SU42551A1 - Method for isolating lecithin, guanine, adenine and hypoxanthin from beet syrup - Google Patents

Description

To the author's testimony of N. V. Troitsky, as claimed on November 19, 1934 (Ref. 157428).

on the issuance of the copyright certificate published April 30, 1935.

In the sugar industry, large amounts of molasses are produced as waste. In its main mass, molasses consists of 50% sugar, water and 30% of the so-called non-sugar, consisting of 20% organic and 10% mineral substances.

The organic part of non-sugar molasses consists of nitrogen-free and nitrogenous substances, which in one way or another can be separated from it and disposed of.

The author of the present invention has found that lecithin, guanine, adenine and hypoxanthine can be distinguished from molasses from copper salts. From the precipitate thus obtained, lecithin is recovered by extraction with methyl alcohol. The residue after the removal of copper in the form of sulfurous salt is dissolved in caustic soda, then after neutralizing the excess alkali, guanine falls out of solution. The filtrate is evaporated to dryness, dissolved in sulfuric acid, filtered and, after neutralization with ammonia, a precipitate of guanine precipitates.

Separating the guanine, filtered, again evaporated to dryness and treated with lime. Again filtered, evaporated to dryness in order to obtain adenine and hypoxanthine.

Example. 11000.L molasses is stirred from 25750 l of water, 440 l of 10% solution of copper sulphate is poured and

(1SH

leave the mixture alone until the next day. The next day (after b-12 hours), the liquid that had settled above the sediment siphons off, and the precipitate is filtered on a filterpress. The precipitate which is pushed onto the filter is washed with water until the liquid flowing down from the precipitate takes on a light yellowish tint.

A precipitate of 4 kg is obtained.

Sediment contains:

Guanine5.5 / sg -12.5%

Yadinina 7,7, -17,0

Hypoxanthin ... 1.3, - 2.5 and Lecithin22.0, - 6.0%

To remove lecithin from the precipitate, it is dried and loaded into a percolator system, where it is systematically extracted with methyl alcohol. Methyl alcohol is distilled off in vacuo from the resulting saturated solution, and the residue is dissolved in 5 kg of sulfuric ether. By distilling off the ether, the residual is again dissolved in alcohol and ether once more and lecithin is obtained in an amount of 2.2 kg with a phosphorus content of 6%.

The residual sediment discharged from percolors is transferred to a leaded tank equipped with a stirrer and a 300 l steam coil. The precipitate in the tank is doused with 60 liter of 20% sodium sulphide solution. The mixture is stirred

in TOHKyi gruel, after which it is heated to a boil. In a hot mixture pour a thin stream of another 90 liters of sodium sulfate solution of the same strength. At the end of the addition of the sodium sulphurous solution, the contents of the tank continue to boil for 5 minutes, after which the mixture, 32 liters of water and 30 kg of sulfuric acid, begin to pour in a thin stream until acid reaction to the litmus occurs. At the end of the sulfuric acid addition, the mixture is boiled for another three minutes, then the precipitate is allowed to settle and then filtered. A precipitate containing copper sulphide is obtained. The filtrate is neutralized with caustic soda and then continue to pour it until the alkaline reaction nor the litmus.

The solution is now left alone for a day and receives a precipitate, consisting of guanine, weighing 6 kg.

The precipitate is dissolved by heating in 50./g of sulfuric acid, obtained by displacing 48.75 vz of water and 1.25 l of sulfuric acid; d. 1.84. The solution is separated from sulfur and other insoluble substances by filtration and treated with ammonia 20 / ;, its content in the solution. Mixture: left alone for a day, after which the precipitated guanine is filtered off. After this, the scab is again dissolved in a normal caustic norther solution and precipitated back with sulfuric acid. The resulting guanine is seropalic in color and contains 38% nitrogen. It is 5 kg.

The filtrate obtained after separation of the main mass of guanine is evaporated to dryness; In a strictly neutral environment, a dry residue is obtained, consisting mainly of adenine, hypocantine, and then guanine. He is treated in the following way. Take 21 l of water, pour 3 kg of concentrated sulfuric acid into it, and extract the resulting mixture with heating and remove the residue. . Yadanin, guanine, and hypxanthine are dissolved. The solution is filtered: it is separated from the non-dissolved part i, the filtrate is neutralized with ammonia and then the latter is added to -2% in solution. The mixture is left for one day alone. Guanine is isolated, it is filtered in an amount of V2 .:

This guanine has more teMHyro coloring. The nitrogen content in it.

Lime is added to the filtrate, the ammonia solution is filtered from the insoluble part and evaporated to dryness. The resulting residue contains 7.7 kg of adenine and 1.1 hypoxanthine.

The precipitate consisting of copper sulphide can be processed into copper sulfate using one of the usual methods.

Method 1. Take 66 l of water and shift, with 8. / G of concentrated sulfuric acid and the 2nd precipitate is poured with this mixture. While stirring, the mixture is heated and a mixture of 4 kg of nitric acid and 6 liters of water is poured into it in portions. Heating prodBU1U {yyut until black color of sulphurous copper disappears. Then. solution, pp, is filtered off from the 4th sediment. The precipitate is thoroughly washed with hot water until all copper salts are leached out.

The filtrate, along with industrial water, is concentrated until lOVo coflective copper kyriopoca and fi g is again used in the matter .-- - Method 2. The precipitate -2nd is treated with a solution of iron oxide iron. Copper is perekrashsya in solution by filtration. It is separated from the insoluble precipitate. -Filtrate when heated decomposes with melb. The copper sulfate pacfBOjb, separated by filtration of the precipitated precipitate, is centered to content.

This method is interesting because with its help it is possible to create a sulfur cycle, as a result of which sulfuric acid and sodium hydroxide will be consumed in production.

R and with X about d m ate and a l about in:

Sulfuric acid ..49 kg worth 10 p. 80 k,

izoic acid. 5,6,. „5, 60.

Caustic soda. ..five " . "-" 60 "

Sulfur Natra.30,. „- b„ .г23 р. - K. „

Received:

Guanin. .... 5.5 "g

Yadinina 7.7 "

Hypoxanthin ... i L, 1 „Lecithin ....-...,. .2,2i

16.5 kg

The molasses left over from the 1st sediment separation is fermented in yeast or distillery.

The subject matter of the invention.

A method for isolating lecithin, guanine, adenine and hypoxanthin from molasses by precipitation with copper salts, characterized in that the precipitate obtained after precipitating 53 molasses solution by copper sulfate is subjected to extraction with methyl alcohol to extract the lecithin, the precipitate obtained thereafter is decomposed with sodium sulphide when heated, then sulfuric acid is added

acids and, after filtering the solution from copper sulphide, alkalize it with caustic soda until alkaline reaction to litmus and the precipitated guanine precipitate after standing is separated, cleaned, and the filtrate is evaporated to dryness under strictly neutral reaction, after which the precipitate is dissolved in solutionresulfuric acid , filtered from the undissolved part, the filtrate is neutralized with ammonia and after standing, the precipitated guanine is filtered off, lime is added to the filtrate, filtered again and evaporated to dryness to obtain the residue ins and hypoxanthine.