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Preparation method of nano antimony thioantimonate

A technology of antimony thioantimonate and sodium thioantimonate, applied in antimonate/antimonite, nanotechnology, nanotechnology and other directions, can solve the problem of easy hydrolysis of sodium thioantimonate and easy hydrolysis of antimony trihalide. , waste of environmental water and other problems, to achieve the effect of improving the utilization rate of raw materials, improving the stability and purity, and improving the leaching rate

Inactive Publication Date: 2018-06-15
广西生富锑业科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method reduces the generation of hydrogen sulfide and elemental sulfur, the antimony trihalide is easy to hydrolyze, and a large amount of organic solvents are needed, resulting in waste and pollution of environmental water bodies.
The third method is to use antimony trioxide instead of antimony trihalide to directly react with sodium thioantimonate in aqueous solution to obtain antimony thioantimonate with less free sulfur, but this method needs to be carried out under acidic conditions. Sodium antimonate is easily hydrolyzed, resulting in a decrease in yield

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] The preparation method of nano antimony thioantimonate of the present invention comprises the following steps:

[0034] (1) Add 6.15 mol of sodium sulfide to purified water at a temperature of 50°C under stirring conditions, then add 2.02 mol of elemental sulfur and 1 mol of antimony trioxide, maintain the reaction system at 55°C and stir for 28 minutes, then pump Filter, obtain filtrate, the liquid-solid ratio of described reaction system is 10mL / g;

[0035] (2) cooling and crystallizing the filtrate of step (1) in a low-temperature tank at 0° C. for 20 minutes, separating the crystals and crystallization mother liquor, and obtaining crude crystals of sodium thioantimonate;

[0036] (3) adding the crude crystals of sodium thioantimonate in step (2) into purified water at a temperature of 45° C., stirring for 3 minutes and filtering to obtain a saturated sodium thioantimonate solution;

[0037] (4) recrystallize the saturated sodium thioantimonate solution in step (3) ...

Embodiment 2

[0043] The preparation method of nano antimony thioantimonate of the present invention comprises the following steps:

[0044] (1) Add 6.17 mol of sodium sulfide to purified water at a temperature of 54°C under stirring conditions, then add 2.04 mol of elemental sulfur and 1 mol of antimony trioxide, maintain the reaction system at 60°C and stir for 27 minutes, then pump Filter, obtain filtrate, the liquid-solid ratio of described reaction system is 9mL / g;

[0045] (2) cooling and crystallizing the filtrate of step (1) in a low-temperature tank at 1° C. for 21 minutes, separating the crystals and crystallization mother liquor, and obtaining crude crystals of sodium thioantimonate;

[0046] (3) Add the crude crystals of sodium thioantimonate in step (2) into purified water at a temperature of 42° C., stir for 3.3 minutes and filter to obtain a saturated sodium thioantimonate solution;

[0047] (4) recrystallize the saturated sodium thioantimonate solution in step (3) at 1° C., o...

Embodiment 3

[0053] The preparation method of nano antimony thioantimonate of the present invention comprises the following steps:

[0054] (1) Add 6.19 mol of sodium sulfide to purified water at a temperature of 57°C under stirring conditions, then add 2.07 mol of elemental sulfur and 1 mol of antimony trioxide, maintain the reaction system at 66°C and stir for 26 minutes, then pump Filter, obtain filtrate, the liquid-solid ratio of described reaction system is 8mL / g;

[0055] (2) cooling and crystallizing the filtrate of step (1) in a low-temperature tank at 2° C. for 22 minutes, separating crystals and crystallization mother liquor, and obtaining crude crystals of sodium thioantimonate;

[0056] (3) Add the crude crystals of sodium thioantimonate in step (2) into purified water at a temperature of 39° C., stir for 3.7 minutes and filter to obtain a saturated sodium thioantimonate solution;

[0057] (4) recrystallize the saturated sodium thioantimonate solution in step (3) at 2° C., obt...

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PUM

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Abstract

The invention discloses a preparation method of nano antimony thioantimonate, wherein the preparation method comprises the steps: adding a sodium thioantimonate solution into a complex solution of trivalent antimony, dispersing with ultrasonic waves, controlling the temperature of the reaction system at 20-35 DEG C, adjusting the pH value of the reaction system to 6.3-7.8 with hydrochloric acid, after completion of addition of the sodium thioantimonate solution, continuing to disperse for 10-15 min by ultrasonic waves, filtering to take a filter residue, washing the filter residue with a potassium sodium tartrate solution and purified water, and grinding for 3-5 h by a ball mill, and thus obtaining the product. The content of sulfur in antimony thioantimonate obtained by the preparation method provided by the invention is low, the product is stable and pure, the yield is high, the properties are good, the particles are in nanoscale, and the nano antimony thioantimonate has the advantages of good compatibility with lubricating grease, good extreme pressure wear resistance and good lubrication performance; as an additive, the nano antimony thioantimonate has various properties far beyond the requirements of the national standards on extreme pressure lubricating grease, can be industrially produced and has a good application prospect.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a preparation method of nano antimony thioantimonate. Background technique [0002] Antimony thioantimonate is an excellent extreme pressure anti-wear lubricating grease additive, which can significantly improve the sintering load and load capacity of lubricating grease, reduce the friction coefficient, and is widely used in the fields of mining machinery, ships and military equipment. Antimony thioantimonate has good compatibility with all base greases such as lithium-based grease, clay grease, silicon grease and composite aluminum-based grease, and is suitable for various alloys including chromium tool steel and stainless steel which are difficult to lubricate It has good lubricating effect and good thermal stability, and is suitable for special situations such as high vacuum, high load, and radiation. [0003] At present, there are three main methods for preparing antimony th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G30/02B82Y30/00B82Y40/00C10M125/24C10N30/04C10N30/06
CPCB82Y30/00B82Y40/00C01G30/02C10M125/24C10M2201/084C10N2030/04C10N2030/06C10N2020/06
Inventor 韦竣严韦建初兰岱龙何正军陆宏卫曹应科卢忠讲
Owner 广西生富锑业科技股份有限公司
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