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Preparation methods of rare earth layered hydroxide nanosheets and rare earth layered hydroxide nanosheet sol

A layered hydroxide and nanosheet technology, applied in the field of material science, can solve the problems of slow hydrolysis, poor dispersibility, poor stability, etc., and achieve the effects of simple preparation process, saving raw materials, and convenient operation.

Inactive Publication Date: 2018-05-22
BOHAI UNIV
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  • Application Information

AI Technical Summary

Problems solved by technology

The existing problems are: 1) In terms of synthetic technical route, the precipitant used in the precipitation method, such as hexamethylenetetramine, has slow hydrolysis at room temperature, and easy generation of formaldehyde and its derivatives in the air at high temperature to reduce the precipitation reaction yield. and other shortcomings
Although the hydrothermal method overcomes the above-mentioned shortcomings of the precipitation method, and has the advantages of high product purity and low pollution, the reaction process requires a lot of energy under hydrothermal conditions, and the stability of the reaction process is poor.
2) In terms of the properties of the obtained target product: La prepared by hydrothermal method and normal temperature precipitation method 2 (OH) 4 SO 4 ·nH 2 O is finally crystallized into thicker nano- or micro-sheets due to the higher reaction temperature, especially the product obtained by the precipitation method has a large degree of agglomeration and poor dispersion.
And both of these methods are difficult to achieve large-scale preparation
In addition, the thickness of the laminates of nanosheets prepared by these two methods can reach 30-300nm, and because this compound cannot be prepared by intercalation-exfoliation, it is currently impossible to obtain ultra- Thin rare earth layered hydroxide La 2 (OH) 4 SO 4 ·nH 2 O nanosheets, so the rare-earth layered hydroxide La with good stability cannot be obtained 2 (OH) 4 SO 4 ·nH 2 O nanosheet sol

Method used

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  • Preparation methods of rare earth layered hydroxide nanosheets and rare earth layered hydroxide nanosheet sol
  • Preparation methods of rare earth layered hydroxide nanosheets and rare earth layered hydroxide nanosheet sol
  • Preparation methods of rare earth layered hydroxide nanosheets and rare earth layered hydroxide nanosheet sol

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Experimental program
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Effect test

Embodiment 1

[0033] A kind of rare earth layered hydroxide La 2 (OH) 4 SO 4 ·nH 2 The preparation method of O nanosheet is characterized in that, comprises the following steps:

[0034] (1) Lanthanum nitrate hexahydrate (La(NO 3 ) 3 ·6H 2 O) Mix well in deionized water to prepare La 3+ Lanthanum nitrate (La(NO) with a concentration of 0.03mol / L 3 ) 3 ) solution;

[0035] (2) The amount added is in molar ratio, SO 4 2- : La 3+ =0.5, ammonium sulfate particles ((NH 4 ) 2 SO 4 ) dissolved in lanthanum nitrate (La(NO 3 ) 3 ) solution, dissolved for 10 minutes until completely clear to form a mixed solution;

[0036] (3) Add ammonia water to the mixed solution, adjust the pH of the mixed solution to 6, and continue to stir for 10 minutes to obtain a uniform suspension;

[0037] (4) React the homogeneous suspension, the reaction temperature is 4°C, the reaction time is 48h, and the product is obtained. The product composition is the rare earth layered hydroxide La containing in...

Embodiment 2

[0043] A kind of rare earth layered hydroxide La 2 (OH) 4 SO 4 ·nH 2 The preparation method of O nanosheet is characterized in that, comprises the following steps:

[0044] (1) Lanthanum nitrate hexahydrate (La(NO 3 ) 3 ·6H 2 O) Mix well in deionized water to prepare La 3+ Lanthanum nitrate (La(NO) with a concentration of 0.20mol / L 3 ) 3 ) solution;

[0045] (2) The amount added is in molar ratio, SO 4 2- : La 3+ =10, ammonium sulfate particles ((NH 4 ) 2 SO 4 ) dissolved in lanthanum nitrate (La(NO 3 ) 3 ) solution, dissolved for 20min until completely clear to form a mixed solution;

[0046] (3) Add ammonia water to the mixed solution, adjust the pH of the mixed solution to 10, and continue to stir for 30 minutes to obtain a uniform suspension;

[0047] (4) React the homogeneous suspension with a reaction temperature of 0°C and a reaction time of 1 h to obtain the product, which consists of rare earth layered hydroxide La containing incompletely reacted mot...

Embodiment 3

[0053] A kind of rare earth layered hydroxide La 2 (OH) 4 SO 4 ·nH 2 The preparation method of O nanosheet is characterized in that, comprises the following steps:

[0054] (1) Lanthanum nitrate hexahydrate (La(NO 3 ) 3 ·6H 2 O) Mix well in deionized water to prepare La 3+ Lanthanum nitrate (La(NO) with a concentration of 0.1mol / L 3 ) 3 ) solution;

[0055] (2) The amount added is in molar ratio, SO 4 2- : La 3+ =3, ammonium sulfate particles ((NH 4 ) 2 SO 4 ) dissolved in lanthanum nitrate (La(NO 3 ) 3 ) solution, dissolved for 14min until completely clear to form a mixed solution;

[0056] (3) Add ammonia water to the mixed solution, adjust the pH of the mixed solution to 9, and continue to stir for 20 minutes to obtain a uniform suspension;

[0057] (4) React the homogeneous suspension with a reaction temperature of -4°C and a reaction time of 24 hours to obtain the product, which consists of rare earth layered hydroxide La containing incompletely reacted ...

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Abstract

The invention relates to preparation methods of rare earth layered hydroxide nanosheets and rare earth layered hydroxide nanosheet sol. The preparation method of the nanosheets comprises the followingsteps: preparing a lanthanum nitrate solution with a corresponding concentration, dissolving ammonium sulfate particles into the lanthanum nitrate solution according to a proportion so as to form a mixed solution, adjusting the pH of the mixed solution to 6-10, and continuously stirring to obtain uniform suspension; carrying out a reaction to obtain a product, immediately carrying out centrifugalseparation on the product, and drying to obtain the rare earth layered hydroxide La2(OH)4SO4.nH2O nanosheets. The rare earth layered hydroxide nanosheet sol is prepared by putting the prepared nanosheets into a formamide solution, carrying out ultrasonic centrifugal treatment, and then taking the supernatant. According to the preparation method, the rare earth layered hydroxide La2(OH)4SO4.nH2O nanosheets can be prepared in one step by using an ice-bath method, so that the problem that in the prior art, the compounds cannot be prepared into single-layer nanosheets by using the conventional intercalation-stripping method can be solved; furthermore, the preparation methods are simple in process and convenient to operate, and can realize mass production; the corresponding nanosheet sol is good in stability and material-saving.

Description

Technical field: [0001] The invention belongs to the technical field of material science, and in particular relates to a preparation method of a rare earth layered hydroxide nanosheet and a sol thereof. Background technique: [0002] La 2 (OH) 4 SO 4 ·nH 2 O is a layered rare earth compound RE 2 (OH) 4 SO 4 ·nH 2 One of O. Belonging to anionic layered compounds, the main layer of hydroxide is composed of nine coordination polyhedra [LaO 9 ] are connected by co-planar and common sides, the interlayer SO 4 2- The tetrahedron plays a role of charge balance through the covalent bonding of the two apex oxygen atoms with the adjacent two main layer plates respectively. The compound does not have the traditional layered rare earth compounds (such as RE 2 (OH) 5 A·nH 2 O, A = Cl, NO 3 etc.), so it is impossible to prepare ultra-thin nanosheets by the pillar-stripping process route. Its remarkable advantage is its special chemical ratio: the La / S molar ratio of the co...

Claims

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Application Information

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IPC IPC(8): C01F17/00B82Y40/00
CPCB82Y40/00C01F17/282C01P2002/22C01P2002/72C01P2004/24
Inventor 王雪娇姚传刚张蓉瑜常龙娇王秋实朱革王闯辛双宇
Owner BOHAI UNIV
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