CN104150743B - The method of sludge carbon is prepared in the carbonization of a kind of microwave-assisted hydro-thermal - Google Patents
The method of sludge carbon is prepared in the carbonization of a kind of microwave-assisted hydro-thermal Download PDFInfo
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- CN104150743B CN104150743B CN201410349427.2A CN201410349427A CN104150743B CN 104150743 B CN104150743 B CN 104150743B CN 201410349427 A CN201410349427 A CN 201410349427A CN 104150743 B CN104150743 B CN 104150743B
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Abstract
The invention discloses the method that sludge carbon is prepared in the carbonization of a kind of microwave-assisted hydro-thermal, the sludge carbon stay in grade that the method obtains, available phosphorus, available nitrogen content are high, have good infertile field effect, also can effectively reduce or heavy metal content in fixing mud.The inventive method raw material sources is extensive, and low production cost, processing step is simple, environmental friendliness, is easy to apply.
Description
Technical field
The present invention relates to manipulation of regeneration and the recycling of mud, particularly relate to the method that sludge carbon is prepared in the carbonization of a kind of microwave-assisted hydro-thermal.
Background technology
Along with the universal of municipal sewage plant of China and operation, sludge from wastewater treatment plant output increases fast.Between 2001-2011, the annual production of China's mud with every year on average 15% speed be increased to 2,268 ten thousand tons from 5,670,000 tons.Due to problems such as bioavailability difference and water ratio high (most mud when dispatching from the factory still up to 80%), the transport of excess sludge and safe disposal receive serious restriction.Mud contains the hazardous and noxious substances such as pathogenic agent, heavy metal and persistent organism, without effectively processing disposal, very easily causes secondary pollution to underground water, soil etc., direct threatening environment safety and public health.
Sludge carbonization is a kind of novel sludge disposal technology, not only successfully can realize the minimizing of mud, simultaneously effectively fixing carbon source, and produces carbon-based product and can carry out recycling, efficiently solves the problem of sludge organism utilizability difference.At present, traditional sludge carbonization method is mainly dry method charing, and refer to that under anoxic or oxygen-free environment, carry out pyrolysis to sludge-drying makes organism be converted into charcoal, technique can be summarized as " drying sludge+pyrolyzing sludge ".Main method comprises: (1) high temperature carbonization, such as Chinese patent CN203159415U discloses " sludge high temperature carbonization system ", the utilization of the carbonization carbonizing gas that mud produces by this carbonization system in mummification and carbonization combines with the high temperature deodorization integration process of waste gas, reduce energy consumption, and simplify Equipments Setting.Such as Chinese patent CN203173945U discloses " sludge high temperature carbide furnace ", can realize the mass-producing process of dewatered sludge day output more than 1000 tons.(2) low-temperature carbonization, such as Chinese patent CN101845311A discloses " method that pyrolyzing municipal sludge prepares bio oil and gac simultaneously ", solve the difficult problem that current conventional pyrolyzing sludge method can only obtain single resource product, high-quality biological oil and gac can be obtained simultaneously.Such as Chinese patent CN103523775A discloses " treatment process of mud and the agricultural sludge charcoal of acquisition thereof ", discloses the agricultural sludge charcoal that a kind of low-temperature carbonization method of mud and process thereof obtain.But traditional sludge dry method charring, all has strict demand to moisture percentage in sewage sludge, need first to carry out mummification pre-treatment to dewatered sludge, energy consumption is higher, significantly limit the development of this treatment process.
And hydrothermal carbonization method is without the need to carrying out prior drying to mud, low to the water content requirement of raw sludge, reaction conditions is gentle, and technological process is simple, and thus on energy charge and production control, having obvious advantage, is the show of developing new of current charring process.Such as Chinese patent CN102875005A discloses " a kind of sludge organism charring process based on hydro-thermal reaction ", provides a kind of mud hydro-thermal carbonization technique.
In recent years, microwave technology because of have clean, fast and be easy to the advantages such as manipulation and obtain and develop rapidly, early 1990s, start process microwave technology being introduced sewage sludge, comprise the aspects such as mud Sources decreasing, drying sludge.Such as Chinese patent CN103204611A discloses " method and apparatus based on the source sludge reduction of microwave sludge pretreatment ", efficiently cracking of residual active sludge is realized by microwave under normal pressure opening condition, improve the bioavailability of residual active sludge, but it does not carry out recycling to mud.Up to the present there is not yet the report utilizing the carbonization of microwave-assisted hydro-thermal to prepare sludge carbon.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provide the carbonization of a kind of microwave-assisted hydro-thermal to prepare the method for sludge carbon.
The technical solution used in the present invention is:
A method for sludge carbon is prepared in the carbonization of microwave-assisted hydro-thermal, comprises the steps:
(1) send in hydrothermal reactor by water-containing sludge, sealing, Microwave-assisted firing carries out hydrothermal carbonization reaction, obtains hydrothermal carbonization liquid;
(2) the hydrothermal carbonization liquid obtained is carried out solid-liquid separation, solid product washing, drying, obtain sludge carbon.
Preferably, step (1), controlling hydrothermal reactor internal pressure is 2 ~ 3atm.
Preferably, step (1), controlling Heating temperature is 150 ~ 300 DEG C.
Preferably, step (1), control microwave power is 50 ~ 800W.Preferred, step (1), control microwave power is 200 ~ 600W.
Preferably, step (1), the hydrothermal carbonization reaction times is 30 ~ 150min.
Preferably, step (1), the water ratio of described water-containing sludge is 50 ~ 85wt%.
Preferably, step (2), described drying temperature is 40 ~ 60 DEG C.
The invention has the beneficial effects as follows:
(1) the inventive method raw material sources is extensive, and low production cost, processing step is simple, environmental friendliness, is easy to apply.
(2) the sludge carbon stay in grade of the inventive method acquisition, available phosphorus, available nitrogen content are high, have good infertile field effect; The method can effectively reduce or heavy metal content in fixing mud simultaneously.
Embodiment
The invention discloses the method that sludge carbon is prepared in the carbonization of a kind of microwave-assisted hydro-thermal, comprise the steps: water-containing sludge to send in hydrothermal reactor, sealing, microwave-assisted carries out hydrothermal carbonization reaction, obtain hydrothermal carbonization liquid, centrifugal, washing, dry, obtain sludge carbon.Product sludge carbon contains a large amount of carbon element and nutritive ingredient, can be used for land remediation and improvement, and its proterties is stablized, and repairs, improved effect is lasting for a long time.The material of sludge carbon or a kind of carbon fixation and emission reduction, it is produced and uses has mitigation to Global Carbon discharge.The low raw-material cost that the inventive method adopts, environmental friendliness, preparation technology's simple possible, totally have followed the principle of " turn waste into wealth, three-dimensional agriculture ".
The present invention adopts microwave-assisted can accelerate hydrothermal carbonization reaction process on the one hand, can contribute to the stripping of the noxious pollutants such as heavy metal on the other hand.
Hydrothermal reactor used is salable, resistance to higher temperatures (200 ~ 300 DEG C) and high pressure (2 ~ 3atm).Be furnished with temp probe in hydrothermal reactor, reactor temperature can be controlled in reaction process.
Solid-liquid separating method adopts centrifugation or other modes, and centrifugal rotational speed is preferably 3000 ~ 6000rpm.
Below in conjunction with embodiment, the present invention is described further, but embodiments of the present invention are not limited thereto.
embodiment 1
Be in the domestic sludge feeding hydrothermal reactor of 80wt% by water ratio, sealing, Microwave-assisted firing carries out hydrothermal carbonization reaction, microwave power is 200W, and reactor pressure is 2.3atm, and hydrothermal temperature is 200 DEG C, reaction times is 120min, obtains hydrothermal carbonization liquid; 3000rpm is centrifugal carries out solid-liquid separation, and solid product washes 3 times, 40 DEG C of oven dryings, obtains sludge carbon.
Sludge carbon productive rate is 67%, and organic content is 28.97%, and its available phosphorus, available nitrogen comparatively primary sludge add 33.26%, 36.23% respectively, also containing a large amount of carbon element and nutritive ingredient.Measure its heavy metal, the content in the leaching liquor of Cd, Cu comparatively primary sludge reduces 88.59%, 92.21% respectively.
embodiment 2
Be in the domestic sludge feeding hydrothermal reactor of 85wt% by water ratio, sealing, Microwave-assisted firing carries out hydrothermal carbonization reaction, microwave power is 400W, and reactor pressure is 2.2atm, and it is 250 DEG C that hydrothermal temperature controls, reaction times is 90min, obtains hydrothermal carbonization liquid; 3500rpm is centrifugal carries out solid-liquid separation, and solid product washes 3 times, oven drying at 50 DEG C, obtains sludge carbon.
Sludge carbon productive rate is 61.5%, and organic content is 24.69%, and its available phosphorus, available nitrogen comparatively primary sludge add 33.26%, 35.55% respectively.Measure its heavy metal, the content in the leaching liquor of Cd, Cu comparatively primary sludge reduces 83.12%, 95.16% respectively.
embodiment 3
Be in the domestic sludge feeding hydrothermal reactor of 80wt% by water ratio, sealing, Microwave-assisted firing carries out hydrothermal carbonization reaction, and microwave power is 600W, and reactor pressure is 3atm, and hydrothermal temperature is 300 DEG C, and the reaction times is 90min, obtains hydrothermal carbonization liquid; 3000rpm is centrifugal carries out solid-liquid separation, and solid product washes 3 times, 40 DEG C of oven dryings, obtains sludge carbon.
Sludge carbon productive rate is 55.14%, and organic content is 20.47%, and its available phosphorus, available nitrogen comparatively primary sludge add 32.62%, 36.79% respectively, also containing a large amount of carbon element and nutritive ingredient.Measure its heavy metal, the content in the leaching liquor of Cd, Cu comparatively primary sludge reduces 94.11%, 98.28% respectively.
embodiment 4
Be in the municipal sludge feeding hydrothermal reactor of 80wt% by water ratio, sealing, Microwave-assisted firing carries out hydrothermal carbonization reaction, and microwave power is 500W, and reactor pressure is 2atm, and hydrothermal temperature is 150 DEG C, and the reaction times is 150min, obtains hydrothermal carbonization liquid; 3000rpm is centrifugal carries out solid-liquid separation, and solid product washes 3 times, 40 DEG C of oven dryings, obtains sludge carbon.
Sludge carbon productive rate is 70.01%, and organic content is 32.12%, and its available phosphorus, available nitrogen comparatively primary sludge add 36.70%, 39.53% respectively, also containing a large amount of carbon element and nutritive ingredient.Measure its heavy metal, the content in the leaching liquor of Cd, Cu comparatively primary sludge reduces 90.25%, 94.98% respectively.
embodiment 5
Be in the domestic sludge feeding hydrothermal reactor of 75% by water ratio, sealing, Microwave-assisted firing carries out hydrothermal carbonization reaction, and microwave power is 250W, and reactor pressure is 2.2atm, and hydrothermal temperature is 200 DEG C, and the reaction times is 90min, obtains hydrothermal carbonization liquid; 4000rpm is centrifugal carries out solid-liquid separation, and solid product washes 3 times, oven drying at 60 DEG C, obtains sludge carbon 1.
Similarly, same operation (hydrothermal temperature, reaction times identical) is carried out in without microwave situation with batch mud, acquisition sludge carbon 2.
Sludge carbon 1 productive rate is 75.2%, and sludge carbon 2 productive rate is 78%.Its available phosphorus of mud 1, available nitrogen comparatively primary sludge add 30.06%, 33.55% respectively, and its available phosphorus of mud 2, available nitrogen comparatively primary sludge add 29.26%, 30.55% respectively.Measure its heavy metal, the content in mud 1 in Cd, Cu leaching liquor comparatively primary sludge reduces 74.59%, 92.33% respectively, in mud 2 Cd, Cu leaching liquor content comparatively primary sludge reduce 67.12%, 84.8% respectively.
embodiment 6
Be in the domestic sludge feeding hydrothermal reactor of 80% by water ratio, sealing, Microwave-assisted firing carries out hydrothermal carbonization reaction, and microwave power is 200W, and reactor pressure is 2atm, and hydrothermal temperature is 200 DEG C, and the reaction times is 120min, obtains hydrothermal carbonization liquid; 4000rpm is centrifugal carries out solid-liquid separation, and solid product washes 3 times, oven drying at 40 DEG C, obtains sludge carbon 1.
With batch drying sludge, will pulverize, cross 60 mesh sieves, at sealing (N
2) in retort furnace, 600 DEG C are burnt 4h, obtain sludge carbon 2.
With batch drying sludge, will pulverize, cross 60 mesh sieves, at sealing (N
2) in retort furnace, 400 DEG C are burnt 4h, obtain sludge carbon 3.
Sludge carbon 1 productive rate is 63.8%, and sludge carbon 2 productive rate is 52.17%, and sludge carbon 3 productive rate is 69.34%.Its available phosphorus of mud 1, available nitrogen comparatively primary sludge add 33.6%, 37.9% respectively, its available phosphorus of mud 2, available nitrogen comparatively primary sludge reduce 53.1%, 82.3% respectively, its available phosphorus of mud 3 comparatively primary sludge add 3.9%, available nitrogen comparatively primary sludge reduce 76.6%.Its heavy metal leaching is measured, content in mud 1 in Cd, Cu leaching liquor comparatively primary sludge reduces 82.5%, 95.0% respectively, in mud 2 Cd, Cu leaching liquor content comparatively primary sludge reduce 41.5%, 13.69% respectively, in mud 3 Cd, Cu leaching liquor content comparatively primary sludge reduce 63.3%, 42.7% respectively.
Claims (3)
1. a method for sludge carbon is prepared in the carbonization of microwave-assisted hydro-thermal, comprises the steps:
(1) be that the mud of 50 ~ 85wt% is sent in hydrothermal reactor by water ratio, sealing, controlling hydrothermal reactor internal pressure is 2 ~ 3atm, and Heating temperature is 150 ~ 300 DEG C, Microwave-assisted firing carries out hydrothermal carbonization reaction 30 ~ 150min, obtains hydrothermal carbonization liquid;
(2) the hydrothermal carbonization liquid obtained is carried out solid-liquid separation, solid product washing, 40 ~ 60 DEG C of dryings, obtain sludge carbon.
2. the method for sludge carbon is prepared in microwave-assisted hydro-thermal according to claim 1 carbonization, it is characterized in that: step (1), and control microwave power is 50 ~ 800W.
3. the method for sludge carbon is prepared in microwave-assisted hydro-thermal according to claim 2 carbonization, it is characterized in that: step (1), and control microwave power is 200 ~ 600W.
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| CN105255506A (en) * | 2015-09-10 | 2016-01-20 | 广州中国科学院先进技术研究所 | Method for preparing sludge char through hydrothermal carbonization reinforced by conditioners |
| CN105331376B (en) * | 2015-11-27 | 2017-10-10 | 华中农业大学 | The high-valued processing unit of fresh biomass and method being carbonized based on microwave hydrothermal |
| CN106995350A (en) * | 2017-03-27 | 2017-08-01 | 深圳先进技术研究院 | The preparation method and sludge base charcoal slow-release phosphate fertilizer of sludge base charcoal slow-release phosphate fertilizer |
| CN108975305A (en) * | 2018-08-20 | 2018-12-11 | 宁夏和兴碳基材料有限公司 | A method of carbon-based material is prepared using dewatered sludge |
| CN109320043A (en) * | 2018-11-15 | 2019-02-12 | 天津大学 | A kind of method of microwave coupling stabilizer stably desulphurizing sludge heavy-metal |
| CN109772472B (en) * | 2019-01-17 | 2021-10-15 | 四川大学 | Method for preparing carbon catalytic material from high-water-content excess sludge |
| CN111908753B (en) * | 2020-08-03 | 2023-02-28 | 宁波首创厨余垃圾处理有限公司 | Method for preparing kitchen waste anaerobic biogas residue biochar through ultrasonic-assisted hydrothermal carbonization |
| CN114180997B (en) * | 2021-12-30 | 2023-03-21 | 天津大学 | Electric method combined with hydrothermal method for preparing sewage and peat fertilizer and method thereof |
| CN114854467B (en) * | 2022-05-06 | 2023-02-24 | 河南城建学院 | Device for preparing solid fuel by blending sludge and wood fiber wastes and performing hydrothermal carbonization |
| CN115072962A (en) * | 2022-06-30 | 2022-09-20 | 东方电气集团东方电机有限公司 | Sludge dewatering method based on ultrasound and hydrothermal carbonization |
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