Preparation method of sulfur-phosphorus-nitrogen type extreme-pressure anti-wear agent
An extreme pressure anti-wear agent, sulfur phosphorus nitrogen technology, applied in the field of anti-wear agents, can solve problems such as poor copper sheet corrosion, system copper sheet corrosion, and equipment corrosion, and achieve environmental protection, corrosion reduction, and stable synthesis methods Effect
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[0040] Such as figure 1 As shown, the present invention provides a preparation method of sulfur phosphorus nitrogen type extreme pressure antiwear agent, comprising:
[0041] Step 1, adding propylene oxide dropwise to the dialkyl phosphorodithioate to carry out the first esterification reaction to obtain the first product; wherein,
[0042] The first esterification reaction is:
[0043]
[0044] In the formula, R 1 with R 2 for C 4 ~C 12 Alkyl group; the reaction temperature of the first esterification reaction is 70-85°C, and the reaction time is 1-2h; the acid value of the system is detected during the reaction process, and the second esterification reaction can be carried out when the acid value is not greater than 10KOHmg / g.
[0045] The specific steps are:
[0046] Add 0.32mol of dialkyl phosphorodithioate into a four-necked flask equipped with a thermometer, a reflux condenser, a dropping funnel and a stirrer, and slowly add 0.33mol of propylene oxide dropwise t...
Embodiment 1
[0076] The invention provides a preparation method of sulfur phosphorus nitrogen type extreme pressure antiwear agent, comprising:
[0077] Step 1, the first esterification reaction: add O-n-butyl-O'-2-ethylhexyl dialkyldithio Phosphate ester 0.32mol, slowly add 0.33mol propylene oxide dropwise to the reaction system under the condition of stirring, control the temperature of the system not to exceed 30°C during the dropwise addition process, the appropriate time for the dropwise addition is 45min, and raise the temperature to 75°C after the dropwise addition is completed ℃, heat preservation reaction for 1-2h, and detect the acid value of the system during the process. When the acid value is not greater than 10KOHmg / g, the next step reaction can be carried out.
[0078] Step 2, the second esterification reaction: Slowly add PCl dropwise to the above reaction system through the dropping funnel 3 , the dropping time is preferably 45min. During the dropping process, the reactio...
Embodiment 2
[0083] The invention provides a preparation method of sulfur phosphorus nitrogen type extreme pressure antiwear agent, comprising:
[0084] Replacing O-n-butyl-O'-2-ethylhexyl dialkyl phosphorodithioate with O-sec-butyl-O'-2-ethylhexyl dialkyl phosphorodithioate, other operations Consistent with the description in Example 1.
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