CN113603124A - Preparation method of sea urchin-shaped boehmite powder - Google Patents

Preparation method of sea urchin-shaped boehmite powder Download PDF

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Publication number
CN113603124A
CN113603124A CN202110816053.0A CN202110816053A CN113603124A CN 113603124 A CN113603124 A CN 113603124A CN 202110816053 A CN202110816053 A CN 202110816053A CN 113603124 A CN113603124 A CN 113603124A
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mixed solution
boehmite powder
sea urchin
preparation
alcohol
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Inventor
李丽娟
蔡亮
姬连敏
时东
彭小五
张利诚
宋富根
张禹泽
宋雪雪
聂锋
曾忠民
许淘善
郭凡
王杏芳
贾宇琛
何欣毓
牛勇
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Qinghai Institute of Salt Lakes Research of CAS
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Qinghai Institute of Salt Lakes Research of CAS
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00—Compounds of aluminium
    • C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/88—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by thermal analysis data, e.g. TGA, DTA, DSC
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/30—Particle morphology extending in three dimensions
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

The invention discloses a preparation method of sea urchin-shaped boehmite powder, which comprises the following steps: dissolving aluminum chloride hexahydrate in a water-alcohol mixed solvent to obtain a first mixed solution; adding urea into the first mixed solution, and stirring to obtain a second mixed solution; and carrying out hydrothermal reaction treatment on the second mixed solution, carrying out solid-liquid separation after the reaction is finished, and washing and drying the obtained solid to obtain the sea urchin-shaped boehmite powder. According to the preparation method of the sea urchin-shaped boehmite powder, provided by the invention, impurities, cations and surfactants except aluminum are not introduced in the preparation process and the product, the preparation method has the advantages of high purity and environmental friendliness, and the prepared boehmite powder has the advantages of small average particle size, good dispersibility, large specific surface area and the like.

Description

Preparation method of sea urchin-shaped boehmite powder
Technical Field
The invention belongs to the technical field of chemical production, and particularly relates to a preparation method of sea urchin-shaped boehmite powder.
Background
Boehmite, also called boehmite, has a molecular formula of gamma-AlOOH, belongs to an orthorhombic crystal system, and has a layered structure, in each single structural layer, oxygen ions are arranged at the top points of octahedrons in a cubic close packing manner, aluminum ions are positioned in the center of the octahedrons to form a double-layer structure, hydroxide radicals are positioned on the surface of the layered structure, and the layers are connected together by hydrogen bonds.
Boehmite is a product with high added value and is widely used in flame retardant additives, alumina precursors and medical drugs. Boehmite used for a flame retardant additive needs to have good dispersibility so that boehmite can be uniformly distributed in plastics and organic polymers, and furthermore, boehmite having a smaller particle size and a larger specific surface area is more favorable for close bonding with organic polymers, and improves the flame retardant effect of the flame retardant. The nano alumina is a good ceramic additive material, and the boehmite serving as an alumina precursor is also required to have the characteristics of small granularity, high comparative area and good dispersibility so that the calcined alumina can be tightly combined with a ceramic material.
At present, two methods, namely a liquid phase method and a solid phase method, are mainly used for producing boehmite, wherein the solid phase method is limited to a research stage in a laboratory due to the difficulty of an amplification experiment. The liquid phase method mainly comprises a micro-emulsion method, a sol-gel method, a hydrothermal method, a steam-assisted xerogel conversion method, a steam-assisted wet gel conversion method and the like. The microemulsion method is characterized in that a water solution and a solvent which is not soluble with water are mixed together and then a certain surfactant or cosurfactant is added to form a microemulsion system, the method has simple process and simple operation, but most of the surfactants are environmental harmful substances, so the method is not suitable for large-scale production before the problem of environmental pollution is not solved. The sol-gel method uses metal alkoxy compound or metal organic complex, and includes hydrolysis, polycondensation to gradually gelatinize, and drying heat treatment. The steam-assisted dry gel conversion method and the steam-assisted wet gel conversion method are characterized in that reactant gel and aqueous solution are separated in different containers, and the nano boehmite material with a special morphology is obtained by utilizing the action of high-temperature and high-pressure steam generated in the hydrothermal process, but the requirements on equipment are high, and the process is complex. The hydrothermal method has the advantages of simple operation, low cost and the like, and becomes a main production method of boehmite.
Chinese patent application (application No. 200510127179.8) discloses a preparation method of needle-shaped aluminum hydroxide, but magnesium ions are required to be introduced in the reaction process, and cationic impurities are introduced. Chinese patent application (application No. 201810708225.0) discloses a process for the preparation of hollow microsphere boehmites of high specific area using the environmentally hazardous surfactant cetyl trimethyl ammonium bromide.
Disclosure of Invention
In view of the defects of the prior art, the invention provides the preparation method of the sea urchin-shaped boehmite powder, which has simple process and easy operation and does not introduce impurity cations and surfactants.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of sea urchin-shaped boehmite powder is characterized by comprising the following steps:
dissolving aluminum chloride hexahydrate in a water-alcohol mixed solvent to obtain a first mixed solution;
adding urea into the first mixed solution, and stirring to obtain a second mixed solution;
and carrying out hydrothermal reaction treatment on the second mixed solution, carrying out solid-liquid separation after the reaction is finished, and washing and drying the obtained solid to obtain the sea urchin-shaped boehmite powder.
Preferably, the water in the water-alcohol mixed solvent is deionized water, and the alcohol is absolute ethyl alcohol or isopropanol.
Preferably, the volume ratio of alcohol to water in the water-alcohol mixed solvent is 1: (2.0-2.5).
Preferably, the concentration of aluminum ions in the first mixed solution is 0.27mol/L to 0.53 mol/L.
Preferably, in the second mixed solution, the ratio of the amount of the aluminum ions to the amount of the urea is 1: (2-4).
Preferably, the temperature for the hydrothermal reaction of the second mixed solution is 130-150 ℃ and the time is 11-13 h.
According to the preparation method of the sea urchin-shaped boehmite powder provided by the embodiment of the invention, impurities, cations and surfactants except aluminum are not introduced in the preparation process and the product, so that the preparation method has the advantages of high purity and environmental friendliness, and the prepared boehmite powder has the advantages of small average particle size, good dispersibility, large specific surface area and the like.
Drawings
FIG. 1 is a process flow diagram of a method for preparing sea urchin-like boehmite powder according to an embodiment of the present invention;
FIG. 2 is an SEM photograph of sea urchin-like boehmite powder obtained by production in example 1 of the present invention;
FIG. 3 is an XRD pattern of sea urchin-like boehmite powder obtained by the production of example 1 of the present invention;
FIG. 4 is a TG-DTG diagram of a sea urchin-like boehmite powder obtained by the production in example 1 of the present invention;
FIG. 5 is a graph showing the distribution of the particle size of sea urchin-like boehmite powder obtained in example 1 of the present invention;
FIG. 6 is an SEM photograph of sea urchin-like boehmite powder obtained by production in example 2 of the present invention.
FIG. 7 is an SEM photograph of sea urchin-like boehmite powder obtained by production in example 3 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention are described in detail below with reference to the accompanying drawings. Examples of these preferred embodiments are illustrated in the accompanying drawings. The embodiments of the invention shown in the drawings and described in accordance with the drawings are exemplary only, and the invention is not limited to these embodiments.
It should be noted that, in order to avoid obscuring the present invention with unnecessary details, only the structures and/or processing steps closely related to the scheme according to the present invention are shown in the drawings, and other details not so relevant to the present invention are omitted.
The embodiment of the invention provides a preparation method of sea urchin-shaped boehmite powder, and referring to fig. 1, the preparation method comprises the following steps:
and step S10, dissolving aluminum chloride hexahydrate in the water-alcohol mixed solvent to obtain a first mixed solution.
In a specific scheme, water in the water-alcohol mixed solvent is deionized water, and alcohol is absolute ethyl alcohol or isopropanol.
In a preferred embodiment, the volume ratio of alcohol to water in the water-alcohol mixed solvent is 1: (2.0-2.5).
In a preferred embodiment, the concentration of aluminum ions in the first mixed solution is 0.27mol/L to 0.53 mol/L.
And step S20, adding urea into the first mixed solution, and stirring to obtain a second mixed solution.
In a preferred embodiment, the ratio of the amount of the aluminum ions to the amount of the urea in the second mixed solution is 1: (2-4).
And step S30, carrying out hydrothermal reaction treatment on the second mixed solution, carrying out solid-liquid separation after the reaction is finished, and washing and drying the obtained solid to obtain the sea urchin-shaped boehmite powder.
In a preferable scheme, the temperature for carrying out the hydrothermal reaction on the second mixed solution is 130-150 ℃ and the time is 11-13 h.
The invention prepares the ultrafine boehmite by selecting proper aluminum source and precipitator, and the urea in the mixed solution is decomposed at high temperature to form NH3The aluminum chloride is precipitated under the alkaline condition, the grain size of the precipitate is effectively controlled by the alcohol solvent used as the dispersant, and the proper water-alcohol ratio also plays an effective role in regulating and controlling the growth direction and speed of the seed crystal. The boehmite crystal finally obtained is in a multi-thorn flower shape, has the characteristics of large specific surface area and the like, and has the main component of gamma-AlOOH and better thermal stability.
The sea urchin-shaped boehmite powder prepared by the method can be applied to a flame retardant material, can be decomposed to generate water vapor when being heated, absorbs a large amount of heat, dilutes combustible gas, and generates alumina which is attached to the surface of the material to play a role in oxygen and heat insulation, thereby being a good flame retardant additive.
Example 1
Dissolving 9.65g of aluminum chloride hexahydrate in a mixed solution of 50mL of deionized water and 25mL of anhydrous ethanol, and uniformly stirring to obtain a first mixed solution, wherein the volume ratio of the anhydrous ethanol to the deionized water in the solution is 1:2, and the concentration of aluminum ions is 0.53 mol/L.
And adding 4.8g of urea into the first mixed solution, dissolving, and uniformly stirring to obtain a second mixed solution, wherein the mass ratio of aluminum ions in the solution to the added urea is 1:2.
And placing the obtained second mixed solution in a reaction kettle for hydrothermal reaction, wherein the reaction time is 12 hours, and the reaction temperature is 140 ℃.
After the reaction is finished, naturally cooling the reaction kettle to room temperature, washing and filtering, washing the solid obtained by filtering with deionized water for three times, then washing with absolute ethyl alcohol for two times, and then drying at the drying temperature of 60 ℃ for 6 hours, thereby obtaining the sea urchin-shaped boehmite powder.
FIG. 2 is an SEM photograph of sea urchin-like boehmite powder obtained by the present example; FIG. 3 is an XRD pattern of a urchin-like boehmite powder obtained by the present example; FIG. 4 is a TG-DTG diagram of the urchin-like boehmite powder obtained in the present example; FIG. 5 is a graph showing the particle size distribution of the sea urchin-like boehmite powder obtained in the present example.
As seen from the SEM image of figure 2, the obtained boehmite is in a uniform multi-thorn flower shape (sea urchin shape), the particle size is less than 10 microns, the length of the grown thorns is less than 1 micron, the specific surface area is large, no obvious agglomeration phenomenon exists, the dispersibility is good, and the morphology requirement of the flame retardant additive is met. According to the test, the BET specific surface area of the urchin-shaped boehmite powder obtained in the example is 10m2/g～70m2/g。
As can be seen from the XRD pattern in figure 3, the diffraction peak in the pattern is basically consistent with the diffraction peak of gamma-AlOOH in the orthorhombic system, and no unnecessary impurity peak appears, which indicates that the product prepared by the method is pure gamma-AlOOH, namely boehmite, and the pattern has high peak intensity and narrow half-peak width, thereby indicating that the crystal has good crystallization condition.
As can be seen from the TG-DTG plot of FIG. 4, the primary dehydration temperature was 223 ℃ and the complete dehydration temperature was 380 ℃.
As can be seen from the particle size distribution diagram of FIG. 5, the particle size distribution of γ -AlOOH is uniform, mainly centered around 4 μm.
As flame retardant additives, gamma-AlOOH with Al (OH)3In contrast, Al (OH)3At 200 deg.CThe thermal decomposition is started to generate water vapor, but the curing temperature of the thermoplastic resin is more than 200 ℃, which causes the problem that the surface of the cured plastic is uneven, and the boehmite solves the problem, the initial temperature of boehmite dehydration is more than 200 ℃, the complete dehydration needs to reach 380 ℃, which is higher than the curing temperature of the plastic, and the acid and alkali resistance of the boehmite is stronger.
Example 2
Dissolving 4.83g of aluminum chloride hexahydrate in a mixed solution of 50mL of deionized water and 20mL of anhydrous ethanol, and uniformly stirring to obtain a first mixed solution, wherein the volume ratio of the anhydrous ethanol to the deionized water in the solution is 1:2.5, and the concentration of aluminum ions is 0.286 mol/L.
And adding 4.8g of urea into the first mixed solution, dissolving, and uniformly stirring to obtain a second mixed solution, wherein the mass ratio of aluminum ions in the solution to the added urea is 1: 4.
And placing the obtained second mixed solution in a reaction kettle for hydrothermal reaction, wherein the reaction time is 13h, and the reaction temperature is 130 ℃.
After the reaction is finished, naturally cooling the reaction kettle to room temperature, washing and filtering, washing the solid obtained by filtering with deionized water for three times, then washing with absolute ethyl alcohol for two times, and then drying at the drying temperature of 60 ℃ for 6 hours, thereby obtaining the sea urchin-shaped boehmite powder.
FIG. 6 is an SEM photograph of sea urchin-like boehmite powder obtained by the present example. As seen from the SEM image of FIG. 6, the obtained boehmite had a uniform multi-spike shape (sea urchin shape), a particle size of less than 10 μm, a length of grown spikes of less than 1 μm, and a large specific surface area.
Example 3
9.65g of aluminum chloride hexahydrate is dissolved in a mixed solution of 50mL of deionized water and 25mL of isopropanol, and the mixed solution is uniformly stirred after dissolution to obtain a first mixed solution, wherein the volume ratio of absolute ethyl alcohol to deionized water in the solution is 1:2, and the concentration of aluminum ions is 0.53 mol/L.
And adding 4.8g of urea into the first mixed solution, dissolving, and uniformly stirring to obtain a second mixed solution, wherein the mass ratio of aluminum ions in the solution to the added urea is 1:2.
And placing the obtained second mixed solution in a reaction kettle for hydrothermal reaction, wherein the reaction time is 12 hours, and the reaction temperature is 140 ℃.
After the reaction is finished, naturally cooling the reaction kettle to room temperature, washing and filtering, washing the solid obtained by filtering with deionized water for three times, then washing with absolute ethyl alcohol for two times, and then drying at the drying temperature of 60 ℃ for 6 hours, thereby obtaining the sea urchin-shaped boehmite powder.
FIG. 7 is an SEM photograph of sea urchin-like boehmite powder obtained by the present example; FIG. 7 is an SEM photograph of sea urchin-like boehmite powder obtained by the present example. As seen from the SEM image of FIG. 7, the obtained boehmite was in a uniform multi-spiny shape (sea urchin shape), particle size was less than 10 μm, the length of the grown spines was less than 1 μm, and specific surface area was large.
In summary, according to the preparation method of the sea urchin-shaped boehmite powder provided by the embodiment of the invention, impurities, cations and surfactants except for aluminum are not introduced in the preparation process and the product, so that the preparation method has the advantages of high purity and environmental friendliness, and the prepared boehmite powder has the advantages of small average particle size, good dispersibility, large specific surface area and the like.
The foregoing is directed to embodiments of the present application and it is noted that numerous modifications and adaptations may be made by those skilled in the art without departing from the principles of the present application and are intended to be within the scope of the present application.

Claims (6)

1. A preparation method of sea urchin-shaped boehmite powder is characterized by comprising the following steps:
dissolving aluminum chloride hexahydrate in a deionized water-alcohol mixed solvent to obtain a first mixed solution;
adding urea into the first mixed solution, and stirring to obtain a second mixed solution;
and carrying out hydrothermal reaction treatment on the second mixed solution, carrying out solid-liquid separation after the reaction is finished, and washing and drying the obtained solid to obtain the sea urchin-shaped boehmite powder.
2. The method for producing sea urchin-like boehmite powder according to claim 1, wherein water in the water-alcohol mixed solvent is deionized water, and the alcohol is absolute ethyl alcohol or isopropyl alcohol.
3. The method for producing sea urchin-like boehmite powder according to claim 2, characterized in that the volume ratio of alcohol to water in the water-alcohol mixed solvent is 1: (2.0-2.5).
4. The method for producing a echinoid boehmite powder according to claim 1, characterized in that the concentration of aluminum ions in the first mixed solution is 0.27 to 0.53 mol/L.
5. The method according to claim 1, wherein the amount ratio of the aluminum ions to the urea in the second mixed solution is 1: (2-4).
6. The method for producing a echinoid boehmite powder according to claim 1, characterized in that the temperature at which the second mixed solution is subjected to the hydrothermal reaction is 130 to 150 ℃ for 11 to 13 hours.
CN202110816053.0A 2021-07-19 2021-07-19 Preparation method of sea urchin-shaped boehmite powder Pending CN113603124A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115304405A (en) * 2022-07-29 2022-11-08 广东精英无机材料有限公司 Boehmite digital glaze ink and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4048295A (en) * 1974-12-21 1977-09-13 Condea Chemie Gmbh Process for making extrudates from aluminum oxyhydrates
CN101597076A (en) * 2009-07-01 2009-12-09 武汉科技大学 A kind of Seashell boehmite powder and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4048295A (en) * 1974-12-21 1977-09-13 Condea Chemie Gmbh Process for making extrudates from aluminum oxyhydrates
CN101597076A (en) * 2009-07-01 2009-12-09 武汉科技大学 A kind of Seashell boehmite powder and preparation method thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
徐冰: ""纳米/微米薄水铝石自组装及其生长机理研究"", 《中国博士学位论文全文数据库工程科技Ⅰ辑》 *
潘裕柏等: "《稀土陶瓷材料》", 31 May 2016, 冶金工业出版社 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115304405A (en) * 2022-07-29 2022-11-08 广东精英无机材料有限公司 Boehmite digital glaze ink and preparation method thereof
CN115304405B (en) * 2022-07-29 2023-09-26 广东精英无机材料有限公司 Boehmite digital glaze ink and preparation method thereof

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Application publication date: 20211105