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Production method for sodium pyroantimonate by using high-temperature high-pressure pure-oxygen oxidation

A technology of sodium pyroantimonate, high temperature and high pressure, applied in chemical instruments and methods, inorganic chemistry, antimony compounds, etc., can solve the problems of high anticorrosion requirements for equipment, poor production conditions, product quality fluctuations, etc., and achieve product quality and stability, Mild reaction conditions and stable product quality

Inactive Publication Date: 2013-09-25
CHENZHOU CITY JINGUI SILVER IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the process of producing sodium pyroantimonate by wet method, sodium nitrate, or hydrogen peroxide, or chlorine gas, or air etc. are generally used as oxidants, and there are deficiencies in the technological process: ①When sodium nitrate is used as oxidant, the production Carcinogenic nitrogen oxides produced during the process; serious environmental pollution; poor production conditions and low product quality
② When hydrogen peroxide is used as the oxidant, although this method has the advantages of simple process, good product quality, and easy disposal of the three wastes, it has high requirements for raw materials and high production costs, resulting in poor economic benefits
③When industrial chlorine gas is used as the oxidant, although the product quality of this method is relatively good, the process is complex, the investment is large, the requirements for equipment anti-corrosion are high, and a large amount of waste water is generated
④ When air is used as the oxidant, the method has simple equipment and low production cost, but the product quality fluctuates from time to time and the production cycle is lengthy, and a large amount of sodium thiosulfate by-products are produced
The process uses raw material H 2 o 2 As an oxidant, it participates in the reaction in molecular form, which requires high raw materials, slow oxidation speed, and long production cycle, so the production cost is high

Method used

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  • Production method for sodium pyroantimonate by using high-temperature high-pressure pure-oxygen oxidation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 2000 mL of sodium hydroxide (300 g / L) solution to 200 g of antimony oxide powder containing 52.25% antimony and 13.21% lead, stir at 85°C for 60 min, and then add the purifying agent Na 2 S (55 g / L) solution 5 mL was used to remove impurities, filtered for 60 min after purification, the filtrate was moved to an autoclave, and oxygen was introduced, the temperature was controlled at 120 °C, and the pressure was adjusted and maintained at 1.5 MPa. After 60 min of reaction, antimony The precipitation rate reached 99.15%. After filtration, washing, drying and crushing, 172.6 g of sodium pyroantimonate product was obtained. Product quality analysis results are: Sb: 49.17%; Na 2 O: 12.73%; Pb: 0.0012%; As: 3+ : 0.09%, the appearance color is white, in line with the national standard.

Embodiment 2

[0021] Add 3000 mL of sodium hydroxide (400 g / L) solution to 200 g of antimony oxide powder containing 48.65% antimony and 14.08% lead, stir at 95 °C for 60 min, and then add the purifying agent Na 2 Remove impurities with 5 ml of S (55 g / L) solution, filter after purification for 60 min, move the filtrate to an autoclave, feed oxygen, control the temperature at 150 °C, adjust and maintain the pressure at 2.5 MPa, and react for 50 min, antimony precipitates The yield reached 99.5%, filtered, washed, dried, and pulverized to obtain 161.4 g of sodium pyroantimonate product. Product quality analysis results are: Sb: 49.31%; Na 2 O: 12.47%; Pb: 0.001 1%; As: 3+ : 0.05%, the appearance color is white, in line with the national standard.

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Abstract

The invention discloses a production method for sodium pyroantimonate by using high-temperature high-pressure pure-oxygen oxidation. The method comprises the following steps: with antimony oxide powder as a raw material, leaching the powder in a highly alkaline medium to extract antimony; purifying an obtained leachate; carrying out filtration, feeding an antimony-containing filtrate into an autoclave and controlling temperature to be 110 to 150 DEG C; introducing an oxygen oxidizing medium; adjusting and maintaining pressure to be 1.0 to 2.5 MPa; directly carrying out pressure oxidation, allowing a reaction to last 1 to 6 h and carrying out discharging; carrying out solid-liquid separation so as to obtain a sodium pyroantimonate precipitate; and washing, drying and screening the precipitate so as to obtain a sodium pyroantimonate product. The method provided by the invention has the characteristics of simple process flow, a small amount of needed equipment, low production cost, reinforced process, a short production period, no environmental pollution, stable product quality, etc., and has wide application prospects.

Description

technical field [0001] The invention relates to a wet process for preparing sodium pyroantimonate, in particular to a method for producing sodium pyroantimonate by high-temperature and high-pressure pure oxygen oxidation. It belongs to the field of metallurgy and chemical industry. Background technique [0002] Sodium pyroantimonate (Na 2 h 2 Sb 2 o 7 ·6H 2 O) It is mainly used as clarifier or flame retardant for color TV glass bulbs, electronic tubes and high-grade glass. At present, the demand for it is increasing at home and abroad. There are many production methods for sodium pyroantimonate. The domestic production of sodium pyroantimonate is mainly Mainly wet. In the process of producing sodium pyroantimonate by wet method, sodium nitrate, or hydrogen peroxide, or chlorine gas, or air etc. are generally used as oxidants, and there are deficiencies in the technological process: ①When sodium nitrate is used as oxidant, the production Carcinogenic nitrogen oxides ar...

Claims

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Application Information

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IPC IPC(8): C01G30/00
Inventor 蒋朝金谢兆凤许孔玉刘万里
Owner CHENZHOU CITY JINGUI SILVER IND CO LTD
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