RU1596690C - Method of cleaning unsaponifiable matter of synthetic fatty acid production from sodium and manganic salts of organic acids - Google Patents

Abstract

The invention relates to the production of synthetic fatty acids, in particular the purification of non-washed products from Na and Mn organic salts. , 1, acid The goal is to improve the quality of the target product. For this, the feed product is treated with water (at a weight ratio of 1-10: 1) containing sodium sulfate and cepHyjo or cd-acid in an amount of 0.5-5 wt.%, At 75-95 "C in countercurrent extraction These conditions increase the quality of the target product by reducing the content of Na and Mn salts from 0.02-0.025% to 0.004-0.004% with the exception of the formation of emulsions. (/)

Description

FIELD OF THE INVENTION This invention relates to the purification of unsaturated impurities in the production of synthetic fatty acids FFA. obtained by the oxidation of paraffinic hydrocarbons in the presence of atmospheric oxygen and catalysts, to perfection. This method can be used in the production of FFA for cleaning the inaudible production of synthetic fatty acids from sodium and manganese salts of organic acids.

The aim of the invention is to improve the quality of the target product. ..

Example 1 A sample of the unsaponifiable (a mixture of unsaponifiable I and II in a ratio of 2: 1) is taken with the following indicators:

SL

Sodium content

0.050 metal, wt.%

0) 0d

Manganese Content0.025

metapla, wt.% with

Numbers:

0.5

Acidic 10.5

Essential 15.5

Carbonyl

5.5

Iodine 45.0

1 1 hydroxyl

200 g of unsaponifiables of the indicated composition are kept in a thermostated cabinet under static conditions in a heat-resistant glass at. for 24 hours and then analyze the top layer of the unsaponifiable. The following results are obtained. Concerning sodium sodium metal 0, OH manganese metal 0.025 Numbers: Acid1 J 5 Essential t1.2 Carbonyl .17.1 Iodine 5.1 Hydroxyl 4A, 5 From the obtained 1x data, it can be seen that, by simple sedimentation, KonHqectBo indicated manganese salts and Sodium cannot be removed, since they are solidly soluble in the unsaponifiable and cannot be settled by simple sludge. EXAMPLE 2 (according to the prototype. Processing of non-saponifiable quality with the quality, as in example 1, is carried out in counterflow mode using distilled water packed countercurrent column height of 1.5 m and a diameter 0.05 m, equipped with a glass nozzle, at 75-85 ° C. Water with a temperature of 75-95 ° C is continuously pumped through a dispenser through the distributor to the top of the column, and unchanged with the same temperature to the bottom. Glass beads are used as nozzles. The supply of non-saponified in all experiments is constant and amounts to 1 l / h. The water supply is 0.5 l / h. The ratio is unattainable - water is equal to 2: After the unit enters the mode under conditions x continuous operation immediately after cleaning receive unsaponifiable A3 may.% emulsion 57 wt.%, water OdO wt.%. After 2 hours of settling, an unsaponifiable 60 wt.% Is obtained; emulsions 28.5 wt.% and water 11.5 wt.%. The following are characterized by the following indicators: Content, wt.% Sodium metal 0.025 Manganese metal 0.020 Functional numbers: Acid 0.45 Ethereal 9.6 Carbonyl 15.0 Yard 5.2 lS strong 44.0 I From this example it is seen that The treatment of water-immature water, although it allows them to reduce the sodium and manganese content, is at the same time accompanied by the formation of an emulsion that is stable for more than 2 hours. Example 3 (prototype using a solution of water-soluble; acid (NMC). Conducted according to the steps of Rimer 2, but instead of distilled odes take a 10% solution of low molecular weight acids. The ratio of non-washable - water 2: 1. After 2 h, the mixture is divided into 57% non-viable, 25.5% emulsions, 5% aqueous MK solution. Non-essential ones are characterized by the following parameters: Content, wt.%: Sodium-metal 0.020 Manganese-metal 0.020 Numbers; Acid Ether, Carbonyl Iodine Hydroxyl This example shows that the introduction of NMC into a solution for washing slightly improves Example 4. The proposed method with a lower content of ingredients .. Take unreasonable quality, as in example 1, and process them with water containing 0.5% sodium sulfate and sulfuric acid at a ratio of 1: 1. After stopping the movement of the liquid, the mixture is stratified into 55.5% unsoluble and 44.5% solutions. No emulsion forms. Unsaponifiable are characterized by the following indicators: Content, wt.%: Sodium metal 0.005 Manganese metal 0.005 Numbers: Acid 0, 5 Essential 11.0 Carbonyl 15.0 Iodine 5.1 Hydroxyl 43.0 PRI me R 5 (according to the proposed method for average content of ingredients). Conducted according to the conditions of Example 4, but in a ratio of 2: 1 with water, using water containing sodium sulfate and sulfuric acid. No emulsion formation is observed; 71.5% of the unrefinished and 28.6% of the aqueous solution are obtained after separation. The following are indicators: Content, wt.%: Sodium metal - Traces of Manganese metal Traces of Numbers: Acidic 0.6 Ethereal 10.4 Carbonyl 15.6 Iodine 5.5 Hydroxylated 44.5 Example 6 (based on the proposed method with a maximum content of ingredients). The procedure was carried out according to the conditions of Example 4, but with a ratio of unsaponifiable and water of 10: 1 using water containing 5.0 wt.% Sodium sulfate and sulfuric acid. Emulsion formation is not observed; 91% of unsaponifiable and 9% aqueous solution are obtained after separation. Non-washed ones have indicators: Content, May,%: Sodium metal 0.004 Manganese metal 0.005 Numbers: Acid1jO Essential 11.2 Carbonyl16, 0 Iodine5.7 Hydroxylated 46.0 V Example 7 (according to the proposed method with an average content of ing dientes, but with the replacement of sulfuric acid by salt Hyfo acid). Conducted according to the conditions of Example 5, the solution contains 2.5% sodium sulfate and hydrochloric acid each. Emulsion formation is not observed. 71.5% unsaponifiable and 28.5% aqueous solution are obtained. Unsaponifiable are characterized by the following indicators: Content, wt.%: Sodium metal Traces of Manganese metal Traces of Numbers: Acid. 0.7 Ether. 10.6 Carbonyl 14.8 Iodine 5.0 Hydroxyl 45.0 and measure 8 (comparative, according to the proposed method, the lower limit of the content of ingredients). Conducted according to the conditions of example 4, but take 1: 1 aqueous solution containing 0.25 wt.% Sodium sulfate and sulfuric acid. Immediately after the end of the experiment, 51.2% of the unsaponifiable, 22.2% of the emulsion and 26.6% of the aqueous solution are obtained. After 2 hours, 53.5% of the unsaponifiable, 13.5% of the emulsion and 33% of the aqueous solution have. The indelible are characterized with the following indices: Numbers: Acidic Etheric Carbonyl Il.chmop Hydroxyl Content, May, Iatria-metal Manganese-metal PRI me R 9 (comparison, according to the proposed method beyond the upper limit of the content of ingredients). Conducted according to the conditions of example 6, but the content. sodium sulfate and sulfuric acid is about 10% by weight. Immediately after processing, the amount of non-washed is 90.5% and the aqueous solution is 9.5%. The composition of the mixture after 2 hours does not change. The following have the characteristic: Numbers: Acidic 4.5 Ethereal 11.4 Carbonyl 15.9 Iodine 5.2 Hydroxyl 35.1 Content, wt.%: Sodium metal Manganese metal Example 10 (comparison, the importance of introducing sulfuric acid). Conducted according to the conditions of example 5, but sulfuric acid is not introduced. Immediately after processing, they have unreplaceable 51%, emulsions 28.6% and an aqueous solution of 20.4%. After 2 if, an unsaponifiable 63%, an emulsion tl, 4%, an aqueous solution of 25.6% are obtained. Unsaponifiables are characterized by the following indicators: Content, wt.%: Sodium metal Manganese metal Numbers: Acidic Etheric Carbonyl Iodine Hydroxyl Example 11 (comparison, significant sodium sulfate administration). Conducted according to the conditions of Example 5, but sodium sulfate was not added. Immediately after processing, they have at least 60%, emulsions 13.5%, and an aqueous solution 26.5%. After 2 hours, the resulting 65.8%, emulsion 26.5% were obtained. After 2 hours receive Unsaponifiable - 65.8%, emulsions - 8.5%, an aqueous solution of 25.7%, Unsaponifiables have the following contents: Content, May.%: Sodium metal 0.01 Manganese metal 0.01

Numbers

Acid3.5

Essential10.6

Carbonyl 14.5 Iodine

Hydroxyl A5,4 The results obtained are given in the table, from which we can draw the following conclusions.

By simple sludge, it is not possible to free sodium and m & s extract from salts (example 1). By treatment with water according to the prototype, the salt content can be reduced by 20-50% from the original, but an emulsion stand is formed,. which is unacceptable. due to the entrainment of unreasonable sewage (example 2). Adding 10% NMA to the water for treatment (Example 3) allows the content of these salts to be reduced by 20-60%, but an emulsion stand is also formed. When processing unrefined according to the proposed method (examples 47) in the presence of 0.5-5.0% sodium sulfate and sulfuric (hydrochloric) acid, it is possible to remove these salts by 90% or more, up to trace amounts, while the emulsion is not formed completely. Carrying out the treatment of the sulfite and acid contents unsaponifiable beyond the lower boundary (Example 8) sharply worsens the salt washing depth (up to 40-70%) and leads to the appearance of persistent emulsion, which is unacceptable. After the upper content of the ingredients, the washing values (Example 9) do not improve, therefore, from economic considerations, it makes no sense to increase the concentration. centration of sulfate and sulfuric acid in water; and treatment of oxidate with more than 5 wt.%.

If water is removed from the treatment water, it is not necessary to remove sulfuric acid, then the washing quality deteriorates sharply (Example 10), an emulsion stand forms, which is undesirable, and the degree of salt washing is also reduced. This example proves the relevance of introducing mineral acid into water for the treatment of the indelible.

If sodium sulfate is removed from the water for treatment of the unsaponifiable (Example 11), the depth from the salts is significantly reduced compared to the declared ranges of acid and sodium sulfate concentrations, while at the same time an emulsion is formed, albeit in smaller quantities than. Example 10

The proposed method allows to improve the quality of the target product by reducing the content of Na and Mp salts to 0.004-0.005% and traces against 0.02-0.025% in the known method. sobe, and also exclude the formation of persistent emulsions.

Formulas 3.

The method of purification of the unavailable production of synthetic fatty acids from sodium and manganese salts of organic acids by treatment with water in a mass ratio of 1-10: 1, respectively, at a temperature of 7595 ° C in a countercurrent extraction column, characterized in that, in order to improve the quality of the target product, they use water containing sodium sulfate and sulfuric or hydrochloric acid in an amount of 0.5 | 5 wt.%.

Technological CBoRcrva METHOD

"3.0 48.0

100

57.0 "g, O

Oh Oh

0.0 10.0

51.0

60.0

51 g

90.5

P, 5

5S, S and, 5 2c, 6 13.5

22.2 0.0

n, o 0.0 0.0 26.6 28,)

20,4

4.5 28.5 26.5 9.5

 sulfuric tinctures “use the saline knot.

Table continuation