CN110723774A - Polymeric copper sulfate and iron inorganic composite water purifying agent and preparation method and application thereof - Google Patents
Polymeric copper sulfate and iron inorganic composite water purifying agent and preparation method and application thereof Download PDFInfo
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- CN110723774A CN110723774A CN201910981423.9A CN201910981423A CN110723774A CN 110723774 A CN110723774 A CN 110723774A CN 201910981423 A CN201910981423 A CN 201910981423A CN 110723774 A CN110723774 A CN 110723774A
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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
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/009—Compounds containing, besides iron, two or more other elements, with the exception of oxygen or hydrogen
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/14—Sulfates
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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
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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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
- C02F2101/30—Organic compounds
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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
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Abstract
The invention discloses a polymeric copper sulfate iron inorganic composite water purifying agent, a preparation method and application thereof. The polymeric copper sulfate iron inorganic composite water purifying agent is characterized in that: the polymer comprises copper and iron ions, the sum of the mass concentration of the iron ions and the effective metal ions of the copper ions is 7.42-12.12g/L, and the molar ratio of the copper ions to the iron ions is 0.02-0.05: 1. The preparation method of the polymeric copper sulfate iron inorganic composite water purifying agent takes ferric sulfate, copper sulfate pentahydrate, hydrogen peroxide and sodium carbonate as raw materials, and is synthesized by a prepolymerization method of adding sodium carbonate and copper sulfate into a ferric sulfate solution with a certain proportion for copolymerization, and the polymeric copper sulfate iron inorganic composite water purifying agent has the characteristics of simple process, economy, quickness and the like; the obtained water purifying agent has the advantages of high stability, strong adsorption and bridging capacity on colloidal substances, good coagulation effect, strengthened subsequent treatment and the like, and has higher turbidity and removal rate of organic matters and good water treatment effect under the same dosage.
Description
Technical Field
The invention relates to a polymeric copper sulfate iron inorganic composite water purifying agent, a preparation method and application thereof, belonging to the technical field of environment and chemistry.
Background
In order to deal With The problem, copper ions are introduced into The coagulant as Bacteriostatic agents (Michels, h., Moran, w. and Michel, j. (2008) Antimicrobial Properties sewage Surfaces, With a great amount of copper ions, With a great amount of Antimicrobial activity, so that The Bacteriostatic effects of copper ions in The coagulant are not really caused by The inhibition of The release of copper ions in The case of environmental pollution of copper sludge (2+), Zn 6332 (2) and c. and Cao, x. (2012) Antimicrobial effects of copper ions in cement slurries, which are widely used in sewage treatment, sewage sludge treatment, sewage.
Disclosure of Invention
The invention aims to provide a polymeric copper sulfate iron inorganic composite water purifying agent, a preparation method and application thereof.
The invention provides a polymeric copper sulfate iron inorganic composite water purifying agent, which comprises a polymer of copper iron ions, wherein the copper ions are provided by copper sulfate pentahydrate, copper chloride or copper nitrate, and the iron ions are provided by ferric sulfate. The sum of the mass concentration of the effective metal ions of the iron ions and the copper ions is 7.42-12.12g/L, and the molar ratio of the copper ions to the iron ions is 0.02-0.05: 1.
The invention provides a preparation method of the polymeric copper sulfate iron inorganic composite water purifying agent, which comprises the following steps:
(1) dissolving ferric sulfate in deionized water to obtain ferric sulfate solution (the concentration is 0.05-0.25 mol/L);
(2) stirring under the condition of water bath heating, adding a sodium carbonate solution into the ferric sulfate solution obtained in the step (1) to obtain polymeric ferric sulfate, wherein the alkalization degree is 0.5-1.5, and continuously stirring for 24 hours;
(3) preparing a copper ion solution, and adjusting the pH value to be consistent with the polymeric ferric sulfate in the step (2);
(4) preparing 0.5% (volume percentage) of hydrogen peroxide solution, and adjusting the pH value to be consistent with the polymeric ferric sulfate in the step (2);
(5) stirring under the condition of water bath heating, dripping the hydrogen peroxide solution in the step (4) into the polymeric ferric sulfate in the step (2), and sealing and stirring for 30-60 min;
(6) stirring under the condition of water bath heating, slowly dripping the copper sulfate solution in the step (3) into the polymeric ferric sulfate in the step (5) until the molar ratio of copper ions to iron ions is (0.02-0.05: 1), continuously heating until the solution is clear and transparent, and continuously stirring for 24 hours.
Further, steps (2) and (5) also include maintaining the ferric sulfate and polymeric ferric sulfate solution at 30 ~ 65 ℃ by heating in a water bath.
Further, the dropping speed of the sodium carbonate solution in the step (2) is 0.5 ~ 1mL/min, the dropping speed of the hydrogen peroxide solution in the step (5) is 0.5 ~ 1mL/min, and the dropping speed of the copper sulfate in the step (6) is 0.25 ~ 0.5.5 mL/min.
Further, in the step (3), the copper ion solution includes a copper ion solution prepared from copper sulfate pentahydrate, copper chloride or copper nitrate. The concentration of the prepared copper ion solution is 0.05-0.15 mol/L.
Further, the sodium carbonate solution used in the step (2) is 0.05-0.15mol/L, and the dropping time is 75 ~ 250 min.
Further, 0.1mol/L sodium hydroxide solution was used for pH adjustment in the step (3).
Further, the pH is adjusted in the step (4) by using a 0.1mol/L sulfuric acid solution.
Further, the stirring speed was 300 ~ 500 rpm.
The invention provides application of the polymeric copper ferric sulfate inorganic composite water purifying agent, which is characterized in that the polymeric copper ferric sulfate inorganic composite water purifying agent is applied to domestic sewage treatment, the adding amount of the polymeric copper ferric sulfate inorganic composite water purifying agent is 5 ~ 90mg/L, and the applicable pH range is 5.5 ~ 9.
The invention has the beneficial effects that:
(1) the preparation method of the polymeric copper sulfate iron inorganic composite water purifying agent takes ferric sulfate, copper sulfate pentahydrate, hydrogen peroxide and sodium carbonate as raw materials, and is synthesized by a prepolymerization method of adding the sodium carbonate and the copper sulfate into a ferric sulfate solution with a certain proportion for copolymerization, and the polymeric copper sulfate iron inorganic composite water purifying agent has the characteristics of indirect process, economy, rapidness and the like;
(2) the water purifying agent prepared by the method has the advantages of high stability, strong adsorption and bridging capacity on colloidal substances, good coagulation effect, strengthened subsequent treatment and the like, has higher removal rate on turbidity and organic matters under the same dosage, and has good water treatment effect;
(3) copper ions are introduced in the preparation process and used as disinfection factors to reduce the number of microorganisms in the sediment and slow down the release of bottom mud; the low concentration of copper ions in the settled water promotes the nitrification and denitrification reactions.
Detailed Description
As used herein, the singular forms "a", "an", "the" and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise. It will be further understood that the terms "comprises" and/or "comprising," when used in this specification, specify the presence of stated features, integers, steps, and operations, but do not preclude the presence or addition of one or more other features, integers, steps, and operations.
It will be understood by those skilled in the art that, unless otherwise defined, all terms (including 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. It will be further understood that terms, such as those defined in commonly used dictionaries, should be interpreted as having a meaning that is consistent with their meaning in the context of the prior art and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein.
In order to facilitate understanding of the embodiments of the present invention, the following description will be further explained by taking several specific embodiments as examples, and each embodiment is not to be construed as limiting the embodiments of the present invention.
The invention provides a polymeric copper sulfate and iron inorganic composite water purifying agent, which is characterized in that the water purifying agent is an orange red transparent solution, the sum of the mass concentration of effective metal ions of iron ions and copper ions is 7.42-12.12g/L, and the molar ratio of the copper ions to the iron ions is 0.02-0.05.
A preparation method of a polymeric copper sulfate iron inorganic composite water purifying agent is characterized by comprising the following steps:
(1) dissolving ferric sulfate in deionized water to obtain a ferric sulfate solution;
(2) stirring under the condition of water bath heating, slowly dripping a sodium carbonate solution into the ferric sulfate solution obtained in the step (1) to obtain polymeric ferric sulfate, wherein the alkalization degree is 0.5-1.5, and continuously stirring for 24 hours;
(3) dissolving copper sulfate by using deionized water, and adjusting the pH value to be consistent with the polymeric ferric sulfate in the step (2);
(4) preparing 0.5% hydrogen peroxide solution, and adjusting the pH value to be consistent with the polymeric ferric sulfate in the step (2);
(5) stirring under the condition of water bath heating, dripping the hydrogen peroxide solution in the step (4) into the polymeric ferric sulfate in the step (2), and sealing and stirring for 30-60 min.
(6) And (3) strongly stirring under the condition of heating in a water bath, dripping the copper sulfate solution in the step (3) into the polymeric ferric sulfate in the step (2) until the molar ratio of copper ions to iron ions is (0.02-0.05: 1), continuously heating until the solution is clear and transparent, and continuously stirring for 24 hours.
Preferably, the steps (1) and (5) further comprise the step of keeping the ferric sulfate and the polymeric ferric sulfate solution at 30 ~ ℃ by heating in a water bath, preferably, the dropping speed of the sodium carbonate and copper sulfate solution in the steps (1) and (5) is 0.5 ~ mL/min, preferably, the step (3) can be used for preparing copper ion solution by using copper chloride, copper nitrate and the like in addition to copper sulfate pentahydrate, preferably, the alkalization degree in the step (2) is 0.5-1.5, preferably, the sodium carbonate solution used in the step (2) is 0.05-0.15mol/L, preferably, the pH adjusting in the step (3) is 0.1mol/L sodium hydroxide solution, preferably, the pH adjusting in the step (4) is 0.1mol/L sulfuric acid solution, preferably, the step (3) is used for preparing copper sulfate pentahydrate solution, the concentration is 0.05-0.15mol/L, preferably, the pH adjusting in the step (4) is 0.1mol/L sulfuric acid solution, the step (4) is preferably, the step (3) is used for preparing the solution is 0.5) for preparing the inorganic sulfate solution, the concentration is 0.05-0.15mol/L, the adding speed of the inorganic sulfate solution is 300 mg/L, the inorganic sulfate is suitable for the adding speed of the inorganic copper sulfate is 300, and the adding speed of the inorganic copper sulfate is suitable for the inorganic water purifying agent is.
Example 1: preparation method of polymeric ferric sulfate copper inorganic composite water purifying agent
1) 6.00g of ferric sulfate was weighed and dissolved in 150 ml of deionized water to prepare a ferric sulfate solution, which was allowed to stand for 2 hours.
2) Adding 75-225ml of 0.1mol/L sodium carbonate solution into the ferric sulfate solution in the step 1) at the dropping speed of 0.5 ~ 1ml/min under the condition of hot water bath and stirring at 300 ~ 500rpm, and fully stirring for 24h to dissolve the solution to prepare the polymeric ferric sulfate inorganic water purifying agent with the alkalization degree of 0.5-1.5.
3) 2.5g of anhydrous copper sulfate was weighed and dissolved in 100ml of deionized water, and sodium hydroxide was added to adjust the pH to the same pH as that of the polymeric ferric sulfate and the inorganic water purifying agent in step 2).
4) Preparing 0.5 percent hydrogen peroxide, and adding 0.1mol/L sulfuric acid to ensure that the pH value of the hydrogen peroxide is the same as that of the polymeric ferric sulfate and the inorganic water purifying agent in the step 2).
5) Continuously dropwise adding 6-15ml of copper sulfate solution in the step 3) at the dropping speed of 0.5 ~ 1ml/min under the stirring condition of a hot water bath and 300 ~ 500rpm, and continuously stirring for 24 hours at the speed of 300 ~ 500rpm after dropwise adding is finished to obtain the polymeric ferric sulfate copper inorganic composite water purifying agent with the alkalization degree of 0.5-1.5.
Example 2
The polymeric ferric sulfate and polymeric copper ferric sulfate inorganic composite water purifying agent prepared in the embodiment 1 is used for treating a simulated water sample of a certain Ulmus pumila sewage treatment plant, and the treatment steps are as follows:
the water sample preparation method comprises the following steps: adding sucrose 15-30g, soluble starch 15-30g, potassium dihydrogen phosphate 3.44g and ammonium chloride 3.04g, and dissolving in tap water 1L. Dissolving 40g semen glycines powder in 8L tap water, shaking, standing for 10min, and siphoning 2.88L supernatant to 1L tap water to obtain 3.88L new mixture. 3.88L of the mixture was diluted to 40L. And covering a container with 40L of water sample, and standing for 24 hours to obtain a simulated water sample.
Application example 1
The parameters of the simulated water samples used in this experiment are shown in table 1.
TABLE 1 Critical parameters of simulated water samples
The coagulation effect was expressed as the removal rate of turbidity, COD, DON and TN by treating the water sample with Polyferric Copper sulfate (PFCS) and Polyferric sulfate (PFS) having a degree of alkalization of 0.5, and the experimental results are shown in table 2.
TABLE 2 treatment Effect of PFS and PFCS on simulated Water samples
From the experimental results, it is found that the coagulation effect is not greatly affected by the addition of copper sulfate to the polymeric ferric sulfate. The turbidity removal effect is better, which shows that the copper ions also have good coagulation effect, and the turbidity removal effect of the water purifying agent is improved.
Application example 2
The influence of the precipitation generated by two inorganic high molecular water purifying agents PFCS and PFS on the water quality in the optimal dosage range is researched. Soaking equal mass of precipitate in low concentration physiological saline, measuring COD and NH in water at several time points of 0, 6, 12 and 18 hours4-N and NO3The concentration of N, the results of the experiment are shown in Table 3.
TABLE 3 influence of precipitation of PFS and PFCS coagulation on water quality
According to experimental results, the sediment generated by PFCS under a certain dosage can effectively relieve the release of organic matters and nitrogen in sludge, the inhibition rate of the organic matters is 69%, and the inhibition efficiency of the ammonia nitrogen can reach 80%. The release of nitrate nitrogen varies greatly with time, with an inhibition of 62% at 12 hours and a reduction of 30% at 18 hours, which also indicates that the retention time of the sludge resulting from the decontamination of the contaminated water in the pre-separation water treatment system is preferably kept within 12 hours.
Application example 3
Whether PFCS adversely affected the subsequent biological treatment process was investigated. And (3) respectively introducing the raw water sample, the settled water of the PFS and the settled water of the PFCS into three identical aerobic nitrification reactors, wherein the sludge concentration in the reactors is 950mg/L, aerating, keeping the aeration conditions consistent, aerating for 4 hours, detecting ammonia nitrogen in water between the initial time and each hour, and calculating the removal rate. The results of the experiment are shown in table 4.
TABLE 4 nitration reaction vs. NH4Effect of removal of-N
According to the experimental results, two types of water after coagulation and sedimentation are used for NH4The removal rate and the removal efficiency of the-N are higher than those of water which is not subjected to coagulation treatment, and the pre-separation is beneficial to the nitration process. In the reaction time range of this experiment, NH of PFCS-precipitated water was present in the same amount of water-purifying agent4the-N removal rate is obviously higher than that of PFS settled water, and the most obvious change is realized in the first three hours, which shows that some substances remained in the PFCS settled water have some functions of improving the subsequent nitration process.
Application example 4
The water after the nitrification reaction in the above example 3 was subjected to denitrification reaction, and the anaerobic denitrification effect was measured for the raw water sample and the precipitated water of PFS and PFCS, and the whole water treatment was examinedThe removal rate of TN in the process determines whether PFCS will have some negative impact on the denitrification reaction. By calculating all NO3 in water-N and NH4-N to calculate the removal rate of TN. The results of the experiment are shown in Table 5.
TABLE 5 removal efficiency of TN
According to the experimental results, the denitrification effect of the three water samples is obviously different. The same trend for the three samples is that denitrification efficiency increases with time. Then, in almost all experiments, the denitrification efficiency of the settled water is much higher than that of the raw water. Precipitation levels of PFS and PFCS exceeded 75% TN removal in 4 hours. In the comparison of the two types of settled water, the denitrification rate of PFCS settled water is higher than that of PFS settled water, the difference between the two types of settled water is reduced along with the time, the denitrification efficiency of PFCS at 2 hours is 79.44 percent, the denitrification effect of PFS settled water at 4 hours is similar, and the fastest denitrification rate occurs in the first hour of a PFCS coagulation sample. It is almost twice the PFS sample. It then slowly grows. The denitrification rate of PFS increased almost uniformly over the first two hours and then slowly increased at a lower rate. The significant difference in denitrification between PFCS and PFS indicates that the use of PFCS improves the nitrification and denitrification processes, resulting in higher overall nitrogen removal.
In conclusion, the polymeric copper ferric sulfate composite water purifying agent prepared by the method disclosed by the embodiment of the invention can be stably stored for a long time, and has coagulation effect similar to PFS when being used in a water treatment process of pre-separation and biological treatment, and can inhibit bottom sludge generated in the sewage purification process from covering water upwards to release pollutants, improve the purification effect, stimulate microbial activity in the biological treatment and improve the biological reaction efficiency.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (10)
1. A polymeric copper sulfate iron inorganic composite water purifying agent is characterized in that: a polymer comprising copper iron ions, the copper ions being provided by copper sulphate pentahydrate, copper chloride or copper nitrate, the iron ions being provided by iron sulphate; the sum of the mass concentration of the effective metal ions of the iron ions and the copper ions is 7.42-12.12g/L, and the molar ratio of the copper ions to the iron ions is 0.02-0.05: 1.
2. The preparation method of the polymeric copper sulfate iron inorganic composite water purifying agent of claim 1 is characterized by comprising the following steps:
(1) dissolving ferric sulfate in deionized water to obtain a ferric sulfate solution with the concentration of 0.05-0.25 mol/L;
(2) stirring under the condition of water bath heating, adding a sodium carbonate solution into the ferric sulfate solution obtained in the step (1) to obtain polymeric ferric sulfate, wherein the alkalization degree is 0.5-1.5, and continuously stirring for 24 hours;
(3) preparing a copper ion solution, and adjusting the pH value to be consistent with the polymeric ferric sulfate in the step (2);
(4) preparing a hydrogen peroxide solution with the volume percentage of 0.5%, and adjusting the pH value to be consistent with the polymeric ferric sulfate in the step (2);
(5) stirring under the condition of water bath heating, dripping the hydrogen peroxide solution in the step (4) into the polymeric ferric sulfate in the step (2), and sealing and stirring for 30-60 min;
(6) stirring under the condition of water bath heating, slowly dripping the copper sulfate solution in the step (3) into the polymeric ferric sulfate in the step (5) until the molar ratio of copper ions to iron ions is 0.02-0.05: 1, continuously heating until the solution is clear and transparent, and continuously stirring for 24 hours.
3. The method for preparing the polymeric copper sulfate iron inorganic composite water purifying agent according to claim 2, wherein in the steps (2) and (5), the temperature is maintained at 30 ~ 65 ℃ by heating in water bath.
4. The preparation method of the polymeric copper sulfate iron inorganic composite water purifying agent according to claim 2, wherein the dropping speed of the sodium carbonate solution in the step (2) is 0.5 ~ 1 mL/min;
in the step (5), the dropping speed of the hydrogen peroxide solution is 0.5 ~ 1 mL/min;
the dropping speed of the copper sulfate in the step (6) is 0.25 ~ 0.5.5 mL/min.
5. The method for preparing the polymeric copper sulfate iron inorganic composite water purifying agent according to claim 2, characterized in that: in the step (3), the copper ion solution comprises a copper ion solution prepared from copper sulfate pentahydrate, copper chloride or copper nitrate; the concentration of the prepared copper ion solution is 0.05-0.15 mol/L.
6. The method for preparing the polymeric copper sulfate iron inorganic composite water purifying agent according to claim 2, characterized in that the sodium carbonate solution in the step (2) is 0.05-0.15mol/L, and the dropping time is 75 ~ 250 min.
7. The method for preparing the polymeric copper sulfate iron inorganic composite water purifying agent according to claim 2, characterized in that: in the step (3), 0.1mol/L sodium hydroxide solution was used for pH adjustment.
8. The method for preparing the polymeric copper sulfate iron inorganic composite water purifying agent according to claim 2, characterized in that: in the step (4), a 0.1mol/L sulfuric acid solution is used for adjusting the pH.
9. The method for preparing the polymeric copper sulfate and iron inorganic composite water purifying agent according to claim 2, wherein the stirring speed is 300 ~ 500rpm during the stirring process.
10. The use of the polymeric copper iron sulfate inorganic composite water purifying agent of claim 1 in domestic sewage treatment, wherein the polymeric copper iron sulfate inorganic composite water purifying agent is added in an amount of 5 ~ 90mg/L, and the applicable pH range is 5.5 ~ 9.
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| CN1174177A (en) * | 1996-08-21 | 1998-02-25 | 王全永 | Compound aluminium silicate polymer water purifying agent |
| CN101274780A (en) * | 2008-05-19 | 2008-10-01 | 山西大学 | Polymeric ferric polysulfate composite coagulant and application thereof |
| CN102583672A (en) * | 2012-02-21 | 2012-07-18 | 湖南海利化工股份有限公司 | Polysilicate ferro-copper sulfate composite with wastewater deodorizing and flocculating function and preparation method thereof |
| CN104692510A (en) * | 2015-04-02 | 2015-06-10 | 湖南科技大学 | Preparation method for solid polymer ferric sulfate zinc flocculant |
| CN108996634A (en) * | 2018-07-24 | 2018-12-14 | 河南工程学院 | It is a kind of for handling the preparation method of the polymeric ferric sulfate flocculant of waste water from dyestuff |
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2019
- 2019-10-16 CN CN201910981423.9A patent/CN110723774A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1174177A (en) * | 1996-08-21 | 1998-02-25 | 王全永 | Compound aluminium silicate polymer water purifying agent |
| CN101274780A (en) * | 2008-05-19 | 2008-10-01 | 山西大学 | Polymeric ferric polysulfate composite coagulant and application thereof |
| CN102583672A (en) * | 2012-02-21 | 2012-07-18 | 湖南海利化工股份有限公司 | Polysilicate ferro-copper sulfate composite with wastewater deodorizing and flocculating function and preparation method thereof |
| CN104692510A (en) * | 2015-04-02 | 2015-06-10 | 湖南科技大学 | Preparation method for solid polymer ferric sulfate zinc flocculant |
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