CN111303961A - Recycled ester, preparation method thereof and application thereof in preparation of HZY3 brake fluid - Google Patents
Recycled ester, preparation method thereof and application thereof in preparation of HZY3 brake fluid Download PDFInfo
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- CN111303961A CN111303961A CN202010257366.2A CN202010257366A CN111303961A CN 111303961 A CN111303961 A CN 111303961A CN 202010257366 A CN202010257366 A CN 202010257366A CN 111303961 A CN111303961 A CN 111303961A
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- brake fluid
- hzy3
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- 239000012530 fluid Substances 0.000 title claims abstract description 66
- 150000002148 esters Chemical class 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 11
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 9
- 239000004327 boric acid Substances 0.000 claims abstract description 7
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 6
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 claims abstract description 6
- 230000035484 reaction time Effects 0.000 claims abstract description 4
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 44
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 40
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 40
- -1 polyoxypropylene Polymers 0.000 claims description 27
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 claims description 24
- 229920001451 polypropylene glycol Polymers 0.000 claims description 22
- ZUHZGEOKBKGPSW-UHFFFAOYSA-N tetraglyme Chemical compound COCCOCCOCCOCCOC ZUHZGEOKBKGPSW-UHFFFAOYSA-N 0.000 claims description 22
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims description 14
- 239000002202 Polyethylene glycol Substances 0.000 claims description 14
- 229920001223 polyethylene glycol Polymers 0.000 claims description 14
- 235000010288 sodium nitrite Nutrition 0.000 claims description 12
- COBPKKZHLDDMTB-UHFFFAOYSA-N 2-[2-(2-butoxyethoxy)ethoxy]ethanol Chemical compound CCCCOCCOCCOCCO COBPKKZHLDDMTB-UHFFFAOYSA-N 0.000 claims description 11
- CMGDVUCDZOBDNL-UHFFFAOYSA-N 4-methyl-2h-benzotriazole Chemical compound CC1=CC=CC2=NNN=C12 CMGDVUCDZOBDNL-UHFFFAOYSA-N 0.000 claims description 11
- PTRSTXBRQVXIEW-UHFFFAOYSA-N n,n-dioctylaniline Chemical compound CCCCCCCCN(CCCCCCCC)C1=CC=CC=C1 PTRSTXBRQVXIEW-UHFFFAOYSA-N 0.000 claims description 11
- 230000032050 esterification Effects 0.000 claims description 10
- 238000005886 esterification reaction Methods 0.000 claims description 10
- WPMYUUITDBHVQZ-UHFFFAOYSA-N 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoic acid Chemical compound CC(C)(C)C1=CC(CCC(O)=O)=CC(C(C)(C)C)=C1O WPMYUUITDBHVQZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000009835 boiling Methods 0.000 claims description 8
- 238000011084 recovery Methods 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 6
- LVTYICIALWPMFW-UHFFFAOYSA-N diisopropanolamine Chemical compound CC(O)CNCC(C)O LVTYICIALWPMFW-UHFFFAOYSA-N 0.000 claims description 5
- 229940043276 diisopropanolamine Drugs 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 claims description 3
- 125000005233 alkylalcohol group Chemical group 0.000 claims description 3
- NFHFRUOZVGFOOS-UHFFFAOYSA-N palladium;triphenylphosphane Chemical compound [Pd].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 NFHFRUOZVGFOOS-UHFFFAOYSA-N 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- HXKKHQJGJAFBHI-UHFFFAOYSA-N 1-aminopropan-2-ol Chemical group CC(O)CN HXKKHQJGJAFBHI-UHFFFAOYSA-N 0.000 claims description 2
- 239000004593 Epoxy Substances 0.000 claims description 2
- 238000007259 addition reaction Methods 0.000 claims description 2
- 150000001412 amines Chemical class 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 11
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 description 11
- 238000005516 engineering process Methods 0.000 description 9
- 230000007797 corrosion Effects 0.000 description 7
- 238000005260 corrosion Methods 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 239000000126 substance Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- 239000000654 additive Substances 0.000 description 2
- SCYULBFZEHDVBN-UHFFFAOYSA-N 1,1-Dichloroethane Chemical compound CC(Cl)Cl SCYULBFZEHDVBN-UHFFFAOYSA-N 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 229920002959 polymer blend Polymers 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M139/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing atoms of elements not provided for in groups C10M127/00 - C10M137/00
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F5/00—Compounds containing elements of Groups 3 or 13 of the Periodic Table
- C07F5/02—Boron compounds
- C07F5/04—Esters of boric acids
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M161/00—Lubricating compositions characterised by the additive being a mixture of a macromolecular compound and a non-macromolecular compound, each of these compounds being essential
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/08—Inorganic acids or salts thereof
- C10M2201/082—Inorganic acids or salts thereof containing nitrogen
- C10M2201/083—Inorganic acids or salts thereof containing nitrogen nitrites
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- 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
- C10M2207/024—Hydroxy compounds having hydroxy groups bound to carbon atoms of six-membered aromatic rings having at least two phenol groups but no condensed ring
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- 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
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- 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
- C10M2207/046—Hydroxy ethers
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/28—Esters
- C10M2207/283—Esters of polyhydroxy compounds
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- 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
- C10M2209/105—Polyethers, i.e. containing di- or higher polyoxyalkylene groups of alkylene oxides containing three carbon atoms only
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- 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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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2215/02—Amines, e.g. polyalkylene polyamines; Quaternary amines
- C10M2215/06—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to carbon atoms of six-membered aromatic rings
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2215/00—Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2215/22—Heterocyclic nitrogen compounds
- C10M2215/223—Five-membered rings containing nitrogen and carbon only
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- 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
- C10M2227/06—Organic compounds derived from inorganic acids or metal salts
- C10M2227/061—Esters derived from boron
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Lubricants (AREA)
Abstract
The invention relates to a recycled ester, a preparation method thereof and application thereof in preparing HZY3 brake fluid, wherein the preparation steps of the recycled ester are as follows: adding boric acid, phosphorous acid and high vacuum recovered materials into a reaction kettle according to the mass ratio of 1: 0.0005: 18, performing dehydration reaction under the conditions that the vacuum degree is 0.060-0.065Mpa and the temperature is 140-; carrying out micro dehydration reaction under the conditions that the vacuum degree is more than or equal to 0.096Mpa and the temperature is 155-180 ℃, controlling the reaction time to be more than or equal to 24 hours, and obtaining the recovered ester after the reaction is finished. The preparation process of the recycled ester utilizes high vacuum recycled materials, so that the production cost of the brake fluid can be reduced, and the environment can be protected.
Description
Technical Field
The invention relates to the technical field of brake fluid of an automobile brake system, in particular to recycled ester, a preparation method of the recycled ester and application of the recycled ester in preparation of HZY3 brake fluid.
Background
Currently, the mainstream products in the world are brake fluids of HZY3, HZY4 and HZY5 types which take alcohol ether borate as a main raw material, and synthetic brake fluids of HZY3 and HZY4 borate types are widely applied in the world. The HZY5 type brake fluid is used in a small amount mainly due to its high price. At present, the retail market still widely takes HZY3 level brake fluid as a main material, most of HZY3 brake fluid is prepared by taking alcohol ether as a main material, the brake fluid has the defect of strong hygroscopicity widely, and the brake fluid is easy to absorb moisture after being added, so that great potential safety hazards are brought.
The brake fluid is a working medium for transmitting pressure in hydraulic transmission, and the performance of the brake fluid is directly related to the safety of people's lives and properties, so that the national requirements on the quality of the brake fluid of the automobile are strict. In China, the quality level of the current automobile brake fluid product can meet the use requirements of various vehicles, and in terms of the prior art, the borate brake fluid technology becomes an essential technology of a high-performance borate brake fluid product. In the patent technology and literature published in the state of recent years, many reports and researches about borate technology are already available, and some reports and researches about HZY5 and HZY6 brake fluid production technology are available, but the reports and researches mainly focus on formulation technology, and borate serving as a main raw material of brake fluid is rarely specially reported, and particularly, the treatment of recycled materials in the process of producing borate is not mentioned. The boric acid ester is mainly subjected to dehydration chemical combination reaction in the production process, the recovered substance in the low vacuum stage is mainly water, has no utilization value and is mostly treated as dangerous waste, while the recovered substance in the high vacuum stage contains more alcohol ether, and if the recovered substance is treated as the dangerous waste, the waste is caused and extra treatment cost is increased.
A2002 Chinese patent with 00130831.9 application number discloses an automobile brake fluid and a manufacturing method thereof, boric anhydride, polyethylene glycol methyl ether, diethylene glycol and additives are put into the automobile brake fluid at one time, the automobile brake fluid reacts for 3 to 4 hours under 2 to 3 atmospheric pressures, and brake fluid finished products are obtained through cooling and filtering.
Chinese patent No. 200310112132.5, 2003, discloses a borate brake fluid and a method for preparing the same, which describes the production and manufacturing method of borate brake fluid, but this technology uses diethylene glycol as a main raw material for preparing borate, and thus meets the requirement of HZY3 grade index, but does not mention the treatment scheme of the recycled product after esterification.
The 2003 Chinese patent with application number 03111223.4 discloses a brake fluid for motor vehicles and a production method thereof, which describes a method for producing brake fluid by using polymer mixture produced by diethylene glycol and 1, 1-dichloroethane under the action of a catalyst, and the patent gives technical indexes for preparing HZY4 brake fluid, but does not relate to recycling of high vacuum recyclates.
Disclosure of Invention
The technical problem to be solved is as follows: aiming at the situation that the recycling of high vacuum recovery materials in the preparation process of automobile brake fluid is not involved in the prior art, the invention provides a recovered ester, a preparation method thereof and application thereof in the preparation of HZY3 brake fluid, wherein the high vacuum recovery materials are utilized in the preparation process of the recovered ester, so that the production cost of the brake fluid can be reduced, the environment can be protected, and the HZY3 brake fluid produced by utilizing the formula technology can meet the experimental requirements of rare-moisture resistance and special durable metal corrosion.
The technical scheme is as follows: a preparation method of a recycled ester comprises the following preparation steps:
(1) low vacuum esterification stage: adding boric acid, phosphorous acid and high vacuum recovered materials into a reaction kettle according to the mass ratio of 1: 0.0005: 18, performing dehydration reaction under the conditions that the vacuum degree is 0.060-0.065Mpa and the temperature is 140-;
(2) high vacuum esterification stage: carrying out micro-dehydration reaction under the conditions that the vacuum degree is more than or equal to 0.096Mpa and the temperature is 155-180 ℃, controlling the reaction time to be more than or equal to 24 hours, and obtaining recovered ester after the reaction is finished;
wherein the purity of the boric acid is more than or equal to 99.9 percent, the phosphorous acid is of analytical purity grade, and the high vacuum recovery product is a recovery product obtained in a high vacuum stage by a two-step vacuum method after the esterification of alkyl alcohol ether.
A recovered ester prepared according to the above-described preparation method.
The pH value of the recovered ester is more than or equal to 4.5, the water content is less than or equal to 0.15 percent, and the boiling point is more than or equal to 265 ℃.
The application of the recycled ester in preparing HZY3 brake fluid comprises the following components, by mass, 15-25 parts of polyethylene glycol methyl ether, 0.5-5.0 parts of trihydroxy polyoxypropylene ether, 15-50 parts of recycled ester, 10-15 parts of diethylene glycol, 15-35 parts of triethylene glycol monobutyl ether, 5-20 parts of tetraethylene glycol dimethyl ether, 0.2-1.0 part of methylbenzotriazole, 0.2-1.5 parts of dioctylaniline, 0.5-3.0 parts of 2, 2-bis (4-hydroxyphenyl) propane (bisphenol A), 0.5-3.0 parts of tetra [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester, 0.3-1.0 part of polypropylene glycol 2000, 0.005-0.5 part of sodium nitrite, 0.01-0.5 part of sodium nitrite and 0.1-5.0 part of alkalinity regulator.
The HZY3 brake fluid comprises, by mass, 15-20 parts of polyethylene glycol monomethyl ether, 0.5-3.0 parts of trihydroxy polyoxypropylene ether, 30-45 parts of recycled ester, 10-12 parts of diethylene glycol, 15-25 parts of triethylene glycol monobutyl ether, 5-12 parts of tetraethylene glycol dimethyl ether, 0.5-0.8 part of methylbenzotriazole, 0.5-1.0 part of dioctylaniline, 0.5-2.0 parts of 2, 2-bis (4-hydroxyphenyl) propane (bisphenol A), 0.5-1.0 part of tetra [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester, 0.01-0.2 part of polypropylene glycol 2000, 0.01-0.2 part of sodium nitrite and 0.5-3.0 part of alkalinity regulator.
The HZY3 brake fluid comprises, by mass, 15 parts of polyethylene glycol monomethyl ether, 2 parts of trihydroxy polyoxypropylene ether, 45 parts of recovered ester, 10 parts of diethylene glycol, 20 parts of triethylene glycol monobutyl ether, 5 parts of tetraethylene glycol dimethyl ether, 0.8 part of methylbenzotriazole, 1.0 part of dioctylaniline, 1.0 part of 2, 2-bis (4-hydroxyphenyl) propane (bisphenol A), 0.5 part of tetra [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester, 0.02 part of polypropylene glycol 2000, 0.05 part of sodium nitrite and 2.5 parts of alkalinity regulator.
The molecular formula of the polyethylene glycol monomethyl ether is as follows: CH (CH)3(OCH2CH2)nOH, wherein n is more than or equal to 3, and the low-temperature kinematic viscosity is controlled to be less than or equal to 1000mm at the temperature of minus 40 DEG C2/s。
The alkalinity regulator is monoisopropanolamine, diisopropanolamine or alkoxy fatty alcohol cycloalkyl amine, and the alkoxy fatty alcohol cycloalkyl amine is obtained by addition reaction of fatty amine and epoxy compound.
The preparation method of the HZY3 brake fluid comprises the following steps of sequentially adding polyethylene glycol monomethyl ether, trihydroxy polyoxypropylene ether, recovered ester, diethylene glycol, triethylene glycol monobutyl ether, tetraethylene glycol dimethyl ether, methylbenzotriazole, dioctylaniline, 2-bis (4-hydroxyphenyl) propane (bisphenol A), tetra [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester, polypropylene glycol 2000 and sodium nitrite into a 1.5T reaction kettle, adding an alkalinity regulator to adjust the pH value to be more than 7.5, continuously stirring for 4 hours, filtering through a 0.1um filter, and packaging to obtain the HZY3 brake fluid.
Has the advantages that: the recycled ester, the preparation method thereof and the application thereof in preparing HZY3 brake fluid have the following beneficial effects: according to the invention, the recycled ester is prepared from the high-vacuum recycled material, the boiling point of the prepared recycled ester is higher than 265 ℃, and the dry and wet boiling points of the HZY3 brake fluid prepared from the recycled ester are obviously improved, so that the production and treatment costs are reduced, and the environmental pollution caused by the production and treatment costs can be reduced; meanwhile, the HZY3 brake fluid can meet and is higher than the GB12981-2003 requirement, and not only has high dry and wet boiling points, but also has good low-temperature kinematic viscosity; in addition, the special durable metal corrosion performance of the HZY3 brake fluid is prolonged from 120h specified in GB12981-2003 to 240h, the adaptability of the HZY3 brake fluid is greatly improved, and the HZY3 brake fluid is resistant to thin humidity and can meet the requirement of long-term durable use.
Detailed Description
The high vacuum recovery product used in the following examples is a recovery product obtained in the high vacuum stage by the two-step vacuum method after esterification of alkyl alcohol ether, and contains a high content of low boiling point alcohol ether and high boiling point alcohol ether which is not completely reacted, and the product in the low vacuum stage by the two-step method has low content of effective component alcohol ether, so that the product has no recycling value and is used as wastewater treatment.
Example 1
Firstly, preparing the recovered ester, wherein the preparation steps are as follows:
(1) low vacuum esterification stage: 100kg of boric acid with the purity of more than or equal to 99.9 percent, 0.05kg of phosphorous acid of analytical pure grade and 1800kg of high-vacuum recovered materials are added into a reaction kettle, dehydration reaction is carried out under the conditions that the vacuum degree is 0.060-0.065Mpa and the temperature is 140-;
(2) high vacuum esterification stage: carrying out micro dehydration reaction under the conditions that the vacuum degree is more than or equal to 0.096Mpa and the temperature is 155-180 ℃, controlling the reaction time to be more than or equal to 24 hours, and obtaining the recovered ester after the reaction is finished.
Then 250kg of polyethylene glycol monomethyl ether, 35kg of trihydroxy polyoxypropylene ether, 200kg of recovered ester, 100kg of diethylene glycol, 205kg of triethylene glycol monobutyl ether, 150kg of tetraethylene glycol dimethyl ether, 8kg of methylbenzotriazole, 8kg of dioctylaniline, 5kg of 2, 2-bis (4-hydroxyphenyl) propane (bisphenol A), 4kg of pentaerythritol tetrakis [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], 0.1kg of polypropylene glycol 2000, 3kg of sodium nitrite and diisopropanolamine are added into a 1.5T reaction kettle in sequence to adjust the pH value to be more than 7.5, and the HZY3 brake fluid is prepared by stirring for 4 hours, filtering through a 0.1um filter and subpackaging to obtain the HZY3 brake fluid.
The technical indexes of the braking fluid of HZY3 prepared in example 1 were measured according to the requirements of the special durable metal corrosion test, and the results are shown in table 1 below.
TABLE 1
Example 2
The HZY3 brake fluid is prepared from the recycled ester prepared in example 1 by sequentially adding 200kg of polyethylene glycol monomethyl ether, 25kg of trihydroxy polyoxypropylene ether, 300kg of recycled ester, 100kg of diethylene glycol, 180kg of triethylene glycol monobutyl ether, 100kg of tetraethylene glycol dimethyl ether, 6kg of methylbenzotriazole, 7kg of dioctylaniline, 8kg of 2, 2-bis (4-hydroxyphenyl) propane (bisphenol A), 6kg of tetra [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester, 0.12kg of polypropylene glycol 2000, 1.5kg of sodium nitrite, adding diisopropanolamine to adjust the pH value to be more than 7.5, stirring for 4h, filtering through a 0.1um filter, and subpackaging to obtain the HZY3 brake fluid.
The technical indexes of the braking fluid of HZY3 prepared in example 1 were measured according to the requirements of the special durable metal corrosion test, and the results are shown in table 2 below.
TABLE 2
Example 3
The HZY3 brake fluid is prepared by using the recycled ester prepared in example 1, and the preparation method comprises the following steps of sequentially adding 150kg of polyethylene glycol monomethyl ether, 20kg of trihydroxy polyoxypropylene ether, 450kg of recycled ester, 100kg of diethylene glycol, 200kg of triethylene glycol monobutyl ether, 50kg of tetraethylene glycol dimethyl ether, 8kg of methyl benzotriazole, 10kg of dioctylaniline, 10kg of 2, 2-bis (4-hydroxyphenyl) propane (bisphenol A), 5kg of tetra [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester, 0.2kg of polypropylene glycol 2000, 0.5kg of sodium nitrite, and diisopropanolamine to adjust the pH value to be more than 7.5, stirring for 4 hours, filtering through a 0.1um filter, and subpackaging to obtain the HZY3 brake fluid.
The technical indexes of the braking fluid of HZY3 prepared in example 1 were measured according to the requirements of the special durable metal corrosion test, and the results are shown in table 3 below.
TABLE 3
From the above table 1, table 2 and table 3, it can be seen that the HZY3 borate brake fluid prepared by using the recycled ester technology has a high dry-wet boiling point meeting the requirements of GB12981-2003, and simultaneously has a good low-temperature kinematic viscosity, the formula of the used additive can meet the requirements of a special durable metal corrosion test, and the effect of preventing metal corrosion of the formula is far better than the technical index requirements of GB 12981-2003.
While the embodiments of the present invention have been described in detail, those skilled in the art will recognize that the embodiments of the present invention can be practiced without departing from the spirit and scope of the claims.
Claims (9)
1. A preparation method of recycled ester is characterized by comprising the following preparation steps:
(1) low vacuum esterification stage: adding boric acid, phosphorous acid and high vacuum recovered materials into a reaction kettle according to the mass ratio of 1: 0.0005: 18, performing dehydration reaction under the conditions that the vacuum degree is 0.060-0.065Mpa and the temperature is 140-;
(2) high vacuum esterification stage: carrying out micro-dehydration reaction under the conditions that the vacuum degree is more than or equal to 0.096Mpa and the temperature is 155-180 ℃, controlling the reaction time to be more than or equal to 24 hours, and obtaining recovered ester after the reaction is finished;
wherein the purity of the boric acid is more than or equal to 99.9 percent, the phosphorous acid is of analytical purity grade, and the high vacuum recovery product is a recovery product obtained in a high vacuum stage by a two-step vacuum method after the esterification of alkyl alcohol ether.
2. A recycled ester characterized by: the recovered ester is produced by the process according to claim 1.
3. A recovered ester according to claim 2, wherein: the pH value of the recovered ester is more than or equal to 4.5, the water content is less than or equal to 0.15 percent, and the boiling point is more than or equal to 265 ℃.
4. The application of the recycled ester in preparation of HZY3 brake fluid is characterized in that the HZY3 brake fluid comprises, by mass, 15-25 parts of polyethylene glycol methyl ether, 0.5-5.0 parts of trihydroxy polyoxypropylene ether, 15-50 parts of recycled ester, 10-15 parts of diethylene glycol, 15-35 parts of triethylene glycol monobutyl ether, 5-20 parts of tetraethylene glycol dimethyl ether, 0.2-1.0 part of methylbenzotriazole, 0.2-1.5 parts of dioctylaniline, 0.5-3.0 parts of 2, 2-bis (4-hydroxyphenyl) propane (bisphenol A), 0.3-3.0 parts of tetra [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester, 0.3-1.0 part of polypropylene glycol 2000, 0.005-0.5 part of sodium nitrite, 0.01-0.5 part of alkalinity regulator and 0.1-5.0 part of alkalinity regulator.
5. The application of the recycled ester in preparing HZY3 brake fluid is characterized in that the HZY3 brake fluid comprises, by mass, 15-20 parts of polyethylene glycol methyl ether, 0.5-3.0 parts of trihydroxy polyoxypropylene ether, 30-45 parts of recycled ester, 10-12 parts of diethylene glycol, 15-25 parts of triethylene glycol monobutyl ether, 5-12 parts of tetraethylene glycol dimethyl ether, 0.5-0.8 part of methylbenzotriazole, 0.5-1.0 part of dioctylaniline, 0.5-2.0 part of 2, 2-bis (4-hydroxyphenyl) propane (bisphenol A), 0.5-2.0 part of tetra [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester, 0.5-1.0 part of polypropylene glycol 2000, 0.01-0.2 part of sodium nitrite, 0.01-0.2 part of alkalinity regulator and 0.5-3.5-0 part of alkalinity regulator.
6. The application of the recycled ester in preparing HZY3 brake fluid according to claim 4 is characterized in that the HZY3 brake fluid comprises, by mass, 15 parts of polyethylene glycol methyl ether, 2 parts of trihydroxy polyoxypropylene ether, 45 parts of recycled ester, 10 parts of diethylene glycol, 20 parts of triethylene glycol monobutyl ether, 5 parts of tetraethylene glycol dimethyl ether, 0.8 part of methylbenzotriazole, 1.0 part of dioctylaniline, 1.0 part of 2, 2-bis (4-hydroxyphenyl) propane (bisphenol A), 0.5 part of pentaerythritol tetrakis [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], 0.02 part of polypropylene glycol 2000, 0.05 part of sodium nitrite and 2.5 parts of alkalinity regulator.
7. The use of a recycled ester in the preparation of an HZY3 brake fluid according to claim 4, wherein: the molecular formula of the polyethylene glycol monomethyl ether is as follows: CH (CH)3(OCH2CH2)nOH, wherein n is more than or equal to 3, and the low-temperature kinematic viscosity is controlled to be less than or equal to 1000mm at the temperature of minus 40 DEG C2/s。
8. The use of a recycled ester in the preparation of an HZY3 brake fluid according to claim 4, wherein: the alkalinity regulator is monoisopropanolamine, diisopropanolamine or alkoxy fatty alcohol cycloalkyl amine, and the alkoxy fatty alcohol cycloalkyl amine is obtained by addition reaction of fatty amine and epoxy compound.
9. The application of the recycled ester in preparing HZY3 brake fluid according to claim 4 is characterized in that the HZY3 brake fluid is prepared by the steps of sequentially adding polyethylene glycol methyl ether, trihydroxy polyoxypropylene ether, recycled ester, diethylene glycol, triethylene glycol monobutyl ether, tetraethylene glycol dimethyl ether, methylbenzotriazole, dioctylaniline, 2-bis (4-hydroxyphenyl) propane (bisphenol A), pentaerythrityl tetrakis [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], polypropylene glycol 2000 and sodium nitrite into a 1.5T reaction kettle, adding an alkalinity regulator to adjust the pH value to be more than 7.5, continuously stirring for 4 hours, filtering through a 0.1um filter, and subpackaging to obtain the HZY3 brake fluid.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112481005A (en) * | 2020-12-02 | 2021-03-12 | 安徽天驰先锋油品制造有限公司 | Efficient borate type brake fluid and preparation method thereof |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1107506A (en) * | 1994-07-11 | 1995-08-30 | 北京化工大学 | Method for preparing borate-type hydraulic-brake liquor for car |
| CN1759165A (en) * | 2003-03-12 | 2006-04-12 | 巴斯福股份公司 | Dot 4 brake fluids |
| CN101418249A (en) * | 2008-10-30 | 2009-04-29 | 张家港迪克汽车化学品有限公司 | DOT4 boric acid ester type brake fluid |
| CN101886019A (en) * | 2010-07-21 | 2010-11-17 | 张家港迪克汽车化学品有限公司 | Higher ester type brake fluid |
| CN102796600A (en) * | 2012-08-12 | 2012-11-28 | 湘潭大学 | Preparation method of high-grade borate type automobile brake fluid |
| CN103333188A (en) * | 2013-07-25 | 2013-10-02 | 中国石油化工股份有限公司 | Boric acid ester production method |
| CN103524544A (en) * | 2013-10-16 | 2014-01-22 | 中国石油化工股份有限公司 | Production method of boric acid ester by repeatedly using and purifying waste liquid |
-
2020
- 2020-04-03 CN CN202010257366.2A patent/CN111303961A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1107506A (en) * | 1994-07-11 | 1995-08-30 | 北京化工大学 | Method for preparing borate-type hydraulic-brake liquor for car |
| CN1759165A (en) * | 2003-03-12 | 2006-04-12 | 巴斯福股份公司 | Dot 4 brake fluids |
| CN101418249A (en) * | 2008-10-30 | 2009-04-29 | 张家港迪克汽车化学品有限公司 | DOT4 boric acid ester type brake fluid |
| CN101886019A (en) * | 2010-07-21 | 2010-11-17 | 张家港迪克汽车化学品有限公司 | Higher ester type brake fluid |
| CN102796600A (en) * | 2012-08-12 | 2012-11-28 | 湘潭大学 | Preparation method of high-grade borate type automobile brake fluid |
| CN103333188A (en) * | 2013-07-25 | 2013-10-02 | 中国石油化工股份有限公司 | Boric acid ester production method |
| CN103524544A (en) * | 2013-10-16 | 2014-01-22 | 中国石油化工股份有限公司 | Production method of boric acid ester by repeatedly using and purifying waste liquid |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112481005A (en) * | 2020-12-02 | 2021-03-12 | 安徽天驰先锋油品制造有限公司 | Efficient borate type brake fluid and preparation method thereof |
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