DE141976C - - Google Patents

Description

IMPERIAL

PATENT OFFICE.

GREAT

In practice, there are mainly two methods for representing the glycocolla Consideration:

1. the action of ammonia on chloroacetic acid and

2. the action of ammonia on the nitrile of glycolic acid and saponification of the so resulting amidoacetic acid nitrile with alkalis (Ann. 278, p. 237).

With both methods, the glycocoU arises in abundant yield, but always in addition Alkali or alkaline earth salts of inorganic acids, in particular in addition to salmiak, table salt etc., whereby its pure representation is made significantly more difficult. The glycocolla is as is known, just like these inorganic salts only in water - and very lightly - Soluble, so that detours have to be taken in order to separate it out. That best known deposition process is that of Kraut (Ann. 266, p. 295), which about the poorly soluble copper salt of glycocolla leads. The same is quite well suited for the manufacture of small quantities of glycocolla in the laboratory; for a factory production however, large amounts of glycocolla appear cumbersome and costly.

It has now been found that one can obtain the technically easily obtainable mixtures of glycocolla and the chlorides respectively. Conveniently separate sulfates of sodium or potassium by means of glycerin can. Glycocolla dissolves abundantly in glycerine even at a water bath temperature, while the aforementioned inorganic salts are insoluble therein.

For the practical implementation of the method you can, for. B. work in the following way:

First of all, the procurement of the glycocolla salt mixture is concerned, one of the two ways mentioned at the beginning can be taken:

ι. According to the information from Hantzsch & Silberrad, Ber. XXXIII, 70 a solution of 10 kg of monochloroacetic acid in 5 1 of water with vigorous shaking pour into 120 1 Ammonia, spec. Weight 0.913. After standing for 24 hours, one of the chloroacetic acids used is added equivalent amount of sodium hydroxide, d. H. about 4.5 kg, or potassium hydroxide, d. H. about 7.5 kg, chases away the excess ammonia, evaporates and dries the remaining, approximately molecular mixture of glycocolla and sodium chloride respectively. Potassium chlorine perfectly at about 10 °. Or it will

2. after Eschweiler, Ann. 278, 237, those from commercially available formaldehyde and hydrocyanic acid shown, 30 to 40 percent methylene cyanohydrin solution with five times the volume 3% ammonia water was added and after standing for 12 hours with normal Temperature saponified with caustic soda (or potassium hydroxide) in the calculated amount. After completed Saponification is added in a diluted amount equivalent to the amount of alkali lye used Adding hydrochloric acid or sulfuric acid drives away the unused ammonia and dries it remaining mixture of glycocolla and

Table salt (chlorine potassium) resp. Glycocolla and sodium (potassium) sulfate perfectly at about ι io to i2o °.

The glycocolla salt mixture obtained by one of the two methods or otherwise is now separated in approximately the following way with glycerine, where one is most expedient and cheapest with glycocollar salt mixtures works:

In a suitable vessel equipped with a stirrer and heated by means of an oil bath, the dry, finely ground glycocolla salt mixture is mixed with about ten times the weight of the highest possible percentage of glycerine, whereupon the temperature is increased to around 100 to 150 ⁰ while stirring. The glycocolla goes into solution, while the inorganic salt remains undissolved. After several hours of heating, the stirrer is switched off and allowed to cool. The inorganic salt quickly settles as a solid crust at the bottom of the vessel, whereupon the still warm glycocoll-glycerol solution is drawn off. The glycerol can now be obtained from this solution in various ways: either the glycerine is evaporated in a vacuum or in a stream of superheated steam, or the glycerol is precipitated from the glycerol solution with alcohol or wood spirit.

After recrystallization from water or from aqueous alcohol, the products obtained in this way show the familiar ones
shafts of glycocolla.

For some purposes, e.g. B. for the Dar position of phenylglycine-o-carboxylic acid respectively.

Own from indigo from glycocolla and o-chlorobenzoic acid, one can refrain from separating the glycocollate from the glycerol solution and work directly with this solution.

The method described above can now also be used to its full extent Apply when it comes to the representation or Deposition of the nitrogen-alkylated Glycollus acts.

It is well known that the mono- and dialkylated glycocolls, especially the mono- methylglycocoll (sarcosine) and the dimethylglycocoll, the monoethyl and diethyl glycocoll both in the action of chloroacetic acid on the corresponding mono- and dialkylated Ammoniake (Ann. 129, 35; 132, 1; 140, 217 etc.) as well as by the action of glycolonitrile on the same bases and saponification of the the resulting mono- and dialkylated amidoacetonitriles with fixed alkalis (Ann. 27g, 44). The mixture of alkylated glycocolla obtained in this way as described above and table salt (or potassium chloride) or sodium-potassium) sulfate are then separated with glycerine exactly as described above.

Claims (1)

Patent claim: Process for the separation of glycocolla and its nitrogen-alkylated Derivatives from mixtures of the same with inorganic salts, in particular with sodium chloride, Potassium chlorine, sodium sulphate, potassium sulphate, characterized in that the glycocolls are removed from these mixtures with glycerine.