CN102698712A - Surface modification method of sludge-activated carbon for treating dyeing wastewater - Google Patents
Surface modification method of sludge-activated carbon for treating dyeing wastewater Download PDFInfo
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Abstract
The invention provides a surface modification method of sludge-activated carbon for treating dyeing wastewater, belonging to the technical field of the sludge-activated carbon. The method comprises the following processes of: using residual sludge of a secondary sedimentation tank as a raw material, adding a certain amount of crop straws as an indirect material, performing four processing steps of sludge impregnation activation, high-temperature carbonization, grinding and screening, and activation and modification, controlling the carbonization temperature and time and the concentration of modification solution and the like to modify surface functional groups of the sludge-activated carbon so as to greatly improve the adsorption capability of the sludge-activated carbon. According to the invention, the preparation is simple, the cost is low, the aperture distribution of the sludge-activated carbon can be optimized, the content of surface acid and alkali groups is changed, and the effect on adsorbing the dyeing wastewater is good.
Description
Technical field
The present invention relates to a kind of is the surface modifying method of the active sludge carbon of main raw material(s) with the excess sludge, is applicable to the removal of coloring matter in removal and the sewage of waste water from dyestuff, belongs to the active sludge carbon technical field.
Background technology
In recent years, along with quickening of urbanization process and raising that city environmental quality is required, China's municipal sewage treatment career development very rapidly.The quantity of municipal sewage plant increases year by year, and the output of municipal sludge also increases thereupon, except that containing large quantity of moisture, also contains organic matter, heavy metal and salt and the various invasive organism of difficult degradation in the mud.If mishandling, will cause serious secondary pollution, but organic matter that wherein contains and humus etc. are available resources, sludge stabilization, minimizing, innoxious and resource have caused people's extensive concern.The new Treatment of Sludge method of disposal and the new way of comprehensive utilization of resources are inquired into to the environment easy generation of secondary pollution in traditional treatment and disposal mode such as sanitary landfills, burning, throwing sea etc. therefore, dispose significant to solving sludge of sewage treatment plants.
Active carbon is a kind of microcrystalline carbon with special construction, has abundant pore structure and bigger specific area, has very strong selection adsorption capacity.But because the cost of the raw material of preparation active carbon such as carbonaceous materials such as coal and timber is higher, the exploration of the active carbon that manufacturing price is cheap is also more and more paid attention to.
Contain higher organic carbon in the activated sludge, received scholar's extensive concern with mud as the active carbon raw material.But because the restriction of the performance of mud own, the active sludge carbon specific area of preparing is less, and absorption property is relatively poor, therefore, need carry out surface modification treatment to it, regulates the surperficial soda acid functional group of active sludge carbon, strengthens absorption property.This is very necessary to the application that promotes active sludge carbon.
Summary of the invention
The purpose of this invention is to provide coloring matter in a kind of removal that is applicable to waste water from dyestuff and the sewage removal be the surface modifying method of the active sludge carbon of main raw material(s) with the excess sludge, change its absorption property through the acid and alkaline group that changes the sludge activity carbon surface.
A kind of method that changes the active sludge carbon surface functional group provided by the present invention is prepared the good active sludge carbon of absorption property.This method is a raw material with the second pond excess sludge; Add a certain amount of agricultural crop straw and expect, through the activation of mud dipping, high temperature cabonization as pair; Grinding is sieved; Four steps of activated again modification are carried out modification to the active sludge carbon surface functional group, thereby the absorption property of active sludge carbon is enhanced.
The surface modifying method of a kind of active sludge carbon provided by the present invention is characterized in that, may further comprise the steps:
1) with drying sludge, grind, sieve, keeping particle size range is 40-100 purpose mud granule;
2) agricultural crop straw is dry; Quality percentage composition according to mud is 60-90%; The quality percentage composition of agricultural crop straw is that the ratio of 10-40% is mixed the two, and be 1g with activator solution by solid-to-liquid ratio with this two mixture again: (1-4) ml mixes, and floods 12-24h down in normal temperature; Be dried to constant weight afterwards, obtain the activated sludge particle;
3) with nitrogen as the protection gas; After the activated sludge particle put into Muffle furnace and be warming up to 450-650 ℃ of insulation 30-90min with the heating rate of 6-20 ℃/min; Be cooled to normal temperature; Back hydrochloric acid flush away impurity; The distilled water cyclic washing of using 70-80 ℃ again is to neutral; Oven dry promptly obtains active sludge carbon;
4) active sludge carbon that obtains in the step 3) is further ground, sieves; The active sludge carbon of getting below 200 orders adds modified solution; The solid-liquid amount ratio of active sludge carbon and modified solution is (1-4) g: (10-40) ml, and evenly stir with agitator and to leave standstill at least 4 hours after 4-6 hour, use the distilled water cyclic washing to neutral then; Oven dry makes the active sludge carbon after the modification.
Step 2) activator in is ZnCl
2, KOH or H
2SO
4, its concentration is 3-5mol/L, preferred ZnCl
2
Modified solution in the step 4) is HNO
3, H
2O
2Or ammoniacal liquor, its concentration is 1-7mol/L.
The invention has the advantages that the excess sludge that utilizes the sewage-farm; Carry out the surface texture modification, can optimize the pore-size distribution of active sludge carbon, change surface acid base groups content; Especially the active sludge carbon after the modification has obtained to be rich in acid surface functional group; Absorption property also improves greatly, and dyeing waste water is had good adsorption effect, to the methylene blue clearance up to 92% modified sewage sludge absorbent charcoal.
The specific embodiment
Below in conjunction with the specific embodiment the present invention is described further.
Embodiment 1
1) with drying sludge, grind, sieve, keeping particle size range is 20-60 purpose mud granule;
2), be that 9:1 mixes according to mud and agricultural crop straw mass ratio, again with the ZnCl of this mud granule and 4mol/L with agricultural crop straw (optional maize straw) drying
2Solution is that 1g:2ml mixes by solid-to-liquid ratio, floods 24h down in normal temperature, is dried to constant weight afterwards, obtains the activated sludge particle;
3) with nitrogen as protection gas, after the activated sludge particle put into Muffle furnace and be warming up to 600 ℃ of insulation 60min with the heating rate of 10 ℃/min, be cooled to normal temperature; Back hydrochloric acid flush away impurity; The distilled water cyclic washing of using 70-80 ℃ again is to neutral, and oven dry promptly obtains active sludge carbon;
4) active sludge carbon that obtains in the step 3) is further ground, sieves, get the active sludge carbon below the 10g200 order, add the HNO of 1mol/L
3Solution 100ml evenly stirred 24 hours with agitator, used the distilled water cyclic washing to neutral then, and oven dry makes the active sludge carbon after the modification.
To this modified sewage sludge absorbent charcoal surface functional group with the quantitative analysis of Boehm titration: total acidic group 1.2453mmol/g, carboxyl 0.8026mmol/g, phenolic hydroxyl group 0.1205mmol/g, lactone group 0.0984mmol/g, total alkaline group 0.1543mmol/g.
Absorption property to sludge activity carbon after the modification detects: accurately take by weighing the active sludge carbon 0.1g after the above-mentioned modification; Put into the conical flask of 250ml; Adding 100ml concentration is the methylene blue solution of 100mg/L; Normal temperature stirs 30min down, gets supernatant after leaving standstill, and measures methylene blue concentration with ultraviolet-visible spectrophotometry.Recording clearance is 90.27%, and adsorbance is 88.79%.
Embodiment 2
1) with drying sludge, grind, sieve, keeping particle size range is 20-60 purpose mud granule;
2), be that 9:1 mixes according to mud and agricultural crop straw mass ratio, again with the ZnCl of this mud granule and 4mol/L with agricultural crop straw (optional maize straw) drying
2Solution is that 1g:2ml mixes by solid-to-liquid ratio, floods 24h down in normal temperature, is dried to constant weight afterwards, obtains the activated sludge particle;
3) with nitrogen as protection gas, after the activated sludge particle put into Muffle furnace and be warming up to 600 ℃ of insulation 60min with the heating rate of 10 ℃/min, be cooled to normal temperature; Back hydrochloric acid flush away impurity; The distilled water cyclic washing of using 70-80 ℃ again is to neutral, and oven dry promptly obtains active sludge carbon;
4) active sludge carbon that obtains in the step 3) is further ground, sieves, get the active sludge carbon below the 10g200 order, add the HNO of 3mol/L
3Solution 100ml evenly stirred 24 hours with agitator, used the distilled water cyclic washing to neutral then, and oven dry makes the active sludge carbon after the modification.
To this modified sewage sludge absorbent charcoal surface functional group with the quantitative analysis of Boehm titration: total acidic group 1.4583mmol/g, carboxyl 0.9652mmol/g, phenolic hydroxyl group 0.1125mmol/g, lactone group 0.0855mmol/g, total alkaline group 0.1485mmol/g.
Absorption property to sludge activity carbon after the modification detects: accurately take by weighing the active sludge carbon 0.1g after the above-mentioned modification; Put into the conical flask of 250ml; Adding 100ml concentration is the methylene blue solution of 100mg/L; Normal temperature stirs 30min down, gets supernatant after leaving standstill, and measures methylene blue concentration with ultraviolet-visible spectrophotometry.Recording clearance is 91.07%, and adsorbance is 90.57%.
Embodiment 3
1) with drying sludge, grind, sieve, keeping particle size range is 20-60 purpose mud granule;
2), be that 9:1 mixes according to mud and agricultural crop straw mass ratio, again with the ZnCl of this mud granule and 4mol/L with agricultural crop straw (optional maize straw) drying
2Solution is that 1g:2ml mixes by solid-to-liquid ratio, floods 24h down in normal temperature, is dried to constant weight afterwards, obtains the activated sludge particle;
3) with nitrogen as protection gas, after the activated sludge particle put into Muffle furnace and be warming up to 600 ℃ of insulation 60min with the heating rate of 10 ℃/min, be cooled to normal temperature; Back hydrochloric acid flush away impurity; The distilled water cyclic washing of using 70-80 ℃ again is to neutral, and oven dry promptly obtains active sludge carbon;
4) active sludge carbon that obtains in the step 3) is further ground, sieves, get the active sludge carbon below the 10g200 order, add the HNO of 5mol/L
3Solution 100ml evenly stirred 24 hours with agitator, used the distilled water cyclic washing to neutral then, and oven dry makes the active sludge carbon after the modification.
To this modified sewage sludge absorbent charcoal surface functional group with the quantitative analysis of Boehm titration: total acidic group 1.5689mmol/g, carboxyl 1.0258mmol/g, phenolic hydroxyl group 0.1259mmol/g, lactone group 0.08721mmol/g, total alkaline group 0.1511mmol/g.
Absorption property to sludge activity carbon after the modification detects: accurately take by weighing the active sludge carbon 0.1g after the above-mentioned modification; Put into the conical flask of 250ml; Adding 100ml concentration is the methylene blue solution of 100mg/L; Normal temperature stirs 30min down, gets supernatant after leaving standstill, and measures methylene blue concentration with ultraviolet-visible spectrophotometry.Recording clearance is 92%, and adsorbance is 91.12%.
Embodiment 4
1) with drying sludge, grind, sieve, keeping particle size range is 20-60 purpose mud granule;
2), be that 9:1 mixes according to mud and agricultural crop straw mass ratio, again with the ZnCl of this mud granule and 4mol/L with agricultural crop straw (optional maize straw) drying
2Solution is that 1g:2ml mixes by solid-to-liquid ratio, floods 24h down in normal temperature, is dried to constant weight afterwards, obtains the activated sludge particle;
3) with nitrogen as protection gas, after the activated sludge particle put into Muffle furnace and be warming up to 600 ℃ of insulation 60min with the heating rate of 10 ℃/min, be cooled to normal temperature; Back hydrochloric acid flush away impurity; The distilled water cyclic washing of using 70-80 ℃ again is to neutral, and oven dry promptly obtains active sludge carbon;
4) active sludge carbon that obtains in the step 3) is further ground, sieves, get the active sludge carbon below the 10g200 order, the adding mass fraction is 5% H
2O
2Solution 100ml evenly stirred 24 hours with agitator, used the distilled water cyclic washing to neutral then, and oven dry makes the active sludge carbon after the modification.
To this modified sewage sludge absorbent charcoal surface functional group with the quantitative analysis of Boehm titration: total acidic group 1.2457mmol/g, carboxyl 0.8456mmol/g, phenolic hydroxyl group 0.0983mmol/g, lactone group 0.0652mmol/g, total alkaline group 0.1641mmol/g.
Absorption property to sludge activity carbon after the modification detects: accurately take by weighing the active sludge carbon 0.1g after the above-mentioned modification; Put into the conical flask of 250ml; Adding 100ml concentration is the methylene blue solution of 100mg/L; Normal temperature stirs 30min down, gets supernatant after leaving standstill, and measures methylene blue concentration with ultraviolet-visible spectrophotometry.Recording clearance is 86.79%, and adsorbance is 85.12%.
Embodiment 5
1) with drying sludge, grind, sieve, keeping particle size range is 20-60 purpose mud granule;
2), be that 9:1 mixes according to mud and agricultural crop straw mass ratio, again with the ZnCl of this mud granule and 4mol/L with agricultural crop straw (optional maize straw) drying
2Solution is that 1g:2ml mixes by solid-to-liquid ratio, floods 24h down in normal temperature, is dried to constant weight afterwards, obtains the activated sludge particle;
3) with nitrogen as protection gas, after the activated sludge particle put into Muffle furnace and be warming up to 600 ℃ of insulation 60min with the heating rate of 10 ℃/min, be cooled to normal temperature; Back hydrochloric acid flush away impurity; The distilled water cyclic washing of using 70-80 ℃ again is to neutral, and oven dry promptly obtains active sludge carbon;
4) active sludge carbon that obtains in the step 3) is further ground, sieves, get the active sludge carbon below the 10g200 order, the adding mass fraction is 10% H
2O
2Solution 100ml evenly stirred 24 hours with agitator, used the distilled water cyclic washing to neutral then, and oven dry makes the active sludge carbon after the modification.
To this modified sewage sludge absorbent charcoal surface functional group with the quantitative analysis of Boehm titration: total acidic group 1.1986mmol/g, carboxyl 0.8826mmol/g, phenolic hydroxyl group 0.1005mmol/g, lactone group 0.06194mmol/g, total alkaline group 0.1621mmol/g.
Absorption property to sludge activity carbon after the modification detects: accurately take by weighing the active sludge carbon 0.1g after the above-mentioned modification; Put into the conical flask of 250ml; Adding 100ml concentration is the methylene blue solution of 100mg/L; Normal temperature stirs 30min down, gets supernatant after leaving standstill, and measures methylene blue concentration with ultraviolet-visible spectrophotometry.Recording clearance is 85.23%, and adsorbance is 84.96%.
Embodiment 6
1) with drying sludge, grind, sieve, keeping particle size range is 20-60 purpose mud granule;
2), be that 9:1 mixes according to mud and agricultural crop straw mass ratio, again with the ZnCl of this mud granule and 4mol/L with agricultural crop straw (optional maize straw) drying
2Solution is that 1g:2ml mixes by solid-to-liquid ratio, floods 24h down in normal temperature, is dried to constant weight afterwards, obtains the activated sludge particle;
3) with nitrogen as protection gas, after the activated sludge particle put into Muffle furnace and be warming up to 600 ℃ of insulation 60min with the heating rate of 10 ℃/min, be cooled to normal temperature; Back hydrochloric acid flush away impurity; The distilled water cyclic washing of using 70-80 ℃ again is to neutral, and oven dry promptly obtains active sludge carbon;
4) active sludge carbon that obtains in the step 3) is further ground, sieves, get the active sludge carbon below the 10g200 order, the adding mass fraction is 20% H
2O
2Solution 100ml evenly stirred 24 hours with agitator, used the distilled water cyclic washing to neutral then, and oven dry makes the active sludge carbon after the modification.
To this modified sewage sludge absorbent charcoal surface functional group with the quantitative analysis of Boehm titration: total acidic group 1.171mmol/g, carboxyl 0.8014mmol/g, phenolic hydroxyl group 0.07965mmol/g, lactone group 0.0961mmol/g, total alkaline group 0.1593mmol/g.
Absorption property to sludge activity carbon after the modification detects: accurately take by weighing the active sludge carbon 0.1g after the above-mentioned modification; Put into the conical flask of 250ml; Adding 100ml concentration is the methylene blue solution of 100mg/L; Normal temperature stirs 30min down, gets supernatant after leaving standstill, and measures methylene blue concentration with ultraviolet-visible spectrophotometry.Recording clearance is 85.12%, and adsorbance is 84.48%.
Comparative Examples
1) with drying sludge, grind, sieve, keeping particle size range is 20-60 purpose mud granule;
2), be that 9:1 mixes according to mud and agricultural crop straw mass ratio, again with the ZnCl of this mud granule and 4mol/L with agricultural crop straw (optional maize straw) drying
2Solution is that 1:2 mixes by solid-to-liquid ratio, floods 24h down in normal temperature, is dried to constant weight afterwards, obtains the activated sludge particle;
3) with nitrogen as protection gas, after the activated sludge particle put into Muffle furnace and be warming up to 600 ℃ of insulation 60min with the heating rate of 10 ℃/min, be cooled to normal temperature; The back is with hydrochloric acid flush away impurity; The distilled water cyclic washing of using 70-80 ℃ again is to neutral, and oven dry promptly obtains active sludge carbon.
To this unmodified active sludge carbon surface functional group with the quantitative analysis of Boehm titration: total acidic group 0.5864mmol/g, carboxyl 0.5012mmol/g, phenolic hydroxyl group 0.0258mmol/g, lactone group 0.0095mmol/g, total alkaline group 0.1403mmol/g.
The sludge activity carbon that does not carry out modification is made absorption property to be detected: accurately take by weighing this active sludge carbon 0.1g; Put into the conical flask of 250ml; Adding 100ml concentration is the methylene blue solution of 100mg/L; Normal temperature stirs 30min down, gets supernatant after leaving standstill, and measures methylene blue concentration with ultraviolet-visible spectrophotometry.Recording clearance is 75.12%, and adsorbance is 72.58%.
Can be known that by above instance the content of the active sludge carbon acidic functionality after the modification all has more significantly to be increased, absorption property also all obviously is superior to unmodified active sludge carbon, and is known by embodiment 1-3, within the specific limits, and along with HNO
3The increase of solution concentration, adsorption effect are good more, know by embodiment 4-6, within the specific limits, along with H
2O
2Liquid quality fraction reduces, and adsorption effect is good more.
Claims (4)
1. the surface modifying method of the active sludge carbon of a dye wastewater treatment using is characterized in that, may further comprise the steps:
1) with drying sludge, grind, sieve, keeping particle size range is 40-100 purpose mud granule;
2) agricultural crop straw is dry; Quality percentage composition according to mud is 60-90%; The quality percentage composition of agricultural crop straw is that the ratio of 10-40% is mixed the two, and be 1g with activator solution by solid-to-liquid ratio with this two mixture again: (1-4) ml mixes, and floods 12-24h down in normal temperature; Be dried to constant weight afterwards, obtain the activated sludge particle;
3) with nitrogen as the protection gas; After the activated sludge particle put into Muffle furnace and be warming up to 450-650 ℃ of insulation 30-90min with the heating rate of 6-20 ℃/min; Be cooled to normal temperature; Back hydrochloric acid flush away impurity; The distilled water cyclic washing of using 70-80 ℃ again is to neutral; Oven dry promptly obtains active sludge carbon;
4) active sludge carbon that obtains in the step 3) is further ground, sieves; The active sludge carbon of getting below 200 orders adds modified solution; The solid-liquid amount ratio of active sludge carbon and modified solution is (1-4) g: (10-40) ml, and evenly stir with agitator and to leave standstill at least 4 hours after 4-6 hour, use the distilled water cyclic washing to neutral then; Oven dry makes the active sludge carbon after the modification.
2. according to the method for claim 1, it is characterized in that step 2) in activator be ZnCl
2, KOH or H
2SO
4, its concentration is 3-5mol/L.
3. according to the method for claim 2, it is characterized in that activator is ZnCl
2
4. according to the method for claim 1, it is characterized in that the modified solution in the step 4) is HNO
3, H
2O
2Or ammoniacal liquor, its concentration is 1-7mol/L.
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| CN107500290A (en) * | 2017-10-16 | 2017-12-22 | 安徽工业大学 | Recycling treatment method of cassava alcohol sludge |
| CN108163909A (en) * | 2017-12-25 | 2018-06-15 | 苏州纳贝通环境科技有限公司 | A kind of composite water disposal agent and preparation method thereof |
| WO2020147303A1 (en) * | 2019-01-16 | 2020-07-23 | 中国科学院城市环境研究所 | Sludge-based dephosphoring material and preparation method therefor and treatment method for phosphorus-containing wastewater |
| CN110240386A (en) * | 2019-07-11 | 2019-09-17 | 中国科学院城市环境研究所 | A kind of stalk cooperates with the devices and methods therefor of processing with sludge |
| CN110240386B (en) * | 2019-07-11 | 2023-11-17 | 中国科学院城市环境研究所 | Straw and sludge cooperative treatment device and method |
| TWI717188B (en) * | 2020-01-09 | 2021-01-21 | 國立高雄科技大學 | Method for producing activated carbon by utilizing sludge of dyeing and finishing wastewater |
| CN112079353A (en) * | 2020-09-04 | 2020-12-15 | 仲恺农业工程学院 | Preparation technology of active biochar for modifying traditional Chinese medicine residues |
| CN114768772A (en) * | 2022-06-07 | 2022-07-22 | 陕西科技大学 | Modified hydrothermal carbon, preparation method thereof and process method for removing Cr (VI) in water |
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Application publication date: 20121003 |