CN111018038A - Heavy metal trapping agent and preparation process thereof - Google Patents
Heavy metal trapping agent and preparation process thereof Download PDFInfo
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- CN111018038A CN111018038A CN201911370506.0A CN201911370506A CN111018038A CN 111018038 A CN111018038 A CN 111018038A CN 201911370506 A CN201911370506 A CN 201911370506A CN 111018038 A CN111018038 A CN 111018038A
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- heavy metal
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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
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
Abstract
The invention discloses a heavy metal capture agent and a preparation process thereof, which relate to the technical field of wastewater treatment and are prepared from the following raw materials in parts by weight: 40-60 parts of sodium sulfide, 30-50 parts of trisodium phosphate, 0.5-1 part of cerium and 160-220 parts of water. The preparation method has the advantage of improving the capture efficiency of the heavy metal ions.
Description
Technical Field
The invention relates to the technical field of sewage treatment, in particular to a heavy metal trapping agent and a preparation process thereof.
Background
With the development of the industrialization process in recent decades, the discharge amount of the waste water is increased, thereby causing serious damage to the environment. Various harmful substances in the wastewater are enriched into a biological chain through a water body and finally enter a human body, so that serious toxic and harmful effects are brought to human beings. The heavy metal ions contained in the wastewater are one of the most serious harmful substances which pollute the environment and have the greatest harm to human health, so that how to treat the heavy metal wastewater is generally regarded by all circles.
At present, effective separation processes for removing heavy metal ions in sewage comprise precipitation, ion exchange, electrochemical treatment, membrane technology, evaporation and solidification, reverse osmosis, electrodialysis and the like, but the application of the technologies is sometimes limited by the process and economy, so that the search for a cheaper sewage purification material reduces the cost of sewage treatment, and improves the purification efficiency becomes a problem to be solved urgently in environmental protection.
In recent years, heavy metal scavengers have been the focus of research, and the existing heavy metal scavengers generally use sodium sulfide or chelating agent as a chemical to treat the sewage so as to remove the heavy metal ions in the sewage under the action of the sodium sulfide or chelating agent. However, in the conventional metal scavenger, the respective effective components are easily affected by each other, and the heavy metal ion trapping efficiency is lowered.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a heavy metal trapping agent and a preparation process thereof.
The above object of the present invention is achieved by the following technical solutions:
the heavy metal trapping agent is prepared from the following raw materials in parts by weight:
by adopting the technical scheme, sulfur ions in sodium sulfide in the heavy metal capturing agent can be combined with heavy metal ions to generate insoluble precipitates, trisodium phosphate can be chelated with the heavy metal ions to generate chelated products, and the removal effect of the heavy metal ions is obviously improved under the combined action of the sodium sulfide and the heavy metal ions. In addition, the rare earth metal cerium is added, and has a catalytic enhancement effect on the removal reaction of sodium sulfide and trisodium phosphate and heavy metal ions.
The invention is further configured to: the heavy metal catching agent is also added with 10-30 parts by weight of natural cellulose powder and 8-15 parts by weight of slow release material;
the natural cellulose powder is prepared from the following raw materials in percentage by weight:
the invention is further configured to: the preparation process of the natural cellulose powder comprises the following steps:
step 1: washing bagasse with clear water for 2-3 times, then washing with distilled water for 2-3 times, and drying for later use;
step 2: grinding the bagasse dried in the step 1 by using a grinder, and then sieving the bagasse by using a 100-mesh sieve for later use;
and step 3: soaking the screened bagasse powder in an isopropanol solution with the mass fraction concentration of 20% for 24-36 h, then sequentially washing the soaked bagasse powder with the isopropanol solution with the mass fraction concentration of 20% and deionized water for 3-5 times, and then carrying out suction filtration and drying;
and 4, step 4: and (3) soaking the bagasse powder treated in the step (3) in 0.1mol/L sodium hydroxide solution, stirring for 1-2 h, performing suction filtration, washing with distilled water until the pH value of a washing liquid is 7-8, performing suction filtration again, and drying to obtain natural cellulose powder.
The invention is further configured to: the sustained-release material is prepared from the following raw materials in parts by weight:
by adopting the technical scheme, magnesium chloride hexahydrate, aluminum chloride hexahydrate, potassium acetate, sodium hydroxide and water can be used for preparing the magnesium-aluminum hydrotalcite material with acetate ion intercalation, and the hydrotalcite has a layered double hydroxide with a micropore structure and a memory effect. The heavy metal scavenger has a large specific surface area, so that the heavy metal scavenger adsorbs main components, and due to the memory effect, the layered structure can be recovered by roasting after the heavy metal scavenger is used and recovered, so that the heavy metal scavenger can be recycled. Meanwhile, the polarity of the hydrotalcite is enhanced through intercalation of acetate ions, and when the hydrotalcite is used as the main component of the heavy metal trapping agent, the main component of the heavy metal trapping agent is a polar substance, so that the main component of the heavy metal trapping agent can be better adsorbed by the hydrotalcite, and the adsorption efficiency and the adsorption capacity of the hydrotalcite are improved. The polyhydroxy alkyl acid ester compounds hydrotalcite which adsorbs main components in the heavy metal capture agent to obtain a gel compound, and the gel compound can improve the stability of slow release.
The invention is further configured to: the preparation process of the sustained-release material specifically comprises the following steps:
step a: mixing and dissolving magnesium chloride hexahydrate, aluminum chloride hexahydrate, potassium acetate and water according to the weight ratio of 1: 5 respectively; (ii) a
Step b: mixing sodium hydroxide and water according to a proportion to obtain a sodium hydroxide solution;
step c: b, adding the magnesium chloride solution and the potassium acetate solution obtained in the step a into a sodium hydroxide solution, adjusting the pH to 9-10, and then adding the magnesium chloride solution to obtain a solid-liquid mixture;
step d: and aging the solid-liquid mixture at 65-70 ℃ for 20-24 h, then carrying out suction filtration and washing, and finally drying to obtain the intercalated hydrotalcite.
The invention is further configured to: and c, adding the magnesium chloride solution and the potassium acetate solution into the sodium hydroxide solution and adding paramagnetic ferrite powder at the same time, wherein the mass ratio of the paramagnetic ferrite powder to the magnesium chloride is 1: 1-2, and after the magnesium chloride solution is added, carrying out ultrasonic-assisted reaction.
By adopting the technical scheme, the prepared slow release material has magnetism after the paramagnetic ferrite powder is added, so that the slow release material adsorbing the main components of the heavy metal capture agent can be conveniently recycled after being added into wastewater for treatment, and can be rapidly collected under the action of an external magnetic field, thereby avoiding secondary pollution of the slow release material to the wastewater, simultaneously improving the recycling efficiency of resources and realizing sustainable operation of the process.
A method for preparing the heavy metal capture agent:
s1: stirring and uniformly stirring sodium sulfide, trisodium phosphate, cerium, natural cellulose powder and water according to a proportion to obtain a mixed solution for later use;
s2: adding the slow-release material into the mixed solution, and soaking for 8-12 h;
s3: taking out the sustained-release material soaked in the step S2, drying, crushing, and sieving with a 10-100-mesh sieve to obtain sustained-release granules;
the heavy metal trapping agent can be obtained through the 3 steps.
The invention is further configured to: before the slow release material is added into the mixed solution, the slow release material is sprayed with ethanol steam for 3-6 min, and then the slow release material is added into the mixed solution.
By adopting the technical scheme, when the slow release material is added into the mixed solution, the mixed solution can easily form a layer of liquid film on the surface of the slow release material, and the liquid film can seal micropores in the slow release material, so that air in part of the micropore structure of the slow release material is sealed to prevent the slow release material from further absorbing main components in the heavy metal capture agent. And after the slow release material is sprayed with ethanol steam, more ethanol steam can be filled in the microporous structure of the slow release material, and when the slow release material is added into the mixed solution, the ethanol steam in the microporous structure of the slow release material is cooled and shrunk due to the cooling of the mixed solution, so that certain negative pressure is generated, and the main components and the solvent in the heavy metal capture agent in the mixed solution can partially enter the micropores of the slow release material. And after the mixed liquid part got into the micropore, ethanol steam among the microporous construction can be dissolved in mixed liquid to make the negative pressure in the micropore produce all the time, until permeating mixed liquid in the micropore completely, mixed liquid is at the in-process of infiltration, and the principal ingredients in the heavy metal trapping agent in the mixed liquid adsorbs the surface of micropore, thereby makes the adsorption effect of slow release material to the principal ingredients in the heavy metal trapping agent obtain promoting.
The invention is further configured to: step S4 follows step S3: post-processing, the step S4 operates as follows: carrying out post-treatment on the sustained-release particles obtained in the step S3 by using post-treatment liquid, drying and crushing the sustained-release particles after the post-treatment is finished, and sieving the particles by using a sieve with 10-50 meshes to obtain a heavy metal trapping agent;
the post-treatment liquid comprises the following components in parts by weight:
1-3 parts of nano calcium oxide;
80-100 parts of carboxymethyl cellulose;
200-300 parts of cyclohexane.
By adopting the technical scheme, a carboxymethyl cellulose coating is attached to the surface of the sustained-release particles after the post-treatment process, and nano calcium oxide is dispersed in the carboxymethyl cellulose coating. When the microbial carbon source obtained after the post-treatment is added into the wastewater, the carboxymethyl cellulose coating on the surface of the slow-release particles begins to dissolve when meeting water, a small amount of heat is released after the nano calcium oxide in the carboxymethyl cellulose coating is contacted with the water in a dispersing manner in the dissolving process, the temperature of the slow-release particles is increased, so that the main components in the heavy metal capturing agent in the slow-release particles are activated, the main components in the heavy metal capturing agent are more easily released from the slow-release material, the reaction of the slow-release particles is more sensitive, and the heavy metal capturing agent is more timely released.
Compared with the prior art, the invention has the beneficial effects that:
1. the heavy metal trapping agent containing the sodium sulfide and trisodium phosphate complexing agent is obtained by compounding, so that the trapping efficiency of the heavy metal trapping agent on heavy metal ions is improved;
2. the limited components in the heavy metal ion capturing agent are adsorbed by adding the slow release material, so that when the heavy metal ion capturing agent is added into sewage, the heavy metal ion capturing agent can be adjusted according to the pollution degree of the heavy metal ions in the wastewater, the method is more convenient, and the efficiency is improved.
Detailed Description
The present invention will be described in detail with reference to examples.
The invention discloses a heavy metal trapping agent which is prepared from the following raw materials in parts by weight:
the natural cellulose powder is prepared from the following raw materials in percentage by weight:
the preparation process of the natural cellulose powder comprises the following steps:
step 1: washing bagasse with clear water for 3 times, washing with distilled water for 3 times, and oven drying;
step 2: grinding the bagasse dried in the step 1 by using a grinder, and then sieving the bagasse by using a 100-mesh sieve for later use;
and step 3: soaking the screened bagasse powder in an isopropanol solution with the mass fraction concentration of 20% for 24 hours, then sequentially washing the soaked bagasse powder with the isopropanol solution with the mass fraction concentration of 20% and deionized water for 3 times, and then carrying out suction filtration and drying;
and 4, step 4: and (3) soaking the bagasse powder treated in the step (3) in 0.1mol/L sodium hydroxide solution, stirring for 1h, performing suction filtration, washing with distilled water until the pH value of a washing liquid is 7, performing suction filtration again, and drying to obtain natural cellulose powder.
The sustained-release material is prepared from the following raw materials in parts by weight:
the preparation process of the sustained-release material specifically comprises the following steps:
step a: mixing and dissolving magnesium chloride hexahydrate, aluminum chloride hexahydrate, potassium acetate and water according to the weight ratio of 1: 5 respectively; (ii) a
Step b: mixing sodium hydroxide and water according to a proportion to obtain a sodium hydroxide solution;
step c: b, adding the magnesium chloride solution and the potassium acetate solution obtained in the step a into a sodium hydroxide solution, adding paramagnetic ferrite powder, wherein the mass ratio of the paramagnetic ferrite powder to the magnesium chloride is 1: 2, then adjusting the pH value to 9, then adding the magnesium chloride solution, and carrying out ultrasonic-assisted reaction to obtain a solid-liquid mixture;
step d: and aging the solid-liquid mixture at 70 ℃ for 24h, then carrying out suction filtration and washing, and finally drying to obtain the intercalated hydrotalcite.
A method for a heavy metal scavenger:
s1: stirring and uniformly stirring sodium sulfide, trisodium phosphate, cerium, natural cellulose powder and water according to a proportion to obtain a mixed solution for later use;
s2: spraying ethanol steam on the sustained-release material for 3min, adding the sustained-release material into the mixed solution, and soaking for 8 h;
s3: taking out the sustained-release material soaked in the step S2, drying, crushing, and sieving with a 100-mesh sieve to obtain sustained-release granules;
s4: carrying out post-treatment on the sustained-release particles obtained in the step S3 by using post-treatment liquid, drying and crushing the sustained-release particles after the post-treatment is finished, and sieving the particles by using a 50-mesh sieve to obtain a heavy metal trapping agent; the post-treatment liquid comprises the following components in parts by weight:
1 part of nano calcium oxide;
80 parts of carboxymethyl cellulose;
and 200 parts of cyclohexane.
The heavy metal trapping agent can be obtained through the 4 steps.
The difference between the examples 2-5 and the example 1 is that the raw materials for preparing the heavy metal capture agent are listed in the following table in parts by weight.
Examples 6 to 9 are different from example 1 in that the raw materials for preparing the natural cellulose powder are listed in the following table in parts by weight.
Examples 10 to 13 are different from example 1 in that the following components are listed in the following table in parts by weight in the post-treatment liquid.
Examples 14 to 17 are different from example 1 in that the following table shows the components in the post-treatment liquid in parts by weight.
Examples 18 to 21 are different from example 1 in that the treatment time of the sustained-release material with ethanol vapor sprayed thereon is shown in the following table.
| Examples | Example 18 | Example 19 | Example 20 | Example 21 |
| Time (min) | 3.75 | 4.5 | 5.25 | 6 |
Comparative example
The difference between the comparative example 1 and the example 1 is that the raw material for preparing the heavy metal trapping agent only contains sodium sulfide;
comparative example 2 differs from example 1 in that the raw material for the preparation of the heavy metal scavenger contains only trisodium phosphate;
comparative example 3 differs from example 1 in that the raw material for the preparation of the heavy metal scavenger contains only sodium sulfide and trisodium phosphate.
Detection method
5 parts of Cr with the concentration of 1mol/L are prepared3+1L of the solution was added with 1g of the heavy metal scavenger used in example 1 and comparative examples 1 to 4, and after 1 hour of treatment, the treated Cr was taken out3+The solution was tested for remaining Cr by atomic absorption spectroscopy3+The results are given in the table below.
| Examples | Treated Cr3+Concentration (mol/L) |
| Example 1 | 0.12 |
| Comparative example 1 | 0.43 |
| Comparative example 2 | 0.56 |
| Comparative example 3 | 0.77 |
And (4) conclusion: as can be seen from the test results in the table above, the heavy metal scavenger of example 1 is a couple of Cr3+The highest trapping efficiency, while in comparative example 3 trisodium phosphate and sodium sulphide are also added, for Cr3+The capture efficiency of (a) is lower than that of example 1, indicating that the addition of cerium serves to promote the synergistic treatment of trisodium phosphate and sodium sulfide. As can be seen from comparative examples 1 and 2, the heavy metal ion scavenger of the present application has a superior trapping effect to that of a common single-component heavy metal ion scavenger.
The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above embodiments, and all technical solutions belonging to the idea of the present invention belong to the protection scope of the present invention. It should be noted that modifications and embellishments within the scope of the invention may occur to those skilled in the art without departing from the principle of the invention, and are considered to be within the scope of the invention.
Claims (9)
1. The heavy metal trapping agent is characterized by being prepared from the following raw materials in parts by weight:
2. the heavy metal scavenger according to claim 1, wherein: the heavy metal catching agent is also added with 10-30 parts by weight of natural cellulose powder and 8-15 parts by weight of slow release material;
the natural cellulose powder is prepared from the following raw materials in percentage by weight:
3. the heavy metal scavenger according to claim 1, wherein: the preparation process of the natural cellulose powder comprises the following steps:
step 1: washing bagasse with clear water for 2-3 times, then washing with distilled water for 2-3 times, and drying for later use;
step 2: grinding the bagasse dried in the step 1 by using a grinder, and then sieving the bagasse by using a 100-mesh sieve for later use;
and step 3: soaking the screened bagasse powder in an isopropanol solution with the mass fraction concentration of 20% for 24-36 h, then sequentially washing the soaked bagasse powder with the isopropanol solution with the mass fraction concentration of 20% and deionized water for 3-5 times, and then carrying out suction filtration and drying;
and 4, step 4: and (3) soaking the bagasse powder treated in the step (3) in 0.1mol/L sodium hydroxide solution, stirring for 1-2 h, performing suction filtration, washing with distilled water until the pH value of a washing liquid is 7-8, performing suction filtration again, and drying to obtain natural cellulose powder.
4. The heavy metal scavenger according to claim 1, wherein: the sustained-release material is prepared from the following raw materials in parts by weight:
5. the heavy metal scavenger according to claim 4, wherein: the preparation process of the sustained-release material specifically comprises the following steps:
step a: mixing and dissolving magnesium chloride hexahydrate, aluminum chloride hexahydrate, potassium acetate and water according to the weight ratio of 1: 5 respectively; (ii) a
Step b: mixing sodium hydroxide and water according to a proportion to obtain a sodium hydroxide solution;
step c: b, adding the magnesium chloride solution and the potassium acetate solution obtained in the step a into a sodium hydroxide solution, adjusting the pH to 9-10, and then adding the magnesium chloride solution to obtain a solid-liquid mixture;
step d: and aging the solid-liquid mixture at 65-70 ℃ for 20-24 h, then carrying out suction filtration and washing, and finally drying to obtain the intercalated hydrotalcite.
6. The heavy metal scavenger according to claim 4, wherein: and c, adding the magnesium chloride solution and the potassium acetate solution into the sodium hydroxide solution and adding paramagnetic ferrite powder at the same time, wherein the mass ratio of the paramagnetic ferrite powder to the magnesium chloride is 1: 1-2, and after the magnesium chloride solution is added, carrying out ultrasonic-assisted reaction.
7. A process for preparing a heavy metal scavenger according to claim 1:
s1: stirring and uniformly stirring sodium sulfide, trisodium phosphate, cerium, natural cellulose powder and water according to a proportion to obtain a mixed solution for later use;
s2: adding the slow-release material into the mixed solution, and soaking for 8-12 h;
s3: taking out the sustained-release material soaked in the step S2, drying, crushing, and sieving with a 10-100-mesh sieve to obtain sustained-release granules;
the heavy metal trapping agent can be obtained through the 3 steps.
8. The heavy metal scavenger according to claim 1, wherein: before the slow release material is added into the mixed solution, the slow release material is sprayed with ethanol steam for 3-6 min, and then the slow release material is added into the mixed solution.
9. The heavy metal scavenger according to claim 1, wherein: step S4 follows step S3: post-processing, the step S4 operates as follows: carrying out post-treatment on the sustained-release particles obtained in the step S3 by using post-treatment liquid, drying and crushing the sustained-release particles after the post-treatment is finished, and sieving the particles by using a sieve with 10-50 meshes to obtain a heavy metal trapping agent;
the post-treatment liquid comprises the following components in parts by weight:
1-3 parts of nano calcium oxide;
80-100 parts of carboxymethyl cellulose;
200-300 parts of cyclohexane.
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| CN201911370506.0A CN111018038A (en) | 2019-12-26 | 2019-12-26 | Heavy metal trapping agent and preparation process thereof |
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| CN201911370506.0A CN111018038A (en) | 2019-12-26 | 2019-12-26 | Heavy metal trapping agent and preparation process thereof |
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Citations (5)
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2019
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| US20110226702A1 (en) * | 2008-06-30 | 2011-09-22 | Theodore Sall | Solubilized Heavy Metal Binding Reagent |
| CN103043827A (en) * | 2012-12-07 | 2013-04-17 | 常州大学 | Method for removing niobium from sewage |
| CN104492386A (en) * | 2014-10-27 | 2015-04-08 | 河南城建学院 | Preparation method for oxalic-acid-modified pummelo pericarp biological adsorbent |
| CN105413648A (en) * | 2015-12-20 | 2016-03-23 | 吴涛 | Folium ginkgo adsorbing material and preparation method thereof |
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