CN104148039A - Method for acquiring activated regenerated paracetamol pharmaceutical waste activated carbon through microwave heating - Google Patents

Method for acquiring activated regenerated paracetamol pharmaceutical waste activated carbon through microwave heating Download PDF

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Publication number
CN104148039A
CN104148039A CN201410380076.1A CN201410380076A CN104148039A CN 104148039 A CN104148039 A CN 104148039A CN 201410380076 A CN201410380076 A CN 201410380076A CN 104148039 A CN104148039 A CN 104148039A
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China
Prior art keywords
paracetamol
active carbon
medicinal
activated carbon
microwave
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CN201410380076.1A
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夏洪应
张声洲
张利波
吴坚
彭金辉
王仕兴
刘秉国
许磊
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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 invention relates to a method for acquiring activated regenerated paracetamol pharmaceutical waste activated carbon through microwave heating and belongs to the technical field of resource recycling. The method for acquiring paracetamol pharmaceutical waste activated carbon through microwave heating comprises the following specific steps: paracetamol pharmaceutical waste activated carbon is placed in a microwave oven with power ranging from 0 to 40kW; the temperature rises to 500-700 DEG C at the heating rate of 145-175 DEG C/min and heat preservation is performed for 8-10 min; and the microwave heated paracetamol pharmaceutical waste activated carbon is dried for 24-48 h at the temperature ranging from 105 to 115 DEG C and then is cooled to acquire activated regenerated paracetamol pharmaceutical waste activated carbon. The method works without the use of protective gas, thereby simplifying the test process and operation, consuming less energy and producing no pollution. The activated regenerated activated carbon is characterized in that the absorption property is restored, the specific surface area reaches 1000 m<2>/g above, the total pore volume ranges from 0.95 ml/g to 1.10 ml/g, and the activating regeneration yield exceeds 90%.

Description

The method of the medicinal waste active carbon of a kind of microwave heating activation regeneration paracetamol
Technical field
The method that the present invention relates to the medicinal waste active carbon of a kind of microwave heating activation regeneration paracetamol, belongs to resource circulation utilization technical field.
Background technology
Paracetamol is one of at present main antalgesic, to alimentary canal nonirritant, also can not cause blood coagulation disorders, becomes the main development kind of analgesic-antipyretic.Paracetamol can produce a large amount of impurity in preparation process, produces huge pollution for water resource, so for the most important thing that is treated as of paracetamol sewage.Active carbon has mainly played impurity and the effect except look of removing in paracetamol production process.In paracetamol production process, active carbon powder drops into from reactor top, with the abundant hybrid reaction of paracetamol waste water, and then by filter, waste active carbon is filtered out.Because active carbon is using adsorption capacity later obviously to decline, directly abandon or directly burn so usually not treated.Do like this and not only caused the huge wasting of resources, but also polluted environment.So become the focus of research in the present age for the activating and regenerating technology of discarded active carbon, also become the important topic of pendulum in face of numerous scientific workers.
Along with active carbon is applied widely, activating and regenerating technology more and more causes people's attention.And the feature such as the selective heating of microwave heating technique, firing rate be fast, pollution-free has increased the efficiency of experiment greatly, shorten the reaction time of experiment, greatly reduce energy consumption.
The present invention, using the paracetamol medicinal carbon discarded as raw material, by the mode of heating using microwave, carries out activating and regenerating to discarded active carbon under the condition that does not pass into any protective gas and activated gas.Because promptly making the moisture of active carbon inside, heating using microwave becomes steam, the steam producing contributes to the dredging in active carbon duct and reproduces very much, so recovered rapidly activated carbon adsorptive capacity, accomplish recycling of discarded object, turned waste into wealth, greatly reduced energy resource consumption, realize recycling of discarded object, greatly improve the comprehensive utilization ratio of resource, also reduced the pressure of environmental pollution aspect, produced significant economy and ecological benefits.
In the patent that applicant is 200510019670.9 in the patent No., a kind of " microwave plasma regeneration method of active carbon " disclosed, this method is to utilize microwave-excitation irony discharge body to produce plasma, then plasma is oxidized the organic matter being adsorbed on damp state active carbon, electrolysis degradation of organic substances in simultaneously producing between irony discharge body, active carbon and organic matter, after peroxidating and degraded, make to obtain regeneration activity recovery with the industrial activited carbon of crossing.Foregoing invention is compared with the present invention, the one, raw material of the present invention is powder-material, if add irony discharge body and obstructed protective gas in activation process, because its local electronic temperature is at least 10000 DEG C, be that this discarded active carbon of 200 objects is to be very easy to scaling loss for granularity; The 2nd, foregoing invention has been added irony discharge body, easily form iron ion, and active carbon has the function of adsorbing metal ions under the environment of high temperature humidity.For being used for specially the active carbon of paracetamol production process, can produce secondary pollution to this medicine if be mingled with some metal ions, patient is produced to immeasurable security risk.
In the patent that applicant is 201110343234.2 in the patent No., a kind of " method of microwave-assisted regeneration active carbon " disclosed, this method is that the waste active carbon to produce in sugared production process is raw material, utilize the sodium tartrate aqueous solution or sodium citrate aqueous solution that the organic components such as the caramel in activated carbon granule surface and macropore are leached, then add water and mix and add activating agent absolute ethyl alcohol, Sodium Polyacrylate, natrium citricum or their mixture, with ammoniacal liquor, NaOH or their mixture are adjusted at system pH between 8.5~10.5, be placed in microwave irradiation device radiation treatment 10~30min, thereby realize the regeneration of active carbon.Foregoing invention is compared with the present invention: the one, and said method has been introduced the materials such as absolute ethyl alcohol, Sodium Polyacrylate, natrium citricum in activation process, not only making experimental implementation become complicated cost has increased, but also the secondary pollution that has brought regenerated carbon, and the present invention does not introduce any auxiliary reagent, cleanliness without any pollution, operates also simple completely; The 2nd, in said method, the fineness of discarded active carbon is 5 order~200 orders, and in this experiment, requirement is 200 orders, and it is very very difficult in the situation that fineness is so little, but reaching so good regeneration effect comparatively speaking; The 3rd, in the present invention, microwave activation temperature retention time needs only 8 ~ 10min, and the above-mentioned invention microwave radiation processing 10min~30min that authorized has reduced energy consumption in contrast.
Summary of the invention
For problem and the deficiency of above-mentioned prior art existence, the invention provides the method for the medicinal waste active carbon of a kind of microwave heating activation regeneration paracetamol.This activation method does not pass into protective gas, has simplified experiment flow, operates quite simply, and energy consumption is low and pollution-free, and this activating and regenerating active carbon out recovers original absorption property substantially, and its specific area reaches 1000m 2more than/g, total pore volume is 0.95 ~ 1.10ml/g, and the present invention is achieved through the following technical solutions.
The method of the medicinal waste active carbon of a kind of microwave heating activation regeneration paracetamol, its concrete steps are as follows: first medicinal paracetamol waste active carbon being placed in to power is 0 ~ 40kW microwave oven, after temperature being risen to 500 ~ 700 DEG C with the heating rate of 145 ~ 175 DEG C/min, be incubated 8 ~ 10min, by medicinal the paracetamol after heating using microwave waste active carbon dry 24 ~ 48h under 105 ~ 115 DEG C of conditions, can prepare activating and regenerating paracetamol medicinal carbon after cooling.
The medicinal waste active carbon granularity of described paracetamol is 200 orders, and moisture content is 30 ~ 40%, and methylene blue value is 40 ~ 50mg/g.
The invention has the beneficial effects as follows: (1) this method production technology is very simple, does not pass into protective gas and activated gas, has simplified experiment flow, operate quite simply, energy consumption is lower, with low cost, and pollution-free; (2) this active carbon contains higher moisture, produces rapidly a large amount of steam by heating using microwave, is more conducive to the dredging in duct and reproduces than conventional heating mode, makes activating and regenerating active carbon out recover original absorption property; (3) this method can reduce this active carbon work at the consumption of manufacturing in paracetamol process, has realized the comprehensive utilization of resources of this discarded object simultaneously, has reduced the discharge of discarded object, thereby has reduced environmental pollution, has effectively realized the sustainable development of enterprise.
Brief description of the drawings
Fig. 1 is that the active carbon of the embodiment of the present invention 1 activating and regenerating is at the nitrogen adsorption curve map of 77K;
Fig. 2 is the pore volume distribution figure of the active carbon of the embodiment of the present invention 1 activating and regenerating;
Fig. 3 is the scanning electron microscope (SEM) photograph of waste active carbon of the present invention;
Fig. 4 is the scanning electron microscope (SEM) photograph of the active carbon of the embodiment of the present invention 1 activating and regenerating.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the invention will be further described.In experiment, specific area adopts Full-automatic physical chemical adsorption instrument (Autosorb-1-C, Kang Ta company) to measure, and methylene blue adsorption value is measured according to national standard GB/T 12496.10-1999.
Embodiment 1
The method of the medicinal waste active carbon of this microwave heating activation regeneration paracetamol, its concrete steps are as follows: first medicinal 20g paracetamol waste active carbon being placed in to power is 40kW microwave oven, after temperature being risen to 500 DEG C with the heating rate of 145 ~ 150 DEG C/min, be incubated 8min, by medicinal the paracetamol after heating using microwave waste active carbon dry 24h under 105 DEG C of conditions, can prepare activating and regenerating paracetamol medicinal carbon after cooling; Wherein the medicinal waste active carbon granularity of paracetamol is 200 orders, and moisture content is 40%, and methylene blue value is 48mg/g.
The methylene blue adsorption value of the activating and regenerating paracetamol medicinal carbon preparing through above-mentioned steps is 165.0mg/g, and activating and regenerating yield is 94.38%.
This activating and regenerating paracetamol medicinal carbon, at the nitrogen adsorption curve map of 77K as shown in Figure 1, the pore volume distribution figure of active carbon as shown in Figure 2, the scanning electron microscope (SEM) photograph of waste active carbon as shown in Figure 3, as shown in Figure 4, the BET specific area that the data from Fig. 1 can calculate waste active carbon reaches 252.6m to the active carbon ESEM of activating and regenerating 2/ g, the BET specific area of the active carbon of activating and regenerating reaches 1089m 2/ g, the total pore volume that can calculate waste active carbon from Fig. 2 data is 0.46ml/g, the total pore volume of the active carbon of activating and regenerating is 0.98ml/g.
Embodiment 2
The method of the medicinal waste active carbon of this microwave heating activation regeneration paracetamol, its concrete steps are as follows: first medicinal paracetamol waste active carbon being placed in to power is 40kW microwave oven, after temperature being risen to 600 DEG C with the heating rate of 150 ~ 170 DEG C/min, be incubated 10min, by medicinal the paracetamol after heating using microwave waste active carbon dry 48h under 115 DEG C of conditions, can prepare activating and regenerating paracetamol medicinal carbon after cooling; The medicinal waste active carbon granularity of described paracetamol is 200 orders, and moisture content is 36%, and methylene blue value is 50mg/g.
The methylene blue adsorption value of the activating and regenerating paracetamol medicinal carbon preparing through above-mentioned steps is 187.5mg/g, and activating and regenerating yield is 90.23%.
Embodiment 3
The method of the medicinal waste active carbon of this microwave heating activation regeneration paracetamol, its concrete steps are as follows: first medicinal paracetamol waste active carbon being placed in to power is 1kW microwave oven, after temperature being risen to 700 DEG C with the heating rate of 145 ~ 150 DEG C/min, be incubated 8min, by medicinal the paracetamol after heating using microwave waste active carbon dry 36h under 110 DEG C of conditions, can prepare activating and regenerating paracetamol medicinal carbon after cooling; Wherein the medicinal waste active carbon granularity of paracetamol is 200 orders, and moisture content is 34%, and methylene blue value is 40mg/g.
The methylene blue adsorption value of the activating and regenerating paracetamol medicinal carbon preparing through above-mentioned steps is 172.5mg/g, and activating and regenerating yield is 90.54%.
Embodiment 4
The method of the medicinal waste active carbon of this microwave heating activation regeneration paracetamol, its concrete steps are as follows: first medicinal paracetamol waste active carbon being placed in to power is 20kW microwave oven, after temperature being risen to 550 DEG C with the heating rate of 170 ~ 175 DEG C/min, be incubated 9min, by medicinal the paracetamol after heating using microwave waste active carbon dry 24h under 105 DEG C of conditions, can prepare activating and regenerating paracetamol medicinal carbon after cooling; Wherein the medicinal waste active carbon granularity of paracetamol is 200 orders, and moisture content is 30%, and methylene blue value is 42mg/g.
The methylene blue adsorption value of the activating and regenerating paracetamol medicinal carbon preparing through above-mentioned steps is 168.5mg/g, and activating and regenerating yield is 93.76%.
By reference to the accompanying drawings the specific embodiment of the present invention is explained in detail above, but the present invention is not limited to above-mentioned embodiment, in the ken possessing those of ordinary skill in the art, can also under the prerequisite that does not depart from aim of the present invention, make various variations.

Claims (2)

1. the method for the medicinal waste active carbon of microwave heating activation regeneration paracetamol, it is characterized in that concrete steps are as follows: first medicinal paracetamol waste active carbon being placed in to power is 0 ~ 40kW microwave oven, after temperature being risen to 500 ~ 700 DEG C with the heating rate of 145 ~ 175 DEG C/min, be incubated 8 ~ 10min, by medicinal the paracetamol after heating using microwave waste active carbon dry 24 ~ 48h under 105 ~ 115 DEG C of conditions, can prepare activating and regenerating paracetamol medicinal carbon after cooling.
2. the method for the medicinal waste active carbon of microwave heating activation regeneration paracetamol according to claim 1, is characterized in that: the medicinal waste active carbon granularity of described paracetamol is 200 orders, and moisture content is 30 ~ 40%, and methylene blue value is 40 ~ 50mg/g.
CN201410380076.1A 2014-08-05 2014-08-05 Method for acquiring activated regenerated paracetamol pharmaceutical waste activated carbon through microwave heating Pending CN104148039A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105293489A (en) * 2015-11-16 2016-02-03 昆明理工大学 Regeneration method of waste active carbon for monosodium glutamate by supersonic wave and spray
CN107308926A (en) * 2017-06-02 2017-11-03 昆明理工大学 A kind of method of waste active carbon in microwave hydrogen peroxide combining and regenerating aspirin production process
CN111229191A (en) * 2020-01-19 2020-06-05 内蒙古科技大学 Efficient regeneration activation method for recycling gold-loaded activated carbon
CN113231050A (en) * 2021-04-20 2021-08-10 南京三乐微波技术发展有限公司 Method and device for regenerating waste activated carbon through microwave activation

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5235194A (en) * 1975-09-12 1977-03-17 Toyobo Co Ltd Method for regeneration of active carbon
JPS539293A (en) * 1976-07-14 1978-01-27 Ebara Corp Method and apparatus for regenerating activated carbon
CN1490419A (en) * 2003-08-30 2004-04-21 大连理工大学 Reproducing method for carrier gold activated carbon
CN1562775A (en) * 2004-04-15 2005-01-12 大连理工大学 Restoring method of activated carbon for decomposing, processing and adsorbing organic substance in waste water through microwave irradiation

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5235194A (en) * 1975-09-12 1977-03-17 Toyobo Co Ltd Method for regeneration of active carbon
JPS539293A (en) * 1976-07-14 1978-01-27 Ebara Corp Method and apparatus for regenerating activated carbon
CN1490419A (en) * 2003-08-30 2004-04-21 大连理工大学 Reproducing method for carrier gold activated carbon
CN1562775A (en) * 2004-04-15 2005-01-12 大连理工大学 Restoring method of activated carbon for decomposing, processing and adsorbing organic substance in waste water through microwave irradiation

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105293489A (en) * 2015-11-16 2016-02-03 昆明理工大学 Regeneration method of waste active carbon for monosodium glutamate by supersonic wave and spray
CN105293489B (en) * 2015-11-16 2018-03-06 昆明理工大学 A kind of method of ultrasonic atomization regenerating waste monosodium glutamate activated carbon
CN107308926A (en) * 2017-06-02 2017-11-03 昆明理工大学 A kind of method of waste active carbon in microwave hydrogen peroxide combining and regenerating aspirin production process
CN111229191A (en) * 2020-01-19 2020-06-05 内蒙古科技大学 Efficient regeneration activation method for recycling gold-loaded activated carbon
CN113231050A (en) * 2021-04-20 2021-08-10 南京三乐微波技术发展有限公司 Method and device for regenerating waste activated carbon through microwave activation

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Application publication date: 20141119