CN110040825B - Method for preparing solid rare earth lanthanum modified polymeric ferric sulfate by one-step method - Google Patents
Method for preparing solid rare earth lanthanum modified polymeric ferric sulfate by one-step method Download PDFInfo
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- CN110040825B CN110040825B CN201910264542.2A CN201910264542A CN110040825B CN 110040825 B CN110040825 B CN 110040825B CN 201910264542 A CN201910264542 A CN 201910264542A CN 110040825 B CN110040825 B CN 110040825B
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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
- C02F1/52—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
- C02F1/5245—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents using basic salts, e.g. of aluminium and iron
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Abstract
The invention disclosesA method for preparing solid rare earth lanthanum modified polymeric ferric sulfate by a one-step method is provided. The method comprises the following steps: mixing Melanteritum and oxidant powder at a mass ratio of 0.15-0.20:1, adding water to stir the powder into paste, stirring for a period of time, heating for 30-60 min, uniformly spraying high-concentration sulfuric acid, and adding La-containing solution3+After the medicament powder is fully stirred, adding alkalizer powder, fully stirring, transferring to normal temperature and normal pressure, and aging to obtain a product; wherein the molar ratio of sulfur to iron of the copperas is 1.0-1.5: 1, according to Fe and La3+The molar ratio is 80-120: 1 adding La-containing3+In the amount of the pharmaceutical powder of (1), in terms of OH‑The molar ratio of the powder to Fe is 0.1-0.3: 1. The solid product prepared by the one-step method has low production cost, is convenient to transport and store, and has obvious turbidity removal effect.
Description
Technical Field
The invention relates to the technical field of flocculating agents, in particular to a method for preparing solid rare earth lanthanum modified polymeric ferric sulfate by a one-step method.
Background
In the world of China, rare earth is also used in the field of wastewater treatment in the development of the world nowadays. In view of the specific properties of rare earths themselves, rare earths are playing an increasingly important role in water treatment.
The rare earth composite flocculant (PAC-RE) is prepared by recording that the rare earth chloride, aluminum powder and aluminum chloride are used as raw materials in the preparation and flocculation performance research of rare earth composite flocculant (Schjia, Wang Ruifen and Sunzhong-Zhou rare earth composite flocculant, No. 2 of rare earth volume 34, article number: 1004-.
The research on the preparation of the polymeric flocculant from the rare earth cerium modified industrial waste, namely Li Shang comments, Yang Wei, Pajing and Wang Jun, which is compiled in the first environmental forum paper (abstract) of Chinese scientists all over the world, describes that Li Shang comments and the like take blast furnace gas ash and aluminum smelting ash residues as raw materials, and rare earth cerium is added for modification to prepare the inorganic polymeric flocculant (RE-PAFC).
The preparation of rare earth lanthanum modified self-made aluminum-iron sulfate flocculant and application thereof in soy sauce wastewater treatment, a master academic paper of Shandong university, namely, the preparation of rare earth lanthanum modified self-made aluminum-iron sulfate flocculant by Parajing is described, but the rare earth lanthanum modified self-made aluminum-iron sulfate flocculant belongs to an aluminum-containing flocculant, part of aluminum ions are toxic, the preparation method is complex, different effects are different according to the preparation method, and the prepared liquid flocculant is not easy to store and transport, and the atomization, evaporation and drying costs are high.
Disclosure of Invention
Aiming at the problems, the invention aims to overcome the limitation of the traditional technology for preparing the liquid rare earth modified flocculating agent, prepare the flocculating agent of the rare earth lanthanum modified polyferric sulfate by a simple one-step method, have low production cost, do not need energy consumption, evaporation and drying on liquid products, facilitate transportation and storage of solid products and have obvious turbidity removal effect.
To achieve these objects and other advantages in accordance with the present invention, a method for preparing solid rare earth lanthanum-modified polymeric ferric sulfate in a "one-step" manner, comprises the steps of:
uniformly mixing the copperas and the oxidant powder according to the mass ratio of 0.15-0.20:1, then adding a small amount of water to perform oxidation reaction to make the reactant present a mud-like substance, ensuring that an aqueous medium participates in the reaction, stirring for 20-35 minutes, fully stirring to enable the reagent to uniformly contact, improving the reaction effect, then heating to 100 ℃ and 150 ℃, uniformly spraying sulfuric acid with the mass concentration of 90-98% after 30-60 minutes, and simultaneously adding La-containing sulfuric acid3+The medicament powder is fully stirred for 20-30 minutes, then the viscous reactant is added, alkalizer powder is fully stirred for 20-35 minutes, all substances in the mixed reaction are transferred to normal temperature and normal pressure, and aging is carried out for 36-48 hours to obtain a light yellow solid particle product, wherein the aging aims to evaporate redundant moisture in the product by utilizing waste heat, and finally the light yellow solid particle product with the moisture content of less than 15% is obtained;
wherein the molar ratio of sulfur to iron of the copperas is 1.0-1.5: 1, according to Fe and La3+The molar ratio is 80-120: 1 adding La-containing3+The amount of the medicament powder of (4) is the amount of the alkalizer powder added according to the molar ratio of OH < - > to Fe of 0.1-0.3: 1.
Preferably, the copperas is obtained by drying the byproduct copperas at the temperature of 100-110 ℃ for 60-90 minutes and then grinding. Thus, the adsorption water, crystallization dehydration or structure dehydration on the surface of the byproduct copperas can be removed, and the product quality is improved.
Preferably, the sulfuric acid is added in an atomized spray manner. Therefore, the solid and the liquid can be mixed more uniformly and contacted uniformly, and the reaction effect is improved.
Preferably, the oxidant is one or both of potassium chlorate and sodium chlorate.
Preferably, the La-containing3+The medicament of (1) is one of lanthanum chloride or lanthanum nitrate.
Preferably, the alkalizer is one or more of sodium hydroxide, calcium hydroxide, sodium bicarbonate or potassium bicarbonate.
Preferably, the amount of water added is 0.3 to 0.4 times the mass of the whole powdery raw material. The adding amount of water is determined according to the quality of raw materials, so that the powder is preferably in a mud state, namely, a small amount of water medium is ensured to participate in the hydrolytic polymerization reaction in the reaction, and the reactant is in a sticky state.
Preferably, the reaction process in the method is carried out in a reactor.
The invention at least comprises the following beneficial effects:
firstly, the flocculant for preparing the solid rare earth lanthanum modified polyferric sulfate by the simple one-step method has a technical process different from the conventional liquid-liquid reaction environment, and the final product in the conventional process is changed from liquid to solid, so that certain energy is consumed, and the operation is complicated; in the process, the addition of water is strictly controlled, only the participation of an aqueous medium in the reaction is required to be ensured, the reaction environment for preparing the aqueous solution is not required, and in the reaction process of the product, certain reaction temperature and waste heat are utilized to ensure that the water content of the final product is lower than 15 percent, thereby simplifying the steps of the production process, reducing the energy consumption and facilitating the transportation and the storage.
Secondly, compared with similar rare earth modified flocculating agents prepared by other processes, the turbidity removal effect is obvious under the same condition. Although the turbidity removal rate of the rare earth polymeric aluminum ferric sulfate product obtained by adopting rare earth lanthanum through a complex preparation method is improved by about 10% and reaches 95% at most, the precipitation time is long, and the turbidity removal rate is only about 45% in 10 min. The turbidity removal effect of the solid rare earth lanthanum modified polyferric sulfate product prepared by the simple method is over 95 percent, the turbidity removal can be carried out in a short time, and can reach 95 percent within 10min, and the method has the advantages of low preparation cost, convenient transportation and storage, high turbidity removal speed, high efficiency and the like.
Detailed Description
The present invention is described in further detail below to enable those skilled in the art to practice the invention with reference to the description.
Example 1
Drying the byproduct copperas at the temperature of 100 ℃ for 60 minutes, grinding to obtain copperas, putting the copperas into a reactor, adding potassium chlorate powder, adding water with the amount being approximately 0.4 times of the mass of all powder raw materials, enabling the reactant to be in a mud shape, uniformly stirring and reacting for 30 minutes, heating to 130 ℃, and after 60 minutes, mixing the mixture according to the molar ratio of sulfuric acid to sulfur and iron of the copperas of 1.3: 1 gradually adding sulfuric acid into the mixture in a uniform atomizing and jet mode, and simultaneously adding Fe and La into the mixture3+Adding lanthanum chloride powder with the molar ratio of 100:1, fully stirring for 30 minutes, then adding sodium hydroxide powder, fully stirring for 30 minutes to adjust the OH-/Fe ratio of the flocculant, then transferring all substances obtained in the mixing reaction to an indoor environment at normal temperature and normal pressure, and curingAfter about 48 hours, a light yellow solid granular product with the water content of 13 percent is obtained. Wherein the mass concentration of the sulfuric acid is 95 percent, the mass ratio of the copperas to the potassium chlorate powder is 0.17:1, and the amount of the sodium hydroxide powder is added according to the molar ratio of OH < - > to Fe of 0.1: 1.
Example 2
Uniformly mixing the copperas and the sodium chlorate powder according to the mass ratio of 0.2:1, adding water in an amount which is about 0.3 time of the mass of all powder raw materials to enable a reactant to be in a mud shape, stirring and reacting for 35 minutes, heating to 150 ℃, uniformly spraying sulfuric acid with the mass concentration of 98 percent after 60 minutes, simultaneously adding lanthanum nitrate powder, fully stirring for 30 minutes, adding calcium hydroxide powder, fully stirring for 35 minutes, completely transferring all substances subjected to mixed reaction to a room at normal temperature and normal pressure, and aging for 36 hours to obtain a light yellow solid particle product with the water content of 14 percent;
wherein the molar ratio of sulfur to iron of the copperas is 1.5: 1, according to Fe and La3+The molar ratio is 120: 1 adding lanthanum nitrate powder, and adding calcium hydroxide powder according to the molar ratio of OH < - > to Fe of 0.3: 1.
Example 3
Uniformly mixing the copperas and the potassium chlorate powder according to the mass ratio of 0.15:1, adding water with the amount approximately 0.3 time of the mass of all powder raw materials to enable the reactant to be in a mud shape, stirring and reacting for 20 minutes, heating to 100 ℃, uniformly spraying sulfuric acid with the mass concentration of 90% after 30 minutes, simultaneously adding lanthanum chloride powder, fully stirring for 20 minutes, adding sodium hydroxide powder, fully stirring for 20 minutes, completely transferring all substances subjected to mixed reaction to normal temperature and normal pressure, and aging for 48 hours to obtain a light yellow solid particle product with the water content of 12%;
wherein the molar ratio of sulfur to iron of the copperas is 1.0: 1, according to Fe and La3+The molar ratio is 80: 1 amount of lanthanum chloride powder added, and an amount of sodium hydroxide powder added in a molar ratio of OH "to Fe of 0.1: 1.
The product performance of the solid flocculant prepared by the invention is compared with the product performance of the solid flocculant prepared by the invention in the national standard GB/T14591-2016, and the product performance is as follows in the comparison table 1:
TABLE 1
| Performance index | Example 1 | Example 2 | Example 3 | GB/T14591-2016 |
| Degree of basicity (%) | 13.1558 | 13.1198 | 13.1354 | 5.0—20.0 |
| Total iron content (%) | 20.2643 | 20.1355 | 20.1068 | Greater than or equal to 19.5 |
| Reduced matter mass fraction (%) | 0.0105 | 0.0103 | 0.0137 | Less than or equal to 0.15 |
| pH value (10g/L, aqueous solution) | 2.4 | 2.3 | 2.4 | 1.5—3.0 |
The inventors carried out the following test experiments:
experiment 1
The experimental method comprises the following steps: taking the flood turbidity of about 1300NTU as a water sample during rainstorm, wherein the adding amount of the flocculating agent is 250 mg/L. The method specifically comprises the following steps: putting 500mL of flood water sample into a beaker, adding 250mg/L of flocculant into the beaker, and starting a stirrer to quickly stir for 30s at 300 r/min; stirring at a medium speed of 150r/min for 5 min; stirring at a low speed of 70r/min for 10min, standing for precipitation for 10-30min, taking supernatant liquid 2-3 cm below the liquid surface, measuring residual turbidity, and calculating the turbidity removal rate.
The preparation method of the comparative product 1 is similar to that of example 1, except that the order of adding lanthanum chloride powder is different, and the lanthanum chloride powder is added at last, specifically: drying the byproduct copperas at the temperature of 100 ℃ for 60 minutes, grinding to obtain copperas, putting the copperas into a reactor, adding potassium chlorate powder, uniformly stirring, reacting for 30 minutes, heating to 130 ℃, and after 60 minutes, mixing the mixture according to the molar ratio of sulfuric acid to copperas of 1.3: 1 gradually and uniformly adding sulfuric acid in an atomizing and jet flow manner, fully stirring for 30 minutes, then adding sodium hydroxide powder, fully stirring for 30 minutes to adjust the OH-/Fe ratio of the flocculant, and then according to the Fe and La3+Lanthanum chloride powder was added at a molar ratio of 100:1, and then the above mixed reaction mass was all transferred to normal temperature and pressure and aged for about 48 hours to obtain comparative product 1 as pale yellow solid particles, wherein the mass concentration of sulfuric acid was 98%, the mass ratio of copperas to potassium chlorate powder was 0.17:1, and the amount of sodium hydroxide powder was added at a molar ratio of OH "to Fe of 0.1: 1.
Lanthanum chloride powder is not added in the preparation process of the comparative product 2, the steps and the reaction conditions are slightly different from those of the example 1, other raw materials and the use amount are the same as those of the example 1, and the comparative product 2 prepared is polyferric sulfate (PFS). The method specifically comprises the following steps: drying the byproduct copperas at the temperature of 100 ℃ for 60 minutes, grinding to obtain copperas, putting the copperas into a microwave stirrer, controlling the temperature at the temperature of 80 ℃ and normal pressure, adding 95% sulfuric acid in an atomizing and jet flow manner, stirring uniformly while adding, wherein the molar ratio of the added sulfuric acid to the sulfur and the iron of the copperas is 1.3: 1, sequentially adding potassium chlorate powder and sodium hydroxide powder, and fully stirring every time one reagent is added to obtain a mixture; wherein the mass ratio of the copperas to the potassium chlorate powder is 0.17:1, and the amount of the sodium hydroxide powder is added according to the molar ratio of OH < - > to Fe of 0.1: 1; the mixture was transferred to a reactor at 130 ℃ under normal pressure, and the polymerization was continued for 30 minutes while stirring, and the mixture was taken out of the reactor and aged at normal temperature and normal pressure for 48 hours to obtain comparative product 2(PFS) as pale yellow solid particles.
The flocculants used in the experimental method were the flocculants prepared in comparative product 1, comparative product 2, inventive example 1, inventive example 2 and inventive example 3, respectively, and the flocculation turbidity removal ratio is shown in table 2.
Table 2 (flocculant dosage is 250mg/L, 500mL water sample, operating conditions are the same)
The experimental data in table 2 show that when water samples with the same properties are treated by the same experimental method, the solid rare earth lanthanum modified polyferric sulfate (La-PFS) flocculant prepared by the one-step method with solid raw materials has the advantages of high turbidity removal speed, high turbidity removal rate, simple preparation method, low production cost for preparing the solid (La-PFS) flocculant by the one-step method, and convenience in transportation and storage. Because the synthesis conditions and steps of the rare earth lanthanum modified self-made aluminum-iron flocculant are too complex and inconvenient to operate and the like are recorded in documents of the prior art (the preparation of the rare earth lanthanum modified self-made aluminum-iron flocculant and the application thereof in the treatment of soy sauce wastewater, the university of Shandong, a academic thesis) and the like, the inventor fails to prepare a rare earth lanthanum modified self-made aluminum-iron flocculant product in the prior art (the preparation of the rare earth lanthanum modified self-made aluminum-iron flocculant and the application thereof in the treatment of soy sauce wastewater after many attempts, but shown in fig. 5-4 on page 51 in the documents (the preparation of the rare earth lanthanum modified self-made aluminum-iron flocculant and the application thereof in the treatment of soy sauce wastewater, the university of Shandong, the academic thesis) records of performances at that although the turbidity removal rate of the rare earth polymerized aluminum-iron sulfate product obtained by adopting rare earth lanthanum through a complex preparation method is improved by about 10 percent and reaches 95 percent at most, the precipitation time is long, the turbidity removal rate is only about 45% in 10min, the highest turbidity removal rate of 95% is achieved only when the mixture is kept standing and precipitating for 35min, and the advantages of the invention on the turbidity removal effect and the preparation method are not achieved. The turbidity removal effect of the solid rare earth lanthanum modified polyferric sulfate product prepared by the simple method reaches over 95 percent when the product is kept standing and precipitated for 10min, the turbidity removal speed is high, the efficiency is high, the solid product is prepared by a one-step method, the production cost is low, and the transportation and the storage are convenient.
While embodiments of the invention have been described above, it is not limited to the applications set forth in the description and the embodiments, which are fully applicable to various fields of endeavor for which the invention may be embodied with additional modifications as would be readily apparent to those skilled in the art, and the invention is therefore not limited to the details given herein and to the embodiments shown and described without departing from the generic concept as defined by the claims and their equivalents.
Claims (7)
1. The method for preparing the solid rare earth lanthanum modified polyferric sulfate by the one-step method is characterized by comprising the following steps:
uniformly mixing the copperas and the oxidant powder according to the mass ratio of 0.15-0.20:1, adding water to stir the powder into a mud-like substance, stirring and reacting for 20-35 minutes, then heating to 100 ℃ and 150 ℃, uniformly spraying sulfuric acid with the mass concentration of 90-98 percent after 30-60 minutes, and simultaneously adding La-containing sulfuric acid3+Fully stirring the medicament powder for 20-30 minutes, adding alkalizer powder, fully stirring for 20-35 minutes, transferring all substances subjected to mixed reaction to normal temperature and normal pressure, and aging for 36-48 hours to finally obtain a light yellow solid particle product with the water content of less than 15%;
wherein the molar ratio of sulfur to iron of the copperas is 1.0-1.5: 1, according to Fe and La3+The molar ratio is 80-120: 1 adding La-containing3+In the amount of the pharmaceutical powder of (1), in terms of OH-The molar ratio of Fe to alkalizer is 0.1-0.3:1, adding an amount of alkalizer powder, and oxidizingThe agent is one or two of potassium chlorate or sodium chlorate.
2. The method for preparing solid polymerized ferric sulfate modified by lanthana by the one-step method as claimed in claim 1, wherein the copperas is prepared by drying the byproduct copperas at 100-110 ℃ for 60-90 minutes and grinding.
3. The method for preparing the solid rare earth lanthanum modified polyferric sulfate by the one-step method according to the claim 1 or 2, characterized in that the adding mode of the sulfuric acid is atomized jet flow type adding.
4. The method for preparing solid rare earth lanthanum modified polyferric sulfate according to the one-step method of claim 3, wherein the La-containing polyferric sulfate is prepared by the one-step method3+The medicament of (1) is one of lanthanum chloride or lanthanum nitrate.
5. The method for preparing solid rare earth lanthanum modified polyferric sulfate according to the claim 4, wherein the alkalizer is one or more of sodium hydroxide, calcium hydroxide, sodium bicarbonate or potassium bicarbonate.
6. The method for preparing the solid rare earth lanthanum modified polyferric sulfate by the one-step method according to any one of claims 1 or 2 or 4 to 5, wherein the amount of the added water is 0.3 to 0.4 times of the mass of the whole powder raw material.
7. The method for preparing the solid rare earth lanthanum modified polyferric sulfate by the one-step method according to any one of claims 1, 2 or 4 to 5, wherein the reaction process is carried out in a reactor.
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| CN1219507A (en) * | 1997-12-08 | 1999-06-16 | 孙志坚 | One-step production technique for ferric polysulfate solid water purifier |
| CN103449535A (en) * | 2013-08-30 | 2013-12-18 | 白占卿 | Production method for solid polyferric sulphate |
| CN103803662B (en) * | 2013-12-19 | 2015-10-14 | 广西大学 | A kind of method utilizing oxidation bauxite to prepare solid polymeric aluminum ferric sulfate |
| CN105800749A (en) * | 2014-12-30 | 2016-07-27 | 王建国 | Preparation method for solid polymer ferric sulfate flocculating agent |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO1995023765A1 (en) * | 1994-03-04 | 1995-09-08 | Imperial College Of Science, Technology & Medicine | Preparations and uses of polyferric sulphate |
| CN1219507A (en) * | 1997-12-08 | 1999-06-16 | 孙志坚 | One-step production technique for ferric polysulfate solid water purifier |
| CN103449535A (en) * | 2013-08-30 | 2013-12-18 | 白占卿 | Production method for solid polyferric sulphate |
| CN103803662B (en) * | 2013-12-19 | 2015-10-14 | 广西大学 | A kind of method utilizing oxidation bauxite to prepare solid polymeric aluminum ferric sulfate |
| CN105800749A (en) * | 2014-12-30 | 2016-07-27 | 王建国 | Preparation method for solid polymer ferric sulfate flocculating agent |
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