CS252055B1 - Process for recovering 2-propanol lost in the production of D, L-threo-2-amino-1- (4-nitrophenyl) -1,3-propanediol hydrochloride - Google Patents

Process for recovering 2-propanol lost in the production of D, L-threo-2-amino-1- (4-nitrophenyl) -1,3-propanediol hydrochloride Download PDF

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CS252055B1
CS252055B1 CS837273A CS727383A CS252055B1 CS 252055 B1 CS252055 B1 CS 252055B1 CS 837273 A CS837273 A CS 837273A CS 727383 A CS727383 A CS 727383A CS 252055 B1 CS252055 B1 CS 252055B1
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Czechoslovakia
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propanol
threo
nitrophenyl
amino
production
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CS837273A
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Czech (cs)
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CS727383A1 (en
Inventor
Jan Kostkan
Miluse Maternova
Blanka Vostarkova
Josef Smidek
Jiri Jary
Vera Bartlova
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Jan Kostkan
Miluse Maternova
Blanka Vostarkova
Josef Smidek
Jiri Jary
Vera Bartlova
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Application filed by Jan Kostkan, Miluse Maternova, Blanka Vostarkova, Josef Smidek, Jiri Jary, Vera Bartlova filed Critical Jan Kostkan
Priority to CS837273A priority Critical patent/CS252055B1/en
Publication of CS727383A1 publication Critical patent/CS727383A1/en
Publication of CS252055B1 publication Critical patent/CS252055B1/en

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Abstract

Způsob regenerace 2-propanolu při výrobě hydrochloridu D-L-threo-2-§oetamido-l- -(4-nitrofenyl)-l,3-propanolu. Řešení se týká regenerace 2-propanolu užívaného na promýv&ní produktu. Rozpuštěné balasty se odstraňují účinkem zásad.Method for the regeneration of 2-propanol in the production of D-L-threo-2-acetamido-1-(4-nitrophenyl)-1,3-propanol hydrochloride. The solution relates to the regeneration of 2-propanol used for washing the product. Dissolved ballasts are removed by the action of alkalis.

Description

Při výrobě hydrochloridu D,L-threo-2-amino-l-(4-nitrofenyl)-l,5-propandiol (I) odpadá velké množství 2-propanolu.In the preparation of D, L-threo-2-amino-1- (4-nitrophenyl) -1,5-propanediol (I) hydrochloride, a large amount of 2-propanol is eliminated.

Ve vodném 2-propanolu se provádí např. deacetylace D,L-threo-2-acetamido-l-(4-nitrofenyl)-l,3~propandiolu (II). Vodným i bezvodým 2-propanolem se produkt, tj. hydrochlorid I, promývá.In aqueous 2-propanol, for example, deacetylation of D, L-threo-2-acetamido-1- (4-nitrophenyl) -1,3-propanediol (II) is carried out. Both aqueous and anhydrous 2-propanol wash the product, i.e., hydrochloride I.

Je popsána řada postupů zpracování odpadajícího 2-propanolu. Obvykle se odpadající 2-propanol zpracuje absolutizací.Numerous processes for treating 2-propanol are described. Usually, the 2-propanol which is removed is treated by absolutization.

Z hlediska rozpustnosti hydrochloridu I je výhodné tento produkt promýt 2-propanolem. Po promytí hydrochloridu I obsahuje 2-propanol vedle kyselin řadu různých balastů organické i anorganické povahy a 30 až 50 % hmot, · vody. Značný obsah vody znemožňuje absolutizací. Balastni látky komplikují oddestilování azeotropni směsi a vody (88 % 2-propanolu), protože zanáší destilační zařízení. Z těchto důvodů se promývaoí 2-propanol kanalizoval. Tím se z výroby ztráoí 20 až 5θ % 2-propanolu.In view of the solubility of hydrochloride I, it is preferable to wash this product with 2-propanol. After washing the hydrochloride I, in addition to the acids, the 2-propanol contains a number of different ballasts of organic and inorganic nature and 30 to 50% by weight of water. A considerable water content makes it impossible by absolutisation. Ballasts complicate the distillation of the azeotropic mixture and water (88% 2-propanol) because it clogs the distillation apparatus. For this reason, the 2-propanol wash was drained. As a result, 20 to 5% of 2-propanol is lost from production.

Uvedené nedostatky a ztrátu 2-propanolu odstraňuje postup podle předkládaného vynálezu.Said drawbacks and loss of 2-propanol are eliminated by the process of the present invention.

Podle vynálezu se promývací 2-propanol zbaví většiny kyselin neutralizací přidáním zásady, např. hydroxidu sodného. Potom se oddestiluje vodný 2-propanol s obsahem vody 10 až 12 % hmot.' Během destilace se vyloučí balastni látky v takové formě, kterou lze z vařáku snadno odstranit.According to the invention, the washing 2-propanol is freed of most acids by neutralization by addition of a base, e.g. sodium hydroxide. Aqueous 2-propanol with a water content of 10 to 12% by weight is then distilled off. During the distillation, ballasts in a form that can be easily removed from the digester are deposited.

Uvedeným postupem, tj.regenerací promývacího 2-propanolu, lze vrátit do výroby 20 až 50 % hmot,. 2-propanolu. Další výhoda, kterou vynález přináší, spočívá ve zlepšeni stavu odpadních vod.By this process, i.e. regeneration of the 2-propanol wash, 20 to 50 wt. Of 2-propanol. A further advantage of the invention is the improvement of the wastewater condition.

Vynález a jeho účinky-jsou blíže osvětleny na následujícím příkladu pr ovesní.The invention and its effects are illustrated in more detail in the following example.

PříkladExample

Do 2 litrové baňky opatřené topným hnízdem a sestupným chladičem s teploměrem bylo vneseno 1000 ml roztoku 2-propanolu o složení -30 % hmot. vody, 6 % hmot· kyseliny chlorovodíkové a, octové a 15 % hmot. balastů. Směs byla zneutralizována přidáním 30 g hydroxidu sodného. Potom bylo oddestilováno 450 ml destilátu o složení 90 % hmot. 3r*propanolu, 8 % hmot; vody a 2 % hmot. nečistot. Teplota par dosáhla 82 °C.A 2 liter flask equipped with a heating nest and a descending condenser with a thermometer was charged with 1000 ml of a -30 wt.% 2-propanol solution. water, 6 wt.% and hydrochloric acid, acetic acid, and 15 wt. ballasts. The mixture was neutralized by the addition of 30 g of sodium hydroxide. Thereafter, 450 ml of a 90% by weight distillate were distilled off. 3% propanol, 8 wt%; water and 2 wt. impurities. The vapor temperature reached 82 ° C.

- 2 PfiEDMÉT VYNÁLEZU- 2 SCOPE OF THE INVENTION

Claims (1)

PfiEDMÉT VYNÁLEZUSUBJECT OF THE INVENTION Způsob regenerace 2-propanolu odpadajícího při výrobě hydrochloridu DtL-threo-2-amino-l-(4-nitrofenyl)-l,3-propandiolu, vyznačený tím, že se pH reakční směsi upraví přidáním hydroxidu alkalického kovu nebo soli tohoto kovu a slabé ky seliny na hodnotu pH 5 až 8 a 2-propanol se z reakční směsi oddestiluje z 5® až 100 % hmotnostních·Regeneration method odpadajícího 2-propanol in the manufacture of D T L-threo 2-amino-l- (4-nitrophenyl) -l, 3-propanediol, wherein the pH of the reaction mixture is adjusted by adding alkali metal hydroxide or a salt of this metal and weak acids to a pH of 5 to 8 and 2-propanol are distilled off from the reaction mixture from 5 to 100% by weight ·
CS837273A 1983-10-05 1983-10-05 Process for recovering 2-propanol lost in the production of D, L-threo-2-amino-1- (4-nitrophenyl) -1,3-propanediol hydrochloride CS252055B1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CS837273A CS252055B1 (en) 1983-10-05 1983-10-05 Process for recovering 2-propanol lost in the production of D, L-threo-2-amino-1- (4-nitrophenyl) -1,3-propanediol hydrochloride

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CS837273A CS252055B1 (en) 1983-10-05 1983-10-05 Process for recovering 2-propanol lost in the production of D, L-threo-2-amino-1- (4-nitrophenyl) -1,3-propanediol hydrochloride

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CS727383A1 CS727383A1 (en) 1987-01-15
CS252055B1 true CS252055B1 (en) 1987-08-13

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