DE1026303B - Process for cleaning perchlorethylene - Google Patents
Process for cleaning perchlorethyleneInfo
- Publication number
- DE1026303B DE1026303B DEC11271A DEC0011271A DE1026303B DE 1026303 B DE1026303 B DE 1026303B DE C11271 A DEC11271 A DE C11271A DE C0011271 A DEC0011271 A DE C0011271A DE 1026303 B DE1026303 B DE 1026303B
- Authority
- DE
- Germany
- Prior art keywords
- perchlorethylene
- ammonia
- cleaning
- anhydrous
- alkali
- 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.)
- Pending
Links
- CYTYCFOTNPOANT-UHFFFAOYSA-N Perchloroethylene Chemical group ClC(Cl)=C(Cl)Cl CYTYCFOTNPOANT-UHFFFAOYSA-N 0.000 title claims description 18
- 229950011008 tetrachloroethylene Drugs 0.000 title claims description 18
- 238000000034 method Methods 0.000 title claims description 5
- 238000004140 cleaning Methods 0.000 title claims 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 18
- 229910021529 ammonia Inorganic materials 0.000 claims description 9
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims description 6
- 239000003513 alkali Substances 0.000 claims description 4
- 150000001342 alkaline earth metals Chemical class 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 150000004649 carbonic acid derivatives Chemical class 0.000 claims description 3
- 239000000706 filtrate Substances 0.000 claims description 2
- YNAVUWVOSKDBBP-UHFFFAOYSA-N Morpholine Chemical compound C1COCCN1 YNAVUWVOSKDBBP-UHFFFAOYSA-N 0.000 description 8
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 7
- 238000009835 boiling Methods 0.000 description 6
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 2
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 2
- HFACYLZERDEVSX-UHFFFAOYSA-N benzidine Chemical compound C1=CC(N)=CC=C1C1=CC=C(N)C=C1 HFACYLZERDEVSX-UHFFFAOYSA-N 0.000 description 2
- PAFZNILMFXTMIY-UHFFFAOYSA-N cyclohexylamine Chemical compound NC1CCCCC1 PAFZNILMFXTMIY-UHFFFAOYSA-N 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- YGYAWVDWMABLBF-UHFFFAOYSA-N Phosgene Chemical compound ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 150000007530 organic bases Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- YNJBWRMUSHSURL-UHFFFAOYSA-N trichloroacetic acid Chemical compound OC(=O)C(Cl)(Cl)Cl YNJBWRMUSHSURL-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
Verfahren zum Reinigen von Perchloräthylen Es wird allgemein angenommen, daß die im technischen Perchloräthylen vorhandenen Verunreinigungen für die Instabilität gegenüber der Hydrolyse, Photolyse und Oxydation verantwortlich gemacht werden müssen. Als Zersetzungsprodukte treten unter anderem Phosgen, Salzsäure und Trichloressigsäure auf, die der Anlaß dazu sind, daß technischies Perchioräthylen Nietalle stark korrodiert.Process for purifying perchlorethylene It is generally believed that the impurities present in technical perchlorethylene are responsible for the instability must be held responsible for hydrolysis, photolysis and oxidation. The decomposition products used include phosgene, hydrochloric acid and trichloroacetic acid which are the reason why technically perchiorethylene rivets strongly corrode.
Es wurde gefunden, daß man Perchloräthylen sehr wirkungsvoll reinigen kann, wenn man es mit wasserfreien Carbonaten oder Oxyden von Alkali- oder Erdalkalimetallen, insbesondere mit Natriumcarbonat oder Natriumbicarbonat, unter gleichzeitigem Einleiten von Ammoniak erhitzt von den anorganischen Bestandteilen, zweckmäßig nach dem Erkalten, filtriert und gegebenenfalls das Filtrat destilliert. It has been found that perchlorethylene can be cleaned very effectively can, if you do it with anhydrous carbonates or oxides of alkali or alkaline earth metals, especially with sodium carbonate or sodium bicarbonate, with simultaneous introduction heated by ammonia by the inorganic components, expediently after cooling, filtered and, if necessary, the filtrate is distilled.
Das Verfahren wird etwa in der Weise ausgeführt, daß das mit bis zu etwa 1 bis 2 Gewichtsprozent Carbonat bzw. Oxyd versetzte Perchloräthylen unter Einleiten eines Ammoniakstromes unter Rückflußküblung längere Zeit zum Sieden erhitzt wird. Nach dem Erkalten und dem Abtrennen des verwendeten Carbonates oder Oxydes durch Filtrieren und gegebenenfalls anschließende Destillation erhält man ein Perchloräthylen, das nach Zugabe von 0,01 bis 1 Gewichtsprozent einer organischen Base, z. B. Cyclohexylamin, Morpholin, und 0,001 bis 0,1 Gewichtsprozent eines Phenols als Stabilisatoren praktisch stabil ist und nicht mehr korrodierend wirkt. The method is carried out in such a way that the with to Perchlorethylene added to about 1 to 2 percent by weight of carbonate or oxide Introducing a stream of ammonia heated to boiling for a long time under reflux will. After cooling and the separation of the carbonate or oxide used filtering and, if necessary, subsequent distillation gives a perchlorethylene, after the addition of 0.01 to 1 percent by weight of an organic base, e.g. B. Cyclohexylamine, Morpholine, and 0.001 to 0.1 percent by weight of a phenol are practical as stabilizers is stable and no longer has a corrosive effect.
Zwar ist es bereits bekannt, daß man technisches Perchloräthylen durch Behandeln mit Alkali- und Erdalkalibydroxyden in Gegenwart von Wasser. welches nachher auf recht kostspielige Weise wieder entfernt werden muß, reinigen kann. Demgegenüber gelingt es. mit dem Verfahren die mit der Wasserentfernung verbundenen Arbeitsgänge einzusparen indem man das zu reinigende Perchloräthylen in Abwesenheit von Wasser und unter gleichzeitigem Einleiten von Ammoniak mit trockenen Oxyden oder Carbonaten von Alkali- oder Erdalkalimetallen behandelt. It is already known that technical grade perchlorethylene is used by treating with alkali and alkaline earth hydroxides in the presence of water. which must then be removed again in a very expensive way, can clean. In contrast, it succeeds. with the procedure those associated with water removal Saving work steps by using the perchlorethylene to be cleaned in the absence of water and with simultaneous introduction of ammonia with dry oxides or carbonates of alkali or alkaline earth metals.
Auch ist es bekannt, Perchloräthylen bei Temperaturen zwischen 200 und 8000 C über für die Chlorwasserstoffabspaltung bekannte Katalysatoren, wie z. B. die Oxyde des Aluminiums, Siliciums und Magnesiums, zu leiten. Die damit verbundenen Maßnahmen erfordern aber einen erheblichen technischen Aufwand, der sich nach dem vorliegenden Verfahren erübrigt. It is also known to use perchlorethylene at temperatures between 200 and 8000 C over known catalysts for the elimination of hydrogen chloride, such as. B. to conduct the oxides of aluminum, silicon and magnesium. The associated However, measures require a considerable technical effort, which depends on the No need for existing proceedings.
Beispiel 1 2,5 1 technisches Perchloräthylen und O g wasserfreie Soda werden unter Einleiten eines kräftigen Ammoniakstromes und unter Rückflußkühlung erhitzt. Example 1 2.5 1 technical grade perchlorethylene and 0 g anhydrous Soda become with the introduction of a vigorous stream of ammonia and under reflux cooling heated.
Kurz vor Erreichung des Kochpunktes wird die Zu- fuhr von Ammoniak stark reduziert, so daß etwa 10 Gasbiasen/Min. durch das Perchloräthylen perlen.Shortly before the boiling point is reached, the drove from ammonia greatly reduced, so that about 10 gas biases / min. pearl through the perchlorethylene.
Nach 2stündigem Kochen wird die Ammoniakzufuhr abgestellt, nach weiterem halbstündigem Kochen wird das Perchloräthylen abgekühlt und filtriert. Es ist gelb gefärbt und kann zur Entfärbung mit Entfärbungskohle oder ähnlich wirkenden Stoffen behandelt werden. Der Kochtest ergibt einen pH-Wert zwischen 4 und 8. Es gibt mit Benzidin innerhalb von 24 Stunden keine Gelbfärbung. Nach Zumischen von 0,03 O/o Morpholin und 0,006 O/o Phenol erhält man ein stabiles Perchloräthylen.After 2 hours of boiling, the ammonia supply is turned off, after another After half an hour of boiling, the perchlorethylene is cooled and filtered. It's yellow colored and can be decolorized with decolorizing charcoal or similar substances be treated. The boiling test results in a pH value between 4 and 8. There is also Benzidine did not turn yellow within 24 hours. After adding 0.03% Morpholine and 0.006% phenol give a stable perchlorethylene.
An Stelle der wasserfreien Soda kann man auch z. B. Natriumbicarbonat, Kaliumcarbonat, Calciumcarbonat oder Calciumoxyd verwenden. Instead of the anhydrous soda you can also use z. B. Sodium bicarbonate, Use potassium carbonate, calcium carbonate or calcium oxide.
Beispiel 2 Ein wie im Beispiel 1 mit wasserfreier Soda und Ammoniak behandeltes technisches Perchloräthylen wird zur Entfärbung destilliert. Dem ohne Abschleiden eines Vorlaufs aufgefangenen Destillat werden 0.020/0 Morpholin und 0.0060/, Phenol zugesetzt. Example 2 As in Example 1 with anhydrous soda and ammonia treated technical grade perchlorethylene is distilled to decolorize. The one without Separating a forerunner collected distillate will be 0.020 / 0 morpholine and 0.0060 /, phenol added.
Beispiel 3 8 t technisches Perchloräthylen werden mit 8 kg wasserfreier Soda zersetzt und im Rührhehälter zum Sieden unter Rückflußkühlung erhitzt. Gleichzeitig wird kräftig Ammoniak eingeleitet. Sobald eine Probe beim Kochtest einen p11-Wert von mindestens 4,0 ergibt, wird auf etwa 600 C abgekühlt und filtriert. Darauf wird das Perchloräthylen unter Zusatz von 1 kg wasserfreier Soda und 2,4 kg Morpholin destilliert. Dem Destillat werden noch 0,006 °/o Phenol zugesetzt. Das so erhaltene Perchloräthylen gibt mit Benzidin innerhalb von 24 Stunden keine Gelbfärbung und korrodiert nicht. Example 3 8 t of technical perchlorethylene become anhydrous with 8 kg Soda decomposes and refluxed in a stirred tank. Simultaneously vigorous ammonia is introduced. As soon as a sample has a p11 value in the boiling test of at least 4.0 results, is cooled to about 600 C and filtered. On it will the perchlorethylene with the addition of 1 kg of anhydrous soda and 2.4 kg of morpholine distilled. 0.006% phenol is added to the distillate added. The perchlorethylene thus obtained does not give benzidine within 24 hours Yellow in color and does not corrode.
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DEC11271A DE1026303B (en) | 1955-05-20 | 1955-05-20 | Process for cleaning perchlorethylene |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DEC11271A DE1026303B (en) | 1955-05-20 | 1955-05-20 | Process for cleaning perchlorethylene |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE1026303B true DE1026303B (en) | 1958-03-20 |
Family
ID=7014951
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DEC11271A Pending DE1026303B (en) | 1955-05-20 | 1955-05-20 | Process for cleaning perchlorethylene |
Country Status (1)
| Country | Link |
|---|---|
| DE (1) | DE1026303B (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2084937A (en) * | 1935-04-04 | 1937-06-22 | Dow Chemical Co | Purification of tetrachloroethylene |
| US2280794A (en) * | 1940-07-11 | 1942-04-28 | Du Pont | Purification of tetrachlorethylene |
-
1955
- 1955-05-20 DE DEC11271A patent/DE1026303B/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2084937A (en) * | 1935-04-04 | 1937-06-22 | Dow Chemical Co | Purification of tetrachloroethylene |
| US2280794A (en) * | 1940-07-11 | 1942-04-28 | Du Pont | Purification of tetrachlorethylene |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| DE1026303B (en) | Process for cleaning perchlorethylene | |
| CH407115A (en) | Process for purifying reducible, cyclic, organic compounds | |
| DE551338C (en) | Process for the production of phenolate liquor | |
| DE508953C (en) | Process for the purification of synthetic organic products from carbon oxides | |
| DE654191C (en) | Process for the production of high-quality, low-boiling hydrocarbons | |
| AT221475B (en) | Process for the production of stable alkali perborate | |
| AT119490B (en) | Process for cleaning or regenerating alkaline solutions contaminated with organic substances. | |
| DE566517C (en) | Process for purifying the contact fluid in the production of acetaldehyde from acetylene | |
| DE350808C (en) | Process for the preparation of diethyl sulfate | |
| DE1058946B (en) | Wastewater treatment | |
| DE724814C (en) | Method of depilation of skins or pelts | |
| DE349265C (en) | Procedure for processing the gas water | |
| AT118229B (en) | Process for cleaning up waste alkaline solutions contaminated with organic substances. | |
| DE322461C (en) | Process for cleaning alkaline waste liquors contaminated and colored by organic additions | |
| DE723340C (en) | Process for separating pure phenol mixtures from phenol-containing distillation products | |
| DE585421C (en) | Manufacture of potash | |
| DE18722C (en) | Process for the preparation of magnesia or magnesium carbonate on ammonium magnesium carbonate | |
| AT203483B (en) | Process for cleaning impure, especially strong-smelling cresols | |
| AT73773B (en) | Process for the regeneration of mercury catalysts. | |
| DE541472C (en) | Process for the purification of benzoic acid | |
| AT105343B (en) | Process for the production of aluminum chloride. | |
| DE839639C (en) | Process for the processing of aqueous, zinc chloride-containing waste solutions from cellulose esterification | |
| DE1008001B (en) | Process for removing titanium compounds from polyethylene | |
| AT228742B (en) | Process for the processing of partially degraded working solutions in the production of hydrogen peroxide by the anthraquinone process | |
| CH133468A (en) | Process for cleaning alkaline solutions. |