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A kind of method that hydrothermal method prepares orpiment crystal

A technology of hydrothermal method and orpiment, which is applied in chemical instruments and methods, arsenic compounds, inorganic chemistry, etc., can solve the problems of long reaction time, high energy consumption, and complicated preparation of raw materials, and achieve reduced leaching toxicity and low energy consumption , The effect of simple process

Active Publication Date: 2021-09-07
CENT SOUTH UNIV +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The above method for preparing orpiment crystals has the problems of complex preparation of raw materials, long reaction time, high reaction temperature, large energy consumption, and difficult repetition.

Method used

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  • A kind of method that hydrothermal method prepares orpiment crystal
  • A kind of method that hydrothermal method prepares orpiment crystal
  • A kind of method that hydrothermal method prepares orpiment crystal

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Weigh 9.0g sodium sulfide nonahydrate and 3.25g sodium arsenite, the molar ratio of sulfur to arsenic is 3:2, put it in 500mL (0.92MH 2 SO 4 ) aqueous solution, fully reacted at room temperature for 24 hours, filtered and washed with water, dried in vacuum at 50° C., and ground to obtain amorphous arsenic trisulfide powder. according to figure 1 , figure 2 , the synthesized product is amorphous amorphous arsenic trisulfide with loose structure and small particles.

[0030] Take 1.0g of arsenic sulfide powder and place it in a 25mL hydrothermal reaction kettle, add 5mL of water with a pH of 2 adjusted with HCl, and react at 210°C for 48h to obtain orpiment crystals. Depend on image 3 It can be seen that, through the hydrothermal reaction, the amorphous arsenic trisulfide is transformed into spherical particles of a certain size, and the columnar crystals grow radioactively on the surface, and the spherical particles tend to agglomerate.

Embodiment 2

[0032] The preparation method is the same as in Example 1, except that the solid-to-liquid ratios of amorphous arsenic trisulfide and water in Example 2 are 1:1, 1:3, 1:7, and 1:9, respectively. Depend on Figure 4 , with the solid-liquid ratio from (1:1) g / mL to (1:9) g / mL, the intensity of the diffraction peak of orpiment increases gradually, and the crystal form is good.

Embodiment 3

[0034] The preparation method is the same as in Example 1, except that the pH values ​​in Example 3 are 5.0, 7.0, 9.0, and 12.0, respectively. according to Figure 5 , as the pH increases, the particle surface gradually transforms from radioactive prisms / needles to inhomogeneous, irregular particles or sheet accumulation, and the crystal form becomes worse.

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Abstract

The invention discloses a method for preparing orpiment crystals by a hydrothermal method. The orpiment crystals are obtained by hydrothermally treating amorphous arsenic trisulfide as a raw material at a temperature of 180° C. to 270° C. for 6 hours to 48 hours. The present invention uses amorphous arsenic trisulfide as a raw material, through strictly controlling the temperature and time of hydrothermal treatment, transforms amorphous arsenic trisulfide into stable orpiment crystals, and further optimizes the pH, solid-liquid Ratio, temperature and time can make orpiment crystals have good crystal form, high conversion rate, and no other impurities, and realize the controllable synthesis of orpiment crystals.

Description

technical field [0001] The invention belongs to the technical field of orpiment preparation, and relates to a method for preparing orpiment crystals by a hydrothermal method, in particular to a method for hydrothermally converting amorphous arsenic trisulfide into orpiment crystals. Background technique [0002] As a trace element exported from the lithosphere to the ocean by the submarine hydrothermal system, its stable existence in the solid phase is of great significance for reducing the transformation and migration of arsenic to the environment and the geochemical cycle of arsenic. Orpiment is a typical sulfur-arsenic mineral that exists stably in nature. According to the Eh-pH diagram, orpiment is the main mineral phase of arsenic at 25°C-100°C, and it shows stability in a wide pH range. Godelitsas et al. (Godelitsas A, et al. Marine Chemistry, 2015.) and Dekov et al. (Dekov V M, et al. Marine Geology, 2013.) found that seafloor hydrothermal fluids were Stable orpiment...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G28/00
CPCC01G28/008C01P2002/72C01P2004/03
Inventor 柯勇闵小波许秋婧柴立元王静雯吴理觉付海阔梁彦杰徐慧姚理为
Owner CENT SOUTH UNIV