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Preparation method for carbonate type hydrotalcite compound powder

A hydrotalcite and carbonate type technology, applied in aluminum carbonate compounds, hydrotalcite, nickel compounds, etc., can solve the problems of slow reaction speed, easy particle size growth, low solubility of raw materials, etc., and achieve accelerated reaction and crystal development. Complete, good dispersion effect

Inactive Publication Date: 2018-12-07
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the hydrothermal method uses insoluble divalent metal hydroxides as raw materials, which have problems such as low solubility of raw materials, slow reaction speed, and easy growth of particle size.
[0005] Chinese patent (CN 102350288 A) reported the use of ultrasonic-hydrothermal coupling technology to prepare TiO with a high degree of dispersant and uniform particle size 2 Nanotubes, but ultrasonic technology is mainly used as a dispersion method for the synthesis of LDHs. At present, ultrasonic waves are only introduced in the precipitation process of the co-precipitation method or in the dispersion process of LDHs products, but ultrasonic-assisted reactions and nucleation are introduced in the preparation of LDHs by the hydrothermal method. and scattered studies have not been reported

Method used

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  • Preparation method for carbonate type hydrotalcite compound powder
  • Preparation method for carbonate type hydrotalcite compound powder
  • Preparation method for carbonate type hydrotalcite compound powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] MgO, Al(OH) 3 , MgCO 3 ·Mg(OH) 2 ·H 2 O was mixed and added to a 1.2L reaction kettle at a molar ratio of 7:4:3, and 975mL of deionized water was added with a solid content of 7.5wt%. After stirring evenly, the temperature was raised to 165°C, and ultrasonically After hydrothermal reaction for 1h, after cooling, the product was separated from solid and liquid and dried to obtain MgAl-CO 3 2- -LDHs powder. By XRD results such as figure 1 As shown, the peak shape of each characteristic diffraction peak is sharp, the baseline is smooth, and there is no impurity peak, indicating that the product has a single crystal phase and good crystallinity. Utilize infrared spectrum to carry out qualitative analysis to this sample, the result is as follows figure 2 As shown, 3464cm -1 The absorption peak at is due to the stretching vibration of hydroxyl groups on the laminate. 3069cm -1 The absorption peak at is caused by the interlayer CO 3 2- Due to hydrogen bonding with...

Embodiment 2

[0044] Mg(OH) 2 , Al(OH) 3 , MgCO 3 ·Mg(OH) 2 ·H 2 O was mixed and added to a 1.2L reactor at a molar ratio of 4:2:1, and 975mL of deionized water was added with a solid content of 5wt%. After stirring evenly, the temperature was raised to 120°C, and ultrasonic hydrothermal heating was carried out at an ultrasonic power of 1200W. After reacting for 0.5h, after cooling, the product was separated from solid and liquid and dried to obtain MgAl-CO 3 2- -LDHs powder. The average particle size D of the product 50 = 1.81 μm (P[X] = 85.3%), the agglomeration index was 3.5.

Embodiment 3

[0046] Ca(OH) 2 , Al(OH) 3 , CaCO 3 Mix them into a 1.2L reactor according to the molar ratio of 28:11:2, add 975mL of deionized water with a solid content of 20wt%, stir evenly, heat up to 200°C, and perform ultrasonic hydrothermal reaction at 500W ultrasonic power 8h, after cooling, the product was separated from solid and liquid and dried to obtain CaAl-CO 3 2- -LDHs powder, the average particle size of the product D 50 = 3.67 μm (P[X] = 78%), the agglomeration index was 4.1.

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Abstract

The invention provides a preparation method for carbonate type hydrotalcite compound powder. The method comprises the following steps: taking divalent metal oxide or hydroxide and trivalent metal hydroxide as main raw materials; compounding with divalent metal carbonate (normal salt or subcarbonate) of the same metal of the divalent metal oxide or hydroxide, for supplying carbonate; directly compounding the hydrotalcite compound with regular structure and uniform grain size through one-step ultrasonic-assisted hydrothermal reaction. The preparation method belongs to atom economy reaction; thereaction speed is high; no waste is discharged during the process; the product can be directly dried without washing, so that water resource can be greatly saved; the method has the characteristics ofsimple technological process, environmental protection and easiness in industrial production.

Description

technical field [0001] The invention belongs to the field of preparation of inorganic functional materials, and in particular relates to a preparation method of carbonate-type hydrotalcite compound powder. Background technique [0002] LDHs is the abbreviation of layered double hydroxides (layered double hydroxides), also known as hydrotalcite compounds, is a two-dimensional anionic layered composite hydroxide, composed of nano-scale laminates and layers similar to brucite Interanion composition, the general formula is Among them, M and N are divalent and trivalent metal ions (M=Mg 2+ 、Ni 2+ 、Co 2+ , Zn 2+ etc., N=Al 3+ , Fe 3+ 、Cr 3+ etc.), A n- is an interlayer anion (such as CO 3 2- , Cl - , OH - 、PO 4 3- , NO 3 - etc.), x is N 3+ / (M 2+ +N 3+ ) ratio, m is the amount of crystal water. LDHs materials have many unique properties such as acidity and alkalinity, memory effect, microporous structure, tunability of laminate cations and interlayer anion exc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F7/00C01G9/00C01G51/00C01G53/00
CPCC01G9/006C01G51/006C01G53/006C01P2002/22C01P2002/82C01P2002/88C01P2002/72C01P2004/03C01P2004/52C01P2006/12C01P2004/61C01F7/782C01F7/785
Inventor 郑占丰谷献模刘致帮任少奇马鹏伟裴林娟
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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