CN111268778A - Heavy metal trapping agent and preparation method and preparation device thereof - Google Patents
Heavy metal trapping agent and preparation method and preparation device thereof Download PDFInfo
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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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
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- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D3/00—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances
- A62D3/30—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by reacting with chemical agents
- A62D3/33—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by reacting with chemical agents by chemical fixing the harmful substance, e.g. by chelation or complexation
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
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- B01F33/811—Combinations of similar mixers, e.g. with rotary stirring devices in two or more receptacles in two or more consecutive, i.e. successive, mixing receptacles or being consecutively arranged
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
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- B01F33/836—Mixing plants; Combinations of mixers combining mixing with other treatments
- B01F33/8362—Mixing plants; Combinations of mixers combining mixing with other treatments with chemical reactions
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- C—CHEMISTRY; METALLURGY
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- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
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- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D2101/00—Harmful chemical substances made harmless, or less harmful, by effecting chemical change
- A62D2101/08—Toxic combustion residues, e.g. toxic substances contained in fly ash from waste incineration
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- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D2101/00—Harmful chemical substances made harmless, or less harmful, by effecting chemical change
- A62D2101/40—Inorganic substances
- A62D2101/43—Inorganic substances containing heavy metals, in the bonded or free state
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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
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Abstract
The invention relates to a heavy metal trapping agent, and a preparation method and a preparation device thereof. The heavy metal trapping agent is prepared from the following raw materials in parts by mole: 0.5-2 parts of macromolecular organic amine, 0.5-2 parts of micromolecular organic amine, 0.5-2 parts of alkaline substance and 0.5-2 parts of sulfide. The heavy metal trapping agent is easy to form flocculent precipitate with complex heavy metal ions and can fix the heavy metal ions for a long time.
Description
Technical Field
The invention relates to the field of environmental management, in particular to a heavy metal trapping agent, a preparation method and a preparation device thereof.
Background
The heavy metal trapping agent is a chemical product capable of strongly chelating with heavy metal ions, and a chelate salt formed by the heavy metal trapping agent and the heavy metal ions is generally insoluble in water and has stable performance. Therefore, the heavy metal collector can be widely used in the fields of waste incineration fly ash treatment, heavy metal wastewater treatment and the like.
At present, the research on heavy metal trapping agents is mostly focused on organic matters containing coordination atoms such as N/O/P/S. Some heavy metal collectors have been marketed, such as polysulfides (PSf) and trithiocarbonates (TTC), trimercaptotriazine (TMT), Dithiocarbamates (DTC). Although the above heavy metal collectors have achieved industrial application, they all have some drawbacks: PSf and TTC are mainly effective against ionic heavy metal, and basically ineffective against complex heavy metal ions, and waste water treated by polysulfide is easy to be turbid and light yellow; although TMT can remove part of complex heavy metal, TMT mainly removes ionic heavy metal, and the use pH range of TMT is narrow, and the TMT is suitable for being used under neutral to alkalescence; the DTC heavy metal trapping agent has better effect on removing the complex heavy metal in the heavy metal trapping agents. However, in the preparation process of the DTC heavy metal trapping agent, small-molecule organic amine is generally used as a raw material, and in the actual use process, the DTC heavy metal trapping agent is easy to decompose and lose water, is not easy to complex, flocculate and precipitate, and is at a disadvantage in long-term measurement.
Disclosure of Invention
Based on the heavy metal trapping agent, the invention provides a heavy metal trapping agent. The heavy metal trapping agent is easy to form flocculent precipitate with complex heavy metal ions and can fix the heavy metal ions for a long time.
The specific technical scheme is as follows:
the heavy metal trapping agent is prepared from the following raw materials in parts by mole:
the invention also provides a preparation method of the heavy metal trapping agent.
The specific technical scheme is as follows:
a preparation method of a heavy metal trapping agent comprises the following steps:
mixing the macromolecular organic amine and the micromolecular organic amine, and then adding an alkaline substance to obtain a first mixture;
adding the sulfide to the first mixture to obtain a second mixture;
reacting the second mixture at 10-40 ℃ for 10-60 min.
The invention also provides a preparation device of the heavy metal trapping agent.
The specific technical scheme is as follows:
a preparation device of a heavy metal trapping agent comprises a first-stage mixer, a second-stage mixer and a third-stage reactor;
and conveying the macromolecular organic amine, the micromolecular organic amine and the alkaline substance to the first-stage mixer, conveying the obtained first mixture to the second-stage mixer, mixing the first mixture with the sulfide in the second-stage mixer, and conveying the obtained second mixture to the third-stage reactor.
Compared with the prior art, the invention has the following beneficial effects:
the heavy metal trapping agent takes macromolecular organic amine and micromolecular organic amine as mixed amine, and the mixed amine is mixed with a certain proportion of alkaline substances and sulfides to prepare the dithiocarbamate heavy metal trapping agent. The S atom can be used as a coordination atom due to the characteristic of lone pair electrons, and forms a complex with macromolecular organic amine and micromolecular organic amine firstly, and then is combined with heavy metal ions to form a sulfide. In the process of forming a complex with mixed amine, the macromolecular organic amine has a plurality of different substituents, the different substituents have different electron donating capacities, the macromolecular organic amine can capture a plurality of metal ions after being supplied to an S atom, the micromolecular organic amine also forms a complex with the S atom at the moment, a plurality of middle complexes simultaneously appear in the system, at the moment, the complexes are classified into middle alkali or weak acid, can easily perform a complex reaction with heavy metal ions classified into middle acid or weak alkali according to an acid-base theory, and have a capturing effect on a plurality of heavy metal ions. And the complex formed is not easily decomposed. Namely, the addition of the mixed amine is more beneficial to forming a stable dithiocarbamate compound with sulfide, is easy to complex, flocculate and precipitate, and plays a role in fixing heavy metal ions for a long time. In conclusion, the heavy metal trapping agent disclosed by the invention can form long-term stable complex flocculation precipitation with heavy metal ions, and has excellent performance.
Drawings
FIG. 1 is a schematic diagram of a preparation device of a heavy metal trapping agent.
Detailed Description
The present invention will be described in further detail with reference to specific examples. The present invention may be embodied in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The heavy metal trapping agent is prepared from the following raw materials in parts by mole:
the heavy metal trapping agent takes macromolecular organic amine and micromolecular organic amine as mixed amine, and the mixed amine is mixed with a certain proportion of alkaline substances and sulfides to prepare the dithiocarbamate heavy metal trapping agent. The mixed amine is more favorable for forming a stable dithiocarbamate compound with sulfide, is easy to complex, flocculate and precipitate, and plays a role in fixing heavy metal ions for a long time.
Preferably, the molar ratio of the macromolecular organic amine to the small-molecular organic amine is 1: (0.5-2).
Further preferably, the molar ratio of the macromolecular organic amine to the small-molecular organic amine is 1: (0.8-1.5).
In the mixed amine, the molar ratio of the macromolecular organic amine to the micromolecules has certain influence on the long-acting heavy metal ion fixing effect of the heavy metal trapping agent.
Preferably, the macromolecular organic amine is selected from one or two of N, N-dimethyl-1, 3-propane diamine and fatty amidopropyl secondary amine.
Understandably, the macromolecular organic amine can be obtained from byproducts in the production of tertiary amine surfactants or amine dyes, the byproduct treatment of related industries can be effectively solved, the waste utilization is realized, and the preparation method is green, economic and environment-friendly.
Preferably, the small-molecule organic amine is selected from one or more of dimethylamine, diethylamine and propylenediamine.
Preferably, the alkaline substance is selected from one or more of alkali metal hydroxide, ammonia water and triethanolamine.
Preferably, the sulphide is carbon disulphide.
In some preferred embodiments, the heavy metal trapping agent is prepared from the following raw materials in parts by mole:
the inventor of the invention finds in experiments that when the macromolecular organic amine is fatty amide propyl secondary amine and the micromolecular organic amine is diethylamine, the prepared heavy metal trapping agent has good flocculation and precipitation effects with heavy metal ions, and the precipitation effects can be stably maintained for a long time.
A preparation method of a heavy metal trapping agent comprises the following steps:
mixing the macromolecular organic amine and the micromolecular organic amine, and then adding an alkaline substance to obtain a first mixture;
adding the sulfide to the first mixture to obtain a second mixture;
reacting the second mixture at 10-40 ℃ for 10-60 min.
Preferably, the second mixture is reacted at 15-30 ℃ for 10-30 min.
A preparation device of a heavy metal trapping agent comprises a first-stage mixer, a second-stage mixer and a third-stage reactor;
and conveying the macromolecular organic amine, the micromolecular organic amine and the alkaline substance to the first-stage mixer, conveying the obtained first mixture to the second-stage mixer, mixing the first mixture with the sulfide in the second-stage mixer, and conveying the obtained second mixture to the third-stage reactor.
It will be appreciated that the plant also comprises a finished product collection tank into which the products produced by the three-stage reactor are conveyed.
The preparation method of the heavy metal trapping agent adopts a continuous reaction device, and comprises the steps of conveying macromolecular organic amine, micromolecular organic amine and liquid alkali to a first-stage mixer for mixing to obtain a first mixture, mixing the first mixture and a sulfide in a second-stage mixer to obtain a second mixture, and conveying the second mixture to a third-stage reactor for reaction. By adopting the mixing method and the mixing device, the reaction heat can be effectively controlled in the mixing process, the reaction heat can be quickly removed conveniently, and on the other hand, the amines can be uniformly mixed, and the reaction uniformity is better. Meanwhile, the process route of the continuous production is simple, the whole synthesis process can realize the continuous input of materials and the output of products, and the production efficiency can be greatly improved.
The following is a further description with reference to specific examples.
Example 1
The embodiment provides a heavy metal trapping agent, a preparation method and a preparation device thereof. The method comprises the following steps of:
as shown in fig. 1, an aqueous solution of N, N-dimethyl-1, 3-propanediamine (in which N, N-dimethyl-1, 3-propanediamine is added in an amount of 1mol) having a mass fraction of 40% and an aqueous solution of dimethylamine (in which dimethylamine is added in an amount of 1mol) having a mass fraction of 40% are fed into a primary mixer through an inlet a and an inlet B, respectively, and then a liquid caustic soda (in which sodium hydroxide is added in an amount of 1mol) having a mass fraction of 32% is fed into the primary mixer through an inlet C and mixed to obtain a first mixture.
And conveying the first mixture to a secondary mixer, and then conveying 1mol of carbon disulfide to the secondary mixer through a D inlet to obtain a second mixture through mixing.
And conveying the second mixture into a three-stage reactor, reacting at 30 ℃ for 30min, and conveying a reaction product into a finished product tank to obtain the heavy metal trapping agent with the active matter concentration of 40%.
Example 2
This example provides a heavy metal trapping agent, a method for producing the same, and an apparatus for producing the same, which are substantially the same as in example 1 except that the kinds of the macromolecular organic amine and the small-molecular organic amine are different from those in example 1. The method comprises the following specific steps:
respectively conveying a 40% by mass of an aqueous solution of fatty amidopropyl secondary amine (wherein the addition amount of the fatty amidopropyl secondary amine is 1mol) and a 40% by mass of an aqueous solution of diethylamine (wherein the addition amount of the diethylamine is 1mol) to a primary mixer through an inlet A and an inlet B, and then conveying 32% by mass of liquid caustic soda (wherein the addition amount of sodium hydroxide is 1mol) to the primary mixer through an inlet C to obtain a first mixture through mixing.
And conveying the first mixture to a secondary mixer, and then conveying 1mol of carbon disulfide to the secondary mixer through a D inlet to obtain a second mixture through mixing.
And conveying the second mixture to a three-stage reactor, reacting at 30 ℃ for 30min, and conveying a reaction product to a finished product tank to obtain the heavy metal trapping agent.
Example 3
This example provides a heavy metal trapping agent, a method and an apparatus for producing the same, which are substantially the same as those in example 2 except that the amount of diethylamine added is different from that in example 2. The method comprises the following specific steps:
respectively delivering a 40% by mass aqueous solution of fatty amidopropyl secondary amine (wherein the adding amount of the fatty amidopropyl secondary amine is 1mol) and a 40% by mass aqueous solution of diethylamine (wherein the adding amount of the diethylamine is 1.5mol) to a first-stage mixer through an inlet A and an inlet B, and then delivering 32% by mass liquid caustic soda (wherein the adding amount of the sodium hydroxide is 1mol) to the first-stage mixer through an inlet C to obtain a first mixture through mixing.
And conveying the first mixture to a secondary mixer, and then conveying 1mol of carbon disulfide to the secondary mixer through a D inlet to obtain a second mixture through mixing.
And conveying the second mixture to a three-stage reactor, reacting at 30 ℃ for 30min, and conveying a reaction product to a finished product tank to obtain the heavy metal trapping agent.
Example 4
This example provides a heavy metal trapping agent, a method and an apparatus for producing the same, which are substantially the same as those in example 2 except that the amount of diethylamine added is different from that in example 2. The method comprises the following specific steps:
respectively conveying a 40% by mass of an aqueous solution of fatty amidopropyl secondary amine (wherein the addition amount of the fatty amidopropyl secondary amine is 1mol) and a 40% by mass of an aqueous solution of diethylamine (wherein the addition amount of the diethylamine is 2mol) to a primary mixer through an inlet A and an inlet B, and then conveying 32% by mass of liquid caustic soda (wherein the addition amount of sodium hydroxide is 1mol) to the primary mixer through an inlet C to obtain a first mixture through mixing.
And conveying the first mixture to a secondary mixer, and then conveying 1mol of carbon disulfide to the secondary mixer through a D inlet to obtain a second mixture through mixing.
And conveying the second mixture to a three-stage reactor, reacting at 30 ℃ for 30min, and conveying a reaction product to a finished product tank to obtain the heavy metal trapping agent.
Comparative example 1
This comparative example provides a heavy metal trapping agent, and a method and an apparatus for producing the same, which are substantially the same as those in example 2 except that no fatty amidopropyl secondary amine was added. The method comprises the following specific steps:
and (2) conveying a 40% diethylamine aqueous solution (wherein the adding amount of diethylamine is 1mol) to a first-stage mixer through an inlet B, and then conveying 32% liquid caustic soda (wherein the adding amount of sodium hydroxide is 1mol) to the first-stage mixer through an inlet C to mix to obtain a first mixture.
And conveying the first mixture to a secondary mixer, and then conveying 1mol of carbon disulfide to the secondary mixer through a D inlet to obtain a second mixture through mixing.
And conveying the second mixture to a three-stage reactor, reacting at 30 ℃ for 30min, and conveying a reaction product to a finished product tank to obtain the heavy metal trapping agent.
Comparative example 2
This comparative example provides a heavy metal trapping agent, and a method and an apparatus for producing the same, which are substantially the same as in example 2 except that fatty amidopropyl secondary amine was replaced with dihexylamine. The method comprises the following specific steps:
respectively conveying a 40% by mass fraction dihexylamine aqueous solution (wherein the adding amount of the dihexylamine is 1mol) and a 40% by mass fraction diethylamine aqueous solution (wherein the adding amount of the diethylamine is 1mol) to a first-stage mixer through an inlet A and an inlet B, and then conveying 32% by mass fraction liquid caustic soda (wherein the adding amount of the sodium hydroxide is 1mol) to the first-stage mixer through an inlet C to obtain a first mixture through mixing.
And conveying the first mixture to a secondary mixer, and then conveying 1mol of carbon disulfide to the secondary mixer through a D inlet to obtain a second mixture through mixing.
And conveying the second mixture to a three-stage reactor, reacting at 30 ℃ for 30min, and conveying a reaction product to a finished product tank to obtain the heavy metal trapping agent.
Performance testing
The heavy metal collecting agents obtained in examples 1-4 and comparative examples 1-2 were used for the fly ash heavy metal leaching experiment.
The leaching experiment method comprises the following steps:
(1) the stabilizing treatment method comprises the steps of calculating the adding amount of the heavy metal trapping agent obtained in each of examples 1-4 and comparative examples 1-2 according to the proportion that the mass of the heavy metal trapping agent/the mass of fly ash is 3%, weighing according to the calculated adding amount, fully dissolving the heavy metal trapping agent/fly ash in 100mL of distilled water, then mixing the heavy metal trapping agent/fly ash with 100g of fly ash (600 g of fly ash is taken and equally divided into 6 parts), fully stirring the mixture to form slurry, maintaining the slurry at room temperature for 24 hours, then placing the slurry in an oven to dry at 40 ℃, taking out the slurry, grinding the slurry into powder to be subjected to leaching experiments.
(2) According to the regulation of acetic acid buffer solution method for leaching toxicity of solid waste (HJT300-2007), 100g of stabilized fly ash sample is weighed in a 2L extraction bottle, 34.5ml of glacial acetic acid is diluted to 2L by deionized water, and the pH value is 2.64 +/-0.05. Fixing the extraction bottle on a turnover type oscillation device with the rotation speed of 30r/min, and oscillating for 18 h. And (3) after oscillation is finished, taking down the extraction bottle, standing for about 30min, measuring the pH of the supernatant by using a pH meter after the residual solid is precipitated, carrying out vacuum filtration on the leaching solution by using a 0.45-micron filter membrane, leaching by using dilute nitric acid, acidifying until the pH is less than 2, and storing at 4 ℃.
(3) Long-term stability test: and (3) storing the stabilized fly ash sample prepared in the step (1) at a sealed room temperature for 6 months, and extracting the stabilized fly ash sample after 6 months according to the method in the step (2).
The concentrations of Pb, Zn and Cd in the leachate after the samples are subjected to suction filtration are measured by an inductively coupled plasma emission spectrum, and the measurement results are shown in Table 1.
TABLE 1
As can be seen from Table 1, the macro-molecular organic amine and the micro-molecular organic amine are used together as the mixed amine, which is beneficial to flocculation and precipitation of heavy metal ions, wherein the matching mode of the fatty amide propyl secondary amine and the diethylamine has more prominent effect. Meanwhile, the heavy metal trapping agent can keep the action on heavy metal ions for a long time and has stable performance.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. The heavy metal trapping agent is characterized by being prepared from the following raw materials in parts by mole:
2. the heavy metal trapping agent according to claim 1, wherein the molar ratio of the macromolecular organic amine to the small organic amine is 1: (0.5-2).
3. The heavy metal trapping agent according to claim 2, wherein the molar ratio of the macromolecular organic amine to the small organic amine is 1: (0.8-1.5).
4. The heavy metal collector of claim 3, wherein the macromolecular organic amine is selected from one or both of N, N-dimethyl-1, 3-propanediamine and fatty amidopropyl secondary amine.
5. The heavy metal trapping agent according to claim 3, wherein the small organic amine is one or more selected from dimethylamine, diethylamine and propylenediamine.
6. The heavy metal collector according to claim 3, wherein the alkaline substance is one or more selected from the group consisting of alkali metal hydroxide, ammonia water and triethanolamine.
7. Heavy metal trap according to claim 3, characterized in that the sulphide is carbon disulphide.
8. The heavy metal collector of any one of claims 1 to 7, wherein the heavy metal collector is prepared from the following raw materials in parts by mole:
9. a process for the preparation of a heavy metal trap according to any of claims 1 to 8, comprising the steps of:
mixing the macromolecular organic amine and the micromolecular organic amine, and then adding an alkaline substance to obtain a first mixture;
adding the sulfide to the first mixture to obtain a second mixture;
reacting the second mixture at 10-40 ℃ for 10-60 min.
10. The preparation device of the heavy metal trapping agent is characterized by comprising a first-stage mixer, a second-stage mixer and a third-stage reactor;
and conveying the macromolecular organic amine, the micromolecular organic amine and the alkaline substance to the first-stage mixer, conveying the obtained first mixture to the second-stage mixer, mixing the first mixture with the sulfide in the second-stage mixer, and conveying the obtained second mixture to the third-stage reactor.
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| CN112972976A (en) * | 2021-02-05 | 2021-06-18 | 南京理工大学 | Method for co-processing solid-liquid phase product of fly ash coal ash hydrothermal reaction |
| RU2794937C1 (en) * | 2022-06-14 | 2023-04-25 | Акционерное общество "Ижевский электромеханический завод "Купол" | Method for producing a heavy metal precipitator for wastewater treatment |
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| CN110563622A (en) * | 2019-09-05 | 2019-12-13 | 南通乐尔环保科技有限公司 | Synthetic method of mixed heavy metal capture agent |
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| CN112972976A (en) * | 2021-02-05 | 2021-06-18 | 南京理工大学 | Method for co-processing solid-liquid phase product of fly ash coal ash hydrothermal reaction |
| RU2794937C1 (en) * | 2022-06-14 | 2023-04-25 | Акционерное общество "Ижевский электромеханический завод "Купол" | Method for producing a heavy metal precipitator for wastewater treatment |
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