CN112892474A - Multifunctional industrial water treatment agent and preparation method thereof - Google Patents
Multifunctional industrial water treatment agent and preparation method thereof Download PDFInfo
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- 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
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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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
- B01J20/0229—Compounds of Fe
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- 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
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
Abstract
The invention discloses a preparation method of a multifunctional industrial water treatment medicament, which comprises the following steps: dissolving sucrose in 70-90 wt% concentrated sulfuric acid solution, then placing the solution in an ice bath at the temperature of-5-0 ℃, stirring the solution for 30-60 min, filtering the solution after the reaction is finished, taking precipitate, and washing the precipitate for 2-3 times by using deionized water; uniformly mixing the obtained precipitate with a dilute sulfuric acid solution with the mass fraction of 10-20 wt%, adding dimethyl titanate, stirring and reacting at 80-140 ℃ for 1-3 h, filtering, removing dimethyl titanate, drying the obtained precipitate, and calcining to obtain a mesoporous carbon material; and dissolving the obtained mesoporous carbon material in a ferric trichloride solution, adding ammonium chloride, performing ultrasonic mixing for 30min, standing overnight, taking out the mesoporous carbon material, washing, and drying at the temperature of 50-80 ℃ under a vacuum condition to obtain the multifunctional industrial water treatment agent. The industrial water treatment agent obtained by the method has obvious effect of removing pollutants in sewage.
Description
Technical Field
The invention belongs to the technical field of industrial water treatment, and particularly relates to a multifunctional industrial water treatment agent and a preparation method thereof.
Background
Water is an indispensable substance for human survival and development. With the growth of population and the development of society, the living environment of human beings is increasingly worsened, and the problems of water resource waste, pollution and the like are increasingly highlighted. Water and other resources are very important resources in daily life and production activities of human beings, and belong to basic resources of national economy.
The use of water resources is divided into industrial water and domestic water. The industrial water is characterized by serious pollution, high treatment cost and large consumption. At present, the utilization rate of industrial water in China is less than one half of that in developed countries, and the reuse rate is less than 60%. The total water consumption of unit national production is 50 to 100 times of that of developed countries, and the unit consumption of water is obviously higher than that of developed countries in Europe and America. The steel industry and the chemical industry are absolutely major households for industrial water, taking the steel industry as an example, about 50 tons of water are needed for producing ton steel in China, but less than 6 tons of water are needed in developed countries such as America, Japan and the like, and the gap is obvious. The limited human resources coupled with the low level of our energy savings have resulted in rapid energy consumption and drastic environmental degradation.
At present, the technology commonly used for industrial water treatment agents is also disclosed. For example, a chinese patent application No. cn202010675076.x discloses a papermaking wastewater treatment agent and a preparation method thereof, wherein the papermaking wastewater treatment agent is composed of the following raw materials in parts by weight: 0.5-2 parts of industrial water glass, 2-7 parts of ferric salt, 45-65 parts of aluminum sulfate, 2-4 parts of hydrochloric acid and 0.2-1 part of oxidant, and stirring and mixing uniformly to prepare the papermaking wastewater treatment agent for deep coagulation treatment of papermaking wastewater. The invention also provides a preparation method of the treatment agent for papermaking wastewater, and the water treatment agent is formed by stirring the components.
For another example, chinese patent application No. CN201910998349.1 discloses a water treatment agent, which comprises the following main components: 50-55% of organic modified concave-convex soil, 12-16% of phosphonate, 9-11% of polycarboxylate, 6-11% of organic phosphonate and 7-23% of sulfonate copolymer, wherein the phosphonate is carboxyl ethylidene diphosphonate or inorganic polyphosphonate, the polycarboxylate is polyquaternary ammonium sodium, and the organic modified concave-convex soil is composed of concave-convex soil, a modifier and distilled water.
Although the above treatment agents can be used in sewage treatment to some extent, their raw material composition contains various compounds, such as organic phosphines, which are likely to cause secondary pollution and are not easily removed.
The nano porous Carbon material (NPC) refers to a Carbon material with a nano pore channel structure, and the pore diameter is generally less than 100 nm. The porous carbon can be divided into microporous carbon (Micropore less than or equal to 2nm), mesoporous carbon (Mesopore, 2-50 nm) and macroporous carbon material (Macropore, more than or equal to 50nm) according to pore size, wherein the microporous carbon can be further divided into first-grade microporous carbon (C: (C) (C))<0.8nm) and secondary microporous carbon (0.8 nm-2 nm). The mesoporous carbon is a novel non-silicon-based mesoporous material with the particle size of 2nm<Pore diameter<50nm, and has huge specific surface area (up to 2500 m)2Per gram) and pore volume (up to 2.25cm3And/g) are highly expected to be applied to catalyst carriers, hydrogen storage materials, electrode materials and the like, and therefore, the catalyst is highly regarded by people.
Based on the performance of mesoporous carbon, the inventor expects a functionalized mesoporous carbon material to be obtained through functionalization, and the functionalized mesoporous carbon material has good effect when being used in industrial water treatment.
Disclosure of Invention
The invention mainly aims to solve the problems in the prior art and provides a multifunctional industrial water treatment medicament and a preparation method thereof. The water treatment agent prepared by the preparation method can effectively remove pollutants in industrial sewage and has good effect.
The purpose of the invention and the technical problem to be solved are realized by adopting the following technical scheme.
The invention provides a preparation method of a multifunctional industrial water treatment medicament, which comprises the following steps:
dissolving sucrose in 70-90 wt% concentrated sulfuric acid solution, then placing the solution in an ice bath at the temperature of-5-0 ℃, stirring the solution for 30-60 min, filtering the solution after the reaction is finished, taking precipitate, and washing the precipitate for 2-3 times by using deionized water;
uniformly mixing the obtained precipitate with a dilute sulfuric acid solution with the mass fraction of 10-20 wt%, adding dimethyl titanate, stirring and reacting at 80-140 ℃ for 1-3 h, filtering, removing dimethyl titanate, drying the obtained precipitate, and calcining to obtain a mesoporous carbon material;
and dissolving the obtained mesoporous carbon material in a ferric trichloride solution, adding ammonium chloride, performing ultrasonic mixing for 30min, standing overnight, taking out the mesoporous carbon material, washing, and drying at the temperature of 50-80 ℃ under a vacuum condition to obtain the multifunctional industrial water treatment agent.
In the preparation method, the ratio of sucrose to concentrated sulfuric acid is 1 g: (1-2) mL.
In the preparation method, the ratio of sucrose to dilute sulfuric acid is 1 g: (2-3) mL.
In the preparation method, the mass ratio of the sucrose to the dimethyl titanate is 1: (0.05-0.1).
In the preparation method, the dibutyl phthalate is removed by soaking in water and/or methanol.
In the preparation method, the calcination is a procedure calcination, and the specific process is as follows: the temperature rise rate is 50 ℃/h in the range of 0-800 ℃, the temperature is kept for 2h at 800 ℃, the temperature rise rate is 80 ℃/h in the range of 800-1200 ℃, the temperature is kept for 5h at 1200 ℃, and the temperature is reduced to the room temperature according to the natural temperature reduction rate after the temperature is kept.
In the preparation method, the ratio of the mesoporous carbon material to the ferric chloride solution is 1 g: (3-5) mL.
In the preparation method, the concentration of the ferric trichloride solution is 10-20 wt%.
In the preparation method, the mass ratio of the mesoporous carbon material to the ammonium chloride is 1: (0.05-0.1).
By the technical scheme, the invention at least has the following advantages: the multifunctional industrial water treatment agent is a composite material of mesoporous carbon material loaded with iron ions, integrates the good adsorption performance of mesoporous carbon and the covalent bonding performance of iron ions, can remove various pollutants in sewage when being used for sewage treatment, and has an obvious effect. In the process of preparing the mesoporous carbon material, sucrose is used as a carbon source, the sucrose is rich in source and low in price, firstly, a carbonization effect is performed through a concentrated sulfuric acid solution, and then, pores are formed on a carbonized product in a dilute sulfuric acid solution environment through dimethyl titanate; the environment of the dilute sulfuric acid solution can promote the pore-forming effect of the dimethyl titanate, so that the carbonized product generates a large number of pore structures and a high specific surface area; the structural stability of the overall material can then be improved by means of calcination. The mesoporous carbon material obtained by the method has the advantages of high specific surface area, uniform aperture and high pore volume. And finally, soaking the mesoporous carbon material in an iron trichloride solution, and loading iron ions on the mesoporous carbon material under the catalysis of ammonium chloride and the ultrasonic action to obtain the treating agent for treating the industrial sewage. Test results show that the treatment agent can obviously improve the removal of pollutants in sewage, and the material has good stability and can be used for a long time. Compared with the prior art, the preparation method is simple, the raw materials are common compounds in the field, the sources are rich, and the whole preparation cost is low.
The foregoing is a summary of the present invention, and in order to provide a clear understanding of the technical means of the present invention and to be implemented in accordance with the present specification, the following is a detailed description of the preferred embodiments of the present invention.
Detailed Description
In order to make the technical means, the creation features, the achievement purposes and the effects of the invention easy to understand, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Dissolving 100g of sucrose in 150mL of concentrated sulfuric acid solution with the mass fraction of 80 wt%, then placing the solution in an ice bath at the temperature of minus 5-0 ℃ and stirring for 50min, filtering after the reaction is finished, taking a precipitate, and washing the precipitate for 2-3 times by using deionized water to obtain a carbonized product. Uniformly mixing the carbonized product with 250mL of dilute sulfuric acid solution with the mass fraction of 15 wt%, adding 8g of dimethyl titanate, stirring and reacting at 110 ℃ for 2h, then filtering, soaking in deionized water to remove the dimethyl titanate, drying the obtained precipitate, and then performing programmed calcination, wherein the specific process comprises the following steps: the temperature rise rate is 50 ℃/h in the range of 0-800 ℃, the temperature is kept for 2h at 800 ℃, the temperature rise rate is 80 ℃/h in the range of 800-1200 ℃, the temperature is kept for 5h at 1200 ℃, and the temperature is reduced to the room temperature according to the natural cooling rate after the temperature is kept, so that the mesoporous carbon material is obtained. The obtained mesoporous carbon material is subjected to pore structure analysis by adopting a gas adsorption (BET) method, and the detection shows that the specific surface area of the mesoporous carbon material is 2915m2(ii)/g, average pore diameter of 12.5nm and pore volume of 3.211 cc/g.
Dissolving 100g of the obtained mesoporous carbon material in 400mL of 15 wt% ferric trichloride solution, adding 7g of ammonium chloride, carrying out ultrasonic mixing for 30min, standing overnight, taking out the mesoporous carbon material, washing, and finally drying at 65 ℃ under a vacuum condition to obtain the multifunctional industrial water treatment agent.
Example 2
Dissolving 100g of sucrose in 100mL of 90 wt% concentrated sulfuric acid solution, then placing the solution in an ice bath at the temperature of minus 5-0 ℃ to stir for 60min, filtering after the reaction is finished, taking a precipitate, and washing the precipitate for 2-3 times by using deionized water to obtain a carbonized product. Mixing the carbonized product with 300mL of dilute solution with the mass fraction of 10 wt%After sulfuric acid solution is uniformly mixed, 5g of dimethyl titanate is added, stirring reaction is carried out for 2 hours at the temperature of 80 ℃, then filtration is carried out, deionized water is used for soaking to remove the dimethyl titanate, the obtained precipitate is dried, and then program calcination is carried out, wherein the specific process comprises the following steps: the temperature rise rate is 50 ℃/h in the range of 0-800 ℃, the temperature is kept for 2h at 800 ℃, the temperature rise rate is 80 ℃/h in the range of 800-1200 ℃, the temperature is kept for 5h at 1200 ℃, and the temperature is reduced to the room temperature according to the natural cooling rate after the temperature is kept, so that the mesoporous carbon material is obtained. The obtained mesoporous carbon material is subjected to pore structure analysis by adopting a gas adsorption (BET) method, and the detection shows that the specific surface area of the mesoporous carbon material is 2418m2(ii)/g, average pore diameter of 12.1nm and pore volume of 3.031 cc/g.
And dissolving 100g of the obtained mesoporous carbon material in 300mL of 10 wt% ferric trichloride solution, adding 5g of ammonium chloride, carrying out ultrasonic mixing for 30min, standing overnight, taking out the mesoporous carbon material, washing, and finally drying at 70 ℃ under a vacuum condition to obtain the multifunctional industrial water treatment agent.
Example 3
Dissolving 100g of sucrose in 200mL of concentrated sulfuric acid solution with the mass fraction of 70 wt%, then placing the solution in an ice bath at the temperature of minus 5-0 ℃ to stir for 30min, filtering after the reaction is finished, taking a precipitate, and washing the precipitate for 2-3 times by using deionized water to obtain a carbonized product. Uniformly mixing the carbonized product with 200mL of dilute sulfuric acid solution with the mass fraction of 15 wt%, adding 10g of dimethyl titanate, stirring and reacting at 90 ℃ for 1h, then filtering, soaking in deionized water to remove the dimethyl titanate, drying the obtained precipitate, and then performing programmed calcination, wherein the specific process comprises the following steps: the temperature rise rate is 50 ℃/h in the range of 0-800 ℃, the temperature is kept for 2h at 800 ℃, the temperature rise rate is 80 ℃/h in the range of 800-1200 ℃, the temperature is kept for 5h at 1200 ℃, and the temperature is reduced to the room temperature according to the natural cooling rate after the temperature is kept, so that the mesoporous carbon material is obtained. The obtained mesoporous carbon material is subjected to pore structure analysis by adopting a gas adsorption (BET) method, and the detection shows that the specific surface area of the mesoporous carbon material is 2507m2(ii)/g, average pore diameter of 6.6nm and pore volume of 2.910 cc/g.
And dissolving 100g of the obtained mesoporous carbon material in 500mL of 10 wt% ferric trichloride solution, adding 10g of ammonium chloride, carrying out ultrasonic mixing for 30min, standing overnight, taking out the mesoporous carbon material, washing, and finally drying at the temperature of 50 ℃ under a vacuum condition to obtain the multifunctional industrial water treatment agent.
Example 4
Dissolving 100g of sucrose in 200mL of concentrated sulfuric acid solution with the mass fraction of 80 wt%, then placing the solution in an ice bath at the temperature of minus 5-0 ℃ and stirring for 40min, filtering after the reaction is finished, taking a precipitate, and washing the precipitate for 2-3 times by using deionized water to obtain a carbonized product. Uniformly mixing the carbonized product with 200mL of dilute sulfuric acid solution with the mass fraction of 15 wt%, adding 5g of dimethyl titanate, stirring and reacting at 100 ℃ for 1h, then filtering, soaking in deionized water to remove the dimethyl titanate, drying the obtained precipitate, and then performing programmed calcination, wherein the specific process comprises the following steps: the temperature rise rate is 50 ℃/h in the range of 0-800 ℃, the temperature is kept for 2h at 800 ℃, the temperature rise rate is 80 ℃/h in the range of 800-1200 ℃, the temperature is kept for 5h at 1200 ℃, and the temperature is reduced to the room temperature according to the natural cooling rate after the temperature is kept, so that the mesoporous carbon material is obtained. The obtained mesoporous carbon material is subjected to pore structure analysis by a gas adsorption (BET) method, and the detection shows that the specific surface area of the mesoporous carbon material is 2124m2(ii)/g, average pore diameter was 9.3nm, and pore volume was 3.005 cc/g.
Dissolving 100g of the obtained mesoporous carbon material in 300mL of 10 wt% ferric trichloride solution, adding 10g of ammonium chloride, carrying out ultrasonic mixing for 30min, standing overnight, taking out the mesoporous carbon material, washing, and finally drying at the temperature of 50 ℃ under a vacuum condition to obtain the multifunctional industrial water treatment agent.
Example 5
Dissolving 100g of sucrose in 200mL of 90 wt% concentrated sulfuric acid solution, then placing the solution in an ice bath at the temperature of minus 5-0 ℃ to stir for 30min, filtering after the reaction is finished, taking a precipitate, and washing the precipitate for 2-3 times by using deionized water to obtain a carbonized product. Uniformly mixing the carbonized product with 300mL of dilute sulfuric acid solution with the mass fraction of 10 wt%, adding 5g of dimethyl titanate, stirring and reacting at 120 ℃ for 3 hours, filtering, and adding deionized waterSoaking to remove dimethyl titanate, drying the obtained precipitate, and performing programmed calcination, wherein the specific process comprises the following steps: the temperature rise rate is 50 ℃/h in the range of 0-800 ℃, the temperature is kept for 2h at 800 ℃, the temperature rise rate is 80 ℃/h in the range of 800-1200 ℃, the temperature is kept for 5h at 1200 ℃, and the temperature is reduced to the room temperature according to the natural cooling rate after the temperature is kept, so that the mesoporous carbon material is obtained. The obtained mesoporous carbon material is subjected to pore structure analysis by adopting a gas adsorption (BET) method, and the detection shows that the specific surface area of the mesoporous carbon material is 2158m2(ii)/g, average pore diameter of 10.2nm and pore volume of 2.514 cc/g.
And dissolving 100g of the obtained mesoporous carbon material in 300mL of 20 wt% ferric trichloride solution, adding 8g of ammonium chloride, carrying out ultrasonic mixing for 30min, standing overnight, taking out the mesoporous carbon material, washing, and finally drying at the temperature of 50 ℃ under a vacuum condition to obtain the multifunctional industrial water treatment agent.
Example 6
Dissolving 100g of sucrose in 100mL of 90 wt% concentrated sulfuric acid solution, then placing the solution in an ice bath at the temperature of minus 5-0 ℃ to stir for 40min, filtering after the reaction is finished, taking a precipitate, and washing the precipitate for 2-3 times by using deionized water to obtain a carbonized product. Uniformly mixing the carbonized product with 300mL of dilute sulfuric acid solution with the mass fraction of 20 wt%, adding 8g of dimethyl titanate, stirring and reacting at 130 ℃ for 2 hours, then filtering, soaking in deionized water to remove the dimethyl titanate, drying the obtained precipitate, and then performing programmed calcination, wherein the specific process is as follows: the temperature rise rate is 50 ℃/h in the range of 0-800 ℃, the temperature is kept for 2h at 800 ℃, the temperature rise rate is 80 ℃/h in the range of 800-1200 ℃, the temperature is kept for 5h at 1200 ℃, and the temperature is reduced to the room temperature according to the natural cooling rate after the temperature is kept, so that the mesoporous carbon material is obtained. The obtained mesoporous carbon material is subjected to pore structure analysis by adopting a gas adsorption (BET) method, and the detection shows that the specific surface area of the mesoporous carbon material is 2268m2(ii)/g, average pore diameter 9.1nm, and pore volume 2.116 cc/g.
Dissolving 100g of the obtained mesoporous carbon material in 300mL of 15 wt% ferric trichloride solution, adding 8g of ammonium chloride, carrying out ultrasonic mixing for 30min, standing overnight, taking out the mesoporous carbon material, washing, and finally drying at 80 ℃ under a vacuum condition to obtain the multifunctional industrial water treatment agent.
Example 7
Dissolving 100g of sucrose in 200mL of 90 wt% concentrated sulfuric acid solution, then placing the solution in an ice bath at the temperature of minus 5-0 ℃ to stir for 40min, filtering after the reaction is finished, taking a precipitate, and washing the precipitate for 2-3 times by using deionized water to obtain a carbonized product. Uniformly mixing the carbonized product with 200mL of dilute sulfuric acid solution with the mass fraction of 20 wt%, adding 9g of dimethyl titanate, stirring and reacting for 1h at 140 ℃, then filtering, soaking with methanol to remove the dimethyl titanate, drying the obtained precipitate, and then performing programmed calcination, wherein the specific process is as follows: the temperature rise rate is 50 ℃/h in the range of 0-800 ℃, the temperature is kept for 2h at 800 ℃, the temperature rise rate is 80 ℃/h in the range of 800-1200 ℃, the temperature is kept for 5h at 1200 ℃, and the temperature is reduced to the room temperature according to the natural cooling rate after the temperature is kept, so that the mesoporous carbon material is obtained. The obtained mesoporous carbon material is subjected to pore structure analysis by adopting a gas adsorption (BET) method, and the detection shows that the specific surface area of the mesoporous carbon material is 2024m2(ii)/g, average pore diameter of 6.9nm and pore volume of 2.513 cc/g.
Dissolving 100g of the obtained mesoporous carbon material in 400mL of 20 wt% ferric trichloride solution, adding 5g of ammonium chloride, carrying out ultrasonic mixing for 30min, standing overnight, taking out the mesoporous carbon material, washing, and finally drying at 80 ℃ under a vacuum condition to obtain the multifunctional industrial water treatment agent.
Example 8
Dissolving 100g of sucrose in 200mL of concentrated sulfuric acid solution with the mass fraction of 80 wt%, then placing the solution in an ice bath at the temperature of minus 5-0 ℃ and stirring for 40min, filtering after the reaction is finished, taking a precipitate, and washing the precipitate for 2-3 times by using deionized water to obtain a carbonized product. Uniformly mixing the carbonized product with 200mL of dilute sulfuric acid solution with the mass fraction of 20 wt%, adding 5g of dimethyl titanate, stirring and reacting at 100 ℃ for 1.5h, then filtering, soaking with methanol to remove the dimethyl titanate, drying the obtained precipitate, and then carrying out programmed calcination, wherein the specific process comprises the following steps: in the 0-800 deg.C regionThe temperature rise rate is 50 ℃/h, the temperature is kept for 2h at 800 ℃, the temperature rise rate is 80 ℃/h between 800 ℃ and 1200 ℃, the temperature is kept for 5h at 1200 ℃, and the temperature is reduced to room temperature according to the natural temperature reduction rate after the temperature is kept, so that the mesoporous carbon material is obtained. The obtained mesoporous carbon material is subjected to pore structure analysis by adopting a gas adsorption (BET) method, and the detection shows that the specific surface area of the mesoporous carbon material is 2301m2(ii)/g, average pore diameter of 11.7nm and pore volume of 2.138 cc/g.
And dissolving 100g of the obtained mesoporous carbon material in 300mL of 15 wt% ferric trichloride solution, adding 9g of ammonium chloride, carrying out ultrasonic mixing for 30min, standing overnight, taking out the mesoporous carbon material, washing, and finally drying at 80 ℃ under a vacuum condition to obtain the multifunctional industrial water treatment agent.
Comparative example 1
Dissolving 100g of sucrose in 150mL of concentrated sulfuric acid solution with the mass fraction of 80 wt%, then placing the solution in an ice bath at the temperature of minus 5-0 ℃ and stirring for 50min, filtering after the reaction is finished, taking a precipitate, and washing the precipitate for 2-3 times by using deionized water to obtain a carbonized product. Uniformly mixing the carbonized product with 250mL of deionized water, adding 8g of dimethyl titanate, stirring and reacting at 110 ℃ for 2h, filtering, drying the obtained precipitate, and performing programmed calcination, wherein the specific process comprises the following steps: the temperature rise rate is 50 ℃/h in the range of 0-800 ℃, the temperature is kept for 2h at 800 ℃, the temperature rise rate is 80 ℃/h in the range of 800-1200 ℃, the temperature is kept for 5h at 1200 ℃, and the temperature is reduced to the room temperature according to the natural cooling rate after the temperature is kept, so that the mesoporous carbon material is obtained. The obtained mesoporous carbon material is subjected to pore structure analysis by adopting a gas adsorption (BET) method, and the detection shows that the specific surface area of the mesoporous carbon material is 1015m2(ii)/g, average pore diameter was 2.5nm, and pore volume was 0.794 cc/g.
Dissolving 100g of the obtained mesoporous carbon material in 400mL of 15 wt% ferric trichloride solution, adding 7g of ammonium chloride, carrying out ultrasonic mixing for 30min, standing overnight, taking out the mesoporous carbon material, washing, and finally drying at 65 ℃ under a vacuum condition to obtain the industrial water treatment agent.
Test examples comprehensive treatment Performance of Water treatment agentEvaluation of
Subject: the water quality condition measured before the treatment of the wastewater produced by a certain pharmaceutical growth is as follows: chemical Oxygen Demand (COD) of 320mg/L and Biochemical Oxygen Demand (BOD)5) 210mg/L, 156mg/L suspended matter (SS), 48mg/L Total Phosphorus (TP), cyanide ion (CN)-) Fluoride ion (F) at a concentration of 135mg/L-) The concentration was 62 mg/L.
Test agents: examples 1 to 8 and comparative example 1.
The experimental method comprises the following steps: the water treatment agent was added in an amount of 20mg/L, and after stirring for 5min, the concentration of each contamination index of the supernatant was measured, and the results are shown in Table 1.
TABLE 1 summary of the respective contamination index concentrations (in mg/L units)
As is clear from the results shown in Table 1, the industrial water treatment agent of the present invention has a remarkable effect of removing pollutants from sewage. Compared with the comparative example 1, the embodiments 1 to 8 of the invention are different only in that the obtained mesoporous carbon material is obviously superior to the mesoporous carbon material obtained by the conventional pore-forming method by pore-forming the carbonized product in the environment of the dilute sulfuric acid solution, has higher specific surface area and pore volume, is used for preparing the water treatment agent, and obviously improves the pollutant removal performance.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (9)
1. A preparation method of a multifunctional industrial water treatment medicament comprises the following steps:
dissolving sucrose in 70-90 wt% concentrated sulfuric acid solution, then placing the solution in an ice bath at the temperature of-5-0 ℃, stirring the solution for 30-60 min, filtering the solution after the reaction is finished, taking precipitate, and washing the precipitate for 2-3 times by using deionized water;
uniformly mixing the obtained precipitate with a dilute sulfuric acid solution with the mass fraction of 10-20 wt%, adding dimethyl titanate, stirring and reacting at 80-140 ℃ for 1-3 h, filtering, removing dimethyl titanate, drying the obtained precipitate, and calcining to obtain a mesoporous carbon material;
and dissolving the obtained mesoporous carbon material in a ferric trichloride solution, adding ammonium chloride, performing ultrasonic mixing for 30min, standing overnight, taking out the mesoporous carbon material, washing, and drying at the temperature of 50-80 ℃ under a vacuum condition to obtain the multifunctional industrial water treatment agent.
2. The method of claim 1, wherein the ratio of sucrose to concentrated sulfuric acid is 1 g: (1-2) mL.
3. The method of claim 1, wherein the ratio of sucrose to dilute sulfuric acid is 1 g: (2-3) mL.
4. The preparation method according to claim 1, wherein the mass ratio of sucrose to dimethyl titanate is 1: (0.05-0.1).
5. The method of claim 1, wherein the dibutyl phthalate is removed by soaking with water and/or methanol.
6. The preparation method of claim 1, wherein the calcination is a procedure calcination, and the specific process is as follows: the temperature rise rate is 50 ℃/h in the range of 0-800 ℃, the temperature is kept for 2h at 800 ℃, the temperature rise rate is 80 ℃/h in the range of 800-1200 ℃, the temperature is kept for 5h at 1200 ℃, and the temperature is reduced to the room temperature according to the natural temperature reduction rate after the temperature is kept.
7. The production method according to claim 1, wherein the ratio of the mesoporous carbon material to the ferric trichloride solution is 1 g: (3-5) mL.
8. The method according to claim 1, wherein the concentration of the ferric trichloride solution is 10 to 20 wt%.
9. The production method according to claim 1, wherein the mass ratio of the mesoporous carbon material to ammonium chloride is 1: (0.05-0.1).
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| Publication number | Priority date | Publication date | Assignee | Title |
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101033082A (en) * | 2007-04-18 | 2007-09-12 | 大连理工大学 | Method of preparing titanium dioxide, stannum dioxide and doping composite fiber material thereof |
| CN101780952A (en) * | 2010-03-26 | 2010-07-21 | 上海交通大学 | Method for preparing loading functional oxide porous carbon |
| US20100291167A1 (en) * | 2008-09-29 | 2010-11-18 | Sony Corporation | Porous carbon material composites and their production process, adsorbents, cosmetics, purification agents, and composite photocatalyst materials |
| CN102145295A (en) * | 2011-01-27 | 2011-08-10 | 攀枝花学院 | Method for preparing doped porous titanium dioxide |
| CN103303912A (en) * | 2013-07-05 | 2013-09-18 | 黑龙江大学 | Preparation method of high-specific-surface-area porous nitrogen-doped graphitizing carbon nanomaterial |
| CN105692582A (en) * | 2016-01-08 | 2016-06-22 | 中国环境科学研究院 | Method for synthesizing mesoporous carbon material through saccharides without assistance of surfactant |
| CN107552050A (en) * | 2016-07-01 | 2018-01-09 | 中国石油天然气股份有限公司 | A kind of ferriferous oxide catalyst of monoblock type mesoporous carbon-loaded and preparation method thereof |
| CN108079737A (en) * | 2017-12-18 | 2018-05-29 | 宁波市河清源技术转移服务有限公司 | A kind of preparation method of multi-stage porous formaldehyde adsorbent |
| CN110227459A (en) * | 2019-05-15 | 2019-09-13 | 东北电力大学 | A kind of preparation method of tripolite loading solid super strong acids fenton catalyst |
-
2021
- 2021-01-15 CN CN202110052292.3A patent/CN112892474B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101033082A (en) * | 2007-04-18 | 2007-09-12 | 大连理工大学 | Method of preparing titanium dioxide, stannum dioxide and doping composite fiber material thereof |
| US20100291167A1 (en) * | 2008-09-29 | 2010-11-18 | Sony Corporation | Porous carbon material composites and their production process, adsorbents, cosmetics, purification agents, and composite photocatalyst materials |
| CN101780952A (en) * | 2010-03-26 | 2010-07-21 | 上海交通大学 | Method for preparing loading functional oxide porous carbon |
| CN102145295A (en) * | 2011-01-27 | 2011-08-10 | 攀枝花学院 | Method for preparing doped porous titanium dioxide |
| CN103303912A (en) * | 2013-07-05 | 2013-09-18 | 黑龙江大学 | Preparation method of high-specific-surface-area porous nitrogen-doped graphitizing carbon nanomaterial |
| CN105692582A (en) * | 2016-01-08 | 2016-06-22 | 中国环境科学研究院 | Method for synthesizing mesoporous carbon material through saccharides without assistance of surfactant |
| CN107552050A (en) * | 2016-07-01 | 2018-01-09 | 中国石油天然气股份有限公司 | A kind of ferriferous oxide catalyst of monoblock type mesoporous carbon-loaded and preparation method thereof |
| CN108079737A (en) * | 2017-12-18 | 2018-05-29 | 宁波市河清源技术转移服务有限公司 | A kind of preparation method of multi-stage porous formaldehyde adsorbent |
| CN110227459A (en) * | 2019-05-15 | 2019-09-13 | 东北电力大学 | A kind of preparation method of tripolite loading solid super strong acids fenton catalyst |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117224450A (en) * | 2023-11-10 | 2023-12-15 | 广州市玑蜜生物科技有限公司 | Fennel face essence with good moisture retention and preparation method thereof |
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