimethylaminoethyl methacrylate, diethylaminoethyl methacrylate, and N, N-dimethylacrylamide.
According to the polymer, the content of the ethylene monomer structural unit (1) and the acrylate structural unit can be selected within a wide range, and preferably, the content of the ethylene structural unit (1) is 0.1-99.9 wt% and the content of the acrylate structural unit is 0.1-99.9 wt% based on the total weight of the polymer; more preferably, the content of the ethylene structural unit (1) is 10 to 30 wt% and the content of the acrylate structural unit is 70 to 90 wt%, based on the total weight of the polymer. The preferable content is more favorable for fully playing the function of the ethylene monomer structural unit, and further the polymer with better acid removal performance is obtained.
The polymer of the invention has a molecular weight of 500-100000, a molecular weight distribution of 1.0-8.0, preferably 100-35000, and a molecular weight distribution of 1.5-5.0.
The treating agent of the present invention can be prepared by a method of the prior art, which comprises: and (2) in the presence of an initiator, carrying out polymerization reaction on a monomer mixture, wherein the monomer mixture contains acrylamide and a monomer A, and the monomer A is the ethylene monomer with the structure of the formula (1).
The method for producing a polymer according to the present invention, wherein the weight ratio of the monomer mixture to the initiator is not particularly limited, and is preferably 1: (1X 10)-6-3×10-2) More preferably, the molar ratio is 1: (1X 10)-5-5×10-3)。
In the method for preparing the treating agent according to the present invention, the type of the initiator is not particularly limited, but in order to improve the overall performance of the polymer, the initiator is preferably an azo initiator or a peroxide initiator, and preferably azobisisobutyronitrile or benzoyl peroxide.
The invention can adopt the following technical scheme:
dissolving the treating agent in a solvent, and refining the lubricating oil sample by the solvent to obtain the lubricating oil with the acid value of less than 0.03 mgKOH/g;
the treating agent is a polymer, wherein the polymer contains an ethylene monomer structural unit and an acrylamide structural unit, and the ethylene monomer structural unit has a structure shown in a formula (1):
the formula (1) wherein n is 1 or 2, and R1 and R2 are each independently H or a C1-C20 alkanyl group.
The weight percentage of the lubricating oil sample to the treating agent is (85-99%): (0.1-15%).
Preferably, the lubricating oil sample is a naphthenic oil.
Preferably, the treating agent is dissolved in a solvent, and the lubricating oil sample is solvent refined, wherein the reaction time is 0.1-1 hour.
Preferably, the treating agent is dissolved in a solvent, and the lubricating oil sample is subjected to solvent refining, wherein the reaction temperature is 90-130 ℃.
Preferably, the treating agent is dissolved in a solvent, and the lubricating oil sample is solvent-refined and left to stand for 0.5 to 1.5 hours.
Preferably, the weight percentage of the lubricating oil sample to the treating agent is (90-95%): (5-10%).
Compared with the prior art, the treating agent adopted by the invention is a polymer, wherein the polymer contains an ethylene monomer structural unit and an acrylamide structural unit, and can react with organic acid in a lubricating oil sample, so that the organic acid is consumed, and the purpose of reducing the acid value of the lubricating oil sample is achieved. The treating agent adopted by the invention is non-corrosive, is easy to remove, and cannot pollute the environment and samples. Experiments show that the acid value of the lubricating oil sample treated by the method is 0.01-0.03 mgKOH/g.
Detailed Description
The present invention will be described in further detail below with reference to examples, but it should be noted that the examples of the present invention are only for illustrating the technical aspects of the present invention, and the scope of the present invention is not limited to the following examples.
Synthesis of treating agent
Example A1
4.10 g of butyl acrylate, 3.04 g of n being 1 and R being at room temperature1、R2Are all CH3The vinyl monomer of formula (1) in (2) was dissolved in 20ml of ethyl acetate, and the reaction vessel was purged with nitrogen gas and deoxygenated for 20 minutes. Adding 0.05 g of azobisisobutyronitrile, transferring into a polymerization bottle, introducing nitrogen to remove oxygen for 20 minutes, then pumping under reduced pressure to remove oxygen, introducing nitrogen for 20 minutes, reacting at 70 ℃ for 8 hours, and precipitating in n-hexane to obtain a colloidal polymer 1, wherein the molecular weight is 7800 and the molecular weight distribution is 1.78. The content of the structural unit 1 is 42.5 percent
Example A2
At room temperature, 10 g of methyl acrylate, 9.12 g of n are 1 and R is1、R2Are all CH3The vinyl monomer of formula (1) in (2) was dissolved in 20ml of ethyl acetate, and the reaction vessel was purged with nitrogen gas and deoxygenated for 20 minutes. Add azobisisobutyronitrile 0.05 g and transfer to a polymerization flaskIntroducing nitrogen to remove oxygen for 20 minutes, then pumping under reduced pressure to remove oxygen, introducing nitrogen for 20 minutes, reacting at 70 ℃ for 8 hours, and precipitating in n-hexane to obtain a colloidal polymer 1, wherein the molecular weight is 25000 and the molecular weight distribution is 2.23. The content of the structural unit 1 is 47.6 percent
Example A3
At room temperature, 5.0 g of lauric acrylate, 9.12 g of n is 1 and R is1、R2Are all CH3The vinyl monomer of formula (1) in (2) was dissolved in 20ml of ethyl acetate, and the reaction vessel was purged with nitrogen gas and deoxygenated for 20 minutes. Adding 0.05 g of azobisisobutyronitrile, transferring into a polymerization bottle, introducing nitrogen to remove oxygen for 20 minutes, then pumping under reduced pressure to remove oxygen, introducing nitrogen for 20 minutes, reacting at 70 ℃ for 8 hours, and precipitating in n-hexane to obtain a colloidal polymer 1, wherein the molecular weight is 68000 and the molecular weight distribution is 5.8. The content of the structural unit 1 is 64.1 percent
Example A4
5.0 g of methyl acrylate, 9.12 g of n is 1 and R is at room temperature1、R2The vinyl monomer having the structure of formula (1) which is C4H9 was dissolved in 20ml of ethyl acetate, and the reaction vessel was purged with nitrogen and deoxygenated for 20 minutes. Adding 0.05 g of azobisisobutyronitrile, transferring into a polymerization bottle, introducing nitrogen to remove oxygen for 20 minutes, then pumping under reduced pressure to remove oxygen, introducing nitrogen for 20 minutes, reacting at 70 ℃ for 8 hours, and precipitating in n-hexane to obtain a colloidal polymer 1, wherein the molecular weight is 15400 and the molecular weight distribution is 2.0 by measurement. The content of the structural unit 1 is 64.1 percent
[ example B1 ]
9 kg of a sample of a lubricating oil having an acid value of 0.28mgKOH/g and 0.5 kg of a furfural solvent as the polymer treating agent described in example A1 were mixed, stirred at 100 ℃ and subjected to a refining reaction for 0.1 hour. Then, the mixture was allowed to stand at a constant temperature of 100 ℃ for 1 hour. Cooling to 60 ℃, and filtering to obtain a lubricating oil finished product. The obtained lubricating oil product was sampled and measured for acid value to be 0.01 mgKOH/g.
[ example B2 ]
20 kg of a sample of a lubricating oil having an acid value of 0.58mgKOH/g and 1 kg of a furfural solvent to which the polymer treating agent described in example A1 was added were mixed, stirred at a temperature of 120 ℃ and subjected to a refining reaction for 0.5 hour. Then standing at constant temperature of 120 ℃ for 1 hour to separate phases. Cooling to 60 ℃, and filtering to obtain a lubricating oil finished product. The obtained lubricating oil product was sampled and measured to have an acid value of 0.02 mgKOH/g.
[ example B3 ]
3 kg of a sample of a lubricating oil having an acid value of 0.63mgKOH/g and 0.15 kg of a furfural solvent to which the polymer treating agent described in example A2 was added were mixed, stirred at 120 ℃ and subjected to a refining reaction for 0.15 hour. Then standing at constant temperature of 120 ℃ for 1 hour to separate phases. Cooling to 60 ℃, and filtering to obtain a lubricating oil finished product. The obtained lubricating oil product was sampled and measured for acid value to be 0.01 mgKOH/g.
[ example B4 ]
2 kg of a sample of a lubricating oil having an acid value of 0.84mgKOH/g and 0.04 kg of a furfural solvent to which the polymer treating agent described in example A3 was added were mixed, stirred at 100 ℃ and subjected to a refining reaction for 0.1 hour. Then standing at constant temperature of 100 ℃ for 1 hour to separate phases. And cooling to 60 ℃, and extracting the upper oil phase to obtain a finished lubricating oil product. The obtained lubricating oil product was sampled and measured for acid value to be 0.01 mgKOH/g.
[ example B5 ]
10 kg of a sample of a lubricating oil having an acid value of 4.15mgKOH/g and 0.31 kg of a furfural solvent to which the polymer treating agent described in example A4 was added were mixed, stirred at 100 ℃ and subjected to a refining reaction for 0.2 hour. Then standing at constant temperature of 100 ℃ for 1 hour to separate phases. And cooling to 60 ℃, and extracting the upper oil phase to obtain a finished lubricating oil product. The obtained lubricating oil product was sampled and measured for acid value to be 0.01 mgKOH/g.
[ example B6 ]
7 kg of a sample of a lubricating oil having an acid value of 3.25mgKOH/g and 0.28 kg of a furfural solvent to which the polymer treating agent described in example A1 was added were mixed, stirred at 100 ℃ and subjected to a refining reaction for 0.15 hour. Then standing at constant temperature of 100 ℃ for 1 hour to separate phases. And cooling to 60 ℃, and extracting the upper oil phase to obtain a finished lubricating oil product. The obtained lubricating oil product was sampled and measured for acid value to be 0.01 mgKOH/g.
[ example B7 ]
6 kg of a sample of a lubricating oil having an acid value of 1.25mgKOH/g and 0.25 kg of the NMP solvent to which the polymer treating agent described in example A1 had been added were mixed, stirred at 120 ℃ and then allowed to stand at 120 ℃ for 1.5 hours to phase-separate. And cooling to 60 ℃, and extracting the upper oil phase to obtain a finished lubricating oil product. The obtained lubricating oil product was sampled and measured to have an acid value of 0.02 mgKOH/g.
[ example B8 ]
15 kg of a sample of a lubricating oil having an acid value of 4.49mgKOH/g and 0.72 kg of the NMP solvent to which the polymer treating agent described in example A2 had been added were mixed, stirred at 120 ℃ and then allowed to stand at 120 ℃ for 1.5 hours to phase-separate. And cooling to 60 ℃, and extracting the upper oil phase to obtain a finished lubricating oil product. The obtained lubricating oil product was sampled and measured to have an acid value of 0.02 mgKOH/g.
The above description of the embodiments is provided to aid in understanding the methods and core concepts of the present invention. It should be noted that, for a person skilled in the art, several modifications and changes can be made to the present invention without departing from the scope of the invention as defined in the appended claims.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art. The general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (8)
1. A treatment method for reducing the acid value of lubricating oil, characterized in that the method comprises:
the used treating agent is a polymer consisting of ethylene monomer structural units and acrylate structural units;
the vinyl monomer structural unit has a structure represented by formula (1):
wherein n is 1 or 2, R1 and R2 are each independently H or C1-C20 alkanyl;
the total weight of the polymer is taken as a reference, the content of the ethylene structural unit (1) is 42.5-64.1 wt%, and the content of the acrylate structural unit is 35.9-57.5 wt%;
the molecular weight of the polymer is between 500 and 100000, and the molecular weight distribution is 1.0-8.0.
2. The method of reducing the acid number of a lubricating oil according to claim 1, wherein:
r1 and R2 are each independently H, CH3, C2H5 or C4H 9.
3. The method of reducing the acid number of a lubricating oil according to claim 1, wherein:
dissolving the treating agent in a solvent, and refining the lubricating oil sample by the solvent; standing after refining;
the weight percentage of the lubricating oil sample to the treating agent is (85-99%): (0.1-15%).
4. The method of claim 3, wherein the treatment is carried out in the presence of a catalyst to reduce the acid number of the lubricating oil
The weight percentage of the lubricating oil sample to the treating agent is (90-95%): (4-10%).
5. The method of claim 3, wherein the treatment comprises:
the purification reaction time is 0.1 to 1 hour.
6. The method of claim 3, wherein the treatment comprises:
the refining reaction temperature is 90-130 ℃.
7. The method of reducing the acid number of a lubricating oil according to claim 5, wherein:
the standing time is 0.5-1.5 hours.
8. The method of claim 3, wherein the treatment comprises:
the lubricating oil samples were naphthenic base oils;
the solvent is furfural or NMP.
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| JPH03137295A (en) * | 1989-10-24 | 1991-06-11 | Sannopuko Kk | Lubricant for pigment-coated paper |
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| JP5239531B2 (en) * | 2008-06-16 | 2013-07-17 | 株式会社リコー | Image carrier protecting agent, protective layer forming apparatus, image forming method, image forming apparatus, and process cartridge |
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2017
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| JPH03137295A (en) * | 1989-10-24 | 1991-06-11 | Sannopuko Kk | Lubricant for pigment-coated paper |
| JPH05117681A (en) * | 1991-10-30 | 1993-05-14 | Mitsubishi Heavy Ind Ltd | Refrigerator oil |
| CN102977976A (en) * | 2006-04-24 | 2013-03-20 | 卢布里佐尔公司 | Star polymer lubricating composition |
| CN102911780A (en) * | 2012-10-26 | 2013-02-06 | 中国石油化工股份有限公司 | Treating method for lubrication oleic acid values |
| CN104629868A (en) * | 2015-02-02 | 2015-05-20 | 中国石油大学(华东) | Preparation method of low-sulfur diesel oil antiwear agent |
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