PL422B1 - Method of obtaining methyl alcohol from methyl chloride. - Google Patents
Method of obtaining methyl alcohol from methyl chloride. Download PDFInfo
- Publication number
- PL422B1 PL422B1 PL422A PL42220A PL422B1 PL 422 B1 PL422 B1 PL 422B1 PL 422 A PL422 A PL 422A PL 42220 A PL42220 A PL 42220A PL 422 B1 PL422 B1 PL 422B1
- Authority
- PL
- Poland
- Prior art keywords
- methyl chloride
- methyl
- chloride
- methyl alcohol
- alcohol
- Prior art date
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- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 title claims description 26
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 title claims description 23
- 229940050176 methyl chloride Drugs 0.000 title claims description 12
- 238000000034 method Methods 0.000 title claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 2
- 239000011230 binding agent Substances 0.000 claims description 2
- 239000012751 acid resistant agent Substances 0.000 claims 1
- 239000007789 gas Substances 0.000 claims 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 5
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 238000005684 Liebig rearrangement reaction Methods 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- NEHMKBQYUWJMIP-NJFSPNSNSA-N chloro(114C)methane Chemical compound [14CH3]Cl NEHMKBQYUWJMIP-NJFSPNSNSA-N 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
Description
Pierwszenstwo: 4 pazdziernika 1913 r. (St. Zj. Am.).Wiadomo, ze mozna otrzymywac me¬ tan juz oddawna prawie za darmo i to badz z gazu ziemnego badz przez syn¬ tetyczne wytwarzanie podlug róznych katalitycznych metod. Nie brakowalo licznych badan dla wytworzenia cennych pochodnych metylu z tego weglowodoru.Jako najbardziej prosta i celowa droge ku temu uznano za wlasciwa: CH4^CH3C1^CH3 CH.Te reakcje, jako zasadnicze dla alko¬ holu metylowego, sa zdawna znane, lecz techniczne wytwarzanie alkoholu metylo¬ wego na tej drodze dotychczas bylo niemozliwe. Dla pierwszej fazy prze¬ miany gazu blotnego w alkohol mety*- lowy, mianowicie dla wyrobu chlorku metylu, technicznie uzyteczne sposoby sa juz obecnie opracowane, przeciwnie, tak latwe na pozór zadanie zamiany chloru znajdujacego sie w chlorku metylu na wodorotlenek, jest dotychczas nie rozwiazane w sposób zadawalniajacy.Badania podjete przez Berthelota, a zmie¬ rzajace ku temu, raczej odstraszaly od pracy w celu technicznego wykorzysta¬ nia tej reakcji, potrzebowal on bowiem dla przemiany 2 1 chlorku metylu w alkohol metylowy przez zagrzewanie z lugiem potasowym na 100°, calego tygodnia (porównaj Berthelot, Liebigs Annalen Bd. 105, S. 244). Nie bylo prze¬ widziane, ze reakcja w innych warun¬ kach, zwlaszcza przy wyzszych tempe¬ raturach, moze byc przeprowadzona predzej, a pomimo to z dobrym rezul¬ tatem.Stwierdzono, ze zaleznie od warun¬ ków pracy w rzeczywistosci przebiegaja dwa procesy, a mianowicie:1. CH3Cl+ H.OH = HCI+ CH3 OH CH3CI H CH3 2. + \o = 2HCL -f \o CH3C1 H/ CH/ Wynalazek daje moznosc reakcje pierwsza CH3Cl+H.OH=HCl+CH8OH przeprowadzic w dowolnych rozmiarach i tak nia kierowac, by w najkrótszym czasie wytworzyl sie przy najwiekszej wydajnosci alkohol drzewny.Wlasciwosc nowego sposobu wyjasni sie najlepiej z praktycznego przykladu.Autoklaw, zaopatrzony w mieszadlo, dopuszczajacy czynne cisnienie az do 25 Atm., napelnia sie do polowy mle¬ kiem wapiennem, które zawiera w litrze wody okolo 150 g Ca (OH)2. Nastepnie zamykamy aparat i zagrzewamy w przy¬ blizeniu do 190°. Gdy osiagnie sie te temperature manometr autoklawu wska¬ zuje mniej wiecej 12 Atm. cisnienia.Wtedy dopuszczamy z griibosciennego zbiornika tyle chlorku metylu, &z mano¬ metr wskaze okolo 20 Atm. Mieszadlo puszcza sie teraz w pelny bieg w przy¬ blizeniu przez 15 minut i przy tempe¬ raturze 190°, a doprowadzanie chlorku metylu przez wentyl tak sie reguluje, by calkowite cisnienie bylo stale przy 2i) Atm. Po tym czasie panuje w apara¬ cie nawet przy zamknietym wentylu cisnienie jeszcze okolo 18 Atm., zlozone z cisnien wody, alkoholu drzewnego, chlorku metylu i eteru metylowego, któ¬ rego sie wytworzylo od 5 — 10°/0- W warunkach, sprzyjajacych szybkiej przemianie chlorku metylu na alkohol metylowy trudno zapobiec tworzeniu sie eteru metylowego, lecz przy taniosci wyjsciowego produktu ten przypadek jest maloznaczacy.Z danych liczbowych przykladu wy¬ nika, ze przeciwcisnienie chlorku metylu w tym wypadku wynosi na poczatku 8 Atm., na koncu zas 2 Atm. To prze¬ ciwcisnienie chlorku metylu jest zasad¬ nicza cecha nowego sposobu, poniewaz od jego wielkosci zalezy w znacznej mierze i predkosc reakcji.Zamiast wodorotlenku wapnia, jako czynnika wiazacego kwas, moze byc naturalnie uzytym równiez lug sodowy, weglan sodu lub wapnia, albo siarczan sodu lub wapnia.Uzyta tu ilosc wody moze sie wahac w szerokich granicach. Mozna wytwo¬ rzyc w lugu koncowym alkohol 7, 10, wzgl. 20%. PLFirst place: October 4, 1913 (United States of America) It is known that it is possible to obtain methane for a long time almost for free, either from natural gas or by synthetic preparation of the soil by various catalytic methods. There has been a lot of research into the preparation of the valuable methyl derivatives from this hydrocarbon. The most straightforward and expedient route to this has been found to be the right one: CH4 → CH3C1 → CH3 CH. These reactions, being essential for methyl alcohol, are long known, but the technical preparation of methyl alcohol on this route has hitherto been impossible. For the first phase of the conversion of the mud to methyl alcohol, namely for the production of methyl chloride, technically useful methods have already been developed, on the contrary, the seemingly easy task of converting chlorine in methyl chloride into hydroxide has not yet been solved. The research undertaken by Berthelot to do so rather discouraged him from working to exploit this reaction technically, since he needed to convert 2 liters of methyl chloride into methyl alcohol by heating with potassium liquor to 100 ° C. a whole week (cf. Berthelot, Liebigs Annalen Bd. 105, p. 244). It was not foreseen that the reaction under other conditions, especially at higher temperatures, could be carried out sooner, and yet with good results. It has been found that, depending on the operating conditions, two processes actually take place, namely: 1. CH3Cl + H.OH = HCI + CH3 OH CH3CI H CH3 2. + \ o = 2HCL -f \ o CH3C1 H / CH / The invention allows the first reaction CH3Cl + H.OH = HCl + CH8OH to be carried out in any size and so be used, The properties of the new method are best explained from a practical example: an autoclave, equipped with a stirrer, permitting an active pressure of up to 25 Atm., is half filled with lime milk, which is contained in a liter water, about 150 g Ca (OH) 2. Then we close the apparatus and heat it up to approximately 190 °. When this temperature is reached, the autoclave manometer reads about 12 atm. Then we let in as much methyl chloride from the deep-wall tank as the manometer shows about 20 atm. The agitator is now run at approximately 15 minutes at a temperature of 190 ° C and the supply of methyl chloride through the valve is adjusted so that the total pressure is kept constantly at 2 µm. After this time, even with the valve closed, there is still a pressure of about 18 atm., Consisting of the pressures of water, wood alcohol, methyl chloride and methyl ether, which was formed from 5 - 10 ° / 0- under favorable conditions. the rapid conversion of methyl chloride to methyl alcohol is difficult to prevent the formation of methyl ether, but with the cheapness of the starting product, this case is unimportant. From the numerical data of the example it appears that the back pressure of methyl chloride in this case is 8 atm at first, and finally 2 Atm. This counterpressure of methyl chloride is an essential feature of the new process, since its size depends to a large extent on the speed of the reaction. Instead of calcium hydroxide as the acid-binding agent, sodium hydroxide, sodium or calcium carbonate, or sulfate can also be used naturally. sodium or calcium The amount of water used here can vary widely. Alcohol 7, 10 or twenty%. PL
Claims (2)
Publications (1)
| Publication Number | Publication Date |
|---|---|
| PL422B1 true PL422B1 (en) | 1924-08-30 |
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