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

Inactive Publication Date: 2018-06-08
NORTHWEST INSTITUTE FOR NON-FERROUS METAL RESEARCH
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Problems solved by technology

[0004] At present, there are few domestic reports on the synthesis method of trinuclear molybdenum, and there is no total synthesis technology of trinuclear molybdenum additives. Related reports (CN 10238214 A) adopt molybdenum-containing substances to react with dialkyldithiocarbamate. In the first method, since the dialkyldithiocarbamate is dinuclear molybdenum and the molybdenum content is low, it is difficult to form a trinuclear molybdenum structure with a high molybdenum content.
Direct purchase of foreign monopoly product ammonium thirteen thiomolybdate crystals as the starting raw material, and the addition of catalytic potassium cyanide in the process is likely to produce highly toxic cyanide gas, which is not conducive to health and environmental protection, and the raw materials are limited. method is not feasible

Method used

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  • Preparation method of organic three-nuclear molybdenum additive
  • Preparation method of organic three-nuclear molybdenum additive

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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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Abstract

The invention discloses a preparation method of an organic three-nuclear molybdenum additive. The preparation method comprises the following steps: firstly, preparing tetralkyl disulfide thiuram by adopting dialkyl secondary amine, carbon disulphide, ethanol aqueous solution of sodium hydroxide and hydrogen peroxide; secondly, preparing a crude organic three-nuclear molybdenum additive by adoptingammonium trithio molybdate crystals, the tetralkyl disulfide thiuram and a mixed solvent; thirdly, performing post-treatment on the crude organic three-nuclear molybdenum additive to obtain an oily organic three-nuclear molybdenum additive. The invention creatively designs the preparation method of the organic three-nuclear molybdenum additive; the organic three-nuclear molybdenum additive is synthesized by adopting the ammonium trithio molybdate crystals and the tetralkyl disulfide thiuram; compared with the existing two-nuclear molybdenum additive, the molybdenum content is higher; under the same friction performance, the adding amount of the additive added into lubricating oil is smaller, and the friction resistance is more excellent; toxic and harmful raw materials are not used in a preparation process, the emission of the toxic and harmful gas is also avoided, and the method is green and environment-friendly.

Description

technical field [0001] The invention belongs to the technical field of lubricating oil additives, and in particular relates to a preparation method of an organic tri-nuclear molybdenum additive. Background technique [0002] As we all know, the high soot in diesel oil will enter the engine oil with the engine working, which will significantly increase the kinematic viscosity of the oil, produce yield stress at low temperature and greatly reduce the anti-wear performance, accelerate engine wear, and thus have a harmful impact on the performance of the lubricating oil. [0003] Although the traditional molybdenum disulfide, nano-molybdenum disulfide, MoDTC, MoDDP and ZnDDP have excellent performance in improving the anti-wear and anti-friction properties, they are still helpless in the face of the harm of diesel engine soot to the performance of lubricating oil. At the same time, soot Harmful ions in soot or atomic group intermediates with low-energy electrons will cause fatal...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F11/00C10M139/00C07C333/32C10N30/06
CPCC07C333/32C07F11/005C10M139/00C10M2227/09C10N2030/06
Inventor 李延超李来平张新蒋丽娟刘燕杨建
Owner NORTHWEST INSTITUTE FOR NON-FERROUS METAL RESEARCH
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