DE2036120A1 - Production of wool wax alcohols and acids - from wool grease - Google Patents

Abstract

Wool grease is saponified with caustic alkali in a co-solvent mixture of isopropanol and water. Wool wax alcohols are extracted from the saponified mixture using hexane or heptane as solvent and the extract is washed first with dilute KOH and then with water. Extraction and washing are best achieved in a continuous countercurrent rotary disc extraction column. The solvent is evaporated from the purified extract to recover the wool wax alcohols. The raffinate is acidified and stripped free of the solvent fraction in a continuous stripper still to recover fatty acids which are water-washed and dried.

Description

Process for the production of wool-paraffin alcohols and wool-paraffin fatty acids The invention relates to the production of wool-paraffin alcohols, oils and wool-paraffin fatty acids and is specifically aimed at the production of these substances from wool fat.

It is already known such alcohols and fatty acids from wool fat to win by saponifying the wool fat, then from the saponified Mass with a solvent extracted the non-saponifiable constituents that Solvent then withdrawn and the solvent from the Extract is evaporated to obtain the unsaponifiable constituents.

The known process for the production of wool-paraffin alcohols by saponifying the wool fat and then extracting the unsaponified Mixing must be carried out under very carefully controlled conditions, to prevent undesired phases and the formation of undesired emulsions. For this and other reasons it is very difficult to be complete or substantial to achieve complete saponification of the wool fat.

The main object of the invention is therefore to provide a method of treatment of wool fat, with the help of which wool-paraffin alcohols and wool-paraffin acids can be separated from it as purely as possible.

This task is subordinated to the goal of a process to complete Saponification of the wool fat to sharp, making it an alcohol with very low Saponification value is obtained.

Another goal is to create such a method with With the help of this, in continuous extraction, wool-paraffin alcohols are obtained can be carried out from saponified wool fat. Next is a method for Extraction of wool-paraffin alcohols from a soap can be created by Soap is obtained from wool fat. Another object of the invention is therein to see a process for obtaining wool fat fatty acids from the raffinate, which results from the extraction of the wool paraffin alcohol from saponified wool fat results.

In the method according to the invention, the wool fat is first with Using an alkaline substance saponified, taking a mixture with isopropyl alcohol and water is generated as a solvent; then the wool paraffin alcohol extracted from the saponified mixture, using heptane or hexane as the solvent is used; then finally the IIeptane-wool-paraffin-alcohol-extract washed out with a solution of sodium hydroxide and then with water, to remove any impurities it contains.

An advantage of this method can be seen that the dilution of the saponified product with a certain amount of isopropyl alcohol and water prevents the emulsification of the system and a good separation of the phases during the subsequent extraction stages allowed.

According to the invention, the extraction step, and, if this is desired, the washing step is best carried out in one go and after Countercurrent rotating disk extraction column carried out. Latter can take the form of the well-known turntable drum or the so-called turbo mixer of General Amerlcan Transpitation Corporation, New York.

By the method according to the invention, wool grease can be removed in a period of time can be saponified in less than twenty-four hours so that it is an alcohol ingredient with a saponification value that is less than 2.0. The extraction of the wool paraffin alcohol from the saponified mixture thereby using heptane as a solvent can be performed with an extraction efficiency of 95 percent when the ratio of the solvent to added substance is 1: 1. Higher ratios of the solvent relative to the substance feed can lead to an even higher extraction efficiency and also lead to a purer product (alcohol and fatty acids).

When saponifying wool fat, sodium hydroxide or potassium hydroxide can be used be used. However, sodium hydroxide is preferred. The amount of used Sodium hydroxide should normally be around 11 to 12 percent of the amount of wool fat (in percent by weight), which are fed to the saponification boiler.

In this boiler suitable stirring devices are available, which chemical reaction between the alkaline substance and the fatty acids in wool fat accelerate.

Complete saponification up to at least 99 percent is essential, if a wool-paraffin alcohol is to be obtained, its saponification value is 2 or is less than 2. It is an advantage of the invention that it provides a satisfactory Process is created to saponify wool fat in a way so that an alcohol component can be obtained with a saponification value of 2 or less It has been shown to use isopropyl alcohol as an additional solvent to water facilitates the saponification process in the process stage of saponifying the wool fat, so that it has become possible to achieve 99 percent saponification in 24 hours at moderate To achieve temperature and atmospheric pressure. In addition, the isopropyl alcohol has an effect also as an additional solvent during the subsequent stages of the extraction and the purification of the wool paraffin alcohol and wool fat fatty acid components.

When carrying out the saponification stage, the mixture of isopropyl alcohol, Water and wool fat are a uniform substance, with sufficient mechanical processing the saponification of wool fat which is difficult to saponify can be up to 95 percent in Six to eight hours can be done and up to 99 percent in twenty-four Hours or less at atmospheric pressure, then a wool paraffin in alcohol which has a saponification value of 2 or less.

The process described here, which is isopopyl alcohol in the saponification step as an additional solvent.

used together with water makes the creation of a wool-paraffin-alcohol ingredient possible with a low saponification value as indicated above.

The amount of isopropyl alcohol used can be around the above to achieve the result mentioned, of about 30 percent dis 50 percent (weight percent) vary based on the weight of the wool fat.

In Table I below are data from several series of experiments indicated, in which the same type of wool fat was always used and this one was saponified according to the invention. In each case, medium to thorough mixing was achieved carried out.

T A B E L L E I attempt solution temp. Treatment pressure saponification value No. mean ° C time (hours) kg / cm2 d. Alcohol 1 50% H2O 104 8 Atmos. 6.7 40% IPA 2 45% H2O 37% IPA 98 21 "1.9 3 40% H2O 115 7-8 1.05-1.4 2.2 4 235% H2O 118-121 24 1.05-1.4 19.6 As can be seen from Table I, the has the test series 2 (21 hours) obtained substance a saponification value of 1.9 and the substance from test series 1 (8 hours) had a saponification value of 6.7. Against it have the substances obtained from test series 4 and 3, for which no isopropyl alcohol was added to the water, saponification values of 2.2 in the case of the test series 3, in which 40 ffi of water and a treatment time of 7 to 8 hours are applied were or 19.6 in the test series 4, in which 235% water during the treatment time has been used for 24 hours. In the test series 3 and 4, a printing device needed.

The saponified wool grease is then mixed with a mixture of isopropyl alcohol and water, thereby preventing emulsification, so that a sharp separation of the phases is possible during the subsequent extraction stage. With a saponified one Mixture of 4,000 kg of lanolin with 455 kg of sodium hydroxide and 1,6o0 kg of isopropyl alcohol and 1,720 kg of water was made, it was made with about 8,000 kg of isopropyl alcohol and 19 800 kg of water diluted. From the above numbers it can be seen that during the saponification about 0.4 parts isopropyl alcohol and approximately 0.43 parts of water to 1 part of lanolin can be used while for diluting of the saponified product to about 2 parts isopropyl alcohol and about 5 parts water 1 part of lanolin can be taken.

The saponified wool fat is then further treated to make the wool paraffin alcohol to extract. The extract and the extracted side (raffinate) are then treated, to pull out the wool paraffin alcohol and the fatty acid component.

According to the invention, the extraction of the wool paraffin alcohol from the soap isopropanol-water mixture carried out continuously through application of hexane or heptane as a solvent. Because hexane is volatile and easily inflammable Is solvent, the less volatile heptane is better used 'that is when performing the extraction as just as suitable as the hexane has proven.

The extraction is preferably carried out in a known, with rotating Disks equipped, carried out in countercurrent operation extraction column. Briefly stated, the flower of the "type" extraction column consists of a number of compartments, which are formed by several stator rings, and are located in each compartment in the middle a turntable, that of the rotating drive shaft will be carried. A detailed description can be found in Chemical Engineering Progress, Vol. 51, No. 3, March 1955, 141.

The extraction of the wool paraffin alcohol from the saponified wool fat mixture takes place in the extraction column in such a way that heptane is added to the lower end of the column will. This then flows upwards against the saponified, which sinks in countercurrent Mixture that is fed to the column at the top. The saponified mixture of Soaps, water, and isopropyl alcohol will get rid of the discs in large numbers small droplets dispersed (in the following in contrast to the homogeneous phase of heptane called the discontinuous phase), where the size of the droplets depends on the speed of rotation of the rotor, which has a very important influence on the extraction conditions Has.

The saponified substance should be adequately treated with isopropyl alcohol and Water should be mixed so that the separation of the phases in the extraction process is easy going on. The concentration of isopropyl alcohol in the soap mixture, Water and isopropyl alcohol added to the extraction column fed should be high enough so that there is as little as possible in the extraction column fixed. Substances can form.

In a special experimental example of the extraction stage, the Solvent (e.g. heptane) of the extraction column in a ratio ltl relative for the supplied solution.

Soaps, water and isopropyl alcohol are added to the wool-paraffin alcohol segregate from this mixture. This corresponds to a ratio of over 5: .t of the solvent heptane to the extracted wool-paraffin alcohol in contrast to Ratios on the order of 80: 1 in the known processes where the extraction is carried out in portions. The temperature s, although the watery one The solution as well as the solvent is kept at: about .55 to 60 degrees, the Temperature in the extraction column to about 38 degrees C or a little above in order to prevent solids from building up in the column. The rotor speed is held at about 30 to 60 revolutions per minute.

With the above method, wool-paraffin alcohol from saponified wool fats with a average extraction efficiency of 95 percent and more can be extracted. The extraction efficiency is determined by separating the extracted raffinate and measuring the amount of extractable Material that has not been extracted by the extraction step. The definite one Extraction efficiency is between about 86.4 percent and 97.7 percent.

The one composed of solvent (heptane) and wool paraffin in alcohol Extract is drawn off at the top of the extraction column and used to remove the Soap ingredients washed, from which the fatty acids are then extracted, such as this is described below. The extract is used for washing Extraction column supplied, in the countercurrent initially a dilute aqueous Solution of potassium hydroxide (about 1% KOH) in aqueous solution) and then Water is added to wash out the potassium hydroxide. ~ This washout of the Extract with an aqueous alkaline solution can be done by adding the solution of the extraction column with rotating disks in the amount of about one digit until one twentieth of the amount of the supplied extract is fed. The rotor speed amounts to about 50 to 60 revolutions per minute.

The effect of this washing treatment on the extract is demonstrated by the following Ash content data of unwashed and washed extract clearly:% Ash unwashed extract 0.81 1400G extract with 200ML 1 percent KOH solution washed 0.02 (then with 100ML 50-50 isopropyl alcohol and water) The washing of the extract with water and then with an alkaline solution has the other Purpose to remove the isopropyl alcohol oil from the extract. This is especially true in the Desirable in view of the possible recovery of isopropyl alcohol. Of the Isopropyl alcohol and the soaps washed out of the extract can be mixed with the in the raffinate obtained in the extraction stage described earlier are combined.

The washed extract of heptane-wool-paraffin-alcohol is then subjected to a treatment in an evaporation unit, which is then subjected to vacuum distillation followed in which the solvent secreted and the wool-paraffin-alcohol part is won. The solvent can be returned to the container from to which it was originally fed to the extraction column.

The quality of the wool-paraffin-alcohol obtained with the process according to the invention is illustrated by the data recorded in Table II, those from experiments obtained: T A B E L L E II water absorption 1300 M.P. (° C) 50-51 saponification value 6.0 hydroxyl value 160 cholesterol 31.8% color (30% CCl @) absorption in a DU 24000 spectrometer .39 abs. At 470 0.13? Abs. At 520 ash 0.7% That Raffinate, i.e. the soap-water-isopropyl alcohol extracted from the solution, the from the wool-paraffin-alcohol part secreted in the extraction stage Mainly from soaps, from fatty acids and some unsaponifiable substances. It It also contains about 4 to 10 percent heptane and 7 to 15 percent isopropyl alcohol. The washed out, which with the help of the alkaline solution and the water from the heptane extract of the saponified wool fat has been washed out, preferably with the raffinate united.

About the solvent and the fatty acids contained in the raffinate are to be obtained, the latter is acidified, e.g. with dilute sulfuric acid, to extract the fatty acids from the soaps contained in the raffinate The mixture from fatty acids and solvents into a continuously operating separation column pumped to recover the solvents (heptane and isopropyl alcohol) and to completely remove them from the raffinate.

The acidification of the raffinate should be carried out so that its pH sufficiently below 7.0 egt. Otherwise a lot of foam would be created during treatment in the separation column to separate the solvents, The use of a continuously operating separation column to recover the Solvent has the further advantage that it produces fatty acids with a good color as there is only a short contact time during the recovery of the solvent is available. The separation column can be a known "rodney-hunt unit".

After separating the solvents, the fatty acids are removed, washed with water and dried.

The properties of the fatty acids obtained in this way are derived from the raffinate represented by the following table.

T A B E L L E III Acid Number 149.0 15% Union Colorimeter Color 3.5-4 Saponification value 170.5 hydroxyl value 58.2 unsaponifiable 7.4% iodine value 10.6 flash point 210 ° C The analysis of the unsaponifiable constituents of the fatty acid content shows that these have a cholesterol value of about 28 percent. This shows that some of the wool-paraffin alcohol has not been extracted but in the raffinate has remained. A fatty acid is obtained by further extraction of the raffinate, which have a saponification value of 178.9 and unsaponifiable constituents of 1.4 percent contains. Another saponification of the Raflnats and subsequent extraction after the process described gives a fatty acid with a saponification value of about 180 and an unsaponifiables content of about 2.6 percent.

Although the value of the unsaponifiable components was 7.4 percent in Table III indicates that wool paraffin alcohol was retained in the raffinate was, then this value agrees with the above-mentioned values of the extraction efficiency which is achievable in practice0 an additional amount of solvent (i.e. a higher ratio) is used in the extraction stage, the amount the unsaponifiable constituents in the fatty acid content are considerably reduced.

Claims (9)

PATENT CLAIMS di Process for the production of wool-paraffin alcohols and wool-paraffin fatty acids, characterized in that wool fat, which is in a mixed solvent of isopropyl alcohol and water is contained'is saponified, the saponified wool fat then becomes a continuous Countercurrent extraction process in a rotating disk extraction column along with introduced a hydrocarbon as a solvent from the group of hexane and heptane that the solvent extract is then in a continuous countercurrent washing process first with a weakly alkaline, aqueous solution and then with water is washed and the solvent is then evaporated from the washed extract, to obtain the wool-paraffin alcohols. 2. The method according to claim 1, characterized in that the solvent, from which the wool-paraffin alcohols are obtained, fed to the extraction stage and is used there as a solvent. 35 Process for the production of wool-paraffin alcohols, thereby characterized in that wool fat initially in a solvent mixture of isopropanol and water saponified, the saponified mass with one from the group consisting of hexane and Heptane selected solvents are treated in a continuous countercurrent process is placed in an extraction column equipped with rotating discs to extract the wool-paraffin alcohol from this mass and that the soapy substances from the 'extract then by treating of the extract in a countercurrent process with a weakly alkaline aqueous solution be washed out. 4. The method according to claim 3, characterized in that the soapy Substances are combined with the raffinate that is produced during solvent extraction the wool-paraffin alcohols -is recovered from the saponified mass. 5. Procedure according to claim 4, characterized in that from the raffinate and the soap-containing Material that is washed out of the extract, fatty acids are obtained. 6. Process for the production of wool-paraffin alcohols, thereby characterized in that wool fat in a solvent mixture of isopropyl alcohol and water is saponified, the saponified mass is subjected to a continuous countercurrent extraction process treated in an extraction column equipped with rotating disks with the aid of heptane is to separate the wool-paraffin-alcohol portion from the saponified mass that the extract of heptane and wool-paraffin alcohol in a continuous countercurrent washing process with a weakly alkaline solution and with water and that heptane from the washed extract portion is evaporated to the representation of the wool-paraffin-alcohol. 7. The method according to claim 6, that the obtained in the extraction process Raffinate from the saponified mass is acidified with a mineral acid and then acidified is subjected to a continuous separation process to recover the solvent and for the representation of the fatty acids. 8. Verrahren according to claim 6, characterized in that the obtained Wool-Paraffin alcohols are subjected to steam distillation. 9. The method according to claim 7, characterized in that the fatty acids are obtained from the raffinate in that the raffinate is diluted with a Acid is acidified to lower its pH well below 7.0, and the Solvent can be distilled therefrom.