CN117959760A - Regeneration method of waste mineral oil extractant - Google Patents
Regeneration method of waste mineral oil extractant Download PDFInfo
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- CN117959760A CN117959760A CN202211312492.9A CN202211312492A CN117959760A CN 117959760 A CN117959760 A CN 117959760A CN 202211312492 A CN202211312492 A CN 202211312492A CN 117959760 A CN117959760 A CN 117959760A
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- mineral oil
- extractant
- oil extractant
- waste mineral
- water
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- 239000002480 mineral oil Substances 0.000 title claims abstract description 120
- 235000010446 mineral oil Nutrition 0.000 title claims abstract description 120
- 239000002699 waste material Substances 0.000 title claims abstract description 87
- 238000011069 regeneration method Methods 0.000 title abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 59
- 238000000034 method Methods 0.000 claims abstract description 46
- 239000012535 impurity Substances 0.000 claims abstract description 44
- 239000007788 liquid Substances 0.000 claims abstract description 22
- 239000000203 mixture Substances 0.000 claims abstract description 19
- 238000000998 batch distillation Methods 0.000 claims abstract description 14
- 230000001172 regenerating effect Effects 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 238000010992 reflux Methods 0.000 claims description 34
- 238000004821 distillation Methods 0.000 claims description 25
- CRSBERNSMYQZNG-UHFFFAOYSA-N 1-dodecene Chemical compound CCCCCCCCCCC=C CRSBERNSMYQZNG-UHFFFAOYSA-N 0.000 claims description 24
- BWDBEAQIHAEVLV-UHFFFAOYSA-N 6-methylheptan-1-ol Chemical compound CC(C)CCCCCO BWDBEAQIHAEVLV-UHFFFAOYSA-N 0.000 claims description 24
- KWOLFJPFCHCOCG-UHFFFAOYSA-N Acetophenone Chemical compound CC(=O)C1=CC=CC=C1 KWOLFJPFCHCOCG-UHFFFAOYSA-N 0.000 claims description 24
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 claims description 24
- KBPLFHHGFOOTCA-UHFFFAOYSA-N caprylic alcohol Natural products CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 claims description 24
- 239000012530 fluid Substances 0.000 claims description 17
- 238000000605 extraction Methods 0.000 claims description 14
- RWNUSVWFHDHRCJ-UHFFFAOYSA-N 1-butoxypropan-2-ol Chemical compound CCCCOCC(C)O RWNUSVWFHDHRCJ-UHFFFAOYSA-N 0.000 claims description 12
- WVYWICLMDOOCFB-UHFFFAOYSA-N 4-methyl-2-pentanol Chemical compound CC(C)CC(C)O WVYWICLMDOOCFB-UHFFFAOYSA-N 0.000 claims description 12
- KFARNLMRENFOHE-UHFFFAOYSA-N 5-methylheptan-1-ol Chemical compound CCC(C)CCCCO KFARNLMRENFOHE-UHFFFAOYSA-N 0.000 claims description 12
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-dimethylformamide Substances CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 12
- 229940069096 dodecene Drugs 0.000 claims description 12
- 238000007670 refining Methods 0.000 claims description 12
- TVMXDCGIABBOFY-UHFFFAOYSA-N n-Octanol Natural products CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims description 11
- 239000000126 substance Substances 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 5
- 238000004891 communication Methods 0.000 claims description 2
- 238000009835 boiling Methods 0.000 abstract description 8
- 230000008929 regeneration Effects 0.000 abstract description 6
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 18
- 238000011084 recovery Methods 0.000 description 15
- 239000000463 material Substances 0.000 description 6
- 230000001276 controlling effect Effects 0.000 description 5
- 239000004480 active ingredient Substances 0.000 description 4
- 239000003921 oil Substances 0.000 description 4
- 239000002199 base oil Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000000638 solvent extraction Methods 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 1
- 230000014509 gene expression Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000013517 stratification Methods 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/74—Recovery of fats, fatty oils, fatty acids or other fatty substances, e.g. lanolin or waxes
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- Extraction Or Liquid Replacement (AREA)
Abstract
The invention provides a method for regenerating a spent mineral oil extractant after use, comprising the steps of: (1) Mixing the used waste mineral oil extractant with water to obtain a mixture, wherein the effective components of the used waste mineral oil extractant are selected from one or two of NMP and DMF; (2) Fully stirring the mixture in the step (1), standing the mixture for layering, retaining the lower layer liquid, and discarding the upper layer liquid; (3) And (3) carrying out negative pressure batch distillation on the lower liquid in the step (2) to remove moisture and impurities in the liquid, thereby obtaining the regenerated waste mineral oil extractant. The invention can effectively remove impurity components which are contaminated by the waste mineral oil extractant and have the boiling point close to or azeotropy with the effective components after long-time use, and can realize the regeneration of the ineffective extractant to the greatest extent.
Description
Technical Field
The invention belongs to the field of waste mineral oil extractants, and particularly relates to a regeneration method of a waste mineral oil extractant.
Background
The waste mineral oil is the mineral oil which is changed when the original physical and chemical properties are changed and the waste mineral oil can not be used continuously due to the effects of impurity pollution, water absorption, oxidation, heat and the like. The current method of treating waste mineral oil is mainly reduced pressure distillation. The distilled waste mineral oil component can not directly reach the application standard of the base oil and needs to be refined. Common refining methods include solvent extraction, hydrofining, adsorption refining, etc.
The solvent extraction refining method is the most widely used method for refining the waste mineral oil at present because of low one-time investment, low production cost and small safety risk. The extractant used for refining the waste mineral oil is mainly N-methylpyrrolidone (NMP) and N, N-Dimethylformamide (DMF). However, after the extractant is recycled for a long time, the impurity content in the extractant is gradually increased, the content of the pure extractant, namely the active component, is gradually reduced, and partial impurities with the boiling point close to that of the pure extractant or azeotropy with that of the pure extractant cannot be removed by a common rectification method, so that the dissolution capacity of the extractant on mineral oil impurities is reduced, the density difference is reduced, the extractant loses the effect of refining waste mineral oil, and the spent extractant becomes a spent extractant. The common rectification method can not effectively improve the purity of the invalid extractant, and the invalid extractant which can not be used continuously can only be discarded or used as other low-end solvents, and the value is lost.
The impurity components which cause the extractant to lose effectiveness are mainly water, methyl isobutyl carbinol, propylene glycol 1-monobutyl ether, 6-methyl-1-heptanol, isooctanol, n-octanol, 5-methyl-1-heptanol, acetophenone, 1-dodecene, naphthalene and the like through GC-MS analysis on the failure extractant. Because of the complex impurity components, the boiling point is close to NMP (boiling point 204 ℃) or DMF (boiling point 153 ℃) or certain impurity substances form an azeotropic system with a pure extractant under certain conditions, and the common rectification method is difficult to remove and has low efficiency.
Therefore, the problem of regeneration of the spent mineral oil extractant needs to be solved, and the due use value of the spent mineral oil extractant needs to be recovered.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention provides a method for regenerating the used waste mineral oil extractant, after the method is used for regenerating the used waste mineral oil extractant, the content of active components in the extractant can reach more than 99wt percent, preferably more than 99.5wt percent, and the yield of the regenerated extractant can reach more than 85 percent, preferably more than 95 percent. The method can effectively remove impurity components which are contaminated by the waste mineral oil extractant and have the boiling point close to or azeotropic with that of the effective components after long-time use, and can realize the regeneration of the ineffective extractant to the greatest extent.
In particular, one aspect of the present invention provides a method of regenerating spent mineral oil extractant after use, the method comprising the steps of:
(1) Mixing the used waste mineral oil extractant and water according to the mass ratio of 1 (0.5-2) to obtain a mixture, wherein the content of the effective components of the used waste mineral oil extractant is less than or equal to 90wt%, and the effective components are selected from one or two of NMP and DMF;
(2) Fully stirring the mixture in the step (1), standing the mixture for layering, retaining the lower layer liquid, and discarding the upper layer liquid;
(3) And (3) carrying out negative pressure batch distillation on the lower liquid in the step (2) to remove water and impurities in the liquid, and controlling the pressure of the negative pressure batch distillation to be 20-80 kPa and the distillation reflux ratio to be (1-5): 1 to obtain the regenerated waste mineral oil extractant.
In one or more embodiments, the waste mineral oil extractant is formed from a waste mineral oil extractant in a process for refining waste mineral oil.
In one or more embodiments, the impurities in the spent mineral oil extractant after use include one or more substances selected from the group consisting of water, methyl isobutyl methanol, propylene glycol 1-monobutyl ether, 6-methyl-1-heptanol, isooctanol, n-octanol, 5-methyl-1-heptanol, acetophenone, 1-dodecene, and naphthalene.
In one or more embodiments, greater than 90wt% of the impurities in the spent mineral oil extractant after use consist of one or more substances selected from the group consisting of water, methyl isobutyl methanol, propylene glycol 1-monobutyl ether, 6-methyl-1-heptanol, isooctanol, n-octanol, 5-methyl-1-heptanol, acetophenone, 1-dodecene, and naphthalene.
In one or more embodiments, in step (1), the used waste mineral oil extractant and water are mixed in a mass ratio of 1 (0.6 to 1), more preferably in a mass ratio of 1 (0.8.+ -. 0.1).
In one or more embodiments, in step (2), the mixture is stirred for 10 to 60 minutes.
In one or more embodiments, in step (3), the pressure of the negative pressure batch distillation is controlled to be 20 to 50kPa, for example 40 to 50kPa.
In one or more embodiments, in step (3), the rectification reflux ratio is controlled to be (2-4): 1, e.g., (3.+ -. 0.5): 1.
In one or more embodiments, the regenerated spent mineral oil extractant obtained in step (3) has an active component content of greater than or equal to 99wt%.
In another aspect the present invention provides an apparatus for regenerating spent mineral oil extractant after use, the apparatus comprising an extraction tank, a fluid separator and a distillation tank connected in sequence;
The extraction kettle is used for mixing the used waste mineral oil extractant, water and standing and layering of the mixture;
the fluid separator is used for separating upper-layer liquid and lower-layer liquid which are formed after standing and layering in the extraction kettle;
The distillation still comprises a still body, a rectifying tower, a condenser, a reflux ratio controller, a first collecting tank and a second collecting tank, wherein the fluid separator is communicated with the still body, the still body is communicated with the rectifying tower, the condenser and the reflux ratio controller are arranged at the top of the rectifying tower, the condenser, the reflux ratio controller and the rectifying tower are communicated in pairs, the first collecting tank and the second collecting tank are respectively communicated with the reflux ratio controller, and the distillation still is used for carrying out negative pressure intermittent rectification on lower-layer liquid in the fluid separator.
In one or more embodiments, the rectifying column is used to rectify the material at the bottom of the tank.
In one or more embodiments, the apparatus further comprises a distillation device in communication with the first or second collection tank for distilling the cut-off moisture and impurities or the regenerated spent mineral oil extractant.
The apparatus of the present invention may be used to carry out the method of the present invention for regenerating spent mineral oil extractant after use.
Drawings
FIG. 1 is a process flow diagram of the method for regenerating spent mineral oil extractant after use of the present invention.
Fig. 2 is a schematic diagram of the apparatus for practicing the post-use spent mineral oil extractant regeneration method of the present invention in some embodiments of the present invention. In fig. 2, 100 is an extraction kettle, 200 is a fluid separator, 300 is a rectifying tower, 400 is a kettle body, 500 is a condenser, 600 is a reflux ratio controller, 700 is a first collecting tank, and 800 is a second collecting tank.
Detailed Description
So that those skilled in the art can appreciate the features and effects of the present invention, a general description and definition of the terms and expressions set forth in the specification and claims follows. Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs, and in the event of a conflict, the present specification shall control.
The theory or mechanism described and disclosed herein, whether right or wrong, is not meant to limit the scope of the invention in any way, i.e., the present disclosure may be practiced without limitation to any particular theory or mechanism.
Herein, "comprising," "including," "containing," and similar terms are intended to cover the meaning of "consisting essentially of … …" and "consisting of … …," e.g., "a consisting essentially of B and C" and "a consisting of B and C" should be considered to have been disclosed herein when "a comprises B and C" is disclosed herein.
In this document, all features such as values, amounts, and concentrations that are defined as ranges of values or percentages are for brevity and convenience only. Accordingly, the description of a numerical range or percentage range should be considered to cover and specifically disclose all possible sub-ranges and individual values (including integers and fractions) within the range.
Herein, unless otherwise specified, percentages refer to mass percentages, and proportions refer to mass ratios.
Herein, when embodiments or examples are described, it should be understood that they are not intended to limit the invention to these embodiments or examples. On the contrary, all alternatives, modifications, and equivalents of the methods and materials described herein are intended to be included within the scope of the invention as defined by the appended claims.
In this context, not all possible combinations of the individual technical features in the individual embodiments or examples are described in order to simplify the description. Accordingly, as long as there is no contradiction between the combinations of these technical features, any combination of the technical features in the respective embodiments or examples is possible, and all possible combinations should be considered as being within the scope of the present specification.
The working principle of the method for regenerating the waste mineral oil extractant of the invention is as follows: the materials polluted by the waste mineral oil extractant in the solvent extraction refining process of the waste mineral oil are insoluble in water or azeotropy with water, while the pure extractant DMF or NMP is mutually soluble with water and does not form azeotropy with water. The inventor of the invention has found through intensive research that water is adopted as an extraction medium, a water-insoluble part is separated out, substances which are azeotroped with water are further rectified and separated out together with water, so that impurity components which are close to or azeotroped with the boiling point of the pure extractant are removed, the content of effective components in the regenerated extractant can reach more than 99wt% and even more than 99.5wt%, the regenerated waste mineral oil extractant can be recycled to the greatest extent, and the production cost and the investment cost are reduced.
As shown in fig. 1, the method for regenerating a spent mineral oil extractant after use of the present invention comprises the steps of:
(1) Mixing the used waste mineral oil extractant and water according to the mass ratio of 1 (0.5-2) to obtain a mixture, wherein the content of the effective components of the used waste mineral oil extractant is less than or equal to 90wt%, and the effective components are selected from one or two of NMP and DMF;
(2) Fully stirring the mixture in the step (1), standing the mixture for layering, retaining the lower layer liquid, and discarding the upper layer liquid;
(3) And (3) carrying out negative pressure batch distillation on the lower liquid in the step (2) to remove water and impurities in the liquid, and controlling the pressure of the negative pressure batch distillation to be 20-80 kPa and the distillation reflux ratio to be (1-5): 1 to obtain the regenerated waste mineral oil extractant.
In the present invention, the waste mineral oil extractant means a reagent for extracting impurities in waste mineral oil, and its main component (active component) is selected from NMP and DMF.
In the invention, the used waste mineral oil extractant is formed by the waste mineral oil extractant in the process of refining waste mineral oil. The impurities in the used waste mineral oil extractant are mainly one or more substances selected from water, methyl isobutyl carbinol, propylene glycol 1-monobutyl ether, 6-methyl-1-heptanol, isooctyl alcohol, n-octyl alcohol, 5-methyl-1-heptanol, acetophenone, 1-dodecene and naphthalene. Typically, more than 90% by weight of the impurities in the spent mineral oil extractant after use consist of one or more substances selected from the group consisting of water, methyl isobutyl methanol, propylene glycol 1-monobutyl ether, 6-methyl-1-heptanol, isooctanol, n-octanol, 5-methyl-1-heptanol, acetophenone, 1-dodecene, and naphthalene.
In the step (1) and the step (2), part of impurities in the waste mineral oil extractant are insoluble in water, enter an upper oil phase after layering, and are removed by discarding the upper oil phase. In step (1), the mass ratio of the spent mineral oil extractant to water may be 1 (0.5-2), such as 1:0.6, 1:0.7, 1:0.8, 1:0.9, 1:1, 1:1.5. In some preferred embodiments, the mass ratio of spent mineral oil extractant to water is 1 (0.6-1), more preferably 1 (0.7-1:0.9), such as 1:0.8, which facilitates improved purity and recovery of the effective components of the recovered extractant.
In step (2), the time required for sufficiently stirring the mixture in step (1) is usually 10 to 60 minutes, for example, 20 minutes, 30 minutes, 40 minutes, 50 minutes.
In the step (3), the lower water phase obtained by layering is subjected to negative pressure batch rectification, so that impurities azeotropy with water are further removed. In step (3), the rectification pressure is preferably controlled to 20 to 50kPa, for example 40 to 50kPa, which is advantageous in improving the purity and recovery rate of the effective components of the recovered extractant. The rectification reflux ratio in step (3) is preferably controlled to be (2 to 4): 1, more preferably (2.5 to 3.5): 1, for example, 3:1, which is advantageous in improving the purity and recovery rate of the effective components of the recovered extractant.
In a preferred embodiment, the regenerated spent mineral oil extractant obtained in step (3) has an active component content (i.e. purity) of 99 wt.% or more, more preferably 99.5 wt.% or more.
In a preferred embodiment, the recovery rate (actual recovery mass/theoretical recoverable mass) of the spent mineral oil extractant regenerated using the method of the invention is greater than or equal to 85%, preferably greater than or equal to 95%.
In some embodiments, the recovery rate is greater than or equal to 95% by controlling the mass ratio of waste mineral oil extractant to water in step (1), 1 (0.6-1), and controlling the rectification pressure in step (3) to 20-50 kPa, and the rectification reflux ratio to (2-4): 1, such that the active component content of the regenerated waste mineral oil extractant is greater than or equal to 99.5 wt%.
The equipment for regenerating the used waste mineral oil extractant (the equipment of the invention for short) comprises an extraction kettle, a fluid separator and a distillation kettle which are sequentially connected, wherein the distillation kettle comprises a kettle body, a rectifying tower, a condenser, a reflux ratio controller, a first collecting tank and a second collecting tank, the fluid separator is communicated with the kettle body, the kettle body is communicated with the rectifying tower, the condenser and the reflux ratio controller are arranged at the top of the rectifying tower, the condenser, the reflux ratio controller and the rectifying tower are communicated with each other in pairs, and the first collecting tank and the second collecting tank are respectively communicated with the reflux ratio controller.
In the equipment, the extraction kettle is used for mixing the used waste mineral oil extractant and water, and then standing and layering the mixture. A fluid separator connected to the extraction tank was used to separate the upper oil phase after stratification of the mixture. The distillation still connected with the fluid separator is used for rectifying the water phase at the lower part of the fluid separator. In the present invention, the configurations of the extraction tank, the fluid separator and the distillation tank, and the tank body, the rectifying column, the condenser, the reflux ratio controller, the first collecting tank and the second collecting tank in the distillation tank are conventional. In the invention, the functions of the kettle body, the rectifying tower, the condenser, the reflux ratio controller, the first collecting tank and the second collecting tank in the distilling kettle are conventional.
In some embodiments, the apparatus of the present invention further comprises a rectifying column coupled to the tank for rectifying the material at the bottom of the tank.
In some embodiments, the apparatus of the present invention further comprises a distillation device coupled to the collection tank for distilling the material in the collection tank.
In some embodiments, the apparatus of the present invention further comprises a reflux ratio controller coupled to the rectification column for regulating the rectification reflux ratio.
The regeneration method of the waste mineral oil extractant uses water as an extraction medium, separates out impurity components which are insoluble in water in the waste mineral oil extractant, and then carries out rectification to obtain the regenerated waste mineral oil extractant with high effective component content. The waste mineral oil extractant recovered by the method of the invention can be continuously recycled for extracting and refining base oil from waste mineral oil or used in other places.
The invention has the following beneficial effects:
1. compared with other methods, the method provided by the invention is simple, the recovery rate is high, and the content of the effective components of the recovered waste mineral oil extractant is high;
2. the method has the advantages of low equipment investment, simple operation and low treatment cost;
3. the regenerated extractant obtained by the invention can be continuously recycled for extracting and refining the base oil from the waste mineral oil.
The invention will be illustrated by way of specific examples. It should be understood that these examples are illustrative only and are not intended to limit the scope of the invention. The methods, reagents and materials used in the examples are those conventional in the art unless otherwise indicated. The starting compounds in the examples are all commercially available.
Equipment example
The apparatus for regenerating the used waste mineral oil extractant of the following examples is shown in fig. 2, and comprises an extraction tank 100, a fluid separator 200 and a distillation tank which are sequentially connected, wherein the distillation tank comprises a tank body 400, a rectification column 300, a condenser 500, a reflux ratio controller 600, a first collecting tank 700 and a second collecting tank 800, the fluid separator 200 is communicated with the tank body 400, the tank body 400 is communicated with the rectification column 300, the condenser 500 and the reflux ratio controller 600 are arranged at the top of the rectification column 300, the condenser 500, the reflux ratio controller 600 and the rectification column 300 are communicated with each other, and the first collecting tank 700 and the second collecting tank 800 are respectively communicated with the reflux ratio controller.
Example 1
The used waste mineral oil extractant treated in this example had NMP as an active ingredient and 83wt% of active ingredient, and its impurities include water, methyl isobutyl carbinol, propylene glycol 1-monobutyl ether, 6-methyl-1-heptanol, isooctanol, n-octanol, 5-methyl-1-heptanol, acetophenone, 1-dodecene and naphthalene, which account for more than 90wt% of the total mass of the impurities.
The used waste mineral oil extractant is regenerated by the following method:
(1) Mixing the used waste mineral oil extractant and water, wherein the mass ratio of the used waste mineral oil extractant to the water is 1:0.8;
(2) Fully stirring for 10min, settling and layering, reserving a lower layer, and discarding an upper layer;
(3) The lower layer adopts negative pressure batch distillation, the pressure is controlled to be 20kPa, the distillation reflux ratio is controlled to be 2:1, and the water and impurities are removed, so that the regenerated waste mineral oil extractant is obtained.
The NMP purity of the recovered regenerated spent mineral oil extractant was 99.6% and the recovery was 95%.
Example 2
The used waste mineral oil extractant treated in this example has NMP as an active ingredient and 90wt% of impurities including water, methyl isobutyl carbinol, propylene glycol 1-monobutyl ether, 6-methyl-1-heptanol, isooctanol, n-octanol, 5-methyl-1-heptanol, acetophenone, 1-dodecene and naphthalene, which account for more than 90wt% of the total mass of the impurities.
The used waste mineral oil extractant is regenerated by the following method:
(1) Mixing the used waste mineral oil extractant and water, wherein the mass ratio of the used waste mineral oil extractant to the water is 1:0.5;
(2) Fully stirring for 10min, settling and layering, reserving a lower layer, and discarding an upper layer;
(3) The lower layer adopts negative pressure batch distillation, the pressure is controlled to be 20kPa, the distillation reflux ratio is controlled to be 2:1, and the water and impurities are removed, so that the regenerated waste mineral oil extractant is obtained.
The recovered regenerated spent mineral oil extractant had an NMP purity of 99.1% and a recovery of 94%.
Example 2 differs from example 1 in that the extractant is added in a different proportion of water, and the result shows that the more the water is added, the easier the oil phase impurities are removed by layering.
Example 3
The used waste mineral oil extractant treated in this example has NMP as an active ingredient and 90wt% of impurities including water, methyl isobutyl carbinol, propylene glycol 1-monobutyl ether, 6-methyl-1-heptanol, isooctanol, n-octanol, 5-methyl-1-heptanol, acetophenone, 1-dodecene and naphthalene, which account for more than 90wt% of the total mass of the impurities.
The used waste mineral oil extractant is regenerated by the following method:
(1) Mixing the used waste mineral oil extractant and water, wherein the mass ratio of the used waste mineral oil extractant to the water is 1:0.8;
(2) Fully stirring for 10min, settling and layering, reserving a lower layer, and discarding an upper layer;
(3) The lower layer adopts negative pressure batch distillation, the pressure is controlled to be 80kPa, the distillation reflux ratio is controlled to be 2:1, and the water and impurities are removed, so that the regenerated waste mineral oil extractant is obtained.
The recovered regenerated spent mineral oil extractant had an NMP purity of 99.5% and a recovery of 86%.
Example 3 differs from example 1 in that the reduced pressure is preferably 20 to 50kPa because the reduced pressure is lower, because the recovered NMP of example 3 has a higher purity but the NMP is decomposed due to a lower vacuum and a higher bottom temperature, resulting in a lower recovery rate.
Example 4
The used waste mineral oil extractant treated in this example has DMF as an effective component and 83wt% of impurities including water, methyl isobutyl carbinol, propylene glycol 1-monobutyl ether, 6-methyl-1-heptanol, isooctanol, n-octanol, 5-methyl-1-heptanol, acetophenone, 1-dodecene and naphthalene, which account for more than 90wt% of the total mass of the impurities.
The used waste mineral oil extractant is regenerated by the following method:
(1) Mixing the used waste mineral oil extractant and water, wherein the mass ratio of the used waste mineral oil extractant to the water is 1:0.8;
(2) Fully stirring for 10min, settling and layering, reserving a lower layer, and discarding an upper layer;
(3) The lower layer adopts negative pressure batch distillation, the pressure is controlled to be 50kPa, the distillation reflux ratio is controlled to be 2:1, and the water and impurities are removed, so that the regenerated waste mineral oil extractant is obtained.
The recovered regenerated spent mineral oil extractant had an NMP purity of 99.7% and a recovery of 96%.
Example 4 and example 1 demonstrate that by controlling the depressurization pressure to 20kPa to 50kPa, removal of impurities azeotroped with water and having an azeotropy temperature lower than NMP can be achieved, and a very high recovery rate can be obtained.
Example 5
The used waste mineral oil extractant treated in this example has DMF as an effective component and 83wt% of impurities including water, methyl isobutyl carbinol, propylene glycol 1-monobutyl ether, 6-methyl-1-heptanol, isooctanol, n-octanol, 5-methyl-1-heptanol, acetophenone, 1-dodecene and naphthalene, which account for more than 90wt% of the total mass of the impurities.
The used waste mineral oil extractant is regenerated by the following method:
(1) Mixing the used waste mineral oil extractant and water, wherein the mass ratio of the used waste mineral oil extractant to the water is 1:0.8;
(2) Fully stirring for 10min, settling and layering, reserving a lower layer, and discarding an upper layer;
(3) The lower layer adopts negative pressure batch distillation, the pressure is controlled to be 50kPa, the distillation reflux ratio is controlled to be 3:1, and the water and impurities are removed, so that the regenerated waste mineral oil extractant is obtained.
The recovered regenerated spent mineral oil extractant had an NMP purity of 99.8% and a recovery of 97%.
Examples 5 and 4 demonstrate that the purity and recovery of the extractant can be further improved by adjusting the reflux ratio to 3:1.
The regeneration treatment method of the waste mineral oil extractant can achieve the purpose of harmless regeneration treatment of the waste mineral oil extractant, and overcomes the defect that the common rectification method can not recover the waste mineral oil extractant. The regeneration treatment method of the waste mineral oil extractant can remove impurities in the extractant, which have the boiling point close to or azeotropic with that of the pure extractant, to the maximum extent, and the recovered extractant can be reused.
The invention has been described above by way of example only in terms of a preferred production form of the invention, but it will be understood that variations and/or modifications can be made by those skilled in the art within the scope of the appended claims without departing from the relevant scope of protection.
Claims (10)
1. A method of regenerating a spent mineral oil extractant after use, the method comprising the steps of:
(1) Mixing the used waste mineral oil extractant and water according to the mass ratio of 1 (0.5-2) to obtain a mixture, wherein the content of the effective components of the used waste mineral oil extractant is less than or equal to 90wt%, and the effective components are selected from one or two of NMP and DMF;
(2) Fully stirring the mixture in the step (1), standing the mixture for layering, retaining the lower layer liquid, and discarding the upper layer liquid;
(3) And (3) carrying out negative pressure batch distillation on the lower liquid in the step (2) to remove water and impurities in the liquid, and controlling the pressure of the negative pressure batch distillation to be 20-80 kPa and the distillation reflux ratio to be (1-5): 1 to obtain the regenerated waste mineral oil extractant.
2. The method of claim 1, wherein the spent mineral oil extractant after use is formed from a spent mineral oil extractant during refining of spent mineral oil.
3. The method of claim 1, wherein the impurities in the spent mineral oil extractant after use comprise one or more substances selected from the group consisting of water, methyl isobutyl methanol, propylene glycol 1-monobutyl ether, 6-methyl-1-heptanol, isooctanol, n-octanol, 5-methyl-1-heptanol, acetophenone, 1-dodecene, and naphthalene; preferably, more than 90wt% of the impurities in the spent mineral oil extractant after use consist of one or more substances selected from the group consisting of water, methyl isobutyl carbinol, propylene glycol 1-monobutyl ether, 6-methyl-1-heptanol, isooctanol, n-octanol, 5-methyl-1-heptanol, acetophenone, 1-dodecene and naphthalene.
4. The method according to claim 1, wherein in the step (1), the used waste mineral oil extractant and water are mixed in a mass ratio of 1 (0.6 to 1), more preferably in a mass ratio of 1 (0.8.+ -. 0.1).
5. The method according to claim 1, wherein in the step (2), the mixture is stirred for 10 to 60 minutes.
6. A method according to claim 1, wherein in step (3) the pressure of the negative pressure batch distillation is controlled to be 20 to 50kPa, such as 40 to 50kPa.
7. The method according to claim 1, wherein in the step (3), the rectification reflux ratio is controlled to be (2 to 4): 1, for example (3.+ -. 0.5): 1.
8. The process of claim 1, wherein the regenerated spent mineral oil extractant obtained in step (3) has an effective component content of greater than or equal to 99wt%.
9. An apparatus for carrying out the method of regenerating used spent mineral oil extractant of any one of claims 1-8, characterized in that the apparatus comprises an extraction tank, a fluid separator and a distillation tank connected in sequence;
The extraction kettle is used for mixing the used waste mineral oil extractant, water and standing and layering of the mixture;
the fluid separator is used for separating upper-layer liquid and lower-layer liquid which are formed after standing and layering in the extraction kettle;
The distillation still comprises a still body, a rectifying tower, a condenser, a reflux ratio controller, a first collecting tank and a second collecting tank, wherein the fluid separator is communicated with the still body, the still body is communicated with the rectifying tower, the condenser and the reflux ratio controller are arranged at the top of the rectifying tower, the condenser, the reflux ratio controller and the rectifying tower are communicated in pairs, the first collecting tank and the second collecting tank are respectively communicated with the reflux ratio controller, and the distillation still is used for carrying out negative pressure intermittent rectification on lower-layer liquid in the fluid separator.
10. The apparatus of claim 9, further comprising distillation means in communication with said first or second collection tank for distilling said cut-off moisture and impurities or said regenerated waste mineral oil extractant.
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