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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

Active Publication Date: 2020-07-28
XINXIANG RICHFUL LUBE ADDITIVE CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007]1. When the sulfur phosphorus nitrogen type complex ester extreme pressure antiwear agent is added to the gear oil compound, it will cause serious corrosion of the copper sheet of the system, often reaching 2d- Level 3a;
[0008]2. When synthesizing the extreme-pressure anti-wear agent disclosed in patent CN1033811A, in order to obtain a better copper corrosion effect, it is often necessary to synthesize it at a higher temperature, which will It causes -P=S- to transform into -P=O- and generates a certain amount of acid gas; on the one hand, it will cause corrosion to equipment, and on the other hand, it will also cause damage to the environment;
[0009]3. When synthesizing the polyphosphoric acid double ester amine salt type extreme pressure anti-wear agent disclosed in the patent US5573696A, its copper sheet corrosion effect is relatively poor, often reaching the level of 2d-2e

Method used

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  • Preparation method of sulfur-phosphorus-nitrogen type extreme-pressure anti-wear agent
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  • Preparation method of sulfur-phosphorus-nitrogen type extreme-pressure anti-wear agent

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preparation example Construction

[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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Abstract

The invention discloses a preparation method of a sulfur-phosphorus-nitrogen extreme-pressure anti-wear agent, which comprises the following steps: dropwisely adding propylene oxide into dialkyl dithiophosphate to carry out first esterification reaction, thereby obtaining a first product, dropwise adding phosphorus chloride into the reaction system of the first product to carry out a second esterification reaction to obtain a second product, adding monochloromethyl sulfide into the reaction system of the second product for substitution reaction to obtain a third product, adding m-CPBA into thereaction system of the third product for oxidation reaction to obtain a fourth product, and adding paraformaldehyde and fatty amine into the reaction system of the fourth product to carry out Mannichreaction, thereby obtaining the sulfur-phosphorus-nitrogen extreme-pressure anti-wear agent. The synthesis method is stable, corrosion of acid gas to equipment is effectively reduced in the synthesisprocess, the environment is protected, and the copper sheet corrosion condition and the liquid phase corrosion condition of a system can be effectively improved when the extreme pressure anti-wear agent is added into a gear oil complexing agent.

Description

technical field [0001] The invention relates to the technical field of antiwear agents, in particular to a preparation method of a sulfur phosphorus nitrogen type extreme pressure antiwear agent. Background technique [0002] Extreme pressure and antiwear performance is an extremely important performance of industrial gear oils. Gear oils often meet the requirements for extreme pressure and antiwear performance by introducing extreme pressure and antiwear agents; as far as the current research situation is concerned, sulfur, phosphorus and nitrogen type Extreme pressure agents are widely used in various gear oil compound formulations because of their excellent high-temperature stability, high-efficiency abrasion resistance, corrosion resistance, anti-oxidation stability, compatibility and multi-effect of additives. [0003] The research on parathion, phosphorus and nitrogen type extreme pressure antiwear agents in foreign countries started in the 1960s, and my country has al...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/40C10M137/14C10N30/06C10N30/12C10N40/04
CPCC07F9/4006C07F9/4071C10M137/14
Inventor 袁小二徐坤范金凤
Owner XINXIANG RICHFUL LUBE ADDITIVE CO LTD
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