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Method for preparing dialkyl dithiophosphate

A technology of dialkyl dithiophosphate and dialkyl dithiophosphate, applied in the field of preparation of dialkyl dithiophosphate, can solve the problems of low production efficiency, long production cycle, waste gas pollution, etc. Achieve high production efficiency, low production cost, and avoid pollution

Inactive Publication Date: 2010-12-22
WEIFANG SHIHUA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The shortcomings of the existing technology are: long production cycle, low production efficiency, and many impurities in the product, serious waste gas pollution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] (1) In a 1000ml closed reaction vessel equipped with an automatic feeding device, an electric stirrer and a condenser, the condenser is connected to the 4-stage absorption conversion tower, add an isobutanol solution with a concentration of 99.5% by weight, start stirring and maintain The system pressure is -0.01MPa. When the control temperature of the automatic feeding device is set to 50°C, the automatic feeding device is used to continuously and uniformly add phosphorus pentasulfide to the isobutanol solution. The weight ratio of the phosphorus pentasulfide to the isobutanol solution The ratio was 1:4.2. After the addition, the reaction was kept for 5 hours to obtain diisobutyl dithiophosphoric acid with a concentration of 83 wt%.

[0021] (2) When the temperature is 30°C, slowly add sodium hydroxide solution with a concentration of 20 wt% into the reaction vessel, and the adding weight ratio of sodium hydroxide to diisobutyl dithiophosphoric acid is 1:1, The neutraliza...

Embodiment 2

[0024] (1) In a 1000ml closed reaction vessel equipped with an automatic feeding device, an electric stirrer and a condenser, the condenser is connected to a 6-stage absorption conversion tower, add an ethanol solution with a concentration of 99.5% by weight, start stirring, and maintain the system pressure When the control temperature of the automatic feeding device is set to 70°C, the automatic feeding device is used to continuously and uniformly add phosphorus pentasulfide to the ethanol solution. The weight ratio of the phosphorus pentasulfide to the ethanol solution is 1:4.5. After that, the reaction was kept for 4 hours to obtain diethyl dithiophosphoric acid with a concentration of 84 wt%.

[0025] (2) When the temperature is 40°C, slowly add sodium hydroxide solution with a concentration of 19% by weight into the reaction vessel, and the adding weight ratio of sodium hydroxide to diethyldithiophosphoric acid is 1:1.05. The neutralization reaction starts the tail gas produ...

Embodiment 3

[0028] (1) In a 1000ml closed reaction vessel equipped with an automatic feeding device, an electric stirrer and a condenser, the condenser is connected to a 7-stage absorption conversion tower, add isopropanol solution with a concentration of 99.5% by weight, start stirring, and maintain The system pressure is 0.03MPa, and when the control temperature of the automatic feeding device is set to 85°C, the automatic feeding device is used to continuously and uniformly add phosphorus pentasulfide to the isopropanol solution, and the weight ratio of the phosphorus pentasulfide to the isopropanol solution is 1:4.6. After the addition, the reaction is kept for 3 hours to obtain diisopropyl dithiophosphoric acid with a concentration of 85% by weight.

[0029] (2) At a temperature of 50°C, slowly add a sodium hydroxide solution with a concentration of 18% by weight to the reaction vessel, and the added weight ratio of sodium hydroxide to dipropylbutyl dithiophosphoric acid is 1:1.1. The n...

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Abstract

The invention discloses a method for preparing dialkyl dithiophosphate, comprising the following steps: (1) continuously adding phosphorus pentasulfide in an alcohol solution under stirring when the pressure is minus 0.01-0.05MPa and the temperature is 30-100 DEG C, and preserving the temperature and reacting for 2-5h to obtain dialkyl phosphorodithioicacid, wherein the weight ratio of the added phosphorus pentasulfide to the alcohol solution is 1: 4.0-4.8; and (2) under the temperature of 20-60 DEG C, adding a sodium hydroxide solution with the concentration of 15-25wt% in the dialkyl phosphorodithioicacid based on the weight ratio of 1: 1.0-1.1, and performing neutralization reaction to obtain the dialkyl dithiophosphate. In the invention, the reaction of the phosphorus pentasulfide and the alcohol solution has good effect, short reaction time, short production cycle and high product yield, and the waste gas generated by the reaction can be recycled, thus the invention is an environment-friendly and efficient production process.

Description

Technical field [0001] The invention relates to the technical field of collector preparation, in particular to a preparation method of dialkyl dithiophosphate. Background technique [0002] Dialkyl dithiophosphate is a commonly used sulfide ore collector, commonly known as black medicine. Compared with another commonly used collector xanthate, the flotation properties of black medicine have two main characteristics:( 1) The collecting power is low and the selectivity is high, especially for pyrites. Therefore, it is used as a priority flotation collector in the flotation of copper and lead-zinc sulfide ore containing high iron sulfide. Good quality concentrates can be obtained, and at the same time, many kinds of black medicine have better gold collection performance; (2) Good stability, can be used at a lower pH value without being quickly decomposed. [0003] The preparation method of dialkyl dithiophosphate is to use phosphorus pentasulfide to react with different alcohols to g...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/17
Inventor 张冶
Owner WEIFANG SHIHUA CHEM
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