CN112831656B - Regeneration method of naphthenic acid extraction organic phase - Google Patents
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Abstract
The invention discloses a method for regenerating naphthenic acid extraction organic phase, which comprises the steps of firstly taking aged naphthenic acid and adding sulfonated kerosene, then adding hydrochloric acid solution to react for 2-60 min, separating to obtain organic phase, and then adding pure water to the organic phase to wash the organic phase to be close to neutrality; then, carrying out reduced pressure distillation on the organic phase at the temperature of 80-400 ℃ and the pressure of 5-100000 Pa, and continuously adding a naphthenic acid regenerant at a constant speed under the stirring condition in the whole reduced pressure distillation process, wherein the total volume of the added naphthenic acid regenerant is 5-50% of the volume of the organic phase; then the gas phase obtained by reduced pressure distillation is treated by a multi-stage condenser to obtain condensate, namely the regenerated naphthenic acid, wherein the exhaust temperature of the multi-stage condenser is 20-80 ℃. The invention is a simple and effective method for regenerating naphthenic acid extraction organic phase, which solves the problem of poor regeneration effect of the existing aged naphthenic acid.
Description
Technical Field
The invention belongs to the technical field of extraction solvent regeneration, and particularly relates to a regeneration method of an organic phase extracted from naphthenic acid.
Background
Rare earth metals (rare earth metals), also called rare earth elements or rare metals, are the general names of 17 elements of scandium, yttrium and lanthanide series in IIIB group of the periodic Table of elements, and are usually represented by R or RE. Rare earth metals have extremely important applications and are important components of modern high-tech new materials. A series of compound semiconductors composed of rare earth metals and nonferrous metals, electro-optical materials, special alloys, novel functional materials, organic metal compounds, etc. all require the use of rare earth metals with unique properties. Rare earth metals have been widely used in contemporary communication technologies, electronic computers, space development, medical and health, photosensitive materials, photoelectric materials, energy materials, catalyst materials, and the like.
At present, rare earth leachate is obtained from rare earth-containing mines by adopting an in-situ leaching method for rare earth metal preparation, and then rare earth metal is obtained by separating and extracting the rare earth leachate from a rare earth-containing mine by adopting an extraction solvent, wherein naphthenic acid is widely used in a rare earth extraction process as a special-effect extractant for separating rare earth yttrium, but the naphthenic acid organic phase is recycled for a long time, and is inevitably subjected to reactions and changes such as esterification and oxidation gradually to generate an aging phenomenon, so that the acid value is rapidly reduced, the phase separation time is prolonged, the extraction separation performance is reduced, and the use value is gradually lost. From the appearance of the organic phase, the aging process of the naphthenic acid organic phase is a change process from the transparency to the turbidity, the color to the dark brown. Generally, naphthenic acid is removed from an organic phase, and the organic phase is replaced with new naphthenic acid or most of the naphthenic acid is replaced, so that the normal separation performance can be recovered, the old replaced organic phase is difficult to dispose, and with the change of a petroleum refining process, the petroleum refining process does not produce the naphthenic acid as a byproduct, the supply of the naphthenic acid is reduced, and the replacement cost is increased, so that the technical personnel in the field try to regenerate the aged naphthenic acid organic phase by various chemical reagents and technical means, but still do not obtain a simple and effective regeneration method.
Disclosure of Invention
Aiming at the defects, the invention discloses a simple and effective method for regenerating naphthenic acid extraction organic phase, which solves the problem of poor regeneration effect of the existing aged naphthenic acid.
The invention is realized by adopting the following technical scheme:
a method for regenerating naphthenic acid extraction organic phase comprises the following steps:
(1) Taking aged naphthenic acid, adding sulfonated kerosene, then adding a hydrochloric acid solution to react for 2-60 min, separating to obtain an organic phase, and then adding pure water into the organic phase to wash the organic phase to be nearly neutral; the volume ratio of the aged naphthenic acid to the hydrochloric acid solution is (1 to 10) to 1;
(2) Carrying out reduced pressure distillation on the organic phase obtained by the treatment in the step (1) under the conditions that the temperature is 80-400 ℃ and the pressure is 5-100000 Pa, continuously adding a naphthenic acid regenerant at a constant speed under the stirring condition in the whole reduced pressure distillation process, wherein the total volume of the added naphthenic acid regenerant is 5-50% of the volume of the organic phase, and the naphthenic acid regenerant is obtained by mixing pure water and fresh naphthenic acid according to the volume ratio of (1-100) to 1;
(3) And (3) passing the gas phase obtained by reduced pressure distillation in the step (2) through a multi-stage condenser to obtain condensate, namely the regenerated naphthenic acid, wherein the exhaust temperature of the multi-stage condenser is 20-80 ℃.
The gas phase obtained by reduced pressure distillation is subjected to heat exchange with cooling water in a multistage condenser and then condensed to obtain regenerated naphthenic acid, the higher the using amount of the cooling water is, the lower the condensing temperature is, so that the naphthenic acid can be completely condensed and recovered, meanwhile, the temperature of non-condensable gas can also be reduced, the naphthenic acid contained in the non-condensable gas is reduced, the exhaust temperature of the multistage condenser is the temperature of the non-condensable gas, if the temperature is higher than 80 ℃, a large amount of naphthenic acid is carried in the non-condensable gas, the loss of the naphthenic acid is caused, the recovery rate of the regenerated naphthenic acid is low, the using amount of the cooling water is increased, and the condensing temperature is increased; if the exhaust temperature of the multi-stage condenser is less than 20 ℃, although the condensing temperature is low, the recovery rate of the regenerated naphthenic acid is high, the consumption of cooling water is large, the cost is high, and the realization is difficult.
Furthermore, the adding volume of the sulfonated kerosene in the step (1) is 5-20% of the volume of the aged naphthenic acid. The addition of sulfonated kerosene can increase the fluidity of aged naphthenic acid, but the addition of excessive sulfonated kerosene can dilute naphthenic acid, so that the acid value of the obtained regenerated naphthenic acid is greatly reduced, and the extraction effect of the naphthenic acid is influenced.
Further, the mass fraction of the hydrochloric acid solution in the step (1) is 10-30%.
Further, pure water is added to the organic phase in the step (1) to wash the pH value to 6 to 7.
Further, the stirring speed in the step (2) is 5-50 r/min. The stirring speed is controlled to ensure that the organic phase is heated uniformly, the distillation speed is accelerated, the naphthenic acid is promoted to be distilled completely, and the reduced pressure distillation efficiency is improved.
Compared with the prior art, the technical scheme has the following beneficial effects:
1. the invention adds hydrochloric acid into the aging naphthenic acid to react, removes metal and nonmetal impurities in the aging naphthenic acid, adds quantitative sulfonated kerosene into the aging naphthenic acid to increase the fluidity of the aging naphthenic acid, enlarges the density difference of a water phase and an organic phase to be beneficial to the separation of the two phases, promotes the hydrochloric acid to remove the impurities in the aging naphthenic acid, controls the dosage of the sulfonated kerosene simultaneously, prevents the aging naphthenic acid system from emulsifying, thereby causing phase splitting difficulty; then the organic phase after impurity removal is distilled under reduced pressure, and a small amount of regenerant prepared from pure water and fresh naphthenic acid is added in the distillation process to induce the ineffective naphthenic acid to be converted into effective naphthenic acid, thereby improving the regeneration efficiency of the aged naphthenic acid.
2. The invention has simple process, strong operability and low regeneration cost of the naphthenic acid, the regenerated naphthenic acid is changed from the original turbid and lightproof black color to semitransparent dark cyan, the color of the regenerated naphthenic acid is similar to that of the new naphthenic acid, the acid value is improved to about 0.77 from 0.42, the extraction performance of the regenerated naphthenic acid is close to that of the fresh naphthenic acid, and the problem of poor regeneration effect of the existing aged naphthenic acid is solved.
Detailed Description
The invention is further illustrated by the following examples, which are not to be construed as limiting the invention thereto. The specific experimental conditions and methods not indicated in the following examples are generally conventional means well known to those skilled in the art.
Example 1:
a method for regenerating naphthenic acid extraction organic phase comprises the following steps:
(1) Taking aged naphthenic acid and adding sulfonated kerosene, wherein the adding volume of the sulfonated kerosene is 5% of that of the aged naphthenic acid, then adding 10% by mass of hydrochloric acid solution for reacting for 30min, separating to obtain an organic phase, and then adding pure water into the organic phase to wash the pH value to 5; the volume ratio of the aged naphthenic acid to the hydrochloric acid solution is 10;
(2) Carrying out reduced pressure distillation on the organic phase obtained by the treatment in the step (1) under the conditions that the temperature is 300 ℃ and the pressure is 500Pa, and continuously adding a naphthenic acid regenerant at a constant speed under the stirring condition of 10r/min in the whole reduced pressure distillation process, wherein the total volume of the added naphthenic acid regenerant is 5% of the volume of the organic phase, and the naphthenic acid regenerant is obtained by mixing pure water and fresh naphthenic acid according to the volume ratio of 1;
(3) And (3) passing the gas phase obtained by reduced pressure distillation in the step (2) through a multi-stage condenser to obtain condensate, namely the regenerated naphthenic acid, wherein the exhaust temperature of the multi-stage condenser is 40 ℃.
Example 2:
a method for regenerating naphthenic acid extraction organic phase comprises the following steps:
(1) Taking aged naphthenic acid and adding sulfonated kerosene, wherein the volume of the sulfonated kerosene is 15% of the volume of the aged naphthenic acid, then adding a hydrochloric acid solution with the mass fraction of 30% for reacting for 60min, separating to obtain an organic phase, and then adding pure water into the organic phase to wash the pH value to 6.5; the volume ratio of the aged naphthenic acid to the hydrochloric acid solution is 1;
(2) Carrying out reduced pressure distillation on the organic phase obtained by the treatment in the step (1) under the conditions that the temperature is 400 ℃ and the pressure is 100000Pa, and continuously adding a naphthenic acid regenerant at a constant speed under the stirring condition of 20r/min in the whole reduced pressure distillation process, wherein the total volume of the added naphthenic acid regenerant is 30% of the volume of the organic phase, and the naphthenic acid regenerant is obtained by mixing pure water and fresh naphthenic acid according to the volume ratio of 50;
(3) And (3) passing the gas phase obtained by reduced pressure distillation in the step (2) through a multi-stage condenser to obtain condensate, namely the regenerated naphthenic acid, wherein the exhaust temperature of the multi-stage condenser is 80 ℃.
Example 3:
a method for regenerating naphthenic acid extraction organic phase comprises the following steps:
(1) Taking aged naphthenic acid and adding sulfonated kerosene, wherein the adding volume of the sulfonated kerosene is 10% of that of the aged naphthenic acid, then adding hydrochloric acid solution with the mass fraction of 25% for reacting for 2min, separating to obtain an organic phase, and then adding pure water into the organic phase to wash the pH value to 7; the volume ratio of the aged naphthenic acid to the hydrochloric acid solution is 2;
(2) Carrying out reduced pressure distillation on the organic phase obtained by the treatment in the step (1) under the conditions that the temperature is 80 ℃ and the pressure is 5Pa, and continuously adding a naphthenic acid regenerant at a constant speed under the stirring condition of 5r/min in the whole reduced pressure distillation process, wherein the total volume of the added naphthenic acid regenerant is 50% of the volume of the organic phase, and the naphthenic acid regenerant is obtained by mixing pure water and fresh naphthenic acid according to the volume ratio of 100;
(3) And (3) passing the gas phase obtained by reduced pressure distillation in the step (2) through a multi-stage condenser to obtain condensate, namely the regenerated naphthenic acid, wherein the exhaust temperature of the multi-stage condenser is 30 ℃.
Example 4:
a method for regenerating naphthenic acid extraction organic phase comprises the following steps:
(1) Taking aged naphthenic acid and adding sulfonated kerosene, wherein the volume of the sulfonated kerosene is 8% of the volume of the aged naphthenic acid, then adding 20% hydrochloric acid solution by mass fraction for reacting for 45min, separating to obtain an organic phase, and then adding pure water into the organic phase to wash the pH value to 6.5; the volume ratio of the aged naphthenic acid to the hydrochloric acid solution is 3;
(2) Carrying out reduced pressure distillation on the organic phase obtained by the treatment in the step (1) under the conditions that the temperature is 250 ℃ and the pressure is 500Pa, and continuously adding a naphthenic acid regenerant at a constant speed under the stirring condition of 20r/min in the whole reduced pressure distillation process, wherein the total volume of the added naphthenic acid regenerant is 10% of the volume of the organic phase, and the naphthenic acid regenerant is obtained by mixing pure water and fresh naphthenic acid according to the volume ratio of 50;
(3) And (3) subjecting the gas phase obtained by reduced pressure distillation in the step (2) to a multi-stage condenser to obtain condensate, namely the regenerated naphthenic acid, wherein the exhaust temperature of the multi-stage condenser is 40 ℃.
Example 5:
a method for regenerating naphthenic acid extraction organic phase comprises the following steps:
(1) Taking aged naphthenic acid and adding sulfonated kerosene, wherein the volume of the sulfonated kerosene is 5% of the volume of the aged naphthenic acid, then adding 15% by mass of hydrochloric acid solution for reacting for 60min, separating to obtain an organic phase, and then adding pure water into the organic phase to wash the pH value to 7; the volume ratio of the aged naphthenic acid to the hydrochloric acid solution is 1;
(2) Carrying out reduced pressure distillation on the organic phase obtained by the treatment in the step (1) under the conditions that the temperature is 300 ℃ and the pressure is 50Pa, and continuously adding a naphthenic acid regenerant at a constant speed under the stirring condition of 5r/min in the whole reduced pressure distillation process, wherein the total volume of the added naphthenic acid regenerant is 5% of the volume of the organic phase, and the naphthenic acid regenerant is obtained by mixing pure water and fresh naphthenic acid according to the volume ratio of 100;
(3) And (3) subjecting the gas phase obtained by reduced pressure distillation in the step (2) to a multi-stage condenser to obtain condensate, namely the regenerated naphthenic acid, wherein the exhaust temperature of the multi-stage condenser is 20 ℃.
Example 6:
a method for regenerating naphthenic acid extraction organic phase comprises the following steps:
(1) Taking aged naphthenic acid and adding sulfonated kerosene, wherein the volume of the sulfonated kerosene is 10% of the volume of the aged naphthenic acid, then adding 10% by mass of hydrochloric acid solution for reaction for 30min, separating to obtain an organic phase, and then adding pure water into the organic phase to wash the pH value to 6; the volume ratio of the aged naphthenic acid to the hydrochloric acid solution is 4;
(2) Carrying out reduced pressure distillation on the organic phase obtained by the treatment in the step (1) under the conditions that the temperature is 200 ℃ and the pressure is 5Pa, and continuously and uniformly adding a naphthenic acid regenerant under the stirring condition of 15r/min in the whole reduced pressure distillation process, wherein the total volume of the added naphthenic acid regenerant is 15% of the volume of the organic phase, and the naphthenic acid regenerant is obtained by mixing pure water and fresh naphthenic acid according to the volume ratio of 30;
(3) And (3) passing the gas phase obtained by reduced pressure distillation in the step (2) through a multi-stage condenser to obtain condensate, namely the regenerated naphthenic acid, wherein the exhaust temperature of the multi-stage condenser is 60 ℃.
Example 7:
a method for regenerating naphthenic acid extraction organic phase comprises the following steps:
(1) Taking aged naphthenic acid and adding sulfonated kerosene, wherein the volume of the sulfonated kerosene is 12% of the volume of the aged naphthenic acid, then adding a hydrochloric acid solution with the mass fraction of 30% for reaction for 2min, separating to obtain an organic phase, and then adding pure water into the organic phase to wash the pH value to 6; the volume ratio of the aged naphthenic acid to the hydrochloric acid solution is 6;
(2) Carrying out reduced pressure distillation on the organic phase obtained by the treatment in the step (1) under the conditions that the temperature is 400 ℃ and the pressure is 2000Pa, and continuously and uniformly adding a naphthenic acid regenerant under the stirring condition of 50r/min in the whole reduced pressure distillation process, wherein the total volume of the added naphthenic acid regenerant is 20% of the volume of the organic phase, and the naphthenic acid regenerant is obtained by mixing pure water and fresh naphthenic acid according to the volume ratio of 60;
(3) And (3) passing the gas phase obtained by reduced pressure distillation in the step (2) through a multi-stage condenser to obtain condensate, namely the regenerated naphthenic acid, wherein the exhaust temperature of the multi-stage condenser is 70 ℃.
Example 8:
a method for regenerating naphthenic acid extraction organic phase comprises the following steps:
(1) Taking aged naphthenic acid and adding sulfonated kerosene, wherein the adding volume of the sulfonated kerosene is 15% of that of the aged naphthenic acid, then adding 25% by mass of hydrochloric acid solution for reacting for 25min, separating to obtain an organic phase, and then adding pure water into the organic phase to wash the pH value to 7.5; the volume ratio of the aged naphthenic acid to the hydrochloric acid solution is 8;
(2) Carrying out reduced pressure distillation on the organic phase obtained by the treatment in the step (1) under the conditions that the temperature is 80 ℃ and the pressure is 100000Pa, and continuously and uniformly adding a naphthenic acid regenerant under the stirring condition of 40r/min in the whole reduced pressure distillation process, wherein the total volume of the added naphthenic acid regenerant is 30% of the volume of the organic phase, and the naphthenic acid regenerant is obtained by mixing pure water and fresh naphthenic acid according to the volume ratio of 80;
(3) And (3) subjecting the gas phase obtained by reduced pressure distillation in the step (2) to a multi-stage condenser to obtain condensate, namely the regenerated naphthenic acid, wherein the exhaust temperature of the multi-stage condenser is 50 ℃.
Example 9:
a method for regenerating naphthenic acid extraction organic phase comprises the following steps:
(1) Taking aged naphthenic acid and adding sulfonated kerosene, wherein the addition volume of the sulfonated kerosene is 20% of the volume of the aged naphthenic acid, then adding 20% by mass of hydrochloric acid solution for reacting for 15min, separating to obtain an organic phase, and then adding pure water into the organic phase to wash the pH value to 4.5; the volume ratio of the aged naphthenic acid to the hydrochloric acid solution is 10;
(2) Carrying out reduced pressure distillation on the organic phase obtained by the treatment in the step (1) under the conditions of temperature of 100 ℃ and pressure of 5000Pa, and continuously adding a naphthenic acid regenerant at a constant speed under the stirring condition of 25r/min in the whole reduced pressure distillation process, wherein the total volume of the added naphthenic acid regenerant is 5% of the volume of the organic phase, and the naphthenic acid regenerant is obtained by mixing pure water and fresh naphthenic acid according to the volume ratio of 1;
(3) And (3) passing the gas phase obtained by reduced pressure distillation in the step (2) through a multi-stage condenser to obtain condensate, namely the regenerated naphthenic acid, wherein the exhaust temperature of the multi-stage condenser is 30 ℃.
Comparative example 1:
a method for regenerating naphthenic acid extraction organic phase comprises the following steps:
(1) Taking aged naphthenic acid and adding sulfonated kerosene, wherein the volume of the sulfonated kerosene is 10% of the volume of the aged naphthenic acid, then adding 25% by mass of hydrochloric acid solution to react for 60min, separating to obtain an organic phase, and then adding pure water into the organic phase to wash the pH value to 6.5; the volume ratio of the aged naphthenic acid to the hydrochloric acid solution is 10;
(2) Carrying out reduced pressure distillation on the organic phase obtained by the treatment in the step (1) under the conditions of the temperature of 200 ℃ and the pressure of 500 Pa;
(3) And (3) subjecting the gas phase obtained by reduced pressure distillation in the step (2) to a multi-stage condenser to obtain condensate, namely the regenerated naphthenic acid, wherein the exhaust temperature of the multi-stage condenser is 60 ℃.
Comparative example 2:
a method for regenerating naphthenic acid extraction organic phase comprises the following steps:
(1) Taking aged naphthenic acid and adding sulfonated kerosene, wherein the adding volume of the sulfonated kerosene is 25% of the volume of the aged naphthenic acid, then adding 20% hydrochloric acid solution by mass fraction for reacting for 45min, separating to obtain an organic phase, and then adding pure water into the organic phase to wash the pH value to 6.5; the volume ratio of the aged naphthenic acid to the hydrochloric acid solution is 3;
(2) Carrying out reduced pressure distillation on the organic phase obtained by the treatment in the step (1) under the conditions that the temperature is 250 ℃ and the pressure is 500Pa, and continuously and uniformly adding a naphthenic acid regenerant under the stirring condition of 20r/min in the whole reduced pressure distillation process, wherein the total volume of the added naphthenic acid regenerant is 10% of the volume of the organic phase, and the naphthenic acid regenerant is obtained by mixing pure water and fresh naphthenic acid according to the volume ratio of 50;
(3) And (3) subjecting the gas phase obtained by reduced pressure distillation in the step (2) to a multi-stage condenser to obtain condensate, namely the regenerated naphthenic acid, wherein the exhaust temperature of the multi-stage condenser is 40 ℃.
Comparative example 3:
a method for regenerating naphthenic acid extraction organic phase comprises the following steps:
(1) Taking aged naphthenic acid and adding sulfonated kerosene, wherein the volume of the sulfonated kerosene is 30% of the volume of the aged naphthenic acid, then adding 20% hydrochloric acid solution by mass fraction for reacting for 45min, separating to obtain an organic phase, and then adding pure water into the organic phase to wash the pH value to 6.5; the volume ratio of the aged naphthenic acid to the hydrochloric acid solution is 3;
(2) Carrying out reduced pressure distillation on the organic phase obtained by the treatment in the step (1) under the conditions that the temperature is 250 ℃ and the pressure is 500Pa, and continuously and uniformly adding a naphthenic acid regenerant under the stirring condition of 20r/min in the whole reduced pressure distillation process, wherein the total volume of the added naphthenic acid regenerant is 10% of the volume of the organic phase, and the naphthenic acid regenerant is obtained by mixing pure water and fresh naphthenic acid according to the volume ratio of 50;
(3) And (3) passing the gas phase obtained by reduced pressure distillation in the step (2) through a multi-stage condenser to obtain condensate, namely the regenerated naphthenic acid, wherein the exhaust temperature of the multi-stage condenser is 40 ℃.
Experimental example 1:
the regeneration of aged naphthenic acid, which was cloudy and opaque black and had an acid value of 0.42, was carried out according to the methods described in examples 1 to 9 and comparative examples 1 to 4, and the color of the regenerated naphthenic acid obtained was observed and the acid value of the regenerated naphthenic acid was measured, and the specific results are shown in table 1.
TABLE 1 color and acid number of naphthenic acids regenerated
The difference between the comparative example 1 and the method for regenerating aged naphthenic acid is that no regenerant is added in the reduced pressure distillation process, and the data in table 1 shows that although the color of the regenerated naphthenic acid is obviously changed, the acid value of the regenerated naphthenic acid obtained by the method in the comparative example 1 is improved in a small range, and the quality of the regenerated naphthenic acid is not obviously improved, while the acid value of the regenerated naphthenic acid obtained by the method in the invention is obviously improved, and the quality of the regenerated naphthenic acid is effectively improved. Meanwhile, the difference between the comparative example 2 and the comparative example 3 and the method of the present invention is that excessive sulfonated kerosene is added into the aged naphthenic acid, so that the acid value of the regenerated naphthenic acid is lower than that of the regenerated naphthenic acid obtained by the present invention, and the effect obtained by the present invention can not be achieved.
Experimental example 2:
the aged naphthenic acid, the regenerated naphthenic acid treated according to the methods described in examples 1 to 9, and the freshly prepared naphthenic acid (acid value 0.6) were used as extractants for testing, the extractants were added with liquid caustic soda to saponify to 0.3 degree, the yttrium-rich feed liquid with a rare earth ion concentration of 0.5mol/L was mixed with an isovolumetric extractant at 25 ℃ for 15min, and the mixture was allowed to stand and centrifugally phase-split, the extracted aqueous phase was retained, the extractant was further added with hydrochloric acid with a concentration of 6mol/L and mixed for 15min according to the following ratio (extractant: hydrochloric acid = 4) to perform back extraction, and the back-extracted aqueous phase and the aforementioned extracted aqueous phase were analyzed for rare earth components using ICP, and then the separation coefficient β of the extractant was calculated, the specific results are shown in table 2.
TABLE 2 separation coefficient results for each extractant
The data in table 2 show that the extraction performance of the regenerated naphthenic acid obtained by the method of the invention is not much different from that of the freshly prepared naphthenic acid, and is obviously improved compared with the extraction performance of the aged naphthenic acid, which indicates that the regeneration effect of the aged naphthenic acid is good by adopting the method of the invention, the cyclic utilization of the naphthenic acid is realized, the use of the fresh naphthenic acid is reduced, and the production cost is reduced.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (2)
1. A method for regenerating naphthenic acid extraction organic phase is characterized in that: the method comprises the following steps:
(1) Taking aged naphthenic acid and adding sulfonated kerosene, wherein the adding volume of the sulfonated kerosene is 5-20% of the volume of the aged naphthenic acid, then adding a hydrochloric acid solution to react for 2-60 min, separating to obtain an organic phase, and then adding pure water into the organic phase to wash the pH value to 6-7; the volume ratio of the aged naphthenic acid to the hydrochloric acid solution is (1-10) to 1; the mass fraction of the hydrochloric acid solution is 10-30%;
(2) Carrying out reduced pressure distillation on the organic phase obtained by the treatment in the step (1) under the conditions that the temperature is 80-400 ℃ and the pressure is 5-100000 Pa, continuously adding a naphthenic acid regenerant at a constant speed under the stirring condition in the whole reduced pressure distillation process, wherein the total volume of the added naphthenic acid regenerant is 5-50% of the volume of the organic phase, and the naphthenic acid regenerant is obtained by mixing pure water and fresh naphthenic acid according to the volume ratio of (1-100) to 1;
(3) And (3) passing the gas phase obtained by reduced pressure distillation in the step (2) through a multi-stage condenser to obtain condensate, namely the regenerated naphthenic acid, wherein the exhaust temperature of the multi-stage condenser is 20-80 ℃.
2. The method for regenerating the naphthenic acid extraction organic phase according to claim 1, wherein the method comprises the following steps: the stirring speed in the step (2) is 5-50 r/min.
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| CN104862478A (en) * | 2015-05-13 | 2015-08-26 | 广州市吉池环保科技有限公司 | Regeneration method of waste extraction agent for alkaline solution copper extraction and application thereof |
| CN105200234A (en) * | 2015-09-21 | 2015-12-30 | 南昌航空大学 | Regeneration method of aged naphthenic acid organic phase |
| CN106282558A (en) * | 2016-08-28 | 2017-01-04 | 中铝广西有色金源稀土有限公司 | A kind of processing method of organic extractant |
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| CN104862478A (en) * | 2015-05-13 | 2015-08-26 | 广州市吉池环保科技有限公司 | Regeneration method of waste extraction agent for alkaline solution copper extraction and application thereof |
| CN105200234A (en) * | 2015-09-21 | 2015-12-30 | 南昌航空大学 | Regeneration method of aged naphthenic acid organic phase |
| CN106282558A (en) * | 2016-08-28 | 2017-01-04 | 中铝广西有色金源稀土有限公司 | A kind of processing method of organic extractant |
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