Method for preparing sodium pyroantimonate and regenerating and recycling mother liquor

A technology of sodium pyroantimonate and mother liquor, applied in chemical instruments and methods, antimonate/antimonite, antimony compounds, etc., can solve the problem of accumulation of impurity ions, limited cycle times, insufficient product quality of sodium pyroantimonate, etc. question

Active Publication Date: 2021-09-10
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In order to solve the problem of insufficient product quality and the accumulation of arsenic, lead, zinc and other impurity ions in the mother liquor and the limited number of cycles in the direct sodium salt system using high-arsenic antimony white as raw material to prepare sodium pyroantimonate

Method used

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  • Method for preparing sodium pyroantimonate and regenerating and recycling mother liquor
  • Method for preparing sodium pyroantimonate and regenerating and recycling mother liquor
  • Method for preparing sodium pyroantimonate and regenerating and recycling mother liquor

Examples

Experimental program
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Effect test

Embodiment 1

[0044] Measure 450mL of distilled water into the reaction kettle, then add 150g of high-arsenic antimony white according to the mass ratio of high-arsenic antimony white to distilled water at 1:3, and add sodium hydroxide at the mass ratio of sodium hydroxide to high-arsenic antimony white at 1:1 After slurrying, turn on the temperature rise switch of the reaction kettle at the same time, after the temperature of the solution in the kettle rises to 75°C, according to the theoretical requirements of the oxidation of As(III) and Sb(III) in high arsenic antimony white to sodium arsenate and sodium pyroantimonate Take hydrogen peroxide that is 1.2 times the amount of hydrogen peroxide and add it at a rate of 3 mL / min, and keep warm for 1 hour after the addition is complete. Then centrifuge and filter while it is hot, and add hot distilled water to wash according to the mass ratio of hot distilled water and high-arsenic antimony white at 1:2. After filtering the sodium pyroantimonat...

Embodiment 2

[0046] Measure 750mL of distilled water into the reaction kettle, then add 150g of high-arsenic antimony white according to the mass ratio of high-arsenic antimony white to distilled water at 1:5, and add sodium hydroxide at the mass ratio of sodium hydroxide to high-arsenic antimony white at 2:1 After slurrying, turn on the temperature rise switch of the reaction kettle at the same time, after the temperature of the solution in the kettle rises to 60°C, start to oxidize As(III) and Sb(III) into sodium arsenate and sodium pyroantimonate according to the theory of high arsenic antimony white Take 1.4 times the amount of hydrogen peroxide required to take hydrogen peroxide and add it at 4mL / min, and keep warm for 2 hours after the addition is complete. Then vacuum filter while it is hot, and add hot distilled water to wash according to the mass ratio of hot distilled water and high-arsenic antimony white at 3:7. After the sodium pyroantimonate product is filtered, transfer it to ...

Embodiment 3

[0048] Measure 900mL of distilled water into the reaction kettle, then add 150g of high-arsenic antimony white according to the mass ratio of high-arsenic antimony white to distilled water at 6:1, and add sodium hydroxide at the mass ratio of sodium hydroxide to high-arsenic antimony white at 3:1 After slurrying, turn on the temperature rise switch of the reaction kettle at the same time, after the temperature of the solution in the kettle rises to 70°C, start to oxidize As(III) and Sb(III) into sodium arsenate and sodium pyroantimonate according to the theory of high arsenic antimony white Take hydrogen peroxide that is twice the amount of hydrogen peroxide required and add it at a rate of 6 mL / min. After the addition is complete, keep warm for 3 hours. Then vacuum filter while it is hot, and add hot distilled water to wash according to the mass ratio of hot distilled water and high-arsenic antimony white at 3:4. After filtering the sodium pyroantimonate product, transfer it t...

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Abstract

The invention discloses a method for preparing a sodium pyroantimonate product from high-arsenic antimony white and vulcanizing, crystallizing, regenerating and recycling mother liquor, and relates to the field of antimony fine chemicals. According to the method, the low-cost-value high-arsenic antimony white is subjected to alkaline oxidation to prepare the sodium pyroantimonate product with the high additional value, the mother liquor containing impurities such as arsenic, lead and zinc is subjected to sulfuration crystallization to achieve cooling crystallization of sodium arsenate and sulfuration precipitation of lead and zinc ions, and the purified and regenerated mother liquor is continuously used for preparing the sodium pyroantimonate. The sodium pyroantimonate product meets the second-grade product requirement of the Chinese nonferrous metal industry standard (YS / T 22-2010), and the problem of separation of impurities such as antimony, arsenic, lead and zinc during preparation of sodium pyroantimonate from high-arsenic antimony white with complex components is solved. Meanwhile, the mother liquor is efficiently regenerated through vulcanization and crystallization, the problems that arsenic and alkali are difficult to separate and energy consumption is high after evaporation, concentration and crystallization are carried out are solved, and finally, the regenerated mother liquor is used for preparing sodium pyroantimonate, and efficient preparation of a product and recycling of the mother liquor are achieved; technical innovation is provided for high-valued utilization of low-price high-arsenic antimony white and purification and regeneration of mother liquor. The method has the advantages of convenience in operation, stable product components, high mother liquor purification efficiency and the like.

Description

technical field [0001] The invention relates to the field of antimony fine chemicals, in particular to a method for preparing sodium pyroantimonate product by using high-arsenic antimony white, purifying and regenerating mother liquor sulfidation crystallization and its recycling. Background technique [0002] The molecular formula of sodium pyroantimonate is NaSb(OH) 6 , with a density of 3.7g / cm 3 , usually a white powdery compound with good crystallinity and cubic crystal form. The physical and chemical properties of sodium pyroantimonate are insoluble in water, dilute alkali and inorganic acids, soluble in tartaric acid to form antimony tartrate complex ions, and heated and dissolved in sulfuric acid to form antimony sulfate. As a deep-processing product of antimony, sodium pyroantimonate is widely used as a clarifying agent for picture tube glass, optical glass and high-grade glass, as a flame retardant for textiles and plastic products, and as an antimony agent for e...

Claims

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Application Information

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IPC IPC(8): C01G30/02
CPCC01G30/023C01P2002/72C01P2004/03C01P2006/80Y02P10/20
Inventor 唐攒浪唐新村刘好男
Owner CENT SOUTH UNIV
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