CN202343204U - Vacuum microwave desorption ethanol-loaded activated carbon device - Google Patents

Vacuum microwave desorption ethanol-loaded activated carbon device Download PDF

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Publication number
CN202343204U
CN202343204U CN2011204332328U CN201120433232U CN202343204U CN 202343204 U CN202343204 U CN 202343204U CN 2011204332328 U CN2011204332328 U CN 2011204332328U CN 201120433232 U CN201120433232 U CN 201120433232U CN 202343204 U CN202343204 U CN 202343204U
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quartz glass
ethanol
microwave
vacuum
active carbon
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CN2011204332328U
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冯权莉
宁平
连明磊
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Kunming University of Science and Technology
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Kunming University of Science and Technology
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Abstract

The utility model discloses a vacuum microwave desorption ethanol-loaded activated carbon device, belonging to the technical field of industrial water treatment. The device utilizes the separation effect of microwave desorption and the enhancement function of reduced pressure distillation to the separation effect of microwave desorption to perform efficient separation and purification to an ethanol-water system which is loaded on activated carbon. The device comprises a microwave desorption device, a quartz glass reactor, a condenser, a distillate collecting container, a buffer bottle, a vacuum pump, a sheathed thermocouple, a perforated quartz glass sieve plate, a digital display temperature indicator and a vacuum meter. The device also comprises a buffer bottle (5), a vacuum pump (6) and a vacuum meter (12), wherein the collecting container (4) is connected at the back of the buffer bottle (5) and the vacuum pump (6), the vacuum meter (12) is arranged on the buffer bottle (5) and the entire system can keep good tightness. The vacuum microwave desorption ethanol-loaded activated carbon device has the advantages that the device is simple and fast in operation and easy in control and has high regenerated carbon adsorption capacity, less quality loss, sharp peak of ethanol exit concentration curve in a desorption process and high peak value, and high concentration ethanol can be collected in different tanks.

Description

The device of ethanol active carbon is carried in a kind of vacuum microwave desorb
Technical field
The utility model relates to the device that the ethanol active carbon is carried in a kind of vacuum microwave desorb, belongs to the Treatment of Industrial Water technical field.
Background technology
The a large amount of weak liquors that produce in the alcohol industry production process mainly contain ethanol (4%~8%), a small amount of lipid and acid.At present this type weak liquor is mainly adopted the method for direct discharging.Because the ethanol content in the weak liquor is very low, and water can form azeotropic mixture with ethanol, so traditional heating fractional method is very difficult with it separation, and is difficult to produce a desired effect with general wastewater processing technology.
Active carbon is a kind of black porous solid adsorption material, is widely used in the environmental protection, is used to eliminate atmosphere pollution--processing of desulfurization removing nitric and various industrial wastewaters etc.Active carbon has very strong adsorption capacity to the organic matter in the water.To weak liquor, if adopt active carbon adsorption to handle, both recyclable ethanol wherein can solve problem of environmental pollution again.
Reclaim the low-concentration ethanol in the weak liquor with active carbon adsorption; Whether economically viable decisive factor is except the theoretical research basis of adsorption process for this method; The selection of active carbon desorption regeneration and theoretical research thereof are important too, otherwise will certainly bring treatment cost high, cause secondary pollution, administer problems such as not thorough.
The economy of active carbon adsorption depends primarily on regeneration.At present, regeneration method of active carbon mainly contains following several big type: thermal regeneration method, medicament method of reproduction, bio-regeneration method, chemical regeneration method, wet oxidation method of reproduction etc.Wherein the thermal regeneration method is that using, study maximum in the various renovation process also is the most ripe a kind of method.The desorb of tradition alternating temperature can realize through indirect adsorbent or direct the contact with hot gas.To active carbon, often utilize steam to come desorb, because the active carbon coefficient of heat conduction is lower, make whole fixed bed be heated to adsorbate by the temperature of desorb, need the chronic of heating.Another shortcoming of alternating temperature desorb is that energy consumption is big; It is temperature required that regeneration not only need rise to desorb with adsorbate, and for making the further activation of adsorbent, also need temperature further is raised to the activation temperature of adsorbent; And after the heating for multiple times cooling, scaling loss is serious.If utilize superheated steam regeneration, fixed bed is also dry again before adsorbing again.If the organic matter of desorb is moisture, water and organic separation equipment must be set also.
The microwave desorption technique is researched and developed to the purified treatment of low-concentration industrial organic exhaust gas, compares with traditional hot renovation process, and the heating using microwave desorption and regeneration has following advantage: 1) microwave plays the deep layer heat effect to reactant; 2) microwave heating temperature is even; 3) desorption rate is fast; 4) under microwave irradiation, the loss of the electronics of the various adsorbates that are evaporated is different, therefore can realize the selection heating to adsorbate.
Application number is 200820081273.3 " device of ethanol active carbon is carried in a kind of microwave desorb ", discloses a kind of normal pressure microwave desorption apparatus at nitrogen atmosphere.It is following not enough that this installs existence: 1) operating cost is high, necessary use nitrogen in service, otherwise just influence desorption effect, certainly will increase the operating cost expense like this; 2) desorption effect is good not as the vacuum desorption device, and under the similarity condition, vacuum plant desorb concentration of ethanol is at least than high by 5% (except when microwave power is very low) of atmospheric unit; 3) atmospheric unit is separated the at high temperature easy magnesium oxide/absorbent charcoal of oxygen uptake, and the active carbon proportion of goods damageds are high, and this also will increase equipment operating cost expense.
Purification for the low-concentration industrial volatile organic waste gas is reclaimed; It is both economy and effective method that the organic matter active carbon is carried in the microwave desorb, but the vacuum microwave desorption apparatus that vacuum technique is combined with the microwave desorption technique that also reclaims to low-concentration ethanol in the weak liquor at present.
Summary of the invention
The purpose of the utility model is to solve the deficiency of prior art; Provide a kind of vacuum microwave desorb to carry the device of ethanol active carbon; To in weak liquor, low-concentration ethanol being adsorbed saturated year ethanol active carbon, adopt the vacuum microwave desorption apparatus to come desorb to carry the ethanol active carbon, the ethanol-water system of load on the isolating active charcoal; Divide a jar collection to obtain the different stage alcohol product, active carbon is able to regeneration simultaneously.
The device of ethanol active carbon is carried in this vacuum microwave desorb; Comprise microwave desorption apparatus 1, quartz glass reactor 2, condenser 3, distillate collection container 4, armoured thermocouple 8, punching quartz glass sieve plate 9 and digital display temperature indicator 11; Wherein open a circular hole that is complementary with quartz glass reactor 2 external diameters at microwave desorption apparatus 1 center of top position, quartz glass reactor 2 is inserted in the microwave cavity through circular hole and is fixed, the sealing of quartz glass reactor 2 lower ends; The probe of measuring the armoured thermocouple 8 of temperature is inserted into and carries the position of ethanol active carbon 7 beds near the center; Digital display temperature indicator 11 is connected with armoured thermocouple 8, and quartz glass reactor 2 top manifold are connected with condenser 3, and condenser 3 backs receive collection container 4; This device also comprises surge flask 5, vavuum pump 6 and vacuum meter 12; Collection container 4 backs connect surge flask 5 and vavuum pump 6, and vacuum meter 12 is arranged on the surge flask 5, is used to indicate the system vacuum degree.
The described vavuum pump 6 of the utility model is circulation ability of swimming vavuum pump.
The described quartz glass reactor 2 of the utility model is the structure of being made up of quartz glass tube and punching quartz glass sieve plate 9; The quartz glass sieve plate 9 of punching is installed on position, quartz glass tube middle and lower part; And on sieve plate 9 even shakedown one deck quartz glass cotton, be used for holder and carry an ethanol active carbon.
The described condenser 3 of the utility model is more than one water-cooled serpentine (trombone) cooler, adopts series system to connect, and collection container 4 is that receiving flask commonly used is gone up in industry.
Heating using microwave has the selectivity this point, and water is resultful with the separating of component that this type of ethanol can form azeotropic mixture in the ethanol active carbon desorption process for carrying; The second alcohol and water is different to the absorption efficiency of microwave; Cause desorption rate different, form sharp-pointed ethanol exit concentration curve.
Adopt decompression distillation, pressure reduces, and the ethanol in the gas phase increases, and constant boiling point is moved to the direction that increases concentration of alcohol.The experimental study of this device shows, this rule is still set up under the situation of carrying the ethanol active carbon with the microwave for the heating source desorb, and because microwave have conventional heating incomparable selectivity, this rule is reflected more clearly.Compared with the desorb of normal pressure microwave, the peak shape of the exit concentration curve of year ethanol active carbon vacuum microwave desorb is more sharp-pointed, and peak value is higher, explains that the desorption gas composition difference of different periods of desorption process is bigger, and separating effect is better.Operation under vacuum condition can realize this microwave desorption apparatus to loading on the high efficiency separation refining effect of the ethanol-water system on the active carbon, divides jar collection distillate to obtain the alcohol product of high concentration, and active carbon is able to regeneration simultaneously.
To the utility model, result of study shows that microwave power is high more; Desorb is fast more, and the peak shape of the ethanol exit concentration curve of desorption process is sharp-pointed more, and peak value is high more; And more early occur; The desorption gas composition difference that the different periods of desorption process are described is big more, and the separating effect of vacuum microwave desorb is good more, helps the branch jar and collects the ethanol that obtains high concentration.But increase in power, the mass rate of material loss of regenerated carbon also will increase, and therefore will take all factors into consideration microwave power to carrying the influence of ethanol active carbon vacuum microwave desorb, should select microwave power according to the specific requirement of practical application in industry.
The utility model is under vacuum condition, to carry out microwave desorb operation, compares with normal pressure microwave desorption apparatus, and this vacuum microwave desorption apparatus has following advantage:
1) adopt decompression distillation, pressure reduces, and the ethanol in the gas phase increases, and constant boiling point is moved to the direction that increases concentration of alcohol;
2) take normal pressure to adsorb, vacuumize the transformation sorption cycle (PSA) of desorb, not only strengthened desorption rate, and between reactor and condenser, formed barometric gradient, stripping gas can in time be taken the reactor condensation out of;
3) carry the ethanol active carbon and in microwave field, heat up very soon, take air away, prevent airborne oxygen magnesium oxide/absorbent charcoal at high temperature, reduce the active carbon loss, practice thrift cost.
The utlity model has simple in structurely, easy and simple to handle, speed is fast; Control easily; The ethanol exit concentration curve peak shape that the regenerated carbon adsorption capacity is high, mass loss reaches desorption process less is sharp-pointed, and peak value is high, can divide jar to collect the alcohol product of different stage; The concentration of alcohol of collecting is high, the characteristics that operating cost is low.
Description of drawings
Fig. 1 is that ethanol active carbon device sketch map is carried in the vacuum microwave desorb of the utility model.
Fig. 2 is the microwave desorb part and the temperature measurement fraction device sketch map of the utility model.
Fig. 3 is the quartz glass sieve plate sketch map with holes of the utility model.
Among the figure: the 1st, microwave desorption apparatus, the 2nd, quartz glass reactor, the 3rd, condenser, the 4th, distillate collection container, the 5th, surge flask, the 6th, vavuum pump, the 7th, active carbon, the 8th, armoured thermocouple, the 9th, punching quartz glass sieve plate, the 10th, micro-wave oven, the 11st, digital display temperature indicator, the 12nd, vacuum meter, the 13rd, sieve aperture.
The specific embodiment
Below in conjunction with accompanying drawing and embodiment, the utility model is done further to set forth, but the protection domain of the utility model is not limited to said content.
Embodiment 1: the device of ethanol active carbon is carried in the desorb of this vacuum microwave; Comprise microwave resolver 1, quartz glass reactor 2, condenser 3, distillate collection container 4, surge flask 5, circulation ability of swimming vavuum pump 6, armoured thermocouple 8, punching quartz glass sieve plate 9, digital display temperature indicator 11 and vacuum meter 12; Wherein open a circular hole that is complementary with quartz glass reactor 2 external diameters at microwave resolver 1 center of top position; Quartz glass reactor 2 is inserted in the microwave cavity through circular hole and is fixed, the sealing of quartz glass reactor 2 lower ends, and the probe of measuring the armoured thermocouple 8 of temperature is inserted into and carries the position of ethanol active carbon 7 beds near the center; Digital display temperature indicator 11 is connected with armoured thermocouple 8; Quartz glass reactor 2 top manifold are connected with condenser 3, and condenser 3 backs receive collection container 4, and collection container 4 backs connect surge flask 5 and vavuum pump 6; Vacuum meter 12 is arranged on the surge flask 5, is used to indicate the system vacuum degree; Quartz glass reactor 2 is the structure of being made up of quartz glass tube and punching quartz glass sieve plate 9, and quartz glass sieve plate 9 with holes is installed on position, quartz glass tube middle and lower part, and on sieve plate 9 even shakedown one deck quartz glass cotton, be used for a holder year ethanol active carbon.
Shown in Fig. 1~3, it is following to install concrete design parameter:
(1) microwave desorption apparatus 1 is the WP800 type Glanz household microwave oven 10 of reequiping voluntarily, and microwave power is adjustable continuously;
(2) quartz glass sieve plate 9 be positioned at quartz glass tube apart from the lower end 6cm place; Quartz glass tube is Φ 30mm * 200mm; The sieve plate 30mmi.d of punching quartz glass sieve plate, sieve aperture 2mmi.d., nine sieve apertures 13 are uniformly distributed in the square area at sieve plate center;
(3) vavuum pump is SHZ-D (III) circulation ability of swimming vavuum pump, and the absolute pressure of control vacuum plant is at 22.2kpa;
(4) condenser adopts the water-cooled serpentine (trombone) cooler of three series connection, and logical condensed water is partially immersed in coiled pipe in the bosh.
Carry out the active carbon employing ature of coal granular activated carbon that desorb is handled; Active carbon is immersed in the hydrochloric acid of mass concentration 6%, in boiling water, boils 30min then, with distilled water repeatedly rinsing to remove bulky grain and impurity; Rinsing to washings pH value 6 back 105 ℃ dry to constant weight; With 80 mesh sieve elimination granule and powder, be stored in the drier, subsequent use as pretreated seed activity carbon adsorbent.
Technological process:
Prepare saturated year ethanol active carbon: adopt intermittently dynamics device; Adsorption temp is a normal temperature; With 10.000g through pretreated granular activated carbon mixing and absorption in the ethanol water of 300mL mass concentration 4.0%; And with magnetic agitation 2h, with vavuum pump suction filtration 5min, the saturated activity charcoal that leaches is waited until desorb.
The control of microwave desorption and regeneration system and system vacuum degree: place above saturated activity charcoal in the quartz glass reactor, desorb in above-mentioned vacuum microwave desorption apparatus, system vacuum is controlled to be absolute pressure at 22.2kpa.When microwave operational frequencies is 2450MHz, microwave power 680W, during exposure time 90s, desorption efficiency is 99.58%, the regenerated carbon mass rate of material loss is 2.66%.
The condensing and recycling of desorption gas: the mixing of the second alcohol and water that comes out from the reactor head pipeline is separated gassing through condenser 3 condensations, and distillate divides according to ethanol exit concentration curve jar to be collected, and divides that the ethanol mass concentration reaches as high as 64% in jar distillate of collecting.
Can be with the distillate of low concentration again through charcoal absorption-vacuum microwave desorb with further purification ethanol.The utility model adopts above desorption technique condition, and the weak liquor of ethanol mass concentration 4.0% divides a jar collection distillate, the highest ethanol that can be recovered to mass concentration 98% after three charcoal absorptions-vacuum microwave desorption cycle.
Embodiment 2: concrete structure, design parameter, technological process and the equipment that the device of ethanol active carbon is carried in the desorb of this vacuum microwave connects identical with embodiment 1, no longer repeats.Condenser adopts the water-cooled serpentine (trombone) cooler of 2 series connection.
Active carbon is immersed in the hydrochloric acid of mass concentration 8%; In boiling water, boil 30min then; With distilled water repeatedly rinsing removing bulky grain and impurity, rinsing to washings pH value 6 back 105 ℃ dry to constant weight, with 80 mesh sieve elimination granule and powder; Be stored in the drier, subsequent use as pretreated seed activity carbon adsorbent.
Prepare saturated year ethanol active carbon: adopt intermittently dynamics device; Adsorption temp is a normal temperature; With 10.000g through pretreated granular activated carbon mixing and absorption in the ethanol water of 300mL mass concentration 4.0%; And with magnetic agitation 2h, with vavuum pump suction filtration 5min, the saturated activity charcoal that leaches is waited until desorb.
Saturated year ethanol active carbon places the desorb of above-mentioned vacuum microwave desorption apparatus more than inciting somebody to action, and system vacuum is controlled to be absolute pressure at 22.2kpa, when microwave operational frequencies is 2450MHz; Microwave power 320W; During exposure time 90s, desorption efficiency is 96.67%, and the regenerated carbon adsorptive value is 166.57mg/g (new charcoal methylenum careuleum adsorptive value is 146.26mg/g); Mass rate of material loss is 1.21%, and the ethanol mass concentration reaches as high as 54% in the branch jar distillate of collecting.
Can be with the distillate of low concentration again through charcoal absorption-vacuum microwave desorb with further purification ethanol.The utility model adopts above desorption technique condition, and the weak liquor of ethanol mass concentration 4.0% divides a jar collection distillate, the highest ethanol that can be recovered to mass concentration 96% after three charcoal absorptions-vacuum microwave desorption cycle.
Embodiment 3: concrete structure, design parameter, technological process and the equipment that the device of ethanol active carbon is carried in the desorb of this vacuum microwave connects identical with embodiment 1, no longer repeats.Condenser adopts the water-cooled serpentine (trombone) cooler of 4 series connection.
Active carbon is immersed in the hydrochloric acid of mass concentration 5%, in boiling water, boils 30min then, with distilled water repeatedly rinsing removing bulky grain and impurity, rinsing to washings pH value 5 backs 105 OC is dried to constant weight, with 80 mesh sieve elimination granule and powder, is stored in the drier, and is subsequent use as pretreated seed activity carbon adsorbent.
Prepare saturated year ethanol active carbon: adopt intermittently dynamics device; Adsorption temp is a normal temperature; With 10.000g through pretreated granular activated carbon mixing and absorption in the ethanol water of 300mL mass concentration 4.0%; And with magnetic agitation 2h, with vavuum pump suction filtration 5min, the saturated activity charcoal that leaches is waited until desorb.
Saturated year ethanol active carbon places the desorb of above-mentioned vacuum microwave desorption apparatus more than inciting somebody to action; System vacuum is controlled to be absolute pressure at 22.2kpa, when microwave operational frequencies is 2450MHz, and microwave power 136W; During exposure time 145s; Desorption efficiency is 48.54%, and the regenerated carbon mass rate of material loss is 0.89%, and the ethanol mass concentration reaches as high as 47% in the branch jar distillate of collecting.
Can be with the distillate of low concentration again through charcoal absorption-vacuum microwave desorb with further purification ethanol.The utility model adopts above desorption technique condition, and the weak liquor of ethanol mass concentration 4.0% divides a jar collection distillate, the highest ethanol that can be recovered to mass concentration 93% after three charcoal absorptions-vacuum microwave desorption cycle.

Claims (4)

1. the device of ethanol active carbon is carried in a vacuum microwave desorb; Mainly comprise microwave desorption apparatus (1), quartz glass reactor (2), condenser (3), distillate collection container (4), armoured thermocouple (8), punching quartz glass sieve plate (9) and digital display temperature indicator (11); Wherein open a circular hole that is complementary with quartz glass reactor (2) external diameter at microwave desorption apparatus (1) center of top position; Quartz glass reactor (2) is inserted in the micro-wave oven furnace chamber through circular hole and is fixed; The sealing of quartz glass reactor (2) lower end; The probe of armoured thermocouple (8) is inserted into and carries the position of ethanol active carbon (7) bed near the center, and digital display temperature indicator (11) is connected with armoured thermocouple (8), and quartz glass reactor (2) top manifold is connected with condenser (3); Condenser (3) back receives collection container (4); It is characterized in that: this device also comprises surge flask (5), vavuum pump (6) and vacuum meter (12), and collection container (4) back connects surge flask (5) and vavuum pump (6), and vacuum meter (12) is arranged on the surge flask (5).
2. the device of ethanol active carbon is carried in vacuum microwave desorb according to claim 1, it is characterized in that: vavuum pump (6) is a circulation ability of swimming vavuum pump.
3. the device of ethanol active carbon is carried in vacuum microwave desorb according to claim 1; It is characterized in that: the structure of quartz glass reactor (2) for forming by quartz glass tube and punching quartz glass sieve plate (9); Punching quartz glass sieve plate (9) is installed on position, quartz glass tube middle and lower part, and on sieve plate (9), lays the quartz glass cotton layer equably.
4. carry the device of ethanol active carbon according to claim 1,2 or 3 described vacuum microwave desorbs, it is characterized in that: condenser (3) is more than one water-cooled serpentine (trombone) cooler, adopts series system to connect.
CN2011204332328U 2011-11-04 2011-11-04 Vacuum microwave desorption ethanol-loaded activated carbon device Expired - Fee Related CN202343204U (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103272831A (en) * 2013-03-28 2013-09-04 南京工业大学 Apparatus for integrated catalytic oxidation restoration of organochlorine heavily-polluted soil, and technology thereof
CN104891700A (en) * 2015-06-17 2015-09-09 齐齐哈尔医学院 Temperature difference type circulating water purifier
CN106110697A (en) * 2016-08-23 2016-11-16 成都慧信实验设备有限公司 Box electrothermic retorting device
CN115779879A (en) * 2022-12-14 2023-03-14 南通斐腾新材料科技有限公司 Zeolite rapid desorption organic waste gas recovery device and desorption recovery method thereof

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103272831A (en) * 2013-03-28 2013-09-04 南京工业大学 Apparatus for integrated catalytic oxidation restoration of organochlorine heavily-polluted soil, and technology thereof
CN104891700A (en) * 2015-06-17 2015-09-09 齐齐哈尔医学院 Temperature difference type circulating water purifier
CN106110697A (en) * 2016-08-23 2016-11-16 成都慧信实验设备有限公司 Box electrothermic retorting device
CN115779879A (en) * 2022-12-14 2023-03-14 南通斐腾新材料科技有限公司 Zeolite rapid desorption organic waste gas recovery device and desorption recovery method thereof

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