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Preparation method of zinc dialkyldithiophosphate and application of hydrogen peroxide

A technology of dialkyl dithiophosphoric acid and zinc dialkyl dithiosulfate, which is applied in the direction of chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, and lubricating compositions, which can solve the problems affecting product breakage Milk and filtration performance and other problems, to achieve the effect of excellent promotion effect, excellent filterability, and simplified operation steps

Pending Publication Date: 2020-02-28
锦州康泰润滑油添加剂有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, the accelerators used in the above method are still traditional acetic acid, ammonia water, low-molecular alcohol, etc., because acetic acid, ammonia water and other substances will remain in the product, which will affect the demulsification and filtration performance of the product

Method used

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  • Preparation method of zinc dialkyldithiophosphate and application of hydrogen peroxide

Examples

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Effect test

preparation example

[0034] The preparation method of bis-octyl dithiophosphoric acid:

[0035] Add 4.12 mol of isooctyl alcohol into the reaction flask, add 1 mol of phosphorus pentasulfide dropwise, the addition time is 2 hours, the temperature gradually rises to 70-90°C, after the phosphorus pentasulfide is completely added, continue the reaction at 80-90°C for 2 hours, and depressurize Distill for 0.5h to remove unreacted alcohol, absorb the generated hydrogen sulfide, and filter to obtain bis-octyl dithiophosphoric acid for later use.

Embodiment 1

[0037] The preparation method of bis-octyl zinc dithiophosphate follows the steps below:

[0038] Add 10g of 150SN, 40g of zinc dioctyldithiophosphate, and 25g of zinc oxide to the three-necked flask at room temperature, stir evenly, raise the temperature to 60°C, add 20g of 5wt% hydrogen peroxide (5wt% of sulfuric acid) and stir for 0.5h, start dropwise to prepare Example of sulfuric acid 200g, drop time 60min, drop temperature 90°C, maintain 80-90°C for 2h, heat up to 100°C, vacuum 650mmHg, remove water and alcohol under reduced pressure for 1h, add filter aid 2g to filter.

[0039] Filtration speed: 16.2g / min.cm 2 , Filtration yield: 98.0%;

[0040] Product analysis results: zinc content 9.21%, sulfur content 14.6%, phosphorus 7.1%, pH 6.8, chroma: <0.5;

[0041] Thermal decomposition temperature test: 243°C.

Embodiment 2

[0043] The preparation method of bis-octyl zinc dithiophosphate follows the steps below:

[0044] Add 50g of 100SN and 29g of zinc oxide to the there-necked flask at normal temperature, stir evenly, add 0.4g of 100wt% hydrogen peroxide (0.2wt% of sulfuric acid) and stir for 0.1h when the temperature rises to 35°C, start to dropwise add 200g of sulfuric acid in the preparation example, dropwise The time is 300min, the dropping temperature is 35-100°C, and the reaction is maintained at 90-100°C for 0.1h. After the reaction, the temperature is raised to 100°C, the vacuum degree is 640mmHg, the water and alcohol are removed under reduced pressure for 3h, and diatomite filter aid is added 2g filter.

[0045] Filtration speed: 18.2g / min.cm 2 , Filtration yield: 99.0%;

[0046] Product analysis results: zinc content 8.9%, sulfur content 13.7%, phosphorus 6.7%, pH 6.5, chroma: <0.5;

[0047] Thermal decomposition temperature test: 241°C.

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Abstract

The invention provides a preparation method of zinc dialkyldithiophosphate and application of hydrogen peroxide. The preparation method of the zinc dialkyldithiophosphate comprises the following steps: (A) adding base oil and / or a small amount of zinc dialkyldithiophosphate, zinc oxide and hydrogen peroxide, and stirring; and (B) adding dialkyl dithiophosphoric acid to react, and filtering to obtain the zinc dialkyldithiophosphate. The hydrogen peroxide shows a good promoting effect in the preparation process of the zinc dialkyldithiophosphate, and decomposition products are water and oxygen,so that the decomposition products are easy to separate from a target product and free of residues. The process for preparing the zinc dialkyldithiophosphate (hereinafter referred to as ZDDP) by taking the hydrogen peroxide as a saponification accelerant has the characteristics of easiness in product filtration, less filter residue, light color, high pH value, good thermal stability and demulsibility, high zinc oxide utilization rate, greatly improved product quality and yield, greatly reduced waste residue and obviously improved production benefit.

Description

technical field [0001] The invention relates to the field of preparation of zinc dialkyldithiophosphate, in particular to a preparation method of zinc dialkyldithiophosphate and application of hydrogen peroxide. Background technique [0002] Zinc dialkyldithiophosphate is a multi-effect lubricating oil additive with excellent properties such as anti-oxidation, anti-wear, anti-friction, extreme pressure and anti-corrosion. Since its invention in the 1900s, it has been an indispensable additive in internal combustion engine oil and other oil products, and has also been widely used in gear oil, hydraulic oil and other industrial oils, and even in rubber and plastic industries. [0003] The discovery of ZDDP has a history of 80 years. During this period, many researchers have continuously improved its synthesis methods and process routes, especially the saponification process has used different accelerators to promote the production of dialkyl dithio The reaction of phosphoric ...

Claims

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Application Information

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IPC IPC(8): C07F9/17C10M137/10C10N30/08
CPCC07F9/17C10M137/10C10M2223/045
Inventor 郭松张玉石禹虎背曹宇缐伟芮大庆
Owner 锦州康泰润滑油添加剂有限公司
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