CN1962017A - Air assisted solvent extraction method and equipment - Google Patents
Air assisted solvent extraction method and equipment Download PDFInfo
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- CN1962017A CN1962017A CN 200510115735 CN200510115735A CN1962017A CN 1962017 A CN1962017 A CN 1962017A CN 200510115735 CN200510115735 CN 200510115735 CN 200510115735 A CN200510115735 A CN 200510115735A CN 1962017 A CN1962017 A CN 1962017A
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Abstract
The invention relates to a gas assisting solvent extractive method and relative device, wherein it completes the gas assisting solvent reduce mixed extraction, gas assisting solvent strength extraction and three-phase separation in one device; in the first step, the foams are completed extracted into organic, and process the abundant separation on the extractive solvent; in the second step, it processes gas assisting solvent strength liquid-liquid extraction; in the expandable separation area, it completes the three-phase separation, and the assisting solvent gas solvent extraction. The invention comprises gas assisting solvent reduce extraction area with gas distributor, gas assisting solvent strength extraction area with motion element, and three-phase expandable separation area with foam expandable channel. The invention can improve the separate efficiency and extraction ability, without secondary pollution of heavy phase.
Description
Technical field
The present invention relates to a kind of air assisted solvent extraction method and equipment, specifically relate to the method and apparatus of a kind of gas secondary solvent extraction organic matter or ionic species.
Background technology
Liquid-liquid extraction process or solvent extraction process, it is unit operations important in the chemical industry, application is very extensive, for example separation and purification of chemical industry, medicine, metallurgy, wastewater treatment and product etc., so the research to its method of operating and equipment is scientific research personnel's research emphasis, also has important significance for theories and practical significance always.When traditional extracting process is operated under comparing condition greatly with equipment, as in the extraction water solution when a small amount of organic matter or ionic species, two-phase is compared often bigger, and extractant disperses difficulty, the restriction that balanced each other of extraction process simultaneously and its separative efficiency that is difficult to further improve.The aspect is in extraction process in addition, and a part of extractant often residues in the raffinate phase, has not only caused the loss of extractant, has caused the secondary pollution problem to raffinate phase again.Improve the loss of its extraction efficiency and ability and minimizing extractant and, be difficult to be resolved more satisfactorily often existing contradiction between the secondary pollution of raffinate phase.
Research is different from traditional extraction process extraction new method, develops new extraction equipment, with promoting the progress and development of abstraction technique, solves the problem that exists in the traditional extraction process.Air assisted solvent extraction method and equipment will be new research directions, separative efficiency and extracting power that it can not only strengthening extraction equipment, and reduce the extractant loss and to the secondary pollution of raffinate phase, have better application prospect.
Summary of the invention
The objective of the invention is to develop a kind of air assisted solvent extraction method, adopt this extracting process to strengthen the extract and separate efficient of solvent extraction equipment, and reduce the loss of extractant and the secondary pollution of raffinate phase.
Another object of the present invention is to provide a kind of equipment that is applicable to above-mentioned air assisted solvent extraction method.
The objective of the invention is to realize by the following technical solutions:
A kind of air assisted solvent extraction method of the present invention is: gas mainly is set in solvent extraction equipment helps and subtract mixed extraction section, gas helps strengthening extraction district and three-phase enlarging Disengagement zone, when gas helps reinforcement solvent extraction operation, carrying out gas simultaneously helps and subtracts mixed extracting operation, promptly help to subtract and mix extraction section at the gas that is arranged in light phase import bottom, the bubble population enrichment of utilize rising waits to extract organic matter or ionic species, utilizes a liquid-vapor interface enrichment part to be dissolved in extractant in the heavy phase simultaneously; Help in the strengthening extraction operation at gas, the process that the bubble population forced fluid of rising-liquid mixes promotes two-phase interface to upgrade, and finishes gas and helps the strengthening extraction process; Utilize the smooth extraction solvent of buffer action of inside and outside enlarging in three-phase enlarging Disengagement zone, utilize the passage amplification effect to slow down bobble rise velocity, and reduction is to the disturbance of extractant layer, finish the separation of three-phase, carry out the liquid-liquid interface extraction in the time of the organic matter of extractant layer absorption bubble institute enrichment or ionic species, stream adds the auxiliary extraction solvent to finish three phase separation and liquid-liquid interface layer extraction process better simultaneously in case of necessity, further strengthen the air assisted solvent extraction process, the auxiliary extraction solvent needn't enter gas with extractant and help the strengthening extraction district, this extracting process is finished gas and is helped to subtract and mix extraction in an extraction equipment, the air assisted solvent extraction process that gas helps operations such as strengthening extraction and three-phase enlarging are separated to form, and three parts are mutually promoted, and have higher using value.
The invention provides the equipment that is applicable to air assisted solvent extraction method, equipment body comprises mainly that gas helps to subtract and mixes extraction section 4, gas helps strengthening extraction district 5, three-phase enlarging Disengagement zone 9, gas distributor 2,3, it is characterized in that gas helps the bottom that subtracts mixed extraction section 4 that gas distribution grid 2, gas inlet tube 3 and heavy out 1 are set, top is provided with extractant import 21; Gas helps moving component (as sieve plate or rotating disk) 6 and driving shaft 7 is set in the strengthening extraction district 5, and they rely on the drive unit 13 at equipment top to drive, and its top is provided with heavy phase import 8; Bubble enlarging path 10 is set in the three-phase enlarging Disengagement zone 9, and this bubble enlarging path 10 places in the solvent layer 11 when operation, and the top in enlarging district 9 is provided with the auxiliary extraction solvent and adds inlet 12 and gas vent 14, and sidewall is provided with solvent outlet 15; Help strengthening extraction district 5 that five analytical sampling mouth 16-20 are set along gas.
Air assisted solvent extraction method of the present invention, this extracting process has made full use of the immixture of bubble for liquid-liquid two-phase when gas helps the strengthening extraction operation, promote the interface of two-phase to upgrade and fully mixing, and the parts of motion are beneficial to being evenly distributed of bubble in the equipment, both promote mutually, it also has treating capacity big, reliable in structure, be convenient to operation and mass-transfer efficiency advantages of higher, guarantee both disposal abilities of locking equipment, but be right after gas and help the gas of bottom, strengthening extraction district to help to subtract extraction section has made full use of bubble population enrichment organic matter or ionic species again when operation the ability of mixing, reduce the loss of extractant and to the secondary pollution of heavy phase, the design of three-phase enlarging Disengagement zone has reduced the disturbance of bubble to the extractant layer, the extractant layer can absorb the organic matter or the ionic species of bubble institute enrichment, and further strengthening extraction separates; This method is workable, and stability is high, and it is obvious to strengthen separating effect, and can reduce the loss of extractant.
A kind of air assisted solvent extraction equipment of the present invention, adopt the unique design of three kinds of operating spaces, gas helps the strengthening extraction district to realize that strengthening extraction separates, gas helps to subtract and mixes the secondary pollution to heavy phase that extraction section reduces the extractant loss and causes therefrom, be easy to realize, the design of three-phase enlarging Disengagement zone reduces the disturbance of bubble to the extractant layer, and can add the separation process of auxiliary extraction agent strengthening extraction, the auxiliary extraction agent needn't enter gas with extractant and help the strengthening extraction district, this facility compact, easy to operate has higher utility.
Description of drawings
Fig. 1 is the overall structure schematic diagram of a kind of air assisted solvent extraction equipment of the present invention, wherein
1, heavy out 2, gas feed 3, gas distribution grid
4, gas help subtract mix extraction section 5, gas helps strengthening extraction district 6, moving component
7, driving shaft 8, heavy phase import 9, three-phase enlarging Disengagement zone
10, bubble enlarging passage 11, extractant layer 12, auxiliary extraction solvent add inlet
13, drive unit 14, gas vent 15, extractant outlet
16, sample tap 1 17, sample tap 2 18, sample tap 3
19, sample tap 4 20, sample tap 5 21, extractant import
The specific embodiment
Below by specific embodiment technical scheme of the present invention is further described:
Embodiment 1 is a kind of making of air assisted solvent extraction method device therefor:
As shown in Figure 1, the invention provides a kind of air assisted solvent extraction method device therefor, comprising mainly that gas helps to subtract mixes extraction section 4, gas helps strengthening extraction district 5, three-phase enlarging Disengagement zone 9, gas distributor 2,3 is characterized in that, gas helps and subtracts the bottom of mixing extraction section 4 distribution of gas dress device 2 and 3 and heavy out 1 are set, and top is provided with extractant import 21; Gas helps moving component (sieve plate or rotating disk 6) and driving shaft 7 is set in the strengthening extraction district 5, and they rely on the drive unit 13 at equipment top to drive, and its top is provided with heavy phase import 8; Three-phase enlarging Disengagement zone 9 is provided with interior bubble enlarging path 10, this bubble enlarging path 10 places in the solvent layer 11 when operation, the top of enlarging Disengagement zone 9 is provided with secondary solvent and adds inlet 12 and gas vent 14, sidewall is provided with solvent outlet 15, along tower body 5 analytical sampling mouth 16-20 (numbering 1-5 from top to bottom) is set.
Embodiment 1,
Press accompanying drawing 1, get the long 100cm that is, the hollow glass tube of internal diameter 2.7cm is an equipment body, its underpart 30cm is that gas helps to subtract and mixes extraction section 4, do not add moving component, leave light phase solvent import 21 at its top, top 70cm is that gas helps strengthening extraction district 5, leave heavy phase import 8 on its top, built-in sieve diameter 0.7cm, percent opening is 47.0% stainless steel sieve plate 6, be fixed on the stainless steel driving shaft 7, the sieve plate spacing is 2.5cm, and the gap of sieve plate and tower body is 0.2cm, the conical flask of termination one 1000ml under the main tower, bottle is left heavy out 1 and gas distributor tube mouth 2 in the end, and gas distribution grid is that a diameter is that the average pore size of 4cm is 20 microns a sintering glass plate 3, the enlarging Disengagement zone 9 that the last termination of main tower is fired especially, bubble enlarging 10 is inverted taper, the upper edge is apart from outer enlarging upper edge 6cm, and outer enlarging upper edge is provided with gas vent 14 and auxiliary extraction solvent inlet 12, and drive unit 13 places cat head, drive sieve plate 6 vibrations by stainless steel driving shaft 7, each phase flow rate is controlled by spinner flowmeter.
Embodiment 2 and 3 helps gentle organic matter butyl acetate in the extraction water when helping operation for the air assisted solvent extraction equipment that use embodiment 1 made do not have gas
Embodiment 2, the butyl acetate aqueous solution-kerosene system
Air assisted solvent extraction equipment with embodiment 1 made, the butyl acetate aqueous solution of 0.53v% enters gas with the flow of 100ml/min from heavy phase import 8 and helps strengthening extraction district 5, the kerosene that does not contain butyl acetate enters gas with the flow of 4ml/min from solvent phase import 21 and helps strengthening extraction district 5, both are in a ratio of 25: 1, the two phase countercurrent flow operation, 4.5 hertz of vibration frequencies, amplitude 0.5cm, the nitrogen of compression in the steel cylinder enters gas through air inlet pipe 2 and gas distributor 3 and helps to subtract and mix extraction section 4, it is that gas flow rate is when being zero that no gas helps, begin to operate that to go out tower aqueous phase butyl acetate content behind the 50min be 0.15v%, extraction efficiency is 72%, help strengthening extraction district the 2nd and 5 sample tap sample analysis at gas, aqueous phase butyl acetate content is for Wei not 0.23v% and 0.15v%, when gas helps extracting operation, the gas superficial flow velocity is 0.038m/min, begin to operate that to go out tower aqueous phase butyl acetate content behind the 50min be 0.10v%, extraction efficiency 81%, help strengthening extraction district the 2nd and 5 sample tap sample analysis at gas, aqueous phase butyl acetate content is for Wei not 0.20v% and 0.13v%.By the extraction efficiency that has or not gas to help more as can be seen, the extraction yield of air assisted solvent extraction has improved 9.0% when helping than no gas, gas helps extraction to strengthen extraction efficiency, when having or not gas to help solute concentration along tower distribute more as can be seen, gas helps and subtracts the effect that the bubble population that mixes extraction section 4 has enrichment organic matter butyl acetate.
That discharges in embodiment 3, the penicillin production contains butyl acetate waste acid water-nonane system
Air assisted solvent extraction equipment with embodiment 1 made, the flow that contains butyl acetate waste acid water 75ml/min that discharges in the penicillin production of 0.38v% enters gas from heavy phase import 8 and helps strengthening extraction district 5, not containing the butyl acetate nonane enters gas with the flow of 2.5ml/min from solvent phase import 21 and helps strengthening extraction district 5, both are in a ratio of 30: 1, the two phase countercurrent flow operation, 4.5 hertz of vibration frequencies, amplitude 0.5cm, the nitrogen of compression in the steel cylinder enters gas through air inlet pipe 2 and gas distributor 3 and helps to subtract and mix extraction section 4, it is that gas flow rate is when being zero that no gas helps, begin to operate and go out that butyl acetate content is 0.13v% in the tower waste acid water behind the 40min, extraction efficiency is 66%, and when gas helped extracting operation, the gas superficial flow velocity was 0.030m/min, go out behind the beginning operation 40min that butyl acetate content is 0.11v% in the tower waste acid water, extraction efficiency 71%.More as can be seen, the extraction yield of air assisted solvent extraction has improved 5.0% by the extraction efficiency that has or not gas to help, and gas helps extraction to strengthen extraction efficiency equally, compare with embodiment 2, the reduction of gas superficial flow velocity, two-phase is compared increase, and gas helps the reinforcement centrifugation of extracting operation to reduce.
Embodiment 4 for the air assisted solvent extraction equipment that uses embodiment 1 made do not have gas help gentle when helping operation extractant loss and to the mensuration of heavy phase secondary pollution degree
Embodiment 4
Air assisted solvent extraction equipment with embodiment 1 made, running water enters gas with the flow of 90ml/min from heavy phase import 8 and helps strengthening extraction district 5, butyl acetate enters gas with the flow of 4ml/min from solvent phase import 21 and helps strengthening extraction district 5, both are in a ratio of 22.5: 1, counter-current operation, 4.5 hertz of vibration frequencies, amplitude 0.5cm, the nitrogen of compression in the steel cylinder enters gas through air inlet pipe 2 and gas distributor 3 and helps to subtract and mix extraction section 4, measure butyl acetate under the different condition and come characterize solvents residual at water aqueous phase residual, it is that gas flow rate is when being zero that no gas helps, begin to operate that to go out tower aqueous phase butyl acetate content behind the 30min be 0.35v%, when gas helped extracting operation, the gas superficial flow velocity was 0.030m/min, began to operate that to go out tower aqueous phase butyl acetate content behind the 30min be 0.28v%.By the extraction efficiency that has or not gas to help more as can be seen, gas helps the bubble population that subtracts confounding 4 to have the effect that enrichment is dissolved in the extractant butyl acetate in the heavy phase water, air assisted solvent extraction alleviated the secondary pollution of extractant to heavy phase, extractant has reduced 20.0% owing to being dissolved in the amount that heavy phase loses.
Claims (12)
1, a kind of air assisted solvent extraction method, it is characterized in that, comprise mainly at one that gas helps and subtract mixed extraction section (4), gas helps strengthening extraction district (5), in the extraction equipment of three-phase enlarging Disengagement zone (9), finishing gas helps to subtract and mixes extraction, gas helps strengthening extraction, and enlarging such as separates at the air assisted solvent extraction process that operation is formed with three-phase, heavy phase and solvent be counter-current operation mutually, help the process that motion bubble in the mixed extraction section (4) is finished concentration and separation organic matter or ionic species that subtracts at gas, reduce extractant owing to being dissolved in that heavy phase is lost and to the secondary pollution of heavy phase, help at gas and to carry out gas in the strengthening extraction district (5) and help the reinforcement liquid-liquid extraction, improve both extraction efficiencies of locking equipment, three-phase is finished in enlarging Disengagement zone (9) and is separated, and when operation bubble enlarging passage (10) places in the solvent layer (11), extractant phase (need assist in case of necessity and add extractant) absorbs entrained organic matter or the ionic species of bubble, further finishes gas and helps extraction process.
By the described air assisted solvent extraction method of claim 1, it is characterized in that 2, this method is applicable to that light phase extractant has the volatility of certain surface-active or appropriateness.
By the described air assisted solvent extraction method of claim 1, it is characterized in that 3, heavy phase and light counter-current operation are mutually compared between 100: 1 and 5: 1.
4, by the described air assisted solvent extraction method of claim 1, it is characterized in that bubble enlarging passage (10) places in the solvent layer (11) during extracting operation, solvent layer and heavy phase interface are no more than the upper edge of bubble enlarging passage (10).
5, by the described air assisted solvent extraction method of claim 1, it is characterized in that, extra additional auxiliary extraction agent is further to finish the air assisted solvent extraction process in solvent layer can to add inlet by the auxiliary extraction solvent at different materials, and this auxiliary extraction agent does not enter gas with extractant and helps strengthening extraction district (5).
6, by the described air assisted solvent extraction method of claim 1, it is characterized in that at different materials, gas can be air and nitrogen.
7, by the described air assisted solvent extraction method device therefor of claim 1-6, it is characterized in that, the extraction equipment main body comprises mainly that gas helps and subtracts mixed extraction section (4), its top is provided with extractant import (21), its lower end is provided with distribution device in gas-fluid (2,3) and heavy out (1), gas helps strengthening extraction district (5), its top is provided with heavy phase import (8), moving component (6) and driving shaft (7) are set in the district, the drive unit at equipment top (13) drives moving component (6) motion by driving shaft (7), three-phase enlarging Disengagement zone (9), its inside is provided with bubble enlarging passage (10), the upper end is provided with secondary solvent import (12) and gas vent (14), and sidewall is provided with solvent outlet (15).
8, by the described air assisted solvent extraction device therefor of claim 7, it is characterized in that gas helps the upper end that subtracts mixed extraction section (4) that extractant import (21) is set, extractant directly enters gas and helps strengthening extraction district (5).
By the described air assisted solvent extraction device therefor of claim 7, it is characterized in that 9, the length that gas helps strengthening extraction district (5) and gas to help and subtracts mixed extraction section (4) compares between 5: 1 and 0.5: 1.
10,, it is characterized in that gas helps and subtracts the gentle length sum in strengthening extraction district (5) and three phase separation enlarging district (9) length of helping of mixed extraction section (4) and compare between 5: 1 and 10: 1 by the described air assisted solvent extraction device therefor of claim 7.
11, by the described air assisted solvent extraction device therefor of claim 7, it is characterized in that, comprise in the three phase separation enlarging district (9) that bubble enlarging split tunnel (10) and its upper edge are not higher than the upper edge in three phase separation enlarging district (9).
12, by the described air assisted solvent extraction device therefor of claim 7, it is characterized in that, gas help strengthening extraction district (5) gentle help to subtract in the mixed extraction section (4) all moving component can be set.
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| CNB200510115735XA CN100486664C (en) | 2005-11-10 | 2005-11-10 | Air assisted solvent extraction method and equipment |
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| CNB200510115735XA CN100486664C (en) | 2005-11-10 | 2005-11-10 | Air assisted solvent extraction method and equipment |
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| CN1962017A true CN1962017A (en) | 2007-05-16 |
| CN100486664C CN100486664C (en) | 2009-05-13 |
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| CN102233199A (en) * | 2010-04-30 | 2011-11-09 | 中国科学院过程工程研究所 | Three-phase solvent gas assisted extraction subsection-inlet back-mixing controllable continuous extraction device |
| CN102284191A (en) * | 2010-06-18 | 2011-12-21 | 中国科学院过程工程研究所 | Three-phase solvent air assisted extraction method of |
| CN102284190A (en) * | 2010-06-18 | 2011-12-21 | 中国科学院过程工程研究所 | Three-phase solvent air-assist continuous extraction method |
| CN102743896A (en) * | 2012-06-21 | 2012-10-24 | 中国科学院过程工程研究所 | Tower-type mixing and clarification extraction device with multiple gas stripping sections and extraction method therefor |
| CN103122408A (en) * | 2013-01-28 | 2013-05-29 | 中国科学院过程工程研究所 | Method and device for extracting and separating praseodymium and neodymium |
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| CN103752036B (en) * | 2014-01-20 | 2015-07-01 | 中国科学院青岛生物能源与过程研究所 | Bubble-assisted organic liquid film generator |
| CN105115848A (en) * | 2015-07-20 | 2015-12-02 | 山东科技大学 | Reflux type oil sand oil content and moisture synchronous determination system and determination method |
| CN107828961A (en) * | 2017-11-02 | 2018-03-23 | 中国科学院过程工程研究所 | A kind of extracting process of rare earth element ion and obtained rare-earth enrichment liquid |
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Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| GB2192811B (en) * | 1986-07-26 | 1990-04-18 | Ronald Priestley | Gas dispersed packed extraction column |
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- 2005-11-10 CN CNB200510115735XA patent/CN100486664C/en not_active Expired - Fee Related
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| CN102233199A (en) * | 2010-04-30 | 2011-11-09 | 中国科学院过程工程研究所 | Three-phase solvent gas assisted extraction subsection-inlet back-mixing controllable continuous extraction device |
| CN102233199B (en) * | 2010-04-30 | 2013-12-11 | 中国科学院过程工程研究所 | Three-phase solvent gas assisted extraction subsection-inlet back-mixing controllable continuous extraction device |
| CN102284191A (en) * | 2010-06-18 | 2011-12-21 | 中国科学院过程工程研究所 | Three-phase solvent air assisted extraction method of |
| CN102284190A (en) * | 2010-06-18 | 2011-12-21 | 中国科学院过程工程研究所 | Three-phase solvent air-assist continuous extraction method |
| CN102284190B (en) * | 2010-06-18 | 2013-08-21 | 中国科学院过程工程研究所 | Three-phase solvent air-assist continuous extraction method |
| CN102284191B (en) * | 2010-06-18 | 2014-02-26 | 中国科学院过程工程研究所 | Three-phase solvent air assisted extraction method |
| CN102743896B (en) * | 2012-06-21 | 2014-07-30 | 中国科学院过程工程研究所 | Tower-type mixing and clarification extraction device with multiple gas stripping sections and extraction method therefor |
| CN102743896A (en) * | 2012-06-21 | 2012-10-24 | 中国科学院过程工程研究所 | Tower-type mixing and clarification extraction device with multiple gas stripping sections and extraction method therefor |
| CN103122408A (en) * | 2013-01-28 | 2013-05-29 | 中国科学院过程工程研究所 | Method and device for extracting and separating praseodymium and neodymium |
| CN103122408B (en) * | 2013-01-28 | 2014-11-05 | 中国科学院过程工程研究所 | Method and device for extracting and separating praseodymium and neodymium |
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| CN103752036B (en) * | 2014-01-20 | 2015-07-01 | 中国科学院青岛生物能源与过程研究所 | Bubble-assisted organic liquid film generator |
| CN103896296A (en) * | 2014-03-18 | 2014-07-02 | 中国科学院过程工程研究所 | Method and device for extracting boron from saline brine by using air-floatation polymers |
| CN103896296B (en) * | 2014-03-18 | 2016-04-13 | 中国科学院过程工程研究所 | A kind of air supporting polymkeric substance is from the method and apparatus of salt lake brine boron extraction |
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