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Method for directly preparing Sb4O5Cl2 from Sb2O3 and hydrochloric acid aqueous solution

A hydrochloric acid aqueous solution, sb2o3 technology, applied in chemical instruments and methods, inorganic chemistry, antimony compounds, etc., can solve the problems of high reaction temperature, inconvenient use, high concentration of hydrochloric acid, and achieve mild production process conditions, easy to control, and high purity. Effect

Active Publication Date: 2020-06-05
KUNMING HANCHUANG SCI & TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method is the method for preparing SbOCl, although this method only uses Sb 2 o 3 and hydrogen chloride gas to prepare SbOCl, when returning to the mother liquor, the SbOCl yield can reach more than 90%, but the invention has high reaction temperature, high concentration of hydrochloric acid, high cost of hydrogen chloride gas, and inconvenient use; Sb can also be prepared by hydrolysis 4 o 5 Cl 2， However, the cost will be further increased, and these deficiencies have caused the patent to have no industrial application reports so far.

Method used

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  • Method for directly preparing Sb4O5Cl2 from Sb2O3 and hydrochloric acid aqueous solution
  • Method for directly preparing Sb4O5Cl2 from Sb2O3 and hydrochloric acid aqueous solution
  • Method for directly preparing Sb4O5Cl2 from Sb2O3 and hydrochloric acid aqueous solution

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Embodiment 1

[0069] In order to further illustrate the content of the present invention, the present invention is further described in the following examples.

[0070] In this example, exemplification according to the present invention was carried out in a 2000 ml glass beaker with a mechanical stirring paddle in a constant temperature water bath. The hydrochloric acid adopts industrial hydrochloric acid (37.5%), and the water adopts domestic drinking water. Prepare 1000 ml of an aqueous solution containing 0.6 mol / l hydrochloric acid. Heating to 30°C, under stirring, 111 g of Sb 2 o 3 (purity > 99.00%) added to the liquid, Sb 2 o 3 After the addition, keep the temperature at 30°C and stir the reaction for 1 hour to complete the Sb 4 o 5 Cl 2Crystal preparation reactions. After the reaction, the obtained slurry was filtered. Sb 4 o 5 Cl 2 Crystalline product The product was washed with 30 ml of water. Then dry to constant weight in a vacuum oven with a water extraction system....

Embodiment 2

[0073] In this example, exemplification according to the present invention was carried out in a 2000 ml glass beaker with a mechanical stirring paddle in a constant temperature water bath. First prepare 1000 milliliters of an aqueous solution containing 0.45 mol / l hydrochloric acid, the reagent is analytically pure hydrochloric acid, and the water is distilled water. This solution was heated to 55°C, and 90 g of Sb 2 o 3 (purity > 99.00%) added to the liquid, Sb 2 o 3 After the addition, keep the temperature at 55°C and stir the reaction for 40 minutes to complete the Sb 4 o 5 Cl 2 Crystal preparation reactions. After the reaction, the slurry was filtered. Sb 4 o 5 Cl 2 Crystalline product The product was washed with 30 ml of water. Then dry to constant weight in a vacuum oven with a water extraction system. Yield 106.4 g Sb 4 o 5 Cl 2 crystals. The crystal contains 76.34% of antimony (76.35% in theory) and 11.12% of chlorine (11.11% in theory). X-ray diffract...

Embodiment 3

[0075] In this example, examples according to the present invention were carried out in a 2000 ml plastic beaker with a mechanical stirring paddle and a constant temperature water bath. The hydrochloric acid adopts industrial hydrochloric acid (37.5%), and the water adopts domestic drinking water. First prepare 1000 milliliters of an aqueous solution containing 0.76 mol / l hydrochloric acid. This solution was heated to 40°C, and 120 g of Sb 2 o 3 (purity > 99.00%) added to the liquid, Sb 2 o 3 After the addition, keep the temperature at 40°C and stir the reaction for 1 hour to complete the Sb 4 o 5 Cl 2 Crystal preparation reactions. After the reaction, the slurry was filtered. Sb 4 o 5 Cl 2 Crystalline product The product was washed with 30 ml of water. Then dry to constant weight in a vacuum oven with a water extraction system. Yield 130.1 g Sb 4 o 5 Cl 2 crystals. The crystal contains 76.31% of antimony (76.35% in theory) and 11.22% of chlorine (11.11% in th...

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Abstract

The invention relates to a method for directly preparing Sb4O5Cl2 from Sb2O3 and a hydrochloric acid aqueous solution. The method comprises the following steps: preparing a hydrochloric acid aqueous solution as a synthesis initial solution containing a certain hydrochloric acid concentration range from hydrochloric acid and water, heating the synthesis initial solution to a certain temperature range, adding Sb2O3 into the synthesis initial solution which is heated to a proper temperature, reacting the solution for a period of time in a continuous stirring state to form Sb4O5Cl2 crystals, separating the crystals and a synthetic tail liquid from the aqueous solution, washing the crystals with water or ethanol, and drying the washed crystals, so as to obtain the Sb4O5Cl2 crystals. The methodhas the characteristics of short preparation time, high product purity, low energy consumption and no emission of waste liquid and waste gas in the preparation process.

Description

technical field [0001] The invention belongs to the field of inorganic chemical industry and non-ferrous metallurgy, and mainly relates to a product preparation method of an antimony compound, in particular to a kind of Sb 4 o 5 Cl 2 method of preparation. Background technique [0002] Sb 4 o 5 Cl 2 It is one of the two important intermediate substances that make the chlorine-antimony flame retardant synergistic system produce a flame retardant effect in the combustion process. At the same time, it is also a method for the purification of nickel, cobalt and germanium in an aqueous solution of zinc sulfate that the inventor applied for. "An important part of the activator. [0003] Although Sb 4 o 5 Cl 2 The content in SbOCl is lower than that of SbOCl. When used alone as a flame retardant, the flame retardant effect is slightly worse, but when it is used in combination with halogen, it also has excellent halogen-antimony flame retardant synergistic performance. It ...

Claims

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Application Information

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IPC IPC(8): C01G30/00
CPCC01G30/00C01P2004/30C01P2004/61C01P2002/72C01P2004/03
Inventor 张旭张云彭沈庆峰耿惠
Owner KUNMING HANCHUANG SCI & TECH CO LTD
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