CN106311202A - Preparation method of sludge char catalyst as well as catalyst and application - Google Patents
Preparation method of sludge char catalyst as well as catalyst and application Download PDFInfo
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- CN106311202A CN106311202A CN201510387206.9A CN201510387206A CN106311202A CN 106311202 A CN106311202 A CN 106311202A CN 201510387206 A CN201510387206 A CN 201510387206A CN 106311202 A CN106311202 A CN 106311202A
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Abstract
The invention relates to a sludge char catalyzed wet air oxidation catalyst as well as a preparation method and an application thereof. Activated sludge in a urban sewage treatment plant is used as a raw material; metal elements contained in the activated sludge are used as active components; polyanion cellulose, hydroxyethyl cellulose or xanthan gum are used as molding promoters, and sludge powder and the molding promoters are fully mixed; mixing and kneading, extrusion moulding, drying, and charing and activation are carried out, in order to obtain the sludge char catalyst. The sludge char catalyst has the advantages of high activity for catalysis of the wet air oxidation reaction, low dipping amount of active components, simple preparation, easy recovery of the catalyst, low cost, and the like. The activity of the sludge char catalyst is kept after about 200 hours of continuous operation of catalysis in the wet air oxidation reaction, and the sludge char catalyst is hopeful to be applied to industrial apparatuses for catalysis and wet air oxidation treatment of high concentration organic waste water which is difficult to be biochemically degraded.
Description
Technical field
The present invention relates to a kind of sludge carbon catalytic wet oxidation catalyst and its preparation method and application, it is adaptable to CWO processes indegradable industrial effluent, belong to water technology and solid waste resource recovery disposes field.
Background technology
Improving constantly recently as China's urban wastewater treatment rate, urban wastewater treatment firm excess sludge production sharply increases.Mud is the by-product in biochemical processing procedure of sewage, multiple-microorganism Organic substance that the zoogloea formed adsorbs with it and the aggregation that inorganic matter forms.The process technique of mud routine mainly has landfill, compost, burning and building materials utilization etc..Pyrolyzing sludge process is to be 250～800 DEG C in pressure-fired, pyrolysis temperature, carries out under conditions of anoxia, stops certain time, and the Organic substance in mud is converted into gas by thermal cracking, condensed after obtain pyrolysis oil.Sludge pyrolytic oil mainly by aliphatic, alkene race and on a small quantity other compounds form.Pyrolyzing sludge technology does not produces the feature such as dioxin, recovery bio oil owing to having, and is the most increasingly paid close attention to by each side.
Wet oxidation process (Wet Air Oxidation is called for short WAO) is a kind of important poisonous, harmful, the effective treating method of high concentrated organic wastewater of degraded grown up from the 1950's.It is under the conditions of high temperature (150～350 DEG C) and high pressure (0.5～20MPa), with the oxygen in air as oxidant, in the liquid phase organic pollution is oxidized to CO2And H2The inorganic matters such as O or the chemical process of small organic molecule；There is no NO in the processX、SO2Discharge with the harmful gas such as HCl.In heterogeneous system CWAO method, catalyst is to participate in reaction, the beneficially recycling of catalyst with the form of solid.In CWAO reaction, the use of catalyst can improve oxidant utilization and organic removal rate, and therefore the development of effective catalyst is the key of the actual application of this technology.
Containing substantial amounts of Organic substance and metallic element in mud, sludge carbon catalyst can be prepared by relevant physics, chemical activation method, this catalyst is applied in CWAO system, organic clearance can be improved, realize the purpose of the treatment of wastes with processes of wastes against one another, it is achieved that the recycling of mud.
Summary of the invention
The purpose of the present invention is to propose to a kind of in CWAO reacts, there is highly active catalyst of process persistent organic pollutants and preparation method thereof, improve organic clearance, thus promote the extensive application of CWAO technology.
The present invention relates to a kind of sludge carbon catalytic wet oxidation catalyst and its preparation method and application, process organic industrial sewage for CWO.
The preparation method step of the sludge carbon catalyst that the present invention provides is as follows:
(1) mud after city domestic sewage treatment plant being dehydrated, is dried 10～48h at 80～120 DEG C, and carries out mechanical activation comminution, made 200～300 mesh sieves, and obtained sewage sludge powder；
(2), after gained sewage sludge powder mixes with shaping assistant, adding deionized water to total water content is 20～50wt.%, and after carrying out kneading, extrusion obtains column mud；Shaping assistant used is: one or both in polyanion cellulose (PAC) or hydroxyethyl cellulose (HEC), and usage amount is 0～2wt.%；Described extrusion operates, and extrudes a diameter of 2～6mm；
(3) with nitrogen as protection gas; column mud step (2) obtained is dried 2～4h with the ramp of 2～10 DEG C/min to 80～120 DEG C; then, after carrying out calcining 2～8h at 400～800 DEG C, it is cooled to room temperature, i.e. obtains sludge carbon catalyst.
The sludge carbon catalyst that can step (3) be obtained one or more solution in hydrochloric acid, sulphuric acid, nitric acid, perchloric acid, phosphoric acid, acetic acid, sodium hydroxide or the hydrogen peroxide of 5～50wt.% soaks 1～24h at a temperature of 5～80 DEG C, between sludge carbon catalyst and the solution soaked, consumption volume ratio is 1:1～1:5, sludge carbon to water outlet pH value after soaking with deionized water rinsing is 6～8, after drying at 10～105 DEG C, i.e. prepare the sludge carbon catalyst of surface modification.
Can be by the sludge carbon catalyst incipient impregnation RuCl of gained sludge carbon catalyst or surface modification3、H2PtCl6、Pd(NO3)2、RhCl3Or IrCl3In one or more solution, in Ru, Pt, Pd, Rh and Ir, one or more are as active component, in the solution impregnated, the gross mass of Ru, Pt, Pd, Rh or Ir accounts for the percentage ratio of the sludge carbon catalyst of dipping or the sludge carbon catalyst gross mass of surface modification is 0.0～5.0wt.%, crosses leaching solid product and prepares transition metal modified sludge carbon catalyst 300～500 DEG C of calcinings 2～8h.
When the sludge carbon catalyst prepared according to above-mentioned preparation method is transition metal modified sludge carbon catalyst, its for CWO process organic wastewater intermittent reaction condition be:
Catalyst amount has unlimited range, reaction temperature: 120～275 DEG C, oxygen pressure: 0.1～7.0MPa, mixing speed: 400～800r/min；
Or for CWO process organic wastewater successive reaction condition be:
Catalyst amount has unlimited range, reaction temperature: 120～275 DEG C, air pressure: 1.0～7.0MPa, air speed: 0.5～4.0h-1。
The concentration of model compound analyzed by the P1201 type high performance liquid chromatograph using Dalian Yilite Analytical Instrument Co., Ltd to produce.Use the TOC-VCPH/CPN analysis-e/or determining waste water TOC that Shimadzu Corporation produces.Thunder magnetic PHS-3C Accurate pH meter is used to measure water sample pH.
Experimental technique scheme is:
→ strength test → successive reaction evaluation prepared by column sludge carbon catalyst.
Intermittent reaction: adding 1g sludge carbon catalyst in 200mL 5000mg/L metacresol, being passed through oxygen pressure is 0.40MPa, and rotating speed is 600rpm, and temperature is 160 DEG C.
Successive reaction: adding 10mL catalyst in the reactor, volume of water sample air speed LHSV is 1h-1, reaction temperature is 180 DEG C.
High activated catalyst is selected to carry out successive reaction to evaluate its life-span.
The column sludge activity Pd/carbon catalyst of the present invention has the advantage that
1. utilize the metal contained in mud as active component, decrease the pickup of active component；
2. this catalyst has higher activity for high concentration, organic wastewater with difficult degradation thereby；
3. this catalyst has good stability during CWAO degradation of organic substances；
4. this catalyst has bigger specific surface area, and active component has good dispersibility thereon；
5. the production cost of this catalyst is relatively low.
Accompanying drawing explanation
Fig. 1 sludge carbon catalyst intermittent reaction metacresol clearance figure.
Fig. 2 sludge carbon catalyst intermittent reaction TOC clearance figure.
Fig. 3 sludge carbon catalyst successive reaction metacresol clearance figure.
Fig. 4 sludge carbon catalyst successive reaction TOC clearance figure.
Detailed description of the invention
CWAO sludge carbon catalyst of the present invention, can process organic wastewater with difficult degradation thereby, improves organic clearance, thus promotes the extensive application of CWAO technology.
The present invention is described in detail below in conjunction with embodiment and accompanying drawing.
Embodiment 1:
1. by 105 DEG C of dry 12h of city domestic sewage treatment plant mud, and carry out mechanical activation comminution, made 200 mesh sieves.
2., after gained sewage sludge powder and shaping assistant HEC (usage amount is 0.5wt.%) are sufficiently mixed, add deionized water (water content is 25wt.%), carry out extrusion after abundant kneading, extrude a diameter of 4mm.
3. with nitrogen as protection gas, the bar shaped mud of extrusion is warming up to 120 DEG C of dry 4h with 3 DEG C/min, after then carrying out calcining 4h at 600 DEG C, is cooled to room temperature, obtains sludge carbon.
4. CWAO intermittent reaction experiment condition: be 160 DEG C in temperature, oxygen pressure is 0.40MPa, mixing speed: 600r/min, sludge carbon dosage is 5g/L, and metacresol initial concentration is 5000mg/L, after reaction 90min, metacresol conversion ratio is 30.5%, and TOC clearance is 20.7%.
Embodiment 2:
1. city domestic sewage treatment plant CAST technique is produced 105 DEG C of dry 12h of mud, and carry out mechanical activation comminution, made 300 mesh sieves.
2., after gained sewage sludge powder and shaping assistant HEC (usage amount is 0.5wt.%) are sufficiently mixed, add deionized water (water content is 25wt.%), carry out extrusion after abundant kneading, extrude a diameter of 3.5mm.
3. with nitrogen as protection gas, the bar shaped mud of extrusion is warming up to 120 DEG C of dry 4h with 3 DEG C/min, after then carrying out calcining 4h at 600 DEG C, is cooled to room temperature, obtains sludge carbon.
4. to soak 4h on the perchloric acid of above-mentioned sludge carbon 10wt.%, solution usage is 200mL, and treatment temperature is 60 DEG C, and sludge carbon to the water outlet pH value after soaking with deionized water rinsing is 6, after sludge carbon after process is dried at 20 DEG C, i.e. prepare the sludge carbon of surface modification.
5. CWAO intermittent reaction experiment condition: be 160 DEG C in temperature, oxygen pressure is 0.40MPa, mixing speed: 600r/min, the sludge carbon dosage of surface modification is 5g/L, metacresol initial concentration is 5000mg/L, after reaction 90min, metacresol conversion ratio is 65.3% (Fig. 1), and TOC clearance is 39.2% (Fig. 2).
Embodiment 3:
1. by city domestic sewage treatment plant A2/ O technique produces 105 DEG C of dry 12h of mud, and carries out mechanical activation comminution, makes 200 mesh sieves.
2., after gained sewage sludge powder and shaping assistant HEC (usage amount is 0.5wt.%) are sufficiently mixed, add deionized water (water content is 25wt.%), carry out extrusion after abundant kneading, extrude a diameter of 3.5mm.
3. with nitrogen as protection gas, the bar shaped mud of extrusion is warming up to 120 DEG C of dry 4h with 3 DEG C/min, after then carrying out calcining 4h at 700 DEG C, is cooled to room temperature, obtains sludge carbon.
4. to soak 12h on the sulphuric acid of above-mentioned sludge carbon 20wt.%, treatment temperature is 40 DEG C, and the sludge carbon after soaking with deionized water rinsing is 6 to water outlet pH value, after the sludge carbon after process is dried at 20 DEG C, i.e. prepares the sludge carbon of surface modification.
5. the sludge carbon of surface modification is impregnated 0.9wt.%H2PtCl6Solution, dip time is 24h, and activity component load quantity is 1wt.%, and 500 DEG C of calcining 4h prepare required sludge carbon catalyst.Sludge carbon catalyst in CWAO successive reaction therebetween cresol conversion be 100% (Fig. 3), TOC clearance is 85% (Fig. 4).
Embodiment 4:
1. by the 105 DEG C of dry 12h of mud after hydraulic pressure dehydration in patent (CN201310409054.9), and carry out mechanical activation comminution, made 300 mesh sieves.
2., after gained sewage sludge powder and shaping assistant PAC (usage amount is 0.5wt.%) are sufficiently mixed, add deionized water (water content is 25wt.%), carry out extrusion after abundant kneading, extrude a diameter of 4mm.
3. with nitrogen as protection gas, the bar shaped mud of extrusion is warming up to 120 DEG C of dry 4h with 3 DEG C/min, after then carrying out calcining 4h at 800 DEG C, is cooled to room temperature, obtains sludge carbon.
4. on the nitric acid of above-mentioned sludge carbon 20wt.%, 12h solution usage is soaked as 150mL, treatment temperature is 40 DEG C, sludge carbon after soaking with deionized water rinsing is 6 to water outlet pH value, after the sludge carbon after process is dried at 20 DEG C, i.e. prepares the sludge carbon of surface modification.
5. CWAO intermittent reaction experiment condition: be 160 DEG C in temperature, oxygen pressure is 0.40MPa, mixing speed: 600r/min, the sludge carbon dosage of surface modification is 5g/L, and metacresol initial concentration is 5000mg/L, after reaction 90min, metacresol conversion ratio is 55.3%, and TOC clearance is 39.2%.
Embodiment 5:
1. by the 105 DEG C of dry 12h of mud after hydraulic pressure dehydration in patent (CN201310409054.9), and carry out mechanical activation comminution, made 300 mesh sieves.
2., after gained sewage sludge powder and shaping assistant PAC (usage amount is 1wt.%) are sufficiently mixed, add deionized water (water content is 20wt.%), carry out extrusion after abundant kneading, extrude a diameter of 4mm.
3. with nitrogen as protection gas, the bar shaped mud of extrusion is warming up to 120 DEG C of dry 4h with 3 DEG C/min, after then carrying out calcining 4h at 400 DEG C, is cooled to room temperature, obtains sludge carbon.
4. on the phosphoric acid of above-mentioned sludge carbon 20wt.%, 24h solution usage is soaked as 100mL, treatment temperature is 20 DEG C, sludge carbon after soaking with deionized water rinsing is 6 to water outlet pH value, after the sludge carbon after process is dried at 20 DEG C, i.e. prepares the sludge carbon of surface modification.
5. CWAO intermittent reaction experiment condition: be 160 DEG C in temperature, oxygen pressure is 0.40MPa, mixing speed: 600r/min, the sludge carbon dosage of surface modification is 5g/L, and metacresol initial concentration is 5000mg/L, after reaction 90min, metacresol conversion ratio is 50.1%, and TOC clearance is 35.7%.
Embodiment 6:
1. by city domestic sewage treatment plant A2/ O technique produces 105 DEG C of dry 10h of mud, and carries out mechanical activation comminution, makes 200 mesh sieves.
2., after gained sewage sludge powder and shaping assistant PAC (usage amount is 0.5wt.%) are sufficiently mixed, add deionized water (water content is 25wt.%), carry out extrusion after abundant kneading, extrude a diameter of 3.5mm.
3. with nitrogen as protection gas, the bar shaped mud of extrusion is warming up to 120 DEG C of dry 4h with 3 DEG C/min, after then carrying out calcining 4h at 500 DEG C, is cooled to room temperature, obtains sludge carbon.
4. to soak 12h on the acetic acid of above-mentioned sludge carbon 20wt.%, solution usage is 50mL, and treatment temperature is 40 DEG C, and sludge carbon to the water outlet pH value after soaking with deionized water rinsing is 6, after sludge carbon after process is dried at 20 DEG C, i.e. prepare the sludge carbon of surface modification.
5. by the sludge carbon incipient impregnation 0.9wt.%Pd (NO of surface modification3)2Solution, dip time be 24h activity component load quantity be 1wt.%, 500 DEG C calcining 4h prepare required sludge carbon catalyst.Sludge carbon catalyst in CWAO successive reaction therebetween cresol conversion be 100%, TOC clearance is 80%.
Claims (6)
1. the preparation method of a sludge carbon catalyst, it is characterised in that:
Step is as follows:
(1) mud after city domestic sewage treatment plant being dehydrated, is dried 10～48h at 80～120 DEG C, and carries out mechanical activation comminution, made 200～300 mesh sieves, and obtained sewage sludge powder；
(2), after gained sewage sludge powder mixes with shaping assistant, adding deionized water to total water content is 20～50wt.%, and after carrying out kneading, extrusion obtains column mud；Shaping assistant used is: one or both in polyanion cellulose (PAC) or hydroxyethyl cellulose (HEC), and usage amount is 0～2wt.%；Described extrusion operates, and extrudes a diameter of 2～6mm；
(3) with nitrogen as protection gas; column mud step (2) obtained is dried 2～4h with the ramp of 2～10 DEG C/min to 80～120 DEG C; then, after carrying out calcining 2～8h at 400～800 DEG C, it is cooled to room temperature, i.e. obtains sludge carbon catalyst.
2. according to the preparation method described in claim 1, it is characterized in that: the sludge carbon catalyst that can step (3) be obtained one or more solution in hydrochloric acid, sulphuric acid, nitric acid, perchloric acid, phosphoric acid, acetic acid, sodium hydroxide or the hydrogen peroxide of 5～50wt.% soaks 1～24h at a temperature of 5～80 DEG C, between sludge carbon catalyst and the solution soaked, consumption volume ratio is 1:1～1:5, sludge carbon to water outlet pH value after soaking with deionized water rinsing is 6～8, after drying at 10～105 DEG C, i.e. prepare the sludge carbon catalyst of surface modification.
3. according to the preparation method described in claim 1 or 2, it is characterised in that: can be by the sludge carbon catalyst incipient impregnation RuCl of gained sludge carbon catalyst or surface modification3、H2PtCl6、Pd(NO3)2、RhCl3Or IrCl3In one or more solution, in Ru, Pt, Pd, Rh and Ir, one or more are as active component, in the solution impregnated, the gross mass of Ru, Pt, Pd, Rh or Ir accounts for the percentage ratio of the sludge carbon catalyst of dipping or the sludge carbon catalyst gross mass of surface modification is 0.0～5.0wt.%, excessively takes solid product and prepares transition metal modified sludge carbon catalyst 300～500 DEG C of calcinings 2～8h.
4. the sludge carbon catalyst prepared according to the arbitrary described preparation method of claim 1-3.
5. described in a claim 4, cross the application in CWO processes organic wastewater of the sludge carbon catalyst.
6. according to the application described in claim 5, it is characterised in that:
When described sludge carbon catalyst is transition metal modified sludge carbon catalyst, its for CWO process organic wastewater intermittent reaction condition be:
Catalyst amount has unlimited range, reaction temperature: 120～275 DEG C, oxygen pressure: 0.1～7.0MPa, mixing speed: 400～800r/min；
Or for CWO process organic wastewater successive reaction condition be:
Catalyst amount has unlimited range, reaction temperature: 120～275 DEG C, air pressure: 1.0～7.0MPa, air speed: 0.5～4.0h-1。
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| CN107010807A (en) * | 2017-03-14 | 2017-08-04 | 北京顺鸿金建环境科技发展有限公司 | A kind of method that hydrothermal carbonization processing sludge prepares fuel |
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| CN108892615A (en) * | 2018-08-15 | 2018-11-27 | 南京工业大学 | A kind of application for the sludge Pd/carbon catalyst that surface is modified |
| CN108993518A (en) * | 2018-08-16 | 2018-12-14 | 南京工业大学 | A kind of heterogeneous lightwave CATV catalyst of nanocomposite and its preparation and application |
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| CN110311145A (en) * | 2019-07-01 | 2019-10-08 | 江苏乾景新能源产业技术研究院有限公司 | A method of fuel-cell catalyst is prepared using sludge |
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| CN113941343A (en) * | 2021-11-08 | 2022-01-18 | 武汉纺织大学 | Sludge-based composite catalyst and preparation method and application thereof |
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Application publication date: 20170111 |