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Method for preparing antimony thioantimonate based on stable reaction system

A technology of antimony thioantimonate and reaction system, which is applied in the direction of antimonate/antimonite, etc., can solve the problems of sodium thioantimonate being decomposed by acid or complicated operation, and achieves high yield and simple preparation process , product pure effect

Active Publication Date: 2013-07-24
湖南益阳生力材料科技有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Aiming at the deficiencies of the prior art, the present invention provides a method for preparing antimony thioantimonate based on a stable reaction system; it solves the problem of hydrolysis or thiolation of antimony halides under alkaline conditions existing in the preparation process of antimony thioantimonate. Sodium antimonate is decomposed by acid or complicated to operate

Method used

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  • Method for preparing antimony thioantimonate based on stable reaction system
  • Method for preparing antimony thioantimonate based on stable reaction system

Examples

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Effect test

Embodiment 1

[0025] (1) Preparation of sodium antimonate

[0026] Add 105g of antimony white to 315mL of 200g / L NaOH solution, leach at 85°C for 3.5h, continuously add 123mL of 30wt% hydrogen peroxide dropwise during leaching, cool, crystallize and filter to obtain 169g of sodium antimonate, the temperature of the solution after cooling is 5 -10°C.

[0027] (2) Preparation of sodium thioantimonate solution

[0028] Dissolve 722g of sodium sulfide nonahydrate to prepare a 668mL solution, then add 169 grams of sodium antimonate obtained in step (1), control the reaction temperature at 95°C, stir for 3.0h, cool to below 5°C, and filter to obtain thiononahydrate Sodium antimonate crystal 255.08g, this crystal configuration is 923mL, the sodium thioantimonate solution containing antimony 70g / L.

[0029] (3) Prepare antimony trichloride solution by leaching antimony white with hydrochloric acid.

[0030] Add 870mL of 37wt% concentrated hydrochloric acid and 155.3g of NaCl to make a 1600mL sol...

Embodiment 2

[0039] (1) Preparation of sodium antimonate

[0040] Add 110g of antimony white to 440mL of 250g / L NaOH solution, leaching at 80°C for 4h, continuously add 132mL of 27wt% hydrogen peroxide dropwise during the leaching process, cool, crystallize and filter to obtain 180g of sodium antimonate, the temperature of the solution after cooling is 5 -10°C.

[0041] (2) Preparation of sodium thioantimonate solution

[0042] Dissolve 840g of sodium sulfide nonahydrate to form a 900mL solution, then add 180g of sodium antimonate obtained in step (1), control the reaction temperature at 95°C, stir and react for 2.5h, cool to below 5°C, and filter to obtain thioantimony nonahydrate Sodium antimonate crystal 250g, this crystal preparation is 745mL solution, obtains the sodium thioantimonate solution containing antimony 85g / L.

[0043] (3) Prepare antimony trichloride solution by leaching antimony white with hydrochloric acid.

[0044] Add 870mL of 37wt% concentrated hydrochloric acid and...

Embodiment 3

[0051] (1) Preparation of sodium antimonate

[0052] Add 125g of antimony white to 375mL of 300g / L NaOH solution, leach at 90°C for 3h, slowly add 145mL of 30wt% hydrogen peroxide dropwise during the leaching process, cool, crystallize, and filter to obtain 205g of sodium antimonate. The temperature of the solution after cooling is 5- 10°C.

[0053] (2) Preparation of sodium thioantimonate solution

[0054] Adopt 837g sodium sulfide nonahydrate to dissolve and be made into 780mL solution, then add the 195g sodium antimonate that step (1) obtains. Control the reaction temperature at 90°C, stir for 2.5 hours, cool to below 5°C, and filter to obtain 297 g of sodium thioantimonate nonahydrate crystals, which are prepared into 752 mL of sodium thioantimonate solution containing 100 g / L antimony.

[0055] (3) Prepare antimony trichloride solution by leaching antimony white with hydrochloric acid.

[0056] Add 870mL of 37wt% concentrated hydrochloric acid and 155.3g of NaCl to mak...

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Abstract

The invention provides a method for preparing antimony thioantimonate based on a stable reaction system, belonging to the technical field of preparation for chemical products. The method comprises the following steps of: preparing a high-concentration Sb<3+> ion conjugate solution, which is not hydrolyzed under acidic, alkali and neutral conditions, by using antimony white as a raw material through acidification and conjugation; preparing sodium thioantimonate under alkali conditions; and then reacting the Sb<3+> ion conjugate solution and a sodium thioantimonate solution to prepare antimony thioantimonate. By using the method, the problems that antimony halide is hydrolyzed under alkali conditions and sodium thioantimonate is decomposed when being in contact with acid are solved; and the obtained antimony thioantimonate is high in purity and good in performance, and can be used as an extreme pressure antiwear additive for lubricating grease and a solid lubricant. The preparation process is simple, clean and stable, no side reaction occurs in the preparation course, the yield is high, the product is pure, the performance is good, and the method is suitable for industrial production.

Description

technical field [0001] The invention relates to a method for preparing antimony thioantimonate, in particular to a method for preparing antimony thioantimonate based on a stable reaction system; it belongs to the technical field of chemical product preparation. technical background [0002] Antimony thioantimonate is a reddish-brown amorphous powder, easily soluble in alkali, insoluble in organic solvents and inorganic acids. Antimony thioantimonate is a lubricating grease additive, which has excellent extreme pressure and anti-wear lubrication performance, and can greatly improve the load-carrying and anti-wear capabilities of grease, far superior to traditional WS 2 ,MoS 2 And graphite, have good compatibility with various base greases including lithium-based grease, silicone grease, clay grease and composite aluminum-based grease, etc., and have good compatibility with traditional MoS 2 Difficult-to-lubricate chrome tool steels and stainless steels are lubricated well. ...

Claims

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Application Information

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IPC IPC(8): C01G30/02
Inventor 杨喜云段习韬徐徽石西昌陈亚
Owner 湖南益阳生力材料科技有限公司
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