The method of purifying ethyl alcohol

 

(57) Abstract:

The invention relates to the alcohol industry, in particular to a method of purification of ethanol from impurities. The method consists of passing ethyl alcohol through a porous sorbent selected from the range of: silicon oxide, aluminum oxide, synthetic zeolite and natural zeolite, activated by the air flow when 350-460oC, then cooled in an atmosphere of inert gas through the resulting alcohol is passed inert gas, then diluted with water and subjected to distillation to remove impurities isopropyl alcohol. Typically, porous sorbent is subjected to regeneration in the stream of inert gas at elevated temperature and in an inert gas applied nitrogen, argon, helium, carbon dioxide or any mixture. The method allows to produce a high quality product. 2 C.p. f-crystals.

The invention relates to the alcohol industry, in particular to develop methods of cleaning with ethyl alcohol to obtain a product of high quality.

Ethyl alcohol is an important product in the production of alcoholic beverages. For food purposes, it is produced usually by distillation brazennose Saharsa, such as potatoes and different types of cereals: rye, wheat, barley, rice, maize. The result is a raw alcohol containing significant impurities of fusel oils. The most important by-products of alcoholic fermentation are acetaldehyde, acetal, glycerol, succinic acid and so-called fusel oil, which is a mixture of butyl and amyl alcohols and their higher homologues. Succinic acid and fusel oils are not formed from sugar, but as a result of a special process of fermentation of amino acids obtained from protein nutrient substrate.

The most common methods of purification of ethanol from impurities are azeotropic, extractive, salt distillation and membrane cleaning methods [C. I. Zverev. The production of high-purity ethanol. Journe. Go active. Chemistry, 1997, so 70, vol. 7, pp. 1154-1158].

Most studies have reported the purification of ethanol relates to the removal of certain impurities, in particular methanol, aldehydes, fusel oils, etc. To remove these impurities most commonly used distillation purification of ethanol at atmospheric pressure. The result is rectified spirits with reduced significantly the number of impurities. The difference 5962-67. Alcohol should be transparent, colorless, without foreign inclusions, taste and smell characteristic of each species produced from the corresponding raw materials, without taste and odor foreign substances.

For the manufacture of vodka uses water-alcohol mixture composed of ethyl alcohol to a certain degree of purification and purified water, with the addition of various ingredients to improve the smell and increasing the range of taste. In the manufacture of vodka use alcohols of different varieties, including low quality.

Currently in the process of purification of ethanol is the purpose of using a more simple and cheap method while maintaining the high quality of the target product.

The most common tool for cleaning from fusel oil is always served fresh charcoal. The latter operates mainly chemically oxidizing alcohols using concentrated in its pores oxygen; alcohols thus turn into acid (aldehydes), which form esters. Of these esters is retained by the coal, the part remains in the purified alcohol, so filtering through charcoal, thinning wkno using a modified and partially activated charcoal from hard wood. Water-alcohol mixture to clean the treated activated carbon. However, the goal of cleaning when this is not achieved, because the oxygen contained in the pores of activated carbon oxidizes methanol, propyl, butyl and amyl alcohols (fusel oil) to harmful aldehydes and esters that remain in the finished product. Despite the decline of various impurities present in the water-alcohol mixture, using this process, bottled vodka can be muddy sediment. The source of this sediment is used activated carbon containing multivalent cations of calcium and magnesium.

A known method of purifying ethyl alcohol by pretreatment of the concentrated ethyl alcohol with sodium borohydride, passing it through activated charcoal and selection of the distilled spirits rectification [RF Patent 2046787, From 07 To 31/08, 27.10.95]. Using this method increases the effectiveness of activated carbon, reduces losses of the target product and allows to obtain ethyl alcohol of high purity, suitable for optical measurements.

A known method of purification of water-ethanol mixtures on activated carbons using CBE is the minimization of the content in vodka unpleasant taste substances due to the formation of so-called clathrate compounds. It is assumed that the clathrate compounds, formed during blending of ethanol with water at high temperatures, capture and unpleasant taste compounds such as acetals and hemiacetals. Once captured in the cavity of clathrates these undesirable compounds are not removed or poorly removed by activated carbon [RF Patent 2107679, From 07 To 31/08, 27.03.98].

Closest to the claimed is a method of using activated carbon as adsorbent [U.S. Patent 5370891, With 12 3/08, 1990]. According to this method, the cleaning process is performed using the transmission of water-alcohol mixture through three layers of activated charcoal at 5-20oC.

The disadvantage of this method is the low efficiency of treatment and the high cost of the ongoing process, as the high selectivity for the target product is achieved by the fact that, as raw materials use of low-quality varieties of alcohol containing substantial amounts of isopropyl alcohol, which cause hard taste on organoleptic properties. In addition, regeneration of activated carbon in such quantities becomes economically not profitable.

All known methods do not is t eat cold.

In the patent GB 2127011, 04.04.1984 described method for separating ethanol from a mixture with organic substances, including higher branched alcohols, branched or cyclic alkanes, aromatic hydrocarbons or ethers by passing the mixture through a molecular sieve. Share the mixture contains up to 20 wt.% ethyl alcohol. This meant that all these connections are bigger than molecules of ethyl alcohol. This is the principle of the separation of mixtures. Molecules of ethanol are held molecular sieve and larger molecules pass through the column and collected in the receiver. Then the ethanol is removed from the molecular sieve by displacement alcohol vapor with an inert gas when heated. This method cannot be applied in the food or medical industry, as extracted from the molecular sieve by displacement with an inert gas while heating the product will be contaminated by impurity substances and must be subjected to a complicated procedure, additional purification. Foreign substances may also appear in the catalytic transformation of chemical compounds that occur at elevated temperatures by heating molecule purification of ethyl alcohol, high quality commercial product.

The problem is solved as a method of purification of ethyl alcohol.

In the reaction column loaded sorbent with a specific surface area of not less than 150 m2/g, selected from a number of: silicon oxide, aluminum oxide, synthetic zeolite, a natural mineral, activated sorbent stream of air for 2-3 hours at 420-460oC, cooled to room temperature in a stream of inert carrier gas (nitrogen, argon, helium or CO2). A mixture of ethyl alcohol from fusel oils are passed through a column of adsorbent in the atmosphere of inert gas. After separation of the initial fraction, alcohol-enriched part of the impurity substances (methyl alcohol, acetaldehyde, ethyl acetate), collect the fraction of pure ethanol before other parts of the impurities (butyl and amyl alcohols) at the outlet of the adsorber. The control in the absence of impurities in the collected liquid is carried out chromatographically. Ethanol is collected in a container through which the inert gas bubbled to push traces of dissolved oxygen. Another part of the impurities (butyl and amyl alcohols and ethers), remaining on the sorbent is removed from the sorbent by wgrywanie in a stream of inert gas at elevated temperatures. The cleaned portion of the alcohol is separated, diluted with water and subjected to distillation to remove isopropyl alcohol. Highlighted in the regeneration of alcohols fusel oils can be used as a flavoring in confectionery industry.

The resulting rectified spirit has a high purity and can be used for medical purposes, and also to produce vodka of the highest quality.

The difference of the proposed method from the method described in patent GB 2127011, is to use a different technique of allocation of ethyl alcohol, based on the different ability of substances to keep a porous solid sorbent by passing the flow of liquid substances through the sorbent.

The invention is illustrated by the following examples.

Example 1.

33,32 g Al2(SO4)39H2O dissolved in 150 ml of water and added with stirring to a solution of 8.0 g of powder SiO2in 40,2 ml of 17.4 M NaOH solution. The obtained gel is subjected to crystallization at a temperature of 180oC for 3 days. The formed precipitate is filtered off, washed with distilled water, dried at 120oC. the resulting powder with a molar otoshiana column. Then activate the flow of air at a temperature of 350oWith 2 hours. Cooled in a stream of inert nitrogen gas. Raw alcohol with the impurity content of fusel oils 5 wt.%, supplied with a bulk velocity of 1.0 h-1is passed through the sorbent at room temperature. After separation of the initial fraction, alcohol-enriched part of the impurity substances (methyl alcohol, acetaldehyde, ethyl acetate), collect the fraction of pure ethanol before other parts of the impurities (butyl and amyl alcohols) at the outlet of the adsorber. The control in the absence of impurities in the collected liquid is carried out chromatographically. Ethanol is collected in a container through which bubbled nitrogen. The sorbent in an adsorption column is subjected to regeneration by heating in a stream of nitrogen at a temperature of 200oC. After separation of the purified part of her alcohol diluted with water in ratio 1:1 and subjected to rectification. The resulting rectified spirit meets the requirements of GOST 5964-82. Output pure fractions of 45 wt.% from the missed volume of crude alcohol.

Example 2.

As sorbent use synthetic zeolite NaA with a molar ratio of SiO2/Al2O3= 2.0 and a specific surface area of 150 m2nd fraction 35 wt.% from the missed volume of crude alcohol, containing 10 wt.% admixtures.

Example 3.

As the adsorbent used is a synthetic zeolite of the type pentasil with a molar ratio of SiO2/Al2O3= 42.0 and a specific surface area of 500 m2/, process Conditions as in example 1, but as the inert gas used is helium. The yield of pure fraction of 65% of the missed volume of crude alcohol containing 5 wt.% admixtures.

Example 4.

As the adsorbent used-Al2ABOUT3with a specific surface area of 180 m2/, process Conditions as in example 1, but as the inert gas used WITH2. Output pure fractions of 15% of the missed volume of crude alcohol containing 10 wt.% admixtures.

Example 5.

As the adsorbent used SIO, SIS2with a specific surface area of 200 m2/, process Conditions as in example 1. Output pure fractions of 55% of the missed volume of crude alcohol containing 7 wt.% admixtures.

Example 6.

As the adsorbent use natural mineral clinoptilolite with a specific surface area of 150 m2/, process Conditions as in example 1, but as the inert gas, a mixture, steriodogenesis.

As can be seen from the examples, the proposed method allows to obtain the product (ethyl alcohol) with high quality, high yield.

1. The method of purification of ethanol from impurities, which consists in the fact that ethanol is passed through a porous sorbent selected from the range of: silicon oxide, aluminum oxide, synthetic zeolite and natural zeolite, activated by the air flow when 350-460oC, then cooled in an atmosphere of inert gas through the resulting alcohol is passed inert gas, then diluted with water and subjected to distillation to remove impurities isopropyl alcohol.

2. The method according to p. 1, characterized in that the porous sorbent is subjected to regeneration in the stream of inert gas at elevated temperature.

3. The method according to PP. 1 and 2, characterized in that as the inert gas used nitrogen, argon, helium, carbon dioxide or any mixture.

 

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