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Nano barium sulfate and preparation method thereof

A technology of nano barium sulfate and ammonium sulfate, applied in nanotechnology, nanotechnology, calcium/strontium/barium sulfate and other directions, can solve the problems such as the width of nano barium sulfate, the inability of nano barium sulfate to meet the requirements in the field of battery separators, and the like. The effect of mild process conditions and low equipment requirements

Active Publication Date: 2015-02-11
HONGXING XINHUANG EXACT CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The prior art discloses the preparation of nano-barium sulfate with a wide particle distribution, and the prepared nano-barium sulfate cannot meet the requirements in the field of battery separators

Method used

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  • Nano barium sulfate and preparation method thereof
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[0032] The preparation method of nanometer barium sulfate of the present invention comprises following steps:

[0033] (1) Raw material treatment process: Ba(OH) 2 ·8H 2 O is purified to obtain Ba(OH) with a calcium content of less than 200ppm 2 ·8H 2 O is crystallized, ammonium sulfate is purified to obtain ammonium sulfate with a calcium content of less than 200ppm; in a specific embodiment, Ba(OH) is obtained in operation (1) 2 ·8H 2 The calcium content in O is less than 50ppm; The calcium content in obtaining ammonium sulfate is preferably less than 50ppm; In a specific embodiment, the purified Ba(OH) described in operation (1) 2 ·8H 2 The method of O includes: preparing barium hydroxide concentration as Ba 2+ 0.5-2.5mol / L solution, the preferred concentration is 1.5-2.5mol / L, heated until completely dissolved, heat-preserved and filtered to obtain the filtrate, the filtrate is cooled to crystallize, the obtained crystal is subjected to solid-liquid separation, and t...

Embodiment 1

[0070] Combine below figure 1 Shown in the process flow diagram, the present invention prepares the process of nanometer barium sulfate.

[0071] (1) Raw material processing process

[0072] Determination of commercially available 1000kg industrial grade Ba(OH) 2 ·8H 2 Calcium content in O raw material is 473.2ppm, stand-by. Determination of commercially available 1000kg industrial grade (NH 4 ) 2 SO 4 The content of calcium in the medium is 525.6ppm.

[0073] (2) Preparation process of Ba-EDTA

[0074] The Ba(OH) obtained in step (1) 2·8H 2 O crystals are placed in a stirring heating pot and prepared to a concentration of 30 kg / m 3 barium hydroxide solution, add EDTA to make the concentration of EDTA in the solution after adding be 40 kg / m 3 , heat the mixed solution to 83°C, maintain the temperature for 35 minutes under stirring, then pass through cooling water to cool below 30°C, filter it precisely and accurately measure [Ba 2+ ] Concentration is 0.0477mol / L. ...

Embodiment 2

[0081] Combine below figure 1 Shown in the process flow diagram, the present invention prepares the process of nanometer barium sulfate.

[0082] (1) Raw material processing process

[0083] Will commercially buy 1000kg of industrial grade Ba(OH) 2 ·8H 2 The O raw material is prepared into a solution with a concentration of 2.5 mol / L, heated to 90°C under stirring, completely dissolved, heat-preserved and filtered, and the filter residue is discarded, the filtrate is cooled to 30°C for crystallization, separated by filtration, and the mother liquor is used to dissolve the barium hydroxide raw material. The crystal is used to prepare Ba-EDTA solution, and the calcium content in the crystal is determined to be 200ppm.

[0084] Will commercially buy 1000kg industrial grade (NH 4 ) 2 SO 4 Make a solution of 0.8mol / L, add ammonium carbonate under stirring to make the concentration of ammonium carbonate in the solution 2.4mol / L, stir at room temperature for 25 minutes, separat...

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Abstract

The invention discloses a preparation method of nano barium sulfate. The preparation method comprises the following procedures: (1) raw material treatment procedure: respectively purifying Ba(OH)2.8H2O and ammonium sulfate until the calcium content is less than 200ppm; (2) Ba-EDTA preparation procedure: preparing the obtained Ba(OH)2. 8H2O crystal into a solution, adding EDTA into the barium hydroxide solution, heating the mixed solution to 80-85 DEG C, cooling and filtering to obtain a solution with Ba<2+> concentration of 0.01-0.10mol / L; (3) mixed solution preparation procedure; (4) spray pyrolysis reaction and finished product generation procedure: carrying out a centrifugal spray reaction on the obtained solution, centrifugally separating the slurry generated after reaction to obtain solids, washing the solids by using the barium hydroxide solution, and drying to obtain a nano barium sulfate product. The invention also provides nano barium sulfate prepared by the method. The content of barium sulfate prepared by the method disclosed by the invention is higher than 99.10% and is preferably higher than 99.2%; the whiteness is higher than 98.5%, the water content is lower than 0.5%, and the iron content is lower than 5.0ppm; and the particle size range of primary particles is 20-50nm.

Description

technical field [0001] The invention relates to the technical field of preparation of fine inorganic chemical fillers, in particular to a nano barium sulfate and a preparation method thereof. Background technique [0002] Nano-barium sulfate is widely used in coatings, inks, daily chemicals and other industries. Due to its excellent chemical stability, corrosion resistance to various acidic media such as HCl and HF, and high thermal conductivity and other characteristics, it has received great attention in the field of battery separators in recent years. Great attention. [0003] The prior art discloses that the particle distribution of the prepared nano-barium sulfate is relatively wide, and the prepared nano-barium sulfate cannot meet the requirements in the field of battery separators. Contents of the invention [0004] The technical problem solved by the present invention is to provide a narrow distribution of nano-barium sulfate; more specifically, the technical prob...

Claims

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Application Information

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IPC IPC(8): C01F11/46B82Y30/00
Inventor 姜志光华东曹玉欣严家铎
Owner HONGXING XINHUANG EXACT CHEM
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