Micron-sized barium sulfate micro-sphere synthesis method

A synthesis method, barium sulfate technology, applied in chemical instruments and methods, calcium/strontium/barium compounds, calcium/strontium/barium sulfate, etc. The efficiency is not very high, and the effect of strong controllability of product shape, high yield and good particle size uniformity is achieved.

Active Publication Date: 2018-09-14
BEIJING INSTITUTE OF PETROCHEMICAL TECHNOLOGY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The microemulsion method will introduce a large amount of organic solvents and surfactants, which will bring a lot of pollution; the microreactor method is difficult to mass-produce to industrial level due to the limitation of equipment; the high gravity method is due to the limitation of its production equipment. The barium sulfate particle size distribution range is wide, and the degree of homogeneity is not high; the complexation precipitation method achieves the purpose of homogeneous precipitation by controlling the supersaturation in the solution. It is a mild reaction, controllable operating conditions, and simple experimental equipment. method, but the disadvantage of the complex method is that the barium sulfate particles synthesized by the general method are submicron barium sulfate, and due to the existence of complexes, the yield is not very high

Method used

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  • Micron-sized barium sulfate micro-sphere synthesis method
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  • Micron-sized barium sulfate micro-sphere synthesis method

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Experimental program
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Effect test

Embodiment 2

[0034](1) Put the three-neck flask with a stirring device into a constant temperature oil bath, add 1.0mol / L BaCl 2 2H 2 O solution, followed by EDTA with Ba 2+ Add 1.0mol / L EDTA·2Na complexing agent at a molar ratio of 1.2:1, and control the temperature at 20°C to form a stable complex solution;

[0035] (2) Regulate step (1) complex solution pH to 7-10 with sodium hydroxide solution, after pH value is stable, according to S 2 o 8 2- with Ba 2+ Add 1.0mol / L Na at a molar ratio of 1:1 2 S 2 o 8 , after the reaction is complete, a white turbid solution with a pH of 5 is obtained;

[0036] (3) Stand still for 1 day, after centrifugation, wash with deionized water until the pH is neutral, and dry the obtained solid phase separation at 120° C. for 12 hours to obtain barium sulfate spherical particles with a yield of more than 90%.

[0037] Observe above-mentioned obtained barium sulfate sample with ZEISS-SUPRA55 type field emission scanning electron microscope (Scanning e...

Embodiment 3

[0039] (1) Put the three-neck flask with a stirring device into a constant temperature oil bath, add 1.0mol / L BaCl 2 2H 2 O solution, followed by EDTA with Ba 2+ Add 1.0mol / L EDTA·2Na complexing agent at a molar ratio of 2:1, and control the temperature at 30°C to form a stable complex solution;

[0040] (2) Regulate the pH of the complex solution in step (1) to 7-10 with sodium hydroxide solution, after the pH value is stable, add excess Na 2 S 2 o 8 , after the reaction is complete, a white turbid solution with a pH of 2 is obtained;

[0041] (3) Stand still for 1 day, after centrifugation, wash with deionized water until the pH is neutral, and dry the obtained solid phase separation at 120° C. for 12 hours to obtain barium sulfate microspheres with a yield of 90%.

[0042] Observe above-mentioned obtained barium sulfate sample with ZEISS-SUPRA55 type field emission scanning electron microscope (Scanning electron microscope, SEM), as image 3 shown, from image 3 It c...

Embodiment 4

[0044] (1) Put the three-neck flask with a stirring device into a constant temperature oil bath, add 1.0mol / L BaCl 2 2H 2 O solution, followed by EDTA with Ba 2+ Add 1.0mol / L EDTA·2Na complexing agent at a molar ratio of 2:1, and control the temperature at 95°C to form a stable complex solution;

[0045] (2) Regulate the pH of the complex solution in step (1) to 8-9 with sodium hydroxide solution, after the pH value is stable, add excess K 2 S 2 o 8 , after the reaction is complete, a white turbid solution with a pH of 4 is obtained;

[0046] (3) Stand still for 1 day, after centrifugation, wash with deionized water until the pH is neutral, and dry the obtained solid phase separation at 120° C. for 12 hours to obtain barium sulfate microspheres with a yield of 93%.

[0047] Observe above-mentioned obtained barium sulfate sample with ZEISS-SUPRA55 type field emission scanning electron microscope (Scanning electron microscope, SEM), as Figure 4 shown, from Figure 4 It c...

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Abstract

The invention discloses a micron-sized barium sulfate micro-sphere synthesis method, and belongs to the technical field of chemical synthesis. A micron-sized barium sulfate micro-sphere is synthesizedby a reaction system comprising S2O8<2-> soluble salt, Ba<2+> soluble salt and complexing agents, and the shape of the barium sulfate micro-sphere is regulated by changing the mole ratio of the Ba<2+> soluble salt and the complexing agents, complexing temperature and the addition amount of the S2O8<2-> soluble salt. The synthesis method is simple, efficient, environmentally friendly and free frompollution, the yield of the prepared micron-sized barium sulfate micro-sphere reaches 90% or more, the particle size of the prepared micron-sized barium sulfate micro-sphere is 0.8-3 micrometers, andgranularity uniformity is good.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, in particular to a method for synthesizing micron-scale barium sulfate microspheres. Background technique [0002] Barium sulfate, as an economical barite raw material with high whiteness, acid and alkali resistance, non-toxic and harmless, and high reflectivity, has been widely used in catalyst carriers, adsorbents, medical contrast agents, and polymers. Additives and other fields. In addition, the shape and particle size of barium sulfate determine its application path. Among them, barium sulfate microspheres with uniform particle size have the advantages of high light reflectivity, and the diffusion layer prepared by barium sulfate microspheres has uniform pore distribution and relatively high density. The characteristic of large pore volume can be used to filter the interfering substances in the sample to be tested and make it penetrate evenly to the next layer, which is widely us...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F11/46
CPCC01F11/462C01P2004/32C01P2004/61C01P2004/62
Inventor 靳海波刘月姣杨索和郭晓燕何广湘
Owner BEIJING INSTITUTE OF PETROCHEMICAL TECHNOLOGY
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