阅读说明：本技术 一种Class7硼酸脂型制动液及制备方法 (Class7 boric acid ester type brake fluid and preparation method thereof ) 是由 周广来 王健 裘旭荣 杨亚青 戴天 于 2021-09-27 设计创作，主要内容包括：本发明公开一种Class7硼酸脂型制动液及制备方法,按照质量分数包括以下物质：8％至12％四乙二醇丁醚；3％至5％三乙二醇丁醚；2％至5％四乙二醇甲醚；75％至80％三乙二醇甲醚；3％至6％硼酸；0.02％至0.05％双酚A；本发明还公开了该制动液的制备方法,包括以下步骤：步骤一、将三乙二醇甲醚、四乙二醇甲醚及硼酸按照所述质量分数投入反应釜中,控制反应温度进行合成反应；步骤二、真空下脱水反应；在反应期间应不断搅拌,反应时间大于等于4小时；步骤三、充分反应后得到硼酸脂,再混合其他物质得目标产品；本发明具有高的干、湿沸点,还具有良好的低温运动黏度,橡胶适应性好。(The invention discloses a Class7 boric acid ester type brake fluid and a preparation method thereof, wherein the brake fluid comprises the following substances in percentage by mass: from 8% to 12% tetraethyleneglycol monobutyl ether; 3% to 5% butyl triethylene glycol; 2% to 5% tetraethylene glycol methyl ether; 75% to 80% triethylene glycol methyl ether; 3% to 6% boric acid; 0.02% to 0.05% bisphenol a; the invention also discloses a preparation method of the brake fluid, which comprises the following steps: putting triethylene glycol methyl ether, tetraethylene glycol methyl ether and boric acid into a reaction kettle according to the mass fraction, and controlling the reaction temperature to carry out synthetic reaction; step two, carrying out dehydration reaction under vacuum; stirring continuously during the reaction, wherein the reaction time is more than or equal to 4 hours; step three, obtaining boric acid ester after full reaction, and mixing other substances to obtain a target product; the invention has high dry and wet boiling points, good low-temperature kinematic viscosity and good rubber adaptability.)

1. A Class7 boric acid ester type brake fluid is characterized in that:

the material comprises the following substances in percentage by mass:

2. the brake fluid of the Class7 borate type according to claim 1, wherein: also comprises 0.05 to 0.08 percent of 2,6 di-tert-butyl-p-cresol by mass fraction.

3. The brake fluid of the Class7 borate type according to claim 1, wherein: and benzotriazole with the mass fraction of 0.06-0.15 percent is also included.

4. The brake fluid of the Class7 borate type according to claim 1, wherein: also included are metal corrosion inhibitors.

5. The brake fluid of claim 4, which is of the Class7 borate type, wherein: the metal inhibitor comprises

0.2 to 0.5 mass percent of monoethanolamine;

0.02 to 0.05 percent of alkyl imidazoline quaternary ammonium salt by mass fraction.

6. The brake fluid of the Class7 borate type according to claim 1, wherein: comprises 0.01 to 0.03 percent of dodecenylsuccinic acid by mass fraction.

7. The brake fluid of the Class7 borate type according to claim 1, wherein: comprises 0.3 to 0.74 percent of di-n-butylamine by mass fraction.

8. The brake fluid of the Class7 borate type according to claim 1, wherein: the material comprises the following substances in percentage by mass:

9. a method for preparing a Class7 boric acid ester type brake fluid as claimed in any one of claims 1 to 8, wherein: the method comprises the following steps:

synchronously putting triethylene glycol methyl ether, tetraethylene glycol methyl ether and boric acid into a reaction kettle according to the mass fraction, and controlling the reaction temperature to be 95-105 ℃ for synthetic reaction;

stirring continuously during the reaction, wherein the reaction time is more than or equal to 1 hour;

step two, carrying out dehydration reaction under vacuum;

stirring continuously during the reaction, wherein the reaction time is more than or equal to 4 hours;

and step three, obtaining the boric acid ester after full reaction, and mixing other substances to obtain the target product.

10. The method of claim 9, wherein: the dehydration reaction temperature in the second step is 175-185 ℃.

Technical Field

The invention relates to the technical field of brake fluid, in particular to a Class7 boric acid ester type brake fluid and a preparation method thereof.

Background

The brake fluid is a liquid medium for transmitting brake pressure in a hydraulic brake system, and is applied to motor vehicles adopting the hydraulic brake system. In recent years, with the rapid development of the automobile industry, more stringent requirements are put on the performance of brake fluid for motor vehicles. The international traffic standard for brake fluid ISO4925, 2020 edition adds a new brake fluid quality grade, Class7, than 2006 edition. Compared with other quality grades, the grade brake fluid is required to have more excellent high and low temperature performance, and the performance difference is particularly expressed on three indexes of equilibrium reflux boiling point, wet equilibrium reflux boiling point and low-temperature kinematic viscosity at minus 40 ℃.

The brake fluid is used in hydraulic brake or clutch system of automobile and is important matter for ensuring the stable and sensitive operation of automobile brake system and the running safety of automobile. A plurality of rubber sealing elements are assembled in the brake system and are immersed in brake fluid for a long time under the high-temperature condition, and the adaptability of the brake fluid to the rubber material not only influences the mechanical strength and the volume change of the rubber material, but also influences the performance of the brake fluid, and is directly related to the safety and reliability of the brake system.

Disclosure of Invention

The invention aims to provide a Class7 boric acid ester type brake fluid which has high dry and wet boiling points, good low-temperature kinematic viscosity and good rubber adaptability.

In order to solve the technical problem, the technical scheme of the invention is as follows: a Class7 boric acid ester type brake fluid comprises the following substances in percentage by mass:

preferably, the composition also comprises 0.05 to 0.08 percent of 2,6 di-tert-butyl-p-cresol by mass fraction. The invention improves the stability of oxidation resistance of the product by adding 2,6 di-tert-butyl-p-cresol into the system.

Preferably, the composition also comprises benzotriazole with the mass fraction of 0.06 percent to 0.15 percent. According to the invention, benzotriazole is added into the composition to be used as a copper corrosion inhibitor, so that the corrosion of the composition to metal is effectively inhibited.

Preferably, a metal corrosion inhibitor is also included. The present invention effectively inhibits the corrosion of metals of the present invention by adding an amount of a metal corrosion inhibitor to the composition.

Preferably the metal inhibitor comprises

0.2 to 0.5 mass percent of monoethanolamine;

0.02 to 0.05 percent of alkyl imidazoline quaternary ammonium salt by mass fraction.

The two are mutually matched to effectively inhibit the corrosivity of metal, and simultaneously the rubber is synergistically balanced with the methyl ether borate to swell to a certain degree, so that the rubber leather wrist is protected.

The dodecenylsuccinic acid comprises 0.01 to 0.03 mass percent of dodecenylsuccinic acid. In order to further inhibit the metal corrosion and improve the rubber adaptability, the invention also adds a certain amount of dodecenylsuccinic acid.

Preferably, the composition comprises 0.3 to 0.74 mass percent of di-n-butylamine. According to the invention, di-n-butylamine is added into the system as an alkalinity regulator, the pH value of the product is regulated to 7-11, and the corrosion of metal is inhibited.

Preferably, the following substances are included according to mass fraction:

the invention aims to provide a method for preparing a boric acid ester type brake fluid of Class7, and the brake fluid with excellent rubber adaptability is prepared.

In order to solve the technical problem, the technical scheme of the invention is as follows: a preparation method of a Class7 boric acid ester type brake fluid comprises the following steps:

synchronously putting triethylene glycol methyl ether, tetraethylene glycol methyl ether and boric acid into a reaction kettle according to the mass fraction, and controlling the reaction temperature to be 95-105 ℃ for synthetic reaction;

stirring continuously during the reaction, wherein the reaction time is more than or equal to 1 hour;

step two, carrying out dehydration reaction under vacuum;

stirring continuously during the reaction, wherein the reaction time is more than or equal to 4 hours;

and step three, obtaining the boric acid ester after full reaction, and mixing other substances to obtain the target product.

The dehydration reaction temperature in the second step is preferably 175 to 185 ℃.

The invention ensures full reaction and dehydration through the matching of the process and the parameters; the reaction temperature or dehydration temperature is insufficient, the reaction is insufficient, and the product quality is influenced.

By adopting the technical scheme, the invention has the beneficial effects that:

according to the invention, the tetraethylene glycol butyl ether improves the equilibrium reflux boiling point of the product, and the tetraethylene glycol butyl ether, the triethylene glycol butyl ether and the methyl ether borate cooperate to balance the swelling of rubber, so that rubber leather wrists are protected; furthermore, the rubber adaptability of the brake fluid is comprehensively ensured in a synergistic manner by matching with bisphenol A protective rubber, and the rubber adaptability test requirement specified by the standard is met and higher;

on the basis of the application of borate technology, the invention adds tetraethylene glycol methyl ether, and provides a borate modified ethylene glycol methyl ether which can meet and is higher than ISO 4925: the boric acid ester type brake fluid of Class7 required by 2020 has high dry and wet boiling points and good low-temperature kinematic viscosity, and can meet the conditions that the dry boiling point is more than 270 ℃, the wet boiling point is more than 180 ℃, and the low-temperature kinematic viscosity is less than 700mm²The technical requirement of/s and good rubber adaptability.

Thereby achieving the above object of the present invention.

Detailed Description

In order to further explain the technical solution of the present invention, the present invention is explained in detail by the following specific examples.

Example 1

The embodiment discloses a Class7 boric acid ester type brake fluid and a preparation method thereof, wherein the mass fractions of the components in the embodiment are shown in table 1, and the specific preparation method comprises the following steps:

step one, synchronously putting triethylene glycol methyl ether, tetraethylene glycol methyl ether and boric acid into a reaction kettle according to the mass fraction, and controlling the reaction temperature to carry out synthetic reaction at 100 ℃;

stirring continuously during the reaction, wherein the reaction time is more than or equal to 1 hour;

step two, carrying out dehydration reaction under vacuum;

the dehydration reaction temperature in the second step is 180 ℃.

Stirring continuously during the reaction, wherein the reaction time is more than or equal to 4 hours;

and step three, obtaining the boric acid ester after full reaction, and mixing other substances to obtain the target product.

Example 2

The embodiment discloses a Class7 boric acid ester type brake fluid and a preparation method thereof, wherein the mass fractions of the components in the embodiment are shown in table 1, and the specific preparation method comprises the following steps:

synchronously putting triethylene glycol methyl ether, tetraethylene glycol methyl ether and boric acid into a reaction kettle according to the mass fraction, and controlling the reaction temperature to carry out synthetic reaction at 95 ℃;

stirring continuously during the reaction, wherein the reaction time is more than or equal to 1 hour;

step two, carrying out dehydration reaction under vacuum;

the dehydration reaction temperature in the second step is 180 ℃.

Stirring continuously during the reaction, wherein the reaction time is more than or equal to 4 hours;

and step three, obtaining the boric acid ester after full reaction, and mixing other substances to obtain the target product.

Example 3

The embodiment discloses a Class7 boric acid ester type brake fluid and a preparation method thereof, wherein the mass fractions of the components in the embodiment are shown in table 1, and the specific preparation method comprises the following steps:

step one, synchronously putting triethylene glycol methyl ether, tetraethylene glycol methyl ether and boric acid into a reaction kettle according to the mass fraction, and controlling the reaction temperature to be 105 ℃ for synthetic reaction;

stirring continuously during the reaction, wherein the reaction time is more than or equal to 1 hour;

step two, carrying out dehydration reaction under vacuum;

the dehydration reaction temperature in the second step was 185 ℃.

Stirring continuously during the reaction, wherein the reaction time is more than or equal to 4 hours;

and step three, obtaining the boric acid ester after full reaction, and mixing other substances to obtain the target product.

Example 4

The embodiment discloses a Class7 boric acid ester type brake fluid and a preparation method thereof, wherein the mass fractions of the components in the embodiment are shown in table 1, and the specific preparation method comprises the following steps:

step one, synchronously putting triethylene glycol methyl ether, tetraethylene glycol methyl ether and boric acid into a reaction kettle according to the mass fraction, and controlling the reaction temperature to carry out synthetic reaction at 100 ℃;

stirring continuously during the reaction, wherein the reaction time is more than or equal to 1 hour;

step two, carrying out dehydration reaction under vacuum;

the dehydration reaction temperature in the second step was 175 ℃.

Stirring continuously during the reaction, wherein the reaction time is more than or equal to 4 hours;

and step three, obtaining the boric acid ester after full reaction, and mixing other substances to obtain the target product.

Example 5

The embodiment discloses a Class7 boric acid ester type brake fluid and a preparation method thereof, wherein the mass fractions of the components in the embodiment are shown in table 1, and the specific preparation method comprises the following steps:

step one, synchronously putting triethylene glycol methyl ether, tetraethylene glycol methyl ether and boric acid into a reaction kettle according to the mass fraction, and controlling the reaction temperature to carry out synthetic reaction at 100 ℃;

stirring continuously during the reaction, wherein the reaction time is more than or equal to 1 hour;

step two, carrying out dehydration reaction under vacuum;

the dehydration reaction temperature in the second step is 180 ℃.

Stirring continuously during the reaction, wherein the reaction time is more than or equal to 4 hours;

and step three, obtaining the boric acid ester after full reaction, and mixing other substances to obtain the target product.

Table 1 composition and amount (mass%/%) of brake fluid obtained in examples 1 to 5

Dosage of	Example 1	Example 2	Example 3	Example 4	Example 5
						Tetraethylene glycol butyl ether	8	9	10	11	12
Triethylene glycol butyl ether	5	4	3	3	4
						Tetraethylene glycol methyl ether	3	3	2	5	4
Triethylene glycol methyl ether	80	79	78	75	75
						Boric acid	3	4	6	5	4
Bisphenol A	0.02	0.03	0.04	0.05	0.03
						2,6 di-tert-butyl-p-cresol	0.08	0.06	0.08	0.05	0.05
Benzotriazole	0.15	0.13	0.1	0.06	0.08
						Ethanolamine	/	0.2	0.24	0.5	0.2
Alkyl imidazoline quaternary ammonium salt	/	0.05	0.02	0.03	0.03
						Dodecenylsuccinic acid	0.01	0.03	0.02	0.01	0.01
Di-n-butylamine	0.74	0.5	0.5	0.3	0.6

Table 2 tabulation of performance index of examples 1 to 5 brake fluids

TABLE 3 rubber Adaptation Performance index of brake fluids of examples 1 to 5

The performances of the brake fluid obtained in the embodiments 1 to 5 of the invention are detailed in tables 2 and 3, the tetraethylene glycol butyl ether in the invention improves the equilibrium reflux boiling point of the product, and the tetraethylene glycol butyl ether, the triethylene glycol butyl ether and the methyl ether borate synergistically balance the swelling of the rubber, thereby protecting the rubber leather wrist; furthermore, the rubber adaptability of the comprehensive synergetic brake fluid matched with bisphenol A meets and is higher than the rubber adaptability test requirement specified by the standard; the invention adds tetraethylene glycol methyl ether on the basis of the technical application of borate, and provides a borate modified ethylene glycol methyl ether which can meet and is higher than ISO 4925: the boric acid ester type brake fluid of Class7 required by 2020 has high dry and wet boiling points and good low-temperature kinematic viscosity, and can meet the conditions that the dry boiling point is more than 270 ℃, the wet boiling point is more than 180 ℃, and the low-temperature kinematic viscosity is less than 700mm²The technical requirement of/s.