CN100486664C - Air assisted solvent extraction method and equipment - Google Patents
Air assisted solvent extraction method and equipment Download PDFInfo
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- CN100486664C CN100486664C CNB200510115735XA CN200510115735A CN100486664C CN 100486664 C CN100486664 C CN 100486664C CN B200510115735X A CNB200510115735X A CN B200510115735XA CN 200510115735 A CN200510115735 A CN 200510115735A CN 100486664 C CN100486664 C CN 100486664C
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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 ion.
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 ion, 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.In extraction process, a part of extractant can residue in the heavy phase, has not only caused the loss of extractant, has caused the secondary pollution to heavy phase again on the other hand.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 heavy 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 heavy phase, have application promise in clinical practice.
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 heavy 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 is set respectively in solvent extraction equipment helps and subtract mixed extraction section, gas helps strengthening extraction district and three-phase enlarging Disengagement zone, carrying out gas when gas helps strengthening extraction operation helps and subtracts mixed extracting operation, promptly help to subtract and mix extraction section at the gas that is positioned at extractant import bottom, utilize the bubble population enrichment of rising to wait to extract organic matter or ion, utilize a liquid-vapor interface enrichment part to be dissolved in extractant in the heavy phase simultaneously, finish gas and help to subtract and sneak out journey; Help the strengthening extraction district at gas, the process that the bubble population forced fluid of rising-liquid mixes promotes solvent and heavy phase interface to upgrade, and finishes gas and helps forced fluid-liquid extraction process; In three-phase enlarging Disengagement zone utilizes, the smooth extraction extractant of the buffer action of outer enlarging, utilize the amplification effect of bubble enlarging passage 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, add the auxiliary extraction agent simultaneously in case of necessity so that finish three phase separation better and liquid-liquid interface layer extraction process, further strengthen air assisted solvent extraction, the auxiliary extraction agent needn't enter gas with extractant and help the strengthening extraction district, this extracting process is finished to be helped to subtract by gas in an extraction equipment and is mixed extraction, the air assisted solvent extraction process that gas helps processes such as strengthening extraction and three phase separation to form, and three parts are mutually promoted, and have higher using value in extraction industry.
The equipment that is applicable to air assisted solvent extraction method provided by the invention, 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 distribution grid 3, it is characterized in that gas helps the bottom that subtracts mixed extraction section 4 that gas distribution grid 3, gas inlet tube 2 and heavy out 1 are set, top is provided with extractant import 21; Gas helps moving component 6 and driving shaft 7 is set in the strengthening extraction district 5, and they are driven by the drive unit 13 at equipment top, and gas helps the top in strengthening extraction district that heavy phase import 8 is set; Bubble enlarging path 10 is set in the three-phase enlarging Disengagement zone 9, and this bubble enlarging path 10 places in the extractant layer 11 when operation, and the top of three-phase enlarging Disengagement zone 9 is provided with auxiliary extraction agent import 12 and gas vent 14, and sidewall is provided with extractant outlet 15; Help strengthening extraction district 5 that five sample tap 16-20 are set along gas.
Air assisted solvent extraction method of the present invention, when helping the strengthening extraction operation, gas made full use of the immixture of bubble for liquid-liquid two-phase, promoting extractant to upgrade to reach with the interface of heavy phase fully mixes, 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, 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 absorbs the organic matter or the ionic species of bubble institute enrichment, and further strengthening extraction separates; This method strong operability, stability is high, and it is obvious to strengthen separating effect, and reduces 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 that the design of three-phase enlarging Disengagement zone reduces the disturbance of bubble to the extractant layer, the auxiliary extraction agent does not enter gas with extractant and helps 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 inlet tube 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 agent import
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:
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, it is characterized in that gas helps the bottom that subtracts mixed extraction section 4 that gas distribution grid 3 and heavy out 1 are set, top is provided with extractant import 21; Gas helps moving component 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, and this bubble enlarging path 10 places in the extractant layer 11 when operation, and the top of three-phase enlarging Disengagement zone 9 is provided with auxiliary extraction agent import 12 and gas vent 14, and sidewall is provided with extractant outlet 15; Along tower body 5 sample tap 16-20 (numbering 1-5 from top to bottom) are set.
Press accompanying drawing 1, get the long 100cm that is, the hollow glass tube of internal diameter 2.7cm is an equipment body, the 30cm of hollow glass tube bottom is that gas helps to subtract and mixes extraction section 4, do not add moving component, help the top that subtracts mixed extraction section to leave extractant import 21 at gas, top 70cm is that gas helps strengthening extraction district 5, help top, strengthening extraction district to leave heavy phase import 8 at gas, built-in sieve diameter 0.7cm, percent opening is that 47.0% stainless steel sieve plate is as moving component 6, be fixed on the stainless steel driving shaft 7, the sieve plate spacing is 2.5cm, the gap of sieve plate and tower body is 0.2cm, the conical flask of termination one 1000ml under the main tower, heavy out 1 and gas inlet tube 2 are left in the bottle end, gas distribution grid 3 is that a diameter is 20 microns sintering glass plate for the 4cm average pore size, the three-phase enlarging Disengagement zone 9 that the last termination of main tower is fired especially, bubble enlarging path 10 is inverted tapered channel, the upper edge of bubble enlarging passage is apart from outer enlarging upper edge 6cm, outer enlarging upper edge is provided with gas vent 14 and auxiliary extraction agent import 12, drive unit 13 places cat head, drive the sieve plate vibration by stainless steel driving shaft 7, each phase flow rate is controlled by spinner flowmeter.
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 extractant import 21 and helps strengthening extraction district 5, both are in a ratio of 25: 1 by volume, the two phase countercurrent flow operation, 4.5 hertz of sieve plate vibration frequencies, amplitude 0.5cm, the nitrogen of compression in the steel cylinder enters gas through gas inlet tube 2 and gas distribution grid 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, by have, when no gas helps 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 extractant import 21 and helps strengthening extraction district 5, both are in a ratio of 30: 1 by volume, the two phase countercurrent flow operation, 4.5 hertz of sieve plate vibration frequencies, amplitude 0.5cm, the nitrogen of compression in the steel cylinder enters gas through gas inlet tube 2 and gas distribution grid 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%, when gas helps extracting operation, the gas superficial flow velocity is 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%.By have, extraction efficiency that no gas helps more as can be seen, the extraction yield of air assisted solvent extraction has improved 5.0%, 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.
Air assisted solvent extraction equipment with embodiment 1 made, running water enters gas with the flow of 90ml/min from heavy phase import 8 as heavy phase and helps strengthening extraction district 5, butyl acetate enters gas with the flow of 4ml/min from extractant import 21 and helps strengthening extraction district 5, both are in a ratio of 22.5:1 by volume, counter-current operation, 4.5 hertz of sieve plate vibration frequencies, amplitude 0.5cm, the nitrogen of compression in the steel cylinder enters gas through gas inlet tube 2 and gas distribution grid 3 and helps to subtract and mix extraction section 4, measure butyl acetate under the different condition and characterize extractant 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 have, extraction efficiency that no gas helps more as can be seen, gas helps the bubble population that subtracts mixed extraction section 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 (11)
1, a kind of air assisted solvent extraction method, it is characterized in that, comprise 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, the air assisted solvent extraction process that gas helps strengthening extraction and three-phase enlarging lock out operation to be formed, heavy phase and extractant counter-current operation, help the process that motion bubble in the mixed extraction section (4) is finished enrichment organic matter or ion that subtracts at gas, help at gas and to carry out gas in the strengthening extraction district (5) and help the reinforcement liquid-liquid extraction, three-phase is finished liquid-liquid-gas three phase separation in enlarging Disengagement zone (9), bubble enlarging passage (10) places in the extractant layer (11) during operation, extractant and auxiliary extraction agent absorb entrained organic matter or the ion of bubble, further finish gas and help extraction process.
2, by the described air assisted solvent extraction method of claim 1, it is characterized in that this method is applicable to have surface-active and volatile extractant.
3, by the described air assisted solvent extraction method of claim 1, it is characterized in that, heavy phase and extractant counter-current operation, its volume is 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) placed in the extractant layer (11) when gas helped extracting operation, extractant 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 the auxiliary extraction agent does not enter gas with extractant and helps strengthening extraction district (5).
6, by the described air assisted solvent extraction method device therefor of claim 1-5, it is characterized in that, gas helps the top that subtracts mixed extraction section (4) that extractant import (21) is set, and gas helps the lower end that subtracts mixed extraction section (4) that gas distribution grid (3) and heavy out (1) are set; Gas helps the top in strengthening extraction district (5) that heavy phase import (8) is set, and gas helps moving component (6) and driving shaft (7) are set in the strengthening extraction district, and moving component (6) is connected with drive unit (13) by driving shaft (7); The inside of three-phase enlarging Disengagement zone (9) is provided with bubble enlarging passage (10), and the upper end of three-phase enlarging Disengagement zone is provided with auxiliary extraction agent import (12) and gas vent (14), and the sidewall of three-phase enlarging Disengagement zone (9) is provided with extractant outlet (15).
7, by the described air assisted solvent extraction device therefor of claim 6, 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 6, it is characterized in that 8, 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.
9,, it is characterized in that gas helps and subtracts the gentle length sum in strengthening extraction district (5) and three-phase enlarging Disengagement zone (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 6.
10, by the described air assisted solvent extraction device therefor of claim 6, it is characterized in that bubble enlarging passage (10) is set in the three-phase enlarging Disengagement zone (9), and the upper edge of bubble enlarging passage (10) is not higher than the upper edge of three-phase enlarging Disengagement zone (9).
11, by the described air assisted solvent extraction device therefor of claim 6, it is characterized in that gas helps moving component (6) is set in the strengthening extraction district (5).
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CN114849475B (en) * | 2022-04-27 | 2023-11-07 | 华东理工大学 | Microporous membrane for membrane extraction, continuous countercurrent microporous membrane extractor and separation method |
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Citations (1)
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US4786414A (en) * | 1986-07-26 | 1988-11-22 | Ronald Priestley | Gas dispersed packed extraction column |
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US4786414A (en) * | 1986-07-26 | 1988-11-22 | Ronald Priestley | Gas dispersed packed extraction column |
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