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Preparation method of nitrogen-containing thiophosphoric acid derivative
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A derivative, thiophosphoric acid technology, applied in the petrochemical field, can solve the problems of insufficient extreme pressure anti-wear and anti-wear properties, unstable lubricating oil additives, turbidity, etc., to achieve good extreme pressure and anti-wear properties, low temperature Good fluidity and stable performance
Inactive Publication Date: 2021-10-19
沈阳华仑润滑油添加剂有限公司
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Problems solved by technology
[0002] The operation of equipment is inseparable from lubricating oil additives, and lubricating oil cannot be separated from lubricating oil additives. Lubricating oil additives are the essence of various modern high-grade lubricating oils. At present, there is a large demand for lubricating oils in the market, which leads to The market demand for lubricating oil additives is also constantly increasing. At present, the properties of lubricating oil additives in the market are unstable, and turbidity will appear when stored at low temperature or for a long time, and their extreme pressure and anti-wear properties cannot meet the needs of high-end products. Therefore, we have designed a preparation method of nitrogen-containing derivatives of sulfuric acid to solve the above problems
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Embodiment 1
[0018] A preparation method of nitrogen-containing derivatives of sulfuric acid, comprising the following steps;
[0019] S1: Prepare a reaction kettle with a condensing reflux device, a thermometer, a sealed stirring rod and a hydrogensulfide absorption device;
[0020] S2: Put 75g of n-butanol and 130g of isooctyl alcohol into the reaction kettle, and add 111g of phosphorus pentasulfide in batches under stirring at room temperature. The reaction time is 2.5h;
[0021] S3: After the reaction is completed, adjust the temperature of the reactor to <30°C, and start adding 60g of propylene oxide dropwise under the liquid surface. After the dropwise addition, adjust the temperature to 60-65°C, and the reaction time is 2h;
[0022] S4: After the reaction is completed, add 30g of formaldehyde and 92.5 dodecylamine to the reaction kettle for reaction, heat to 85±5°C for 3 hours, then raise the temperature to 105-120°C, and dehydrate under the vacuum degree of -0.9~-1.0MPa After 2 ...
Embodiment 2
[0024] A preparation method of nitrogen-containing derivatives of sulfuric acid, comprising the following steps;
[0025] S1: Prepare a reaction kettle with a condensing reflux device, a thermometer, a sealed stirring rod and a hydrogensulfide absorption device;
[0026] S2: Put 88g of n-butanol and 100g of isooctyl alcohol into the reaction kettle, and add 111g of phosphorus pentasulfide in batches under stirring at room temperature. The reaction time is 2.5h;
[0027] S3: After the reaction is completed, adjust the temperature of the reactor to <30°C, and start adding 60g of propylene oxide dropwise under the liquid surface. After the dropwise addition, adjust the temperature to 60-65°C, and the reaction time is 2h;
[0028] S4: After the reaction is completed, add 30g of formaldehyde and 92.5 dodecylamine to the reaction kettle to react, heat to 85±5°C for 3 hours, then raise the temperature to 105-120°C, and dehydrate under the vacuum degree of -0.9~-1.0MPa After 2 hour...
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Abstract
The invention discloses a preparation method of a nitrogen-containing thiophosphoric acid derivative. The preparation method is characterized by comprising the following steps: (a) reacting C4-C8 monohydric alcohol with phosphorus pentasulfide to obtain an intermediate dialkyl thiophosphate; (b) dropwise adding alkylene oxide into the product in the step (a) at low temperature to obtain a product dialkyl phosphorodithioate; and (c) adding C1-C4 aldehyde and C12-C18 alkyl primary amine into the product obtained in the step (b) for reaction, and dehydrating to obtain the lubricating oil additive. The nitrogen-containing thiophosphoric acid derivative provided by the invention has the advantages of reasonable design, good low-temperature fluidity, stable performance and good extreme pressure wear resistance, and meets the performance requirements of medium and heavy load vehicles and industrial gear oil.
Description
technical field [0001] The invention relates to the field of petrochemical technology, in particular to a preparation method of nitrogen-containing derivatives of phosphoric acidsulfur. Background technique [0002] The operation of equipment is inseparable from lubricating oil additives, and lubricating oil cannot be separated from lubricating oil additives. Lubricating oil additives are the essence of various modern high-grade lubricating oils. At present, there is a large demand for lubricating oils in the market, which leads to The market demand for lubricating oil additives is also constantly increasing. At present, the properties of lubricating oil additives in the market are unstable, and turbidity will appear when stored at low temperature or for a long time, and their extreme pressure and anti-wear properties cannot meet the needs of high-end products. Therefore, we have designed a preparation method of nitrogen-containing derivatives of sulfuric acid to solve the ...
Claims
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