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Zinc dialkyl dithiophosphate and preparation method thereof

A technology of zinc dialkyldithiophosphate and sulfuric acid, which is applied in the field of rubber vulcanization accelerators, can solve the problems of increasing the application of catalyst ammonia water, poor anti-aging and yellowing resistance, and severe local reactions, and meet the production process conditions Ease of control, good yellowing resistance, excellent rubber properties

Pending Publication Date: 2021-09-24
XINXIANG RICHFUL LUBE ADDITIVE CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in this preparation method, the application of catalyst ammonia water is increased, which increases the difficulty of the post-processing of the product and increases the production cost.
In addition, adding sulfuric acid and zinc oxide at the same time will cause severe local reactions, and the production process conditions are difficult to control and stabilize, which is not conducive to stable production
[0005] At present, zinc dialkyldithiophosphate on the market, as an accelerator, has poor anti-aging and yellowing resistance in vulcanized rubber, which can no longer meet the market's demand for performance.

Method used

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  • Zinc dialkyl dithiophosphate and preparation method thereof
  • Zinc dialkyl dithiophosphate and preparation method thereof
  • Zinc dialkyl dithiophosphate and preparation method thereof

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preparation example Construction

[0025] A kind of preparation method of zinc dialkyl dithiophosphate, such as figure 1 Shown, described preparation method comprises:

[0026] Step S1: react alcohol with phosphorus pentasulfide to prepare sulfuric acid. Wherein, alcohol can be a kind of alcohol, also can be the mixture of two kinds of alcohols, for example n-butanol and isooctyl alcohol, or their mixture.

[0027] Step S2: react phosphoric acid with ammonia water to prepare ammonium salt.

[0028] Step S3: reacting the ammonium salt with zinc nitrate to prepare zinc dialkyldithiophosphate.

[0029] Step S4: Separating the reaction product of step S3 and washing it with distilled water; removing water under reduced pressure; adding a filter aid and filtering to obtain a finished product of zinc dialkyldithiophosphate.

[0030] Among them, ammonia water participates in the reaction, and the final product is ammonium nitrate, which is convenient for the treatment of later products; the reaction will not cause ...

Embodiment 1

[0046] Add 14.7g (10% of the total amount) n-butanol and isooctyl alcohol (mix well) in the four-necked flask, and connect the tail gas treatment device, and the phosphorus pentasulfide of 80.0g (the P content of the selected phosphorus pentasulfide is 28.1-28.2 %) into the flask, after heating up to 70°C, start to drop the remaining 132.3g of mixed alcohol to ensure that the temperature of the reaction system does not exceed 75°C, after the addition, raise the temperature of the system to 95°C and keep it for about 2.0h, and cool down after the reaction To below 20 ° C, sulfuric acid is obtained.

[0047] Add 25.0 g of ammonia water into the reaction system dropwise in 6 times at intervals of 15 minutes to ensure that the reaction system does not exceed 35° C. After the addition, keep warm for 1.0 h to obtain the ammonium salt.

[0048] Will prepare 120.0g Zn(NO3) 2 (a solution with a mass fraction of 40%) was added to a constant pressure dropping funnel, and evenly added dr...

Embodiment 2

[0050] It is 27.9-28.1% that the phosphorus pentasulfide in the embodiment 1 is changed into the phosphorus pentasulfide of P content, all the other parts are kept the same with embodiment 1, make light yellow transparent finished product, be recorded as: product 2.

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PUM

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Abstract

The invention discloses zinc dialkyl dithiophosphate and a preparation method thereof. The preparation method comprises the steps of S1, enabling alcohol and phosphorus pentasulfide to react to prepare thiophosphoric acid; S2, reacting thiophosphoric acid with ammonia water to prepare ammonium salt; and S3, reacting the ammonium salt with zinc nitrate to prepare zinc dialkyl dithiophosphate. Ammonia water participates in the reaction, the final product is ammonium nitrate, later product treatment is facilitated, local violent reaction cannot be caused in the reaction, and production process conditions are easy to control; and rubber vulcanized by the zinc dialkyl dithiophosphate product has good yellowing resistance, the vulcanization performance is excellent, and the vulcanized rubber performance is excellent.

Description

technical field [0001] The invention relates to the technical field of rubber vulcanization accelerators, in particular to a zinc dialkyl dithiophosphate and a preparation method thereof. Background technique [0002] Rubber vulcanization accelerator is a general term for a class of substances that can accelerate the vulcanization speed, reduce the vulcanization temperature, reduce the amount of vulcanization agent, and improve the physical and mechanical properties of rubber. It is one of the essential basic materials for the rubber industry. For light-colored vulcanizates, anti-yellowing performance is an important indicator of its quality, and it is also an indicator that users are most concerned about and the easiest to detect. The aging ability has a decisive function. Ultraviolet radiation and heat will oxidize and yellow the rubber surface, and deteriorate the mechanical properties. Adding accelerators with poor mechanical properties to the rubber will make the hardn...

Claims

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Application Information

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IPC IPC(8): C07F9/17C08K5/5398C08L21/00
CPCC07F9/17C08K5/5398C08L2201/08C08L21/00
Inventor 王建王倩倩徐坤范金凤
Owner XINXIANG RICHFUL LUBE ADDITIVE CO LTD
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