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Magnesium borate whisker hydrothermal synthesis preparation method

A magnesium borate whisker and hydrothermal synthesis technology, applied in chemical instruments and methods, single crystal growth, crystal growth, etc., can solve problems such as the coexistence of agglomerates, high energy consumption, and uneven morphology, and achieve product morphology The effect of regularity, uniform particle size and regular shape

Inactive Publication Date: 2007-03-28
TSINGHUA UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In order to overcome the existing problems in the preparation of magnesium borate whiskers, such as high energy consumption, uneven appearance, and the coexistence of agglomerates, the present invention provides a new method for preparing magnesium borate whiskers with regular appearance.

Method used

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preparation example Construction

[0022] The invention provides a co-precipitation-hydrothermal-roasting preparation method of magnesium borate whiskers, using inorganic magnesium salts and borates as raw materials, and inorganic alkalis as precipitants, and first synthesizing uniform and fine magnesium borate salts under normal temperature conditions Precursor, and then control the hydrothermal process to realize the directional growth of basic magnesium borate whiskers, and then carry out phase transformation and structural reformation under medium temperature conditions, thereby preparing magnesium borate whiskers with regular shape and uniform particle size ,Specific steps are as follows:

[0023] Prepare inorganic magnesium salt, borate and inorganic alkali solution with a concentration of 1-5 mol / liter, and add the inorganic alkali solution dropwise to the magnesium-containing For the mixed solution of salt and borate, the molar ratio of magnesium salt, borate and alkali is controlled to be 1:1~3:1~4 to ...

Embodiment 1

[0030] Prepared with 1mol / L MgCl 2and 3mol / L Na 3 BO 3 60ml of the mixed solution of 4mol / L KOH solution, 60ml of 4mol / L KOH solution, add the KOH solution (101 / min) MgCl at 25°C under stirring (350 rpm) 2 and Na 3 BO 3 The mixed solution, maintaining MgCl 2 :Na 3 BO 3 : KOH molar ratio is 1: 3: 4, obtains white emulsion precursor; Precursor is placed in hydrothermal reaction kettle, adds 0.1% ethanol, heats up (10 ℃ / min) to 120 ℃ after airtight, stirs (120 RPM) under constant temperature reaction for 1 hour, cooling, washing, and filtering to obtain a hydrothermal product; put the hydrothermal product in an air roaster, and treat it at 750°C for 1 hour to obtain an average diameter of 10nm, an average length of 0.5μm, and a long diameter Magnesium borate whiskers with a ratio of 50.

Embodiment 2

[0032] Prepared with 1mol / L MgSO 4 and 1mol / L K 3 BO 3 60ml of mixed solution, 60ml of 1mol / L NaOH solution, add NaOH solution (1ml / min) MgSO 4 and K 3 BO 3 A mixed solution of MgSO 4 : K 3 BO 3 : NaOH molar ratio is 1: 1: 1, obtains white emulsion precursor; Precursor is placed in hydrothermal reaction kettle, adds 1% acetone, heats up (5 ℃ / min) to 300 ℃ after airtight, stirs (80 RPM) under constant temperature for 30 hours, cooling, washing, and filtering to obtain hydrothermal products; put the hydrothermal products in an air roaster and treat them at 650°C for 5 hours to obtain an average diameter of 100nm, an average length of 20μm, and a long diameter Magnesium borate whiskers with a ratio of 200.

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Abstract

The invention relates to a hydrothermal synthesis manufacturing method for magnesium borate crystal whisker that adopts inorganic magnesium salt, magnesium borate and inorganic alkali as main raw material, adding inorganic alkali into mixture solution of magnesium salt and borate at 10-90 degree centigrade, taking hydrothermal treatment to normal temperature product at 100-300 degree centigrade, realizing directional growth through controlling hydrothermal rocks constituents and technology condition to gain one dimension appearance feather alkali magnesium borate crystal whisker, washing, drying the hydrothermal product, and baking under the existence of crystallographic form transforming agent at 600-800 degree centigrade to realize structure reconstruction and phase converting to gain regular appearance and equal size magnesium borate crystal whisker. The invention has the advantages of simple technology, mild condition, cheap raw material, and easy to be manufactured.

Description

technical field [0001] The invention relates to a new hydrothermal synthesis process for preparing magnesium borate whiskers, belonging to the technical field of inorganic chemical engineering. Background technique [0002] my country is a country with large magnesium resources, and the salt lake magnesium salt and magnesite resources are very rich, but at present, most of the magnesium salt products are primary products with little technical content and low added value, such as magnesium chloride, magnesium sulfate, magnesium carbonate, ordinary magnesium oxide and hydroxide Magnesium etc. Most advanced magnesium salt functional materials with high added value and rapidly growing market demand, such as magnesium salt whiskers, are still in the experimental research stage, which restricts the large-scale and high utilization of magnesium resources. [0003] Among the advanced magnesium salt functional materials, the research and development of one-dimensional magnesium borat...

Claims

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Application Information

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IPC IPC(8): C30B7/10C30B29/22C30B29/62
Inventor 向兰朱万诚朱慎林
Owner TSINGHUA UNIV
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