WO2002085784A1 - Process for the preparation of inorganic nanoparticles - Google Patents

Process for the preparation of inorganic nanoparticles Download PDF

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Publication number
WO2002085784A1
WO2002085784A1 PCT/IN2002/000108 IN0200108W WO02085784A1 WO 2002085784 A1 WO2002085784 A1 WO 2002085784A1 IN 0200108 W IN0200108 W IN 0200108W WO 02085784 A1 WO02085784 A1 WO 02085784A1
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WIPO (PCT)
Prior art keywords
template
nanoparticles
solid
reactant
anyone
Prior art date
Application number
PCT/IN2002/000108
Other languages
French (fr)
Inventor
Vinodkumar Ramniranjan Dhanuka
Gangundi Prakash Babu
Charu Rajesh Vatsa
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Hindustan Lever Limited
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Publication of WO2002085784A1 publication Critical patent/WO2002085784A1/en

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
    • C01B33/187—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates
    • C01B33/193—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates of aqueous solutions of silicates
    • 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
    • C01F7/04—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom
    • C01F7/14—Aluminium oxide or hydroxide from alkali metal aluminates
    • C01F7/141—Aluminium oxide or hydroxide from alkali metal aluminates from aqueous aluminate solutions by neutralisation with an acidic agent
    • C01F7/142—Aluminium oxide or hydroxide from alkali metal aluminates from aqueous aluminate solutions by neutralisation with an acidic agent with carbon dioxide
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/04—Oxides; Hydroxides
    • C01G23/047—Titanium dioxide
    • C01G23/07—Producing by vapour phase processes, e.g. halide oxidation
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/01—Crystal-structural characteristics depicted by a TEM-image
    • 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
    • C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
    • 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
    • C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • 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
    • C01P2004/32—Spheres
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/51—Particles with a specific particle size distribution
    • C01P2004/52—Particles with a specific particle size distribution highly monodisperse size distribution
    • 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
    • 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
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/12—Surface area
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/19—Oil-absorption capacity, e.g. DBP values
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/141—Feedstock

Definitions

  • the present invention relates to a process for the preparation of inorganic nanoparticles using a solid template.
  • Nanoparticles are those particles having a particle size less than 100 nm.
  • a process for the preparation of inorganic nanoparticles comprising: i. contacting the solid template with at least one reactant in the form of liquid or solution ii. exposing the wet solid template to a reactant in the gaseous form iii. allowing the formation of the nanoparticles on the template and iv. Optionally separating the template to recover the desired nanoparticles.
  • a process for the preparation of inorganic nanoparticles comprising: i. contacting the solid template with water or water comprising at least one metal salt dissolved in it; ii. exposing the wet solid template to carbon di oxide or gaseous form of metal salts over a period greater than 10 minutes; iii. allowing the formation of the nanoparticles on the template; iv. and optionally separating the template to recover the desired nanoparticles
  • the process comprises contacting the silica or aluminium containing alkaline material on to a solid template and reacting it with carbon dioxide over a period of not less than 10 minutes allowing the formation of the nanoparticles on the template and optionally separating the template to recover the desired nanoparticles.
  • the process comprises contacting the solid template with water and reacting the said wet solid template with silicon or aluminium or titanium containing gaseous reactant over a period of not less than 10 minutes allowing the formation of the nanoparticles on the template and optionally separating the template to recover the desired nanoparticles.
  • the invention essentially provides for process of preparation of nanoparticles wherein the inorganic nanoparticles is formed on a solid template by exposing the solid template wetted with a liquid or a solution of a metal salt.
  • the solid templates can be made of any known material e.g. ceramic, metal, polymer etc.
  • a solid that can be separated from the nanoparticles with minimal amounts of the solid contaminating the nanoparticles may be relatively ashless cellulosic material such as paper, fabric, wood or other synthetic material.
  • the nanoparticles may be separated from the solid template by mechanical means or by calcining the template.
  • Temperature of the reaction can be upto 120 °C.
  • the preferred temperature range is 15-75°C.
  • Concentration range of the reactant where metal salts are dissolved in water that is used to wet the solid template can range from 0.5 to 50% and is preferably 5-15%. It is preferable to have the rate of reaction slow and is advantageous to complete the reaction over a period of 10 minutes to 24 hours and most preferably over 8 -16 hours.
  • IR Infra red spectroscopy
  • TEM transmission electron microscopy
  • Ashless Whatman No. 44 filter paper was used as the solid template. The initial weight of the paper was determined. The filter paper was dipped in distilled water. The wet solid template was taken out of the solution and was reacted with titanium tetrachloride vapours for a period of 2 hours. The solid template is dried simultaneously. The dried template was washed with distilled water and dried. The template was calcined at 650 °C for 2 hours. The ash containing the nanoparticles of titanium dioxide was weighed and characterised by IR spectroscopy and the particle size was measured by transmission electron microscopy (TEM).
  • TEM transmission electron microscopy
  • the IR spectrum of the ash obtained above was recorded as its KBr pellet.
  • the Fig. la shows two intense bands at 1085-1090 and 795-800 cm “1 which are characteristic of Si-O vibrations of silica.
  • Fig. lb shows two bands at 724 and 603 cm "1 and
  • Fig. lc shows a strong band at 677 cm “1 which are characteristic of aluminium oxide and titanium dioxide, respectively. All the above spectra show that the reaction was complete and that there were no other significant peaks visible.
  • the ash was suspended in isopropyl alcohol (IP A).
  • IP A isopropyl alcohol
  • a drop of this suspension was placed on carbon coated or formvar coated copper grid and observed under transmission electron microscope (Phillips CM 200).
  • the micrographs (Fig. 2 a-c) were recorded at magnifications and several grids were viewed for each sample.
  • the particle size of silica was found to be in the range 8-60 nm, alumina was in the range 50-80 nm, and titania 15-20 nm.

Abstract

Process for the preparation of inorganic nanoparticles comprising contacting a solid template with at least one reactant in the form of liquid and/or solution to thereby provide said solid template with said reactant thereon; exposing the wet solid template thus obtained a reactant in the gaseous form; allowing the formation of the nanoparticles from said template; and optionally, separating the template to recover the desired nanoparticles.

Description

PROCESS FOR THE PREPARATION OF INORGANIC NANOPARTICLES
Technical Field:
The present invention relates to a process for the preparation of inorganic nanoparticles using a solid template.
Background and Prior art:
The synthesis and characterisation of inorganic nanoparticles is a rapidly emerging field with wide ranging applications in catalysis, diagnostics, electronics and communications. Nanoparticles are those particles having a particle size less than 100 nm.
A number of methods for preparation of nanoparticles that involve chemical or physical methods have been reported in literature. The most common physical method involves gas condensation technique where metal vapours are condensed in the form of nanoparticles. The major problem with this method is that due to inhomogeneous heating of the source the control over the particle size and distribution is not possible. Aerosol generation method involves the passing of the reactant gas through the flame and due to the high surface to volume ratio nanoparticles are formed. Chemical processes such as microemulsion method involves the precipitation within aqueous micelles of water-in-oil microemulsions. The reported methods are laborious, time consuming, multi-step, expensive and difficult to scale up to commercial process.
Most of the important inorganic nanoparticles such as silica, alumina, titania, zinc oxide etc are thermally stable and hence have a wide range of applications.
US 5580655 (Dow Corning Corp.) 1996, discloses a process for the preparation of web-like nanoparticles of silica by laser vaporisation of silicon metal in a helium/oxygen atmosphere in a diffusion cloud chamber.
We have now been able to develop a simple, cost effective process for the preparation of inorganic nanoparticles for e.g. silica, alumina and titania etc. that involves the generation of the nanoparticles on a solid template which is later recovered if desired. Description of the Invention:
According to the present invention there is provided a process for the preparation of inorganic nanoparticles comprising: i. contacting the solid template with at least one reactant in the form of liquid or solution ii. exposing the wet solid template to a reactant in the gaseous form iii. allowing the formation of the nanoparticles on the template and iv. Optionally separating the template to recover the desired nanoparticles.
According to the preferred aspect of the present invention there is provided a process for the preparation of inorganic nanoparticles comprising: i. contacting the solid template with water or water comprising at least one metal salt dissolved in it; ii. exposing the wet solid template to carbon di oxide or gaseous form of metal salts over a period greater than 10 minutes; iii. allowing the formation of the nanoparticles on the template; iv. and optionally separating the template to recover the desired nanoparticles
According to one preferred aspect of the invention the process comprises contacting the silica or aluminium containing alkaline material on to a solid template and reacting it with carbon dioxide over a period of not less than 10 minutes allowing the formation of the nanoparticles on the template and optionally separating the template to recover the desired nanoparticles.
According to another preferred aspect of the invention the process comprises contacting the solid template with water and reacting the said wet solid template with silicon or aluminium or titanium containing gaseous reactant over a period of not less than 10 minutes allowing the formation of the nanoparticles on the template and optionally separating the template to recover the desired nanoparticles.
Detailed description of the invention: The invention essentially provides for process of preparation of nanoparticles wherein the inorganic nanoparticles is formed on a solid template by exposing the solid template wetted with a liquid or a solution of a metal salt. The solid templates can be made of any known material e.g. ceramic, metal, polymer etc. When we wish to separate the nanoparticles form the solid template it is particularly preferred to have a solid that can be separated from the nanoparticles with minimal amounts of the solid contaminating the nanoparticles. Particular examples of such material may be relatively ashless cellulosic material such as paper, fabric, wood or other synthetic material. The nanoparticles may be separated from the solid template by mechanical means or by calcining the template.
Temperature of the reaction can be upto 120 °C. The preferred temperature range is 15-75°C. Concentration range of the reactant where metal salts are dissolved in water that is used to wet the solid template can range from 0.5 to 50% and is preferably 5-15%. It is preferable to have the rate of reaction slow and is advantageous to complete the reaction over a period of 10 minutes to 24 hours and most preferably over 8 -16 hours.
The invention will now be illustrated by the following non-limiting examples.
Examples:
Example 1: i. Process for the preparation of nanoparticles of alumina or silica Ashless Whatman No. 44 filter paper was used as the solid template. The initial weight of the paper was determined. The filter was dipped in 15% sodium silicate solution prepared from commercially available neutral sodium silicate solution having a Siθ2/Na2O = 3.02 or 7.5% sodium aluminate solution prepared from commercially available sodium aluminate solution 1:1 in water (Al2O3/Na2O = 0.75). The wet solid template was taken out of the solution and was reacted with carbon dioxide for a period of 18 hours. The solid template is dried simultaneously. The dried template was washed with distilled water and dried. The template was calcined at 650 °C for 2 hours. The ash containing the naoparticles of silica or alumina was weighed and characterised by Infra red spectroscopy (IR) and the particle size was measured by transmission electron microscopy (TEM). ii. Process for the preparation of nanoparticles of titania
Ashless Whatman No. 44 filter paper was used as the solid template. The initial weight of the paper was determined. The filter paper was dipped in distilled water. The wet solid template was taken out of the solution and was reacted with titanium tetrachloride vapours for a period of 2 hours. The solid template is dried simultaneously. The dried template was washed with distilled water and dried. The template was calcined at 650 °C for 2 hours. The ash containing the nanoparticles of titanium dioxide was weighed and characterised by IR spectroscopy and the particle size was measured by transmission electron microscopy (TEM).
iii. Infra red Spectroscopy:
The IR spectrum of the ash obtained above was recorded as its KBr pellet. The Fig. la shows two intense bands at 1085-1090 and 795-800 cm"1 which are characteristic of Si-O vibrations of silica. Fig. lb shows two bands at 724 and 603 cm"1 and Fig. lc shows a strong band at 677 cm"1 which are characteristic of aluminium oxide and titanium dioxide, respectively. All the above spectra show that the reaction was complete and that there were no other significant peaks visible.
iv. Transmission electron microscopy:
The ash was suspended in isopropyl alcohol (IP A). A drop of this suspension was placed on carbon coated or formvar coated copper grid and observed under transmission electron microscope (Phillips CM 200). The micrographs (Fig. 2 a-c) were recorded at magnifications and several grids were viewed for each sample. The particle size of silica was found to be in the range 8-60 nm, alumina was in the range 50-80 nm, and titania 15-20 nm.

Claims

L A process for the preparation of inorganic nanoparticles comprising:
i) providing a solid template with at least one reactant thereon; ii) exposing the solid template with said reactant to another reactant in a gaseous form; and iii) allowing formation of the desired nanoparticles on the said template.
2. A process as claimed in claim 1 comprising separating the nanoparticles from said sohd template to thereby recover the desired inorganic nanoparticles.
3. A process as claimed in anyone of claims 1 or 2 wherein-
i) said solid template is contacted with at least one reactant in the form of liquid and/or solution to thereby provide said solid template with said reactant thereon; ii) exposing the wet solid template thus obtained under (i) above to a reactant in the gaseous form; iii) allowing the formation of the nanoparticles from said template; and iv) optionally, separating the template to recover the desired nanoparticles.
4. A process as claimed in anyone of claims 1 to 3 comprising:
i) contacting the said solid template with water and/or water comprising at least one metal salt dissolved in it; ii) exposing the wet solid template to carbon dioxide or gaseous form of metal salts for a period greater than 10 minutes; iii) allowing the formation of nanoparticles on the template; and iv) optionally, separating the template; to recover the desired nanoparticles.
5. A process as claimed in anyone of claims 1 to 4 comprising-
i) providing said solid template with silica or aluminium containing alkaline material as said reactant; ii) reacting the thus provided reactant on said solid template under (i) above with carbon dioxide over a period of not less than 10 minutes; iii) allowing the formation of the desired inorganic nanoparticles on the template; and optionally iv) separating the template to recover the desired nanoparticles.
6. A process as claimed in anyone of claims 1 to 4 comprising:
i) contacting the solid template with water; ii) reacting the wet solid template with anyone or more of silica, alumina and titania containing gaseous reactant over a period of not less than 10 minutes; iii) allowing the formation of the nanoparticles on the template ; and optionally iv) separating the template to recover the desired nanoparticles.
7. A process as claimed in anyone of claims 1 to 6 wherein said solid template used is selected from one or more of ceramic, metal, polymer, ashless cellulosic material.
8. A process as claimed in claim 7 wherein to facilitate separation of the nanoparticles from said solid template the solid template use is selectively obtained of ashless cellulosic material selected from paper, fabric, wood selected synthetic materials.
9. A process as claimed in anyone of claims 1 to 8 wherein said nanoparticles are separated from the solid template by mechanical means andor by calcining the template.
10. A process as claimed in claim 9 wherein temperature of the reaction is up to 120 °C preferably in the range of 15-75 °C.
11. A process as claimed in anyone of claims 4 to 10 wherein concentration of the metal salt dissolved in water to wet solid template is used in the range from 0.5 to 50% preferably 5-15%.
12. A process as claimed in anyone of claims 1 to 11 wherein said rate of reaction is selected such as to complete the reaction over a period of 10 minutes to 24 hours and more preferably 8-16 hours.
13. A process for the manufacture of inorganic nanoparticles substantially as herein described and illustrated with reference to the accompanying examples.
PCT/IN2002/000108 2001-04-19 2002-04-18 Process for the preparation of inorganic nanoparticles WO2002085784A1 (en)

Applications Claiming Priority (2)

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IN352/MUM/2001 2001-04-19
IN352MU2001 2001-04-19

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1997040105A1 (en) * 1996-04-22 1997-10-30 Rhodia Chimie Method for preparing hollow silica particles
CN1301590A (en) * 1999-12-29 2001-07-04 中国科学院生态环境研究中心 Method and equipoment for synthesizing nanometer particle by film reactor

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1997040105A1 (en) * 1996-04-22 1997-10-30 Rhodia Chimie Method for preparing hollow silica particles
CN1301590A (en) * 1999-12-29 2001-07-04 中国科学院生态环境研究中心 Method and equipoment for synthesizing nanometer particle by film reactor

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
CRACIUN R: "Characterization of mixed amorphous/crystalline cerium oxide supported on SiO2", SOLID STATE IONICS, NORTH HOLLAND PUB. COMPANY. AMSTERDAM, NL, vol. 110, no. 1-2, 1 July 1998 (1998-07-01), pages 83 - 93, XP004123850, ISSN: 0167-2738 *
DATABASE WPI Section Ch Week 200161, Derwent World Patents Index; Class J04, AN 2001-542323, XP002211841 *
PLYUTO, YURI ET AL: "Ag nanoparticles synthesised in template-structured mesoporous silica films on a glass substrate", CHEMICAL COMMUNICATIONS (CAMBRIDGE) (1999), (17), 1653-1654, XP001096086 *

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