WO2009127773A1 - Method of using an electric field in the synthesis of materials - Google Patents

Method of using an electric field in the synthesis of materials Download PDF

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Publication number
WO2009127773A1
WO2009127773A1 PCT/FI2009/000048 FI2009000048W WO2009127773A1 WO 2009127773 A1 WO2009127773 A1 WO 2009127773A1 FI 2009000048 W FI2009000048 W FI 2009000048W WO 2009127773 A1 WO2009127773 A1 WO 2009127773A1
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Prior art keywords
synthesis
dielectric layer
materials
dielectric
typically
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PCT/FI2009/000048
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French (fr)
Inventor
Mika Tapio Reijonen
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Mika Tapio Reijonen
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Publication of WO2009127773A1 publication Critical patent/WO2009127773A1/en

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006Controlling or regulating processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/08Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J19/087Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B30/00Production of single crystals or homogeneous polycrystalline material with defined structure characterised by the action of electric or magnetic fields, wave energy or other specific physical conditions
    • C30B30/02Production of single crystals or homogeneous polycrystalline material with defined structure characterised by the action of electric or magnetic fields, wave energy or other specific physical conditions using electric fields, e.g. electrolysis
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0803Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy
    • B01J2219/0805Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges
    • B01J2219/0807Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges involving electrodes
    • B01J2219/0809Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electric or magnetic energy giving rise to electric discharges involving electrodes employing two or more electrodes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0873Materials to be treated
    • B01J2219/0875Gas
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0873Materials to be treated
    • B01J2219/0877Liquid
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0873Materials to be treated
    • B01J2219/0879Solid

Definitions

  • An invention is a synthesis method using of a direct electric field.
  • the synthesis of the materials is affected by causing polarization of materials by the electric field.
  • the invention can be used with medicines and other materials in synthetic chemistry, medicine chemistry, polymer chemistry, biochemistry and nanotechnology.
  • Microwaves are affected by an electric field, and in this Wikipedia article there are told for causing reaction without solvent, but also a solvent can be used, such as in a publication Microwave- assisted wet chemical synthesis: advantages, significance, and steps to industrialization, Shangzhao Shi and Jiann-Yang Hwang. Journal of Minerals & Materials Characterization & Engineering, Vol. 2, No. 2,p. 101-110, 2003 www.imp.mtu.edu/jmnice/issue2- 2/3_Shi_Micro wave-assisted_wet_chemical_synthesis.pdf gotten 11 April 2008.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Electrochemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

A synthesis method using polarization of materials by an electric field consists of two electrodes (1 and 4), an insulation layer (2), a dielectric layer (3) where the synthesis takes place, a voltage supply (5), a closed circuit and a synthesis container.

Description

METHOD OF USING AN ELECTRIC FIELD IN THE SYNTHESIS OF MATERIALS
TECHNICAL FIELD
An invention is a synthesis method using of a direct electric field. The synthesis of the materials is affected by causing polarization of materials by the electric field. The invention can be used with medicines and other materials in synthetic chemistry, medicine chemistry, polymer chemistry, biochemistry and nanotechnology.
BACKGROUND OF THE INVENTION
Synthesis methods have been developed during many years, and a significant step was uses microwaves during synthesis. For example in the article of Nature journal, Microwave chemistry, Out of the kitchen http://www.nature.com/drugdisc/news/articles/421571a.html gotten 11 April 2008 is told of the benefits of the method, such as for example it can get more desired product, and on the other hand, less by-products. There are more information about using microwaves in chemistry e.g. in Wikipedia http://en. wikipedia.org/wiki/Micro wave_chemistry_gotten 11 April 2008. Microwaves are affected by an electric field, and in this Wikipedia article there are told for causing reaction without solvent, but also a solvent can be used, such as in a publication Microwave- assisted wet chemical synthesis: advantages, significance, and steps to industrialization, Shangzhao Shi and Jiann-Yang Hwang. Journal of Minerals & Materials Characterization & Engineering, Vol. 2, No. 2,p. 101-110, 2003 www.imp.mtu.edu/jmnice/issue2- 2/3_Shi_Micro wave-assisted_wet_chemical_synthesis.pdf gotten 11 April 2008.
The use of the microwaves is not restricted to organic synthesis, but microwaves are used also with inorganic materials, such as it is presented in Microwave-assisted synthesis of inorganic materials http://www.scs.uiuc.edu/chem/research/materials/seminar_abstracts/2006- 2007ZHelmich.abstract_copy.pdf gotten 11 April 2008. Microwaves have also other effects than heat motion of molecules and so reaction rate connected effects. On the page http://www.tan-delta.com/basics.html gotten 11 April 2008 it is told the theory on effects of microwaves, where it is presented polarization and conduction mechanisms (dipolar polarization, conduction mechanisms and interfacial polarization). Such according to the same inventor as now, Reijonen M. electrical crystallization invention WO/2007/017552 the main thing is that there are not forming an electrical double layer, whereby so it do not happen extremely fast potential drop with a short distance of polarization effect. Other electrode (1) has been coated with an insulating layer (2), whereby there is no threat of electrolysis and other electrode (4) is without an insulating layer, and so it happens conduction from this electrode (4) to the dielectric material (3). Electrodes (1 and 4) are attached to a controllable power supply (5) by cables.
With the help of the microwaves, the synthesis will get benefits, when it has e.g. an accelerated reaction rate and an improved yield. The method is environmentally friendly and can make synthesis even without solvent, and so it will get cleaner products. The microwave technology is applied for example in the area of drug discovery, for example
Collins, M. Drug discovery at the speed of light http://www.cem.de/documents/pdf/microwave_synthesis_theory.pdf and in the nanotechnology area, such as in US patent publication Lin L. et al. Localized synthesis and self-assembly of nanostructures 7,311,776 25 December 2007 presents using of the electric field in the synthesis of nanostructures and in self-organizing.
There are many problems of using microwaves in synthesis. One problem is extremely difficult to get in the large scale to make synthesis. In addition, microwaves heat materials rapidly and compounds can be sensitive to heat, so the compounds decompose. The use of microwaves needs for radiation protection, and it is an indirect method compared to the presenting method.
Each microwave oven user knows that you cannot put it a normal metal container neither empty glass, but, for example you can put a glass of water. Microwaves heat water, but not glass. You can put for example solid table sugar, and it warms. Many materials are polar or could making polar, and so this invention method works in many applications. Molecules in food, also other than water molecules, for example mono-, di- and polysaccharides, amino acids, lipids and proteins are affected by microwaves. So microwaves affect to different materials by a different way. Materials can be shared to three different classes: conductor, insulator and dielectric
(http://www.cem.com/synthesis/niwbscs.asp gotten 11 April 2008). Words insulator and dielectric are often synonyms, such as in Wikipedia "A dielectric is a non-conducting substance, i.e. an insulator." http://en.wikipedia.org/wiki/Dielectric gotten 11 April 2008.
By the same inventor, Reijonen M. electrical crystallization invention WO/2007/01755 both in the claims of patent and in the examples it is clarified that the crystallizing material is in a dielectric area. In the presenting invention, the synthesis takes place there. The dielectric area (2) can be pure material for example as the molten or as a solid material or for example as gel, whereby, although gel would include water, so an electric double layer is not formed in a remarkable way. In addition, it can be used electricity non-conduction emulsion. Also aqueous solution can be electricity non-conducting dielectric mixture, such aqueous solution of the table sugar.
SUMMARY OF THE INVENTION
According to the presenting method it can be changed directly polaricity of materials by an electric field. Because almost all materials are Polaris able and temporary Polaris able in the molecules occurs often, and so the method can used widely. For example most drugs and organic compounds are dielectric, and the application area is extremely large. Other electrode (1) has been coated with an insulating layer (2), whereby there are not threaten with electrolysis, and other electrode (4) is without an insulating layer and so it happens conduction form this electrode to the dielectric material (3), where the synthesis takes place. Electrodes (1 and 4) are attached with conductors to a controllable power supply (5).
Now presented method has several advantages. Unlike by using the microwaves, it does not need to use heating, if it is not wanted. The presenting method has extremely good scaling benefits comparing to e.g. microwave systems. The apparatus can be like as an accumulator like several plates. According to the method use it is also not need the radiation protection, and the method is easy to combine with other process, such as recrystallization. DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
During the synthesis it is easily to change an electric force and its direction and other conditions, such as temperature, pH, pressure and mixing. Synthesis, crystallization and re- crystallization can make in the same device and the controlling of the process can be carried out with an analysis of input/output energies, and with the using of Process analytical tool (PAT) tools, such as spectroscopic and x-ray diffraction methods, also in line, such as Raman, NIR, IR NMR, XRD and conductance etc. based methods. According to the method, it is able to also to follow and to change the synthesis consumed voltage and current as a function of time.
Examples
Example 1
The synthesis of coumarin on Knoevenagel condensation using an electric field in the dielectric area (3) during the synthesis, such as A tentative rationalization of microwave effects in organic synthesis according to the reaction medium, and mechanistic considerations http://www.sciencedirect.com/science?_ob=ArticleURL&_udi=B6THR-44C8TB9-
T&_user= 10&_rdoc= 1 &_fmt=&_orig=search&_sort=d&view=c&_acct=C000050221 &_v ersion=l&_urlVersion=0&_userid=10&md5=264635c5dfde945b22face4cbf2e04d3 gotten 11 April 2008.
Example 2
Synthesis of 2-amino-3-cyanopyridine derivatives without solvent using electric field in the dielectric area (3) during the synthesis, such as One-pot synthesis of 2- amino-3-cyanopyridine derivatives under microwave irradiation without solvent www.arkat-usa.org/get-file.php?fileid=l 8884 gotten 11 April 2008.
Example 3
Synthesis of peptides is using electric field in the dielectric area (3) during the synthesis, such as microwaves are used in Novel method for solid phase peptide synthesis using microwave energy www.cem.de/documents/produkte/peptid/ APSJCollinsPaper.pdf gotten 11 April 2008.
For those skilled in the arts are clear that the invention is not limited to the presented details, such for example as in the choice of the electrodes and of dielectric materials or a voltage or current magnitude, known synthesis methods combined to this invention and flow through methods for a continuous process.
For those skilled in the arts can make synthesis according to e.g. Chudoba T. et al. Method of chemical reactions conduction and chemical reactor WO2007040415 and thus the difference is that the both electrodes are insulated or none. So again problems with lack of free electrons and voltage breakdown arise. The crystallization method by Reijonen M. Method and apparatus using of the electric field for controlling of the crystallizing of material or materials WO2007017552 they do not apply it for synthesis. Crystallization is used for e.g. purification use by recrystallizations.
BRIEF DESCRIPTION OF THE FIGURES
FIG 1. The principle using of the electric field in the materials synthesis. Electrodes (1 and 4) have attached to the adjustable power supply (5). The insulating layer (2) is between the another electrode (1) on and insulating layer (2) and another electrode, in the dielectric layer (3) the synthesis of the materials takes place.

Claims

1. A method using polarization for the controlling of the synthesizing of materials consists of - two electrodes (1 and 4)
- an insulation layer (2)
- a dielectric layer (3) where the synthesis takes place
- a voltage supply (5) and a closed circuit
- a synthesis container.
2; The method according to the claim 1 starting materials intermediate and final products of the synthesis are as a dielectric solid, liquid and/or gas or combinations thereof in a dielectric layer (3).
3. The method according to the claim 2 starting materials, intermediate and final products of the synthesis can be mixed with a dielectric material or materials in a dielectric layer (3).
4. The method according to the claim 3 in a dielectric layer (3) there are starting materials, intermediate and final products of the synthesis as a dielectric material or materials, which can be as a liquid, melt or their mixture including inorganic, organic materials or combinations thereof. Other examples as the components of the mixture are water for example in gel or emulsion, alcohols, such as ethanol, propanol, ketones such as acetone, glycerol, pentane, hexane, carbon tetrachloride, chloroform, benzene, toluene, petrol, turpentine, sugars, proteins, fats, such as olive oil, rapeseed oil, cocoa butter, linseed oil or biopolymer or mixture of biopolymers.
5. The method according to the claim 1 a dielectric layer (2) is formed of typically polyethene, polycarbonate, polyvinyl chloride, polyester, polymethylmethacrylate, polystyrene, polyamide, polyisoprene, polyformaldehyde, polysulfone, polytetrafluorethene, phenolic plastic, aminoplast, quartz, ceramic material, rubber, bakelite, luster, porcelain, glue, varnish, paint, a product of petrochemistry, an oxide of metal or glass or combinations thereof.
6. The method according to the claim 1 a dielectric layer (2) is thin, typically in 10-100 micrometers thick, and the synthesis area can be regulated, typically in a 0.5-10 cm width.
7. The method according to the claim 1 the voltage (5) can be regulated by using typically high voltages and if needed a small current.
8. The method according to the claim 1 the voltage (5) can be regulated in a 0-10000 kV area, and if necessary, the direction of the voltage can be changed.
9. The method according to the claim 1 the system can be typically multiplied as a pile, roll, radius or cylinder like.
10. The apparatus as claimed in the claim 1, wherein the width of a dielectric layer (2) can be changed, the adjustable voltage supply functions in a 0- + 100000 kV area, a dielectric layer (3), where the synthesis takes place is 0.5-10 cm width. The apparatus contains of metal electrodes (1 and 4).
PCT/FI2009/000048 2008-04-15 2009-04-14 Method of using an electric field in the synthesis of materials WO2009127773A1 (en)

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FI20080284A FI20080284L (en) 2008-04-15 2008-04-15 A method of using an electric field in the synthesis of substances
FI20080284 2008-04-15

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4297186A (en) * 1976-03-16 1981-10-27 Killer Walter Hp Method and apparatus for reducing the activation energy of chemical reactions
US20030192780A1 (en) * 2002-04-15 2003-10-16 Timo Ala-Kleme Insulator electrode devices
WO2007017552A1 (en) * 2005-08-10 2007-02-15 Mika Tapio Reijonen Method and apparatus using of the electric field for controlling of the crystallizing of material or materials

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4297186A (en) * 1976-03-16 1981-10-27 Killer Walter Hp Method and apparatus for reducing the activation energy of chemical reactions
US20030192780A1 (en) * 2002-04-15 2003-10-16 Timo Ala-Kleme Insulator electrode devices
WO2007017552A1 (en) * 2005-08-10 2007-02-15 Mika Tapio Reijonen Method and apparatus using of the electric field for controlling of the crystallizing of material or materials

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FI20080284L (en) 2009-10-16

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