Method for rapidly preparing intercalation-type vermiculite by dry method

A vermiculite, fast technology, applied in chemical instruments and methods, inorganic chemistry, non-metallic elements, etc., can solve the problems of long intercalation reaction time, low efficiency, unfavorable industrial production, etc., to improve the intercalation reaction efficiency, simplify the Craftsmanship, the effect of reduced time

Inactive Publication Date: 2017-08-08
无锡永高新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the intercalation method of vermiculite is mostly to achieve the purpose of intercalation by stirring in the intercalation agent hot water solution...

Method used

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  • Method for rapidly preparing intercalation-type vermiculite by dry method
  • Method for rapidly preparing intercalation-type vermiculite by dry method
  • Method for rapidly preparing intercalation-type vermiculite by dry method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] The vermiculite of Shijiazhuang Dongping Mining and Building Materials Factory was pulverized through a jet mill and passed through a 100-mesh sieve to obtain the raw material vermiculite VMT.

[0016] The chemical composition is: SiO 2 : 41.2%, AL 2 o 3 : 12.68%, MgO: 24.22%, CaO: 0.96%, FeO: 1.54%, Fe 2 o 3 : 4.06%, TiO 2 : 1.33%, K 2 O: 5.97%, P 2 o 5 : 0.06%, H 2 O: 3%, Na 2 O: 1.6%, MnO: 0.043%, TiO: 5.097%, loss on ignition 6.71%.

[0017] Put 40 grams of VMT sample and 2 times of CEC dodecyltrimethylammonium bromide into the HAAKE torque rheometer, mix and stir at 120°C for 30min at a speed of 120rpm, take out the sample after centrifugation and filtration, Repeatedly washed 5 to 7 times with deionized water, after Ag ＋ No white precipitate (AgBr) was detected. Finally, the sample obtained by centrifugation and filtration was dried and ground into powder to obtain sample VMT12H. X-ray powder diffraction (XRD) tests were performed on VMT and VMT12H res...

Embodiment 2

[0020] Put 40 grams of VMT sample and cetyltrimethylammonium bromide with 2 times CEC into the HAAKE torque rheometer, mix and stir at 120°C for 30min at a speed of 120rpm, take out the sample after centrifugation and filtration, Repeatedly washed 5 to 7 times with deionized water, after Ag ＋ No white precipitate (AgBr) was detected. Finally, the sample obtained by centrifugation and filtration was dried and ground into powder to obtain sample VMT16H. X-ray powder diffraction (XRD) tests were performed on VMT and VMT12H respectively, and the corresponding patterns are as follows image 3 shown.

[0021] image 3 It is the XRD comparison pattern of samples VMT and VMT16H, the (001) plane diffraction peak of VMT in the figure is d The value, that is, the (001) interplanar spacing is 1.46nm. VMT16H d The diffraction peak with a value of 1.46nm disappeared, and a new diffraction peak at 5.25nm appeared at the same time. It shows that after dry intercalation, the intercalatio...

Embodiment 3

[0023] Put 40 grams of VMT sample and octadecyltrimethylammonium bromide with 2 times CEC into the HAAKE torque rheometer, mix and stir at 120°C for 30min at a speed of 120rpm, take out the sample after centrifugation and filtration, Repeatedly washed 5 to 7 times with deionized water, after Ag ＋ No white precipitate (AgBr) was detected. Finally, the sample obtained by centrifugation and filtration was dried and ground into powder to obtain sample VMT18H. X-ray powder diffraction (XRD) tests were performed on VMT and VMT18H respectively, and the corresponding patterns are as follows Figure 4 shown.

[0024] Figure 4 It is the XRD comparison pattern of samples VMT and VMT18H, the (001) plane diffraction peak of VMT in the figure is d The value, that is, the (001) interplanar spacing is 1.46nm. VMT18H d The diffraction peak with a value of 1.46nm disappeared, and a new diffraction peak at 4.58nm appeared at the same time. It shows that after dry intercalation, the interc...

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Abstract

The invention relates to a preparation method for organic intercalation modification of vermiculite. Disclosed is a method for quickly preparing intercalated vermiculite by dry method, which is characterized in that raw material of vermiculite is used as raw material, pulverized by jet mill, and then mixed with a certain proportion (2 times of CEC) of intercalation agent (dodecyl Trimethylammonium bromide, hexadecyltrimethylammonium bromide, octadecyltrimethylammonium bromide) were mixed and stirred for a certain period of time (30min) at a certain temperature (120°C) in the HAAKE torque rheometer ), the intercalation type vermiculite can be obtained, and the interlayer spacing of the vermiculite (001) crystal plane is enlarged to 4.03-5.25nm. Different from the traditional heating and stirring method to prepare intercalated clay minerals, the advantages of this method are (1) it can produce fast and efficient intercalation reaction, reduce the time of intercalation reaction and improve the efficiency of intercalation reaction; (2) There is no introduction of a liquid phase, and the final product does not need to be dried, which greatly simplifies the intercalation process.

Description

technical field [0001] The invention relates to the technique of performing dry organic intercalation modification on vermiculite and vermiculite concentrate so as to quickly obtain intercalation type vermiculite. It is a pre-process for the preparation of vermiculite nanocomposites. [0002] technical background [0003] Vermiculite is a magnesium-containing hydroaluminosilicate secondary metamorphic mineral with a layered structure of 2:1, mainly the alteration product of biotite and phlogopite by low-temperature hydrothermal action, and its chemical formula is Mg x (H 2 O){Mg 3-x [AlSi 3 o 10 ](OH) 2}. The crystal structure of vermiculite is composed of a unit structure layer composed of two layers of silicon-oxygen tetrahedral network layers and a layer of magnesium-oxygen octahedral layer. Since Al often replaces Si in silicon-oxygen tetrahedrons, the vermiculite structure layer is often negatively charged. , so there are cations between the structural layers to p...

Claims

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Application Information

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IPC IPC(8): C01B33/44
CPCC01B33/44C01P2002/72
Inventor 王智辉王彩虹韩炜张东元
Owner 无锡永高新材料科技有限公司
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