Preparation method of shape-controllable magnesium hydroxide with low specific surface area

A technology of magnesium hydroxide and sodium hydroxide, applied in the direction of magnesium hydroxide, etc., can solve the problems such as no magnesium hydroxide morphology, and achieve the effects of controllable morphology, extended flame retardancy, and increased phase boundary area

Active Publication Date: 2020-01-14
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are no reports on the regulation of the morphology of magnesium hydroxide with low specific surface area in published papers and patents

Method used

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  • Preparation method of shape-controllable magnesium hydroxide with low specific surface area
  • Preparation method of shape-controllable magnesium hydroxide with low specific surface area
  • Preparation method of shape-controllable magnesium hydroxide with low specific surface area

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Configure 1.0mol / L MgCl 2 1L each of aqueous solution and 1.7mol / L NaOH aqueous solution. The above two aqueous solutions all entered the microreactor for contact, mixing and reaction at a flow rate of 100mL / min, n(Mg 2+ ):n(OH -)=1:1.7, the reaction temperature is 60°C. After the reaction slurry flows out from the outlet of the microreactor, it directly enters the hydrothermal synthesis kettle, and performs the first hydrothermal at 180° C., and the hydrothermal time is 4 hours. After the first hydrothermal treatment, the slurry was centrifuged to obtain a filter cake. At this time, the solid content of the filter cake was 18.49 wt.% calculated as magnesium hydroxide. Get 15g of filter cake, add 26.62g of water and 4.65g of NaOH to it, adjust the solid content and sodium hydroxide concentration in the slurry to 6wt.% and 3M in terms of magnesium hydroxide, and carry out the second hydrothermal treatment at 180°C , The water heating time is 4h. After the second hyd...

Embodiment 2

[0035] Configure 1mol / L MgCl 2 1L each of aqueous solution and 2.0mol / L NaOH aqueous solution. The above two aqueous solutions all entered the microreactor for contact, mixing and reaction at a flow rate of 100mL / min, n(Mg 2+ ):n(OH - )=1:2.0, the reaction temperature is 60°C. After the reaction slurry flows out from the outlet of the microreactor, it directly enters the hydrothermal synthesis kettle, and performs the first hydrothermal at 180° C., and the hydrothermal time is 4 hours. After the first hydrothermal treatment, the slurry was centrifuged to obtain a filter cake. At this time, the solid content in the filter cake was 36.33wt.% in terms of magnesium hydroxide. Take 15g of filter cake, add 66.67g of water and 9.14g of NaOH to it, adjust the solid content and sodium hydroxide concentration in the slurry to 6wt.% and 3M in terms of magnesium hydroxide, and carry out the second hydrothermal treatment at 180°C , The water heating time is 4h. After the second hydrot...

Embodiment 3

[0037] Configure 1mol / L MgCl 2 1L each of aqueous solution and 1.2mol / L NaOH aqueous solution. The above two aqueous solutions all entered the microreactor for contact, mixing and reaction at a flow rate of 100mL / min, n(Mg 2+ ):n(OH - )=1:1.7, the reaction temperature is 60°C. After the reaction slurry flows out from the outlet of the microreactor, it directly enters the hydrothermal synthesis kettle, and performs the first hydrothermal at 200° C., and the hydrothermal time is 4 hours. After the first hydrothermal treatment, the slurry was centrifuged to obtain a filter cake. At this time, the solid content of the filter cake was 18.49 wt.% calculated as magnesium hydroxide. Take 15g of filter cake, add 30.22g of water and 5.05g of NaOH therein, adjust the solid content and sodium hydroxide concentration in the slurry to 6wt.% and 3M in terms of magnesium hydroxide, and carry out the second hydrothermal treatment at 220°C , The water heating time is 6h. After the second h...

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Abstract

The invention provides a method for adjusting and controlling magnesium hydroxide with the low specific surface area. The shape-controllable magnesium hydroxide with the low specific surface area is prepared through a method of combination of the precipitation process of a confined space and hydro-thermal treatment, wherein the specific surface area is equal to or smaller than 5 m<2>/g. The methodcomprises the specific processes: a magnesium chloride aqueous solution and a sodium hydroxide aqueous solution are prepared correspondingly and continuously introduced into a microreactor to be subject to a precipitation reaction, reaction slurry is subjected to hydro-thermal treatment twice after flowing out from the microreactor, after hydro-thermal treatment is completed, the slurry is centrifuged, washed and dried, and then the magnesium hydroxide with the low specific surface area is obtained. The shape of the magnesium hydroxide with the low specific surface area can be adjusted and controlled by changing the molar ratio of Mg2+ and OH-. The precipitation process is achieved in the microreactor, the reaction process is semicontinuous and easy to amplify, and thus an obtained product is low in specific surface area, controllable in shape and good in lot-to-lot repeatability.

Description

technical field [0001] The invention relates to a method for regulating and controlling the morphology of magnesium hydroxide with a low specific surface area, and belongs to the fields of inorganic materials and material engineering. Background technique [0002] With the improvement of my country's environmental protection standards, the market demand for halogen-free flame retardants is increasing year by year. Magnesium hydroxide has the advantages of high decomposition temperature, good smoke suppression effect, safety and non-toxicity, and stable performance. As an environmentally friendly green inorganic flame retardant, it has been widely used in plastics, rubber, wire and cable and other fields. The flame retardancy of magnesium hydroxide is significantly affected by its particle size, particle size distribution, specific surface area, and morphology. Researchers can adjust the particle size, particle size distribution, specific surface area and morphology of magne...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F5/22
CPCC01F5/22C01P2004/03C01P2004/22C01P2006/12
Inventor 陈光文杨梅罗腊梅
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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