CN104587834A - Device and method for separating and recovering high-boiling-point organic matter from low-concentration aqueous solution - Google Patents
Device and method for separating and recovering high-boiling-point organic matter from low-concentration aqueous solution Download PDFInfo
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Abstract
The invention discloses a device and a method for separating and recovering high-boiling-point and water soluble organic matter from a low-concentration aqueous solution and directly obtaining high-purity liquid organic matter by using a pervaporation-fractional condensation coupling process. The method comprises the following steps that a low-pressure atmosphere is formed on the downstream side of a pervaporation membrane through a vacuum pump firstly, then high-boiling-point organic matter in a weak solution are subjected to selective enrichment by taking the pervaporation membrane as a mass transfer separation medium, and low-pressure mixed steam which penetrates through the pervaporation membrane and is enriched on the downstream side of the membrane is subjected to fractional condensation; and high-boiling-point organic matter steam is trapped in a first-stage condenser so as to generate high-purity liquid organic matter, non-condensed steam and a small part of organic steam are trapped in a second-stage condenser, and then return to a raw material slot by a circulating pump. According to the invention, through the adoption of the pervaporation-fractional condensation coupling process, no chemical reagent is required to be added, therefore, the secondary pollution is eliminated, and the implementation of the method is not limited by gas-liquid equilibrium; and the method is operated simply, rapidly and efficiently, and high-boiling-point liquid organic matter with purity over 99.9 wt % can be directly obtained.
Description
Technical field
The present invention relates to a kind of device and method of separation and recovery high boiling point organic compound from low concentration aqueous solution, belong to Chemical Engineering separation technology field.
Background technology
From weak solution, reclaim high boiling point organic compound have wide range of applications in fields such as biomass fuel extraction, purifications of waste water.Furfural and aniline are one of amine and the representational high boiling point organic compound of furans ring system most respectively, are separated directly to obtain high-purity furfural and aniline has important value from weak solution.
The production of furfural (formal name used at school furtural) is obtained by the hemicellulose material in acidic hydrolysis living beings (corncob, cotton seed hull etc.) raw material.In hydrolyzate after hydrolysis, the mass percentage of furfural is about 2 ~ 8 wt%, current domestic furfural mill adopts way of distillation separating-purifying furfural from hydrolyzate, first time is first rectifying, furfural content can be increased to concentration when 90 wt% ~ 92 wt%(water and furfural constant boiling point), and then adopt multistage rectification to carry out the refining of furfural.Distillation process can consume a large amount of steam, and therefore energy consumption accounts for the very large proportion of furfural production cost, and the energy consumption how reducing furfural separation and recovery is the focus of research.
Chinese patent CN103214439A discloses a kind of utilization and is filled with furfural in the ADSORPTION IN A FIXED BED hydrolyzate of nonpolar macroporous adsorption resin, and then the furfural eluent of higher concentration is obtained by eluant, eluent desorb, finally obtain furfural target product after treatment again, the technique of this absorption-desorption is more loaded down with trivial details, and equipment investment is large.Chinese patent CN103254158A discloses the method and device that utilize biomass by hydrolyzation coupling infiltration evaporation separation of produced furfural: infiltrating and vaporizing membrane has high adsorptive selectivity to furfural in hydrolyzate, when the furfural of Preferential adsorption in film and a small amount of water being sucked out with the formal solution of low pressure mixed vapour by vacuumizing in the downstream of film after film adsorption equilibrium, finally again furfural and water vapour condensation are collected, the furfural that this technique is collected still needs refining further, and the power consumption of the subtractive process of furfural is very large.
Aniline is one of important intermediate of chemical industry, in the industries such as dyestuff, agricultural chemicals, rubber chemicals, there is extensive use, Aniline content higher (mass fraction 1wt% ~ 3wt%), current industrial conventional aniline waste water process means have extraction, absorption method.Absorption method is not suitable for the higher aniline waste water of concentration for the treatment of, and the regeneration of adsorbent is more difficult, and after regeneration several times, adsorption capacity loss is larger.Extraction (CN1600696A, CN102936079A) easily causes the secondary pollution of water body, needs multitple extraction, and equipment investment is large, and be difficult to obtain can the high-purity aniline of reuse.
Summary of the invention
, aniline waste water treatment process loaded down with trivial details this present situation large for furfural production energy consumption, the present invention aims to provide higher boiling, water soluble organic substance-furfural and aniline in a kind of low energy consumption, flow process simple infiltration evaporation-fractional condensaion coupling device and technique separation and recovery low concentration aqueous solution.
The device of a kind of separation and recovery high boiling point organic compound from low concentration aqueous solution provided by the invention, comprise infiltration evaporation section and fractional condensaion section, described infiltration evaporation section comprises raw material storage tank, feed liquid circulating pump, infiltration evaporation groove, is provided with infiltration vaporization membrane module in infiltration evaporation groove; Described fractional condensaion section comprises first order condenser and second level condenser, first order condenser and second level condenser are connected in series, second level condenser ends is connected with vavuum pump, first order condenser lower end connects the first storage tank, condenser lower end, the second level connects the second storage tank, and the second storage tank connects raw material storage tank by circulating pump.
The method of a kind of separation and recovery high boiling point organic compound from low concentration aqueous solution provided by the invention, comprises the following steps:
(1) aqueous solution of low-concentration organic is passed into infiltration evaporation groove, fully contact with the infiltrating and vaporizing membrane with Selective Separation organics function at the upstream side of film and reach adsorption dynamics and balance;
(2) produce low-voltage vacuum by vavuum pump in infiltrating and vaporizing membrane downstream, the high boiling point organic compound-water making upstream side be adsorbed on film surface is vaporized, and forms organic matter-water low pressure mixed vapour through film at the downstream desorption of infiltrating and vaporizing membrane;
(3) organic matter of the downstream enrichment of film-water low pressure mixed vapour is passed into successively the condenser of two series connection, the first condenser temperatures is selected according to absolute pressure numerical values recited, in first order condenser, obtain the liquid high boiling point organic compound of high-purity, purity is greater than 99.9wt%;
(4) water vapour be not condensed and fraction organic steam are trapped within the condenser of the second level, and second level condenser is connected with infiltration evaporation groove, are transported in infiltration evaporation groove by fraction organic steam and carry out secondary separation recovery.
In such scheme, described low concentration aqueous solution is the aqueous solution of organic concentration in 0.1 ~ 8 wt% scope.
In such scheme, described high boiling point organic compound is boiling point at the amine of 150 ~ 230 DEG C of scopes and furan nucleus series normal temperature liquid state organics.
In such scheme, described high boiling point organic compound is furfural or aniline.The concentration of described furfural aqueous solution is: 1wt% ~ 8wt%; The concentration of aniline-water solution is: 0.1wt% ~ 4wt%.
In such scheme, the described infiltrating and vaporizing membrane with Selective Separation organics function is polyether-block-polyamide film.
In such scheme, the pressurized vacuum conditions in described infiltrating and vaporizing membrane downstream is: absolute pressure is in 30 ~ 2000 Pa scopes.
In such scheme, described first order condenser temperature controls at-30 ~ 30 DEG C; The temperature of second level condenser is-200 ~-50 DEG C.
In such scheme, the initial temperature of the aqueous solution of described low-concentration organic is 30 ~ 95 DEG C.
There is due to infiltration evaporation membrane separating process provided by the invention the advantages such as separative efficiency is high, energy consumption is low, technique is simple, non-secondary pollution, and: (1) aniline is higher boiling, water soluble organic substance, directly can be recovered to the colourless aniline liquid of high-purity from the low aqueous solution by infiltration evaporation-fractional condensaion coupling technique; (2) furfural is higher boiling (161.7 DEG C) water soluble organic substance, furfural in hydrolyzate can be recovered to the colourless furfuraldehyde liquid of high-purity by technique one step of infiltration evaporation-fractional condensaion, this method reduces the energy consumption of separation and recovery furfural from rare hydrolyzate, has very important industrial application value.
Operation principle of the present invention: because infiltration evaporation UF membrane has not by the advantage of VLE restriction, there is the organic matter in high adsorptive selectivity infiltrating and vaporizing membrane Preferential adsorption low concentration aqueous solution, then the opposite side of film vacuumizes and makes the organic matter of absorption and a small amount of water vapor, finally the low pressure organic steam (organic matter has higher boiling point) of tunicle enrichment and water vapour are carried out fractional condensaion, first the organic steam of easy condensation is trapped within first order condenser, and the water vapour be not condensed and fraction organic steam are trapped within the condenser of the second level.By infiltration evaporation-fractional condensing process, wherein higher boiling, water miscible aniline, furfural are extracted from respective low concentration aqueous solution, and the purity of the furfural reclaimed and aniline is all greater than 99.9wt%.
Of the present invention
beneficial effect:
(1) directly can be separated from low concentration aqueous solution by infiltration evaporation-fractional condensaion coupling technique and obtain high-purity higher boiling liquid state organics;
(2) separation process is without the need to adding chemical reagent, non-secondary pollution;
(3) temperature of separation process Central Plains feed liquid controls to operate at lower temperature (lower than 95 DEG C), and energy consumption is low and separative efficiency is high;
(4) coupling technique flow process is simple, easy to operate, and the high-purity organic matter of acquisition is without the need to being further purified;
(5) first fractional condensing process is applied to pervaporation method and reclaims high boiling point organic compound, add second level condenser, make the recovery utilization rate of aniline or furfural product high.
Accompanying drawing explanation
Fig. 1 is infiltration evaporation of the present invention-fractional condensing process schematic flow sheet.
In figure: 1-raw material storage tank; 2-feed liquid circulating pump; 3-infiltration evaporation groove; 4-first order condenser; 5-second level condenser; 6-vavuum pump; 7-valve, 8-first storage tank; 9-second storage tank; 10-raffinate circulating pump.
Detailed description of the invention
Further illustrate the present invention below by embodiment, but be not limited to following examples.
Embodiment 1: the device of separation and recovery high boiling point organic compound from low concentration aqueous solution
As shown in Figure 1, comprise infiltration evaporation section and fractional condensaion section, described infiltration evaporation section comprises raw material storage tank 1, feed liquid circulating pump 2, infiltration evaporation groove 3, is provided with infiltration vaporization membrane module in infiltration evaporation groove 3; Described fractional condensaion section comprises first order condenser 4 and second level condenser 5, first order condenser 4 and second level condenser 5 are connected in series, second level condenser 5 is connected with vavuum pump 6, namely vavuum pump is connected at condensed in two stages device end, first order condenser 4 lower end connects the first storage tank 8 by valve 7, second level condenser 5 lower end connects the second storage tank 9, second storage tank 9 by valve and connects raw material storage tank 1 by raffinate circulating pump 10.After condensation, product enters into storage tank by Valve controlling.
The technical process of employing said apparatus separation and recovery high boiling point organic compound is:
Because infiltration evaporation UF membrane has not by the advantage of VLE restriction, there is the organic matter in high adsorptive selectivity infiltrating and vaporizing membrane Preferential adsorption low concentration aqueous solution, then the opposite side of film vacuumizes and makes the organic matter of absorption and a small amount of water vapor, finally the low pressure organic steam (organic matter has higher boiling point) of tunicle enrichment and water vapour are carried out fractional condensaion, first the organic steam of easy condensation is trapped within first order condenser, enter in the first storage tank after condensation, the water vapour be not condensed and fraction organic steam are trapped within the condenser of the second level, enter in the second storage tank after condensation, liquid in second storage tank enters into raw material storage tank through raffinate circulating pump.By infiltration evaporation-fractional condensing process, wherein higher boiling, water miscible aniline, furfural are extracted from respective low concentration aqueous solution, and the purity of the furfural reclaimed and aniline is all greater than 99.9wt%.
Embodiment 2: separation and recovery higher boiling furfural from low concentration aqueous solution
(1) be that the furfural aqueous solution of 2 wt% is heated to 80 DEG C by concentration, passed in infiltration evaporation groove by furfural aqueous solution by feed liquid circulating pump with flow velocity 120 L/h circulation, film is adsorbed and reaches balance, in membrane module, the area of infiltrating and vaporizing membrane is 20.4cm
2;
(2) in the downstream of film, the end of condensed in two stages device vacuumizes, make film downstream pressure maintain absolute pressure 30 Pa;
(3) the low pressure mixed vapour of furfural and water is introduced temperature is-29 DEG C, heat exchange area is 0.1 m
2first order condenser in, the furfural be not condensed is introduced in the second level condenser of connecting with first order condenser with the low pressure mixed vapour of water, and second level condenser temperature is-196 DEG C;
(4) adopting karl Fischer Moisture Meter to record the furfural purity of collecting in first order condenser is 99.92 wt%, and collection rate is 240 g/ (m
2h); The furfural purity of collecting in the condenser of the second level is 25 wt%, and collection rate is 610 g/ (m
2h).
Embodiment 3: separation and recovery higher boiling furfural from low concentration aqueous solution
(1) be that the furfural aqueous solution of 3 wt% is heated to 60 DEG C by concentration, pass in infiltration vaporization membrane module with pump by furfural aqueous solution with flow velocity 120 L/h circulation, film is adsorbed and reaches balance, in membrane module, the area of infiltrating and vaporizing membrane is 20.4cm
2;
(2) in the downstream of film, the end of condensed in two stages device vacuumizes, make film downstream pressure maintain absolute pressure 250 Pa;
(3) the low pressure mixed vapour of furfural and water is introduced temperature is-8 DEG C, heat exchange area is 0.1 m
2first order condenser in, the furfural be not condensed is introduced in the second level condenser of connecting with first order condenser with the low pressure mixed vapour of water, and second level condenser temperature is-196 DEG C.
(4) adopting karl Fischer Moisture Meter to record the furfural purity of collecting in first order condenser is 99.94 wt%, and collection rate is 270 g/ (m
2h); The furfural purity of collecting in the condenser of the second level is 27 wt%, and collection rate is 320 g/ (m
2h).
Embodiment 4: separation and recovery higher boiling furfural from low concentration aqueous solution
(1) be that the furfural aqueous solution of 5 wt% is heated to 70 DEG C by concentration, pass in infiltration vaporization membrane module with pump by furfural aqueous solution with flow velocity 120 L/h circulation, film is adsorbed and reaches balance, in membrane module, the area of infiltrating and vaporizing membrane is 20.4cm
2;
(2) in the downstream of film, the end of condensed in two stages device vacuumizes, and makes film downstream pressure maintain absolute pressure 1000 Pa;
(3) the low pressure mixed vapour of furfural and water is introduced temperature is 10 DEG C, heat exchange area is 0.1 m
2first order condenser in, the furfural be not condensed is introduced in the second level condenser of connecting with first order condenser with the low pressure mixed vapour of water, and second level condenser temperature is-196 DEG C.
(4) adopting karl Fischer Moisture Meter to record the furfural purity of collecting in first order condenser is 99.95 wt%, and collection rate is 492 g/ (m
2h); The furfural purity of collecting in the condenser of the second level is 29 wt%, and collection rate is 510 g/ (m
2h).
Embodiment 5: separation and recovery higher boiling aniline from low concentration aqueous solution
(1) be that the aniline-water solution of 1 wt% is heated to 80 DEG C by concentration, pass in infiltration vaporization membrane module with pump by aniline-water solution with flow velocity 120 L/h circulation, film is adsorbed and reaches balance, in membrane module, the area of infiltrating and vaporizing membrane is 20.4cm
2;
(2) in the downstream of film, the end of condensed in two stages device vacuumizes, make film downstream pressure maintain absolute pressure 50 Pa;
(3) the low pressure mixed vapour of aniline and water is introduced temperature is-25 DEG C, heat exchange area is 0.1 m
2first order condenser in, the aniline be not condensed is introduced in the second level condenser of connecting with first order condenser with the low pressure mixed vapour of water, and second level condenser temperature is-196 DEG C.
(4) adopting karl Fischer Moisture Meter to record the aniline purity of collecting in first order condenser is 99.91 wt%, and collection rate is 395 g/ (m
2h); The aniline purity of collecting in the condenser of the second level is 1 wt%, and collection rate is 410 g/ (m
2h).
Embodiment 6: separation and recovery higher boiling aniline from low concentration aqueous solution
(1) be that the aniline-water solution of 0.2 wt% is heated to 70 DEG C by concentration, pass in infiltration vaporization membrane module with pump by aniline-water solution with flow velocity 120 L/h circulation, film is adsorbed and reaches balance, in membrane module, the area of infiltrating and vaporizing membrane is 20.4cm
2;
(2) in the downstream of film, the end of condensed in two stages device vacuumizes, and makes film downstream pressure maintain absolute pressure 500 Pa;
(3) the low pressure mixed vapour of aniline and water is introduced temperature is 3 DEG C, heat exchange area is 0.1 m
2first order condenser in, the aniline be not condensed is introduced in the second level condenser of connecting with first order condenser with the low pressure mixed vapour of water, and second level condenser temperature is-196 DEG C.
(4) adopting karl Fischer Moisture Meter to record the aniline purity of collecting in first order condenser is 99.94 wt%, and collection rate is 50 g/ (m
2h); The aniline purity of collecting in the condenser of the second level is 10 wt%, and collection rate is 400 g/ (m
2h).
Embodiment 7: separation and recovery higher boiling aniline from low concentration aqueous solution
(1) be that the aniline-water solution of 3 wt% is heated to 60 DEG C by concentration, pass in infiltration vaporization membrane module with pump by aniline-water solution with flow velocity 120 L/h circulation, film is adsorbed and reaches balance, in membrane module, the area of infiltrating and vaporizing membrane is 20.4cm
2;
(2) in the downstream of film, the end of condensed in two stages device vacuumizes, make film downstream pressure maintain absolute pressure 1200 Pa;
(3) the low pressure mixed vapour of aniline and water is introduced temperature is 13 DEG C, heat exchange area is 0.1 m
2first order condenser in, the aniline be not condensed is introduced in the second level condenser of connecting with first order condenser with the low pressure mixed vapour of water, and second level condenser temperature is-196 DEG C.
(4) adopting karl Fischer Moisture Meter to record the aniline purity of collecting in first order condenser is 99.93 wt%, and collection rate is 90 g/ (m
2h); The aniline purity of collecting in the condenser of the second level is 12 wt%, and collection rate is 380 g/ (m
2h).
Embodiment 8: separation and recovery higher boiling aniline from low concentration aqueous solution
(1) be that the aniline-water solution of 2 wt% is heated to 50 DEG C by concentration, pass in infiltration vaporization membrane module with pump by aniline-water solution with flow velocity 120 L/h circulation, film is adsorbed and reaches balance, in membrane module, the area of infiltrating and vaporizing membrane is 20.4cm
2;
(2) in the downstream of film, the end of condensed in two stages device vacuumizes, make film downstream pressure maintain absolute pressure 250 Pa;
(3) the low pressure mixed vapour of aniline and water is introduced temperature is 20 DEG C, heat exchange area is 0.1 m
2first order condenser in, the aniline be not condensed is introduced in the second level condenser of connecting with first order condenser with the low pressure mixed vapour of water, and second level condenser temperature is-196 DEG C.
(4) adopting karl Fischer Moisture Meter to record the aniline purity of collecting in first order condenser is 99.96 wt%, and collection rate is 104 g/ (m
2h); The aniline purity of collecting in the condenser of the second level is 47 wt%, and collection rate is 395 g/ (m
2h).
Claims (9)
1. the device of a separation and recovery high boiling point organic compound from low concentration aqueous solution, it is characterized in that: comprise infiltration evaporation section and fractional condensaion section, described infiltration evaporation section comprises raw material storage tank, feed liquid circulating pump, infiltration evaporation groove, is provided with infiltration vaporization membrane module in infiltration evaporation groove; Described fractional condensaion section comprises first order condenser and second level condenser, and first order condenser and second level condenser are connected in series, and second level condenser is connected with vavuum pump.
2. the method for separation and recovery high boiling point organic compound from low concentration aqueous solution, is characterized in that: comprise the following steps:
(1) aqueous solution of low-concentration organic is passed into infiltration evaporation groove, fully contact with the infiltrating and vaporizing membrane with Selective Separation organics function at the upstream side of film and reach adsorption dynamics and balance;
(2) produce low-voltage vacuum by vavuum pump in infiltrating and vaporizing membrane downstream, the high boiling point organic compound-water making upstream side be adsorbed on film surface is vaporized, and forms low pressure mixed vapour through film at the downstream desorption of infiltrating and vaporizing membrane;
(3) the low pressure mixed vapour of the downstream enrichment of film is passed into successively the condenser of two series connection, the first condenser temperatures is selected according to absolute pressure numerical values recited, in first order condenser, obtain the liquid high boiling point organic compound of high-purity, purity is greater than 99.9wt%;
(4) water vapour be not condensed and fraction organic steam are trapped within the condenser of the second level, and second level condenser is connected with infiltration evaporation groove, are transported in infiltration evaporation groove by fraction organic steam and carry out secondary separation recovery.
3. the method for separation and recovery high boiling point organic compound from low concentration aqueous solution according to claim 2, is characterized in that: described low concentration aqueous solution is the aqueous solution of organic concentration in 0.1 ~ 8 wt% scope.
4. the method for separation and recovery high boiling point organic compound from low concentration aqueous solution according to claim 2, is characterized in that: described high boiling point organic compound is boiling point at the amine of 150 ~ 230 DEG C of scopes and furan nucleus series normal temperature liquid state organics.
5. the method for separation and recovery high boiling point organic compound from low concentration aqueous solution according to claim 4, is characterized in that: described high boiling point organic compound is furfural or aniline.
6. the method for separation and recovery high boiling point organic compound from low concentration aqueous solution according to claim 2, is characterized in that: the described infiltrating and vaporizing membrane with Selective Separation organics function is polyether-block-polyamide film.
7. the method for separation and recovery high boiling point organic compound from low concentration aqueous solution according to claim 2, is characterized in that: the pressurized vacuum conditions in described infiltrating and vaporizing membrane downstream is: absolute pressure is in 30 ~ 2000 Pa scopes.
8. the method for separation and recovery high boiling point organic compound from low concentration aqueous solution according to claim 2, is characterized in that: described first order condenser temperature controls at-30 ~ 30 DEG C; The temperature of second level condenser is-200 ~-50 DEG C.
9. the method for separation and recovery high boiling point organic compound from low concentration aqueous solution according to claim 2, is characterized in that: the initial temperature of the aqueous solution of described low-concentration organic is 30 ~ 95 DEG C.
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| CN110538480A (en) * | 2019-09-25 | 2019-12-06 | 上海电气集团股份有限公司 | condensing system and condensing method |
| CN111115939A (en) * | 2020-02-24 | 2020-05-08 | 上海电气集团股份有限公司 | Organic wastewater treatment system and method |
| CN111203109A (en) * | 2020-01-15 | 2020-05-29 | 南京工业大学 | Novel pervaporation circulation heat exchange system and method |
| CN112537873A (en) * | 2020-10-12 | 2021-03-23 | 太原理工大学 | Treatment process and device for coal chemical wastewater containing fine dust |
| CN114716098A (en) * | 2022-03-25 | 2022-07-08 | 上海电气集团股份有限公司 | Treatment method and treatment system for crystalline silicon texturing wastewater |
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Application publication date: 20150506 |