Preparation method of diisooctyl dithiophosphate zinc salt
A technology of zinc diisooctyl dithiophosphate and zinc isooctyl dithiophosphate, applied in the field of preparation of zinc diisooctyl dithiophosphate with low acid value, can solve the problem of affecting the anti-corrosion performance of hydraulic oil and corrosion resistance, affect the anti-emulsification performance and filterability of hydraulic oil, affect the filterability and anti-emulsification of hydraulic oil, etc., to achieve the effect of improving performance, reducing acid value, and expanding the scope of application
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[0038] The invention provides a kind of preparation method of zinc diisooctyl dithiophosphate, comprising the following steps:
[0039] A) After reacting isooctyl alcohol, phosphorus pentasulfide and zinc oxide, a reaction intermediate system is obtained;
[0040] B) After cooling down the reaction intermediate system obtained in the above steps, adding an organic amine to react again to obtain zinc diisooctyl dithiophosphate.
[0041] In the invention, firstly, after reacting isooctanol, phosphorus pentasulfide and zinc oxide, a reaction intermediate system is obtained.
[0042] The present invention does not have special limitation to the addition amount of described isooctyl alcohol and phosphorus pentasulfide, can get final product with the routine consumption of this type of reaction well known to those skilled in the art, and those skilled in the art can select according to actual production situation, quality requirement and product requirement. Adjustment, the molar r...
Embodiment 1
[0086] Add 500kg of isooctyl alcohol into the reaction kettle as a base material, add 1000kg of solid phosphorus pentasulfide, and stir to form a slurry. Gradually add 1865 kg of isooctyl alcohol into the reactor, and keep the temperature at 100-105°C. After adding iso-octanol, maintain 110° C. for 1 hour, and filter to obtain 3184 kg of sulfuric acid.
[0087] Add 400kg of the last batch of finished products into the reaction kettle as a base material, add 412kg of zinc oxide and stir at high speed to disperse into a uniform slurry and heat up to 50°C, then slowly add 3187kg of sulfuric acid to maintain the temperature in the kettle at 90-110°C. After adding sulfuric acid, keep the temperature at 105°C for 2 hours, then cool down to 50°C and add 9.5kg of triethylamine to neutralize the free sulfuric acid, continue to react for 20min, vacuum remove the water generated by the reaction and triethylamine not involved in the reaction. Ethylamine. Directly filter to obtain produc...
Embodiment 2
[0090] Add 500kg of isooctyl alcohol into the reaction kettle as a base material, add 1000kg of solid phosphorus pentasulfide, and stir to form a slurry. Gradually add 1865 kg of isooctyl alcohol into the reactor, and keep the temperature at 100-105°C. After adding iso-octanol, the reaction was maintained at 110° C. for 1 hour, and 3187 kg of phosphoric acid was obtained by filtration.
[0091] Add 400kg of the last batch of finished products into the reaction kettle as a base material, add 412kg of zinc oxide and stir at a high speed to disperse into a uniform slurry and heat up to 50°C, then slowly add 3187kg of sulfuric acid and 9.5kg of triethylamine respectively to maintain the kettle The internal temperature is 90-110°C. After the sulfuric acid was added, the temperature was maintained at 105°C for 2 hours, and the water generated by the reaction and triethylamine not involved in the reaction were removed in a vacuum. Directly filter to obtain product 3895kg, i.e. zinc...
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