BE509446A - - Google Patents
Info
- Publication number
- BE509446A BE509446A BE509446DA BE509446A BE 509446 A BE509446 A BE 509446A BE 509446D A BE509446D A BE 509446DA BE 509446 A BE509446 A BE 509446A
- Authority
- BE
- Belgium
- Prior art keywords
- amines
- amine
- mixture
- ammonia
- alkali metal
- Prior art date
Links
- 238000000034 method Methods 0.000 claims description 19
- 150000001412 amines Chemical class 0.000 claims description 15
- CURLTUGMZLYLDI-UHFFFAOYSA-N carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 8
- 239000001569 carbon dioxide Substances 0.000 claims description 8
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 239000003153 chemical reaction reagent Substances 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 238000004821 distillation Methods 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- -1 isobutyl propyl Chemical group 0.000 claims description 4
- 238000009835 boiling Methods 0.000 claims description 3
- 150000003947 ethylamines Chemical class 0.000 claims description 2
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 claims description 2
- 229910000288 alkali metal carbonate Inorganic materials 0.000 claims 1
- 150000008041 alkali metal carbonates Chemical class 0.000 claims 1
- 229910001514 alkali metal chloride Inorganic materials 0.000 claims 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 claims 1
- 239000000376 reactant Substances 0.000 claims 1
- NIWMEUWZZDPUEQ-UHFFFAOYSA-M sodium;azane;hydroxide Chemical compound N.[OH-].[Na+] NIWMEUWZZDPUEQ-UHFFFAOYSA-M 0.000 claims 1
- 239000000126 substance Substances 0.000 claims 1
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 9
- FAPWRFPIFSIZLT-UHFFFAOYSA-M sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 6
- 239000001184 potassium carbonate Substances 0.000 description 5
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 5
- 239000003513 alkali Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 229910000027 potassium carbonate Inorganic materials 0.000 description 4
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 3
- 235000015450 Tilia cordata Nutrition 0.000 description 3
- 235000011941 Tilia x europaea Nutrition 0.000 description 3
- 230000000875 corresponding Effects 0.000 description 3
- 239000004571 lime Substances 0.000 description 3
- 235000011164 potassium chloride Nutrition 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 239000011780 sodium chloride Substances 0.000 description 3
- FXZWPZMCZNJILD-UHFFFAOYSA-N N-[(6-bromopyridin-3-yl)methyl]ethanamine;hydrochloride Chemical compound Cl.CCNCC1=CC=C(Br)N=C1 FXZWPZMCZNJILD-UHFFFAOYSA-N 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M NaHCO3 Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- 125000004432 carbon atoms Chemical group C* 0.000 description 2
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- 150000001805 chlorine compounds Chemical class 0.000 description 2
- 150000003956 methylamines Chemical class 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000001103 potassium chloride Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 241000238876 Acari Species 0.000 description 1
- 235000016068 Berberis vulgaris Nutrition 0.000 description 1
- 241000335053 Beta vulgaris Species 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N Carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N HCl Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- KDSNLYIMUZNERS-UHFFFAOYSA-N Isobutylamine Chemical compound CC(C)CN KDSNLYIMUZNERS-UHFFFAOYSA-N 0.000 description 1
- JJWLVOIRVHMVIS-UHFFFAOYSA-N Isopropylamine Chemical compound CC(C)N JJWLVOIRVHMVIS-UHFFFAOYSA-N 0.000 description 1
- TYJJADVDDVDEDZ-UHFFFAOYSA-M Potassium bicarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 description 1
- 238000010533 azeotropic distillation Methods 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N potassium Chemical group [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 229910052700 potassium Chemical group 0.000 description 1
- 239000011591 potassium Chemical group 0.000 description 1
- 239000011736 potassium bicarbonate Substances 0.000 description 1
- 235000015497 potassium bicarbonate Nutrition 0.000 description 1
- 229910000028 potassium bicarbonate Inorganic materials 0.000 description 1
- 229940094025 potassium bicarbonate Drugs 0.000 description 1
- 235000011181 potassium carbonates Nutrition 0.000 description 1
- 159000000001 potassium salts Chemical class 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 150000003141 primary amines Chemical class 0.000 description 1
- 125000006308 propyl amino group Chemical group 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 150000003335 secondary amines Chemical class 0.000 description 1
- 238000001577 simple distillation Methods 0.000 description 1
- 150000003385 sodium Chemical group 0.000 description 1
- KEAYESYHFKHZAL-UHFFFAOYSA-N sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 239000001187 sodium carbonate Substances 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- POECFFCNUXZPJT-UHFFFAOYSA-M sodium;carbonic acid;hydrogen carbonate Chemical compound [Na+].OC(O)=O.OC([O-])=O POECFFCNUXZPJT-UHFFFAOYSA-M 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 230000001131 transforming Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D7/00—Carbonates of sodium, potassium or alkali metals in general
- C01D7/16—Preparation from compounds of sodium or potassium with amines and carbon dioxide
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/141—Feedstock
Description
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PROCEDE DE FABRICATION DE CARBONATES ALCALINS.
Il est connu de fabriquer du carbonate de soude par les procédés dits de la "soude à l'ammoniaque".
Il est également connu de remplacer dans ces procédés l'ammonia- que par, soit les méthylamines obtenues par la distillation des vinasses de betteraves, soit les éthylamines "obtenues par décomposition des éthers or- ganiques". Ces derniers procédés ont pu être étendus à la fabrication du carbonate de potassium qui était impossible avec les procédés de la-soude à l'ammoniaque proprement dite. Tous ces procédés aux amines n'ont pu trou- ver l'application industrielle importante, notamment à cause de caractéris- tiques inacceptables de leurs conditions opératoires.
Dans son brevet français du 5 avril 1950 intitulé "Procédé pour la préparation de carbonates de potassium", la demanderesse a breveté un procédé pour la fabrication du carbonate de potassium dans lequel on utilise,, dans un procédé analogue aux procédés précités, un réactif animé constitué par un mélange d'amines primaires ou secondaires; l'application de ce pro- cédé a conduit à de nouvelles découvertes et à une extension du domaine d'applications de ce procédé.
La présente invention a pour objet un procédé'dans lequel on uti- lise un cycle analogue à celui des procédés dits de la soude à l'ammoniaque pour la fabrication de carbonates alcalins (carbonate de sodium ou carbonate de potassium) à partir des chlorures éorrespondants, dans lequel on substi- tue à l'ammoniaque un réactif aminé constitué par une amine ou un mélange d'amines dont le poids moléculaire est plus élevé que celui desféthylamines, c'est-à-dire possédant un nombre d'atomes de carbone supérieur à 2, et dont les points d'ébullition sont tels qu'on puisse facilement les récupérer hors de leurs solutions aqueuses par distillation simple ou azéotropique.
On a trouvé que notamment les amines en C3 et en C4, amines propy-
<Desc/Clms Page number 2>
tiques et isopropyliques, butyliques et isbutyliques, remplissent particu- lièrement bien ces conditions.
La réaction est vraisemblablement la suivante:
En présence d'anhydride carbonique, l'amine se transforme en car- bonate d'amine, qui réagit avec le chlorure alcalin pour donner le bicarbona- te alcalin qui précipite et du chlorhydrate d'amine:
EMI2.1
dans-laquelle M est du sodium ou du potassium R et R' sont des radicaux alcoyles dont le nombre d'atomes de carbone est supérieur à 2.
Le chlorhydrate d'amine est récupéré hors des eaux-mères, par exemple de la chaux et par distillation.
Le procédé suivant l'invention présente les avantages caractéris- tiques suivants: a) La bicarbonatation peut être réalisée à la pression atmosphéri- que, même en utilisant du .gaz carbonique dilué, tel que, par exemple, le gaz carbonique couramment produit dans les fours à chaux. b) L'utilisation du chlorure alcalin est presque totale, le rende- ment étant de 95 % pour le chlorure de sodium ou le chlorure de potassium. c) L'opération peut avoir lieu en solution concentrée de réactif, ce qui présente le double avantage : utilise un appareillage de volume réduit pour une production donnée ;
de plus, la perte en réactif est d'au- tant plus faible que l'on travaille en solution plus concentrée. d) Par suite du coefficient de volatilité élevé des amines ou mé- langes d'amines choisies, leur distillation hors des solutions aqueuses qui les contiennent est facile et économique, malgré leur point d'ébullition re- lativement élevé. e) Il est possible d'utiliser des proportions stoéchiométriques d'amines et de chlorures alcalins, tout en conservant un rendement presque quantitatif. Il en résulte une énorme simplification des processus habituels de distillation et de récupération du réactif du fait que, à la fin de l'opé- ration, la presque totalité de l'amine se trouve à l'état de chlorhydrate; il est alors possible de simplifier la tour de récupération par suppression de la partie où se fait habituellement la distillation du carbonate d'amine.
On donne ci-après deux exemples d'application du procédé qui ne sont nullement limitatifs: EXEMPLE 1 : On met en présence 200 cm3 d'isopropylamine en solution aqueuse à 40 % et 70 gr. de chlorure de sodium ordinaire. On agite modérément et on fait passer un courant de gaz carbonique dilué à 35 % dans un gaz inerte (azote par exemple) sans agir sur la température. Les gaz sortants sont constitués par de l'azote pur au début de la réaction. La teneur en gaz car- bonique des gaz sortants augmente et la réaction est pratiquement terminée lorsque la teneur des gaz sortants atteint la teneur des gaz à l'arrivée.
On recueille un précipité de bicarbonate de sodium correspondant à un ren- dement de 95 %.
<Desc/Clms Page number 3>
EXEMPLE 2 :
On met en présence 200 cm3 d'amine isobutylique en solution aqueu- se à 40% et 70 gr. de chlorure de potassium technique. On agite modérément et on fait passer un courait de gaz carbonique tel qu'il sort d'un four à chaux, c'est-à-dire pratiquement dilué à 30 %. Lorsque la réaction est termi- née, c'est-à-dire lorsque le gaz carbonique sortant a une teneur de 30 % do CO2, on recueille un précipité de carbonate de potassium correspondant à un rendement de 95 %.
L'invention permet également de réaliser une certaine pu- rification des sels de potassium du fait que, lorsqu'on utilise comme matière première des chlorures de potassium techniques, c'est-à-dire renfermant une certaine proportion de chlorure de sodium, on obtient, après transformation, un bicarbonate de potassium débarrassé de la plus grande partie de sodium.
<Desc / Clms Page number 1>
METHOD OF MANUFACTURING ALKALINE CARBONATES.
It is known to manufacture sodium carbonate by the so-called "ammonia soda" processes.
It is also known practice to replace ammonia in these processes with either the methylamines obtained by the distillation of beet vinasses, or the ethylamines "obtained by decomposition of organic ethers". These latter processes could be extended to the manufacture of potassium carbonate which was impossible with the ammonia-soda processes proper. All these amine processes have not been able to find significant industrial application, in particular because of unacceptable characteristics of their operating conditions.
In its French patent of April 5, 1950 entitled "Process for the preparation of potassium carbonates", the applicant patented a process for the manufacture of potassium carbonate in which is used, in a process similar to the aforementioned processes, a lively reagent consisting of a mixture of primary or secondary amines; the application of this process has led to new discoveries and to an extension of the field of applications of this process.
The present invention relates to a process in which a cycle similar to that of the so-called soda-ammonia processes is used for the manufacture of alkaline carbonates (sodium carbonate or potassium carbonate) from the corresponding chlorides. , in which ammonia is substituted with an amine reagent consisting of an amine or a mixture of amines the molecular weight of which is higher than that of the methylamines, that is to say having a number of carbon atoms greater than 2, and whose boiling points are such that they can easily be recovered from their aqueous solutions by simple or azeotropic distillation.
It has been found that in particular the C3 and C4 amines, propyl amines
<Desc / Clms Page number 2>
ticks and isopropyls, butyls and isbutyls meet these conditions particularly well.
The reaction is likely as follows:
In the presence of carbon dioxide, the amine turns into an amine carbonate, which reacts with the alkali chloride to give the alkali bicarbonate which precipitates and amine hydrochloride:
EMI2.1
in which M is sodium or potassium R and R ′ are alkyl radicals with a number of carbon atoms greater than 2.
The amine hydrochloride is recovered from mother liquors, for example lime and by distillation.
The process according to the invention has the following characteristic advantages: a) The bicarbonation can be carried out at atmospheric pressure, even using dilute carbon dioxide, such as, for example, the carbon dioxide commonly produced in lime kilns. b) The use of alkali chloride is almost total, the yield being 95% for sodium chloride or potassium chloride. c) The operation can take place in a concentrated reagent solution, which has the double advantage: uses equipment of reduced volume for a given production;
moreover, the loss of reagent is all the smaller as one works in a more concentrated solution. d) Owing to the high volatility coefficient of the selected amines or amine mixtures, their distillation from the aqueous solutions which contain them is easy and economical, despite their relatively high boiling point. e) It is possible to use stoichiometric proportions of amines and alkali chlorides, while maintaining an almost quantitative yield. This results in an enormous simplification of the usual processes of distillation and recovery of the reagent since, at the end of the operation, almost all of the amine is in the hydrochloride state; it is then possible to simplify the recovery tower by eliminating the part where the distillation of the amine carbonate is usually carried out.
Two examples of application of the process which are in no way limiting are given below: EXAMPLE 1: 200 cm3 of isopropylamine in 40% aqueous solution and 70 g are brought together. of ordinary sodium chloride. The mixture is stirred moderately and a stream of carbon dioxide diluted to 35% is passed through an inert gas (nitrogen for example) without affecting the temperature. The outgoing gases consist of pure nitrogen at the start of the reaction. The carbon dioxide content of the outgoing gases increases and the reaction is practically complete when the content of the outgoing gases reaches the content of the incoming gases.
A precipitate of sodium bicarbonate corresponding to a yield of 95% is collected.
<Desc / Clms Page number 3>
EXAMPLE 2:
200 cm3 of isobutyl amine in 40% aqueous solution and 70 g are brought together. of potassium chloride technique. Stir moderately and pass a stream of carbon dioxide as it comes out of a lime kiln, that is to say practically diluted to 30%. When the reaction is complete, that is to say when the leaving carbon dioxide has a content of 30% CO 2, a potassium carbonate precipitate is collected corresponding to a yield of 95%.
The invention also makes it possible to carry out a certain purification of the potassium salts because, when technical potassium chlorides are used as raw material, that is to say ones containing a certain proportion of sodium chloride, they are used as raw material. obtains, after transformation, a potassium bicarbonate freed of the greater part of sodium.
Claims (1)
Publications (1)
Publication Number | Publication Date |
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BE509446A true BE509446A (en) |
Family
ID=148868
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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BE509446D BE509446A (en) |
Country Status (1)
Country | Link |
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BE (1) | BE509446A (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE1021341B (en) * | 1954-12-07 | 1957-12-27 | Sarl Soc D Etudes Chimiques Po | Process for the production of Engel's salt |
DE1074562B (en) * | 1960-02-04 | Societe ä Responsabilite Limitee dite·. Societe d'Etudes Ctiimiques pour !'Industrie et !'Agriculture, Paris | Process for the production of sodium bicarbonate from sodium chloride - potassium chloride mixtures by precipitation with isopropylamine bicarbonate |
-
0
- BE BE509446D patent/BE509446A/fr unknown
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE1074562B (en) * | 1960-02-04 | Societe ä Responsabilite Limitee dite·. Societe d'Etudes Ctiimiques pour !'Industrie et !'Agriculture, Paris | Process for the production of sodium bicarbonate from sodium chloride - potassium chloride mixtures by precipitation with isopropylamine bicarbonate | |
DE1021341B (en) * | 1954-12-07 | 1957-12-27 | Sarl Soc D Etudes Chimiques Po | Process for the production of Engel's salt |
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