CN103466775B - Method for preparing heavy metal ion catching agent - Google Patents
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Abstract
The invention discloses a method for preparing a heavy metal ion catching agent. The heavy metal ion catching agent is mainly formed by being prepared by urea, amine compounds, carbon disulfide, an additive, alkaline matter and distilled water. The heavy metal ion catching agent comprises, by weight, 9-30% of the urea, 1-6% of the amine compounds, 0-4.5% of the additive, 21-45% of the carbon disulfide, 8-17% of the alkaline matter and 20-35% of the distilled water. The method comprises the preparation steps of mixing the urea with the water, adding the alkaline matter to adjust the pH value, adjusting the reaction temperature, adding the micromolecular amine compounds, adding the additive, dropwise adding the carbon disulfide, controlling the temperature to conduct the reaction for a certain time, conducting suction filtration, using ethyl alcohol for conducting washing and drying, and obtaining the polyurea dithiocar-bamate heavy metal ion catching agent. According to the method for preparing the heavy metal ion catching agent, the production cost of the dithiocar-bamate heavy metal ion catching agent is remarkably reduced, and the actual treatment effect, on heavy metal ion waste water, of the heavy metal ion catching agent is good.
Description
Technical field
The present invention relates to technical field of waste water processing, specifically a kind of preparation method of heavy metal ion trapping agent.
Technical background
Mankind nowadays society increases rapidly heavy metal resources demand, in production, processing and use procedure, produce a large amount of wastes containing heavy metal and compound thereof, if its content has exceeded a threshold quantity, just can cause heavy metal contamination, have a strong impact on the utilization of structure, function and the resource of the ecosystem.The industries such as especially smelting, chemical industry, electronics, automobile, mining, plating and light industry are because being used in a large number all kinds of heavy metals and heavy metal compounds to discharge a large amount of waste water containing heavy metal ion.These trade effluents that contain heavy metal can cause serious pollution to surface water and groundwater, and can not biological degradation in environment, easily accumulate, and very easily enter plant materials by root system and by soil Crop, suppress crop growth, promote that drought declines, reduce output, and further enter human body by transmission and the enrichment of food chain, cause canceration, deformity etc., serious harm HUMAN HEALTH.For example, the nuisance disease such as minamata disease (mercury pollution) and itai-itai disease (cadmium pollution) that Japan occurs, the blood lead event of Series of Shuangfeng Xian, central Hunan generation in 2009, and the heavy-metal pollution event that occurs of the ground such as Fengxiang, Shaanxi, Wugang, Hunan, Dongchuan District, Yunnan Province, inland river, Sichuan, Chenzhou, Hunan Province, the improvement of heavy-metal pollution waste water is very urgent.
The treatment process of effluent containing heavy metal ions mainly contains at present: oxidation reduction process, ion exchange method, electrolytic process, reverse osmosis method, By Bubble-floating Method, chemical precipitation method, absorption method etc.Aspect purification efficiency and economic benefit, all there are some problems in these treatment processs, exist remove thoroughly, the shortcoming such as somewhat expensive, generation toxic sludge or other waste materials.For example, conventional alkaline precipitation technique is simple, easy to operate, but removes when contents of many kinds of heavy metal ion not quite applicable, especially for some amphoteric metals, as As, Cr, Cd, Pb, Zn etc., under certain pH value, can form precipitation, and under another pH, may occur anti-moltenly, cause secondary pollution.Along with the development of heavy metal ion sewage disposal technology, various heavy metal ion trapping agent are in succession developed both at home and abroad, heavy metal ion trapping agent is owing to having and the group of the very strong bonding force of heavy metal ion, can effectively remove the heavy metal ion in sewage, and be not subject to the impact of heavy metal ion kind and complexing agent, become the focus of effluent containing heavy metal ions Pollution abatement area research.Current heavy metal ion trapping agent both domestic and external mainly contains two classes: xanthate class and dithiocarbamate(s).
Xanthate class heavy metal ion trapping agent is to carry out xanthogenic acid esterification with dithiocarbonic anhydride and hydroxy-containing compounds to react and form.As insoluble cross-linking starch xanthate, can effectively remove fast, the easy filtration of heavy metal ion and precipitation, pH wide ranges.China investigator is also studied xanthate family macromolecule trapping agent, domestic publication CN85102714, CN1884344, CN1775751A etc. introduced the preparation method and application of xanthate class heavy metal ion trapping agent, all belongs to insoluble xanthate class.Although heavy metal ion is had to good removal effect, because itself is water insoluble, while dispensing in actual use, be difficult to accurately control usage quantity, cause the index such as COD, BOD in sewage easily to exceed standard.
The basic synthetic method of dithiocar-bamate and derivatives class thereof (DTC) heavy metal ion trapping agent is that-CS2-group is grafted on the amino of macromolecular chain.US5013453, US5372726, US6454963, all genus dithiocarbamate(s) heavy metal ion trapping agent that the patents such as US20060060538 relate to.DTC class heavy metal ion trapping agent has represented the heavy metal ion trapping agent that current performance is best, its treatment process simple (can directly throw on former chemical precipitation subtraction unit), expense is low, after accomplishing that situation that contents of many kinds of heavy metal ion coexists is processed next time, get final product meet the requirement of environmental protection, even also can play one's part to the full to coexist salt and complexing salt (as: EDTA, NH3, citric acid etc.) of heavy metal ions in wastewater, and have that flocs unit is thick, precipitation is fast, dehydration is fast, aftertreatment is easy, sludge quantity is few and it is nontoxic to stablize, there is no the features such as secondary public hazards.But due to its main synthetic polyamine compounds exist expensive, have the restraining factors such as certain toxicity, thereby limited the large-scale promotion application of DTC class heavy metal chelating agent.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of new heavy metal ion trapping agent, for containing heavy metal ion sewage disposal, and overcome the production cost of traditional trapping agent high, use inconvenience, easily cause the defect of secondary pollution.
The present invention solves the problems of the technologies described above with following technical scheme:
The preparation method of a kind of heavy metal ion trapping agent of the present invention, it is mainly prepared from by urea, aminated compounds, dithiocarbonic anhydride, auxiliary, alkaline matter and distilled water, each compositions in weight percentage proportioning is as follows: urea 9-30%, aminated compounds 1-6%, auxiliary 0-4.5%, dithiocarbonic anhydride 21-45%, alkaline matter 8-17%, distilled water 20-35%;
Step of preparation process is: urea and alkaline matter are placed in to reactor and add distilled water stirring and dissolving, control temperature of reaction is 25-60 DEG C, then adds aminated compounds, mix and blend reaction 30-60 minute; While needing to add auxiliary, at 40-60 DEG C, add auxiliary mix and blend reaction 30-60 minute, again at normal pressure and 25-40 DEG C, dropwise add dithiocarbonic anhydride, maintain temperature of reaction constant, stirring reaction 90-300 minute, obtains orange-yellow mixing liquid, by this liquid wash with water, after ethanol dehydration through vacuum-drying, get final product to obtain finished product.
The preparation method of heavy metal ion trapping agent of the present invention, described alkaline matter is one or both mixing in sodium hydroxide, potassium hydroxide.
The preparation method of heavy metal ion trapping agent of the present invention, described aminated compounds is one or more mixing in quadrol, triethylene tetramine, diethylenetriamine.
The preparation method of heavy metal ion trapping agent of the present invention, described auxiliary is one or more mixing in starch, Xylo-Mucine, polyacrylamide.
The preparation method of heavy metal ion trapping agent of the present invention, described dry concrete operations are, by mixing liquid vacuum-drying 5 hours at 50 DEG C after washing, dehydration, obtain pressed powder finished product.
The present invention is by carrying out dithioamnoformic acid modifying by urea, obtain the heavy metal ion trapping agent of Urea-based dithiocarbamate(s) polymkeric substance, be main component production heavy metal ion trapping agent owing to adopting urea cheap and easy to get on market, building-up process is simple, workable, cost is low, using method is simple, process containing heavy metal ion sewage effective, there is very strong heavy metal ion capturing ability, the alumen ustum producing is large, settling velocity is fast, and the heavy metal ion inner complex stable chemical nature forming in treating processes, be difficult to cause secondary pollution.Product of the present invention can be used for the industries such as metal manufacture, electronics, plating, chemistry, iron and steel and non-ferrous metal metallurgy and removes containing one or more effluent containing heavy metal ions such as cadmium, chromium, lead, zinc, copper, nickel, manganese.
Embodiment
Below the inventive method is further described.
The heavy metal ion trapping agent preparing by the inventive method is Urea-based dithiocarbamate(s) compound, it is to be mainly prepared from by urea, aminated compounds, dithiocarbonic anhydride, auxiliary, alkaline matter, distilled water, each raw materials by weight proportioning is as follows: urea 9-30%, aminated compounds 1-6%, auxiliary 0-4.5%, dithiocarbonic anhydride 21-45%, alkaline matter 8-17%, distilled water 20-35%.
The basic material that the inventive method adopts is urea, has another name called carbonyl diamine, carboxamide or urea, the organic compound being made up of carbon, nitrogen, oxygen and hydrogen.
The alkaline matter that the inventive method adopts is one or both mixing in sodium hydroxide, potassium hydroxide.
The aminated compounds that the inventive method adopts is one or more mixing in quadrol, triethylene tetramine, diethylenetriamine.
The auxiliary that the inventive method adopts is one or more mixing in starch, Xylo-Mucine, polyacrylamide.
Below the specific embodiment of the inventive method:
Embodiment mono-
Under normal pressure, in tri-mouthfuls of round-bottomed flasks of 500ml of being furnished with induction stirring and reflux condensing tube, proceed as follows: at 25 DEG C, add 36g urea, water 50ml, adds sodium hydroxide 30g, stir 15min, and to control temperature of reaction be 25 DEG C.Add again diethylenetriamine 4g, triethylene tetramine 1g, continue stirring reaction 30 minutes; Then at 25 DEG C, slowly drip dithiocarbonic anhydride 58ml, 1 of p.s., and it is constant to maintain temperature of reaction, for preventing dithiocarbonic anhydride volatilization, when reinforced, can take ice-water bath, continues reaction 90 minutes, obtains orange-yellow mixing liquid.Mixing liquid is washed with water and suction filtration, remove impurity, then with absolute ethanol washing dehydration, then carry out vacuum-drying after 5 hours in 50 DEG C, obtain pressed powder product.
Embodiment bis-
Under normal pressure, in tri-mouthfuls of round-bottomed flasks of 500ml of being furnished with induction stirring and reflux condensing tube, proceed as follows: at 25 DEG C, add 12g urea, water 40ml, adds potassium hydroxide 10g, stir 15min, and to control temperature of reaction be 40 DEG C.Add again quadrol 6.5ml, continue stirring reaction after 45 minutes, at 40 DEG C, add carboxymethyl cellulose 3g mix and blend reaction 30 minutes, at 40 DEG C, slowly drip again dithiocarbonic anhydride 46ml, 1 of p.s., control temperature of reaction constant, for preventing dithiocarbonic anhydride volatilization, when reinforced, can take ice-water bath, continue reaction 180 minutes, obtain orange-yellow mixing liquid.Mixing liquid is washed with water and suction filtration, remove impurity, then with absolute ethanol washing dehydration, then carry out vacuum-drying 5 hours under 50 DEG C of degree, obtain pressed powder product.
Embodiment tri-
Under normal pressure, in tri-mouthfuls of round-bottomed flasks of 500ml of being furnished with induction stirring and reflux condensing tube, proceed as follows: at 50 DEG C, add 59g urea, water 60ml, adds sodium hydroxide 15g, potassium hydroxide 10g, stir 15min, and to control temperature of reaction be 50 DEG C; Add again triethylene tetramine 2.1g, continue stirring reaction after 60 minutes, at 50 DEG C, add starch 5g, polyacrylamide 3.5g, mix and blend reaction 60 minutes, then at 40 DEG C, slowly drip dithiocarbonic anhydride 43.6ml, 1 of p.s., control temperature of reaction is constant, for preventing dithiocarbonic anhydride volatilization, when reinforced, can take ice-water bath, continue reaction 280 minutes, obtain orange-yellow mixing liquid.Mixing liquid is washed with water and suction filtration, remove impurity, then with absolute ethanol washing dehydration, then at 50 DEG C, carry out vacuum-drying 5 hours, obtain pressed powder product.
Embodiment tetra-
Take heavy metal ion trapping agent 10g prepared by embodiment mono-and add in 100ml volumetric flask, to scale, stand-by with distilled water diluting.Get heavy metal ion Pb
2+, Zn
2+, Cu
2+, Cd
2+concentration is respectively the each 500ml of simulated wastewater of 10mg/L, adds heavy metal ion trapping agent 2.5ml, stirs 5min, leave standstill 15min, filter, measure each simulated wastewater actual concentrations value after treatment with ICP, the concentration obtaining after various metal ion treatments is respectively: Zn
2+reach 0.5077mg/L; Cd
2+reach 0.0085mg/L; Cu
2+reach 0.0453mg/L; Pb
2+reach 0.0310mg/L.Its clearance is respectively: Zn
2+clearance 94.9%; Cd
2+clearance 99.9%; Cu
2+clearance 99.5%; Pb
2+clearance 99.7%;
Embodiment five
Take heavy metal ion trapping agent 1g prepared by embodiment bis-and add in 250ml volumetric flask, to scale, stand-by with distilled water diluting.Get heavy metal ion Pb
2+, Zn
2+, Cu
2+, Cd
2+concentration is respectively the each 500ml of simulated wastewater of 10mg/L, adds heavy metal ion trapping agent 2.5ml, stirs 5min, leave standstill 15min, filter, measure each simulated wastewater actual concentrations value after treatment with ICP, the concentration obtaining after various metal ion treatments is respectively: Zn
2+for 0.9210mg/L; Cd
2+for 0.0873mg/L; Cu
2+for 0.7513mg/L; Pb
2+for 0.2098mg/L.
Embodiment six
Take ion heavy metal chelating agent 1g prepared by embodiment tri-and add in 250ml volumetric flask, to scale, stand-by with distilled water diluting.Get heavy metal ion Pb
2+, Zn
2+, Cu
2+, Cd
2+concentration is respectively the each 500ml of simulated wastewater of 10mg/L, adds heavy metal ion trapping agent 2.5ml, stirs 5min, leave standstill 15min, filter, measure each simulated wastewater actual concentrations value after treatment with ICP, the concentration obtaining after various metal ion treatments is respectively: Zn
2+for 1.2077mg/L; Cd
2+for 0.1053mg/L; Cu
2+for 1.3258mg/L; Pb
2+for 0.8672mg/L.
Claims (3)
1. the preparation method of a heavy metal ion trapping agent, it is characterized in that: it is mainly prepared from by urea, aminated compounds, dithiocarbonic anhydride, auxiliary, alkaline matter and distilled water, each compositions in weight percentage proportioning is as follows: urea 9 ?30%, aminated compounds 1 ?6%, auxiliary 0 ?4.5%, dithiocarbonic anhydride 21 ?45%, alkaline matter 8 ?17%, distilled water 20 ?35%; Described aminated compounds is one or more mixing in quadrol, triethylene tetramine, diethylenetriamine; Described auxiliary is one or more mixing in starch, Xylo-Mucine, polyacrylamide;
Step of preparation process is: urea and alkaline matter are placed in to reactor and add distilled water stirring and dissolving, control temperature of reaction and be 25 ?60 DEG C, then add aminated compounds, mix and blend react 30 ?60 minutes; While needing to add auxiliary, 40 ?add at 60 DEG C auxiliary mix and blend react 30 ?60 minutes, again in normal pressure and 25 ?at 40 DEG C, dropwise add dithiocarbonic anhydride, maintain temperature of reaction constant, stirring reaction 90 ?300 minutes, obtain orange-yellow mixing liquid, by this liquid wash with water, after ethanol dehydration through vacuum-drying, get final product to obtain finished product.
2. the preparation method of heavy metal ion trapping agent according to claim 1, is characterized in that: described alkaline matter is one or both mixing in sodium hydroxide, potassium hydroxide.
3. the preparation method of heavy metal ion trapping agent according to claim 1, is characterized in that: described dry concrete operations are, by mixing liquid vacuum-drying 5 hours at 50 DEG C after washing, dehydration, obtains pressed powder finished product.
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| 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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