CN113231017B - Modified superfine powder activated carbon and preparation method and application thereof - Google Patents

Modified superfine powder activated carbon and preparation method and application thereof Download PDF

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CN113231017B
CN113231017B CN202110477921.7A CN202110477921A CN113231017B CN 113231017 B CN113231017 B CN 113231017B CN 202110477921 A CN202110477921 A CN 202110477921A CN 113231017 B CN113231017 B CN 113231017B
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activated carbon
powder activated
bicarbonate
auxiliary agent
modifying
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CN113231017A (en
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周扬
付俊豪
高源�
江进
胡坚鹏
郭钦
潘汉平
黄润
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Guangdong University of Technology
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • B01J20/28016—Particle form
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C02F2101/20—Heavy metals or heavy metal compounds
    • C02F2101/206—Manganese or manganese compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/34—Organic compounds containing oxygen
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/36—Organic compounds containing halogen
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/38—Organic compounds containing nitrogen

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Water Treatment By Sorption (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

The invention discloses modified superfine powder activated carbon and a preparation method and application thereof, wherein the preparation method comprises the following steps: mixing powdery active carbon with the particle size of more than 0.1mm and a modifying additive according to a proportion, and grinding into particles with the particle size of less than 10 mu m to obtain modified superfine powder active carbon; the modifying auxiliary agent comprises the following components in percentage by mass: 45-85% of peroxymonosulfate, 5-15% of silicon dioxide, 5-20% of bicarbonate and 5-20% of phosphate; the mass ratio of the powdery active carbon to the modifying auxiliary agent is 1: (0.01-2). According to the invention, the surface of the activated carbon is subjected to grinding modification, so that the oxygen-containing functional group amount of the surface of the activated carbon is increased, the adsorption capacity of the activated carbon is further enhanced, and the method can be used for treating hydrophilic organic micro-pollutants in water; the modified superfine powder activated carbon and sulfite are combined for further removing manganese ions in water.

Description

Modified superfine powder activated carbon and preparation method and application thereof
Technical Field
The invention relates to the technical field of water treatment, in particular to modified superfine powder activated carbon, and a preparation method and application thereof.
Background
The widespread presence of organic micropollutants in water presents a potential threat to the ecological environment and human health, with hydrophilic organic micropollutants being one of the most frequently detected organic pollutants in the environment (e.g., contrast agents, antibiotics, etc.), receiving widespread attention in the water treatment industry. Most of hydrophilic organic micro-pollutants have certain biotoxicity, can have adverse effects on the growth and development of organisms, and seriously threaten ecological safety and human health. Because the hydrophilic organic micropollutants are relatively strong in polarity and stable in property, the hydrophilic organic micropollutants are difficult to remove by conventional water treatment processes (such as coagulation, precipitation, filtration, biological treatment and the like). Therefore, how to remove hydrophilic organic pollutants in water in a green and efficient way becomes a current research hot spot and difficulty.
The activated carbon is an adsorption material widely applied in the field of water treatment, and has the advantages of wide sources, low price, difficult production of toxic and harmful byproducts, convenient addition and the like. The activated carbon may be classified into columnar activated carbon, crushed activated carbon, powdery activated carbon, and the like in terms of shape. From the classification of manufacturing raw materials, activated carbon mainly uses coal quality, wood and the like as raw materials. Activated carbon has a large specific surface area, a developed pore structure, and a rich surface functional group, and these properties also determine the excellent adsorption capacity of activated carbon. However, because the active carbon of different materials and shapes has larger property difference, the adsorption efficiency of the hydrophilic organic micropollutants is greatly different, and the removal effect is difficult to ensure. In order to solve the problem, chinese patent No. 109499541A discloses a preparation method of superfine powder activated carbon (22 days of 2019, 03 month) but the activated carbon prepared by the method has no regulation and control on the number of oxygen-containing functional groups on the surface and has still to improve the adsorption capacity on hydrophilic organic micro pollutants. Therefore, it is necessary to develop a feasible activated carbon modification method, which can enhance the removal capability of hydrophilic organic micropollutants while retaining the main adsorption characteristics of the activated carbon, and ensure the water quality safety.
Disclosure of Invention
The invention aims at solving the problem that the prior active carbon modification method cannot increase the oxygen-containing functional group on the surface, so that the adsorption capacity on hydrophilic organic micro-pollutants is weak, and provides a preparation method of modified superfine powder active carbon.
It is a further object of the present invention to provide a modified ultrafine powder activated carbon.
It is another object of the present invention to provide the use of the modified ultrafine powder activated carbon described above.
The above object of the present invention is achieved by the following technical solutions:
the preparation method of the modified superfine powder activated carbon comprises the following steps:
mixing powdery active carbon with the particle size of more than 0.1mm and a modifying additive according to a proportion, and grinding into particles with the particle size of less than 10 mu m to obtain modified superfine powder active carbon; the modifying auxiliary agent comprises the following components in percentage by mass: 45-85% of peroxymonosulfate, 5-15% of silicon dioxide, 5-20% of bicarbonate and 5-20% of phosphate; the mass ratio of the powdery active carbon to the modifying auxiliary agent is 1: (0.01-2).
Powdered activated carbon having a particle size of more than 0.1mm may undergo severe extrusion friction during the grinding process, and the active surface inside thereof may be exposed with the grinding process. The modification auxiliary agent can carry out hydrophilic modification on the newly exposed active surfaces in the grinding process, so as to realize in-situ modification of the superfine active carbon. The peroxymonosulfate is used as an oxidant, and can perform epoxidation reaction with unsaturated bonds (such as olefin), aldehyde groups and carbonyl groups on the surface of the superfine activated carbon to generate an epoxidation structure and an internal peroxidation structure on the surface of the carbon material, so that the surface oxygen content of the superfine activated carbon is increased, the hydrophilicity of the superfine activated carbon is enhanced, and the adsorption capacity of the superfine activated carbon on hydrophilic organic pollutants is enhanced. The silica plays a role in strengthening the grinding effect and the modifying effect. Bicarbonate and phosphate stabilize the acid-base nature of the reaction interface. Because the preparation process is not carried out in the solution, the modification reaction only occurs on the surface of the active carbon, but does not go deep into the pore structure inside the active carbon, so that the original adsorption characteristic of the active carbon can be well reserved.
Preferably, the mass ratio of the powdery activated carbon to the modifying auxiliary agent is 1: (0.1-1).
Preferably, the modifying auxiliary agent comprises the following components in percentage by mass: 58-72% of peroxymonosulfate, 8-12% of silicon dioxide, 10-15% of bicarbonate and 10-15% of phosphate.
In the invention, the powdered activated carbon is one or more of coconut activated carbon, coal activated carbon and wood activated carbon.
Preferably, the particle size of the powdered activated carbon is 0.5-1 mm.
The present invention may employ a peroxymonosulfate, bicarbonate, or phosphate salt as is conventional in the art.
Preferably, the peroxymonosulfate is one or two of potassium peroxymonosulfate and sodium peroxymonosulfate.
Preferably, the bicarbonate is one or more of sodium bicarbonate, potassium bicarbonate, ammonium bicarbonate or calcium bicarbonate.
Preferably, the phosphate is one or more of disodium hydrogen phosphate, dipotassium hydrogen phosphate, diammonium hydrogen phosphate, sodium pyrophosphate or potassium pyrophosphate.
The modified superfine powder activated carbon is prepared by the method.
The invention also protects the application of the modified superfine powder active carbon in removing hydrophilic organic micropollutants in water. Preferably, the hydrophilic organic micropollutant is selected from one or two of tetracycline and iopamidol.
The invention also protects the application of the modified superfine powder activated carbon and sulfite in removing manganese ions in water. Preferably, the mass ratio of the modified superfine powder active carbon to the sulfite is 1: (0.01-0.5).
After sulfite and modified superfine powder active carbon are added into a water body, an epoxidation/internal peroxidation structure at the interface of the active carbon oxidizes the sulfite to generate sulfite free radicals, and the sulfite free radicals can be quickly combined with dissolved oxygen to generate SO 5 ·- Free radical, SO 5 ·- Free radical oxidation of divalent manganeseTrivalent manganese is generated, and the trivalent manganese is further disproportionated to generate divalent manganese and manganese dioxide solid due to extremely poor stability, and the free radical chain reaction process is continuously carried out until manganese ions are completely converted into manganese dioxide, so that the removal of manganese ions in water is realized.
Specifically, the sulfite is selected from one or more of sodium sulfite, potassium sulfite, sodium bisulfite or potassium bisulfite.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention utilizes silicon dioxide to strengthen the grinding effect and the modification effect, stabilizes the acid-base property of a reaction interface through bicarbonate and phosphate, and then generates an epoxidation reaction with unsaturated bonds on the surface of active carbon and oxygen-containing functional groups such as carbonyl groups, aldehyde groups and the like by means of peroxymonosulfate to generate an epoxidation structure and an internal peroxidation structure, and increases the content of the oxygen-containing functional groups on the surface, thereby strengthening the adsorption capacity of the active carbon on hydrophilic organic pollutants.
2. The modified auxiliary agent used in the invention is a green and nontoxic chemical agent, so that the modified superfine powder activated carbon obtained by grinding can be directly used in the water treatment process without separation and purification.
3. The modified superfine powder active carbon and sulfite prepared by the invention can generate oxidative active species SO after being added into water 5 ·- And the free radicals can completely convert manganese ions in the water body into manganese dioxide solids, so that the removal of manganese ions in the water body is realized.
Detailed Description
The present invention will be described in further detail with reference to the following specific examples for the purpose of illustration and not limitation, and various modifications may be made within the scope of the present invention as defined by the appended claims. The raw material activated carbon of the embodiment of the invention is coal powder activated carbon sold by the environment industry activated carbon, and the particle size is 0.2-2mm.
Example 1
The preparation method of the modified superfine powder activated carbon comprises the following steps:
the mass ratio is 1:1, mixing the powder activated carbon and a modifying additive, and then placing the mixture into a dry ball mill to be ground into particles with the particle size smaller than 10 mu m, so as to obtain superfine powder activated carbon; the components of the modifying auxiliary agent comprise 72% of potassium hydrogen peroxymonosulfate, 8% of silicon dioxide, 10% of sodium bicarbonate and 10% of disodium hydrogen phosphate according to mass percent.
Example 2
This example 2 differs from example 1 in that the components of the modifying aid comprise, in mass percent, 65% of potassium hydrogen peroxymonosulfate, 10% of silicon dioxide, 12% of sodium bicarbonate and 13% of disodium hydrogen phosphate.
Example 3
This example 3 differs from example 1 in that the components of the modifying auxiliary agent comprise, in mass percent, 58% of potassium hydrogen peroxymonosulfate, 12% of silicon dioxide, 15% of sodium bicarbonate and 15% of disodium hydrogen phosphate.
Example 4
This example 4 differs from example 1 in that the components of the modifying aid comprise, in mass percent, 85% of potassium hydrogen peroxymonosulfate, 5% of silicon dioxide, 5% of sodium bicarbonate, 5% of disodium hydrogen phosphate.
Example 5
This example 5 differs from example 1 in that the components of the modifying auxiliary agent comprise, in mass percent, 45% of potassium hydrogen peroxymonosulfate, 15% of silicon dioxide, 20% of sodium bicarbonate and 20% of disodium hydrogen phosphate.
Example 6
This example 6 differs from example 1 in that the mass ratio of activated carbon to modifying auxiliary agent is 1:0.5.
example 7
This example 7 differs from example 1 in that the mass ratio of activated carbon to modifying auxiliary agent is 1:0.1.
example 8
The difference between this example 8 and example 1 is that the mass ratio of activated carbon to modifying auxiliary agent is 1:2.
example 9
This example 9 differs from example 1 in that the mass ratio of activated carbon to modifying auxiliary agent is 1:0.01.
example 10
The difference between this example 10 and example 1 is that the components of the modifying assistant include, by mass, 72% sodium hydrogen peroxide, 8% silica, 10% potassium hydrogen carbonate, and 10% dipotassium hydrogen phosphate.
Example 11
This example 11 differs from example 1 in that the components of the modifying auxiliary agent comprise, in mass percent, 72% of potassium hydrogen peroxymonosulfate, 8% of silicon dioxide, 10% of ammonium bicarbonate and 10% of diammonium phosphate.
Example 12
This example 12 differs from example 1 in that the components of the modifying auxiliary agent comprise, by mass, 72% of potassium hydrogen peroxymonosulfate, 8% of silicon dioxide, 10% of calcium bicarbonate and 10% of sodium pyrophosphate.
Example 13
This example 13 differs from example 1 in that the components of the modifying auxiliary agent comprise, by mass, 72% of potassium hydrogen peroxymonosulfate, 8% of silicon dioxide, 10% of sodium bicarbonate and 10% of potassium pyrophosphate.
Comparative example 1
The difference between comparative example 1 and example 1 is that the particle size distribution of the powder particles after grinding is 10 to 15. Mu.m.
Comparative example 2
This comparative example 2 differs from example 1 in that the modifying aid does not comprise potassium hydrogen peroxymonosulfate.
Comparative example 3
This comparative example 3 differs from example 1 in that the modifying aid does not include sodium bicarbonate.
Comparative example 4
This comparative example 4 differs from example 1 in that the modifying auxiliary does not include disodium hydrogen phosphate.
Comparative example 5
This comparative example 5 differs from example 1 in that no modifying auxiliary agent was added.
Comparative example 6
This comparative example 6 is different from example 1 in that the powdered activated carbon has a particle size distribution of 0.01 to 0.05mm.
Test characterization
The surface oxygen-containing functional groups of the modified ultrafine powder activated carbon obtained in examples 1 to 13 and comparative examples 1 to 6 were calculated. The method for calculating the oxygen-containing functional group on the surface comprises the following steps: the Boehm titration method utilizes a dilute solution of sodium ethoxide to neutralize acidic oxygen-containing functional groups on the surface of a carbon material, uses the neutralization value of the sodium ethoxide solution to represent carboxyl, lactone group, phenolic hydroxyl and carbonyl, prepares a hydrochloric acid solution and a sodium ethoxide standard solution according to national standard GBT601-2016, and uses a Metrele full-automatic potentiometric titrator for calibration.
0.2g of the modified ultrafine powder activated carbon obtained in examples 1 to 13 and comparative examples 1 to 6 was added to the simulated wastewater having a tetracycline concentration of 0.1mg/L and an iopamidol concentration of 0.1mg/L, respectively, and a quasi-secondary adsorption kinetic curve was measured to calculate the equilibrium adsorption amount. The equilibrium adsorption amount calculating method comprises the following steps: the quasi-secondary adsorption kinetic model generally has better fitting property, and the adsorption performance of the adsorbent can be evaluated by calculating the equilibrium adsorption quantity through a corresponding equation, wherein the quasi-secondary kinetic equation is as follows:
wherein k is 2 G.mg as adsorption rate constant –1 ·min –1 ；q e Mg.g for balancing adsorption quantity –1 ；q t Mg.g as the adsorption amount of the adsorbent at time t –1 。
The content of oxygen-containing functional groups on the surfaces of the products obtained in examples 1 to 13 and comparative examples 1 to 6, and the equilibrium adsorption amounts of the products on the hydrophilic organic pollutants, namely tetracycline and iopamidol, are shown in Table 1.
0.1g of the ultrafine powder activated carbon obtained in example 1 and 50mg of sodium sulfite were added to the simulated wastewater having a manganese ion concentration of 2mg/L, and the concentration of manganese ions in the wastewater was measured by sampling and filtration every 5 minutes. The method for measuring the concentration of manganese ions comprises the following steps: inductively coupled plasma emission spectrometry (ICP-OES). The effect of removing manganese ions in wastewater is shown in Table 2.
TABLE 1
It can be seen from examples 1 to 13 and comparative examples 1 to 6 that when a certain component is absent from the modified auxiliary agent, or the particle size of the modified activated carbon is larger, or the particle size of the raw activated carbon is too small, the content of the oxygen-containing functional group of the prepared modified activated carbon is affected, and the adsorption performance of the modified activated carbon on the hydrophilic organic micropollutants is further affected.
TABLE 2
As can be seen from Table 2, the modified ultrafine powder activated carbon and sulfite of the invention can be used together to remove manganese ions in water with high efficiency.
It is to be understood that the above examples of the present invention are provided by way of illustration only and not by way of limitation of the embodiments of the present invention. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. Any modification, equivalent replacement, improvement, etc. which come within the spirit and principles of the invention are desired to be protected by the following claims.

Claims (9)

1. The preparation method of the modified superfine powder activated carbon is characterized by comprising the following steps of:
mixing powdery active carbon with the particle size of more than 0.1mm and a modifying additive according to a proportion, and grinding into particles with the particle size of less than 10 mu m to obtain modified superfine powder active carbon; the modifying auxiliary agent comprises the following components in percentage by mass: 45-85% of hydrogen peroxide, 5-15% of silicon dioxide, 5-20% of bicarbonate and 5-20% of phosphate; the mass ratio of the powdery active carbon to the modifying auxiliary agent is 1: (0.01-2);
the phosphate is one or more of disodium hydrogen phosphate, dipotassium hydrogen phosphate, diammonium hydrogen phosphate, sodium pyrophosphate or potassium pyrophosphate.
2. The method for preparing modified ultrafine powder activated carbon according to claim 1, wherein the mass ratio of the powder activated carbon to the modifying auxiliary agent is 1: (0.1-1).
3. The method for preparing modified ultrafine powder activated carbon as defined in claim 1, wherein the modification auxiliary agent comprises the following components in percentage by mass: 58-72% of hydrogen peroxide, 8-12% of silicon dioxide, 10-15% of bicarbonate and 10-15% of phosphate.
4. The method for preparing modified ultrafine powder activated carbon according to claim 1, wherein the powder activated carbon is one or more of coconut activated carbon, coal activated carbon and wood activated carbon.
5. The method for preparing modified ultrafine powder activated carbon as defined in claim 1, wherein the peroxymonosulfate is one or both of potassium peroxymonosulfate and sodium peroxymonosulfate.
6. The method for preparing modified ultrafine powder activated carbon of claim 1, wherein the bicarbonate is one or more of sodium bicarbonate, potassium bicarbonate, ammonium bicarbonate, or calcium bicarbonate.
7. A modified ultrafine powder activated carbon characterized by being produced by the production method according to any one of claims 1 to 6.
8. Use of the modified ultrafine powder activated carbon of claim 7 to remove hydrophilic organic micropollutants from water.
9. The use of the modified ultrafine powder activated carbon of claim 7 with sulfite to remove manganese ions from water.
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CN103288201A (en) * 2013-06-20 2013-09-11 哈尔滨工业大学 Water treatment method for removing radioactive iodine pollution through combined use of persulfate and active carbon
JP2013184132A (en) * 2012-03-09 2013-09-19 Swing Corp Regeneration method for used activated carbon and activated carbon and method for manufacturing the same
KR20170100331A (en) * 2016-02-25 2017-09-04 현대자동차주식회사 Activated carbon and method for manufacturing the same
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JP2013184132A (en) * 2012-03-09 2013-09-19 Swing Corp Regeneration method for used activated carbon and activated carbon and method for manufacturing the same
CN103288201A (en) * 2013-06-20 2013-09-11 哈尔滨工业大学 Water treatment method for removing radioactive iodine pollution through combined use of persulfate and active carbon
KR20170100331A (en) * 2016-02-25 2017-09-04 현대자동차주식회사 Activated carbon and method for manufacturing the same
CN108479698A (en) * 2018-03-31 2018-09-04 河南省城乡规划设计研究总院有限公司 A kind of synchronous preparation method for removing the modified activated carbon of heavy metal and organic matter in sewage
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Inventor after: Pan Hanping

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