CN101637669A - High performance liquid-solution solvent extraction method and device - Google Patents
High performance liquid-solution solvent extraction method and device Download PDFInfo
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- CN101637669A CN101637669A CN200910055098A CN200910055098A CN101637669A CN 101637669 A CN101637669 A CN 101637669A CN 200910055098 A CN200910055098 A CN 200910055098A CN 200910055098 A CN200910055098 A CN 200910055098A CN 101637669 A CN101637669 A CN 101637669A
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Abstract
The invention relates to a high performance liquid-solution solvent extraction method and a device, providing a high performance liquid-solution solvent extraction method comprising: extracting an extracted material in a tower type to obtain extract liquor and raffinate; and performing centrifugal extraction to the obtained raffinate to obtain an extraction product. The invention also provides a high performance liquid-solution solvent extraction device.
Description
Technical field
The present invention relates to efficient liquid liquid solvent extraction method, specifically, relate to and utilize extraction tower and Centrifugical extraction technology tandem compound to carry out the new method of liquid liquid solvent extraction.The invention still further relates to the used device of this method.
Background technology
Solvent extraction is the operation of important mass transfer unit, and its basic principle is to distribute different character to realize separation or purification between the liquid mixture solute between the liquid phase of two kinds immiscible (or partial miscibilities) by solute.Solvent extraction is carried out under normal temperature or lower temperature usually, has characteristic of low energy consumption, is applicable to the separation of heat-sensitive substance, can realize the counter-current operation that economic benefit is preferable, helps the large-scale production of serialization.Its range of application has spreaded all over fields such as oil, chemical industry, hydrometallurgy, medicine, atomic energy, bioengineering, new material, environmental protection.
Realize that solvent extraction process must provide gratifying extraction equipment.Liquid-liquid extraction equipment commonly used is that mixer-settler separation, tower separation or Centrifugical extraction separate in the prior art.Mixer-settler has simple in structure, stable characteristics, but owing to be Gravity Separation, the system effect of extracting little for the two-phase density contrast, that continuous phase viscosity is big is undesirable.Tower extraction equipment is especially widely in industrial application, at chemical industry, petroleum refining, industries such as pharmacy are found everywhere high tower, they are of a great variety, spray column is arranged, packed tower, sieve-plate tower, pulse-column, vibrating sieve plate tower, rotating disc column etc., tower extraction equipment has unique advantage, liquid storage amount in its equipment is less, high-altitude development floor space is little, disposal ability is big, good seal performance, be suitable for the inflammable and explosive environment of the big flux of HTHP, but tower extraction equipment is installed, liquid is carried and is required height, easily form liquid flooding and be difficult to recover normal, difficulty is amplified in the equipment design, leave big safety coefficient, can not give full play to equipment effectiveness, it is serious to design when unreasonable back-mixing, as turntable extracting tower or pulsed extraction tower, though extraneous input energy has the effect of pulverizing drop and strengthening mass transfer, but when excessive whipping, can make the back-mixing aggravation, this has not only reduced mass transfer force, and has limited the disposal ability of extraction tower.
It is the novel extraction isolation technics that developed recently gets up that Centrifugical extraction separates, have characteristics such as compact conformation, disposal ability is big, running is steady, low in energy consumption, clean and maintenance is convenient, because centrifugal force can reach the hundred times of gravity usually, the two-phase density contrast is little, viscosity is big and the system of easy emulsification so centrifugal extractor is particularly suitable for handling, as requiring the two-phase density contrast greater than 0.1g/cm in the separation of gravity phase-splitting
3, and in centrifugal extractor, the two-phase density contrast can be as small as 0.01g/cm
3The system that general device is very big for the two-phase density contrast or viscosity is very big is difficult for mixing, and centrifugal extractor has powerful mixed function, and the two-phase logistics is fully mixed, and makes between the two-phase logistics to react at an easy rate or mass transfer.And system less to difference in specific gravity or that viscosity is big also is easy to separate.The mixing of mixture is almost to be to finish simultaneously in an equipment with separating in the centrifugal extractor, and separating effect is good especially again, thereby can improve the quality of products and increase product yield, simplifies flow process, reduces production costs.But shortcoming such as complex structure, processing request height, manufacturing cost are expensive, inconvenient maintenance that now widely used centrifugal extractor exists.
Therefore, this area press for develop a kind of novel, abstraction technique carries out solvent extraction efficiently, thereby can solve the unfavorable problem of effect of extracting in the prior art effectively, reach the purpose of degree of depth extraction, be applicable to the liquid liquid solvent extraction of atomic energy chemical industry, hydrometallurgy, pharmacy and field of petrochemical industry.
Summary of the invention
The invention provides a kind of new method of carrying out liquid liquid solvent extraction.Primary technical problem to be solved by this invention is to provide a kind of new method of carrying out liquid liquid solvent extraction at prior art, to overcome shortcoming such as the undesirable and cost height of existing equipment effect of extracting, solves the problem that liquid liquid solvent extraction exists effectively.Liquid liquid solvent extraction method and device that the present invention adopts, it is simple in structure, implements easily, and is easy to operate, and suitable long-term operation.
On the one hand, the invention provides a kind of efficient liquid liquid solvent extraction method, this method comprises:
Carry out tower extraction to being extracted material, obtain extract and raffinate; And
Raffinate to gained carries out Centrifugical extraction, obtains extraction product.
On the one hand, the invention provides a kind of efficient liquid liquid solvent extraction method, this method comprises:
Carry out Centrifugical extraction to being extracted material, obtain extract and raffinate; And
Raffinate to gained carries out tower extraction, obtains extraction product.
One preferred embodiment in, the mode of described tower extraction and Centrifugical extraction is selected from: counter-current extraction, cross current solvent extraction or their combination.
Another preferred embodiment in, single-stage extraction or multistage combination extraction are adopted in described tower extraction.
Another preferred embodiment in, described Centrifugical extraction adopts single-stage extraction or multistage combination extraction.
On the one hand, the invention provides a kind of efficient liquid liquid solvent extraction device again, this device comprises:
Be used for carrying out tower extraction obtaining the tower extraction equipment of extract and raffinate to being extracted material, and be connected in series with this tower extraction equipment, be used for the raffinate of gained is carried out Centrifugical extraction to obtain the centrifugal extraction equipment of extraction product.
On the one hand, the invention provides a kind of efficient liquid liquid solvent extraction device again, this device comprises:
Be used for carrying out Centrifugical extraction obtaining the centrifugal extraction equipment of extract and raffinate to being extracted material, and be connected in series with this centrifugal extraction equipment, be used for the raffinate of gained is carried out tower extraction to obtain the tower extraction equipment of extraction product.
One preferred embodiment in, described tower extraction equipment is selected from: spray column, packed tower, sieve-plate tower, pulse-column, vibrating sieve plate tower or rotating disc column.
Description of drawings
Fig. 1 is the extraction process flow figure according to tower extraction equipment of an embodiment of the invention and one-stage centrifugal extraction equipment tandem compound.
Fig. 2 be according to another implementation of the invention tower extraction equipment and the extraction process flow figure of two-stage centrifugal extraction equipment tandem compound.
The specific embodiment
The present inventor finds after having passed through extensive and deep research, tower extraction equipment has that the liquid storage amount is less, high-altitude development floor space is little, disposal ability big, good seal performance, be suitable for the distinct advantages of the inflammable and explosive environment of the big flux of HTHP, but difficulty is amplified in the equipment design, sometimes back-mixing is serious, major part belongs to the equipment of gravity type or low separation factor, can not reach the purpose of degree of depth extraction; Separation factor can reach the hundred times of gravity usually during Centrifugical extraction separated, be particularly suitable for handling that the two-phase density contrast is little, viscosity is big and the system of easy emulsification, and has powerful mixed function, the two-phase logistics is fully mixed, make between the two-phase logistics and react at an easy rate or mass transfer, can reach the purpose of degree of depth extraction, but exist shortcomings such as processing request height, manufacturing cost are expensive, running cost height; Under the situation that fully takes into account tower extraction equipment and centrifugal extraction equipment characteristics separately, liquid liquid solvent extraction is carried out in both effective combinations, can greatly improve effect of extracting.Based on above-mentioned discovery, the present invention is accomplished.
In a first aspect of the present invention, a kind of efficient liquid liquid solvent extraction method is provided, this method comprises: be extracted that material enters tower extraction equipment and extractant carries out extract and separate; And the raffinate after tower extraction equipment extraction enters centrifugal extraction equipment, carries out degree of depth extraction.
In a second aspect of the present invention, a kind of efficient liquid liquid solvent extraction method is provided, this method comprises: be extracted that material enters centrifugal extraction equipment and extractant carries out extract and separate; And the raffinate after the centrifugal extraction equipment extraction enters tower extraction equipment, further extracts.
In the method for the invention, extractant can have following three kinds of allocative decisions: (1) extractant all is introduced into the centrifugal extraction equipment extraction, and then through surge tank, enters tower extraction equipment extraction by the pump lifting, realizes counter-current extraction; (2) extractant is divided into two parts as required, a part directly enters tower extraction equipment extraction, and another part is introduced into the centrifugal extraction equipment extraction, and then through surge tank, after promoting by pump and the extractant that directly advances tower enter tower extraction equipment extraction together; (3) extractant is divided into two parts as required, and a part enters tower extraction equipment extraction, and another part enters the centrifugal extraction equipment extraction, realizes cross current solvent extraction.
In the present invention, described tower extraction can be adopted single-stage extraction or multistage combination extraction.
In the present invention, described Centrifugical extraction can adopt single-stage extraction or multistage combination extraction.
In a third aspect of the present invention, a kind of efficient liquid liquid solvent extraction device is provided, this device comprises: tower extraction equipment, and the centrifugal extraction equipment that is connected in series with this tower extraction equipment.This device adopts effective combination of tower extraction equipment, centrifugal extraction equipment, surge tank, valve and pipeline, to reach the purpose of degree of depth liquid liquid solvent extraction.
In the present invention, described tower extraction equipment can be industrial equipment commonly used such as spray column, packed tower, sieve-plate tower, pulse-column, vibrating sieve plate tower, rotating disc column.
In the present invention, described centrifugal extraction equipment is that collection mixes and the equipment that is separated into one, separates by centrifugal force.The design feature of centrifugal extraction equipment and principle can be consulted Chinese patent ZL 96250989.2, ZL 200720103434.X etc.
In the present invention, extractant being had no particular limits, can be this area various extractants commonly used, as benzene etc.
In the method for the invention, operating temperature is had no particular limits, those skilled in the art can make the selection that corresponds to actual needs flexibly according to the production needs of reality, in the hope of reaching desirable effect.
Below referring to accompanying drawing.
Fig. 1 is the extraction process flow figure according to tower extraction equipment of an embodiment of the invention and one-stage centrifugal extraction equipment tandem compound.As shown in Figure 1, be extracted material and at first enter tower extraction equipment 2 and carry out extract and separate, to obtain extract and raffinate with wherein extractant; Then, the raffinate of gained enters centrifugal extraction equipment 3 and extractant wherein carries out degree of depth extraction, obtain comprising the raffinate of extraction product, extractant wherein is again through surge tank 4, after promoting by pump 1 and the extractant that directly enters tower extraction equipment 2 enter tower extraction equipment 2 extractions together.
Fig. 2 be according to another implementation of the invention tower extraction equipment and the extraction process flow figure of two-stage centrifugal extraction equipment tandem compound.As shown in Figure 2, be extracted material and at first enter tower extraction equipment 2 and carry out extract and separate, to obtain extract and raffinate with wherein extractant; Then, the raffinate of gained enters the centrifugal extraction equipment 3 of two-stage series connection
-1With 3
-2Carry out degree of depth extraction with wherein extractant, obtain comprising the raffinate of extraction product, extractant wherein is again through surge tank 4, after promoting by pump 1 and the extractant that directly enters tower extraction equipment 2 enter tower extraction equipment 2 extractions together.
Major advantage of the present invention is:
The present invention is according to actual condition, with tower extraction equipment and Centrifugical extraction technology tandem compound, give full play to the characteristics separately of equipment, invented a kind of more rational gradient distribution extracting process, overcome the equipment that existing tower extraction equipment major part belongs to gravity type or low separation factor, can not reach the shortcoming of degree of depth extraction; Process units of the present invention is simple in structure, implements easily, and is easy to operate, and suitable long-term operation, is adapted at various liquid liquid solvent extraction occasions and promotes the use of.
Embodiment
Further set forth the present invention below in conjunction with specific embodiment.But, should be understood that these embodiment only are used to the present invention is described and do not constitute limitation of the scope of the invention.The test method of unreceipted actual conditions in the following example, usually according to normal condition, or the condition of advising according to manufacturer.Except as otherwise noted, all percentage and umber are by weight.
Embodiment 1:
Use technological process shown in Figure 1 to extract, specific as follows:
1. material properties
(1) be extracted material: caprolactam content is 50-60%, and all the other are water, and mixture density is 1028kg/m
3
(2) extractant: benzene, density are 872kg/m
3
2. the mensuration of caprolactam content
Caprolactam content adopts gas chromatography determination, with reference to DSM385-E and 385-02-E and DSM657-E;
3. effect
The volume flow ratio that is extracted material and extractant is 1: 6, the caprolactam content that is extracted in the material of tower extraction equipment import is 50-60%, the caprolactam content of tower extraction equipment raffinate outlet is 2-4%, after through the centrifugal extraction equipment extraction, the caprolactam content of raffinate is reduced to below 1%, has obviously improved effect of extracting.
Embodiment 2:
Use technological process shown in Figure 2 to extract, specific as follows:
1. material properties
(1) be extracted material: caprolactam content is 50-60%, and all the other are water, and mixture density is 1028kg/m
3
(2) extractant: benzene, density are 872kg/m
3
2. caprolactam content is measured
Caprolactam content adopts gas chromatography determination, with reference to DSM385-E, 385-02-E and DSM657-E;
3. effect
The volume flow ratio that is extracted material and extractant is 1: 6, the caprolactam content that is extracted in the material of tower extraction equipment import is 50-60%, the caprolactam content of tower extraction equipment raffinate outlet is 2-4%, again through after the extraction of two-stage centrifugal extraction equipment, the caprolactam content of raffinate is reduced to below 0.3%, has obviously realized degree of depth extraction.
All quote in this application as a reference at all documents that the present invention mentions, just quoted as a reference separately as each piece document.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after having read above-mentioned instruction content of the present invention, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Claims (8)
1. efficient liquid liquid solvent extraction method, this method comprises:
Carry out tower extraction to being extracted material, obtain extract and raffinate; And
Raffinate to gained carries out Centrifugical extraction, obtains extraction product.
2. efficient liquid liquid solvent extraction method, this method comprises:
Carry out Centrifugical extraction to being extracted material, obtain extract and raffinate; And
Raffinate to gained carries out tower extraction, obtains extraction product.
3. method as claimed in claim 1 or 2 is characterized in that, the mode of described tower extraction and Centrifugical extraction is selected from: counter-current extraction, cross current solvent extraction or their combination.
4. method as claimed in claim 1 or 2 is characterized in that, single-stage extraction or multistage combination extraction are adopted in described tower extraction.
5. method as claimed in claim 1 or 2 is characterized in that, described Centrifugical extraction adopts single-stage extraction or multistage combination extraction.
6. efficient liquid liquid solvent extraction device, this device comprises:
Be used for carrying out tower extraction obtaining the tower extraction equipment (2) of extract and raffinate to being extracted material, and be connected in series with this tower extraction equipment, be used for the raffinate of gained is carried out the centrifugal extraction equipment (3) of Centrifugical extraction to obtain extraction product.
7. efficient liquid liquid solvent extraction device, this device comprises:
Be used for carrying out the centrifugal extraction equipment (3) of Centrifugical extraction to obtain extract and raffinate to being extracted material, and be connected in series with this centrifugal extraction equipment, be used for the raffinate of gained is carried out tower extraction to obtain the tower extraction equipment (2) of extraction product.
8. as claim 6 or 7 described devices, it is characterized in that described tower extraction equipment is selected from: spray column, packed tower, sieve-plate tower, pulse-column, vibrating sieve plate tower or rotating disc column.
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Cited By (11)
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| CN102093176A (en) * | 2010-12-23 | 2011-06-15 | 南京师范大学 | Method for extracting and separating methylal-methanol mixture by using continuous countercurrent rotating disk |
| CN102234248A (en) * | 2010-04-23 | 2011-11-09 | 中国石油化工股份有限公司 | Impurity extraction method for caprolactam production |
| CN102260525A (en) * | 2011-06-17 | 2011-11-30 | 华东理工大学 | Gasoline dealkalizing device and use method thereof |
| CN102320958A (en) * | 2011-06-13 | 2012-01-18 | 华东理工大学 | Method and device for extracting hexahydrobenzoic acid from rearrangement reaction liquid |
| CN103539738A (en) * | 2013-11-01 | 2014-01-29 | 华东理工大学 | Method and device for recovering caprolactam in benzene distillation residue |
| CN104874201A (en) * | 2014-02-27 | 2015-09-02 | 浦华环保有限公司 | Combined centrifugal extractor |
| CN104922931A (en) * | 2015-05-20 | 2015-09-23 | 清华大学 | Pulse feedback oscillation countercurrent extractor |
| CN105447290A (en) * | 2014-08-19 | 2016-03-30 | 徐大鹏 | Evaluation method for heavy petroleum oil separation by supercritical fluid extraction and fractionation |
| CN105621364A (en) * | 2014-11-03 | 2016-06-01 | 中国石油化工股份有限公司 | High-efficiency extraction process in hydrogen peroxide production process |
| CN107803050A (en) * | 2017-12-08 | 2018-03-16 | 中国科学院过程工程研究所 | A kind of dynamic magnetic particle combination membrane extraction device and extracting process |
| CN107982960A (en) * | 2017-12-08 | 2018-05-04 | 中国科学院过程工程研究所 | A kind of magnetic particle combination membrane extraction device and extracting process |
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102234248A (en) * | 2010-04-23 | 2011-11-09 | 中国石油化工股份有限公司 | Impurity extraction method for caprolactam production |
| CN102093176B (en) * | 2010-12-23 | 2014-07-30 | 南京师范大学 | Method for extracting and separating methylal-methanol mixture by using continuous countercurrent rotating disk |
| CN102093176A (en) * | 2010-12-23 | 2011-06-15 | 南京师范大学 | Method for extracting and separating methylal-methanol mixture by using continuous countercurrent rotating disk |
| CN102320958A (en) * | 2011-06-13 | 2012-01-18 | 华东理工大学 | Method and device for extracting hexahydrobenzoic acid from rearrangement reaction liquid |
| CN102320958B (en) * | 2011-06-13 | 2013-11-13 | 华东理工大学 | Method and device for extracting hexahydrobenzoic acid from rearrangement reaction liquid |
| CN102260525A (en) * | 2011-06-17 | 2011-11-30 | 华东理工大学 | Gasoline dealkalizing device and use method thereof |
| CN103539738A (en) * | 2013-11-01 | 2014-01-29 | 华东理工大学 | Method and device for recovering caprolactam in benzene distillation residue |
| CN104874201A (en) * | 2014-02-27 | 2015-09-02 | 浦华环保有限公司 | Combined centrifugal extractor |
| CN105447290A (en) * | 2014-08-19 | 2016-03-30 | 徐大鹏 | Evaluation method for heavy petroleum oil separation by supercritical fluid extraction and fractionation |
| CN105621364B (en) * | 2014-11-03 | 2018-04-10 | 中国石油化工股份有限公司 | A kind of efficient extraction process in hydrogen peroxide production process |
| CN105621364A (en) * | 2014-11-03 | 2016-06-01 | 中国石油化工股份有限公司 | High-efficiency extraction process in hydrogen peroxide production process |
| CN104922931A (en) * | 2015-05-20 | 2015-09-23 | 清华大学 | Pulse feedback oscillation countercurrent extractor |
| CN107803050A (en) * | 2017-12-08 | 2018-03-16 | 中国科学院过程工程研究所 | A kind of dynamic magnetic particle combination membrane extraction device and extracting process |
| CN107982960A (en) * | 2017-12-08 | 2018-05-04 | 中国科学院过程工程研究所 | A kind of magnetic particle combination membrane extraction device and extracting process |
| CN107982960B (en) * | 2017-12-08 | 2019-10-25 | 中国科学院过程工程研究所 | A kind of magnetic particle combined films extraction equipment and extracting process |
| CN107803050B (en) * | 2017-12-08 | 2019-11-08 | 中国科学院过程工程研究所 | A kind of dynamic magnetic particle combined films extraction equipment and extracting process |
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Application publication date: 20100203 |