CN112941536B - Wear-resistant environment-friendly engine cleaning oil and preparation method thereof - Google Patents
Wear-resistant environment-friendly engine cleaning oil and preparation method thereof Download PDFInfo
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Abstract
The invention discloses wear-resistant environment-friendly engine cleaning oil, which comprises the following raw materials in percentage by mass: 93.95-97.84% of saturated synthetic ester oil, 0.15-1% of antiwear agent, 2-5% of carbon deposit cleaning agent and 0.01-0.05% of anti-foaming agent. The prepared engine cleaning oil has good biodegradation rate and lubricating property, is safe and environment-friendly, is suitable for popularization in the cleaning oil field, and has wide development prospect.
Description
Technical Field
The invention relates to the field of cleaning oil, in particular to wear-resistant environment-friendly engine cleaning oil and a preparation method thereof.
Background
In the running process of the engine, lubricating oil generates sludge, colloid, carbon deposit and the like due to high temperature and metal catalytic oxidation, and the accumulated carbon deposit, colloid, sludge and harmful substances in a large quantity can aggravate the abrasion of the engine and reduce the service life of the engine along with the extension of the driving mileage. Currently, engine cleaning oil can be used for maintaining an engine, and cleaning twice a year or cleaning once in twenty thousand kilometers is recommended. Statistics data of the Ministry of public security show that by the year 2020, national motor vehicles hold 3.6 hundred million vehicles, wherein 2.7 hundred million vehicles are stored, and if the engine is cleaned once per vehicle every year, the annual requirement of engine cleaning oil is 94.5 ten thousand tons. However, the existing engine cleaning oil is mineral engine oil, has poor degradability and can cause great pollution when discharged to the environment.
The prior art (CN 100449037C) discloses an engine cleaning oil which is composed of one or more of common engine oils 150SN, 500SN, 650SN, 150BS and korean high-grade engine oil SK70N, SK150N, SK100N as base oils, and preservative, antioxidant, antiwear agent, detergent dispersant and pour point depressant, and optionally defoamer, and the physicochemical index reaches the engine oil standard.
The prior art (CN 105733774B) discloses an engine cleaning oil and a preparation method thereof, and the engine cleaning oil comprises the following components in percentage by weight: 78.6-80.6% of base oil, 8-9% of complexing agent, 0.5-1% of antioxidant corrosion inhibitor, 0.5-1% of extreme pressure antiwear agent, 1-1.6% of pour point depressant, 0.2-0.6% of anti-foaming agent, 3-4% of dispersing agent and 4-5% of detergent. The base oils referred to in claims 2 and 3 are 150N, 600N, 150BS.
The essence of the two patents is mineral type engine oil, and the adopted base oil is mineral base oil which is derived from petroleum and is discharged into the environment to be difficult to degrade, so that the environment is damaged. The cleaning oil is largely used with detergents and dispersants, and the additives can cause great burden to the environment, which is not beneficial to environmental protection. In addition, the engine oil uses zinc dialkyldithiophosphate (ZnDTP) as an antiwear agent, which contains zinc as a metal element. The existing detergents and antiwear agents contain metal elements, and excessive metal elements can generate a large amount of ash, so that a particle catcher of an exhaust gas aftertreatment system is blocked. In view of environmental protection and adaptability to vehicles, there is an urgent need for an engine cleaning oil which is free of detergent, dispersant, metal elements, environmentally friendly and highly protective to engines.
Therefore, it is a significant task to develop a cleaning oil that is biodegradable, compatible with vehicles, and excellent in engine protection.
Disclosure of Invention
In order to solve the problems, the first aspect of the invention provides wear-resistant environment-friendly engine cleaning oil, which comprises the following raw materials in percentage by mass: 93.95-97.84% of saturated synthetic ester oil, 0.15-1% of antiwear agent, 2-5% of carbon deposit cleaning agent and 0.01-0.05% of anti-foaming agent.
As a preferable embodiment, the saturated synthetic ester oil is at least one of polyol ester, polyol complex, sebacate diester, and adipate diester.
As a preferable embodiment, the polyol ester is at least one of trimethylolpropane unit saturated fatty acid ester, pentaerythritol unit saturated fatty acid ester, and dipentaerythritol unit saturated fatty acid ester; the polyol complex ester is at least one of ester oil capped by unit saturated fatty acid after prepolymerization of trimethylolpropane and dibasic acid, and ester oil capped by unit saturated fatty acid after prepolymerization of pentaerythritol and dibasic acid; the diester sebacate is at least one of diisooctyl sebacate, di-sec-octyl sebacate and diisotridecyl sebacate; the adipic acid diester is diisooctyl adipate.
As a preferable scheme, the polyol complex has a kinematic viscosity of 50-180 mm at 40 DEG C 2 /s。
As a preferable scheme, the antiwear agent is at least one of di-n-butyl phosphite, acid phosphate amine salt and dialkyl dithiophosphate.
As a preferable scheme, the phosphorus content of the cleaning oil is 0.02-0.07%.
As a preferable scheme, the carbon deposit cleaning agent is at least one of sulfonated kerosene and ethylene glycol butyl ether.
As a preferable scheme, the mass percentage of the ethylene glycol butyl ether in the cleaning oil is 0-0.5%.
As a preferable scheme, the anti-foaming agent is a composite anti-foaming agent of polymethyl propionate and organic silicone oil.
The invention provides a preparation method of the wear-resistant environment-friendly engine cleaning oil, which comprises the following steps: (1) Weighing a predetermined amount of saturated synthetic ester, an antiwear agent, a carbon deposit cleaning agent and an antifoaming agent, and adding into a reaction container; (2) Fully stirring for 30-60 minutes at normal temperature, wherein the stirring speed is 100-300 r/min.
The beneficial effects are that:
1. according to the invention, the self-made saturated synthetic ester oil is used for dispersing oil sludge, carbon deposit and the like into the cleaning oil through the adsorption of the self-made saturated synthetic ester oil in structural polarity, so that the purpose of cleaning an engine is achieved, and the use of a cleaning agent and a dispersing agent is avoided, which is not possessed by other engine cleaning oils.
2. The cleaning oil disclosed by the invention does not contain any metal element, has excellent biodegradability, has strong compatibility with a particle catcher, can avoid abnormal abrasion, and effectively protects an engine.
Detailed Description
The contents of the present invention can be more easily understood by referring to the following detailed description of preferred embodiments of the present invention and examples included. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In case of conflict, the present specification, definitions, will control.
The term "prepared from …" as used herein is synonymous with "comprising". The terms "comprising," "including," "having," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, step, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, step, method, article, or apparatus.
The conjunction "consisting of …" excludes any unspecified element, step or component. If used in a claim, such phrase will cause the claim to be closed, such that it does not include materials other than those described, except for conventional impurities associated therewith. When the phrase "consisting of …" appears in a clause of the claim body, rather than immediately following the subject, it is limited to only the elements described in that clause; other elements are not excluded from the stated claims as a whole.
When an equivalent, concentration, or other value or parameter is expressed as a range, preferred range, or a range bounded by a list of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when ranges of "1 to 5" are disclosed, the described ranges should be construed to include ranges of "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a numerical range is described herein, unless otherwise indicated, the range is intended to include its endpoints and all integers and fractions within the range.
The singular forms include plural referents unless the context clearly dictates otherwise. "optional" or "any" means that the subsequently described event or event may or may not occur, and that the description includes both cases where the event occurs and cases where the event does not.
Approximating language, in the specification and claims, may be applied to modify an amount that would not limit the invention to the specific amount, but would include an acceptable portion that would be close to the amount without resulting in a change in the basic function involved. Accordingly, the modification of a numerical value with "about", "about" or the like means that the present invention is not limited to the precise numerical value. In some examples, the approximating language may correspond to the precision of an instrument for measuring the value. In the present specification and claims, the range limitations may be combined and/or interchanged, such ranges including all the sub-ranges contained therein if not expressly stated.
Furthermore, the indefinite articles "a" and "an" preceding an element or component of the invention are not limited to the requirements of the number of elements or components (i.e. the number of occurrences). Thus, the use of "a" or "an" should be interpreted as including one or at least one, and the singular reference of an element or component also includes the plural reference unless the amount is obvious to the singular reference.
In order to solve the problems, the first aspect of the invention provides wear-resistant environment-friendly engine cleaning oil, which comprises the following raw materials in percentage by mass: 93.95-97.84% of saturated synthetic ester oil, 0.15-1% of antiwear agent, 2-5% of carbon deposit cleaning agent and 0.01-0.05% of anti-foaming agent.
In some preferred embodiments, the saturated synthetic ester oil is at least one of a polyol ester, a polyol complex, a sebacate diester, and an adipate diester.
In some preferred embodiments, the polyol ester is at least one of trimethylolpropane unit saturated fatty acid ester, pentaerythritol unit saturated fatty acid ester, dipentaerythritol unit saturated fatty acid ester; the polyol complex ester is at least one of ester oil capped by unit saturated fatty acid after prepolymerization of trimethylolpropane and dibasic acid, and ester oil capped by unit saturated fatty acid after prepolymerization of pentaerythritol and dibasic acid; the diester sebacate is at least one of diisooctyl sebacate, di-sec-octyl sebacate and diisotridecyl sebacate; the adipic acid diester is diisooctyl adipate.
In some preferred embodiments, the trimethylolpropane unit saturated fatty acid ester has a molecular structure of:
the trimethylolpropane unit saturated fatty acid ester refers to ester oil prepared by reacting trimethylolpropane with unit saturated fatty acid. The unit saturated fatty acids may be valeric acid, isovaleric acid, caproic acid, enanthic acid, caprylic acid, isooctanoic acid, pelargonic acid, isononanoic acid, capric acid, neodecanoic acid, and the like. R is R 1 、R 2 、R 3 The alkyl chains may be identical.
In some preferred embodiments, the trimethylolpropane unit saturated fatty acid ester is self-made, and the steps comprise the steps of: (1) Weighing a preset amount of trimethylolpropane, valeric acid, heptanoic acid, caprylic acid and capric acid, and heating a reaction container to 190-220 ℃; (2) And (3) sequentially adding trimethylolpropane, valeric acid, heptanoic acid, caprylic acid and capric acid into a reaction container, continuously stirring and reacting for 6-10 hours, and finishing post-refining treatment to obtain the finished product.
In some preferred embodiments, the molar ratio of trimethylolpropane, valeric acid, heptanoic acid, octanoic acid, decanoic acid is 0.5-1.5: 0.1 to 0.3:0.4 to 0.5: 1.2-1.4: 1.2 to 1.4.
In some preferred embodiments, the molar ratio of trimethylolpropane, valeric acid, heptanoic acid, octanoic acid, decanoic acid is 1:0.2:0.46:1.32:1.32.
in some preferred embodiments, the molecular structure of the pentaerythritol unit saturated fatty acid ester is:
the pentaerythritol unit saturated fatty acid ester refers to ester oil prepared by reacting pentaerythritol with unit saturated fatty acid. The unit saturated fatty acids may be valeric acid, isovaleric acid, caproic acid, enanthic acid, caprylic acid, isooctanoic acid, pelargonic acid, isononanoic acid, capric acid, neodecanoic acid, and the like. R is R 1 、R 2 、R 3 、R 4 The alkyl chains may be identical.
In some preferred embodiments, the molecular structure of the dipentaerythritol unit saturated fatty acid ester is:
the dipentaerythritol unit saturated fatty acid ester refers to ester oil prepared by the reaction of dipentaerythritol and unit saturated fatty acid. The unit saturated fatty acids may be valeric acid, isovaleric acid, caproic acid, enanthic acid, caprylic acid, isooctanoic acid, pelargonic acid, isononanoic acid, capric acid, neodecanoic acid, and the like. R is R 1 、R 2 、R 3 、R 4 、R 5 、R 6 The alkyl chains may be identical.
In some preferred embodiments, the dipentaerythritol unit saturated fatty acid ester is self-made, and the steps comprise the steps of: (1) Weighing a preset amount of dipentaerythritol, valeric acid, heptanoic acid, caprylic acid and capric acid, and heating a reaction container to 190-220 ℃; (2) Sequentially adding dipentaerythritol, valeric acid, heptanoic acid, octanoic acid and decanoic acid into a reaction container, continuously stirring and reacting for 6-10 hours, and finishing post-refining treatment to obtain the finished product.
In some preferred embodiments, the mole ratio of dipentaerythritol, valeric acid, heptanoic acid, caprylic acid, and capric acid is 0.5 to 1.5: 3.8-4.0: 0.5 to 0.6: 1.2-1.4: 0.6 to 1.0.
In some preferred embodiments, the molar ratio of dipentaerythritol, valeric acid, heptanoic acid, caprylic acid, capric acid is 1:3.96:0.52:1.32:0.8.
in some preferred embodiments, the trimethylolpropane is pre-polymerized with a dibasic acid, followed by the use of a unit saturated fatty acid-terminated ester oil as polyol complex A.
In some preferred embodiments, the pentaerythritol is pre-polymerized with a dibasic acid, followed by the use of a unit saturated fatty acid terminated ester oil as polyol complex B.
In some preferred embodiments, the polyol complex A has a principal compositional structure of:
the unit saturated fatty acids may be valeric acid, isovaleric acid, caproic acid, enanthic acid, caprylic acid, isooctanoic acid, pelargonic acid, isononanoic acid, capric acid, neodecanoic acid, and the like. R is R 1 、R 2 、R 3 、R 4 The alkyl chains may be identical.
In some preferred embodiments, the main composition of the polyol complex a is that when n is 2, the polyol complex a is a trimethylolpropane pre-polymerized with adipic acid, followed by the use of a unit saturated fatty acid terminated ester oil; when n is 4, the polyol complex A is the ester oil capped by unit saturated fatty acid after the pre-polymerization of trimethylolpropane and sebacic acid.
In some preferred embodiments, the main constituent structure of the polyol complex A is that n is 2, and the polyol complex A is that of trimethylolpropane pre-polymerized with adipic acid, and then the ester oil capped by unit saturated fatty acid is adopted.
In some preferred embodiments, polyol complex A is self-made, and the steps comprise the steps of: (1) Weighing a preset amount of trimethylolpropane, adipic acid, valeric acid, heptanoic acid, octanoic acid and decanoic acid, and heating a reaction container to 190-220 ℃; (2) Adding trimethylolpropane and adipic acid into a reaction container, stirring and reacting for 1-2 hours, adding valeric acid, heptanoic acid, octanoic acid and decanoic acid into the reaction container, continuously stirring and reacting for 6-10 hours, and finishing post-refining treatment to obtain the finished product.
In some preferred embodiments, the molar ratio of trimethylolpropane, adipic acid, valeric acid, heptanoic acid, octanoic acid, decanoic acid is 0.8-1.2: 0.4 to 0.6: 0.2-0.3: 1.5-1.7: 0.2-0.3: 0.2 to 0.3.
In some preferred embodiments, the molar ratio of trimethylolpropane, adipic acid, valeric acid, heptanoic acid, octanoic acid, decanoic acid is 1:0.5:0.23:1.61:0.23:0.23.
in some preferred embodiments, the polyol complex B has a principal compositional structure of:
the unit saturated fatty acids may be valeric acid, isovaleric acid, caproic acid, enanthic acid, caprylic acid, isooctanoic acid, pelargonic acid, isononanoic acid, capric acid, neodecanoic acid, and the like. R is R 1 、R 2 、R 3 、R 4 、R 5 、R 6 The alkyl chains may be identical.
In some preferred embodiments, the polyol complex B has a principal constituent structure wherein when n is 2, polyol complex B is a pre-polymerized of pentaerythritol and adipic acid followed by the use of a unit saturated fatty acid terminated ester oil; when n is 4, the polyol complex ester B is pentaerythritol and sebacic acid prepolymerization, and then unit saturated fatty acid end capped ester oil is adopted.
In some preferred embodiments, the main composition of the polyol complex B is that n is 4, and the polyol complex B is that pentaerythritol is prepolymerized with sebacic acid, and then the ester oil capped with a unit saturated fatty acid is used.
In some preferred embodiments, polyol complex B is self-made, and the steps comprise the steps of: (1) Weighing a preset amount of pentaerythritol, sebacic acid, valeric acid, heptanoic acid, octanoic acid and decanoic acid, and heating a reaction container to 190-220 ℃; (2) And adding pentaerythritol and sebacic acid into a reaction container, stirring and reacting for 1-2 hours, adding valeric acid, heptanoic acid, octanoic acid and decanoic acid into the reaction container, continuously stirring and reacting for 6-10 hours, and finishing post-refining treatment to obtain the finished product.
In some preferred embodiments, the molar ratio of pentaerythritol, sebacic acid, valeric acid, heptanoic acid, octanoic acid, decanoic acid is 0.8-1.2: 0.3 to 0.5:0.6 to 0.9: 1.9-2.3: 0.3 to 0.5:0.3 to 0.5.
In some preferred embodiments, the molar ratio of pentaerythritol, sebacic acid, valeric acid, heptanoic acid, octanoic acid, decanoic acid is 1:0.4:0.72:2.16:0.36:0.36.
in some preferred embodiments, the polyol complex has a kinematic viscosity of 50 to 180 mm at 40 DEG C 2 /s。
In some preferred embodiments, the polyol complex has a kinematic viscosity of 50 to 100 mm at 40 ℃ A 2 /s。
In some preferred embodiments, the polyol complex has a kinematic viscosity of 100 to 180 mm at 40 ℃ of B 2 /s。
In some preferred embodiments, the sebacate diester is sebacic acid with C 6 ~C 13 Ester oil prepared by reacting unit alcohols; the C is 6 ~C 13 The monohydric alcohol is selected from 2-ethylhexanol, sec-octanol and iso-tridecanol.
Diisooctyl sebacate, also known as di (2-ethylhexyl) sebacate, CAS number 122-62-3, is used as a plasticizer for polyvinyl chloride cable materials, cold-resistant films and plasticizers for artificial leather and other resins, and can also be used as a raw material for lubricating oils for jet engines.
The di-sec-octyl sebacate is colorless to pale yellow oily liquid, and can be obtained by direct esterification reaction of the sebacic acid and the sec-octyl sebacate under the catalysis of a catalyst, and then through the refining processes of neutralization, steam stripping, filter pressing and the like.
Diisotridecyl sebacate is colorless to pale yellow oily liquidThe product can be obtained by directly esterifying sebacic acid and isotridecyl alcohol under the catalysis of a catalyst, and then carrying out the refining processes of neutralization, steam stripping, filter pressing and the like. Isotridecyl alcohol is fatty alcohol with branched chain in molecular structure, and is branched chain long-chain C 11 ~C 14 In C 13 The alkyl chain is the most.
In the present invention, diisotridecanol sebacate may be commercially available, for example, as a diisotridecanol sebacate product sold by Basoff, japan, and Mobil, USA.
Diisooctyl adipate, CAS number 103-23-1, pale yellow colorless clear liquid. Slightly odorous, is a crude product obtained by directly esterifying adipic acid and industrial isooctanol (chemical name 2-ethylhexanol) in the presence of a catalyst, and is prepared into a fine product by the industries of neutralization, water washing, steam stripping, filter pressing and the like, and a high-quality product can be obtained by molecular distillation or reduced pressure distillation.
In some preferred embodiments, the antiwear agent is at least one of di-n-butyl phosphite, an amine salt of an acid phosphate, a dialkyl dithiophosphate.
The di-n-butyl phosphite is colorless or pale yellow oily liquid, has a flash point of 120 ℃, is easy to dissolve in organic solvents and is insoluble in water, and the phosphorus content is 14.5% -16%. The applicant finds that the di-n-butyl phosphite extreme pressure wear resistance index is high, the compatibility is good, and the di-n-butyl phosphite extreme pressure wear resistance index can be used for preparing low, medium and high grade industrial gear oil, vehicle gear oil, cutting oil and other oil products.
The acid phosphate amine salt is a multi-effect additive of phosphorus and nitrogen. The applicant finds that the acid phosphate amine salt has the multifunction of wear resistance, corrosion inhibition, rust prevention and the like, has good oil solubility and compatibility in the cleaning oil, and can effectively reduce the dosage of corrosion inhibitors and other additives.
The acid phosphate amine salts of the invention can be commercially available, for example, the acid phosphate amine salt products of the type T308, T308B, sold by the company of the additive of the lubricating oil of the type Zibo Hui Huadan, of the company of the lubricating oil of the type Konta, mallotus; irgalube model 349, manufactured and sold by Basoff, germany.
The applicant has unexpectedly found during the course of experiments that conventional ZnDTP additives are not effective in improving the lubricity of the cleaning oil, which was not expected by the inventors. The applicant has found that the addition of di-n-butyl phosphite, amine acid phosphate salt and dialkyl dithiophosphate to the cleaning oil can solve the lubricating problem well.
The dialkyl dithiophosphate is an ashless sulfur and phosphorus extreme pressure antiwear agent, and does not contain metal elements. Can provide good abrasion resistance under the condition of low addition amount. Can provide a lower coefficient of friction than conventional ZnDTP additives. The agent has good compatibility with oil products.
The dialkyldithiophosphate of the present invention may be commercially available, for example, as Irgalube model 63, manufactured and sold by Basff, germany.
In some preferred embodiments, the cleaning oil has a phosphorus content of 0.02-0.07%.
In some preferred embodiments, the carbon deposit cleaning agent is at least one of sulfonated kerosene and ethylene glycol butyl ether.
In some preferred embodiments, the carbon deposit cleaning agent is sulfonated kerosene and ethylene glycol butyl ether.
The sulfonated kerosene is also called 260 # solvent oil, and is a special kerosene type solvent oil prepared by precisely distilling, cutting and refining hydrogenation raw materials. The sulfonated kerosene has the advantages of uniform and slow evaporation speed, less aromatic hydrocarbon content, no odor, no residue in evaporation, difficult oxidation under heating, low sulfur content, low toxicity, high safety, environmental protection and strong dissolving power.
The sulfonated kerosene in the present invention may be a commercially available product of 260 types of sulfonated kerosene produced and sold by Hainan alliance Limited in the name of Magnomonic, for example.
Ethylene glycol butyl ether, CAS No. 111-76-2, has a medium ether taste, low toxicity, a boiling point of 171 ℃, a relative density of 0.9015, a flash point of 61.1 ℃, a self-ignition point of 472 ℃, is soluble in 20 times of water, and is soluble in most organic solvents and mineral oils. Compared with petroleum hydrocarbon, the epoxy resin modified epoxy resin has higher dilution ratio, and is mainly applied to the fields of paint, printing ink, stamp-pad ink, oil, metal detergent, paint remover, lubricant remover, automobile engine detergent, dry cleaning solvent, epoxy resin solvent, medicine extractant and the like.
In some preferred embodiments, the mass percentage of the ethylene glycol butyl ether in the cleaning oil is 0-0.5%.
In some preferred embodiments, the anti-foaming agent is a complex anti-foaming agent of polymethylpropionate and silicone oil.
The applicant found that the formation of foam which is formed by bringing air into the oil product inevitably occurs during the operation of the engine, and the lubrication performance and the cleaning effect are affected by the formation of foam, and the addition of the compound anti-foaming agent effectively inhibits the generation of foam and promotes the accelerated disappearance of foam.
In some preferred embodiments, the complex anti-foaming agent is T922.
The composite anti-foaming agent in the invention can be a product sold in the T922 model manufactured and sold by the Jinzhou Runfeng chemical industry Co Ltd.
The invention provides a preparation method of the wear-resistant environment-friendly engine cleaning oil, which comprises the following steps: (1) Weighing a predetermined amount of saturated synthetic ester, an antiwear agent, a carbon deposit cleaning agent and an antifoaming agent, and adding into a reaction container; (2) Fully stirring for 30-60 minutes at normal temperature, wherein the stirring speed is 100-300 r/min.
Examples
The following describes the technical solution of the present invention in detail by examples, but the scope of protection of the present invention is not limited to all the examples described. The raw materials of the present invention are all commercially available unless otherwise specified.
Example 1
The first aspect of the embodiment 1 provides an antiwear environment-friendly engine cleaning oil, which comprises the following raw materials in percentage by mass: 97.84% of dipentaerythritol unit saturated fatty acid ester, 0.15% of di-n-butyl phosphite, 2% of sulfonated kerosene and 0.01% of anti-foaming agent T922.
In this embodiment, the dipentaerythritol unit saturated fatty acid ester is self-made, and the steps include the following steps: (1) 1 mol of dipentaerythritol, 3.96 mol of valeric acid, 0.52 mol of heptanoic acid, 1.32 mol of octanoic acid, 0.8 mol of decanoic acid are weighed out, and the temperature of the reaction vessel is raised to 210 ℃; (2) Adding dipentaerythritol, valeric acid, heptanoic acid, caprylic acid and capric acid into a reaction container in sequence, continuously stirring and reacting for 8 hours, and finishing post-refining treatment to obtain the finished product.
In this example, di-n-butyl phosphite is sold as model T304 from the company Bobo Hui Huadan oil additives.
In this example, the sulfonated kerosene is a product No. 260 sold by Hainan alliance Limited in the Magnomonic market.
In this example, the anti-foaming agent is a T922 model product sold by Jinzhou Runzhen chemical Co., ltd.
The second aspect of the present embodiment provides a method for preparing the antiwear environment-friendly engine cleaning oil, where: (1) Weighing 97.84% of dipentaerythritol unit saturated fatty acid ester, 0.15% of di-n-butyl phosphite, 2% of sulfonated kerosene and 0.01% of anti-foaming agent T922, and sequentially adding into a reaction container; (2) Fully stirring for 45 minutes at normal temperature, wherein the stirring speed is 100 r/min, and filtering and packaging the finished product.
Example 2
Embodiment 2 in a first aspect provides an antiwear environment-friendly engine cleaning oil, which comprises the following raw materials in percentage by mass: dipentaerythritol unit saturated fatty acid ester 85.95%, trimethylolpropane unit saturated fatty acid ester 10%, acid phosphate amine salt 1%, sulfonated kerosene 3%, and anti-foaming agent T922.05%.
In this embodiment, the dipentaerythritol unit saturated fatty acid ester is self-made, and the steps include the following steps: (1) 1 mol of dipentaerythritol, 3.96 mol of valeric acid, 0.52 mol of heptanoic acid, 1.32 mol of octanoic acid, 0.8 mol of decanoic acid are weighed out, and the temperature of the reaction vessel is raised to 210 ℃; (2) Adding dipentaerythritol, valeric acid, heptanoic acid, caprylic acid and capric acid into a reaction container in sequence, continuously stirring and reacting for 8 hours, and finishing post-refining treatment to obtain the finished product.
In this embodiment, the saturated fatty acid ester of trimethylolpropane unit is self-made, and the steps include the following steps: (1) 1 mol of trimethylolpropane, 0.2 mol of valeric acid, 0.46 mol of heptanoic acid, 1.32 mol of octanoic acid, 1.32 mol of decanoic acid are weighed out, and the reaction vessel is heated to 210 ℃; (2) And (3) sequentially adding trimethylolpropane, valeric acid, heptanoic acid, caprylic acid and capric acid into a reaction container, continuously stirring and reacting for 8 hours, and finishing post-refining treatment to obtain the finished product.
In this example, the acid amine phosphate salt is the model T308 sold by the company Bobo Hui Huadan oil additive Co.
In this example, the sulfonated kerosene is a product No. 260 sold by Hainan alliance Limited in the Magnomonic market.
In this example, the anti-foaming agent is a T922 model product sold by Jinzhou Runzhen chemical Co., ltd.
The second aspect of the present embodiment provides a method for preparing the antiwear environment-friendly engine cleaning oil, where: (1) Weighing 85.95% of dipentaerythritol unit saturated fatty acid ester, 10% of trimethylolpropane unit saturated fatty acid ester, 1% of acid phosphate amine salt, 3% of sulfonated kerosene and 0.05% of anti-foaming agent T922, and sequentially adding into a reaction container; (2) Fully stirring for 45 minutes at normal temperature, wherein the stirring speed is 100 r/min, and filtering and packaging the finished product.
Example 3
Embodiment 3 in a first aspect provides an antiwear environment-friendly engine cleaning oil, which comprises the following raw materials in percentage by mass: 87.48% of dipentaerythritol unit saturated fatty acid ester, 10% of di-sec-octyl sebacate, 0.5% of acid phosphate amine salt, 1.5% of sulfonated kerosene, 0.5% of ethylene glycol butyl ether and 0.02% of anti-foaming agent T922.
In this embodiment, the dipentaerythritol unit saturated fatty acid ester is self-made, and the steps include the following steps: (1) 1 mol of dipentaerythritol, 3.96 mol of valeric acid, 0.52 mol of heptanoic acid, 1.32 mol of octanoic acid, 0.8 mol of decanoic acid are weighed out, and the temperature of the reaction vessel is raised to 210 ℃; (2) Adding dipentaerythritol, valeric acid, heptanoic acid, caprylic acid and capric acid into a reaction container in sequence, continuously stirring and reacting for 8 hours, and finishing post-refining treatment to obtain the finished product.
In this example, di-sec-octyl sebacate CAS number 2432-87-3.
In this example, the acid phosphate amine salt is the product of Irgalube349, sold by Basoff, germany.
In this example, the sulfonated kerosene is a product No. 260 sold by Hainan alliance Limited in the Magnomonic market.
In this example, the CAS number for butyl cellosolve is 111-76-2.
In this example, the anti-foaming agent is a T922 model product sold by Jinzhou Runzhen chemical Co., ltd.
The second aspect of the present embodiment provides a method for preparing the antiwear environment-friendly engine cleaning oil, where: (1) Weighing 87.48% of dipentaerythritol unit saturated fatty acid ester, 10% of di-sec-octyl sebacate, 0.5% of acid phosphate amine salt, 1.5% of sulfonated kerosene, 0.5% of ethylene glycol butyl ether and 0.02% of anti-foaming agent T922, and sequentially adding into a reaction container; (2) Fully stirring for 45 minutes at normal temperature, wherein the stirring speed is 100 r/min, and filtering and packaging the finished product.
Example 4
Embodiment 4 in a first aspect provides an antiwear environment-friendly engine cleaning oil, which comprises the following raw materials in percentage by mass: polyol complex A77.48%, diisooctyl sebacate 20%, dialkyl dithiophosphate 0.5%, sulfonated kerosene 2%, and anti-foaming agent T922.02%.
In this embodiment, the polyol complex A is self-made, and the steps include the following steps: (1) 1 mol of trimethylolpropane, 0.5 mol of adipic acid, 0.23 mol of valeric acid, 1.61 mol of heptanoic acid, 0.23 mol of octanoic acid, 0.23 mol of decanoic acid are weighed out, and the reaction vessel is heated to 210 ℃; (2) Adding trimethylolpropane and adipic acid into a reaction container, stirring and reacting for 2 hours, adding valeric acid, heptanoic acid, octanoic acid and decanoic acid into the reaction container, continuously stirring and reacting for 8 hours, and finishing post-refining treatment to obtain the finished product.
In this example, polyol complex A has a kinematic viscosity of 80 mm at 40 DEG C 2 /s。
In this example, diisooctyl sebacate CAS number 122-62-3.
In this example, the dialkyldithiophosphate was a model Irgalube63 product sold by Basoff, germany.
In this example, the sulfonated kerosene is a product No. 260 sold by Hainan alliance Limited in the Magnomonic market.
In this example, the anti-foaming agent is a T922 model product sold by Jinzhou Runzhen chemical Co., ltd.
The second aspect of the present embodiment provides a method for preparing the antiwear environment-friendly engine cleaning oil, where: (1) Polyol complex A77.48%, diisooctyl sebacate 20%, dialkyl dithiophosphate 0.5%, sulfonated kerosene 2%, and anti-foaming agent T922 0.02% are sequentially added into a reaction vessel; (2) Fully stirring for 45 minutes at normal temperature, wherein the stirring speed is 100 r/min, and filtering and packaging the finished product.
Example 5
Embodiment 5 in a first aspect provides an antiwear environment-friendly engine cleaning oil, which comprises the following raw materials in percentage by mass: polyol complex ester B77.95%, diisooctyl adipate 16%, acid phosphate amine salt 1%, sulfonated kerosene 5% and anti-foaming agent T922.05%.
In this embodiment, the polyol complex B is self-made, and the steps include the following steps: (1) 1 mol of pentaerythritol, 0.4 mol of sebacic acid, 0.72 mol of valeric acid, 2.16 mol of heptanoic acid, 0.36 mol of octanoic acid, 0.36 mol of decanoic acid are weighed out, and the temperature of the reaction vessel is raised to 210 ℃; (2) Adding pentaerythritol and sebacic acid into a reaction container, stirring and reacting for 2 hours, adding valeric acid, heptanoic acid, octanoic acid and decanoic acid into the reaction container, continuously stirring and reacting for 8 hours, and obtaining the finished product.
In this example, polyol complex B has a kinematic viscosity of 150 mm at 40 DEG C 2 /s。
In this example, diisooctyl adipate CAS number 103-23-1.
In this example, the amine salt of an acid phosphate is the product sold under the name T308B, manufactured and sold by the company Bos Hui Huadan oil additives Co., ltd
In this example, the sulfonated kerosene is a product No. 260 sold by Hainan alliance Limited in the Magnomonic market.
In this example, the anti-foaming agent is a T922 model product sold by Jinzhou Runzhen chemical Co., ltd.
The second aspect of the present embodiment provides a method for preparing the antiwear environment-friendly engine cleaning oil, where: (1) Polyol complex ester B77.95%, diisooctyl adipate 16%, acid phosphate amine salt 1%, sulfonated kerosene 5%, and anti-foaming agent T922 0.05% are sequentially added into a reaction vessel; (2) Fully stirring for 45 minutes at normal temperature, wherein the stirring speed is 100 r/min, and filtering and packaging the finished product.
Example 6
Embodiment 6 in a first aspect provides an antiwear environment-friendly engine cleaning oil, which comprises the following raw materials in percentage by mass: diisotridecyl sebacate 97.17%, di-n-butyl phosphite 0.2%, acid phosphate amine salt 0.6%, sulfonated kerosene 2%, and anti-foaming agent T922.03%.
In this example, diisotridecyl sebacate is a diisotridecyl sebacate product sold by basf corporation of germany.
In this example, di-n-butyl phosphite is sold as model T304 from the company Bobo Hui Huadan oil additives.
In this example, the amine salt of an acid phosphate is the product sold under the model T308 from the company Bo Hui Huadan oil additive Co., ltd
In this example, the sulfonated kerosene is a product No. 260 sold by Hainan alliance Limited in the Magnomonic market.
In this example, the anti-foaming agent is a T922 model product sold by Jinzhou Runzhen chemical Co., ltd.
The second aspect of the present embodiment provides a method for preparing the antiwear environment-friendly engine cleaning oil, where: (1) Diisotridecyl sebacate 97.17%, di-n-butyl phosphite 0.2%, acid phosphate amine salt 0.6%, sulfonated kerosene 2%, and anti-foaming agent T922 0.03%, and sequentially adding into a reaction container; (2) Fully stirring for 45 minutes at normal temperature, wherein the stirring speed is 100 r/min, and filtering and packaging the finished product
Comparative example 1
Comparative example 1 the first aspect provides an antiwear environment-friendly engine cleaning oil, the raw materials comprising the following mass percentages: 97.99% of dipentaerythritol unit saturated fatty acid ester, 2% of sulfonated kerosene and 0.01% of anti-foaming agent T922.
The dipentaerythritol unit saturated fatty acid ester in the comparative example is self-made, and the steps comprise the following steps: (1) 1 mol of dipentaerythritol, 3.96 mol of valeric acid, 0.52 mol of heptanoic acid, 1.32 mol of octanoic acid, 0.8 mol of decanoic acid are weighed out, and the temperature of the reaction vessel is raised to 210 ℃; (2) Adding dipentaerythritol, valeric acid, heptanoic acid, caprylic acid and capric acid into a reaction container in sequence, continuously stirring and reacting for 8 hours, and finishing post-refining treatment to obtain the finished product.
In this comparative example, the sulfonated kerosene was sold as product No. 260 by Hainan allied petrochemical Co., ltd. In the name of China.
In this comparative example, the anti-foaming agent was a T922 model product sold by Jinzhou Runzhen chemical Co., ltd.
The second aspect of the comparative example provides a method for preparing the antiwear environment-friendly engine cleaning oil, which comprises the following steps: (1) Weighing 97.99% of dipentaerythritol unit saturated fatty acid ester, 2% of sulfonated kerosene and 0.01% of anti-foaming agent T922, and sequentially adding into a reaction container; (2) Fully stirring for 45 minutes at normal temperature, wherein the stirring speed is 100 r/min, and filtering and packaging the finished product.
Comparative example 2
Comparative example 2 the first aspect provides an antiwear environment friendly engine cleaning oil, the raw materials comprising the following mass percent: 96.98% of dipentaerythritol unit saturated fatty acid ester, 1% of zinc dialkyl dithiophosphate, 2% of sulfonated kerosene and 0.02% of anti-foaming agent T922.
The dipentaerythritol unit saturated fatty acid ester in the comparative example is self-made, and the steps comprise the following steps: (1) 1 mol of dipentaerythritol, 3.96 mol of valeric acid, 0.52 mol of heptanoic acid, 1.32 mol of octanoic acid, 0.8 mol of decanoic acid are weighed out, and the temperature of the reaction vessel is raised to 210 ℃; (2) Adding dipentaerythritol, valeric acid, heptanoic acid, caprylic acid and capric acid into a reaction container in sequence, continuously stirring and reacting for 8 hours, and finishing post-refining treatment to obtain the finished product.
In this comparative example, zinc dialkyldithiophosphate was a product of the type T203 sold by Hubei Kang Disi chemical Co., ltd.
In this comparative example, the sulfonated kerosene was sold as product No. 260 by Hainan allied petrochemical Co., ltd. In the name of China.
In this comparative example, the anti-foaming agent was a T922 model product sold by Jinzhou Runzhen chemical Co., ltd.
The second aspect of the present embodiment provides a method for preparing the antiwear environment-friendly engine cleaning oil, where: (1) Weighing 96.98% of dipentaerythritol unit saturated fatty acid ester, 1% of zinc dialkyl dithiophosphate, 2% of sulfonated kerosene and 0.02% of anti-foaming agent T922, and sequentially adding into a reaction container; (2) Fully stirring for 45 minutes at normal temperature, wherein the stirring speed is 100 r/min, and filtering and packaging the finished product.
Comparative example 3
Comparative example 3 the first aspect provides an antiwear environment friendly engine cleaning oil, the raw materials comprising the following mass percent: 97.99% of mineral oil, 2% of sulfonated kerosene and 0.01% of anti-foaming agent T922.
In this comparative example, the mineral oil is a 250N type product of mineral oil sold by Shenzhen Cheng Hongda lubrication Co., ltd.
In this comparative example, the sulfonated kerosene was sold as product No. 260 by Hainan allied petrochemical Co., ltd. In the name of China.
In this comparative example, the anti-foaming agent was a T922 model product sold by Jinzhou Runzhen chemical Co., ltd.
The second aspect of the comparative example provides a method for preparing the antiwear environment-friendly engine cleaning oil, which comprises the following steps: (1) Weighing 97.99% of mineral oil, 2% of sulfonated kerosene and 0.01% of anti-foaming agent T922, and sequentially adding into a reaction container; (2) Fully stirring for 45 minutes at normal temperature, wherein the stirring speed is 100 r/min, and filtering and packaging the finished product.
Evaluation of Performance
1) Kinematic viscosity at 40 ℃): with reference to the national standard test method GB/T265, the kinematic viscosity of the test sample, 5 samples were tested for each comparative example, and the data were averaged and reported in Table 1.
2) Biodegradation rate: the biodegradability of the samples is determined with reference to the CEC-L-33-A-93 test method. The biodegradation rate of the oil product is generally more than or equal to 60%, the sample can be judged to be biodegradable, the sample is environment-friendly, 5 samples are tested in each comparative example, and the data are averaged and calculated in Table 1.
3) Lubricity test (four ball frictional wear test): the lubricating properties of the samples were tested with reference to industry standard SH/T0189. The test conditions were 490N,1200r/min,15min, room temperature. The smaller the plaque diameter, the better the lubricity of the oil and the greater the antiwear protection, 5 samples were tested for each comparative example and the data averaged to give Table 1.
4) Phosphorus content test: the phosphorus content of the oil was tested by referring to the national standard GB/T17476 test method, 5 samples were tested for each comparative example, and the data are averaged and reported in Table 1.
TABLE 1
According to the examples 1-6, the comparative examples 1-3 and the data in Table 1, the antiwear environment-friendly engine cleaning oil and the preparation method thereof provided by the invention have the advantages that the prepared engine cleaning oil has good biodegradation rate and lubricating property, is safe and environment-friendly, is suitable for popularization in the cleaning oil field, and has a wide development prospect.
Finally, it should be understood that the foregoing embodiments are merely preferred embodiments of the present invention, and are not intended to limit the invention, but are intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the invention.
Claims (7)
1. An antiwear environment-friendly engine cleaning oil is characterized in that: the raw materials comprise the following components in percentage by mass: 93.95-97.84% of saturated synthetic ester oil, 0.15-1% of antiwear agent, 2-5% of carbon deposit cleaning agent and 0.01-0.05% of anti-foaming agent;
the wear-resistant environment-friendly engine cleaning oil does not contain any metal element;
the saturated synthetic ester oil is at least one of polyol ester, polyol complex ester, sebacate diester and adipic acid diester;
the polyol ester is at least one of trimethylolpropane unit saturated fatty acid ester, pentaerythritol unit saturated fatty acid ester and dipentaerythritol unit saturated fatty acid ester; the polyol complex ester is at least one of ester oil capped by unit saturated fatty acid after prepolymerization of trimethylolpropane and dibasic acid, and ester oil capped by unit saturated fatty acid after prepolymerization of pentaerythritol and dibasic acid; the diester sebacate is at least one of diisooctyl sebacate, di-sec-octyl sebacate and diisotridecyl sebacate; the adipic acid diester is diisooctyl adipate;
the molecular structure of the trimethylolpropane unit saturated fatty acid ester is as follows:
the trimethylolpropane unit saturated fatty acid ester refers to ester oil prepared by the reaction of trimethylolpropane and unit saturated fatty acid;
the molecular structure of the pentaerythritol unit saturated fatty acid ester is as follows:
the pentaerythritol unit saturated fatty acid ester refers to ester oil prepared by reacting pentaerythritol with unit saturated fatty acid;
the molecular structure of the dipentaerythritol unit saturated fatty acid ester is as follows:
the dipentaerythritol unit saturated fatty acid ester refers to ester oil prepared by the reaction of dipentaerythritol and unit saturated fatty acid;
the trimethylolpropane and the dibasic acid are prepolymerized, and then ester oil capped by unit saturated fatty acid is adopted as polyol complex ester A;
the pentaerythritol is prepolymerized with dibasic acid, and then ester oil capped by unit saturated fatty acid is adopted as polyol complex ester B;
the main composition structure of the polyol complex A is as follows:
in the main composition structure of the polyol complex A, when n is 2, the polyol complex A is prepared by prepolymerizing trimethylolpropane and adipic acid, and then adopting unit saturated fatty acid end-capped ester oil; when n is 4, the polyol complex ester A is prepared by prepolymerizing trimethylolpropane and sebacic acid, and then adopting unit saturated fatty acid end-capped ester oil;
the main composition structure of the polyol complex B is as follows:
in the main composition structure of the polyol complex B, when n is 2, the polyol complex B is ester oil capped by unit saturated fatty acid after the pre-polymerization of pentaerythritol and adipic acid; when n is 4, the polyol complex ester B is pentaerythritol and sebacic acid prepolymerization, and then ester oil capped by unit saturated fatty acid is adopted;
the unit saturated fatty acid is at least one of valeric acid, isovaleric acid, caproic acid, heptanoic acid, caprylic acid, isooctanoic acid, pelargonic acid, isononanoic acid, capric acid and neodecanoic acid;
the kinematic viscosity of the polyol complex ester A at 40 ℃ is 50-100 mm 2 /s；
The polyol complex ester has a kinematic viscosity of 100-180 mm at 40 ℃ of B 2 /s。
2. The antiwear environment protection type engine cleaning oil according to claim 1, characterized in that: the antiwear agent is at least one of di-n-butyl phosphite, acid phosphate amine salt and dialkyl dithiophosphate.
3. The antiwear environment protection type engine cleaning oil according to claim 1, characterized in that: the phosphorus content of the cleaning oil is 0.02-0.07%.
4. The antiwear environment protection type engine cleaning oil according to claim 1, characterized in that: the carbon deposit cleaning agent is at least one of sulfonated kerosene and ethylene glycol butyl ether.
5. The antiwear environment protection type engine cleaning oil according to claim 4, wherein: the mass percentage of the ethylene glycol butyl ether in the cleaning oil is 0-0.5%.
6. The antiwear environment protection type engine cleaning oil according to claim 1, characterized in that: the anti-foaming agent is a composite anti-foaming agent of polymethyl propionate and organic silicone oil.
7. A method for preparing the antiwear environment-friendly engine cleaning oil according to any one of claims 1 to 6, which is characterized in that: the method comprises the following steps: (1) Weighing a predetermined amount of saturated synthetic ester, an antiwear agent, a carbon deposit cleaning agent and an antifoaming agent, and adding into a reaction container; (2) Fully stirring for 30-60 minutes at normal temperature, wherein the stirring speed is 100-300 r/min.
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