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Recycled ester, preparation method thereof and application of recycled ester in preparation of HZY3 brake fluid

A technology for brake fluid and recyclate, applied in the field of preparing HZY3 brake fluid, recovering ester and its preparation, can solve the problem of not involving the recycling of high-vacuum recyclate, not mentioning the treatment scheme of the recyclate after esterification, not involving Recyclables treatment and other issues, to achieve good low temperature kinematic viscosity, high dry and wet boiling point, and reduce production and processing costs.

Pending Publication Date: 2020-06-19
张家港迪克汽车化学品有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In 2002, the application number was 00130831.9 Chinese patent, which disclosed automobile brake fluid and its manufacturing method, which is to put boric anhydride, polyglycol methyl ether, diethylene glycol and additives into one time, and react under 2-3 atmospheric pressure After cooling and filtering for 3-4 hours, the finished product of brake fluid was obtained. The patent report mainly prepared HZY3 grade brake fluid. The brake fluid formula technology described in this patent belongs to a lower-grade brake fluid formula type, and It does not involve the treatment of reclaimed materials in the high vacuum stage of the reaction
[0005] In 2003, the Chinese patent with application number 200310112132.5 disclosed a borate brake fluid and its preparation method, and described the production and manufacturing method of borate brake fluid. However, the technology used diethylene glycol As the main raw material for the preparation of boric acid esters, it meets the requirements of the HZY3 level index, but there is no mention of the treatment plan for the recycled products after esterification
[0006] In 2003, the Chinese patent with the application number 03111223.4 disclosed a motor vehicle brake fluid and its production method, and described a polymer produced under the action of diethylene glycol and 1,1-dichloroethane under the action of a catalyst. The method for producing brake fluid from body mixture as raw material, the patent gives the technical indicators for preparing HZY4 brake fluid, but it does not involve the recycling of high-vacuum recyclables

Method used

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  • Recycled ester, preparation method thereof and application of recycled ester in preparation of HZY3 brake fluid
  • Recycled ester, preparation method thereof and application of recycled ester in preparation of HZY3 brake fluid
  • Recycled ester, preparation method thereof and application of recycled ester in preparation of HZY3 brake fluid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] First prepare reclaimed ester, preparation steps are as follows:

[0024] (1) Low vacuum esterification stage: Add 100kg of boric acid with a purity ≥ 99.9%, 0.05kg of analytically pure phosphorous acid, and 1,800kg of high-vacuum recyclate into the reactor. Carry out the dehydration reaction at -165°C, control the heating rate ≤ 5°C / h, and the reaction time ≥ 24h. When the reaction temperature reaches 160°C ~ 165°C, heat slowly, then keep it at 165°C for 1h, and cool down after no moisture slips out to room temperature;

[0025] (2) High-vacuum esterification stage: Under the conditions of vacuum degree ≥ 0.096Mpa and temperature 155-180 ℃, carry out micro-dehydration reaction, control the reaction time ≥ 24h, and recover the ester after the reaction is completed.

[0026] Next, prepare HZY3 brake fluid, its preparation steps are as follows: in the reaction kettle of 1.5T, add polyethylene glycol methyl ether 250kg successively; Trihydroxypolyoxypropylene ether: 35kg;...

Embodiment 2

[0031] Using the recycled ester prepared in Example 1 to prepare HZY3 brake fluid, the preparation steps are as follows: in a 1.5T reactor, add 200 kg of polyglycol methyl ether; trihydroxypolyoxypropylene ether: 25 kg; recycled ester: 300 kg ; Diethylene glycol: 100kg; Triethylene glycol monobutyl ether 180kg; Tetraethylene glycol dimethyl ether: 100kg; Tolyl benzotriazole: 6kg; 4-hydroxyphenyl) propane (bisphenol A): 8kg parts; tetrakis [β-(3,5-di-tert-butyl-4-hydroxyphenyl) propionate] pentaerythritol ester: 6kg parts; polypropylene glycol 2000: 0.12 kg; sodium nitrite: 1.5kg, then add diisopropanolamine to adjust the pH value to above 7.5, then continue to stir for 4 hours, filter through a 0.1um filter and pack separately to obtain HZY3 brake fluid.

[0032] According to the requirements of the special durable metal corrosion experiment, the technical indicators of the HZY3 brake fluid prepared in Example 1 were tested, and the test results are shown in Table 2 below.

...

Embodiment 3

[0036] Using the recycled ester prepared in Example 1 to prepare HZY3 brake fluid, the preparation steps are as follows: in a 1.5T reactor, add polyglycol methyl ether: 150kg; trihydroxypolyoxypropylene ether: 20kg; recycled ester: 450kg; diethylene glycol: 100kg; triethylene glycol monobutyl ether: 200kg; tetraethylene glycol dimethyl ether: 50kg; methyl benzotriazole: 8kg; dioctylaniline: 10kg; 2,2- Bis(4-hydroxyphenyl)propane (bisphenol A): 10kg; tetrakis[β-(3,5-di-tert-butyl-4-hydroxyphenyl) propionate] pentaerythritol ester: 5kg; polypropylene glycol 2000: 0.2 kg; sodium nitrite: 0.5kg, then add diisopropanolamine to adjust the pH value to above 7.5, then continue to stir for 4 hours, filter through a 0.1um filter and pack separately to obtain HZY3 brake fluid.

[0037] According to the requirements of the special durable metal corrosion experiment, the technical indicators of the HZY3 brake fluid prepared in Example 1 were tested, and the test results are shown in Table ...

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Abstract

The invention relates to recycled ester, a preparation method thereof and application of the recycled ester in preparation of HZY3 brake fluid. The preparation method of the recycled ester comprises the following steps of adding boric acid, phosphorous acid and the high-vacuum recycled material into a reaction kettle according to a mass ratio of 1: 0.0005: 18, carrying out dehydration reaction under the conditions that the vacuum degree is 0.060-0.065 Mpa and the temperature is 140-165 DEG C, controlling the temperature rise speed to be less than or equal to 5 DEG C / h and the reaction time tobe more than or equal to 24 hours, slowly heating when the reaction temperature reaches 160-165 DEG C, then carrying out heat preservation at 165 DEG C for 1 hour, and cooling to normal temperature after no moisture slides out, and carrying out a trace dehydration reaction under the conditions that the vacuum degree is greater than or equal to 0.096 Mpa and the temperature is 155-180 DEG C, controlling the reaction time to be greater than or equal to 24 hours, and obtaining the recycled ester after the reaction is finished. In the preparation process of the recycled ester, a high-vacuum recycled material is utilized, so that the production cost of the brake fluid can be reduced, and the environment can be protected.

Description

technical field [0001] The invention relates to the technical field of brake fluid for automobile brake systems, in particular to a recycled ester, a preparation method thereof and an application thereof in preparing HZY3 brake fluid. Background technique [0002] At present, the mainstream products in the world are HZY3, HZY4, HZY5 type brake fluids with alcohol ether borate as the main raw material, and HZY3, HZY4 borate type synthetic brake fluids have been widely used in the world. The use of HZY5 type brake fluid is less, the main reason is its higher price. At present, the retail market is still widely dominated by HZY3 brake fluids. Most of the HZY3 brake fluids are mainly formulated with alcohol ethers. This type of brake fluid generally has the disadvantage of strong hygroscopicity, and it is easy to Absorb water, bring great hidden danger to safety. [0003] Brake fluid is the working medium for transmitting pressure in hydraulic transmission, and its performance...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C10M139/00C07F5/04C10M161/00C10N30/02C10N30/12C10N40/08
CPCC07F5/04C10M139/00C10M161/00C10M2201/083C10M2207/024C10M2207/04C10M2207/046C10M2207/283C10M2209/105C10M2215/042C10M2215/06C10M2215/223C10M2227/061
Inventor 陶佃彬杨飞单猛邹密周凯军曹云龙
Owner 张家港迪克汽车化学品有限公司
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