Preparation method of organic three-nuclear molybdenum additive
A technology of trinuclear molybdenum and additives, applied in the field of lubricant additives, can solve the problems of the total synthesis technology without trinuclear molybdenum additives, difficulty in forming a trinuclear molybdenum structure with molybdenum content, unfavorable health and environmental protection, etc. R & D and marketing, excellent anti-wear performance, low cost effect
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Embodiment 1
[0027] The preparation method of the present embodiment comprises the following steps:
[0028] Step 1, the preparation of tetrahydrocarbyl thiuram disulfide: mix ethanol and distilled water in a volume ratio of 2:1, then add sodium hydroxide to dissolve, and obtain an aqueous ethanol solution with a mass concentration of 5% sodium hydroxide after dissolving. Take 100mL of sodium hydroxide aqueous ethanol solution and add it to a 250mL three-necked flask, then add 5mol of dibutyl secondary amine, and then slowly add carbon disulfide dropwise at a rate of 0.05mL / s under ice-water bath, wherein dibutyl secondary amine and carbon disulfide The molar ratio is 1.35:1. After the dropwise addition, stir at a constant temperature for 2 hours at a temperature of 30°C, then add 5mL of hydrogen peroxide (analytical pure), and react at a constant temperature for 1 hour. After vacuum concentration and evaporation to dryness, the intermediate product disulfide Tetrahydrocarbylthiuram;
[0...
Embodiment 2
[0037] The preparation method of the present embodiment comprises the following steps:
[0038] Step 1, the preparation of tetrahydrocarbyl thiuram disulfide: mix ethanol and distilled water in a volume ratio of 3:1, then add sodium hydroxide to dissolve, and obtain an aqueous ethanol solution with a mass concentration of 5% sodium hydroxide after dissolving. Take 100mL of sodium hydroxide aqueous ethanol and add it to a three-necked flask, then add 5mol of dioctyl secondary amine, and then slowly add carbon disulfide dropwise at a rate of 0.05mL / s under ice-water bath, wherein the moles of dioctyl secondary amine and carbon disulfide The ratio is 1.2:1. After the dropwise addition, stir at a constant temperature for 2 hours at a temperature of 30°C, then add 4 mL of hydrogen peroxide, react at a constant temperature for 1 hour, and concentrate and evaporate to dryness in a vacuum to obtain the intermediate product tetrahydrocarbyl thiuram disulfide;
[0039] Step 2, the prepa...
Embodiment 3
[0046] The preparation method of the present embodiment comprises the following steps:
[0047] Step 1, the preparation of tetrahydrocarbyl thiuram disulfide: mix ethanol and distilled water in a volume ratio of 1:1, then add sodium hydroxide to dissolve, and obtain an ethanol aqueous solution with a mass concentration of 5% sodium hydroxide after dissolving. Take 100mL of sodium hydroxide aqueous ethanol and add it to a three-necked flask, then add 5mol of ditridecylamine, and then slowly add carbon disulfide dropwise at a rate of 0.05mL / s under an ice-water bath, wherein ditridecylamine and carbon disulfide The molar ratio is 1.5:1. After the dropwise addition, stir at a constant temperature for 2 hours at a temperature of 30°C, then add 6mL of hydrogen peroxide, and react at a constant temperature for 1 hour. Mu;
[0048] Step 2, the preparation of organic trinuclear molybdenum additive crude product: the mixed solvent of tetrahydrocarbyl thiuram disulfide and 20mL obtaine...
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