DE818862C - Process for the production of membranes from cellulose ester - Google Patents
Process for the production of membranes from cellulose esterInfo
- Publication number
- DE818862C DE818862C DEK1063A DEK0001063A DE818862C DE 818862 C DE818862 C DE 818862C DE K1063 A DEK1063 A DE K1063A DE K0001063 A DEK0001063 A DE K0001063A DE 818862 C DE818862 C DE 818862C
- Authority
- DE
- Germany
- Prior art keywords
- cellulose ester
- membranes
- cellulose
- solutions
- production
- 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.)
- Expired
Links
- 229920002678 cellulose Polymers 0.000 title claims description 12
- 238000000034 method Methods 0.000 title claims description 6
- 239000012528 membrane Substances 0.000 title claims description 5
- 238000004519 manufacturing process Methods 0.000 title claims description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Natural products CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 239000011148 porous material Substances 0.000 claims description 7
- 238000001704 evaporation Methods 0.000 claims description 5
- 230000008020 evaporation Effects 0.000 claims description 5
- 238000005266 casting Methods 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 238000007792 addition Methods 0.000 claims description 3
- 150000001298 alcohols Chemical class 0.000 claims description 3
- 230000015271 coagulation Effects 0.000 claims description 3
- 238000005345 coagulation Methods 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims 1
- 238000003892 spreading Methods 0.000 claims 1
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 11
- 235000019441 ethanol Nutrition 0.000 description 7
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 239000001913 cellulose Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 235000011187 glycerol Nutrition 0.000 description 3
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 description 2
- 239000000020 Nitrocellulose Substances 0.000 description 2
- FJWGYAHXMCUOOM-QHOUIDNNSA-N [(2s,3r,4s,5r,6r)-2-[(2r,3r,4s,5r,6s)-4,5-dinitrooxy-2-(nitrooxymethyl)-6-[(2r,3r,4s,5r,6s)-4,5,6-trinitrooxy-2-(nitrooxymethyl)oxan-3-yl]oxyoxan-3-yl]oxy-3,5-dinitrooxy-6-(nitrooxymethyl)oxan-4-yl] nitrate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O)O[C@H]1[C@@H]([C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@@H](CO[N+]([O-])=O)O1)O[N+]([O-])=O)CO[N+](=O)[O-])[C@@H]1[C@@H](CO[N+]([O-])=O)O[C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O FJWGYAHXMCUOOM-QHOUIDNNSA-N 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229920001220 nitrocellulos Polymers 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical class CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 1
- 230000001427 coherent effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 235000019439 ethyl acetate Nutrition 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000002602 strong irritant Substances 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/08—Polysaccharides
- B01D71/12—Cellulose derivatives
- B01D71/14—Esters of organic acids
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
- B01D67/0011—Casting solutions therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
- B01D67/0013—Casting processes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2201/00—Foams characterised by the foaming process
- C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
- C08J2201/05—Elimination by evaporation or heat degradation of a liquid phase
- C08J2201/0502—Elimination by evaporation or heat degradation of a liquid phase the liquid phase being organic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/08—Cellulose derivatives
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Dispersion Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Health & Medical Sciences (AREA)
- Materials Engineering (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
Description
Verfahren zur Herstellung von Membranen aus Celluloseester Es ist bekat1nt, daß aus Celluloseestern Filme, auch solche mit verschiedener Porosität durch Aus-I>reiten geeigneter Lösungen und Verdampfung der Lösungsmittel, erzeugt werden. In Lösungen, die als heteropolar wirkenden Zusatz lediglich Methylalkohol enthalten, entstehen auf diese Weise Filme mit geringer l)urchlässigkeit. Versucht man, die l)orengröße und Zahl durch größere Methylalkoholzusätze zu steigern, so erhält man keine zusammenhängenden Filme mehr. Zusammenhängende Filme mit Poren in Größenordnungen von O,I bis jmal 11iooo mm konnten I,isher nur dann erhalten werden, wenn in Kammern mit geeigneter Luftfeuchtigkeit Ceiluloseesterlösungen auf glatten Unterlagen ausgegossen wurden, die als Zusatz Essigsäure oder Amylalkohol enthielten. Weil diese Lösungsmittel stark reizend oder giftig wirken und zudem bei ihrer geringen Verdunstungsgeschwindigkeit eine lange Zeit der Filterfilmentwicklung von 12 bis 24 Stunden erforderlich machen, wurde nach Herstellungsweisen ohne die genannten Zusätze gesucht.Process for the production of membranes from cellulose ester It is known that films made of cellulose esters, even those with different porosities, can be ridden by Aus-I> suitable solutions and evaporation of the solvents. In solutions, which only contain methyl alcohol as a heteropolar additive are formed in this way films with low permeability. If you try the l) oren size and increasing the number by adding larger amounts of methyl alcohol does not result in a coherent one Films more. Contiguous films with pores ranging in size from 0.1 to 1 times 11,000 mm could only be obtained if in chambers with suitable Humidity Ceilulose ester solutions were poured out on smooth surfaces, which contained acetic acid or amyl alcohol as an additive. Because these solvents have a strong irritant or toxic effect and also with their low evaporation rate require a long filter film development time of 12 to 24 hours, a search was made for manufacturing methods without the additives mentioned.
Es wurde nun gefunden, daß bei Ersatz des Amylalkohols durch itthyl-, Isopropylalkohol oder Gemischen davon bei Anwendung von Celluloseestern, die in niederen Alkoholen nicht löslich sind, in Aceton oder Mischungen von Aceton mit Methyl-oder Äthylacetaten, geeignete Gießlösungen zubereitet werden können. Die Porengrößen der daraus herstellbaren Filter sind dabei in weitesten Grenzen variierbar. Denn durch die Menge des zugesetzten einwertigen Alkohols wird bei gleicher Luftfeuchtigkeit die Porosität der entstehenden Filtermembran weitgehendst beeinflußt, derart, daß bei Zugabe von Alkoholmengen bis dicht an die Grenze der Koagulation oder gar 'bis in dieses Gehielt hinein zu den Celluloselösungen ein rasch flltrierender, grobporiger Film und bei Zugabe geringerer Alkoholmengen feinporigere Filme mit geringerer Filtrationsgeschwindigkeit entstehen. Für eine günstige Geschmeidigkeit des Trockenfilters ist der Zusatz geringer Mengen eines mehrwertigen Alkohols, wie z. B. Glycerin, der praktisch nicht verdampft, zweckmäßig. It has now been found that when the amyl alcohol is replaced by itthyl, Isopropyl alcohol or mixtures thereof when using cellulose esters in lower alcohols are not soluble in acetone or mixtures of acetone with Methyl or ethyl acetates, suitable pouring solutions can be prepared. the The pore sizes of the filters that can be produced from them can be varied within the broadest limits. Because due to the amount of monohydric alcohol added, the humidity is the same the porosity of the resulting filter membrane largely influenced, such that with the addition of amounts of alcohol up to close to the limit of coagulation or even 'up to in this content into the cellulose solutions a quick more shimmering, coarse-pored film and, if smaller amounts of alcohol are added, finer-pored films with lower filtration speed. For a favorable suppleness of the dry filter is the addition of small amounts of a polyhydric alcohol, such as z. B. glycerine, which practically does not evaporate, appropriate.
Die genannten leichtflüchtigen Alkohole bringen es mit sich, daß bei relativ dünnflüssigen Celluloselösungen durch die raschen Verdunstungsgeschwindigkeiten starke Strömungen die Ausbildung gleichmäßiger Filme erschweren oder verhindern. The volatile alcohols mentioned mean that with relatively thin cellulose solutions due to the rapid evaporation rates strong currents hinder or prevent the formation of uniform films.
Darum zeigt es sich als vorteilhaft, die Verdunstungsgeschwindigkeit bis zum Gelierungsvorgang an allen Punkten in praktisch gleich starker Art zu verzögern. Dies wird dadurch möglich gemacht, daß eine für Gase und Dämpfe langsam durchlässige Wand, wie sie z. B. dichte Stoffgewebe oder Cellutosepreßmassen darstellen, in möglichst geringem Abstand über der mit der Lösung bedeckten Gießfläche angebracht wird. Diese Wand hat somit die Funktion einer Austauschwand für die Gase zu den Raumen über der ausgegossenen Lösung und denen des Dampfabzuges.That is why it is advantageous to reduce the rate of evaporation to delay in practically the same amount at all points until the gelation process. This is made possible by the fact that one slowly permeable to gases and vapors Wall as it is z. B. represent dense fabric or cellulose pressed masses, in as much as possible a small distance above the casting surface covered with the solution. These Wall thus has the function of an exchange wall for the gases to the rooms above the poured solution and those of the steam vent.
Als Beispiel für die Bereitung einer Gießlösung sei genannt: Zu 100 Volumen einer Cellulosenitratacetonlösung mit loo Cellulose wird eine Lösung aus 10 Volumen Glycerin, 35 Volumen Athylalkohol und 10 Volumen Aceton unter starkem Einrühren eingemischt. Diese Lösung wird nach 24 Stunden auf genau horizontal liegenden Glasplatten ausgegossen. Die Entwicklung der Filme erfolgt bei Zimmertemperatur in der angegebenen Weise. An example for the preparation of a casting solution is: To 100 Volume of a cellulose nitrate acetone solution with 100 cellulose becomes a solution 10 volumes of glycerin, 35 volumes of ethyl alcohol and 10 volumes of acetone under strong Stir in mixed in. This solution will be lying exactly horizontally after 24 hours Poured out glass plates. The films are developed at room temperature in the manner indicated.
Bei Isopropylalkohol zeigt sich für die nicht allzuleicht löslichen Cellulosenitratlösungen, daß II bis 12 Volumen Isopropylalkohol mit o,6 bis I Volumen Glycerin zu 20 Volumen 7- bis Ioo/oiger Celluloseesteracetonlösung ein sehr durchlässiges Filter mit groben Poren ergibt, während bei dem teilweisen Ersatz von I bis 6 Volumen Isopropylalkohol durch Aceton Filter geringerer Durchlässigkeit entstehen, und zwar je geringer und mit kleineren Porendurchmessern, je weniger Alkohol zur Gießlösung gegeben war. In the case of isopropyl alcohol, it shows for the not too easily soluble Cellulose nitrate solutions that II to 12 volumes of isopropyl alcohol with o, 6 to I volume Glycerin to 20 volumes of 7 to 100% cellulose ester acetone solution is a very permeable Filters with coarse pores yields, while with the partial replacement from 1 to 6 volumes Isopropyl alcohol is produced by acetone filters with lower permeability, namely the smaller and with smaller pore diameters, the less alcohol is added to the casting solution was given.
Claims (3)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DEK1063A DE818862C (en) | 1949-12-20 | 1949-12-20 | Process for the production of membranes from cellulose ester |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DEK1063A DE818862C (en) | 1949-12-20 | 1949-12-20 | Process for the production of membranes from cellulose ester |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE818862C true DE818862C (en) | 1951-10-29 |
Family
ID=7208734
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DEK1063A Expired DE818862C (en) | 1949-12-20 | 1949-12-20 | Process for the production of membranes from cellulose ester |
Country Status (1)
| Country | Link |
|---|---|
| DE (1) | DE818862C (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE395705C (en) * | 1923-01-10 | 1924-05-23 | Goerz Photochemische Werke G M | Non-electrical photographic film |
| DE609986C (en) * | 1931-02-07 | 1935-03-04 | Chem Fab Von Heyden Akt Ges | Mouthpiece covering made from cellulose esters or ethers |
| DE713161C (en) * | 1938-04-14 | 1941-11-01 | Hydrierwerke Akt Ges Deutsche | Dissolving, gelatinizing, swelling and softening agents |
| DE724836C (en) * | 1937-05-18 | 1942-09-08 | Kodak Ag | Process for the production of foils |
-
1949
- 1949-12-20 DE DEK1063A patent/DE818862C/en not_active Expired
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE395705C (en) * | 1923-01-10 | 1924-05-23 | Goerz Photochemische Werke G M | Non-electrical photographic film |
| DE609986C (en) * | 1931-02-07 | 1935-03-04 | Chem Fab Von Heyden Akt Ges | Mouthpiece covering made from cellulose esters or ethers |
| DE724836C (en) * | 1937-05-18 | 1942-09-08 | Kodak Ag | Process for the production of foils |
| DE713161C (en) * | 1938-04-14 | 1941-11-01 | Hydrierwerke Akt Ges Deutsche | Dissolving, gelatinizing, swelling and softening agents |
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