CN113968605B - Preparation method of sewage flocculant polyaluminium chloride - Google Patents
Preparation method of sewage flocculant polyaluminium chloride Download PDFInfo
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- CN113968605B CN113968605B CN202010644199.7A CN202010644199A CN113968605B CN 113968605 B CN113968605 B CN 113968605B CN 202010644199 A CN202010644199 A CN 202010644199A CN 113968605 B CN113968605 B CN 113968605B
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- mixed solution
- flocculant
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/48—Halides, with or without other cations besides aluminium
- C01F7/56—Chlorides
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Geology (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The invention belongs to the technical field of chemical materials, and relates to a preparation method of sewage flocculant polyaluminium chloride, which comprises the following steps: step one, dissolving a nonionic surfactant P123 and aluminum isopropoxide in an ethanol solution to obtain a mixed solution I; step two, adding concentrated hydrochloric acid solution into the mixed solution I, and stirring vigorously in air; step three, stirring until a uniform mixed solution is obtained, and obtaining a mixed solution II; and fourthly, placing the mixed solution II in a constant-temperature drying oven, and obtaining white solid powder after the solvent is completely volatilized, namely the prepared polyaluminum chloride flocculant. The preparation method is simple, the operation is easy, the reaction condition is mild, and the aluminum oxide obtained after being burned has high specific surface area, ordered mesoporous pore canal and even particle distribution, and has higher application prospect.
Description
Technical Field
The invention belongs to the technical field of chemical materials, and relates to a preparation method of sewage flocculant polyaluminium chloride.
Background
The environmental protection directly affects the sustainable development of national economy in China. With the rapid increase of the discharge amount of industrial sewage and domestic sewage, the water treatment problem is increasingly prominent, and flocculation technology is widely regarded as a widely used and low-cost treatment technology, which can greatly improve the water treatment efficiency, and one of the most critical problems is the selection and preparation process of flocculant.
In the water treatment process, the wastewater contains not only silt, macromolecular particles and the like, but also dust, humus, starch, cellulose, bacteria and the like with small particle sizes, and the substances are often in a sol state with water, and present sedimentation and polymerization stability, and cannot be removed by a gravity natural sedimentation method, so that a flocculating agent is required to be added. The flocculant is used as an important means for water treatment, has the advantages of wide application range, low price, simple and convenient operation and the like, so that the flocculant can be added in a plurality of water pollution treatment processes to improve the pollutant removal efficiency, thereby achieving the aim of reaching the standard of the water body.
The polyaluminium chloride has excellent bridging adsorption performance, high adsorption and catalytic activity, small dosage and high flocculation speed, and the hydrolysis process is complex and is often accompanied with electrochemical, condensation, adsorption, precipitation and other physical and chemical engineering, so that the polyaluminium chloride has wide application range, such as pharmaceutical wastewater, electroplating wastewater and the like, and can synchronously remove heavy metals, fluorides, oil and other substances in water. The polyaluminium chloride for industrial water treatment in China is produced by a one-step method of acid-soluble aluminum ash, and the polyaluminium chloride produced by the method has high impurity content and low active ingredients. Therefore, the development of the polychlorinated flocculant with higher efficiency, simpler and cleaner process has very important practical significance.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of sewage flocculant polyaluminium chloride, which is characterized by simple equipment, easy operation, less impurity of products, high content of active ingredients and better flocculation effect.
The technical scheme adopted for solving the technical problems is as follows: a preparation method of sewage flocculant polyaluminium chloride comprises the following steps:
step one, dissolving a nonionic surfactant P123 and aluminum isopropoxide in an ethanol solution to obtain a mixed solution I;
step two, adding concentrated hydrochloric acid solution into the mixed solution I obtained in the step one, and stirring vigorously in air;
step three, stirring until a uniform mixed solution is obtained, and obtaining a mixed solution II;
and fourthly, placing the mixed solution II in a constant-temperature drying oven, and obtaining white solid powder after the solvent is completely volatilized, namely the prepared polyaluminum chloride flocculant.
Preferably, the nonionic surfactant P123 is used in the amount of 0.0001 to 0.0006mol in the step one; the dosage of the aluminum isopropoxide in the first step is 3-5 g.
More preferably, the amount of the nonionic surfactant P123 used in the first step is 0.0001mol, 0.0002mol, 0.0003mol and 0.0006mol; the amount of aluminum isopropoxide dissolved in the first step was 4 g.
Preferably, the concentrated hydrochloric acid solution in the second step is used in an amount of 1-4mL.
More preferably, the concentrated hydrochloric acid solution in the second step is used in an amount of 1mL, 2mL, 3mL and 4mL.
Preferably, the temperature of the constant temperature drying oven in the fourth step is set to be 60 ℃.
The beneficial effects of the invention are as follows:
1. according to the invention, the polyaluminum chloride flocculant is synthesized by adopting a one-step method, the synthesized sample has high purity, the synthesis method is simple and easy to operate, and the reaction conditions are mild.
2. The sample obtained by the invention is burned to obtain Al 2 O 3 Has a larger specific surface area (426 m 2 Per g), pore volume (0.60 cm 3 /g), pore size (5.75 nm).
Drawings
FIG. 1 is a diagram of Al after polyaluminium chloride calcination 2 O 3 X-ray diffraction pattern of the powder;
FIG. 2 shows Al after firing of polyaluminium chloride 2 O 3 Nitrogen adsorption and desorption curve graph of powder;
FIG. 3 shows Al after firing of polyaluminium chloride 2 O 3 Transmission electron microscopy of the powder.
Detailed Description
The following description of the related art will be made apparent to, and is not intended to limit the scope of, the embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Referring to fig. 1-3, a method for preparing sewage flocculant polyaluminum chloride comprises the following steps:
step one, dissolving a nonionic surfactant P123 and aluminum isopropoxide in an ethanol solution to obtain a mixed solution I;
step two, adding concentrated hydrochloric acid solution into the mixed solution I obtained in the step one, and stirring vigorously in air;
step three, stirring until a uniform mixed solution is obtained, and obtaining a mixed solution II;
and fourthly, placing the mixed solution II in a constant-temperature drying oven, and obtaining white solid powder after the solvent is completely volatilized, namely the prepared polyaluminum chloride flocculant.
Further, the amount of the nonionic surfactant P123 used in the first step is 0.0001 to 0.0006mol; the dosage of the aluminum isopropoxide in the first step is 3-5 g.
Further, the amount of the nonionic surfactant P123 used in the first step is 0.0001mol, 0.0002mol, 0.0003mol and 0.0006mol; the amount of aluminum isopropoxide dissolved in the first step was 4 g.
Further, the dosage of the concentrated hydrochloric acid solution in the second step is 1-4mL.
Further, the concentrated hydrochloric acid solution in the second step is used in an amount of 1mL, 2mL, 3mL and 4mL.
Further, the temperature of the constant temperature drying oven in the fourth step is set to be 60 ℃.
Embodiment one:
a. 0.0002mol of nonionic surfactant (P123) and 4g of aluminum isopropoxide were dissolved in an ethanol solution;
b. adding 1mL of concentrated hydrochloric acid solution into the mixed solution obtained in the previous step, and stirring vigorously in air;
c. until a uniform mixed solution is obtained;
d. placing the uniformly stirred mixed solution in a constant-temperature drying oven at 60 ℃, and obtaining white solid powder after the solvent is completely volatilized, namely the prepared polyaluminum chloride flocculant;
e. the white solid powder is placed in a muffle furnace to be roasted for 4 hours at 500 ℃ to obtain Al 2 O 3 And (3) a sample.
Embodiment two:
a. 0.0003mol of nonionic surfactant (P123) and 4g of aluminum isopropoxide were dissolved in an ethanol solution;
b. adding 1mL of concentrated hydrochloric acid solution into the mixed solution obtained in the previous step, and stirring vigorously in air;
c. until a uniform mixed solution is obtained;
d. placing the uniformly stirred mixed solution in a constant-temperature drying oven at 60 ℃, and obtaining white solid powder after the solvent is completely volatilized, namely the prepared polyaluminum chloride flocculant;
e. the white solid powder is placed in a muffle furnace to be roasted for 4 hours at 500 ℃ to obtain Al 2 O 3 And (3) a sample.
Embodiment III:
a. 0.0006mol of nonionic surfactant (P123) and 4g of aluminum isopropoxide were dissolved in an ethanol solution;
b. adding 1mL of concentrated hydrochloric acid solution into the mixed solution obtained in the previous step, and stirring vigorously in air;
c. until a uniform mixed solution is obtained;
d. placing the uniformly stirred mixed solution in a constant-temperature drying oven at 60 ℃, and obtaining white solid powder after the solvent is completely volatilized, namely the prepared polyaluminum chloride flocculant;
e. the white solid powder is placed in a muffle furnace to be roasted for 4 hours at 500 ℃ to obtain Al 2 O 3 And (3) a sample.
Embodiment four:
a. 0.0002mol of nonionic surfactant (P123) and 4g of aluminum isopropoxide were dissolved in an ethanol solution;
b. adding 2mL of concentrated hydrochloric acid solution into the mixed solution obtained in the previous step, and stirring vigorously in air;
c. until a uniform mixed solution is obtained;
d. placing the uniformly stirred mixed solution in a constant-temperature drying oven at 60 ℃, and obtaining white solid powder after the solvent is completely volatilized, namely the prepared polyaluminum chloride flocculant;
e. the white solid powder is placed in a muffle furnace to be roasted for 4 hours at 500 ℃ to obtain Al 2 O 3 And (3) a sample.
Fifth embodiment:
a. 0.0002mol of nonionic surfactant (P123) and 4g of aluminum isopropoxide were dissolved in an ethanol solution;
b. adding 3mL of concentrated hydrochloric acid solution into the mixed solution obtained in the previous step, and stirring vigorously in air;
c. until a uniform mixed solution is obtained;
d. placing the uniformly stirred mixed solution in a constant-temperature drying oven at 60 ℃, and obtaining white solid powder after the solvent is completely volatilized, namely the prepared polyaluminum chloride flocculant;
e. the white solid powder is placed in a muffle furnace to be roasted for 4 hours at 500 ℃ to obtain Al 2 O 3 And (3) a sample.
Example six:
a. 0.0002mol of nonionic surfactant (P123) and 4g of aluminum isopropoxide were dissolved in an ethanol solution;
b. adding 4mL of concentrated hydrochloric acid solution into the mixed solution obtained in the previous step, and stirring vigorously in air;
c. until a uniform mixed solution is obtained;
d. placing the uniformly stirred mixed solution in a constant-temperature drying oven at 60 ℃, and obtaining white solid powder after the solvent is completely volatilized, namely the prepared polyaluminum chloride flocculant;
e. the white solid powder is placed in a muffle furnace to be roasted for 4 hours at 500 ℃ to obtain Al 2 O 3 And (3) a sample.
Comparing the samples obtained in examples one to six, table 1 is obtained:
table 1 comparison of results for six sets of examples
In summary, the invention provides a preparation method of sewage flocculant polyaluminium chloride, which has the advantages of simple preparation method, easy operation and mild reaction conditions, and the sintered aluminum oxide has high specific surface area, ordered mesoporous channels, uniform particle distribution and higher application prospect.
It is emphasized that: the above embodiments are merely preferred embodiments of the present invention, and the present invention is not limited in any way, and any simple modification, equivalent variation and modification made to the above embodiments according to the technical substance of the present invention still fall within the scope of the technical solution of the present invention.
Claims (5)
1. The preparation method of the sewage flocculant polyaluminium chloride is characterized by comprising the following steps:
step one, dissolving a nonionic surfactant P123 and aluminum isopropoxide in an ethanol solution to obtain a mixed solution I;
step two, adding concentrated hydrochloric acid solution into the mixed solution I obtained in the step one, and stirring vigorously in air;
step three, stirring until a uniform mixed solution is obtained, and obtaining a mixed solution II;
step four, placing the mixed solution II in a constant temperature drying oven, and obtaining white solid powder after the solvent is completely volatilized, namely the prepared polyaluminum chloride flocculant;
the dosage of the nonionic surfactant P123 in the first step is 0.0001-0.0006mol; the dosage of the aluminum isopropoxide in the first step is 3-5 g.
2. The method for preparing the sewage flocculant polyaluminum chloride according to claim 1, wherein the amount of the nonionic surfactant P123 in the first step is 0.0001mol, or 0.0002mol, or 0.0003mol, or 0.0006mol; the amount of aluminum isopropoxide dissolved in the first step was 4 g.
3. The method for preparing the sewage flocculant polyaluminum chloride according to claim 1, wherein the dosage of the concentrated hydrochloric acid solution in the second step is 1-4mL.
4. The method for preparing the sewage flocculant polyaluminum chloride according to claim 3, wherein the dosage of the concentrated hydrochloric acid solution in the second step is 1mL, or 2mL, or 3mL, or 4mL.
5. The method for preparing a sewage flocculant polyaluminum chloride according to claim 1, wherein the temperature of the constant temperature drying oven in the fourth step is set to 60 ℃.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3896086A (en) * | 1973-06-14 | 1975-07-22 | Degussa | Process for the preparation of biodegradable polycarboxylates |
| CN103395809A (en) * | 2013-07-23 | 2013-11-20 | 浙江万里学院 | Method for synthesizing nanometer gama-Al2O3 by adopting solvent replacement/azeotropic distillation drying method and applications thereof |
| CN107500393A (en) * | 2017-09-29 | 2017-12-22 | 广州百兴网络科技有限公司 | A kind of aluminium polychloride chitin composite flocculant and preparation method and application |
| CN108946835A (en) * | 2018-07-12 | 2018-12-07 | 浙江正洁环境科技有限公司 | A kind of absorption-flocculating settling agent and its preparation method and application |
-
2020
- 2020-07-07 CN CN202010644199.7A patent/CN113968605B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3896086A (en) * | 1973-06-14 | 1975-07-22 | Degussa | Process for the preparation of biodegradable polycarboxylates |
| CN103395809A (en) * | 2013-07-23 | 2013-11-20 | 浙江万里学院 | Method for synthesizing nanometer gama-Al2O3 by adopting solvent replacement/azeotropic distillation drying method and applications thereof |
| CN107500393A (en) * | 2017-09-29 | 2017-12-22 | 广州百兴网络科技有限公司 | A kind of aluminium polychloride chitin composite flocculant and preparation method and application |
| CN108946835A (en) * | 2018-07-12 | 2018-12-07 | 浙江正洁环境科技有限公司 | A kind of absorption-flocculating settling agent and its preparation method and application |
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