The method of purification of ethyl synthetic industrial alcohol from impurities of aldehydes and ketones

 

(57) Abstract:

The invention relates to the field of technology organic chemistry, and in particular to methods of cleaning ethyl synthetic industrial alcohol from impurities of aldehydes and ketones. Cleaning lead processing ethyl synthetic industrial alcohol reagent and caustic alkali, with a reagent selected from a number of: resorcinol, urea, hydroxylamine sulfate, hydrazinehydrate, hydrazine sulfate, sodium sulfite, dymadon, soybean oil, sunflower oil at a ratio of reagent is caustic alkali, followed by boiling and distillation. Purified ethyl synthetic industrial alcohol suitable for use in aerosol preparations. table 2.

The invention relates to the technology of organic chemistry and relates to methods of cleaning ethyl synthetic industrial alcohol (ESTs) from impurities of aldehydes and ketones.

According to the technical requirements in force in Russia (THE 38.402-62-117-90), ESTs may contain not more than 0,7 0,9% volume fraction of acetaldehyde and not more than 0.2% volume fraction of crotonic aldehyde. The content of ketones is not standardized.

A known method of purification of synthetic ethyl flavors [1] the disadvantages of this method include the high cost and lack of efficiency of treatment of the alcohol of the proposed method.

A known method for separating ethanol from water-alcohol solutions, obtained as a waste product in the production of silicon dioxide, processing of 0.8-1.0% per 1 l of a solution of hydrochloric acid hydroxylamine and 3% on 1 l of calcium chloride solution or dilute sulfuric acid of at least 10 g per 1 l of solution, followed by distillation. The disadvantages of this method are the need to use a very large number of reagents, as well as noticeable residual presence in the rectified acetaldehyde [2]

The known method of separation of individual products in the manufacture of synthetic ethanol treatment by sodium bisulfite and sodium hydroxide [3], followed by distillation. The disadvantages of this technical solution should include a high residual content (0.05%) of acetaldehyde in the final technical ethanol.

There is also known a method of rectification of the crude alcohol, which consists in the processing of raw alcohol with a mixture of alkali (caustic soda), potassium manganese acid or bicarbonate of sodium [4] the Composition and amount of the mixture varies depending on the presence and amount of certain impurities. The disadvantages of this method will otnositsa insufficient cleaning efficiency is the reception and is a prototype.

The purpose of the present invention is perhaps more thorough cleaning (the acetic aldehyde and acetone not more than 0.01% volume fraction, the Croton th aldehyde absence) of ESTs according to chromatographic analysis.

This goal is achieved by processing ESTs (specifications 38.402-62-117-90) with a maximum content of impurities with a reagent selected from the range: resorcinol, urea, hydroxylamine sulfate, hydrazinehydrate or hydrazine sulfate, sodium sulfite, dymadon, soybean oil or sunflower oil, hydrate of sodium oxide or potassium and subsequent rectification when the ratio of the alkali reagent (g/DM3ESTS):

resorcinol alkali(2,0-10,0) (1,0-5,0),

urea alkali(1,0-5,0) (0,5-2,5),

hydroxylamine sulfate alkali(1,0-5,0) (0,5-2,5),

the alkali hydrazinehydrate(0,5-2,5) (0,5-2,5),

hydrazine sulfate alkali(0,5-2,5) (0,5-2,5),

sodium sulfite lye(1,0-5,0) (1,0-3,0)

the alkali dimedone(2,0-10,0) (1,0-3,5),

soybean oil lye(2,0-10,0) (1,0-3,5),

sunflower oil lye(2,0-10,0) (1,0-3,5).

Reagent selected from the above range, add these amounts together with the alkali in the untreated ESTs, subjected to boiling for 4 hours and then distilled processed alcohol.

The proposed solution is illustrated by examples of specific performance.

Example 1. In a round bottom glass flask with a capacity of 1.5 liters, equipped with a reverse refrigerator and thermometer, is placed 1 DM3Acts above THE indicators:

mass concentration of acids in terms of acetic acid, mg/DM36,5

the volume fraction of acetaldehyde, 0,52

the volume fraction of crotonic aldehyde, 0,16

the volume fraction of ethyl ether, and 0.8

mass concentration of solids, mg/DM34,5

the volume fraction of polymers of ethylene, no

10 g of resorcinol, 5.0 g of caustic soda, boil the reaction mixture for 4 hours, replace the reflux condenser on Christmas reflux condenser with a length of 25 cm and a downward refrigerator, distilled 10 ml Pradhana that drop, 975 ml of the main fraction is purified acts with the indicators shown in the table. 2. In the flask remains about 25 ml of the cubic residue containing acetic aldehyde-resorcinol the resin oligomers of resorcinol, alkaline condensate crotonic aldehyde and the one hydroxide 3.0 g, potassium manganese acid of 2.0, the Results of the analysis are given in table. 2.

Examples 3 20. In the conditions of example 1, the reactants and their number is listed in the table. 1. The results of the tests cleared ESTs are given in table. 2.

Example 21. In the reactor of stainless steel with a volume of 5 m3fitted with mechanical stirrer, jacketed for heating steam and cooling water, temperature sensors, pressure, upper and lower levels, the pipes for loading, distillation and plum alcohol and VAT residue, heat exchanger and system for collecting Pradhana, the main fraction and VAT residue, download 3750 l ESTs include the stirrer and heating, water flow in the heat exchanger, heating the mass to about 40-50oC and through the loading hatch load 35 kg of resorcinol and 5.0 kg of caustic soda. Hermetically close the hatch reactor and bring the reaction mixture to a boil. The reactor mode "on" works 4 hours.

After 4 hours of boiling in the mode of returning the condensate to the reactor mode ("on") through the sampler will take a sample of the distillate analyzed by chromatograph on the indicators specified in the table. 2. If satisfactory results of the analysis of the reactor is switched to the mode of distillation, which opens the valve of the distillation of alcohol and C is the frame acts. In the reactor remains 150 l VAT residue, which is sent to the tank bottoms and further burning. Cleaned ESTs from collection direct to the consumer.

This demonstrates the practical utility and industrial applicability of the proposed technical solutions.

From the above examples should the possibility of chemical cleaning acts with extreme amounts of impurities in industrial scale.

All reagents used for this purpose are available tonnage industry of Russia.

Quality cleaned ESTs meets the requirements of ethyl alcohol used in the manufacture of aerosol products.

Thus, the use of the reagent of the above number to clear ESTs raw, in contrast to the method according to the prototype, allows you to brush up on alcohol high degree of purification, providing novelty and usefulness of the proposed solutions (inventive step). One of the main advantages of the present invention is maloothodnoj for all types of waste sent less than 7% by weight of the distilled spirits, while when using the cleaning rectification losses are bol the impurities of aldehydes and ketones by treatment with a reagent and a caustic alkali, boiling for 4 h and subsequent partition, characterized in that the reagent is used substances selected from the range: resorcinol, urea, hydroxylamine sulfate, hydrazine hydrate, hydrazine sulfate, sodium sulfite, dymadon, soybean oil, sunflower oil, and as the caustic alkali is caustic soda or caustic potash in the following ratio reagent caustic alkali, g/DM3ethyl alcohol:

resorcinol alkali 2,0 10,0 1,0 5,0;

urea alkali 1,0 5,0 1,0 3,5;

hydroxylamine sulfate alkali 1,0 5,0 0,5 2,5;

hydrazine hydrate alkali 0,5 2,5 0,5 2,5;

hydrazin sulfate alkali 0,5 2,5 0,5 2,5;

sodium sulfite lye 1,0 1,0 3,0 5,0;

dymadon alkali 2,0 10,0 1,0 3,5;

soybean oil alkali 2,0 10,0 1,0 3,5;

sunflower oil alkali 2,0 10,0 1,0 3,5.

 

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1 tbl

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1 tbl, 5 ex

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