CN111533126A - Preparation method of high-compressive-strength high-porosity formed sludge activated carbon - Google Patents
Preparation method of high-compressive-strength high-porosity formed sludge activated carbon Download PDFInfo
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- CN111533126A CN111533126A CN202010440208.0A CN202010440208A CN111533126A CN 111533126 A CN111533126 A CN 111533126A CN 202010440208 A CN202010440208 A CN 202010440208A CN 111533126 A CN111533126 A CN 111533126A
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- C01B32/324—Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
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Abstract
The invention discloses a preparation method of high-compressive-strength high-porosity formed sludge activated carbon, which is characterized in that mechanically dewatered sludge discharged from a sewage treatment plant is taken as a raw material, and the high-compressive-strength high-porosity formed sludge activated carbon is obtained by sequentially carrying out the working procedures of drying, pyrolysis, grinding, mixing, pressing, aging, carbonization and activation. The invention utilizes the mechanical dewatered sludge discharged by the sewage treatment plant to prepare the formed activated carbon, can achieve the aim of treating waste by waste, has simple preparation process and no secondary pollution, and the formed sludge activated carbon has high compressive strength, rich porosity and easy recycling.
Description
Technical Field
The invention relates to a preparation method of formed sludge activated carbon with high compressive strength and high porosity.
Background
In recent years, the sludge discharge amount of China is increased year by year, and the sludge discharge amount per year in China is more than 4000 million tons. The conventional methods of landfill, incineration, agriculture and the like are limited by factors such as land resources, pollutant discharge, heavy metals and the like. The preparation of sludge into an activated carbon adsorbent is one of the research hotspots at home and abroad at present. At present, the common preparation method at home and abroad is that the sludge is pyrolyzed and carbonized at a certain temperature to prepare sludge carbon particles, and then the sludge carbon particles are activated by a physical or chemical activation method to improve the quality of the sludge coalSpecific surface area and adsorption capacity. However, the conventional method mainly has the following two problems: 1) the carbon content of the sludge pyrolytic carbon is low (5-15%), the ash content is high, and the sludge carbon activation and pore-increasing effect is poor; 2) the prepared peat is in a powder or granular state, is easy to run off and has larger recovery difficulty. Based on the above, domestic related researchers have proposed a method for preparing sludge-forming activated carbon, such as: chinese patent application No. 201710940805.8: a method for preparing the formed sludge activated carbon is provided in the 'method for preparing the formed sludge activated carbon', the forming method is to extrude wet sludge into sludge cakes and then carry out pyrolysis carbonization, and as a large amount of water and organic matters are separated out in the pyrolysis carbonization process of the wet sludge cakes, the obtained formed sludge coal has a loose framework and extremely low compressive strength, and is extremely easy to break into powder and particles; chinese patent application No. 201310454943.7: the preparation method of the sludge-based formed magnetic activated carbon provides a method for preparing the formed magnetic sludge activated carbon by using a chemical activation method, but the reaction conditions of the forming and activation methods are harsh, and the chemical activation method not only causes chemical agents (HCl, KOH and ZnCl)2Etc.) and the waste water generated by the activated carbon pickling is very easy to cause secondary pollution.
In order to make up for the current defects, the preparation method of the formed sludge activated carbon, which has the advantages of low cost, no secondary pollution, high compressive strength, good adsorption effect and easy recovery, is urgently needed to be developed.
Disclosure of Invention
The invention aims to provide a preparation method of the formed sludge activated carbon, which has the advantages of low cost, no secondary pollution, high compressive strength, good adsorption effect and easy recovery.
In order to solve the problems, the invention provides a preparation method of a high compressive strength and high porosity formed sludge activated carbon, which is characterized in that mechanically dewatered sludge discharged from a sewage treatment plant is taken as a raw material, and the high compressive strength and high porosity formed sludge activated carbon is obtained by sequentially carrying out the working procedures of drying, pyrolysis, grinding, mixing, pressing, aging, carbonization and activation.
Preferably, the drying is specifically: drying the sludge at 110 +/-5 ℃ until the water content is lower than 40 wt%.
Preferably, the pyrolysis is in particular: and (3) pyrolyzing the sludge to prepare sludge carbon particles, wherein the pyrolysis temperature is 400-900 ℃, and the pyrolysis reaction time is 30-60 minutes.
Preferably, the grinding is in particular: grinding the sludge carbon particles to a particle size of less than 0.125mm to obtain sludge carbon powder.
Preferably, the mixing is specifically: adding 5-30% by mass of organic binder into the sludge carbon powder, and uniformly mixing by a mechanical stirring or ultrasonic method.
More preferably, the organic binder is a phenolic resin, sodium carboxymethylcellulose, bitumen, paraffin oil or rosin.
Preferably, the pressing is in particular: and putting the mixture of the sludge carbon powder and the organic binder into a mold, and pressing for 10-30 minutes to obtain a sample, wherein the pressure is 1-8 Mpa.
Preferably, the aging is specifically: and (3) carrying out heat treatment on the sample for 30-90 minutes at 400-900 ℃ under an inert atmosphere.
Preferably, the carbonization is specifically: and carbonizing the aged sample for 30-90 minutes at the temperature of 110 +/-5 ℃.
Preferably, the activation is in particular: activating the carbonized sample by a physical activation method and taking carbon dioxide or water vapor as an activating agent; the volume concentration of the activating agent is 20-100%, the activating temperature is 700-950 ℃, and the activating time is 30-90 minutes.
Compared with the prior art, the invention has the beneficial effects that: the formed activated carbon is prepared by using the mechanical dewatered sludge discharged by a sewage treatment plant, the purpose of treating waste by waste can be achieved, the preparation process is simple, secondary pollution is avoided, the formed sludge activated carbon has high compressive strength and rich porosity, and is easy to recycle.
Drawings
FIG. 1 is a data plot of the adsorption effect of shaped sludge activated carbon prepared with different activation regimes on different concentrations of methylene blue.
Detailed Description
In order to make the invention more comprehensible, preferred embodiments are described in detail below with reference to the accompanying drawings.
Example 1
Preparing 1# formed sludge activated carbon:
1) 200g of mechanically dewatered sludge is taken and put into a forced air drying oven, dried for 12 hours at 110 ℃ until the sludge is completely dried, and then cooled to room temperature;
2) putting 48.34g of dry sludge into a tubular electric heating furnace, introducing 1L/min of pure nitrogen into the electric heating furnace, carrying out temperature programming to 800 ℃ at a heating rate of 10 ℃/min, carrying out high-temperature pyrolysis on the dried sludge for 1 hour at 800 ℃, and then cooling the dried sludge to room temperature to obtain 20.43g of sludge thermal decomposition sample;
3) grinding the pyrolyzed product in a mortar, and sieving the ground product by using a 120-mesh sieve to obtain granular sludge pyrolytic carbon with the particle size of less than 0.125 mm;
4) weighing 3.24g of binder phenolic resin in a beaker, adding 20ml of absolute ethyl alcohol, stirring with a glass rod until the binder phenolic resin is completely dissolved, adding 12.96g of dry sludge powder, stirring uniformly, placing in an ultrasonic cleaner, running for 40 minutes, and drying to a certain degree;
5) weighing 0.9g of the mixed sludge pyrolytic carbon, putting the mixed sludge pyrolytic carbon into a forming die, pressing the mixed sludge pyrolytic carbon for 15 minutes by using an oil jack, controlling the force to keep the pressure at 2.5MPa, and after pressing, putting a sample into a forced air drying oven to be cured for 1 hour at 110 ℃ so as to prepare dried cake-shaped carbon with the diameter of 15mm and the thickness of 3.5 mm;
6) putting 10 blocks of cake-shaped carbon with the total mass of 7.84g after being pressed into a tubular resistance furnace, heating to 800 ℃ again by a heating rate program of 10 ℃/min under the pure nitrogen atmosphere of 300mL/min, and carbonizing for 1 hour at 800 ℃;
7) after carbonization, continuously introducing nitrogen, rapidly heating to 850 ℃, and introducing 300mL/min CO into the electric heating furnace2And keeping for 30 minutes, and finally cooling to room temperature to obtain a sample with the total mass of 5.83g, namely the No. 1 molded sludge activated carbon.
Adsorbing methylene blue: putting 1# formed sludge activated carbon with the total mass of 5.83g into 9 250mL conical flasks, wherein the conical flasks are respectively filled with methylene blue solutions of 1500mg/L, 1100mg/L, 700mg/L, 400mg/L, 200mg/L, 100mg/L, 60mg/L, 30mg/L and 10mg/L, and the initial pH of the solution is 7; oscillating at room temperature of 25 ℃ in the dark at a speed of 110r/min by using a reciprocating horizontal oscillator until the adsorption is saturated, wherein the adsorption capacity of the 1# shaped sludge activated carbon on methylene blue with different concentrations is shown in figure 1.
As can be seen from FIG. 1, the specific surface area of the obtained No. 1 formed sludge activated carbon is 204.4m2G, compressive strength of 47kg/cm2The IRI drop resistance index is 245, and the saturated adsorption capacity to methylene blue is 253 mg/g.
Example 2
Preparing 2# formed sludge activated carbon:
1) 200g of mechanically dewatered sludge is taken and put into a forced air drying oven, dried for 12 hours at 110 ℃ until the sludge is completely dried, and then cooled to room temperature;
2) 55.37g of dry sludge particles are put into a tubular electric heating furnace, 1L/min of pure nitrogen is introduced into the electric heating furnace, the temperature is programmed to 800 ℃ at the heating rate of 10 ℃/min, the mixture is pyrolyzed at the high temperature of 800 ℃ for 1 hour, and then the mixture is cooled to the room temperature, so that 32.21g of sludge pyrolytic sample is obtained;
3) grinding the pyrolyzed product in a mortar, and sieving the ground product by using a 120-mesh sieve to obtain granular sludge pyrolytic carbon with the particle size of less than 0.125 mm;
4) weighing 5.04g of binder phenolic resin in a beaker, adding 29ml of absolute ethyl alcohol, stirring with a glass rod until the binder phenolic resin is completely dissolved, adding 20.16g of dry sludge powder, stirring uniformly, placing in an ultrasonic cleaner, running for 40 minutes, and drying to a certain degree;
5) weighing 0.9g of the mixed sludge pyrolytic carbon, putting the mixed sludge pyrolytic carbon into a forming die, pressing the mixed sludge pyrolytic carbon for 15 minutes by using an oil jack, controlling the force to keep the pressure at 2.5MPa, and after pressing, putting a sample into a forced air drying oven to be cured for 1 hour at 110 ℃ so as to prepare dried cake-shaped carbon with the diameter of 15mm and the thickness of 3.5 mm;
6) putting 9 cakes of pressed charcoal with the total mass of 6.61g in a tubular resistance furnace, heating to 800 ℃ again at the heating rate of 10 ℃/min in the pure nitrogen atmosphere of 300mL/min, and carbonizing for 1 hour at 800 ℃;
7) after carbonization, continuously introducing nitrogen, rapidly heating to 900 ℃, then introducing 300mL/min H into the electric heating furnace by using a water vapor generator2And keeping the temperature for 60 minutes, and finally cooling to room temperature to obtain a sample with the total mass of 5.43g, namely the 2# formed sludge activated carbon.
The reaction condition of adsorbing methylene blue is the same as that of the example 1, and the adsorbing amount of the 2# formed sludge activated carbon to the methylene blue with different concentrations is shown in the figure 1.
As can be seen from FIG. 1, the obtained 2# shaped sludge activated carbon has a specific surface area of 203m2G, compressive strength of 45kg/cm2The IRI drop resistance index is 167, and the saturated adsorption capacity of the adsorbent 2 to methylene blue is 206 mg/g.
Claims (10)
1. The preparation method of the high-compressive-strength high-porosity formed sludge activated carbon is characterized in that mechanically dewatered sludge discharged by a sewage treatment plant is used as a raw material, and the high-compressive-strength high-porosity formed sludge activated carbon is obtained by sequentially carrying out drying, pyrolysis, grinding, mixing, pressing, aging, carbonization and activation procedures.
2. The method for preparing the high compressive strength and high porosity formed sludge activated carbon as claimed in claim 1, wherein the drying specifically comprises: drying the sludge at 110 +/-5 ℃ until the water content is lower than 40 wt%.
3. The method for preparing the high compressive strength and high porosity formed sludge activated carbon as claimed in claim 2, wherein the pyrolysis specifically comprises: and (3) pyrolyzing the sludge to prepare sludge carbon particles, wherein the pyrolysis temperature is 400-900 ℃, and the pyrolysis reaction time is 30-60 minutes.
4. The method for preparing the high compressive strength and high porosity formed sludge activated carbon as claimed in claim 3, wherein the grinding is specifically: grinding the sludge carbon particles to a particle size of less than 0.125mm to obtain sludge carbon powder.
5. The method for preparing the high compressive strength and high porosity formed sludge activated carbon as claimed in claim 4, wherein the mixing is specifically: adding 5-30% by mass of organic binder into the sludge carbon powder, and uniformly mixing by a mechanical stirring or ultrasonic method.
6. The method of claim 5, wherein the organic binder is phenolic resin, sodium carboxymethylcellulose, pitch, paraffin oil or rosin.
7. The method for preparing the high compressive strength and high porosity formed sludge activated carbon as claimed in claim 5, wherein the pressing is specifically: and putting the mixture of the sludge carbon powder and the organic binder into a mold, and pressing for 10-30 minutes to obtain a sample, wherein the pressure is 1-8 Mpa.
8. The method for preparing the high compressive strength and high porosity formed sludge activated carbon as claimed in claim 7, wherein the aging is specifically: and (3) carrying out heat treatment on the sample for 30-90 minutes at 400-900 ℃ under an inert atmosphere.
9. The method for preparing the formed sludge activated carbon with high compressive strength and high porosity as claimed in claim 8, wherein the carbonization specifically comprises: and carbonizing the aged sample for 30-90 minutes at the temperature of 110 +/-5 ℃.
10. The method for preparing the high compressive strength and high porosity formed sludge activated carbon as claimed in claim 9, wherein the activating is specifically: activating the carbonized sample by a physical activation method and taking carbon dioxide or water vapor as an activating agent; the volume concentration of the activating agent is 20-100%, the activating temperature is 700-950 ℃, and the activating time is 30-90 minutes.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116177802A (en) * | 2023-02-22 | 2023-05-30 | 中交第二公路勘察设计研究院有限公司 | Modularized biodegradation device and method for bionic dolphin |
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2020
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116177802A (en) * | 2023-02-22 | 2023-05-30 | 中交第二公路勘察设计研究院有限公司 | Modularized biodegradation device and method for bionic dolphin |
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