CN104069810B - A kind of method utilizing paper mill sludge and pine copyrolysis to prepare active bio charcoal - Google Patents
A kind of method utilizing paper mill sludge and pine copyrolysis to prepare active bio charcoal Download PDFInfo
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Abstract
The present invention is designed into a kind of method utilizing paper mill sludge and pine copyrolysis to prepare active bio charcoal, it is characterized in that comprising the steps: that (1) carries out pretreatment to paper mill sludge, and (2) pine sawdust is air-dry, shatter; (3) raw sludge and pine sawdust fully mix; (4) pyrolysis oven loading hopper is placed in, in an inert atmosphere isothermal pyrolysis; (5), when constant temperature to reaction produces without gas, stop heating, after naturally cooling to room temperature, namely obtain charcoal; (6) put into the sulfuric acid solution that concentration is 2.5-3.5mol/L, pass into nitrogen, at 500-600 DEG C, constant temperature 20-40min; Then naturally cool to room temperature, namely obtain active bio charcoal.The present invention adopts paper mill sludge and pine sawdust copyrolysis technique to prepare active bio charcoal, not only without the need to drying sludge process, further improve the chemical constituent of adsorbent, and the steam that the moisture in mud can be utilized at high temperature to be formed plays certain activation to charcoal, thus improve the adsorption capacity of charcoal, obtain desirable adsorption effect.
Description
Technical field
The present invention relates to environmental pollution improvement and agriculture and forestry organic waste material recycling field, specifically refer to a kind of method utilizing paper mill sludge and pine copyrolysis to prepare active bio charcoal.
Background technology
Paper mill sludge is the end product generated because of wastewater treatment in paper-making process, according to statistics, often produce 1 ton of recycled writing paper, large appointment produces 700 tons, the mud that water content is 75% ~ 85%, its composition is mainly containing high molecular organic matter and flocculating agent, fillers etc. such as hemicellulose, cellulose and lignin, and not containing heavy metal substance, be a kind of biomass resource.But paper mill sludge is because its moisture content is higher, complicated component, intractability are larger, its disposal cost accounts for greatly more than 50% of water treatment running gear expense, therefore, the handling problems of mud has become the bottleneck of constraint paper mill development, the mud produced not only takies a large amount of soils, and poisonous and harmful element wherein will produce serious influence to environment and the mankind.Because becoming containing abundant carbon the advantage preparing charcoal in paper mill sludge, pyrolyzing sludge is prepared charcoal adsorbent and is widely studied as a kind of desirable Sludge resource utilization method.But because of moisture percentage in sewage sludge higher, traditional pyrolytic process needs mud to carry out drying, which not only adds the operation of Treatment of Sludge, substantially increases the disposal cost of mud especially.In addition, ash contents a large amount of in mud butt also can remain in charcoal, thus has a strong impact on performance and the adsorption effect of charcoal adsorbent.
Summary of the invention
Technical problem to be solved by this invention is that utilize paper mill sludge and the pine copyrolysis providing a kind of absorption property good for the present situation of prior art prepares the method for active bio charcoal, thus makes the charcoal of preparation have desirable adsorption effect.
The present invention solves the problems of the technologies described above adopted technical scheme: this utilizes paper mill sludge and pine copyrolysis to prepare the method for active bio charcoal, it is characterized in that comprising the steps:
(1) paper mill sludge after mechanical dehydration of learning from else's experience carries out pretreatment, is cleaned by Sludge Surface impurity, obtain raw sludge by deionized water;
(2) by collect pine sawdust after natural air drying, shatter and sieve, obtain pine sawdust;
(3) described raw sludge and described pine sawdust are fully mixed by the mass ratio of 9:1-1:9;
(4) mixture of step (3) gained is placed in pyrolysis oven loading hopper, setting reaction temperature is 600-900 DEG C, after temperature reaches setting value and maintenance is stable, passes into nitrogen, raw material is evenly sent in pyrolysis oven, ensures to generate charcoal under anaerobic;
(5), when keeping the constant temperature of 600-900 DEG C to reaction to produce without gas, stop heating, after naturally cooling to room temperature, namely obtain charcoal;
(6) gained charcoal in step (5) is put into the sulfuric acid solution that concentration is 2.5-3.5mol/L, pass into nitrogen, at 500-600 DEG C, constant temperature 20-40min; Then naturally cool to room temperature, namely obtain active bio charcoal;
The amount ratio of described charcoal and described sulfuric acid solution is 1:10-1:50, and wherein the unit of the quality of charcoal is gram, and the volume unit of sulfuric acid solution is milliliter.
Preferably, the pine sawdust described in step (2) crosses 30-50 mesh sieve.
Compared with prior art, the present invention adopts paper mill sludge and pine sawdust copyrolysis technique to prepare active bio charcoal, not only without the need to drying sludge process, further improve the chemical constituent of adsorbent, and the steam that the moisture in mud can be utilized at high temperature to be formed plays certain activation to charcoal, thus improve the adsorption capacity of charcoal, obtain desirable adsorption effect.
Accompanying drawing explanation
Fig. 1 is the electron scanning electromicroscopic photograph of the charcoal of preparation in embodiment 1.
Fig. 2 is the electron scanning electromicroscopic photograph of the charcoal of preparation in comparative example 1.
Fig. 3 is the electron scanning electromicroscopic photograph of the charcoal of preparation in comparative example 2.
Fig. 4 is the electron scanning electromicroscopic photograph of the charcoal of preparation in comparative example 3.
Detailed description of the invention
Below in conjunction with accompanying drawing embodiment, the present invention is described in further detail.
Embodiment 1
(1) paper mill sludge after mechanical dehydration of learning from else's experience carries out pretreatment, is cleaned by Sludge Surface impurity, obtain raw sludge by deionized water;
(2) by collect pine sawdust after natural air drying, shattered 40 mesh sieves;
(3) by gained paper mill sludge in step (1) and step (2) and pine sawdust in mass ratio for 2:3 fully mixes;
(4) mixture of step (3) gained is placed in pyrolysis oven loading hopper, setting reaction temperature is 850 DEG C, after temperature reaches setting value and maintenance is stable, passes into nitrogen, raw material is evenly sent in pyrolysis oven, ensures to generate charcoal under anaerobic;
(5) under setting reaction temperature is the condition of 850 DEG C, continuous heating produces to reaction without gas, and stop heating, after charcoal to be generated naturally cools to room temperature, taking-up is weighed, and packs for subsequent use.
(6) get charcoal in step (5) and put into the sulfuric acid solution that concentration is 3mol/L, the ratio of charcoal and sulfuric acid solution is 1 gram: 30 milliliters; Pass into nitrogen, at 550 DEG C, constant temperature 30min; Then naturally cool to room temperature, namely obtain active bio charcoal.
(7) after the time to be activated terminates, stop heating, naturally cool, taking-up material, can obtain active bio charcoal.
(8) the middle gained active bio charcoal of 0.01g step (7) is got in 100mL conical flask, add 50mL concentration be 90mg/L containing Pb (II) solution, conical flask is put into constant temperature oscillator, under room temperature, adsorb with the speed oscillation of 125rpm, the residual quantity of Pb in solution (II) is measured after adsorption equilibrium, and calculated equilibrium adsorption capacity.
Active bio charcoal productive rate prepared by the present embodiment is 15.8%, and its electron scanning electromicroscopic photograph as shown in Figure 1.As seen from the figure, the charcoal fibre structure after activation obtains further fragmentation, and pore distribution becomes more unordered, and structure becomes more loose, and surface roughness obviously increases, thus improves its absorption property.The active bio charcoal specific area of preparation is 338.9m
2/ g, adsorption capacity is 976.7mg/g.
The computing formula of described charcoal productive rate is:
η＝W
1/W
0×100％
In formula: W
0for quality (g) raw materials used before pyrolytic reaction; W
1for the quality (g) of gained charcoal after pyrolytic reaction; η is the productive rate of charcoal.
The mensuration of described charcoal specific area adopts JW-BK122W type specific surface and Porosimetry to measure.
The computing formula of described charcoal adsorption capacity is:
Q＝V×(C
0-C)/W
In formula: V is the volume (mL) of Pb (II) solution; C
0for adsorbing the concentration (mg/L) of Pb (II) in front solution; C is the concentration (mg/L) of Pb (II) in solution after absorption; W is the quality (g) of charcoal; Q is adsorption capacity (mg/g).
After described absorption, in solution, the mensuration of the concentration of Pb (II) adopts xylenol orange AAS.
Calculating and the detection method of following each embodiment and comparative example are same as described above.
Embodiment 2
(1) paper mill sludge after mechanical dehydration of learning from else's experience carries out pretreatment, is cleaned by Sludge Surface impurity, obtain raw sludge by deionized water;
(2) by collect pine sawdust after natural air drying, shattered 40 mesh sieves;
(3) by gained paper mill sludge in step (1) and step (2) and pine sawdust in mass ratio for 1:9 fully mixes;
(4) mixture of step (3) gained is placed in pyrolysis oven loading hopper, setting reaction temperature is 600 DEG C, after temperature reaches setting value and maintenance is stable, passes into nitrogen, raw material is evenly sent in pyrolysis oven, ensures to generate charcoal under anaerobic;
(5) under setting reaction temperature is the condition of 600 DEG C, continuous heating produces to reaction without gas, and stop heating, after charcoal to be generated naturally cools to room temperature, taking-up is weighed, and packs for subsequent use.
(6) get charcoal in step (5) after the sulfuric acid solution activation that concentration is 3mol/L, put into pyrolysis oven loading hopper, pass into nitrogen, regulate activation temperature to be 550 DEG C, soak time is 30min.The amount ratio of charcoal and sulfuric acid solution is 1 gram: 12 milliliters.
(7) after the time to be activated terminates, stop heating, naturally cool, taking-up material, can obtain active bio charcoal.
(8) the middle gained active bio charcoal of 0.01g step (7) is got in 100mL conical flask, add 50mL concentration be 90mg/L containing Pb (II) solution, conical flask is put into constant temperature oscillator, room temperature, adsorb with the speed oscillation of 125r/min, the residual quantity of Pb in solution (II) is measured after adsorption equilibrium, and calculated equilibrium adsorption capacity.
Embodiment 3
(1) paper mill sludge after mechanical dehydration of learning from else's experience carries out pretreatment, is cleaned by Sludge Surface impurity, obtain raw sludge by deionized water;
(2) by collect pine sawdust after natural air drying, shattered 40 mesh sieves;
(3) by gained paper mill sludge in step (1) and step (2) and pine sawdust in mass ratio for 1:5 fully mixes;
(4) mixture of step (3) gained is placed in pyrolysis oven loading hopper, setting reaction temperature is 750 DEG C, after temperature reaches setting value and maintenance is stable, passes into nitrogen, raw material is evenly sent in pyrolysis oven, ensures to generate charcoal under anaerobic;
(5) under setting reaction temperature is the condition of 750 DEG C, continuous heating produces to reaction without gas, and stop heating, after charcoal to be generated naturally cools to room temperature, taking-up is weighed, and packs for subsequent use.
(6) get charcoal in step (5) after the sulfuric acid solution activation that concentration is 3mol/L, put into pyrolysis oven loading hopper, pass into nitrogen, regulate activation temperature to be 550 DEG C, soak time is 30min.The amount ratio of charcoal and sulfuric acid solution is 1 gram: 20 milliliters.
(7) after the time to be activated terminates, stop heating, naturally cool, taking-up material, can obtain active bio charcoal.
(8) the middle gained active bio charcoal of 0.01g step (7) is got in 100mL conical flask, add 50mL concentration be 90mg/L containing Pb (II) solution, conical flask is put into constant temperature oscillator, room temperature, adsorb with the speed oscillation of 125r/min, the residual quantity of Pb in solution (II) is measured after adsorption equilibrium, and calculated equilibrium adsorption capacity.
Embodiment 4
(1) paper mill sludge after mechanical dehydration of learning from else's experience carries out pretreatment, is cleaned by Sludge Surface impurity, obtain raw sludge by deionized water;
(2) by collect pine sawdust after natural air drying, shattered 40 mesh sieves;
(3) by gained paper mill sludge in step (1) and step (2) and pine sawdust in mass ratio for 1:1 fully mixes;
(4) mixture of step (3) gained is placed in pyrolysis oven loading hopper, setting reaction temperature is 900 DEG C, after temperature reaches setting value and maintenance is stable, passes into nitrogen, raw material is evenly sent in pyrolysis oven, ensures to generate charcoal under anaerobic;
(5) under setting reaction temperature is the condition of 900 DEG C, continuous heating produces to reaction without gas, and stop heating, after charcoal to be generated naturally cools to room temperature, taking-up is weighed, and packs for subsequent use.
(6) get charcoal in step (5) after the sulfuric acid solution activation that concentration is 3mol/L, put into pyrolysis oven loading hopper, pass into nitrogen, regulate activation temperature to be 550 DEG C, soak time is 30min.The amount ratio of charcoal and sulfuric acid solution is 1 gram: 40 milliliters.
(7) after the time to be activated terminates, stop heating, naturally cool, taking-up material, can obtain active bio charcoal.
(8) the middle gained active bio charcoal of 0.01g step (7) is got in 100mL conical flask, add 50mL concentration be 90mg/L containing Pb (II) solution, conical flask is put into constant temperature oscillator, room temperature, adsorb with the speed oscillation of 125r/min, the residual quantity of Pb in solution (II) is measured after adsorption equilibrium, and calculated equilibrium adsorption capacity.
Embodiment 5
(1) paper mill sludge after mechanical dehydration of learning from else's experience carries out pretreatment, is cleaned by Sludge Surface impurity, obtain raw sludge by deionized water;
(2) by collect pine sawdust after natural air drying, shattered 40 mesh sieves;
(3) by gained paper mill sludge in step (1) and step (2) and pine sawdust in mass ratio for 5:1 fully mixes;
(4) mixture of step (3) gained is placed in pyrolysis oven loading hopper, setting reaction temperature is 900 DEG C, after temperature reaches setting value and maintenance is stable, passes into nitrogen, raw material is evenly sent in pyrolysis oven, ensures to generate charcoal under anaerobic;
(5) under setting reaction temperature is the condition of 900 DEG C, continuous heating produces to reaction without gas, and stop heating, after charcoal to be generated naturally cools to room temperature, taking-up is weighed, and packs for subsequent use.
(6) get charcoal in step (5) after the sulfuric acid solution activation that concentration is 3mol/L, put into pyrolysis oven loading hopper, pass into nitrogen, regulate activation temperature to be 550 DEG C, soak time is 30min.The amount ratio of charcoal and sulfuric acid solution is 1 gram: 50 milliliters.
(7) after the time to be activated terminates, stop heating, naturally cool, taking-up material, can obtain active bio charcoal.
(8) the middle gained active bio charcoal of 0.01g step (7) is got in 100mL conical flask, add 50mL concentration be 90mg/L containing Pb (II) solution, conical flask is put into constant temperature oscillator, room temperature, adsorb with the speed oscillation of 125r/min, the residual quantity of Pb in solution (II) is measured after adsorption equilibrium, and calculated equilibrium adsorption capacity.
Embodiment 6
(1) paper mill sludge after mechanical dehydration of learning from else's experience carries out pretreatment, is cleaned by Sludge Surface impurity, obtain raw sludge by deionized water;
(2) by collect pine sawdust after natural air drying, shattered 40 mesh sieves;
(3) by gained paper mill sludge in step (1) and step (2) and pine sawdust in mass ratio for 9:1 fully mixes;
(4) mixture of step (3) gained is placed in pyrolysis oven loading hopper, setting reaction temperature is 850 DEG C, after temperature reaches setting value and maintenance is stable, passes into nitrogen, raw material is evenly sent in pyrolysis oven, ensures to generate charcoal under anaerobic;
(5) under setting reaction temperature is the condition of 850 DEG C, continuous heating produces to reaction without gas, and stop heating, after charcoal to be generated naturally cools to room temperature, taking-up is weighed, and packs for subsequent use.
(6) get charcoal in step (5) after the sulfuric acid solution activation that concentration is 3mol/L, put into pyrolysis oven loading hopper, pass into nitrogen, regulate activation temperature to be 550 DEG C, soak time is 30min.The amount ratio of charcoal and sulfuric acid solution is 1 gram: 30 milliliters.
(7) after the time to be activated terminates, stop heating, naturally cool, taking-up material, can obtain active bio charcoal.
(8) the middle gained active bio charcoal of 0.01g step (7) is got in 100mL conical flask, add 50mL concentration be 90mg/L containing Pb (II) solution, conical flask is put into constant temperature oscillator, room temperature, adsorb with the speed oscillation of 125r/min, the residual quantity of Pb in solution (II) is measured after adsorption equilibrium, and calculated equilibrium adsorption capacity.
In embodiment 2 to embodiment 6, the productive rate of active bio charcoal is between 12-21%, and specific area is at 300-350m
2between/g, adsorption capacity between 950-1000mg/g, electron-microscope scanning structure and embodiment 1 similar.
Comparative example 1
(1) paper mill sludge after mechanical dehydration of learning from else's experience carries out pretreatment, is cleaned by Sludge Surface impurity, obtain raw sludge by deionized water;
(2) by collect pine sawdust after natural air drying, shattered 40 mesh sieves;
(3) by gained raw sludge in step (1) and step (2) and pine sawdust in mass ratio for 2:3 mixes;
(4) mixture of step (3) gained is placed in pyrolysis oven loading hopper, setting reaction temperature is 850 DEG C, after temperature reaches setting value and maintenance is stable, passes into nitrogen, raw material is evenly sent in pyrolysis oven, ensures to generate charcoal under anaerobic;
(5) under setting reaction temperature is the condition of 850 DEG C, continuous heating produces to reaction without gas, and stop heating, after charcoal to be generated naturally cools to room temperature, taking-up is weighed, and packs for subsequent use.
(6) the middle gained charcoal of 0.01g step (3) is got in 100mL conical flask, add 50mL concentration be 90mg/L containing Pb (II) solution, conical flask is put into constant temperature oscillator, adsorb with the speed oscillation of 125rpm under room temperature, the residual quantity of Pb in solution (II) is measured after adsorption equilibrium, and calculated equilibrium adsorption capacity.
Charcoal productive rate prepared by the present embodiment is 15.8%, and its electron scanning electromicroscopic photograph as shown in Figure 2.As seen from the figure, the fibrous gap structure of the charcoal rule obtained by mud and pine sawdust pyrolysis is destroyed, and defines irregular projection, presents irregular loose structure.The charcoal specific area of preparation is 186.3m
2/ g, adsorption capacity is 536.5mg/g.
Comparative example 2
(1) paper mill sludge after mechanical dehydration of learning from else's experience carries out pretreatment, is cleaned by Sludge Surface impurity, obtain raw sludge by deionized water;
(2) the pure mud getting certain mass in step (1) is placed in pyrolysis oven loading hopper, setting reaction temperature is 750 DEG C, after temperature reaches setting value and maintenance is stable, passes into nitrogen, raw material is evenly sent in pyrolysis oven, ensures to generate charcoal under anaerobic;
(3) under setting reaction temperature is the condition of 750 DEG C, continuous heating produces to reaction without gas, and stop heating, after charcoal to be generated naturally cools to room temperature, taking-up is weighed, and packs for subsequent use.
(4) the middle gained charcoal of 0.01g step (3) is got in 100mL conical flask, add 50mL concentration be 90mg/L containing Pb (II) solution, conical flask is put into constant temperature oscillator, room temperature, adsorb with the speed oscillation of 125r/min, the residual quantity of Pb in solution (II) is measured after adsorption equilibrium, and calculated equilibrium adsorption capacity.
Charcoal productive rate prepared by this comparative example is 10.2%, and its electron scanning electromicroscopic photograph as shown in Figure 3.As seen from the figure, the charcoal surface obtained by pyrolyzing sludge is comparatively closely knit, has obvious clustering phenomena, space skewness, and top layer gap structure is not very abundant.Preparing charcoal specific area is 45.1m
2/ g, adsorption capacity is 129.8mg/g.
Comparative example 3
(1) by collect pine sawdust after natural air drying, shattered 40 mesh sieves;
(2) pine sawdust getting certain mass in step (1) is placed in pyrolysis oven loading hopper, setting reaction temperature is 750 DEG C, after temperature reaches setting value and maintenance is stable, passes into nitrogen, raw material is evenly sent in pyrolysis oven, ensures to generate charcoal under anaerobic;
(3) under setting reaction temperature is the condition of 750 DEG C, continuous heating produces to reaction without gas, and stop heating, after charcoal to be generated naturally cools to room temperature, taking-up is weighed, and equips for subsequent use.
(4) the middle gained charcoal of 0.01g step (3) is got in 100mL conical flask, add 50mL concentration be 90mg/L containing Pb (II) solution, conical flask is put into constant temperature oscillator, room temperature, adsorb with the speed oscillation of 125rpm, the residual quantity of Pb in solution (II) is measured after adsorption equilibrium, and calculated equilibrium adsorption capacity.
Charcoal productive rate prepared by the present embodiment is 23.7%, its electron scanning electromicroscopic photograph as shown in Figure 4, as seen from the figure, the orifice throat ratio on the charcoal surface obtained by pine sawdust pyrolysis is more smooth, regular, present fibrous gap structure, but the ablation of partial pore hole wall is caved in, blocking space and crack.The charcoal specific area of preparation is 26.5m
2/ g, adsorption capacity is 75.8mg/g.
Claims (2)
1. utilize paper mill sludge and pine copyrolysis to prepare a method for active bio charcoal, it is characterized in that comprising the steps:
(1) paper mill sludge after mechanical dehydration of learning from else's experience carries out pretreatment, is cleaned by Sludge Surface impurity, obtain raw sludge by deionized water;
(2) by collect pine sawdust after natural air drying, shatter and sieve, obtain pine sawdust;
(3) described raw sludge and described pine sawdust are fully mixed by the mass ratio of 9:1-1:9;
(4) mixture of step (3) gained is placed in pyrolysis oven loading hopper, setting reaction temperature is 600-900 DEG C, after temperature reaches setting value and maintenance is stable, passes into nitrogen, raw material is evenly sent in pyrolysis oven, ensures to generate charcoal under anaerobic;
(5), when keeping the constant temperature of 600-900 DEG C to reaction to produce without gas, stop heating, after naturally cooling to room temperature, namely obtain charcoal;
(6) gained charcoal in step (5) is put into the sulfuric acid solution that concentration is 2.5-3.5mol/L, pass into nitrogen, at 500-600 DEG C, constant temperature 20-40min; Then naturally cool to room temperature, namely obtain active bio charcoal;
The amount ratio of described charcoal and described sulfuric acid solution is 1:10-1:50, and wherein the unit of the quality of charcoal is gram, and the volume unit of sulfuric acid solution is milliliter.
2. method according to claim 1, is characterized in that the pine sawdust described in step (2) crosses 30-50 mesh sieve.
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| CN108176359A (en) * | 2018-01-22 | 2018-06-19 | 济南大学 | A kind of preparation method of mixing waste charcoal |
| CN109575929A (en) * | 2018-11-28 | 2019-04-05 | 攀钢集团攀枝花钢铁研究院有限公司 | The method of the agent of heavy-metal contaminated soil complex repairation and its rehabilitating soil |
| CN109603759B (en) * | 2019-01-25 | 2021-05-07 | 太原理工大学 | Modified charcoal adsorbed by dye and preparation method thereof |
| CN110302748B (en) * | 2019-05-05 | 2022-04-05 | 浙江清风源环保科技有限公司 | Preparation method of sludge-based biochar |
| CN112108118B (en) * | 2020-09-21 | 2023-04-25 | 黄河水利职业技术学院 | Fenton sludge and cellulose-based magnetic biomass charcoal and preparation method and application thereof |
| CN113634229A (en) * | 2021-09-02 | 2021-11-12 | 浙江理工大学绍兴柯桥研究院有限公司 | Preparation method and application of biochar with selective adsorption-desorption capacity |
| CN114149004B (en) * | 2021-11-19 | 2023-07-07 | 中国电建集团环境工程有限公司 | Activated carbon preparation method of municipal sludge coupled biomass and activated carbon module |
| CN114733480A (en) * | 2022-03-28 | 2022-07-12 | 上海园林绿化建设有限公司 | Modified biochar and preparation method thereof |
| CN116082092B (en) * | 2023-01-12 | 2024-04-19 | 南开大学 | Preparation method of biochar, and method and application for returning tail vegetables to field |
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