CN110563622A - Synthetic method of mixed heavy metal capture agent - Google Patents
Synthetic method of mixed heavy metal capture agent Download PDFInfo
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- CN110563622A CN110563622A CN201910835226.6A CN201910835226A CN110563622A CN 110563622 A CN110563622 A CN 110563622A CN 201910835226 A CN201910835226 A CN 201910835226A CN 110563622 A CN110563622 A CN 110563622A
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- carbon disulfide
- mixed
- heavy metal
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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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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C333/00—Derivatives of thiocarbamic acids, i.e. compounds containing any of the groups, the nitrogen atom not being part of nitro or nitroso groups
- C07C333/14—Dithiocarbamic acids; Derivatives thereof
- C07C333/16—Salts of dithiocarbamic acids
-
- 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
-
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Business, Economics & Management (AREA)
- Emergency Management (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention discloses a synthetic method of a mixed heavy metal capture agent, which comprises the following steps: s1 sampling: taking carbon disulfide, caustic alkali and organic mixed amine for standby, and synthesizing by S2: the carbon disulfide, caustic and organic mixed amine mixed reaction and S3 carbon disulfide recovery are carried out in a carbon disulfide excess solvent process: and (4) distilling and recovering the excessive carbon disulfide synthesized in the step S2 step by step in a mode of firstly carrying out normal pressure and then carrying out reduced pressure. The method does not need complicated manual steps without mixing, avoids the defect of uneven mixing, does not need high temperature and high pressure, has small energy consumption and simple and reliable process, almost has chelation and precipitation effects on all transition-state heavy metals, and has better stabilization effect on heavy metals in fly ash compared with single thiocarbamate.
Description
Technical Field
The invention relates to the technical field of organic mixed amine synthesis, in particular to a synthetic method of a mixed heavy metal capture agent.
Background
municipal solid waste is a complex mixed waste containing considerable amounts of heavy metals. When municipal solid waste is treated by adopting an incineration method, a large amount of volatile elements such as heavy metals of lead, cadmium, zinc, mercury, chromium and the like are volatilized into flue gas due to high temperature and are finally enriched in fly ash. Therefore, the waste incineration fly ash has great harm to the environment and human bodies, and heavy metals in the fly ash need to be stabilized and treated to reach the landfill standard and then concentrated.
The fly ash solidification and stabilization technologies mainly comprise cement solidification, medicament stabilization, asphalt solidification and resin solidification, and a medicament stabilization method can be independently used and has the advantages of small volume-increasing ratio, low energy consumption, simple process and the like, so that the fly ash solidification and stabilization technology is widely used. The molecular structure of the thiocarbamate contains polar groups, so that the thiocarbamate has extremely strong complexing ability with various heavy metals, and has the characteristics of low dosage, high reaction speed, small water solubility of generated chelate and the like, and has very wide application prospect compared with other heavy metal collecting agents.
studies have shown that (Hangon G, Bradshaw D, Ekmekci Z. the Journal of the South African Institute of Mining and metals, 2005,105: 199-206) compared to using a single trapping agent, different mixed group trapping agents have synergistic effects, mainly due to the fact that the synergistic effect between long and short hydrocarbon chains and functional groups is fully utilized to improve the heavy metal stabilization performance and the adsorption characteristics of the mixed trapping agent on the surface of the fly ash condensate are better than those of a single trapping agent.
However, at present, mixed thioamino carboxylates cannot be synthesized using conventional methods, and the mixed thioamino carboxylates in practical use are all prepared by artificially mixing single thioamino carboxylates by mechanical stirring and then using them. But has the defects of uneven mixing, complex operation and the risk of polluting the field environment in the mixing process.
Disclosure of Invention
The present invention aims to provide a method for synthesizing a mixed heavy metal scavenger, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a synthetic method of a mixed heavy metal capture agent comprises the following steps:
s1: sampling: taking carbon disulfide, caustic alkali and organic mixed amine for standby;
S2: synthesizing: carbon disulfide, caustic alkali and organic mixed amine are mixed and reacted by a carbon disulfide excess solvent method.
Preferably, the molar ratio of the organic mixed amine to the caustic alkali to the carbon disulfide is 1: 4 to 6.
preferably, the organic mixed amine is a plurality of dimethylamine, diethylamine, ethylmethyldiamine, diethylamine, propylethyldiamine, and diethylamine.
Preferably, the organic mixed amine accounts for 30-50% of the total mass.
Preferably, the caustic is in the form of powder, granules or flakes.
preferably, the caustic is sodium hydroxide or potassium hydroxide.
Preferably, the synthesis temperature in the step S2 is 0-40 ℃, and the synthesis time is 2-6 h.
preferably, the method further comprises the following steps: s3: and (3) recovering carbon disulfide: and (4) distilling and recovering the excessive carbon disulfide synthesized in the step S2 step by step in a mode of firstly carrying out normal pressure and then carrying out reduced pressure.
Preferably, the atmospheric distillation temperature in the step S3 is 70 to 80 ℃.
Compared with the prior art, the invention has the beneficial effects that:
1. The mixed thioamino carboxylate is synthesized by the one-step method, the complicated steps of manual operation and no mixing are not needed, and the defect of uneven mixing is avoided;
2. The preparation method for synthesizing the mixed thioamino carboxylate by the one-step method does not need high temperature and high pressure, has low energy consumption and simple and reliable process;
3. The mixed thioamino carboxylate heavy metal capture agent synthesized by the one-step method has chelation and sedimentation effects on almost all transition-state heavy metals, and has better stabilization effect on heavy metals in fly ash compared with single thioamino carboxylate.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all 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.
The invention provides a technical scheme that:
example 1
A synthetic method of a mixed heavy metal capture agent comprises the following steps: the method comprises the following steps:
s1: sampling: taking carbon disulfide, caustic alkali and organic mixed amine for standby application, wherein the molar ratio of the organic mixed amine to the caustic alkali to the carbon disulfide is 1: 4, the organic mixed amine is dimethylamine, diethylamine and ethylmethyldiamine, the organic mixed amine accounts for 30% of the total mass, the caustic alkali is in powder form, and the reaction is convenient, and the caustic alkali is sodium hydroxide;
S2: synthesizing: mixing carbon disulfide, caustic alkali and organic mixed amine by using a carbon disulfide excessive solvent method for reaction at the temperature of 0 ℃ for 2 hours;
S3: and (3) recovering carbon disulfide: and (4) distilling and recovering the excessive carbon disulfide synthesized in the step S2 step by adopting a mode of firstly carrying out normal pressure distillation and then carrying out reduced pressure distillation, wherein the normal pressure distillation temperature is 70 ℃.
Example 2
A synthetic method of a mixed heavy metal capture agent comprises the following steps: the method comprises the following steps:
S1: sampling: taking carbon disulfide, caustic alkali and organic mixed amine for standby application, wherein the molar ratio of the organic mixed amine to the caustic alkali to the carbon disulfide is 1: 6, the organic mixed amine is dimethylamine, diethylamine, ethylmethyldiamine, diethylamine, propylethyldiamine and diethylamine, the organic mixed amine accounts for 50% of the total mass, the caustic alkali is flaky and is convenient to react, and the caustic alkali is potassium hydroxide;
s2: synthesizing: mixing carbon disulfide, caustic alkali and organic mixed amine by using a carbon disulfide excessive solvent method for reaction at the temperature of 40 ℃ for 6 hours;
s3: and (3) recovering carbon disulfide: and (4) distilling and recovering the excessive carbon disulfide synthesized in the step S2 step by adopting a mode of firstly carrying out normal pressure distillation and then carrying out reduced pressure distillation, wherein the normal pressure distillation temperature is 80 ℃.
Example 3
A synthetic method of a mixed heavy metal capture agent comprises the following steps: the method comprises the following steps:
s1: sampling: taking carbon disulfide, caustic alkali and organic mixed amine for standby application, wherein the molar ratio of the organic mixed amine to the caustic alkali to the carbon disulfide is 1: 5, the organic mixed amine is diethylamine, ethylmethyldiamine, diethylamine and propylethyldiamine, the organic mixed amine accounts for 40% of the total mass, the caustic alkali is granular, the reaction is convenient, and the caustic alkali is sodium hydroxide;
S2: synthesizing: mixing carbon disulfide, caustic alkali and organic mixed amine by using a carbon disulfide excessive solvent method for reaction at the temperature of 20 ℃ for 4 hours;
S3: and (3) recovering carbon disulfide: and (4) distilling and recovering the excessive carbon disulfide synthesized in the step S2 step by adopting a mode of firstly carrying out normal pressure distillation and then carrying out reduced pressure distillation, wherein the normal pressure distillation temperature is 75 ℃.
The reaction equation is:
R-NH+CS2+MOH→R-N-CS2M+H2O
wherein R-NH is organic mixed amine, and M is Na or K.
Test of
Adding 47.5 parts of carbon disulfide with the purity of 99% and 15 parts of mixed organic amine with the purity of 99% into a reactor (the mass ratio of dimethylamine to diethylamine in the mixed organic amine is n (dimethylamine): n (diethylamine): 3: 7), cooling the mixture at about 20 ℃ under stirring, adding 5 parts, 4 parts and 4 parts of flaky sodium hydroxide (with the purity of 96%) into the reactor by 3 times, stirring for about 10 minutes after each addition, controlling the temperature during alkali addition to be 15-30 ℃, stirring and reacting for 2 hours at 20 ℃ after the caustic alkali is added, and finishing the reaction. And distilling and recovering the excessive carbon disulfide solvent step by step under normal pressure and reduced pressure to obtain the required dimethyl-diethyl mixed sodium thiocarbamate product.
The test reagent selects dimethyl-diethyl mixed sodium thiocarbamate, dimethyl sodium thiocarbamate and diethyl sodium thiocarbamate which are prepared by the test, and inspects the chelating effect of the heavy metal in the fly ash under the condition of 2 percent of the using amount.
the different agent stabilized samples were a (raw ash + 2% dimethyl-diethyl mixed sodium thiocarbamate), B (raw ash + 2% dimethyl sodium thiocarbamate), C (raw ash + 2% diethyl sodium thiocarbamate). The leaching experiment is according to the regulation of acetic acid buffer solution method for leaching toxicity of solid waste, and the test results are shown in the following table 1.
Table 1 shows the stabilizing effect of the mixed heavy metal scavenger on the heavy metal in fly ash
Note: the standard value is taken from GB 16889-2008; ND means sample not detected
The data result in table 1 shows that the mixed heavy metal scavenger prepared by the invention can completely meet the landfill standard specified in GB 16889-2008 at a dosage of 2%, and the mixed heavy metal scavenger with different functional groups has a better stabilization effect on heavy metals in fly ash than a single agent.
Claims (9)
1. A synthetic method of a mixed heavy metal capture agent is characterized in that: the method comprises the following steps:
S1: sampling: taking carbon disulfide, caustic alkali and organic mixed amine for standby;
S2: synthesizing: carbon disulfide, caustic alkali and organic mixed amine are mixed and reacted by a carbon disulfide excess solvent method.
2. the method for synthesizing the mixed heavy metal scavenger according to claim 1, wherein the method comprises the following steps: the molar ratio of the organic mixed amine to the caustic alkali to the carbon disulfide is 1: 4-6.
3. the method for synthesizing the mixed heavy metal scavenger according to claim 2, wherein the method comprises the following steps: the organic mixed amine is a plurality of dimethylamine, diethylamine, ethylmethyldiamine, diethylamine, propylethyldiamine and diethylamine.
4. The method for synthesizing the mixed heavy metal scavenger according to claim 3, wherein the method comprises the following steps: the organic mixed amine accounts for 30-50% of the total mass.
5. The method for synthesizing the mixed heavy metal scavenger according to claim 1, wherein the method comprises the following steps: the caustic alkali is in the form of powder, granules or flakes.
6. The method for synthesizing the mixed heavy metal scavenger according to claim 5, wherein the method comprises the following steps: the caustic alkali is sodium hydroxide or potassium hydroxide.
7. the method for synthesizing the mixed heavy metal scavenger according to claim 1, wherein the method comprises the following steps: the synthesis temperature in the step S2 is 0-40 ℃, and the synthesis time is 2-6 h.
8. the method for synthesizing the mixed heavy metal scavenger according to claim 1, wherein the method comprises the following steps: further comprising the steps of:
S3: and (3) recovering carbon disulfide: and (4) distilling and recovering the excessive carbon disulfide synthesized in the step S2 step by step in a mode of firstly carrying out normal pressure and then carrying out reduced pressure.
9. the method for synthesizing the mixed heavy metal scavenger according to claim 8, wherein the method comprises the following steps: the atmospheric distillation temperature in the step S3 is 70-80 ℃.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111268778A (en) * | 2020-03-04 | 2020-06-12 | 广州天赐高新材料股份有限公司 | Heavy metal trapping agent and preparation method and preparation device thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104528910A (en) * | 2014-12-18 | 2015-04-22 | 淄博金鼎光电科技有限公司 | Synthetic process of heavy metal chelating agent |
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- 2019-09-05 CN CN201910835226.6A patent/CN110563622A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104528910A (en) * | 2014-12-18 | 2015-04-22 | 淄博金鼎光电科技有限公司 | Synthetic process of heavy metal chelating agent |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111268778A (en) * | 2020-03-04 | 2020-06-12 | 广州天赐高新材料股份有限公司 | Heavy metal trapping agent and preparation method and preparation device thereof |
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Application publication date: 20191213 |