CN111302464B - Preparation method of polyaluminum sulfatochloride flocculant - Google Patents
Preparation method of polyaluminum sulfatochloride flocculant Download PDFInfo
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- CN111302464B CN111302464B CN202010307695.3A CN202010307695A CN111302464B CN 111302464 B CN111302464 B CN 111302464B CN 202010307695 A CN202010307695 A CN 202010307695A CN 111302464 B CN111302464 B CN 111302464B
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- 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
Abstract
The invention discloses a preparation method of a polyaluminum sulfatochloride flocculant, which comprises the following steps: adding 1-3 tons of sulfuric acid, 8-15 tons of aluminum hydroxide, 3-5 tons of water and 15-20 tons of hydrochloric acid into a reaction kettle A according to the following weight ratio, and reacting for 2-4 hours at high temperature and high pressure to prepare aluminum chloride liquid; adding 10-15 tons of aluminum sulfate liquid, sodium citrate and a stabilizer consisting of sodium metaaluminate into the reaction kettle B, and reacting for 2-4 hours under normal pressure to obtain aluminum sulfate liquid; conveying the aluminum chloride liquid to a reaction kettle C, pumping 6-10 tons of calcium aluminate powder and 15-20 tons of water, reacting for 1-2h at normal pressure, pumping aluminum sulfate liquid, and reacting for 2-3h at normal pressure to obtain a reaction product; and then carrying out filter pressing, drying and packaging to obtain the polyaluminum sulfatochloride flocculant. The detection result of the polyaluminum sulfate chloride flocculant product prepared by the method is that the content of aluminum oxide reaches 30-35%, the basicity reaches 65-90%, the content of sulfate radicals reaches 5.5-6.5%, and the flocculant has a high-efficiency flocculation effect and can quickly purify pollutants such as heavy metal ions, COD (chemical oxygen demand), TP (thermal transfer printing) and the like in wastewater.
Description
Technical Field
The invention relates to the technical field of flocculating agents, in particular to a preparation method of a polyaluminum sulfatochloride flocculating agent.
Background
At present, the problem of the disordered discharge of industrial waste liquid of enterprises of chemical engineering, metallurgy, pharmacy and the like is prominent. Heavy metal pollutants such as arsenic, mercury, chromium, nickel and the like are easily and illegally discharged along with waste liquid, so that surrounding soil, rivers and underground water are polluted, and the change of ecological environment is caused. The removal of heavy metals from waste streams by flocculation-coagulation is one of the most common methods for the disposal of industrial waste streams. Flocculants commonly used in the market include inorganic flocculants and organic flocculants, and specifically include polyaluminium chloride (PAC), polyaluminium sulfate (PAS), polyferric chloride (PFC), polyferric sulfate (polyferric sulfate), Polyacrylamide (PAM), and the like.
The polyaluminium chloride flocculant is accompanied by physical and chemical processes of charge neutralization, adsorption bridging, net catching, rolling, sweeping and the like, and has good flocculation effect. Compared with the traditional inorganic flocculant, the polyaluminium chloride structurally consists of a multi-carboxyl complex with various forms, has high flocculation and precipitation speed, wide applicable pH value range, no corrosion to pipeline equipment and obvious water purification effect, and can effectively remove heavy metal ions such as chromaticness, SS, COD, BOD, arsenic, mercury and the like in water, thereby drawing great attention in the water treatment field, becoming a hotspot of the research of inorganic polymeric flocculant at home and abroad, and having wide application in the fields of drinking water, industrial water, sewage treatment and the like. The flocculation capability of PAC is closely related to its basicity, generally requiring that the basicity of PAC of a water treatment agent must be greater than 40%. Basicity is an important indicator of polyaluminium chloride production and is defined as: hydrogen and oxygen in polyaluminium chloride
The mass percentage of the radical ion to the aluminum ion, i.e., the basicity formula, is [ OH—〕/〔Al3+X 100% of the total weight. The polyaluminium chloride is a polymer of basic aluminium salt between aluminium trichloride and aluminium hydroxide, and OH in the polyaluminium chloride—The amount of (A) determines the form of the polyaluminium chloride, and the molecular structure of the polyaluminium chloride is accompanied by OH—The basicity of the polyaluminium chloride is increased. At present, the polyaluminum chloride (PAC) used in the market has the aluminum oxide content of 20-25% and the basicity of the product is 40-50%, and due to the low basicity, the pH value of the water body added with the flocculant is obviously reduced, and lime or alkali is required to be added to adjust the pH value. The polyaluminium chloride provided at present has the defects of low flocculation speed, poor flocculation effect, high production cost and the like, and water-insoluble substances and heavy metals are easy to exceed the standard.
Disclosure of Invention
The invention provides a preparation method of a polyaluminum sulfatochloride flocculant, aiming at the defects of the traditional polyaluminum chloride flocculant. The detection result of the polyaluminum sulfate chloride flocculant product prepared by the method is that the content of aluminum oxide reaches 30-35%, the basicity reaches 65-90%, the content of sulfate radicals reaches 5.5-6.5%, and the flocculant has a high-efficiency flocculation effect and can quickly purify pollutants such as heavy metal ions, COD (chemical oxygen demand), TP (thermal transfer printing) and the like in wastewater.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a preparation method of polyaluminum sulfatochloride flocculant comprises the following steps:
(1) adding 1-3 tons of sulfuric acid, 8-15 tons of aluminum hydroxide, 3-5 tons of water and 15-20 tons of hydrochloric acid into a reaction kettle A according to the following weight ratio, and reacting for 2-4 hours at high temperature and high pressure to prepare aluminum chloride liquid;
(2) adding 10-15 tons of aluminum sulfate liquid, sodium citrate and a stabilizer consisting of sodium metaaluminate into the reaction kettle B, and reacting for 2-4 hours under normal pressure to obtain aluminum sulfate liquid;
(3) conveying the aluminum chloride liquid to a reaction kettle C, pumping 6-10 tons of calcium aluminate powder and 15-20 tons of water, reacting for 1-2h at normal pressure, pumping aluminum sulfate liquid, and reacting for 2-3h at normal pressure to obtain a reaction product;
(4) and (3) carrying out filter pressing, drying and packaging on the reaction product to obtain the polyaluminum sulfatochloride flocculant.
Furthermore, the dosage of the sodium citrate and the sodium metaaluminate in the stabilizing agent is 0.5-3.0kg and 10-50kg respectively.
Further, the aluminum sulfate liquid contains 7.5% of alumina.
Further, the concentration of the sulfuric acid is 80%, and the concentration of the hydrochloric acid is 30%.
Further, the step (1) is a reaction at 150 ℃ and under 0.4-0.6 MPa; the step (2) is reaction at 70-90 ℃; in the step (3), the reaction temperature at the front section is 100-120 ℃, and the reaction temperature at the rear section is 80-100 ℃.
Further, the drying is carried out by adopting a spray drying mode.
Compared with the prior art, the invention has the advantages and beneficial effects that:
the method improves the sulfate radical content by controlling the proportion of aluminum sulfate and aluminum chloride, and adds a stabilizer consisting of sodium citrate and sodium metaaluminate and raw materials of calcium aluminate powder and the like in the preparation process, so that the flocculant has better flocculation effect. The product index of the polyaluminum sulfate chloride flocculant prepared by the invention conforms to the requirements of 30-35% of aluminum oxide content, 65-90% of basicity, 5.5-6.5% of sulfate radical content, less than or equal to 0.3% of insoluble substance mass fraction, 3.5-4.5 of pH value (10 g/L aqueous solution), and each index conforms to the provisions of GB 15892-2009. The prepared polyaluminum sulfatochloride flocculant can quickly purify pollutants such as heavy metal ions, COD (chemical oxygen demand), TP (thermal transfer protocol) and the like in wastewater, and has wide market application prospect.
Drawings
FIG. 1 is a process flow diagram of the polyaluminum sulfatochloride flocculant of the present invention.
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 preparation method of polyaluminum sulfatochloride flocculant comprises the following steps:
(1) adding 2 tons (with the concentration of 80%) of sulfuric acid, 10 tons of aluminum hydroxide, 4 tons of water and 16 tons (with the concentration of 30%) of hydrochloric acid into a reaction kettle A according to the following weight ratio, and reacting for 3 hours at the temperature of 140 ℃ under the pressure of 0.5MPa to prepare aluminum chloride liquid;
(2) adding 13 tons of aluminum sulfate liquid (the content of alumina is 7.5 percent), 1kg of sodium citrate and 20kg of sodium metaaluminate into a reaction kettle B, and reacting at the temperature of 80 ℃ under normal pressure for 3 hours to obtain aluminum sulfate liquid;
(3) conveying the aluminum chloride liquid to a reaction kettle C, pumping 8 tons of calcium aluminate powder and 16 tons of water, reacting at the normal pressure of 100 ℃ for 1 hour, pumping aluminum sulfate liquid, and reacting at the normal pressure of 80 ℃ for 2 hours to obtain a reaction product;
(4) and (3) carrying out filter pressing, spray drying and packaging on the reaction product to obtain the polyaluminum sulfatochloride flocculant.
Example 2
A preparation method of polyaluminum sulfatochloride flocculant comprises the following steps:
(1) adding 3 tons (with the concentration of 80%) of sulfuric acid, 12 tons of aluminum hydroxide, 5 tons of water and 20 tons (with the concentration of 30%) of hydrochloric acid into a reaction kettle A according to the following weight ratio, and reacting for 2.5 hours at the temperature of 150 ℃ under the pressure of 0.4MPa to prepare aluminum chloride liquid;
(2) adding 12 tons of aluminum sulfate liquid (the content of alumina is 7.5 percent), 1.5kg of sodium citrate and 30kg of sodium metaaluminate into a reaction kettle B, and reacting at the temperature of 90 ℃ under normal pressure for 2 hours to obtain aluminum sulfate liquid;
(3) conveying the aluminum chloride liquid to a reaction kettle C, pumping 7 tons of calcium aluminate powder and 18 tons of water, reacting at the normal pressure of 120 ℃ for 1 hour, pumping aluminum sulfate liquid, and reacting at the normal pressure of 90 ℃ for 3 hours to obtain a reaction product;
(4) and (3) carrying out filter pressing, spray drying and packaging on the reaction product to obtain the polyaluminum sulfatochloride flocculant.
Example 3
A preparation method of polyaluminum sulfatochloride flocculant comprises the following steps:
(1) adding 3 tons (with the concentration of 80%) of sulfuric acid, 15 tons of aluminum hydroxide, 4 tons of water and 18 tons (with the concentration of 30%) of hydrochloric acid into a reaction kettle A according to the following weight ratio, and reacting for 3.5 hours at the temperature of 135 ℃ under 0.6MPa to prepare aluminum chloride liquid;
(2) adding 14 tons of aluminum sulfate liquid (the content of alumina is 7.5 percent), 2.5kg of sodium citrate and 40kg of sodium metaaluminate into a reaction kettle B, and reacting at the temperature of 80 ℃ under normal pressure for 3.5 hours to obtain aluminum sulfate liquid;
(3) conveying the aluminum chloride liquid to a reaction kettle C, pumping 8 tons of calcium aluminate powder and 15 tons of water, reacting at the normal pressure and the temperature of 100 ℃ for 1 hour, pumping the aluminum sulfate liquid, and reacting at the normal pressure and the temperature of 100 ℃ for 2 hours to obtain a reaction product;
(4) and (3) carrying out filter pressing, spray drying and packaging on the reaction product to obtain the polyaluminum sulfatochloride flocculant.
Example 4
A preparation method of polyaluminum sulfatochloride flocculant comprises the following steps:
(1) adding 2.5 tons of sulfuric acid (with the concentration of 80%), 12 tons of aluminum hydroxide, 4 tons of water and 15 tons of hydrochloric acid (with the concentration of 30%) into a reaction kettle A according to the following weight ratio, and reacting for 3 hours at the temperature of 140 ℃ under 0.5MPa to prepare aluminum chloride liquid;
(2) adding 12 tons of aluminum sulfate liquid (the content of alumina is 7.5 percent), 3kg of sodium citrate and 20kg of sodium metaaluminate into a reaction kettle B, and reacting at the temperature of 80 ℃ under normal pressure for 3 hours to obtain aluminum sulfate liquid;
(3) conveying the aluminum chloride liquid to a reaction kettle C, pumping 10 tons of calcium aluminate powder and 16 tons of water, reacting at 100 ℃ under normal pressure for 1 hour, pumping aluminum sulfate liquid, and reacting at 80 ℃ under normal pressure for 3 hours to obtain a reaction product;
(4) and (3) carrying out filter pressing, spray drying and packaging on the reaction product to obtain the polyaluminum sulfatochloride flocculant.
The polyaluminum sulfatochloride flocculant prepared by the invention is used for detecting the performance of products according to the GB15892-2009 method, and the detection result is shown in Table 1.
Table 1: performance test results of polyaluminum sulfatochloride flocculant
The polyaluminum sulfate chloride flocculant product prepared by the invention has the advantages that the content of aluminum oxide reaches 30-35%, the basicity reaches 65-90%, the content of sulfate radicals reaches 5.5-6.5%, the mass fraction of insoluble substances is less than or equal to 0.1%, the pH value (10 g/L aqueous solution) is 3.5-4.5, and all indexes meet the regulations of GB 15892-2009.
The polyaluminum sulfatochloride flocculant prepared by the invention is applied to the treatment of wastewater of chemical plants, the water quality standard of the chemical plants is shown in table 2, the products of examples 1 to 4 and commercial PAC flocculant are added according to the dosage of 0.5%, and the treatment result is shown in table 3.
Table 2: water quality index of industrial waste water from chemical plant
Table 3: the polyaluminum sulfatochloride flocculant has the effect of purifying wastewater
From the results, the polyaluminum sulfatochloride flocculant prepared by the invention can well remove pollutants such as heavy metal ions, COD (chemical oxygen demand), TP (thermal transfer protocol) and the like in wastewater, and has good market prospect in industrial wastewater treatment.
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 (5)
1. A preparation method of polyaluminum sulfatochloride flocculant is characterized by comprising the following steps: the method comprises the following steps:
(1) adding 1-3 tons of sulfuric acid, 8-15 tons of aluminum hydroxide, 3-5 tons of water and 15-20 tons of hydrochloric acid into a reaction kettle A according to the following weight ratio, and reacting for 2-4 hours at high temperature and high pressure to prepare aluminum chloride liquid;
(2) adding 10-15 tons of aluminum sulfate liquid, sodium citrate and a stabilizer consisting of sodium metaaluminate into the reaction kettle B, and reacting for 2-4 hours under normal pressure to obtain aluminum sulfate liquid;
(3) conveying the aluminum chloride liquid to a reaction kettle C, pumping 6-10 tons of calcium aluminate powder and 15-20 tons of water, reacting for 1-2h at normal pressure, pumping aluminum sulfate liquid, and reacting for 2-3h at normal pressure to obtain a reaction product;
(4) filter pressing, drying and packaging the reaction product to obtain the polyaluminum sulfatochloride flocculant;
the dosage of the sodium citrate and the sodium metaaluminate in the stabilizer is 0.5-3.0kg and 10-50kg respectively;
the step (1) is to react at the temperature of between 0.4 and 0.6MPa and between 130 and 150 ℃; the step (2) is reaction at 70-90 ℃; in the step (3), the reaction temperature at the front section is 100-120 ℃, and the reaction temperature at the rear section is 80-100 ℃.
2. The method for preparing the polyaluminum sulfatochloride flocculant according to claim 1, wherein the flocculant is prepared by the following steps: the aluminum sulfate liquid contains 7.5% of alumina.
3. The method for preparing the polyaluminum sulfatochloride flocculant according to claim 1, wherein the flocculant is prepared by the following steps: the concentration of the sulfuric acid is 80%, and the concentration of the hydrochloric acid is 30%.
4. The method for preparing the polyaluminum sulfatochloride flocculant according to claim 1, wherein the flocculant is prepared by the following steps: the drying is carried out in a spray drying mode.
5. The method for preparing the polyaluminum sulfatochloride flocculant according to claim 1, wherein the flocculant is prepared by the following steps: the polyaluminum sulfate chloride flocculant has the aluminum oxide content of 30-35%, the basicity of 65-90% and the sulfate radical content of 5.5-6.5%.
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| CN112142172A (en) * | 2020-08-04 | 2020-12-29 | 广西锋盛环保科技有限公司 | Method for preparing polyaluminum sulfatochloride water treatment agent |
| CN112125380A (en) * | 2020-08-04 | 2020-12-25 | 广西锋盛环保科技有限公司 | Method for preparing white polyaluminium chloride |
| CN112142173A (en) * | 2020-08-04 | 2020-12-29 | 广西锋盛环保科技有限公司 | Preparation method of high-basicity polyaluminium chloride water purifying agent |
| CN111892141B (en) * | 2020-08-26 | 2022-08-05 | 浙江工业大学 | Method for preparing composite flocculant by using waste aluminum scraps |
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| US5523000A (en) * | 1994-06-29 | 1996-06-04 | Ecolab Inc. | Improved pH driven method for wastewater separation using an amphoteric dicarboxylate and a cationic destabilizer composition |
| CN101885525B (en) * | 2009-05-11 | 2012-02-15 | 山东德科生物科技开发有限公司 | Production method of polymerized aluminium ferric chloride sulphate |
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