Synthesis method of ordered ultramicroporous silicon dioxide

A technology of silicon dioxide and synthesis method, applied in the direction of silicon dioxide, silicon oxide, etc., can solve the problems of unsuitability for large-scale industrial production and application, harsh reaction conditions, complex production process, etc., and achieves stable shape and stable price. The effect of low cost and simple reaction system

Inactive Publication Date: 2014-12-03
JIANGXI AGRICULTURAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Although the above synthesis method can obtain ordered ultra-microporous materials, the templates used may need to be compounded, which is cumbersome to operate; or expensive,

Method used

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  • Synthesis method of ordered ultramicroporous silicon dioxide
  • Synthesis method of ordered ultramicroporous silicon dioxide
  • Synthesis method of ordered ultramicroporous silicon dioxide

Examples

Experimental program
Comparison scheme
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Embodiment 1～4

[0022] A kind of synthetic step of ordered ultramicroporous silica is as follows: at the temperature of 35 DEG C, sodium silicate and hydroabietyltrimethylammonium bromide (DTAB) are dissolved in deionized water, under the condition of stirring Slowly add inorganic acid dropwise until the pH of the solution is 8-10, and the ratio of material to SiO 2 :DTAB:HCl:H 2 O=1.0: 0.2: (1.4~2.1): 808.0, wherein the amount of HCl added is 2.1 in Example 1, 1.9 in Example 2, 1.7 in Example 3, and 1.4 in Example 2. After continuing to stir for 24 hours, move into hydrothermal In the reaction kettle, stand at 100° C. for crystallization for 24 hours, wash, filter and dry to obtain ordered ultramicroporous silicon dioxide precursor powder.

[0023] Carry out X-ray diffraction test to the product precursor of embodiment 1~4 respectively, the result is by figure 1 It can be seen that as the addition of HCl gradually decreases, the pH value of the system gradually increases, the sharpness and...

Embodiment 5～7

[0025] The preparation method is the same as in Example 2, except that the addition of DTAB is changed to prepare ultra-microporous silica, and the material ratio is SiO 2 :DTAB:HCl:H 2 O=1.0: (0.1~0.25): 1.9:808.0, wherein the addition amount of DTAB, embodiment 2 is 0.2, embodiment 5 is 0.1, embodiment 6 is 0.15, embodiment 7 is 0.25.

[0026] Carry out X-ray diffraction test to the product precursor of embodiment 5~7 respectively, and compare with embodiment 2, the result is by figure 2 It can be seen that with the gradual increase of the amount of DTAB added, the sharpness and peak intensity of the diffraction peaks of the samples show a trend of increasing first and then decreasing. When the material ratio is SiO 2 : DTAB = 1: 0.2, the sample at 2θ = 2.98°, 5.17° and 5.91° (d 100 =2.96nm,d 110 = 1.71nm, d 200 =1.49nm) the 100, 110 and 200 crystal plane diffraction peaks of the hexagonal phase appear respectively ( figure 2 -Example 2), illustrating that the sample...

Embodiment 8

[0028] The preparation conditions of the ultramicroporous silica precursor are the same as in Example 2, and the precursor is heated to 823K for calcination at a rate of 1K / min for 4h, and the calcined sample is at 2θ=3.11°, 5.33° and 6.14° (d 100 =2.84nm,d 110 = 1.66nm, d 200 =1.44nm) the 100, 110 and 200 crystal plane diffraction peaks of the hexagonal phase appear respectively ( image 3 ), indicating that the sample still maintains a highly ordered hexagonal ultramicroporous structure after calcination.

[0029] The transmission electron microscope characterization of embodiment 8 sees Figure 4 , the sample shows a regular and orderly channel structure in the direction of parallel channels ( Figure 4 .a), in the direction perpendicular to the channel, the sample still shows unconventional long-range ordered hexagonal ultramicropore channels ( Figure 4.b), the pore size is about 1.8nm, and the hole wall is 1nm.

[0030] N of Example 8 2 Adsorption-desorption charac...

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Abstract

The invention discloses a synthesis method of ordered ultramicroporous silicon dioxide, which comprises the following steps: proportionally dissolving a silicon source and a template in deionized water, slowly and dropwisely adding an acid solution to a pH value while stirring, transferring into a hydrothermal reaction kettle, standing at a certain temperature to crystallize, washing, filtering, drying to obtain ultramicroporous silicon dioxide precursor powder, and calcining to obtain the ordered ultramicroporous silicon dioxide molecular sieve. The ultramicroporous silicon dioxide has the characteristics of large specific area, high pore volume and highly ordered pore size; and the synthesis method has the advantage of simple technique and low production cost, and is suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to the field of inorganic porous materials, in particular to a method for synthesizing ordered ultramicroporous silica. Background technique [0002] In 1992, Mobil scientists first synthesized the highly ordered mesoporous molecular sieve M41S by using cationic quaternary ammonium salts with long-chain structures as structure guides, and introduced the concept of "template" in the explanation of material structure formation , established the important position of surfactants with amphiphilic groups in the synthesis of mesoporous materials. Since then, surfactants with different properties, such as nonionic surfactants, anionic surfactants, and amphoteric surfactants, have also been applied to the development of mesoporous materials, and many mesoporous materials with new structures have emerged, such as SBA -n, HMS-X, MSU, FDU, etc. People are constantly trying to increase the pore size of mesoporous materials in order to devel...

Claims

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Application Information

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IPC IPC(8): C01B33/12
Inventor 王鹏徐丽锋王宗德范国荣陈尚钘赵振东
Owner JIANGXI AGRICULTURAL UNIVERSITY
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