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Synthetic method for high length-diameter ratio layered doubled hydroxides grafted by organosilane

A synthesis method and organosilane technology, which is applied in the synthesis field of high aspect ratio organosilane grafted hydrotalcite mineral materials, can solve the problems of large stacking thickness, single shape, poor affinity, etc., and achieve uniform grain size distribution, Uniform shape and particle size to prevent secondary pollution

Inactive Publication Date: 2012-08-01
GUANGZHOU INST OF GEOCHEMISTRY - CHINESE ACAD OF SCI
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  • Description
  • Claims
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Problems solved by technology

The synthesized hydrotalcite is mainly lamellar crystals with a single shape; at the same time, its particle size is about several hundred nanometers to several microns, and the c-axis direction has a large stacking thickness of several microns, which is difficult to peel off
On the other hand, because the surface of hydrotalcite is hydrophilic and oleophobic, its affinity with organic matter is poor, and the interaction with organic matter is very weak.
Especially when it is added to the polymer matrix as a filler, due to the difference in surface affinity between the hydrotalcite and the polymer material, the hydrotalcite is prone to agglomeration; at the same time, due to the existence of a mutually repulsive interface between the two, It will also significantly affect the mechanical properties, barrier properties, etc. of the composite material.

Method used

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  • Synthetic method for high length-diameter ratio layered doubled hydroxides grafted by organosilane
  • Synthetic method for high length-diameter ratio layered doubled hydroxides grafted by organosilane
  • Synthetic method for high length-diameter ratio layered doubled hydroxides grafted by organosilane

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Experimental program
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Effect test

Embodiment 1

[0033] in Mg 2+ 、Al 3+ Hydrotalcite is a metal framework ion, gamma -Acicular organosilane-grafted hydrotalcite nanocrystals prepared with aminopropyltriethoxysilane as a shape-controlling and grafting modifier.

[0034] Weigh 9.6 g Mg(NO 3 ) 2 ?6H 2 O and 4.7 g Al(NO 3 ) 3 ?9H 2 O is co-dissolved in 44 cm 3 In deionized water (solution A), 4 g NaOH was dissolved in 50 cm 3 deionized water (solution B). At room temperature, solutions A and B were added dropwise to 50 ml of deionized water, and stirred rapidly, and the dropping speed was controlled to stabilize the pH value of the mixed solution at about 10. After the dropwise addition, it was washed and centrifuged until the centrifuged liquid became neutral, and the obtained precipitate was dried at 80°C for 12 h to obtain a hydrotalcite with a Mg / Al ratio of 3. The finely ground solid powder was calcined at 500°C for 6 h to obtain white composite metal oxide powder. Weigh 1.0 g composite metal oxide powder and a...

Embodiment 2

[0037]in Mg 2+ 、Al 3+ Hydrotalcite is used as metal skeleton ion, and γ-aminopropyltrimethoxysilane is used as morphology control and grafting modifier to prepare rod-shaped organosilane-grafted hydrotalcite nanocrystals.

[0038] Weigh 19.2 g Mg(NO 3 ) 2 ?6H 2 O and 9.4 g Al(NO 3 ) 3 ?9H 2 O is co-dissolved in 88 cm 3 In deionized water (solution A), 8 g NaOH was dissolved in 100 cm 3 deionized water (solution B). At room temperature, solutions A and B were added dropwise to 100 ml of deionized water, and stirred rapidly, and the dropping speed was controlled to stabilize the pH value of the mixed solution at about 10. After the dropwise addition, wash and centrifuge until the centrate is neutral. The resulting precipitate was dried at 80 °C for 12 h to obtain a hydrotalcite with a Mg / Al ratio of 3. The finely ground solid powder was calcined at 500°C for 6 h to obtain white composite metal oxide powder. Weigh 2.0 g composite metal oxide powder and add to 100 ml, ...

Embodiment 3

[0040] With Zn 2+ 、Al 3+ Hydrotalcite is a metal framework ion, gamma -Aminopropyltrimethoxysilane as a Morphology Controlling and Grafting Modifier for the Preparation of Fibrous Hydrotalcite Nanocrystals.

[0041] Weigh 10.9 g Zn(NO 3 ) 2 ?6H 2 O and 4.7 g Al(NO 3 ) 3 ?9H 2 O is co-dissolved in 44 cm 3 In deionized water (solution A), 8 g NaOH was dissolved in 50 cm 3 deionized water (solution B). Add solutions A and B dropwise to 50 ml deionized water at room temperature, and stir rapidly, and control the rate of addition to stabilize the pH value of the mixed solution at about 9. After the dropwise addition, wash and centrifuge until the centrate is neutral. The resulting precipitate was dried at 80 °C for 12 h to obtain a hydrotalcite with a Zn / Al ratio of 3. The finely ground solid powder was calcined at 500°C for 6 h to obtain white composite metal oxide powder. Weigh 2.0g composite metal oxide powder and add to 100ml, 0.3mol L -1 Na 2 CO 3 solution, ad...

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Abstract

The invention discloses a synthetic method for high length-diameter ratio layered doubled hydroxides grafted by organosilane, namely a roasting-restoring method. According to the synthetic method provided by the invention, a precursor of the layered doubled hydroxides prepared by co-precipitation is roasted and is structurally constructed (in a condition containing a single negative ion of CO3<->) by using the 'structural memory effect' of the layered doubled hydroxides. Equivalently, the cruder precursor of the layered doubled hydroxides with uneven appearance and grains, and impure phase and interlayer negative ions is crystallized again, so as to ensure that the purity, the features, the grain diameter and the like of the product are uniform. The obtained layered doubled hydroxides grafted by the organosilane is in a nanometer level, can be expected to improve the dispersity in a macromolecule base body material and is used for preparing the high-property nanometer composite material. The metal salt adopted by the synthetic method is NO3<->, CO2 in air and solution in a synthetic process enter a reaction system, and the final interlayer negative ion is CO3<2->, so as to avoid potential secondary pollution.

Description

technical field [0001] The invention belongs to the field of mineral material synthesis, in particular to a synthesis method of high aspect ratio organic silane grafted hydrotalcite mineral material. Background technique [0002] Hydrotalcite-like layered minerals, also known as anionic clays, are a general term for a class of layered doubled hydroxides (LDHs). Part of the Mg in its brucite-type octahedral structure 2+ By Al 3+ After the isotropic replacement of high-valent metal ions, the excess positive charge is released from the interlayer CO 3 2– Equilibrium of anions. The representative structural formula of hydrotalcite minerals can be expressed as: M +2 1–x m +3 x (OH) 2 A x / n n– mH 2 O, where M +2 is a +2 valent metal ion, M +3 It is a +3-valent metal ion, and A is an interlayer anion. Due to the unique positively charged laminate structure, excellent interlayer anion exchange performance and "roasting-recovery" (structural memory) characteristics, su...

Claims

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Application Information

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IPC IPC(8): C01B13/14C01F7/02C01G9/02C01G3/02C01G51/04C01G53/04C01F11/02B82Y30/00B82Y40/00
Inventor 何宏平陶奇朱建喜袁鹏
Owner GUANGZHOU INST OF GEOCHEMISTRY - CHINESE ACAD OF SCI
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