CA1264724A - Process for the production of a porous structure comprising an organic material dispersed in a binder - Google Patents
Process for the production of a porous structure comprising an organic material dispersed in a binderInfo
- Publication number
- CA1264724A CA1264724A CA000505264A CA505264A CA1264724A CA 1264724 A CA1264724 A CA 1264724A CA 000505264 A CA000505264 A CA 000505264A CA 505264 A CA505264 A CA 505264A CA 1264724 A CA1264724 A CA 1264724A
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- Prior art keywords
- organic material
- binder
- agglomerate
- powdered
- mixture
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12N—MICROORGANISMS OR ENZYMES; COMPOSITIONS THEREOF; PROPAGATING, PRESERVING, OR MAINTAINING MICROORGANISMS; MUTATION OR GENETIC ENGINEERING; CULTURE MEDIA
- C12N11/00—Carrier-bound or immobilised enzymes; Carrier-bound or immobilised microbial cells; Preparation thereof
- C12N11/02—Enzymes or microbial cells immobilised on or in an organic carrier
- C12N11/10—Enzymes or microbial cells immobilised on or in an organic carrier the carrier being a carbohydrate
- C12N11/12—Cellulose or derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12N—MICROORGANISMS OR ENZYMES; COMPOSITIONS THEREOF; PROPAGATING, PRESERVING, OR MAINTAINING MICROORGANISMS; MUTATION OR GENETIC ENGINEERING; CULTURE MEDIA
- C12N11/00—Carrier-bound or immobilised enzymes; Carrier-bound or immobilised microbial cells; Preparation thereof
- C12N11/02—Enzymes or microbial cells immobilised on or in an organic carrier
- C12N11/08—Enzymes or microbial cells immobilised on or in an organic carrier the carrier being a synthetic polymer
- C12N11/082—Enzymes or microbial cells immobilised on or in an organic carrier the carrier being a synthetic polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds
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- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Zoology (AREA)
- Engineering & Computer Science (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Organic Chemistry (AREA)
- Genetics & Genomics (AREA)
- Chemical & Material Sciences (AREA)
- Wood Science & Technology (AREA)
- Biotechnology (AREA)
- Microbiology (AREA)
- Biochemistry (AREA)
- General Engineering & Computer Science (AREA)
- General Health & Medical Sciences (AREA)
- Biomedical Technology (AREA)
- Molecular Biology (AREA)
- Immobilizing And Processing Of Enzymes And Microorganisms (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
- Medicines Containing Material From Animals Or Micro-Organisms (AREA)
- Medicinal Preparation (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
ABSTRACT OF THE DISCLOSURE
A process is disclosed for the production of a porous structure comprising an organic material dispersed in a binder. The process comprises mixing together a powdered organic material or a mixture of such materials or a powdered support loaded with such material and a powdered binder in a dry state, subjecting the obtained dry mixture to an agglomerating treatment, subjecting the formed agglomerate to a grinding treatment, and compressing the ground agglomerate so as to form a compact, all these operations being effected at a temperature below 340°K, preferably at room temperature.
A process is disclosed for the production of a porous structure comprising an organic material dispersed in a binder. The process comprises mixing together a powdered organic material or a mixture of such materials or a powdered support loaded with such material and a powdered binder in a dry state, subjecting the obtained dry mixture to an agglomerating treatment, subjecting the formed agglomerate to a grinding treatment, and compressing the ground agglomerate so as to form a compact, all these operations being effected at a temperature below 340°K, preferably at room temperature.
Description
i47~
The present invention relates to a process for the production of a porous structure comprising at least one organic material dispersed in a binder.
There are several existing types of porous structures comprising an organic material dispersed in a binder. Such structures have many application~s t Viz . in chemical and especially in biochemical processes and analyses, in biological tests, pharmacology and food industry.
The known processes for the production of those porous structures in general comprise a treatment at a temperature considerably exceeding room temperature and being potentially destructive for the organic material or the bond between the latter and its support in the structure.
It ensues therefrom that the fixation oE the organic material to the support is necessarily the terminal phase of the production; as a result of which the fixation is more difficult to realize and the desired distribution of the organic material throughout the structure is thereby impaired. Especially if the organic material has to be ~ixed to a powdered support, the fixation of the material to the support is controlled more easily if it is carried out on a powdered support that has not yet been incorporated into the binder. As the coupling of support and organic material is preferably realized in the form of covalent bonding, producing it with the already incorporated support should be avoided.
US Patent 3,766,013 describes processes for the productioll of a porous structure comprising a binding agent in which coup]ing of an organic material, in this case an enzyme, takes place on an organic support already i n c o r p o r a t e d i n t o t h e b i n d e r , b e i n g polytetrafluoroethylene in this case. It is stated that coupling can also be realized before fibrillation of the binder, i.e., with a support not yet incorporated into the binder, if the enzyme is resistant to high temperature, but in practice the enzymes and generally the biological i47;~4 material to be incorporated are destroyed at the temperatures required for the other phases of the production process.
An object of the invention is to provide a process that can be carried out under such conditions that the organic material, optionally already fixed to a support, can be incorporated into the binder without this organic material and/or its fixation to the support being destroyed.
10Accordingl~, one aspect of the invention provides a process for the production of a porous structure comprising an organic material dispersed in a binder, comprising the steps of:
(a) fixing the organic material to a powdered support, thus forming a powdered support loaded with the organic material, (b) mixing together the thus formed loaded powdered support with a powdered binder in a dry state so as to form a mixture, 20(c) subjecting the thus formed mixture to an agglomerating treatment so as to form an agglomerate, (d) subjecting the thus formed agglolnerate to a grindin~ treatment so as to form a ground agglomerate, and (e) compressing the ground agglomerate to form a compact, all these steps being effected at a temperature below 340K.
Another aspect of the invention provides a process for the production of a porous structure comprising an organic material dispersed in a binder, comprising the steps oE:
(a) mixing together the organic material in the form of a powder and a powdered binder in a dry state so as to form a mixture, (b) subjecting the mixture to an agglomerating treatment so as to form an agglomerate, (c) subjecting the thus formed agglomerate to a grinding treatment so as tG form a ground agglomerate,and ~ d) compressing the ground agglomerate so as to form a compact, all these operations being eEfected at a temperature below 340K.
Although the use of one organic material has been mentioned, the invention also contemplates the incorporation of several organic materials into a binder and especially the incorporation of a mixture of organic materials in well determined proportions.
~ he invention enables an organic material such as an enzyme, micro-organism or organelle, or a mixture of such organic materials in well defined proportions to be incorporated in finely divided form into a porous matrix of a binder without the organic material or mixture of organic materials having to undergo any wet treatment or any treatment at high temperature that might damage it.
~lthough the process according to the invention can be applied to incorporating an organic material as such or a mixture of organic materials in a finely divided form into a porous binder matrix, it is however especially applicable for such an incorporation of a support or substrate to which has been fixed an active organic substance such as an enzyme, micro~organism or organelle or to which has been fixed a mixture of such organic substances in well defined proportions. The process according to the invention is also applicable to incorporating a mixture of such supports.
Thus, the invention provides a process for incorporating at least one support to which at least one organic substance has been fixed in a porous binder matrix without this incorporation requiring any wet treatment or any treatment at high temperature that would impair the fixation of the organic material to the support or that might inhibit or destroy said material. For this purpose, according to a particular embodiment of the invention, the organic material is fixed to a support, whereupon the powdered support loaded with the organic material and the powdered binder in a dry state are mixed together so as to form a mixture.
1~i4~ 4 Preferably all those operations are carried out at room temperature.
According to an advantageous e~odiment of the invention the compact is submitted to a rolling operation so as to convert it to film.
It should be noted that a process comprising successive operations comparable to that of the invention is known for the production of an electrode layer for a fuel battery.
According to the process known fro~ European Published ~pplication ~3,632, a fine inorganic electroconductive powder is mixed with a binder. It has been established according to the present invention that surprisingly a comparable succession of operations also allows the incorporation of an organic material into a binder for producing a porous structure intended for biological and analogous applications, without alteration of the organic material.
In contrast, the process of European Published 20 Application 43,632 does not allow maintenance of the delicate fixation of an organic material to a support unaltered during the incorporation of the latter in a finely divided ~orm into a porous binder matrix.
The incorporation of an organic material, particularly cellulose/ into a binder, being polytetrafluoroethylene in this case, is known from French Patent 2,237,989. The incorporation, however, takes place by a wet process, as a matter of fact in view of a later extraction of the organic matter whose spoiling during said known process should thus not be avoided.
The structure to be produced by the process according to the present invention is generally a structure in the form of a film or a disc, thus extending itself essentially in two dimensions, but it can also be a three-dimensional structure. The porous structure is constituted by the dispersion of the organic material or of a powdered support loaded with said organic material in ~i47~4 a porous matrix consisting of a binder. The support may also be microporous. The organic m~terial is, e.~., a protein and more particularly an enzyme. Examples of organic materials are disclosed in US Patent 3,766,013.
Further examples of organic materials that can be used in the process according to the present invention are cellulose and freeze-dried yeasts. Still further examples, viz. amyloglucosidase are cited in "Immobilized Enzymes, J.C. Johnson, Noyes Data Corporation 1979".
The organic material, viz. the enzyme, may be coupled to a powdered support. ~xamples of such supports can be found in US Patent 3,766,013 and in the "Immobilized Enzymes" article cited above.
Coupling of the powdered support and the organic material is realized before the support is incorporated into the structure by the process according to the present invention. The peculiarities of the coupling reaction do not fall within the scope of the present patent application. The realization of couplings of this kind is described in the above cited publication "Immobilized Enzymes".
It should be noted that the coupling of the organic material to the support is preferably by covalent bonding and that the coupling reaction which is known as such is a difficult and complex one.
It is important according to the invention that this reaction is realized on the organic material and on the support prior to their incorporation into the structure. Dosage is then controlled more easily and more 3~ precisely. It is also important that the support provided with the organic material does not require submission thereafter to operations that could spoil the organic material or its fixation to the support, such as treat~ent in wet conditions or at high temperatures.
The binder should be suitable for the formation of a porous matrix. It may thus be selected from polyethylene, polypropylene, polyvinyl chloride, polyfluorocarbons and polytetraEluoroethylene.
7'~4 If it is desired to limit or to avoid the hydrophohic character of the binder, the powder constituting it may be hydrophilized before the other process operations. This hydrophilization may consist in a treatment by a known hydrophilizing liquid such as one of the liquids mentioned in ~S Patent 4,252,878.
The preferred process comprises the Eollowing successive operations.
In a first operation, the organic material or the support loaded wi-th the organic material and the powdered binder in dry state are mixed together so as to form a mixture. Said organic material or said support loaded with the organic material is preEerably already in powdered form.
However, the application of the process to materials or to loaded supports not in that form is not excluded. The material or tl~e loaded support needs then to be made powdery before or during the mixing operation.
The percentages of the constituents to be mixed depend on the nature of the binder and on the nature of the support and/or of the organic material, but the amount by weight of the binder with respect to the entire mixture normally remains below 30%. Mixing can occur in any type of powder mixer, e.g., a ball mill wherein the balls have a speed of some 0.1 to 1 m/s with respect to the vat.
In a second operation the dry mixture is submitted to an agglomeration treatment for forming agglomerates. This can be realized in a ball mill wherein the balls have a speed that markedly exceeds the speed applied for forming the mixture, e.g., a speed of about 4 to 6 m/s with respect to the vat.
This agglomeration treatment may last for several hours. After this operation the mill contains agglomerates in the form of a skin having a surface area of several sq. cm to several hundreds of sq. cm.
The agglomeration step can also be achieved by other means than a ball mill. It is sufficient to knead 47~4 the mixture, i.e~, to subject the mixture to violent successive acts oE deformation and shearing.
In a third operation the agglomerates are ground so as to Eorm ground agglomerates, e.g., in a mixer or in a mill such as a coffee mill.
In a fourth operation the ground agglomerates or their efficient fraction, e.g., the fraction passing a sieve of 0.5 mm of mesh size, are compressed in a press up to a thickness of several centimeters.
In a fifth operation, which is not always required, the compact is submitted to rolling until its thickness is reduced to a ratio of 1/10 to l/50.
The successive rolling steps may be effected on a compact with a rolling-direction which is turned through 90 with respect to the rolling-direction of the former step.
All these operations can take place at room temperature and in any case at a temperature below 340K.
The following Examples illustrate the invention.
~xample I
20 g of a very fine alumina powder are activated by washing first in ~M HCl, then in 0.02 M of acetate (buffer, pH = 4.2).
The powder i9 dispersed in a 0.02 M acetate solution (buffer, pH - 5) and exposed to a dye for 20 minutes. After having been washed in 0.02 M of acetate (pH 4.2) the powder is mixed with 100 ml of aqueous amyloglucosidase solution (90 units) or 8 hours (as described at page 17 of the above-cited publication "Immobilized Enzymes"). In this way a powder is obtained consisting of an alumina substrate covered with adsorbed amyloglucosidase.
E~ual amounts of this substrate with the enzyme adsorbed thereon and of polytetrafluoroethylene ~marketed under the trade mark TEFLON 10 N) are placed in a laboratory ball mill.
4 stainless-steel balls of 30 mm diameter are also placed in the ball mill.
7~4 The ball mill is opened after 2 hours of operation; its walls are covered with a "skin" formed by the polytetrafluoroethylene and the substrate on which the enzyme is adsorbed.
The skin is collected and ground in a kitchen mixer.
20 g are collected and placed in a press to form a compact oE 3.5 mm x 70 mm x 70 mm.
This compact is then cold-rolled so as to obtain a foil having a thickness oE 0.2 mm and a surface area of 510 x 135 mm .
~xample II
g of freeæe-dried yeast and 50 g of polytetrafluoroethylene powder are placed in a laboratory ball mill, whereupon the procedure of Example I is repeated so as to obtain a foil.
Starting from this foil, discs having a diameter of 5 mm are punched and these can be used for example, in the production of ethanol.
Example III
50 g of polytetrafluoroethylene powder (marketed under the trade mark TEFLON 10 N) and 50 g of cellulose powder are placed in a laboratory ball mill.
~ stainless-steel balls of 30 mm diameter are added thereto. The ball mill is opened after 2 hours of operation; its walls are covered by a "skin" formed by the cellulose and the polytetrafluoroethylene.
The skin is collected and ground in a kitchen mixer.
20 g are collected and placed in a press to form a compact of 3.5 mm x 70 mm x 70 mm in size.
Then this compact is cold-rolled so as to yield a foil 0.2 mm thick and 510 x 135 mm2 in surface area.
T h i s f o i l c o n t a i n s 9 . 5 m g o f polytetrafluoroethylene and cellulose per cm2.
After imbibition in water it is established that the foil has adsorbed 20% of its volume of water.
i47;~
Example IV
The procedure of Example III is repeated but the polytetrafluoroethylene powder is hydrophilised before it is introduced into the ball mill, S For that purpose the polytetraEluoroethylene powder is dipped in a 40~ by weight solution oE the product marketed under the trademark ZONYL FSN and is maintained therein for 5 days~
When a sample of the foil obtained is dipped in water it is established that after 3Q seconds said foil has adsorbed 50% of its volume of water.
The invention is not limited to the above-described embodiments and within the scope of the invention many modifications can be applied.
~or example, following the procedure of Example I, other enzymes adsorbed on the same or another substrate can be used and the final product is not necessarily formed into a foil. Starting from this foil, discs can be punched and other porous structures can be realized as well.
Further, in Example II the foil may be maintained as final product and other porous structures can be realized with the binder and said freeze-dried yeasts or other organic materials~
. . . , _, . .
The present invention relates to a process for the production of a porous structure comprising at least one organic material dispersed in a binder.
There are several existing types of porous structures comprising an organic material dispersed in a binder. Such structures have many application~s t Viz . in chemical and especially in biochemical processes and analyses, in biological tests, pharmacology and food industry.
The known processes for the production of those porous structures in general comprise a treatment at a temperature considerably exceeding room temperature and being potentially destructive for the organic material or the bond between the latter and its support in the structure.
It ensues therefrom that the fixation oE the organic material to the support is necessarily the terminal phase of the production; as a result of which the fixation is more difficult to realize and the desired distribution of the organic material throughout the structure is thereby impaired. Especially if the organic material has to be ~ixed to a powdered support, the fixation of the material to the support is controlled more easily if it is carried out on a powdered support that has not yet been incorporated into the binder. As the coupling of support and organic material is preferably realized in the form of covalent bonding, producing it with the already incorporated support should be avoided.
US Patent 3,766,013 describes processes for the productioll of a porous structure comprising a binding agent in which coup]ing of an organic material, in this case an enzyme, takes place on an organic support already i n c o r p o r a t e d i n t o t h e b i n d e r , b e i n g polytetrafluoroethylene in this case. It is stated that coupling can also be realized before fibrillation of the binder, i.e., with a support not yet incorporated into the binder, if the enzyme is resistant to high temperature, but in practice the enzymes and generally the biological i47;~4 material to be incorporated are destroyed at the temperatures required for the other phases of the production process.
An object of the invention is to provide a process that can be carried out under such conditions that the organic material, optionally already fixed to a support, can be incorporated into the binder without this organic material and/or its fixation to the support being destroyed.
10Accordingl~, one aspect of the invention provides a process for the production of a porous structure comprising an organic material dispersed in a binder, comprising the steps of:
(a) fixing the organic material to a powdered support, thus forming a powdered support loaded with the organic material, (b) mixing together the thus formed loaded powdered support with a powdered binder in a dry state so as to form a mixture, 20(c) subjecting the thus formed mixture to an agglomerating treatment so as to form an agglomerate, (d) subjecting the thus formed agglolnerate to a grindin~ treatment so as to form a ground agglomerate, and (e) compressing the ground agglomerate to form a compact, all these steps being effected at a temperature below 340K.
Another aspect of the invention provides a process for the production of a porous structure comprising an organic material dispersed in a binder, comprising the steps oE:
(a) mixing together the organic material in the form of a powder and a powdered binder in a dry state so as to form a mixture, (b) subjecting the mixture to an agglomerating treatment so as to form an agglomerate, (c) subjecting the thus formed agglomerate to a grinding treatment so as tG form a ground agglomerate,and ~ d) compressing the ground agglomerate so as to form a compact, all these operations being eEfected at a temperature below 340K.
Although the use of one organic material has been mentioned, the invention also contemplates the incorporation of several organic materials into a binder and especially the incorporation of a mixture of organic materials in well determined proportions.
~ he invention enables an organic material such as an enzyme, micro-organism or organelle, or a mixture of such organic materials in well defined proportions to be incorporated in finely divided form into a porous matrix of a binder without the organic material or mixture of organic materials having to undergo any wet treatment or any treatment at high temperature that might damage it.
~lthough the process according to the invention can be applied to incorporating an organic material as such or a mixture of organic materials in a finely divided form into a porous binder matrix, it is however especially applicable for such an incorporation of a support or substrate to which has been fixed an active organic substance such as an enzyme, micro~organism or organelle or to which has been fixed a mixture of such organic substances in well defined proportions. The process according to the invention is also applicable to incorporating a mixture of such supports.
Thus, the invention provides a process for incorporating at least one support to which at least one organic substance has been fixed in a porous binder matrix without this incorporation requiring any wet treatment or any treatment at high temperature that would impair the fixation of the organic material to the support or that might inhibit or destroy said material. For this purpose, according to a particular embodiment of the invention, the organic material is fixed to a support, whereupon the powdered support loaded with the organic material and the powdered binder in a dry state are mixed together so as to form a mixture.
1~i4~ 4 Preferably all those operations are carried out at room temperature.
According to an advantageous e~odiment of the invention the compact is submitted to a rolling operation so as to convert it to film.
It should be noted that a process comprising successive operations comparable to that of the invention is known for the production of an electrode layer for a fuel battery.
According to the process known fro~ European Published ~pplication ~3,632, a fine inorganic electroconductive powder is mixed with a binder. It has been established according to the present invention that surprisingly a comparable succession of operations also allows the incorporation of an organic material into a binder for producing a porous structure intended for biological and analogous applications, without alteration of the organic material.
In contrast, the process of European Published 20 Application 43,632 does not allow maintenance of the delicate fixation of an organic material to a support unaltered during the incorporation of the latter in a finely divided ~orm into a porous binder matrix.
The incorporation of an organic material, particularly cellulose/ into a binder, being polytetrafluoroethylene in this case, is known from French Patent 2,237,989. The incorporation, however, takes place by a wet process, as a matter of fact in view of a later extraction of the organic matter whose spoiling during said known process should thus not be avoided.
The structure to be produced by the process according to the present invention is generally a structure in the form of a film or a disc, thus extending itself essentially in two dimensions, but it can also be a three-dimensional structure. The porous structure is constituted by the dispersion of the organic material or of a powdered support loaded with said organic material in ~i47~4 a porous matrix consisting of a binder. The support may also be microporous. The organic m~terial is, e.~., a protein and more particularly an enzyme. Examples of organic materials are disclosed in US Patent 3,766,013.
Further examples of organic materials that can be used in the process according to the present invention are cellulose and freeze-dried yeasts. Still further examples, viz. amyloglucosidase are cited in "Immobilized Enzymes, J.C. Johnson, Noyes Data Corporation 1979".
The organic material, viz. the enzyme, may be coupled to a powdered support. ~xamples of such supports can be found in US Patent 3,766,013 and in the "Immobilized Enzymes" article cited above.
Coupling of the powdered support and the organic material is realized before the support is incorporated into the structure by the process according to the present invention. The peculiarities of the coupling reaction do not fall within the scope of the present patent application. The realization of couplings of this kind is described in the above cited publication "Immobilized Enzymes".
It should be noted that the coupling of the organic material to the support is preferably by covalent bonding and that the coupling reaction which is known as such is a difficult and complex one.
It is important according to the invention that this reaction is realized on the organic material and on the support prior to their incorporation into the structure. Dosage is then controlled more easily and more 3~ precisely. It is also important that the support provided with the organic material does not require submission thereafter to operations that could spoil the organic material or its fixation to the support, such as treat~ent in wet conditions or at high temperatures.
The binder should be suitable for the formation of a porous matrix. It may thus be selected from polyethylene, polypropylene, polyvinyl chloride, polyfluorocarbons and polytetraEluoroethylene.
7'~4 If it is desired to limit or to avoid the hydrophohic character of the binder, the powder constituting it may be hydrophilized before the other process operations. This hydrophilization may consist in a treatment by a known hydrophilizing liquid such as one of the liquids mentioned in ~S Patent 4,252,878.
The preferred process comprises the Eollowing successive operations.
In a first operation, the organic material or the support loaded wi-th the organic material and the powdered binder in dry state are mixed together so as to form a mixture. Said organic material or said support loaded with the organic material is preEerably already in powdered form.
However, the application of the process to materials or to loaded supports not in that form is not excluded. The material or tl~e loaded support needs then to be made powdery before or during the mixing operation.
The percentages of the constituents to be mixed depend on the nature of the binder and on the nature of the support and/or of the organic material, but the amount by weight of the binder with respect to the entire mixture normally remains below 30%. Mixing can occur in any type of powder mixer, e.g., a ball mill wherein the balls have a speed of some 0.1 to 1 m/s with respect to the vat.
In a second operation the dry mixture is submitted to an agglomeration treatment for forming agglomerates. This can be realized in a ball mill wherein the balls have a speed that markedly exceeds the speed applied for forming the mixture, e.g., a speed of about 4 to 6 m/s with respect to the vat.
This agglomeration treatment may last for several hours. After this operation the mill contains agglomerates in the form of a skin having a surface area of several sq. cm to several hundreds of sq. cm.
The agglomeration step can also be achieved by other means than a ball mill. It is sufficient to knead 47~4 the mixture, i.e~, to subject the mixture to violent successive acts oE deformation and shearing.
In a third operation the agglomerates are ground so as to Eorm ground agglomerates, e.g., in a mixer or in a mill such as a coffee mill.
In a fourth operation the ground agglomerates or their efficient fraction, e.g., the fraction passing a sieve of 0.5 mm of mesh size, are compressed in a press up to a thickness of several centimeters.
In a fifth operation, which is not always required, the compact is submitted to rolling until its thickness is reduced to a ratio of 1/10 to l/50.
The successive rolling steps may be effected on a compact with a rolling-direction which is turned through 90 with respect to the rolling-direction of the former step.
All these operations can take place at room temperature and in any case at a temperature below 340K.
The following Examples illustrate the invention.
~xample I
20 g of a very fine alumina powder are activated by washing first in ~M HCl, then in 0.02 M of acetate (buffer, pH = 4.2).
The powder i9 dispersed in a 0.02 M acetate solution (buffer, pH - 5) and exposed to a dye for 20 minutes. After having been washed in 0.02 M of acetate (pH 4.2) the powder is mixed with 100 ml of aqueous amyloglucosidase solution (90 units) or 8 hours (as described at page 17 of the above-cited publication "Immobilized Enzymes"). In this way a powder is obtained consisting of an alumina substrate covered with adsorbed amyloglucosidase.
E~ual amounts of this substrate with the enzyme adsorbed thereon and of polytetrafluoroethylene ~marketed under the trade mark TEFLON 10 N) are placed in a laboratory ball mill.
4 stainless-steel balls of 30 mm diameter are also placed in the ball mill.
7~4 The ball mill is opened after 2 hours of operation; its walls are covered with a "skin" formed by the polytetrafluoroethylene and the substrate on which the enzyme is adsorbed.
The skin is collected and ground in a kitchen mixer.
20 g are collected and placed in a press to form a compact oE 3.5 mm x 70 mm x 70 mm.
This compact is then cold-rolled so as to obtain a foil having a thickness oE 0.2 mm and a surface area of 510 x 135 mm .
~xample II
g of freeæe-dried yeast and 50 g of polytetrafluoroethylene powder are placed in a laboratory ball mill, whereupon the procedure of Example I is repeated so as to obtain a foil.
Starting from this foil, discs having a diameter of 5 mm are punched and these can be used for example, in the production of ethanol.
Example III
50 g of polytetrafluoroethylene powder (marketed under the trade mark TEFLON 10 N) and 50 g of cellulose powder are placed in a laboratory ball mill.
~ stainless-steel balls of 30 mm diameter are added thereto. The ball mill is opened after 2 hours of operation; its walls are covered by a "skin" formed by the cellulose and the polytetrafluoroethylene.
The skin is collected and ground in a kitchen mixer.
20 g are collected and placed in a press to form a compact of 3.5 mm x 70 mm x 70 mm in size.
Then this compact is cold-rolled so as to yield a foil 0.2 mm thick and 510 x 135 mm2 in surface area.
T h i s f o i l c o n t a i n s 9 . 5 m g o f polytetrafluoroethylene and cellulose per cm2.
After imbibition in water it is established that the foil has adsorbed 20% of its volume of water.
i47;~
Example IV
The procedure of Example III is repeated but the polytetrafluoroethylene powder is hydrophilised before it is introduced into the ball mill, S For that purpose the polytetraEluoroethylene powder is dipped in a 40~ by weight solution oE the product marketed under the trademark ZONYL FSN and is maintained therein for 5 days~
When a sample of the foil obtained is dipped in water it is established that after 3Q seconds said foil has adsorbed 50% of its volume of water.
The invention is not limited to the above-described embodiments and within the scope of the invention many modifications can be applied.
~or example, following the procedure of Example I, other enzymes adsorbed on the same or another substrate can be used and the final product is not necessarily formed into a foil. Starting from this foil, discs can be punched and other porous structures can be realized as well.
Further, in Example II the foil may be maintained as final product and other porous structures can be realized with the binder and said freeze-dried yeasts or other organic materials~
. . . , _, . .
Claims (9)
PROPERTY OR PRIVILEGE IS CLAIMED ARE DEFINED AS FOLLOWS:
1. A process for the production of a porous structure comprising an organic material dispersed in a binder, comprising the steps of:
(a) fixing the organic material to a powdered support, thus forming a powdered support loaded with said organic material, (b) mixing together the thus formed loaded powdered support with a powdered binder in a dry state so as to form a mixture, (c) subjecting the thus formed mixture to an agglomerating treatment so as to form an agglomerate, (d) subjecting the thus formed agglomerate to a grinding treatment so as to form a ground agglomerate, and (e) compressing the ground agglomerate to form a compact, all these steps being effected at a temperature below 340°K.
(a) fixing the organic material to a powdered support, thus forming a powdered support loaded with said organic material, (b) mixing together the thus formed loaded powdered support with a powdered binder in a dry state so as to form a mixture, (c) subjecting the thus formed mixture to an agglomerating treatment so as to form an agglomerate, (d) subjecting the thus formed agglomerate to a grinding treatment so as to form a ground agglomerate, and (e) compressing the ground agglomerate to form a compact, all these steps being effected at a temperature below 340°K.
2. A process according to claim 1, in which all of steps (a) to (e) are effected at room temperature.
3. A process according to claim 1 and comprising a final step of subjecting the compact to a rolling treatment until a film is obtained.
4. A process according to claim 1, 2 or 3, in which the binder is polyethylene, polypropylene, polyvinyl chloride, a polyfluorocarbon or polytetrafluoroethylene.
5. A process according to claim 1, 2 or 3, and including the preliminary step of hydrophilizing the powdered binder.
6. A process according to claim 1, 2 or 3, in which the organic material is fixed to a powdered support by covalent bonding
7. A process according to claim 1, 2 or 3, in which the organic material is a biologically active material.
8. A process according to claim 1, 2 or 3, in which the organic material is an enzyme.
9. A process for the production of a porous structure comprising an organic material dispersed in a binder, comprising the steps of:
(a) mixing together the organic material in the form of a powder and a powdered binder in a dry state so as to form a mixture, (b) subjecting said mixture to an agglomerating treatment so as to form an agglomerate, (c) subjecting the thus formed agglomerate to a grinding treatment so as to form a ground agglomerate, and (d) compressing the ground agglomerate so as to form a compact, all these operations being effected at a temperature below 340°K.
(a) mixing together the organic material in the form of a powder and a powdered binder in a dry state so as to form a mixture, (b) subjecting said mixture to an agglomerating treatment so as to form an agglomerate, (c) subjecting the thus formed agglomerate to a grinding treatment so as to form a ground agglomerate, and (d) compressing the ground agglomerate so as to form a compact, all these operations being effected at a temperature below 340°K.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| LU85822A LU85822A1 (en) | 1985-03-27 | 1985-03-27 | PROCESS FOR PRODUCING A POROUS STRUCTURE COMPRISING ORGANIC MATERIAL DISPERSED IN A BINDER |
| LU85.822 | 1985-03-27 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA1264724A true CA1264724A (en) | 1990-01-23 |
Family
ID=19730427
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA000505264A Expired - Lifetime CA1264724A (en) | 1985-03-27 | 1986-03-27 | Process for the production of a porous structure comprising an organic material dispersed in a binder |
Country Status (6)
| Country | Link |
|---|---|
| EP (1) | EP0200245B1 (en) |
| JP (1) | JPS61227024A (en) |
| AT (1) | ATE56752T1 (en) |
| CA (1) | CA1264724A (en) |
| DE (1) | DE3674238D1 (en) |
| LU (1) | LU85822A1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2770565A1 (en) | 2013-02-26 | 2014-08-27 | Vito NV | Method of manufacturing gas diffusion electrodes |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3766013A (en) * | 1971-08-24 | 1973-10-16 | American Cyanamid Co | Preparation of water-insoluble carrier bound enzymes |
| US3843443A (en) * | 1973-03-30 | 1974-10-22 | J Fishman | Polypeptide materials bound to fluorocarbon polymers |
| GB1468356A (en) * | 1973-07-18 | 1977-03-23 | Ici Ltd | Porous diaphragms |
| NL8003949A (en) * | 1980-07-09 | 1982-02-01 | Electrochem Energieconversie | METHOD FOR MANUFACTURING A COAT OF AN ELECTRODE FOR A CELL, IN PARTICULAR FOR A FUEL CELL. |
-
1985
- 1985-03-27 LU LU85822A patent/LU85822A1/en unknown
-
1986
- 1986-03-26 EP EP86200517A patent/EP0200245B1/en not_active Expired - Lifetime
- 1986-03-26 AT AT86200517T patent/ATE56752T1/en not_active IP Right Cessation
- 1986-03-26 JP JP61068253A patent/JPS61227024A/en active Pending
- 1986-03-26 DE DE8686200517T patent/DE3674238D1/en not_active Expired - Lifetime
- 1986-03-27 CA CA000505264A patent/CA1264724A/en not_active Expired - Lifetime
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2770565A1 (en) | 2013-02-26 | 2014-08-27 | Vito NV | Method of manufacturing gas diffusion electrodes |
Also Published As
| Publication number | Publication date |
|---|---|
| LU85822A1 (en) | 1986-10-06 |
| ATE56752T1 (en) | 1990-10-15 |
| JPS61227024A (en) | 1986-10-09 |
| EP0200245B1 (en) | 1990-09-19 |
| EP0200245A1 (en) | 1986-11-05 |
| DE3674238D1 (en) | 1990-10-25 |
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| Date | Code | Title | Description |
|---|---|---|---|
| MKLA | Lapsed |