CN104529920A - Method for preparing novel heavy metal capture agent - Google Patents
Method for preparing novel heavy metal capture agent Download PDFInfo
- Publication number
- CN104529920A CN104529920A CN201410848489.8A CN201410848489A CN104529920A CN 104529920 A CN104529920 A CN 104529920A CN 201410848489 A CN201410848489 A CN 201410848489A CN 104529920 A CN104529920 A CN 104529920A
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- Prior art keywords
- heavy metal
- novel heavy
- water
- preparation
- trapping agent
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D251/00—Heterocyclic compounds containing 1,3,5-triazine rings
- C07D251/02—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings
- C07D251/12—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members
- C07D251/26—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members with only hetero atoms directly attached to ring carbon atoms
- C07D251/38—Sulfur atoms
-
- 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
- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
- C02F1/62—Heavy metal compounds
Abstract
The invention discloses a method for preparing a novel heavy metal capture agent. The method includes the following steps that I, cyanuric chloride reacts on a sulfhydrylization reagent in water solutions at the temperature of 10 DEG C-70 DEG C, and the reaction time is 1-8 h; II, the PH is adjusted to be 10, and undissolved substances are filtered out; III, hydrochloric acid is added into a product in the step II for acidification, and then a large amount of sediments are obtained; IV, the sediments obtained in the step III are separated and are cleaned by water until the cleaned water is neutral, and the obtained sediment solids are dried; V, the sediments obtained in the step IV are dispersed in water and then are mixed with sodium hydroxide liquid, and therefore the novel heavy metal capture agent is obtained. According to the method, flammable and combustible organic solvents are not used, so production operation is safe; the concept of environment protection is penetrated in the method, unlike a traditional organic reaction which needs an additionally arranged solvent recovery device, the method is relatively lower in cost, and a good reaction effect can be obtained just through selection of pure water.
Description
Technical field:
The present invention relates to a kind of preparation method of novel heavy metal trapping agent, belong to industrial wastewater treatment technology field.
Background technology:
The heavy metal wastewater thereby of the relevant industries such as smelting, electrolysis, plating belongs to one of the most unmanageable trade effluent.Heavy metal has enriching, is difficult to degrade in the environment, and its pollution produced is different from some can by the pollution of nature purification itself.Heavy metal can enrichment in human body, causes poisoning, is directly detrimental to health.At present, China, in the exploitation of heavy metal, smelting, the course of processing, causes serious metallic pollution, and environmental quality worsens, and in the situation of increasingly aggravating, prevention and control situation is very severe.
Heavy metal in waste water content is high, and kind is many, and form, the valence state of existence are also different with different enterprise.Because the heavy metal in water cannot destroy decomposition, in waste water, various additive, complex compound, auxiliary component complexity, together with being sequestered in, deal with very difficult with heavy metal ion.
Traditional heavy metal chelating agent comprises PH conditioning agent, sulfide, sulfohydrate etc.Exist with the moderate water-cut stage of PH conditioning agent following not enough: after precipitation, need readjustment PH just can discharge; Have various heavy to coexist in waste water, during containing amphoteric metal, PH is higher, and precipitation can be dissolved again; There is complex compound in waste water, neutralization precipitation is difficult to remove; Deposit seeds is little, not easily precipitates.Following shortcoming is there is: sulfide precipitation particle is little, is unfavorable for precipitation process with sulfide precipitation; Remain in water, when pH value reduces, generate poisonous hydrogen sulfide.
In recent years, increasing modified organisms is used to effluent containing heavy metal ions process, from development trend, mainly towards two aspect progress: utilize macromolecular material for raw material on the one hand, increase the molecular weight of chelating molecule; Increase molecule chelating capacity on the other hand, namely increase the quantity of chelation group on molecule.And effective chelation group is few on macromole, and sequestering power is more weak.
Summary of the invention:
The present invention seeks to, be used for making up the deficiencies in the prior art, a kind of preparation method of novel heavy metal trapping agent is provided.
To achieve these goals, technical scheme of the present invention is as follows:
Novel heavy metal trapping agent a preparation method, comprise following step:
(I) in temperature 10 DEG C ~ 70 DEG C aqueous solution, cyanuric chloride and sulfhydrylization reagent react, and the reaction times is 1-8h;
(II) regulate PH to 10, cross and filter insolubles;
(III) in the product of step (II), add hydrochloric acid and carry out acidifying, obtain and precipitate in a large number;
(IV) separating step (III) gained precipitation, it is neutral for being precipitated to cleaning water outlet with water flushing, and gained precipitated solid is dried;
(V) after step (IV) gained is deposited in disperses in water, mix with caustic lye of soda, obtained novel heavy metal trapping agent.
The preparation method of described a kind of novel heavy metal trapping agent, described sulfhydrylization reagent is Na
2s solution and NaSH solution.
The preparation method of described a kind of novel heavy metal trapping agent, described Na
2s solution is the Na by emulsifying agent and 60% purity
2s is dissolved in pure water, and elimination insolubles obtains.
The preparation method of described a kind of novel heavy metal trapping agent, NaSH solution be by purity be 70% NaSH be dissolved in pure water, elimination insolubles obtains.
The preparation method of described a kind of novel heavy metal trapping agent, in described step (V), precipitation is 1: 3.5 with the weight ratio of sodium hydroxide.
The preparation method of described a kind of novel heavy metal trapping agent, the massfraction of described sodium hydroxide is 30%.
According to the heavy metal chelating agent that the preparation method of described a kind of novel heavy metal trapping agent prepares.
The invention has the beneficial effects as follows:
1. conventional sulfhydrylization reagent is a lot, and as thiocarbamide, basic metal sodium polysulphide, trithiocarbonic acid sodium etc., their prices are more expensive, participate in reaction, and step is complicated.The present invention adopts two kinds of cheap sulfhydrylization reagents, and according to certain ratio, control reinforced at low temperatures, raw material hydrolytic spoilage is few, and raw material is fully used.
2. present invention uses a certain amount of emulsifying agent, reasonably control temperature of reaction, whole system is comparatively even, and range of temperature is little, without High Temperature, for the consuming little energy heated, if temperature is too high, then side reaction increases, and the impurity of generation is more, is unfavorable for products production.
3. the present invention has certain perspective in theory, selects water to make solvent, from change Molecular connectivity and structure properties, increases chelation group aspect and starts with, to development and the development of novel environment friendly heavy metal chelating agent, have initiation, pushing effect.In process of production, do not use inflammable and explosive organic solvent, production operation safety, run through the theory of environmental protection, and unlike traditional organic reaction, need solvent recovery unit have been increased, cost is lower comparatively speaking, only selects pure water just can obtain good reaction effect.
Accompanying drawing explanation
Fig. 1 is reaction principle figure of the present invention.
Fig. 2 is process flow sheet of the present invention.
Embodiment:
The technique means realized to make the present invention, creation characteristic, reaching object and effect is easy to understand, below in conjunction with specific embodiment, setting forth the present invention further.
Embodiment 1
By 1000g pure water, 1g emulsifying agent, 200gNa
2s (purity is 60%) mixes, and elimination insolubles, obtains Na
2s liquid; Dissolved by 600gNaSH (purity is 70%) 1000g pure water, elimination insolubles, obtains NaSH liquid; To Na
2s drop adds NaSH liquid, meanwhile, slowly adds cyanuric chloride 500g (purity is 99.5%), and stir, control temperature is no more than 12 DEG C; After adding, then stir half an hour, reactant is warming up to 70 DEG C, stir, insulation 3h; Be incubated complete, mixture is down to room temperature, regulate PH to 10 with NaOH, filtering separation insolubles; To the HCl liquid that filtrate added drop-wise concentration is 15%, limit edged stirs, and continues 2 hours, regulates PH to 2-3, and point water obtains solid; Gained solid pure water is cleaned to water outlet PH=7, then drying solid; Take 100g gained solid to disperse in 350g pure water, then with 350g massfraction 30%NaOH liquid, fully mix, stirring and dissolving, filtering and impurity removing, obtain bright orange transparent liquid, this product and novel environment friendly high-efficiency heavy metal chelating agent.
Get certain density heavy metal ion-containing waste water 1L, add according to the amount of 200ppm the heavy metal chelating agent that the present invention obtains, stirring reaction 5 minutes, staticly settle 20 minutes, get supernatant liquor, measure the rear water sample heavy metal ion content of process with atomic absorption spectrophotometer, calculate clearance.
| Project-embodiment 1 | Cu 2+Ion | Ni 2+Ion | Cr 3+Ion | Cd 2+Ion | Pb 2+Ion |
| Former water concentration of heavy metal ion | 45ppm | 40ppm | 35ppm | 30ppm | 30ppm |
| Concentration of heavy metal ion after process | 0.01ppm | 0.12ppm | 0.31ppm | 0.42ppm | 0.38ppm |
| Removal of heavy metal ions rate | Nearly 100% | 99.7％ | 99.1％ | 98.6％ | 98.7％ |
Embodiment 2
By 900g pure water, 1.2g emulsifying agent, 180gNa
2s (purity is 60%) mixes, and elimination insolubles, obtains Na
2s liquid; Dissolved by 620gNaSH (purity is 70%) 1100g pure water, elimination insolubles, obtains NaSH liquid; To Na
2s drop adds NaSH liquid, meanwhile, slowly adds cyanuric chloride 500g (purity is 99.5%), and stir, control temperature is no more than 12 DEG C; After adding, then stir half an hour, reactant is warming up to 65 DEG C, stir, insulation 3h; Be incubated complete, mixture is down to room temperature, regulate PH to 10 with NaOH, filtering separation insolubles; To the HCl liquid that filtrate added drop-wise concentration is 12%, limit edged stirs, and continues 2 hours, regulates PH to 2-3, and point water obtains solid; Gained solid pure water is cleaned to water outlet PH=7, then drying solid; Take 100g gained solid to disperse in 350g pure water, then with 350g massfraction 30%NaOH liquid, fully mix, stirring and dissolving, filtering and impurity removing, obtain bright orange transparent liquid, this product and novel environment friendly high-efficiency heavy metal chelating agent.
Get certain density heavy metal ion-containing waste water 1L, add according to the amount of 200ppm the heavy metal chelating agent that the present invention obtains, stirring reaction 5 minutes, staticly settle 20 minutes, get supernatant liquor, measure the rear water sample heavy metal ion content of process with atomic absorption spectrophotometer, calculate clearance.
| Project-embodiment 2 | Cu 2+Ion | Ni 2+Ion | Cr 3+Ion | Cd 2+Ion | pb 2+Ion |
| Former water concentration of heavy metal ion | 45ppm | 40ppm | 35ppm | 30ppm | 30ppm |
| Concentration of heavy metal ion after process | 0.01ppm | 0.10ppm | 0.33ppm | 0.40ppm | 0.41ppm |
| Removal of heavy metal ions rate | Nearly 100% | 99.8％ | 99.1％ | 98.7％ | 98.6％ |
Embodiment 3
By 800g pure water, 1.5g emulsifying agent, 160gNa2S (purity is 60%) mixing, elimination insolubles, obtains Na2S liquid; Dissolved by 640gNaSH (purity is 70%) 1200g pure water, elimination insolubles, obtains NaSH liquid; To Na
2s drop adds NaSH liquid, meanwhile, slowly adds cyanuric chloride 500g (purity is 99.5%), and stir, control temperature is no more than 12 DEG C; After adding, then stir half an hour, reactant is warming up to 60 DEG C, stir, insulation 3h; Be incubated complete, mixture is down to room temperature, regulate PH to 10 with NaOH, filtering separation insolubles; To the HCl liquid that filtrate added drop-wise concentration is 10%, limit edged stirs, and continues 2 hours, regulates PH to 2-3, and point water obtains solid; Gained solid pure water is cleaned to water outlet PH=7, then drying solid; Take 100g gained solid to disperse in 350g pure water, then with 350g massfraction 30%NaOH liquid, fully mix, stirring and dissolving, filtering and impurity removing, obtain bright orange transparent liquid, this product and novel environment friendly high-efficiency heavy metal chelating agent.
Get certain density heavy metal ion-containing waste water 1L, add according to the amount of 200ppm the heavy metal chelating agent that the present invention obtains, stirring reaction 5 minutes, staticly settle 20 minutes, get supernatant liquor, measure the rear water sample heavy metal ion content of process with atomic absorption spectrophotometer, calculate clearance.
| Project-embodiment 3 | Cu 2+Ion | Ni 2+Ion | Cr 3+Ion | Cd 2+Ion | Pb 2+Ion |
| Former water concentration of heavy metal ion | 45ppm | 40ppm | 35ppm | 30ppm | 30ppm |
| Concentration of heavy metal ion after process | 0.01ppm | 0.11ppm | 0.31ppm | 0.41ppm | 0.40ppm |
| Removal of heavy metal ions rate | Nearly 100% | 99.7％ | 99.1％ | 98.6％ | 98.7％ |
More than show and describe ultimate principle of the present invention and principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and specification sheets just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.Application claims protection domain is defined by appending claims and equivalent thereof.
Claims (7)
1. a preparation method for novel heavy metal trapping agent, is characterized in that, comprises following step:
(I) in temperature 10 DEG C ~ 70 DEG C aqueous solution, cyanuric chloride and sulfhydrylization reagent react, and the reaction times is 1-8h;
(II) regulate PH to 10, cross and filter insolubles;
(III) in the product of step (II), add hydrochloric acid and carry out acidifying, obtain and precipitate in a large number;
(IV) separating step (III) gained precipitation, it is neutral for being precipitated to cleaning water outlet with water flushing, and gained precipitated solid is dried;
(V) after step (IV) gained is deposited in disperses in water, mix with caustic lye of soda, obtained novel heavy metal trapping agent.
2. the preparation method of a kind of novel heavy metal trapping agent according to claim 1, is characterized in that, described sulfhydrylization reagent is Na
2s solution and NaSH solution.
3. the preparation method of a kind of novel heavy metal trapping agent according to claim 2, is characterized in that, described Na
2s solution is the Na by emulsifying agent and 60% purity
2s is dissolved in pure water, and elimination insolubles obtains.
4. the preparation method of a kind of novel heavy metal trapping agent according to claim 2, is characterized in that, NaSH solution be by purity be 70% NaSH be dissolved in pure water, elimination insolubles obtains.
5. a kind of novel heavy metal trapping agent according to claim 1 preparation method, it is characterized in that, precipitation is 1: 3.5 with the weight ratio of sodium hydroxide in described step (V).
6. the preparation method of a kind of novel heavy metal trapping agent according to claim 5, is characterized in that, the massfraction of described sodium hydroxide is 30%.
7. the heavy metal chelating agent that the preparation method of a kind of novel heavy metal trapping agent according to above arbitrary claim prepares.
Priority Applications (1)
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| CN201410848489.8A CN104529920A (en) | 2014-12-26 | 2014-12-26 | Method for preparing novel heavy metal capture agent |
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| CN201410848489.8A CN104529920A (en) | 2014-12-26 | 2014-12-26 | Method for preparing novel heavy metal capture agent |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105036281A (en) * | 2015-06-25 | 2015-11-11 | 山西省化工研究所（有限公司） | Preparation of organic sulfur heavy metal capturing agent and recycling and treating method of filtrate thereof |
| CN107970903A (en) * | 2017-11-29 | 2018-05-01 | 郑州大学 | A kind of preparation method for the chelating function fiber for adsorbing heavy metal ion |
| CN111377875A (en) * | 2018-12-28 | 2020-07-07 | 国家电投集团远达环保工程有限公司重庆科技分公司 | Preparation method and application of 2, 4, 6-trimercapto-s-triazine disodium salt aqueous solution |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105036281A (en) * | 2015-06-25 | 2015-11-11 | 山西省化工研究所（有限公司） | Preparation of organic sulfur heavy metal capturing agent and recycling and treating method of filtrate thereof |
| CN107970903A (en) * | 2017-11-29 | 2018-05-01 | 郑州大学 | A kind of preparation method for the chelating function fiber for adsorbing heavy metal ion |
| CN111377875A (en) * | 2018-12-28 | 2020-07-07 | 国家电投集团远达环保工程有限公司重庆科技分公司 | Preparation method and application of 2, 4, 6-trimercapto-s-triazine disodium salt aqueous solution |
| CN111377875B (en) * | 2018-12-28 | 2021-08-03 | 国家电投集团远达环保工程有限公司重庆科技分公司 | Preparation method and application of 2, 4, 6-trimercapto-s-triazine disodium salt aqueous solution |
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Application publication date: 20150422 |
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