CN101955840A - High boiling point boric acid ester type synthetic brake fluid and preparation method thereof - Google Patents
High boiling point boric acid ester type synthetic brake fluid and preparation method thereof Download PDFInfo
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- CN101955840A CN101955840A CN201010260887XA CN201010260887A CN101955840A CN 101955840 A CN101955840 A CN 101955840A CN 201010260887X A CN201010260887X A CN 201010260887XA CN 201010260887 A CN201010260887 A CN 201010260887A CN 101955840 A CN101955840 A CN 101955840A
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Abstract
The invention relates to a high boiling point boric acid ester type synthetic brake fluid and a preparation method thereof. The synthetic brake fluid is characterized by being prepared from the following components in percentage by weight through compounding: 5-15% of triethylene glycol monomethyl ether mixture (TM alcohol ether), 85-90% of TM alcohol ether borate (TMB), 0.8-1.2% of glycol, 0.13-0.2% of 2,6-di-tert-butyl-4-methylphenol (antiager 264), 0.08-0.1% of benzotriazole and 1.5-2.5% of pH value regulator. The invention has the following characteristics of simple process, stable product performance and no boron element separation; the product has high dry and wet equilibrium reflux boiling points and excellent comprehensive properties comprising excellent high temperature air resisting property, low temperature flowing property, metal corrosion resisting property for brake systems, compatibility with rubber elements, compatibility with other alcohol ether type brake fluids and the like; and the technical characteristics of the product reaches and exceeds the technical requirements of HZY4 in national standard GB12891 and DOT4 in American FMVSS. NO. 116 and are equivalent to the standard level of 'Super DOT4' brake fluid widely used in every European country.
Description
Technical field
The invention belongs to organic chemical industry's synthetic automobile field of chemicals, particularly relate to a kind of high boiling point borate-type synthetic brake fluid and preparation method thereof.
Background technology
Motor vehicle brake fluid is to be used for the working medium that hydraulic braking system for automobile transmits pressure, is to make wheel drag realize a kind of functional liquid of braking effect, and the quality condition of motor vehicle brake fluid is directly connected to the driving safety of vehicle.
Along with the improvement of highway, the raising of the speed of a motor vehicle is slowed down in the driving and the increasing of sharp cut-off number of times, and the thermal load that breaking system is born is more and more higher.The particularly fast development of light, the car of novel high speed, then require braking fluid can adapt to wide temperature range and chemical constitution with the best, borate type braking fluid high is done because of it has, wet boiling point, and lower low temperature viscosity becomes the research focus of various countries braking fluid manufacturing firm.
The new motor vehicle brake fluid standard GB12981-2003 " motor vehicle brake liquid " of China integrates with world standard, it is mandatory national standard, HZY3 in the national standard, HZY4, HZY5 specification correspond respectively to international DOT3, DOT4 and DOT5 specification, and back two kinds belong to the high boiling point braking fluid.
Implementing of new standard is beneficial to standard and improves China's motor vehicle brake fluid overall quality level, also points the direction for synthetic brake fluid research simultaneously.Under the increasing situation of high-performing car, the usage quantity proportion of the synthetic motor vehicle brake fluid HZY3 (DOT3) of alcohol ether type can be fewer and feweri, will obtain great development and have high level cadre more, wet equilibrium reflux boiling point, lower low temperature viscosity and the ester type brake fluid of low water sensitivity.
Summary of the invention
The objective of the invention is to satisfy above-mentioned Brake Fluid Standard requirement, providing a kind of is basic material with triethylene glycol methyl ether mixture (TM alcohol ether), carry out the basal liquid that acid esterification obtains the high boiling point borate type braking fluid by its excessive method, add subsidiary material then and obtain high boiling point borate-type synthetic brake fluid, its technology is simple, and quality product meets in the standard GB 12891 high boiling point borate-type synthetic brake fluid of the technical requirements of DOT4 and preparation method thereof among the HZY4 and U.S. FMVSS.NO.116 standard.
Technical scheme of the present invention is:
A kind of high boiling point borate-type synthetic brake fluid, with triethylene glycol methyl ether mixture (TM alcohol ether), TM alcohol ether boric acid ester (TMB), polyoxyethylene glycol, 2,6-di-tert-butyl-4-methy phenol (antioxidant 264), benzotriazole, pH value conditioning agent are component, form through composite, it is characterized in that: the proportioning of used prescription (counting by weight percentage) content is:
Triethylene glycol methyl ether mixture (TM alcohol ether) 5-15
TM alcohol ether boric acid ester (TMB) 85-90
Ethylene glycol 0.8-1.2
2,6 di tert butyl 4 methyl phenol (antioxidant 264) 0.13-0.2
Benzotriazole 0.08-0.1
PH value conditioning agent total amount 1.5-2.5
Described pH value conditioning agent is organic high boiling liquid combination, as trolamine, and dicyclohexyl amine, one or both combinations in the dodecyl diethyleneglycolamin.
A kind of high boiling point borate-type synthetic brake fluid preparation method, it is characterized in that: (1) is squeezed into TM alcohol ether 200-260kg in the esterifying kettle, heats up to stir, when temperature rises to 50-100 ℃, again boric acid 20-30kg is dropped in the still and carry out esterification, open vacuum pump intensification dehydration simultaneously.Control reaction temperature is between 100-120 ℃ in the reaction process, vacuum tightness 0.07-0.09Mpa, reaction times 2.5-3 hour.Make faint yellow transparent TM alcohol ether boric acid ester product.(2) above-mentioned TM alcohol ether boric acid ester is squeezed in the composite still, getting the TM alcohol ether that accounts for gross weight 5%-15% weight percentage simultaneously also squeezes in the still, heat up and stir, when temperature rises to 50-70 ℃, percentage ratio adds antioxidant 264: 0.13-0.2 by weight successively, benzotriazole: 0.08-0.10, polyoxyethylene glycol: 0.8-1.2 adds pH value conditioning agent dicyclohexyl amine: 1.0-1.5 at last, trolamine and dodecyl diethyleneglycolamin: 0.5-1.5, insulated and stirred is 1 hour under normal pressure, be cooled to room temperature, make faint yellow transparent ester type brake fluid product, sampling detects its equilibrium reflux boiling point＞250 ℃, wet boiling point＞180 ℃ ,-40 ℃ of kinematic viscosity＜1500mm
2/ s, pH value are 8.5-9.5.
Beneficial effect of the present invention
The present invention has following characteristics: 1, technology is simple, and product performance are stable, and do not have the boron element to separate out phenomenon; 2, the borate type braking fluid of the inventive method preparation have high do, wet equilibrium reflux boiling point and excellent comprehensive performance, comprise have the anti-vapour lock performance of excellent high-temperature, low temperature flowability, prevent breaking system corrosion of metal performance, with the rubber parts compatibility and with the consistency of other alcohol ether type braking fluid etc.; 3, the key technical indexes of high boiling point borate-type synthetic brake fluid of the present invention is as follows: ERBT is 259 ℃, and WERBP is 193 ℃, and-40 ℃ kinematic viscosity is 969mm
2/ s, 100 ℃ kinematic viscosity is 2.37mm
2/ s, pH value is 8.9, water ratio＜0.1%, the technical feature of product reaches and surpasses the technical requirements of DOT4 among the HZY4 and U.S. FMVSS.NO.116 standard in the standard GB 12891, can satisfy simultaneously the technical requirements of Volkswagen's internal standard, be equivalent to the specification level of European various countries widely used " super DOT4 braking fluid ".
Embodiment
The basal liquid of countries in the world synthetic brake fluid mostly is an alkoxyl group multicondensed ethylene glycol ether mixture.The present invention is based on the experience of in the past being engaged in alcohol ether type braking fluid manufacturing technology, select the glycol ether [RO-(CH of oxyethane (EO) adduct number n 〉=3
2CH
2O))
n-H, n 〉=3] suitable component as the high boiling point braking fluid, therefore select the component of the polyoxyethylene monomethyl ether mixture of n=3 as the basal liquid of this braking fluid, wherein the triethylene glycol monomethyl ether ingredients constitute is more than 50%, the equilibrium reflux boiling point of TM alcohol ether is 245-255 ℃, kinematic viscosity＜400mm of-40 ℃
2/ s, the TM alcohol ether is high boiling solvent, is suitable as the thinner of high boiling point braking fluid.
The present invention adopts classical esterification process to make TM alcohol ether boric acid ester, abbreviates TMB as.The synthetic method of TM alcohol-ether mixture boric acid ester (TMB) is: the TM alcohol ether with excessive proportioning weight part drops in the still earlier, heat up and stir, when temperature rises to 70-80 ℃, boric acid with weight part drops in the still again, when heat temperature raising to 100 ℃, begin esterification, open vacuum pump simultaneously to get rid of moisture and the low boilers that reaction generates.Controlled temperature is between 110-120 ℃ in the reaction process, and vacuum tightness 0.07-0.09Mpa reaction times 2.5-3 hour, makes faint yellow transparent TM alcohol ether boric acid ester.After the cooling cooling, detect its boiling point reflux, wet boiling point, three indexs of-40 ℃ of kinematic viscosity.
TM alcohol ether boric acid ester has do, the wet equilibrium reflux boiling point higher than TM alcohol ether, and low temperature viscosity also increases many.The present invention adopts the technical measures control esterification yield of TM alcohol ether partial esterification, promptly selecting on the material proportion under the excessive 20-30% situation of TM alcohol ether, make boric acid can reach rapidly fully and transform that this boron carboxylate that transforms fully accounts for more than 70% of resultant of reaction.And in esterification reaction product, contain still nonesterified excessive TM alcohol ether, and can reduce the low temperature viscosity of boron carboxylate self, its whole manufacturing process is greatly simplified, wherein some esterified prod itself is exactly qualified ester type brake fluid.And the boron element can not occur and separate out phenomenon.
The pH value conditioning agent is selected the combination of high boiling point liquid organic compound, trolamine for example, dicyclohexyl amine, a kind of or two kinds of combinations of dodecyl diethyleneglycolamin.Not only realize the composite homogeneity of braking fluid mediation easily, and, help the standing storage of braking fluid product because the boiling point of these compounds is also very high, not volatile.
Embodiment 1:
(1) earlier TM alcohol ether 212kg is squeezed in the esterifying kettle, heat up and stir, when temperature rises to 70-80 ℃, again boric acid 18kg is dropped in the still and carry out esterification, when heat temperature raising to 100 ℃, begin esterification, open vacuum pump intensification dehydration simultaneously, control reaction temperature is between 100-110 ℃ in the reaction process, vacuum tightness 0.07-0.08Mpa in 2 hours reaction times, makes faint yellow transparent boric acid ester product, after the cooling cooling, detecting its equilibrium reflux boiling point through sampling is 257, and wet boiling point is 184 ℃, and-40 ℃ of kinematic viscosity are 1459mm
2/ s; (2) above-mentioned TM alcohol ether boric acid ester is squeezed in the composite still, getting the TM alcohol ether of 5% weight percentage simultaneously also squeezes in the still, heat up and stir, when temperature rises to 50-70 ℃, percentage ratio adds antioxidant 264 by weight successively: 0.13, benzotriazole: 0.08, polyoxyethylene glycol: 0.8, add pH value conditioning agent dicyclohexyl amine at last: 1.5, insulated and stirred is 1 hour under normal pressure, after composite the finishing, be cooled to room temperature, make faint yellow transparent ester type brake fluid product, it is 251 that sampling detects its equilibrium reflux boiling point, wet boiling point is 181 ℃, and-40 ℃ of kinematic viscosity are 1325mm
2/ s, pH value are 9.2.
Embodiment 2:
(1) earlier TM alcohol ether 212kg is squeezed in the esterifying kettle, heat up and stir, when temperature rises to 70-80 ℃, boric acid 20kg is dropped in the still carry out esterification again, open vacuum pump intensification dehydration simultaneously.Control reaction temperature is between 100-110 ℃ in the reaction process, vacuum tightness 0.07-0.08Mpa, 2.5 hours reaction times.Make faint yellow transparent boric acid ester product.After the cooling cooling, detecting its equilibrium reflux boiling point through sampling is 268 ℃, and wet boiling point is 189 ℃, and-40 ℃ of kinematic viscosity are 1640mm
2/ s; (2) above-mentioned TM alcohol ether boric acid ester is squeezed in the composite still, getting the TM alcohol ether of 10% weight percentage simultaneously also squeezes in the still, heat up and stir, when temperature rises to 50-70 ℃, percentage ratio adds antioxidant 264 by weight successively: 0.18, and benzotriazole: 0.10, polyoxyethylene glycol: 1.0, add pH value conditioning agent dicyclohexyl amine at last: 1.0, trolamine: 1.0.Insulated and stirred is 1 hour under normal pressure, after composite the finishing, is cooled to room temperature, makes faint yellow transparent ester type brake fluid product, and it is 257 ℃ that sampling detects its equilibrium reflux boiling point, and wet boiling point is 184 ℃, and-40 ℃ of kinematic viscosity are 1080mm
2/ s, pH value are 8.9.
Embodiment 3:
(1) earlier TM alcohol ether 212kg is squeezed in the esterifying kettle, heat up and stir, when temperature rises to 70-80 ℃, again boric acid 26kg is dropped in the still and carry out esterification, open vacuum pump intensification dehydration simultaneously, control reaction temperature is between 100-120 ℃ in the reaction process, vacuum tightness 0.07-0.09Mpa, 2 hours reaction times.Make faint yellow transparent TM alcohol ether boric acid ester product, after the cooling cooling, detecting its equilibrium reflux boiling point through sampling is 275 ℃, and wet boiling point is 195 ℃, and-40 ℃ of kinematic viscosity are 1719mm
2/ s; (2) above-mentioned TM alcohol ether boric acid ester is squeezed in the composite still, getting the TM alcohol ether of 15% weight percentage simultaneously also squeezes in the still, heat up and stir, when temperature rose to 50-70 ℃, percentage ratio added antioxidant 264 by weight successively: 0.2, and benzotriazole: 0.10, polyoxyethylene glycol: 1.2, add pH value conditioning agent dicyclohexyl amine at last: 1.0, the dodecyl diethyleneglycolamin: 1.5, insulated and stirred is 1 hour under normal pressure.After composite the finishing, be cooled to room temperature, make faint yellow transparent ester type brake fluid product.It is 259 ℃ that sampling detects its equilibrium reflux boiling point, and wet boiling point is 189 ℃, and-40 ℃ of kinematic viscosity are 909mm
2/ s, pH value are 8.5.
Claims (3)
1. high boiling point borate-type synthetic brake fluid, with triethylene glycol methyl ether mixture (TM alcohol ether), TM alcohol ether boric acid ester (TMB), polyoxyethylene glycol, 2,6-di-tert-butyl-4-methy phenol (antioxidant 264), benzotriazole, pH value conditioning agent are component, form through composite, it is characterized in that: the proportioning of used prescription (counting by weight percentage) content is:
Triethylene glycol methyl ether mixture (TM alcohol ether) 5-15
TM alcohol ether boric acid ester (TMB) 85-90
Ethylene glycol 0.8-1.2
2,6 di tert butyl 4 methyl phenol (antioxidant 264) 0.13-0.2
Benzotriazole 0.08-0.1
PH value conditioning agent total amount 1.5-2.5
2. high boiling point ester type brake fluid as claimed in claim 1 is characterized in that: the pH value conditioning agent of use is organic high boiling liquid combination, as trolamine, and bicyclohexylamine, one or both combinations in the dodecyl diethyleneglycolamin.
3. high boiling point borate-type synthetic brake fluid preparation method, it is characterized in that: (1) is squeezed into TM alcohol ether 200-260kg in the esterifying kettle, heats up to stir, when temperature rises to 50-100 ℃, again boric acid 20-30kg is dropped in the still and carry out esterification, open vacuum pump intensification dehydration simultaneously.Control reaction temperature is between 100-120 ℃ in the reaction process, vacuum tightness 0.07-0.09Mpa, reaction times 2.5-3 hour.Make faint yellow transparent TM alcohol ether boric acid ester product.(2) above-mentioned TM alcohol ether boric acid ester is squeezed in the composite still, getting the TM alcohol ether of 5%-15% weight percentage simultaneously also squeezes in the still, heat up and stir, when temperature rises to 50-70 ℃, percentage ratio adds antioxidant 264: 0.13-0.2 by weight successively, benzotriazole: 0.08-0.10, polyoxyethylene glycol: 0.8-1.2 adds pH value conditioning agent bicyclohexylamine: 1.0-1.5 at last, trolamine and dodecyl diethyleneglycolamin: 0.5-1.5, insulated and stirred is 1 hour under normal pressure, be cooled to room temperature, make faint yellow transparent ester type brake fluid product, sampling detects its equilibrium reflux boiling point＞250 ℃, wet boiling point＞180 ℃ ,-40 ℃ of kinematic viscosity＜1500mm
2/ s, pH value are 8.5-9.5.
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| CN201010260887XA CN101955840A (en) | 2010-08-24 | 2010-08-24 | High boiling point boric acid ester type synthetic brake fluid and preparation method thereof |
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| CN201010260887XA CN101955840A (en) | 2010-08-24 | 2010-08-24 | High boiling point boric acid ester type synthetic brake fluid and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103013629A (en) * | 2011-09-28 | 2013-04-03 | 天津博克尼科技发展有限公司 | Synthetic automobile brake fluid |
| CN104611092A (en) * | 2015-02-12 | 2015-05-13 | 辽宁润迪汽车环保科技股份有限公司 | Advanced locomotive brake fluid composition |
| CN104629884A (en) * | 2015-02-12 | 2015-05-20 | 辽宁润迪汽车环保科技股份有限公司 | Advanced automobile brake fluid composition |
| CN104962348A (en) * | 2015-06-05 | 2015-10-07 | 上海金灿润滑油有限公司 | Brake fluid for motor vehicle |
| CN106118821A (en) * | 2016-06-27 | 2016-11-16 | 辽宁道博精细化学品生产有限公司 | A kind of alcohol ether boric acid ester type DOT 4 braking fluid |
| CN108219902A (en) * | 2016-12-13 | 2018-06-29 | 比亚迪股份有限公司 | A kind of motor vehicle brake fluid composition and motor vehicle brake fluid and preparation method thereof |
| CN106118821B (en) * | 2016-06-27 | 2019-07-16 | 辽宁道博精细化学品生产有限公司 | A kind of alcohol ether boric acid ester type DOT 4 braking fluid |
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| CN1107506A (en) * | 1994-07-11 | 1995-08-30 | 北京化工大学 | Method for preparing borate-type hydraulic-brake liquor for car |
| WO2004081155A1 (en) * | 2003-03-12 | 2004-09-23 | Basf Aktiengesellschaft | Dot 4 brake fluids |
| CN1226400C (en) * | 2003-11-14 | 2005-11-09 | 华南理工大学 | Boric acid ester brake fluid and its preparing process |
| 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 |
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2010
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| CN1107506A (en) * | 1994-07-11 | 1995-08-30 | 北京化工大学 | Method for preparing borate-type hydraulic-brake liquor for car |
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| CN1226400C (en) * | 2003-11-14 | 2005-11-09 | 华南理工大学 | Boric acid ester brake fluid and its preparing process |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103013629A (en) * | 2011-09-28 | 2013-04-03 | 天津博克尼科技发展有限公司 | Synthetic automobile brake fluid |
| CN104611092A (en) * | 2015-02-12 | 2015-05-13 | 辽宁润迪汽车环保科技股份有限公司 | Advanced locomotive brake fluid composition |
| CN104629884A (en) * | 2015-02-12 | 2015-05-20 | 辽宁润迪汽车环保科技股份有限公司 | Advanced automobile brake fluid composition |
| CN104629884B (en) * | 2015-02-12 | 2018-03-30 | 辽宁润迪汽车环保科技股份有限公司 | A kind of high-grade braking liquid for car composition |
| CN104962348A (en) * | 2015-06-05 | 2015-10-07 | 上海金灿润滑油有限公司 | Brake fluid for motor vehicle |
| CN106118821A (en) * | 2016-06-27 | 2016-11-16 | 辽宁道博精细化学品生产有限公司 | A kind of alcohol ether boric acid ester type DOT 4 braking fluid |
| CN106118821B (en) * | 2016-06-27 | 2019-07-16 | 辽宁道博精细化学品生产有限公司 | A kind of alcohol ether boric acid ester type DOT 4 braking fluid |
| CN108219902A (en) * | 2016-12-13 | 2018-06-29 | 比亚迪股份有限公司 | A kind of motor vehicle brake fluid composition and motor vehicle brake fluid and preparation method thereof |
| CN108219902B (en) * | 2016-12-13 | 2021-04-20 | 比亚迪股份有限公司 | Automobile brake fluid composition, automobile brake fluid and preparation method thereof |
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Application publication date: 20110126 |