CN112142172A - Method for preparing polyaluminum sulfatochloride water treatment agent - Google Patents
Method for preparing polyaluminum sulfatochloride water treatment agent Download PDFInfo
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- CN112142172A CN112142172A CN202010772395.2A CN202010772395A CN112142172A CN 112142172 A CN112142172 A CN 112142172A CN 202010772395 A CN202010772395 A CN 202010772395A CN 112142172 A CN112142172 A CN 112142172A
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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
- 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
- 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
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
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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
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/56—Macromolecular compounds
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- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
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- Inorganic Chemistry (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a method for preparing a polyaluminium sulfate chloride water treatment agent, which comprises the following steps of reacting 10-15 parts of aluminium hydroxide and 15-20 parts of hydrochloric acid at high temperature and high pressure for 2-4 hours; adding 10-15 parts of aluminum sulfate liquid and 15-20 parts of water into aluminum chloride liquid, reacting for 1-2h, adding 0.01-0.05 part of polyethylene glycol and 0.01-0.05 part of hexadecyl trimethyl ammonium bromide, and reacting for 1-2h to obtain aluminum sulfate-chloride mixed solution; and then adding 0.05-0.10 part of chitosan, heating and stirring for 30-60min, and then carrying out filter pressing, drying and packaging to obtain the polyaluminium sulfate chloride water treatment agent. The polyaluminum sulfatochloride water treatment agent prepared by the invention has large specific surface area, good adsorption performance, improved flocculation performance and flocculation effect, good stability, capability of quickly removing pollutants such as turbidity, chromaticity, heavy metal ions, COD (chemical oxygen demand) and the like, and wide application prospect in sewage or drinking water treatment.
Description
Technical Field
The invention relates to the technical field of sewage treatment, in particular to a method for preparing a polyaluminum sulfatochloride water treatment agent.
Background
The flocculation process is one of the key links in the modern urban water supply and industrial wastewater treatment process, and can remove the sensory indexes such as turbidity, chromaticity and the like of raw water and various toxic and harmful pollutants. Polyaluminium is used as a flocculating agent which is most widely applied in the aspect of water treatment and is widely applied to the fields of drinking water, industrial wastewater and domestic sewage treatment.
The current products of polyaluminium flocculant mainly comprise polyaluminium chloride (PAC), polyaluminium sulfate (PAS), polyaluminium sulfate chloride (PACS), polyaluminium phosphate chloride (PPAC), polyaluminium sulfate ferric chloride (PAFCS) and polyaluminium silicate (PASI). Currently, the most widely used and studied is polyaluminum chloride (PAC), however, there has been little research on polyaluminum sulfatochloride. Polyaluminum sulfatochloride (PASC) is introduced in the PAC structure as S042-The resulting polyaluminum chloride containing sulfate ligands. The turbidity removal effect of the PASC is obviously better than that of PAC, and the speed of alum floc from small to large and the sedimentation speed of the PASC in the flocculation process are higher than those of PAC. The above results indicate that the flocculation performance of PASC is superior to that of PAC and PAS and the stability is higher than that of PAS. However, the polyaluminum sulfatochloride (PACS) provided at present has the defects of not ideal flocculation effect, poor product stability, weak adsorption performance, complex preparation process and the like. Therefore, the research on the high-performance polyaluminum sulfatochloride has important significance in water treatment.
Disclosure of Invention
The invention provides a method for preparing a polyaluminium sulfate-aluminum chloride water treatment agent aiming at the problems of the current flocculant. The polyaluminum sulfatochloride water treatment agent prepared by the invention has large specific surface area, good adsorption performance, improved flocculation performance and flocculation effect, good stability, capability of quickly removing pollutants such as turbidity, chromaticity, heavy metal ions, COD (chemical oxygen demand) and the like, and wide application prospect in sewage or drinking water treatment.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a method for preparing a polyaluminium sulfate chloride water treatment agent comprises the following steps:
(1) according to the following weight ratio, 10-15 parts of aluminum hydroxide and 15-20 parts of hydrochloric acid are reacted for 2-4h at high temperature and high pressure to prepare aluminum chloride liquid;
(2) adding 10-15 parts of aluminum sulfate liquid and 15-20 parts of water into aluminum chloride liquid, reacting for 1-2h, adding 0.01-0.05 part of polyethylene glycol and 0.01-0.05 part of hexadecyl trimethyl ammonium bromide, and reacting for 1-2h to obtain aluminum sulfate-chloride mixed solution;
(3) adding 0.05-0.10 part of chitosan into the aluminum sulfate chloride mixed solution, heating and stirring for 30-60min, and then carrying out filter pressing, drying and packaging to obtain the polyaluminum sulfate chloride water treatment agent.
Further, the drying is drying by using a supercritical fluid.
Further, the supercritical fluid drying is to dry the mixture at the temperature of 40-60 ℃ and the pressure of 5-10MPa by taking carbon dioxide as a drying medium.
Further, the high-temperature high-pressure reaction is carried out at the temperature of 130 ℃ and 150 ℃ and under the pressure of 0.4-0.6 MPa.
Further, the temperature of the reaction in the step (2) is 70-90 ℃, and the reaction temperature is 100-120 ℃ after polyethylene glycol and cetyl trimethyl ammonium bromide are added.
Further, the temperature of the chitosan added in the step (3) is 50-70 ℃.
Compared with the prior art, the invention has the advantages and beneficial effects that:
1. the polyaluminum sulfatochloride water treatment agent prepared by the method has large specific surface area, good adsorption performance, improved flocculation performance and flocculation effect, good stability, capability of quickly removing pollutants such as turbidity, chromaticity, heavy metal ions, COD (chemical oxygen demand) and the like, and wide application prospect in sewage or drinking water treatment.
2. According to the invention, polyethylene glycol and hexadecyl trimethyl ammonium bromide are added in the reaction, so that the specific surface area of the flocculating agent can be increased, the advantages of adsorption bridging are exerted, the adsorption of colloid is facilitated, the dispersion among molecules is facilitated, the adsorption performance is obviously improved, and the quick and efficient flocculation effect is realized.
3. The method of the invention also comprisesThe chitosan and the polyaluminium sulfate chloride have good bonding and bridging effects, can promote colloid flocculation, and can also react with Cu through the chitosan2+、Pb2+、Hg2+、Ag+、Ca2+The heavy metal ions form stable complexes and flocculation occurs.
4. The method adopts supercritical fluid drying, can enlarge the aperture and specific surface area of the polyaluminium sulfate chloride, obviously improves the adsorption performance and improves the flocculation effect.
5. The polyaluminum sulfate chloridization water treatment agent prepared by the method has the advantages of 28-32 percent of aluminum oxide, 45-55 percent of basicity, 1-2 percent of sulfate radical and 153-182m of specific surface area2.g-1The preparation process is simple, the cost is low, and the industrial production is easy to realize.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments. It should be emphasized that the following description is merely exemplary in nature and is not intended to limit the scope of the invention or its application.
Example 1
A method for preparing a polyaluminium sulfate chloride water treatment agent comprises the following steps:
(1) according to the following weight ratio, 13 tons of aluminum hydroxide and 18 tons of hydrochloric acid react for 3 hours at 135 ℃ and 0.5MPa high temperature and high pressure to prepare aluminum chloride liquid;
(2) adding 12 tons of aluminum sulfate liquid and 16 tons of water into aluminum chloride liquid, reacting at 80 ℃ for 1.5 hours, adding 60030kg of polyethylene glycol and 35kg of hexadecyl trimethyl ammonium bromide, and reacting at 100 ℃ for 1 hour to obtain an aluminum sulfate and chloride mixed solution;
(3) adding 70kg of chitosan into the aluminum sulfate chloride mixed solution, heating to 60 ℃, stirring for 40min, performing filter pressing, and drying by using supercritical fluid, wherein the drying takes carbon dioxide as a drying medium, and the drying is performed at the temperature of 40 ℃ and the pressure of 8MPa, so as to obtain the polyaluminum sulfate chloride water treatment agent.
The polyaluminum sulfatochloride water treatment agent prepared in the embodiment is detected to be oxidized by trioxaneThe content of dialuminum is 29.3%, the basicity is 58.9%, the content of sulfate radical is 1.4%, the specific surface area is 180.25m2.g-1。
Example 2
A method for preparing a polyaluminium sulfate chloride water treatment agent comprises the following steps:
(1) according to the following weight ratio, 10 tons of aluminum hydroxide and 16 tons of hydrochloric acid react for 2.5 hours at 140 ℃ and 0.4MPa to prepare aluminum chloride liquid;
(2) adding 14.5 tons of aluminum sulfate liquid and 18 tons of water into aluminum chloride liquid, reacting at 70 ℃ for 2 hours, adding 60020kg of polyethylene glycol and 30kg of hexadecyl trimethyl ammonium bromide, and reacting at 120 ℃ for 1.5 hours to obtain an aluminum sulfate and chloride mixed solution;
(3) adding 60kg of chitosan into the aluminum sulfate chloride mixed solution, heating to 60 ℃, stirring for 40min, performing filter pressing, and drying by using supercritical fluid, wherein the drying takes carbon dioxide as a drying medium, and the drying is performed at the temperature of 50 ℃ and the pressure of 6MPa, so as to obtain the polyaluminum sulfate chloride water treatment agent.
Through detection, the polyaluminum sulfate chloride water treatment agent prepared by the embodiment has the aluminum oxide content of 28.5%, the basicity of 49.7%, the sulfate radical content of 1.8% and the specific surface area of 169.47m2.g-1。
Example 3
A method for preparing a polyaluminium sulfate chloride water treatment agent comprises the following steps:
(1) according to the following weight ratio, 14 tons of aluminum hydroxide and 20 tons of hydrochloric acid react for 3.5 hours at 140 ℃ and 0.5MPa to prepare aluminum chloride liquid;
(2) adding 12 tons of aluminum sulfate liquid and 17 tons of water into aluminum chloride liquid, reacting at 80 ℃ for 1.5 hours, adding 60045kg of polyethylene glycol and 25kg of hexadecyl trimethyl ammonium bromide, and reacting at 110 ℃ for 2 hours to obtain an aluminum sulfate and chloride mixed solution;
(3) adding 50kg of chitosan into the aluminum sulfate chloride mixed solution, heating to 70 ℃, stirring for 60min, performing filter pressing, and drying by using supercritical fluid, wherein the drying takes carbon dioxide as a drying medium, and the drying is performed at the temperature of 60 ℃ and the pressure of 8MPa, so as to obtain the polyaluminum sulfate chloride water treatment agent.
Through detection, the polyaluminum sulfate chloride water treatment agent prepared in the embodiment has the aluminum oxide content of 31.5%, the basicity of 52.1%, the sulfate radical content of 1.6%, and the specific surface area of 159..50m2.g-1。
Example 4
A method for preparing a polyaluminium sulfate chloride water treatment agent comprises the following steps:
(1) according to the following weight ratio, 11.5 tons of aluminum hydroxide and 17 tons of hydrochloric acid react for 3 hours at 140 ℃ and 0.6MPa to prepare aluminum chloride liquid;
(2) adding 14 tons of aluminum sulfate liquid and 18 tons of water into aluminum chloride liquid, reacting at 90 ℃ for 1 hour, adding 60035kg of polyethylene glycol and 40kg of hexadecyl trimethyl ammonium bromide, and reacting at 120 ℃ for 1.5 hours to obtain an aluminum sulfate and chloride mixed solution;
(3) adding 85kg of chitosan into the aluminum sulfate chloride mixed solution, heating to 70 ℃, stirring for 30min, performing filter pressing, and drying by using supercritical fluid, wherein the drying takes carbon dioxide as a drying medium, and the drying is performed at the temperature of 40 ℃ and the pressure of 10MPa, so as to obtain the polyaluminum sulfate chloride water treatment agent.
Through detection, the polyaluminum sulfate chloride water treatment agent prepared by the embodiment has the aluminum oxide content of 30.8%, the basicity of 50.7%, the sulfate radical content of 1.7% and the specific surface area of 172.48m2.g-1。
Example 5
A method for preparing a polyaluminium sulfate chloride water treatment agent comprises the following steps:
(1) according to the following weight ratio, 12 tons of aluminum hydroxide and 17 tons of hydrochloric acid react for 4 hours at 135 ℃ and 0.45MPa high temperature and high pressure to prepare aluminum chloride liquid;
(2) adding 15 tons of aluminum sulfate liquid and 50 tons of water into aluminum chloride liquid, reacting at 80 ℃ for 1.5 hours, adding 60040kg of polyethylene glycol and 30kg of hexadecyl trimethyl ammonium bromide, and reacting at 100 ℃ for 2 hours to obtain an aluminum sulfate and chloride mixed solution;
(3) adding 75kg of chitosan into the aluminum sulfate chloride mixed solution, heating to 80 ℃, stirring for 45min, performing filter pressing, and drying by using supercritical fluid, wherein the drying takes carbon dioxide as a drying medium, and the drying is performed at the temperature of 50 ℃ and the pressure of 7MPa, so as to obtain the polyaluminum sulfate chloride water treatment agent.
Through detection, the polyaluminum sulfate chloride water treatment agent prepared by the embodiment has the aluminum oxide content of 31.82%, the basicity of 53.67%, the sulfate radical content of 2.0% and the specific surface area of 164.72m2.g-1。
Comparative example 1
A method for preparing a polyaluminium sulfate chloride water treatment agent comprises the following steps:
(1) according to the following weight ratio, 12 tons of aluminum hydroxide and 17 tons of hydrochloric acid react for 4 hours at 135 ℃ and 0.45MPa high temperature and high pressure to prepare aluminum chloride liquid;
(2) adding 15 tons of aluminum sulfate liquid and 50 tons of water into aluminum chloride liquid, reacting for 1.5 hours at the temperature of 80 ℃, heating to 100 ℃, and continuing to react for 2 hours to obtain an aluminum sulfate-aluminum chloride mixed solution;
(3) adding 75kg of chitosan into the aluminum sulfate chloride mixed solution, heating to 80 ℃, stirring for 45min, performing filter pressing, and drying by using supercritical fluid, wherein the drying takes carbon dioxide as a drying medium, and the drying is performed at the temperature of 50 ℃ and the pressure of 7MPa, so as to obtain the polyaluminum sulfate chloride water treatment agent.
Through detection, the polyaluminum sulfatochloride water treatment agent prepared by the comparative example has the advantages of 31.82 percent of aluminum oxide content, 47.19 percent of basicity, 2.0 percent of sulfate radical content and 102.63m of specific surface area2.g-1。
Comparative example 2
A method for preparing a polyaluminium sulfate chloride water treatment agent comprises the following steps:
(1) according to the following weight ratio, 12 tons of aluminum hydroxide and 17 tons of hydrochloric acid react for 4 hours at 135 ℃ and 0.45MPa high temperature and high pressure to prepare aluminum chloride liquid;
(2) adding 15 tons of aluminum sulfate liquid and 50 tons of water into aluminum chloride liquid, reacting at 80 ℃ for 1.5 hours, adding 60040kg of polyethylene glycol and 30kg of hexadecyl trimethyl ammonium bromide, and reacting at 100 ℃ for 2 hours to obtain an aluminum sulfate and chloride mixed solution;
(3) and (3) carrying out filter pressing on the aluminum sulfate chloride mixed solution, and drying by adopting a supercritical fluid, wherein the drying is carried out by taking carbon dioxide as a drying medium and drying at the temperature of 50 ℃ and the pressure of 7MPa to obtain the polyaluminum sulfate chloride water treatment agent.
Through detection, the polyaluminum sulfatochloride water treatment agent prepared by the comparative example has the advantages of 31.82 percent of aluminum oxide content, 44.31 percent of basicity, 2.0 percent of sulfate radical content and 126.74m of specific surface area2.g-1。
Comparative example 3
A method for preparing a polyaluminium sulfate chloride water treatment agent comprises the following steps:
(1) according to the following weight ratio, 12 tons of aluminum hydroxide and 17 tons of hydrochloric acid react for 4 hours at 135 ℃ and 0.45MPa high temperature and high pressure to prepare aluminum chloride liquid;
(2) adding 15 tons of aluminum sulfate liquid and 50 tons of water into aluminum chloride liquid, reacting at 80 ℃ for 1.5 hours, adding 60040kg of polyethylene glycol and 30kg of hexadecyl trimethyl ammonium bromide, and reacting at 100 ℃ for 2 hours to obtain an aluminum sulfate and chloride mixed solution;
(3) adding 75kg of chitosan into the aluminum sulfate chloride mixed solution, heating to 80 ℃, stirring for 45min, performing filter pressing, and drying at 50 ℃ in hot air to obtain the polyaluminum sulfate chloride water treatment agent.
Through detection, the polyaluminum sulfatochloride water treatment agent prepared by the comparative example has the advantages of 31.82 percent of aluminum oxide content, 53.67 percent of basicity, 2.0 percent of sulfate radical content and 137.17m of specific surface area2.g-1。
Comparative example 4
A method for preparing a polyaluminium sulfate chloride water treatment agent comprises the following steps:
(1) according to the following weight ratio, 12 tons of aluminum hydroxide and 17 tons of hydrochloric acid react for 4 hours at 135 ℃ and 0.45MPa high temperature and high pressure to prepare aluminum chloride liquid;
(2) adding 15 tons of aluminum sulfate liquid and 50 tons of water into aluminum chloride liquid, reacting for 1.5 hours at the temperature of 80 ℃, and reacting for 2 hours at the temperature of 100 ℃ to obtain aluminum sulfate-aluminum chloride mixed solution;
(3) filter pressing the mixed solution of aluminum sulfate and aluminum chloride, and drying the mixed solution of aluminum sulfate and aluminum chloride in hot air at the temperature of 50 ℃ to obtain the polyaluminum sulfate and aluminum chloride water treatment agent.
Through detection, the polyaluminum sulfatochloride water treatment agent prepared by the comparative example has the advantages of 31.82 percent of aluminum oxide content, 37.24 percent of basicity, 2.0 percent of sulfate radical content and 43.18m of specific surface area2.g-1。
The polyaluminum sulfate chloride water treatment agent prepared by the invention is applied to the treatment of wastewater, and the polyaluminum sulfate chloride of the products of examples 1 to 5 and the polyaluminum sulfate chloride of comparative examples 1 to 4 are added according to the dosage of 0.3 percent, and the treatment results are shown in Table 1. Wherein the turbidity in the wastewater is 72.163NTU and Cu2+The content is 3.16mg.L-1、Pb2+The content is 2.31mg.L-1, and the COD content is 346.19 mg/L.
Table 1: the effect of the polyaluminum sulfatochloride of the invention on purifying sewage
From the test results, the polyaluminum sulfatochloride prepared by the method can quickly remove pollutants such as turbidity, heavy metal ions, COD (chemical oxygen demand) and the like in the wastewater, and has wide application prospect.
The foregoing is a more detailed description of the invention in connection with specific/preferred embodiments and is not intended to limit the practice of the invention to those descriptions. It will be apparent to those skilled in the art that various substitutions and modifications can be made to the described embodiments without departing from the spirit of the invention, and such substitutions and modifications are to be considered as within the scope of the invention.
Claims (6)
1. A method for preparing a polyaluminium sulfate-chloride water treatment agent is characterized by comprising the following steps: the method comprises the following steps:
(1) according to the following weight ratio, 10-15 parts of aluminum hydroxide and 15-20 parts of hydrochloric acid are reacted for 2-4h at high temperature and high pressure to prepare aluminum chloride liquid;
(2) adding 10-15 parts of aluminum sulfate liquid and 15-20 parts of water into aluminum chloride liquid, reacting for 1-2h, adding 0.01-0.05 part of polyethylene glycol and 0.01-0.05 part of hexadecyl trimethyl ammonium bromide, and reacting for 1-2h to obtain aluminum sulfate-chloride mixed solution;
(3) adding 0.05-0.10 part of chitosan into the aluminum sulfate chloride mixed solution, heating and stirring for 30-60min, and then carrying out filter pressing, drying and packaging to obtain the polyaluminum sulfate chloride water treatment agent.
2. The method for preparing a polyaluminum sulfatochloride water treatment agent according to claim 1, wherein: the drying is performed by adopting supercritical fluid.
3. The method for preparing a polyaluminum sulfatochloride water treatment agent according to claim 2, wherein: the supercritical fluid drying is carried out by taking carbon dioxide as a drying medium and drying at 40-60 ℃ and 5-10 MPa.
4. The method for preparing a polyaluminum sulfatochloride water treatment agent according to claim 1, wherein: the high-temperature high-pressure reaction is carried out at the temperature of 130-150 ℃ and the pressure of 0.4-0.6 MPa.
5. The method for preparing a polyaluminum sulfatochloride water treatment agent according to claim 1, wherein: the reaction temperature in the step (2) is 70-90 ℃, and the reaction temperature is 100-120 ℃ after polyethylene glycol and hexadecyl trimethyl ammonium bromide are added.
6. The method for preparing a polyaluminum sulfatochloride water treatment agent according to claim 1, wherein: adding chitosan in the step (3) and then controlling the temperature to be 50-70 ℃.
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Cited By (2)
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| CN113292091A (en) * | 2021-05-17 | 2021-08-24 | 太仓市业洪净水新材料有限公司 | Preparation process of polyaluminum chloride polysulfide flocculant for low-temperature high-turbidity water treatment |
| CN114873624A (en) * | 2022-05-30 | 2022-08-09 | 广东碧之江环保能源股份有限公司 | Stable polyaluminium chloride sulfate production method |
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