CN111100727A - Synthetic brake fluid and preparation method thereof - Google Patents
Synthetic brake fluid and preparation method thereof Download PDFInfo
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- CN111100727A CN111100727A CN201911354596.4A CN201911354596A CN111100727A CN 111100727 A CN111100727 A CN 111100727A CN 201911354596 A CN201911354596 A CN 201911354596A CN 111100727 A CN111100727 A CN 111100727A
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- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/26—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds
- C08G65/2618—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing nitrogen
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- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/02—Hydroxy compounds
- C10M2207/023—Hydroxy compounds having hydroxy groups bound to carbon atoms of six-membered aromatic rings
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- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/04—Ethers; Acetals; Ortho-esters; Ortho-carbonates
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- C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
- C10M2209/02—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C10M2209/08—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to a carboxyl radical, e.g. acrylate type
- C10M2209/084—Acrylate; Methacrylate
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- C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
- C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C10M2209/103—Polyethers, i.e. containing di- or higher polyoxyalkylene groups
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- C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
- C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C10M2209/103—Polyethers, i.e. containing di- or higher polyoxyalkylene groups
- C10M2209/108—Polyethers, i.e. containing di- or higher polyoxyalkylene groups etherified
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- C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
- C10M2215/04—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to acyclic or cycloaliphatic carbon atoms
- C10M2215/042—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to acyclic or cycloaliphatic carbon atoms containing hydroxy groups; Alkoxylated derivatives thereof
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- C10M2217/00—Organic macromolecular compounds containing nitrogen as ingredients in lubricant compositions
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- C10M2227/00—Organic non-macromolecular compounds containing atoms of elements not provided for in groups C10M2203/00, C10M2207/00, C10M2211/00, C10M2215/00, C10M2219/00 or C10M2223/00 as ingredients in lubricant compositions
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Abstract
The invention relates to the field of automobile brake fluid, in particular to synthetic brake fluid and a preparation method thereof. The synthetic brake fluid comprises, by weight, 45-75 parts of triethylene glycol methyl ether borate, 10-30 parts of polyethylene glycol ether, 3-15 parts of polyether polyol, 0.5-3 parts of an anti-aging agent, 0.3-1.5 parts of a pH regulator and 0.1-1.0 part of a corrosion inhibitor, wherein the polyether polyol is modified polyether polyol, and the corrosion inhibitor is sodium polyacrylate and sodium nitrite. According to the invention, the modified polyether polyol prepared by a specific method and the corrosion inhibitor with specific components and proportion are added into the brake fluid, so that the low-temperature fluidity of the brake fluid is improved, the high-temperature air resistance of the brake fluid is not influenced, the circulating stability of the brake fluid is enhanced, and the automobile can still keep better braking performance after frequent braking.
Description
Technical Field
The invention relates to the field of automobile brake fluid, in particular to synthetic brake fluid and a preparation method thereof.
Background
The automobile brake fluid is also called brake fluid, is a medium used in a hydraulic braking system and the clutch operation parts of certain automobiles, and the performance of the automobile brake fluid is directly related to the driving safety, so that the national strict requirements on the quality of the automobile brake fluid mainly relate to the high-temperature air resistance, the low-temperature fluidity, the swelling property to rubber, the metal corrosion resistance, the oxidation resistance, the stability and the like of the brake fluid.
With the continuous improvement of automobile technology, brake fluid is also developed into synthetic brake fluid from initial alcohol type brake fluid, currently, the most applied synthetic brake fluid is alcohol ether borate type, which is composed of base fluid, diluent and additive, wherein the base fluid borate enables the brake fluid to have better high-temperature air resistance and water resistance due to the nature of the base fluid borate, but the diluent and the additive are usually added in order to adjust the low-temperature fluidity of the brake fluid, the compatibility with rubber, the metal corrosion resistance, the oxidation resistance and the like. Although the added diluent and additive improve the performances of the brake fluid such as low-temperature fluidity, compatibility with rubber and the like to a certain extent, on one hand, a part of water-absorbing substances such as alcohol diluent is introduced to reduce the high-temperature air resistance of the brake fluid, and on the other hand, the compatibility of the introduced additive and a base fluid needs to be considered, particularly when the automobile frequently runs at high speed, the brake fluid is greatly influenced by heat, and the additive generates precipitates, so that the performance of the brake fluid is influenced, and the brake system of the automobile is blocked.
Disclosure of Invention
In order to solve the technical problems, the invention provides a synthetic brake fluid in a first aspect, wherein the brake fluid comprises raw materials of 45-75 parts of triethylene glycol methyl ether borate, 10-30 parts of polyethylene glycol ether, 3-15 parts of polyether polyol, 0.5-3 parts of an anti-aging agent, 0.3-1.5 parts of a pH regulator and 0.1-1.0 part of a corrosion inhibitor.
According to a preferable technical scheme, the brake fluid comprises, by weight, 60-70 parts of triethylene glycol methyl ether borate, 14-25 parts of polyglycol ether, 7-12 parts of polyether polyol, 1.5-2.5 parts of an anti-aging agent, 0.8-1.2 parts of a pH regulator and 0.5-0.8 part of a corrosion inhibitor.
According to a preferable technical scheme of the invention, the brake fluid comprises, by weight, 63 parts of triethylene glycol methyl ether borate, 17 parts of polyethylene glycol ether, 10 parts of polyether polyol, 2 parts of an anti-aging agent, 0.9 part of a pH regulator and 0.7 part of a corrosion inhibitor.
In a preferred embodiment of the present invention, the polyethylene glycol ether is at least one selected from the group consisting of diethylene glycol methyl ether, triethylene glycol methyl ether, diethylene glycol ethyl ether, triethylene glycol ethyl ether, diethylene glycol butyl ether, and triethylene glycol butyl ether.
As a preferred technical scheme of the invention, the polyether polyol is modified polyether polyol, and the preparation method comprises the following steps:
adding a solvent into a reaction container, adding polyol while stirring, then adding a catalyst, introducing nitrogen, heating to 30-60 ℃, then dropwise adding propylene oxide, controlling the temperature and the dropwise adding speed during dropwise adding, heating to 70-100 ℃ after dropwise adding, preserving heat for 1-3 hours, cooling to below 40 ℃, adding ammonia water for neutralization, standing overnight, and removing the solvent and unreacted propylene oxide through filtration and reduced pressure distillation to obtain the modified polyether polyol.
As a preferable technical scheme of the invention, the molar ratio of the propylene oxide to the polyhydric alcohol is (5-7): 1.
as a preferable technical scheme of the invention, the mass ratio of the solvent to the polyhydric alcohol is (2-3): 1.
in a preferred embodiment of the present invention, the polyol is at least one selected from the group consisting of ethylene glycol, diethylene glycol, triethylene glycol, propylene glycol, trimethylolpropane and tris (2-hydroxyethyl) isocyanurate.
As a preferable technical scheme, the corrosion inhibitor is at least one selected from sodium polyacrylate, benzotriazole, tolyltriazole, sodium nitrite and potassium nitrite.
The second aspect of the present invention provides the method for preparing the synthetic brake fluid, comprising the steps of: sequentially adding triethylene glycol methyl ether borate, polyglycol ether and polyether polyol into a reaction container according to the parts by weight, stirring, mixing and dehydrating; then adding an anti-aging agent, a corrosion inhibitor and a pH regulator into the mixture in sequence, stirring and mixing, and dehydrating to obtain the synthetic brake fluid.
Has the advantages that: the invention provides a synthetic brake fluid, which is prepared by adding modified polyether glycol prepared by a specific method and a corrosion inhibitor with specific components and proportion into the brake fluid, so that the low-temperature fluidity of the brake fluid is improved, the high-temperature air resistance of the brake fluid is not influenced, the circulating stability of the brake fluid is enhanced, and an automobile can still keep better braking performance after frequent braking.
Detailed Description
The disclosure may be understood more readily by reference to the following detailed description of preferred embodiments of the invention and the examples included therein. 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, including definitions, will control.
The terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, process, 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, process, method, article, or apparatus.
When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or as a range 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 a range of "1 to 5" is disclosed, the described range should be interpreted to include the ranges "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.
In addition, the indefinite articles "a" and "an" preceding an element or component of the invention are not intended to limit the number requirement (i.e., the number of occurrences) of the element or component. Thus, "a" or "an" should be read to include one or at least one, and the singular form of an element or component also includes the plural unless the stated number clearly indicates that the singular form is intended.
In order to solve the technical problems, the invention provides a synthetic brake fluid, which comprises, by weight, 45-75 parts of triethylene glycol methyl ether borate, 10-30 parts of polyethylene glycol ether, 3-15 parts of polyether polyol, 0.5-3 parts of an anti-aging agent, 0.3-1.5 parts of a pH regulator and 0.1-1.0 part of a corrosion inhibitor.
In a preferred embodiment, the brake fluid comprises, by weight, 60-70 parts of triethylene glycol methyl ether borate, 14-25 parts of polyethylene glycol ether, 7-12 parts of polyether polyol, 1.5-2.5 parts of an anti-aging agent, 0.8-1.2 parts of a pH regulator, and 0.5-0.8 part of a corrosion inhibitor.
In a more preferred embodiment, the brake fluid comprises, by weight, 63 parts of triethylene glycol methyl ether borate, 17 parts of polyethylene glycol ether, 10 parts of polyether polyol, 2 parts of an anti-aging agent, 0.9 part of a pH regulator and 0.7 part of a corrosion inhibitor.
The triethylene glycol methyl ether borate ester in the present invention is not particularly limited and may be obtained commercially, for example, commercially available products including, but not limited to, products available from Jiangsu Tianyin chemical industries, Ltd.
In some embodiments, the polyethylene glycol ether is selected from at least one of diethylene glycol methyl ether, triethylene glycol methyl ether, diethylene glycol ethyl ether, triethylene glycol ethyl ether, diethylene glycol butyl ether, triethylene glycol butyl ether; preferably, the polyethylene glycol ether is triethylene glycol butyl ether.
In some embodiments, the polyether polyol is a modified polyether polyol, and the method of making comprises the steps of:
adding a solvent into a reaction container, adding polyol while stirring, then adding a catalyst, introducing nitrogen, heating to 30-60 ℃, then dropwise adding propylene oxide, controlling the temperature and the dropwise adding speed during dropwise adding, heating to 70-100 ℃ after dropwise adding, preserving heat for 1-3 hours, cooling to below 40 ℃, adding ammonia water for neutralization, standing overnight, and removing the solvent and unreacted propylene oxide through filtration and reduced pressure distillation to obtain the modified polyether polyol.
In a preferred embodiment, the polyether polyol is a modified polyether polyol, and the preparation method comprises the following steps:
adding a solvent into a reaction container, adding polyol while stirring, adding a catalyst, introducing nitrogen, heating to 45 ℃, then dropwise adding propylene oxide, controlling the temperature to be kept below 50 ℃ when dropwise adding is carried out, controlling the dropwise adding speed, after dropwise adding is finished for 5-6 hours, heating to 80 ℃, preserving heat for 2 hours, cooling to below 40 ℃, adding ammonia water for neutralization, standing overnight, and removing the solvent and unreacted propylene oxide through filtration and reduced pressure distillation to obtain the modified polyether polyol.
In the present invention, the solvent is toluene and the catalyst is Double Metal Cyanide (DMC).
In some embodiments, the molar ratio of propylene oxide to polyol is (5-7): 1; preferably, the molar ratio of propylene oxide to polyol is 6: 1.
in some embodiments, the mass ratio of the solvent to the polyol is (2-3): 1; preferably, the mass ratio of the solvent to the polyol is 2.5: 1.
in some embodiments, the polyol is selected from at least one of ethylene glycol, diethylene glycol, triethylene glycol, propylene glycol, trimethylolpropane, tris (2-hydroxyethyl) isocyanurate; preferably, the polyol is tris (2-hydroxyethyl) isocyanurate with a CAS number of 839-90-7.
The applicant has surprisingly found that when a conventional polyether polyol, such as polypropylene glycol, is added into brake fluid, although the low-temperature fluidity and the compatibility with rubber of the brake fluid can be improved, the high-temperature gas resistance is reduced, but if the modified polyether polyol prepared by the method for preparing the modified polyether polyol according to the present invention is added into the brake fluid, the low-temperature fluidity of the brake fluid is better, and the high-temperature gas resistance is not affected, presumably because long-chain alkyl alcohol and stable five-membered nitrogen ring are introduced into the molecular structure of the polyether polyol, the steric hindrance effect and the electronic effect of carbon nitrogen heterocycle are utilized, and the hydroxyl value and the viscosity of the modified polyether polyol are controlled by regulating and controlling the molar ratio of propylene oxide and the polyol in the synthesis process of the modified polyether polyol, so as to improve the low-temperature stability of the brake fluid, and ensures excellent high-temperature air resistance of the brake fluid.
In some embodiments, the corrosion inhibitor is selected from at least one of sodium polyacrylate, benzotriazole, methyl benzotriazole, sodium nitrite, and potassium nitrite; preferably, the corrosion inhibitor is a mixture of sodium polyacrylate and sodium nitrite, and the weight ratio of the sodium polyacrylate to the sodium nitrite is 0.03: 1, the weight average molecular weight of the sodium polyacrylate is 1000-2000. The sodium polyacrylate of the present invention can be obtained commercially, for example, commercially available sodium polyacrylate includes but is not limited to those obtained from Yuan Shuo Fine Chemicals, Inc. of Suzhou, having a molecular weight of 1000 to 2000.
The applicant unexpectedly found that when a mixture of sodium polyacrylate and sodium nitrite is used as a corrosion inhibitor, the stability of the brake fluid can be obviously improved, and the precipitation phenomenon can not occur after long-term use. The reason is presumed to be that sodium polyacrylate is a linear soluble high molecular compound, the molecular chain of the sodium polyacrylate stretches due to electrostatic repulsion, a functional group with adsorbability is formed on the surface of the sodium polyacrylate, and the compatibility and stability of base liquid, diluent and additives in a system are enhanced by utilizing the steric hindrance effect and the solvation effect of the sodium polyacrylate. However, sodium polyacrylate has strong hydrophilic groups, and the length of a molecular chain influences the fluidity of the brake fluid, so that the weight ratio of the sodium polyacrylate to the sodium nitrite is limited to 0.03: 1, the weight average molecular weight of the sodium polyacrylate is 1000-2000.
The antioxidant of the present invention is not particularly limited, and includes, but is not limited to, bisphenol A, 2, 6-di-tert-butyl-p-cresol, N', N-diphenyl-p-phenylenediamine, benzotriazole, and N-tert-alkyl benzotriazole.
The pH regulator is not particularly limited in the present invention, and includes, but is not limited to, dibutylamine, triethanolamine, and diethanolamine.
The second aspect of the present invention provides a method for preparing the synthetic brake fluid, comprising the steps of: sequentially adding triethylene glycol methyl ether borate, polyglycol ether and polyether polyol into a reaction container according to the parts by weight, stirring, mixing and dehydrating; and then sequentially adding an anti-aging agent, a corrosion inhibitor and a pH regulator into the mixture according to the parts by weight, stirring, mixing and dehydrating to obtain the synthetic brake fluid.
Examples
Example 1
The embodiment provides a synthetic brake fluid, which comprises the following raw materials, by weight, 63 parts of triethylene glycol methyl ether borate, 17 parts of butyl ether triethylene glycol, 10 parts of polyether polyol, 2 parts of bisphenol A, 0.9 part of triethanolamine and 0.7 part of a corrosion inhibitor;
the preparation method of the polyether polyol comprises the following steps: adding toluene into a reaction container, adding tris (2-hydroxyethyl) isocyanurate under stirring, then adding double metal cyanide, introducing nitrogen, heating to 45 ℃, then dropwise adding propylene oxide, controlling the temperature to be kept below 50 ℃ during dropwise adding and the dropwise adding speed, after 5-6 h of dropwise adding is finished, heating to 80 ℃, keeping the temperature for 2h, cooling to below 40 ℃, adding ammonia water for neutralization, standing overnight, filtering, and distilling under reduced pressure to remove a solvent and unreacted propylene oxide, thus obtaining the modified polyether polyol, wherein the molar ratio of the propylene oxide to the tris (2-hydroxyethyl) isocyanurate is 6: 1, the mass ratio of toluene to tris (2-hydroxyethyl) isocyanurate is 2.5: 1; the mass ratio of the corrosion inhibitor is 0.03: 1 of a mixture of sodium polyacrylate and sodium nitrite.
The invention also provides a preparation method of the synthetic brake fluid, which comprises the following steps: sequentially adding triethylene glycol methyl ether borate, polyglycol ether and polyether polyol into a reaction container according to the parts by weight, stirring, mixing and dehydrating; and then sequentially adding an anti-aging agent, a corrosion inhibitor and a pH regulator into the mixture according to the parts by weight, stirring, mixing and dehydrating to obtain the synthetic brake fluid.
Example 2
The embodiment provides a synthetic brake fluid, which comprises the following raw materials, by weight, 45 parts of triethylene glycol methyl ether borate, 10 parts of butyl ether triethylene glycol, 3 parts of polyether polyol, 0.5 part of bisphenol A, 0.3 part of triethanolamine and 0.1 part of a corrosion inhibitor;
the preparation method of the polyether polyol comprises the following steps: adding toluene into a reaction container, adding tris (2-hydroxyethyl) isocyanurate under stirring, then adding double metal cyanide, introducing nitrogen, heating to 45 ℃, then dropwise adding propylene oxide, controlling the temperature to be kept below 50 ℃ during dropwise adding and the dropwise adding speed, after 5-6 h of dropwise adding is finished, heating to 80 ℃, keeping the temperature for 2h, cooling to below 40 ℃, adding ammonia water for neutralization, standing overnight, filtering, and distilling under reduced pressure to remove a solvent and unreacted propylene oxide, thus obtaining the modified polyether polyol, wherein the molar ratio of the propylene oxide to the tris (2-hydroxyethyl) isocyanurate is 6: 1, the mass ratio of toluene to tris (2-hydroxyethyl) isocyanurate is 2.5: 1; the mass ratio of the corrosion inhibitor is 0.03: 1 of a mixture of sodium polyacrylate and sodium nitrite.
The invention also provides a preparation method of the synthetic brake fluid, which comprises the following steps: sequentially adding triethylene glycol methyl ether borate, polyglycol ether and polyether polyol into a reaction container according to the parts by weight, stirring, mixing and dehydrating; and then sequentially adding an anti-aging agent, a corrosion inhibitor and a pH regulator into the mixture according to the parts by weight, stirring, mixing and dehydrating to obtain the synthetic brake fluid.
Example 3
The embodiment provides a synthetic brake fluid, which comprises the following raw materials, by weight, 63 parts of triethylene glycol methyl ether borate, 17 parts of butyl ether triethylene glycol, 10 parts of polyether polyol, 2 parts of bisphenol A, 0.9 part of triethanolamine and 0.7 part of a corrosion inhibitor;
wherein the polyether glycol is polypropylene glycol, is purchased from Haian petrochemical plants in Jiangsu province, and has the molecular weight of 900-1100; the mass ratio of the corrosion inhibitor is 0.03: 1 of a mixture of sodium polyacrylate and sodium nitrite.
The invention also provides a preparation method of the synthetic brake fluid, which comprises the following steps: sequentially adding triethylene glycol methyl ether borate, polyglycol ether and polyether polyol into a reaction container according to the parts by weight, stirring, mixing and dehydrating; and then sequentially adding an anti-aging agent, a corrosion inhibitor and a pH regulator into the mixture according to the parts by weight, stirring, mixing and dehydrating to obtain the synthetic brake fluid.
Example 4
The embodiment provides a synthetic brake fluid, which comprises the following raw materials, by weight, 63 parts of triethylene glycol methyl ether borate, 17 parts of butyl ether triethylene glycol, 10 parts of polyether polyol, 2 parts of bisphenol A, 0.9 part of triethanolamine and 0.7 part of a corrosion inhibitor;
the preparation method of the polyether polyol comprises the following steps: adding toluene into a reaction container, adding tris (2-hydroxyethyl) isocyanurate under stirring, then adding double metal cyanide, introducing nitrogen, heating to 45 ℃, then dropwise adding propylene oxide, controlling the temperature to be kept below 50 ℃ during dropwise adding and the dropwise adding speed, after 5-6 h of dropwise adding is finished, heating to 80 ℃, keeping the temperature for 2h, cooling to below 40 ℃, adding ammonia water for neutralization, standing overnight, filtering, and distilling under reduced pressure to remove a solvent and unreacted propylene oxide, thus obtaining the modified polyether polyol, wherein the molar ratio of the propylene oxide to the tris (2-hydroxyethyl) isocyanurate is 4: 1, the mass ratio of toluene to tris (2-hydroxyethyl) isocyanurate is 2.5: 1; the mass ratio of the corrosion inhibitor is 0.03: 1 of a mixture of sodium polyacrylate and sodium nitrite.
The invention also provides a preparation method of the synthetic brake fluid, which comprises the following steps: sequentially adding triethylene glycol methyl ether borate, polyglycol ether and polyether polyol into a reaction container according to the parts by weight, stirring, mixing and dehydrating; and then sequentially adding an anti-aging agent, a corrosion inhibitor and a pH regulator into the mixture according to the parts by weight, stirring, mixing and dehydrating to obtain the synthetic brake fluid.
Example 5
The embodiment provides a synthetic brake fluid, which comprises the following raw materials, by weight, 63 parts of triethylene glycol methyl ether borate, 17 parts of butyl ether triethylene glycol, 10 parts of polyether polyol, 2 parts of bisphenol A, 0.9 part of triethanolamine and 0.7 part of a corrosion inhibitor;
the preparation method of the polyether polyol comprises the following steps: adding toluene into a reaction container, adding tris (2-hydroxyethyl) isocyanurate under stirring, then adding double metal cyanide, introducing nitrogen, heating to 45 ℃, then dropwise adding propylene oxide, controlling the temperature to be kept below 50 ℃ during dropwise adding and the dropwise adding speed, after 5-6 h of dropwise adding is finished, heating to 80 ℃, keeping the temperature for 2h, cooling to below 40 ℃, adding ammonia water for neutralization, standing overnight, filtering, and distilling under reduced pressure to remove a solvent and unreacted propylene oxide, thus obtaining the modified polyether polyol, wherein the molar ratio of the propylene oxide to the tris (2-hydroxyethyl) isocyanurate is 8: 1, the mass ratio of toluene to tris (2-hydroxyethyl) isocyanurate is 2.5: 1; the mass ratio of the corrosion inhibitor is 0.03: 1 of a mixture of sodium polyacrylate and sodium nitrite.
The invention also provides a preparation method of the synthetic brake fluid, which comprises the following steps: sequentially adding triethylene glycol methyl ether borate, polyglycol ether and polyether polyol into a reaction container according to the parts by weight, stirring, mixing and dehydrating; and then sequentially adding an anti-aging agent, a corrosion inhibitor and a pH regulator into the mixture according to the parts by weight, stirring, mixing and dehydrating to obtain the synthetic brake fluid.
Example 6
The embodiment provides a synthetic brake fluid, which comprises the following raw materials, by weight, 63 parts of triethylene glycol methyl ether borate, 17 parts of butyl ether triethylene glycol, 10 parts of polyether polyol, 2 parts of bisphenol A, 0.9 part of triethanolamine and 0.7 part of a corrosion inhibitor;
the preparation method of the polyether polyol comprises the following steps: adding toluene into a reaction container, adding triethylene glycol under stirring, adding double metal cyanide, introducing nitrogen, heating to 45 ℃, then dropwise adding propylene oxide, controlling the temperature to be below 50 ℃ when dropwise adding is carried out, controlling the dropwise adding speed, after 5-6 h of dropwise adding is finished, heating to 80 ℃, keeping the temperature for 2h, cooling to below 40 ℃, adding ammonia water for neutralization, standing overnight, and removing a solvent and unreacted propylene oxide through filtration and reduced pressure distillation to obtain the modified polyether polyol, wherein the molar ratio of the propylene oxide to the triethylene glycol is 6: 1, the mass ratio of toluene to triethylene glycol is 2.5: 1; the mass ratio of the corrosion inhibitor is 0.03: 1 of a mixture of sodium polyacrylate and sodium nitrite.
The invention also provides a preparation method of the synthetic brake fluid, which comprises the following steps: sequentially adding triethylene glycol methyl ether borate, polyglycol ether and polyether polyol into a reaction container according to the parts by weight, stirring, mixing and dehydrating; and then sequentially adding an anti-aging agent, a corrosion inhibitor and a pH regulator into the mixture according to the parts by weight, stirring, mixing and dehydrating to obtain the synthetic brake fluid.
Example 7
The embodiment provides a synthetic brake fluid, which comprises the following raw materials, by weight, 63 parts of triethylene glycol methyl ether borate, 17 parts of butyl ether triethylene glycol, 10 parts of polyether polyol, 2 parts of bisphenol A, 0.9 part of triethanolamine and 0.7 part of a corrosion inhibitor;
the preparation method of the polyether polyol comprises the following steps: adding toluene into a reaction container, adding tris (2-hydroxyethyl) isocyanurate under stirring, then adding double metal cyanide, introducing nitrogen, heating to 45 ℃, then dropwise adding propylene oxide, controlling the temperature to be kept below 50 ℃ during dropwise adding and the dropwise adding speed, after 5-6 h of dropwise adding is finished, heating to 80 ℃, keeping the temperature for 2h, cooling to below 40 ℃, adding ammonia water for neutralization, standing overnight, filtering, and distilling under reduced pressure to remove a solvent and unreacted propylene oxide, thus obtaining the modified polyether polyol, wherein the molar ratio of the propylene oxide to the tris (2-hydroxyethyl) isocyanurate is 6: 1, the mass ratio of toluene to tris (2-hydroxyethyl) isocyanurate is 1.5: 1; the mass ratio of the corrosion inhibitor is 0.03: 1 of a mixture of sodium polyacrylate and sodium nitrite.
The invention also provides a preparation method of the synthetic brake fluid, which comprises the following steps: sequentially adding triethylene glycol methyl ether borate, polyglycol ether and polyether polyol into a reaction container according to the parts by weight, stirring, mixing and dehydrating; and then sequentially adding an anti-aging agent, a corrosion inhibitor and a pH regulator into the mixture according to the parts by weight, stirring, mixing and dehydrating to obtain the synthetic brake fluid.
Example 8
The embodiment provides a synthetic brake fluid, which comprises the following raw materials, by weight, 63 parts of triethylene glycol methyl ether borate, 17 parts of butyl ether triethylene glycol, 10 parts of polyether polyol, 2 parts of bisphenol A, 0.9 part of triethanolamine and 0.7 part of a corrosion inhibitor;
the preparation method of the polyether polyol comprises the following steps: adding toluene into a reaction container, adding tris (2-hydroxyethyl) isocyanurate under stirring, then adding double metal cyanide, introducing nitrogen, heating to 45 ℃, then dropwise adding propylene oxide, controlling the temperature to be kept below 50 ℃ during dropwise adding and the dropwise adding speed, after 5-6 h of dropwise adding is finished, heating to 80 ℃, keeping the temperature for 2h, cooling to below 40 ℃, adding ammonia water for neutralization, standing overnight, filtering, and distilling under reduced pressure to remove a solvent and unreacted propylene oxide, thus obtaining the modified polyether polyol, wherein the molar ratio of the propylene oxide to the tris (2-hydroxyethyl) isocyanurate is 6: 1, the mass ratio of toluene to tris (2-hydroxyethyl) isocyanurate is 4: 1; the mass ratio of the corrosion inhibitor is 0.03: 1 of a mixture of sodium polyacrylate and sodium nitrite.
The invention also provides a preparation method of the synthetic brake fluid, which comprises the following steps: sequentially adding triethylene glycol methyl ether borate, polyglycol ether and polyether polyol into a reaction container according to the parts by weight, stirring, mixing and dehydrating; and then sequentially adding an anti-aging agent, a corrosion inhibitor and a pH regulator into the mixture according to the parts by weight, stirring, mixing and dehydrating to obtain the synthetic brake fluid.
Example 9
The embodiment provides a synthetic brake fluid, which comprises the following raw materials, by weight, 63 parts of triethylene glycol methyl ether borate, 17 parts of butyl ether triethylene glycol, 10 parts of polyether polyol, 2 parts of bisphenol A, 0.9 part of triethanolamine and 0.7 part of a corrosion inhibitor;
the preparation method of the polyether polyol comprises the following steps: adding toluene into a reaction container, adding tris (2-hydroxyethyl) isocyanurate under stirring, then adding double metal cyanide, introducing nitrogen, heating to 45 ℃, then dropwise adding propylene oxide, controlling the temperature to be kept below 50 ℃ during dropwise adding and the dropwise adding speed, after 5-6 h of dropwise adding is finished, heating to 80 ℃, keeping the temperature for 2h, cooling to below 40 ℃, adding ammonia water for neutralization, standing overnight, filtering, and distilling under reduced pressure to remove a solvent and unreacted propylene oxide, thus obtaining the modified polyether polyol, wherein the molar ratio of the propylene oxide to the tris (2-hydroxyethyl) isocyanurate is 6: 1, the mass ratio of toluene to tris (2-hydroxyethyl) isocyanurate is 2.5: 1; the corrosion inhibitor is sodium nitrite.
The invention also provides a preparation method of the synthetic brake fluid, which comprises the following steps: sequentially adding triethylene glycol methyl ether borate, polyglycol ether and polyether polyol into a reaction container according to the parts by weight, stirring, mixing and dehydrating; and then sequentially adding an anti-aging agent, a corrosion inhibitor and a pH regulator into the mixture according to the parts by weight, stirring, mixing and dehydrating to obtain the synthetic brake fluid.
Example 10
The embodiment provides a synthetic brake fluid, which comprises the following raw materials, by weight, 63 parts of triethylene glycol methyl ether borate, 17 parts of butyl ether triethylene glycol, 10 parts of polyether polyol, 2 parts of bisphenol A, 0.9 part of triethanolamine and 0.7 part of a corrosion inhibitor;
the preparation method of the polyether polyol comprises the following steps: adding toluene into a reaction container, adding tris (2-hydroxyethyl) isocyanurate under stirring, then adding double metal cyanide, introducing nitrogen, heating to 45 ℃, then dropwise adding propylene oxide, controlling the temperature to be kept below 50 ℃ during dropwise adding and the dropwise adding speed, after 5-6 h of dropwise adding is finished, heating to 80 ℃, keeping the temperature for 2h, cooling to below 40 ℃, adding ammonia water for neutralization, standing overnight, filtering, and distilling under reduced pressure to remove a solvent and unreacted propylene oxide, thus obtaining the modified polyether polyol, wherein the molar ratio of the propylene oxide to the tris (2-hydroxyethyl) isocyanurate is 6: 1, the mass ratio of toluene to tris (2-hydroxyethyl) isocyanurate is 2.5: 1; the corrosion inhibitor is prepared from the following components in a mass ratio of 1: 1 of a mixture of sodium polyacrylate and sodium nitrite.
The invention also provides a preparation method of the synthetic brake fluid, which comprises the following steps: sequentially adding triethylene glycol methyl ether borate, polyglycol ether and polyether polyol into a reaction container according to the parts by weight, stirring, mixing and dehydrating; and then sequentially adding an anti-aging agent, a corrosion inhibitor and a pH regulator into the mixture according to the parts by weight, stirring, mixing and dehydrating to obtain the synthetic brake fluid.
Evaluation of Performance
The equilibrium reflux boiling point, the wet equilibrium reflux boiling point, the low-temperature fluidity and the appearance of the brake fluid obtained in the examples of the present invention were measured according to the method disclosed in GB12981-2012, and the results are shown in table 1.
The brake fluid was subjected to repeated heating (70 ℃) and cooling (0 ℃) for 20 cycles, wherein the high temperature duration time was 1 hour and the low temperature duration time was 1 hour for each cycle, and then whether the brake fluid precipitated or became turbid was observed to evaluate the cycle stability of the brake fluid, and the results are shown in table 1.
TABLE 1
According to the results in table 1, the synthetic brake fluid provided by the invention has better high-temperature gas resistance, low-temperature fluidity and cycling stability. Specifically, as can be seen from the results of comparative example 1 and examples 2 to 8, the modified polyether polyol prepared by the specific method in the present invention not only improves the low temperature fluidity of the brake fluid, but also does not affect the high temperature air resistance thereof; the results of the comparative example 1 and the examples 9 to 10 show that the corrosion inhibitor with specific components and proportions is introduced, so that the circulation stability of the brake fluid is enhanced on the premise of reducing the corrosion of the brake fluid to metals, and the automobile can still maintain better braking performance after frequent braking.
The foregoing examples are merely illustrative and serve to explain some of the features of the method of the present invention. The appended claims are intended to claim as broad a scope as is contemplated, and the examples presented herein are merely illustrative of selected implementations in accordance with all possible combinations of examples. Accordingly, it is applicants' intention that the appended claims are not to be limited by the choice of examples illustrating features of the invention. Also, where numerical ranges are used in the claims, subranges therein are included, and variations in these ranges are also to be construed as possible being covered by the appended claims.
Claims (10)
1. The synthetic brake fluid is characterized by comprising, by weight, 45-75 parts of triethylene glycol methyl ether borate, 10-30 parts of polyethylene glycol ether, 3-15 parts of polyether polyol, 0.5-3 parts of an anti-aging agent, 0.3-1.5 parts of a pH regulator and 0.1-1.0 part of a corrosion inhibitor.
2. The synthetic brake fluid according to claim 1, wherein the brake fluid comprises, by weight, 60 to 70 parts of triethylene glycol methyl ether borate, 14 to 25 parts of polyethylene glycol ether, 7 to 12 parts of polyether polyol, 1.5 to 2.5 parts of an anti-aging agent, 0.8 to 1.2 parts of a pH regulator, and 0.5 to 0.8 part of a corrosion inhibitor.
3. The synthetic brake fluid according to claim 1, wherein the brake fluid comprises, by weight, 63 parts of triethylene glycol methyl ether borate, 17 parts of polyethylene glycol ether, 10 parts of polyether polyol, 2 parts of an anti-aging agent, 0.9 part of a pH regulator, and 0.7 part of a corrosion inhibitor.
4. The synthetic brake fluid according to claim 1, wherein the polyethylene glycol ether is at least one selected from the group consisting of diethylene glycol methyl ether, triethylene glycol methyl ether, diethylene glycol ethyl ether, triethylene glycol ethyl ether, diethylene glycol butyl ether, and triethylene glycol butyl ether.
5. The synthetic brake fluid of claim 1, wherein the polyether polyol is a modified polyether polyol and the method of making comprises the steps of:
adding a solvent into a reaction container, adding polyol while stirring, then adding a catalyst, introducing nitrogen, heating to 30-60 ℃, then dropwise adding propylene oxide, controlling the temperature and the dropwise adding speed during dropwise adding, heating to 70-100 ℃ after dropwise adding, preserving heat for 1-3 hours, cooling to below 40 ℃, adding ammonia water for neutralization, standing overnight, and removing the solvent and unreacted propylene oxide through filtration and reduced pressure distillation to obtain the modified polyether polyol.
6. The synthetic brake fluid according to claim 5, wherein the molar ratio of propylene oxide to polyol is (5 to 7): 1.
7. the synthetic brake fluid according to claim 5, wherein the mass ratio of the solvent to the polyol is (2-3): 1.
8. the synthetic brake fluid of claim 5, wherein the polyol is selected from at least one of ethylene glycol, diethylene glycol, triethylene glycol, propylene glycol, trimethylolpropane, tris (2-hydroxyethyl) isocyanurate.
9. The synthetic brake fluid of claim 1, wherein the corrosion inhibitor is at least one selected from the group consisting of sodium polyacrylate, benzotriazole, tolyltriazole, sodium nitrite, and potassium nitrite.
10. The method for preparing a synthetic brake fluid according to any one of claims 1 to 9, comprising the steps of: sequentially adding triethylene glycol methyl ether borate, polyglycol ether and polyether polyol into a reaction container according to the parts by weight, stirring, mixing and dehydrating; then adding an anti-aging agent, a corrosion inhibitor and a pH regulator into the mixture in sequence, stirring and mixing, and dehydrating to obtain the synthetic brake fluid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911354596.4A CN111100727A (en) | 2019-12-25 | 2019-12-25 | Synthetic brake fluid and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911354596.4A CN111100727A (en) | 2019-12-25 | 2019-12-25 | Synthetic brake fluid and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111961521A (en) * | 2020-08-28 | 2020-11-20 | 上海中孚特种油品有限公司 | Ultralow-low-temperature-viscosity borate type synthetic brake fluid and preparation method thereof |
| CN113122357A (en) * | 2021-04-19 | 2021-07-16 | 中国石油化工股份有限公司 | Motor vehicle brake fluid composition and preparation method thereof |
| CN114058425A (en) * | 2020-08-03 | 2022-02-18 | 北京蓝星清洗有限公司 | Motor vehicle brake fluid and preparation method thereof |
| CN116042290A (en) * | 2022-09-29 | 2023-05-02 | 上海本牧实业有限公司 | Flame-retardant stable borate brake fluid and preparation method thereof |
-
2019
- 2019-12-25 CN CN201911354596.4A patent/CN111100727A/en not_active Withdrawn
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114058425A (en) * | 2020-08-03 | 2022-02-18 | 北京蓝星清洗有限公司 | Motor vehicle brake fluid and preparation method thereof |
| CN111961521A (en) * | 2020-08-28 | 2020-11-20 | 上海中孚特种油品有限公司 | Ultralow-low-temperature-viscosity borate type synthetic brake fluid and preparation method thereof |
| CN113122357A (en) * | 2021-04-19 | 2021-07-16 | 中国石油化工股份有限公司 | Motor vehicle brake fluid composition and preparation method thereof |
| CN116042290A (en) * | 2022-09-29 | 2023-05-02 | 上海本牧实业有限公司 | Flame-retardant stable borate brake fluid and preparation method thereof |
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