CN114804311A - Preparation process of high-performance polyaluminum chloride flocculating agent - Google Patents
Preparation process of high-performance polyaluminum chloride flocculating agent Download PDFInfo
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- CN114804311A CN114804311A CN202210387178.0A CN202210387178A CN114804311A CN 114804311 A CN114804311 A CN 114804311A CN 202210387178 A CN202210387178 A CN 202210387178A CN 114804311 A CN114804311 A CN 114804311A
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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
- 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
- C01F7/57—Basic aluminium chlorides, e.g. polyaluminium chlorides
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Abstract
The invention discloses a preparation process of a high-performance polyaluminum chloride flocculant, and relates to the technical field of water purifying agent production. The preparation method of the flocculant comprises the following steps of (1) activating diatomite in a hydrochloric acid solution to obtain activated diatomite; (2) performing polymerization modification on activated diatomite, acrylamide, deionized water, acryloyloxyethyl trimethyl ammonium chloride and 2-vinylpyridine under the action of an initiator to obtain modified diatomite; (3) and loading aluminum chloride in the modified diatomite to obtain the flocculant. The flocculant prepared by the invention has excellent flocculation effect on algae cells, total phosphorus and ammonia nitrogen in wastewater.
Description
Technical Field
The invention relates to the technical field of water purifying agent production, and particularly relates to a preparation process of a high-performance polyaluminum chloride flocculating agent.
Background
Water is a necessary resource for human survival development, but with social development, a large amount of fresh water resources are mixed with some difficultly-degradable high molecular substances, heavy metal ions and the like in the using process, the wastewater is difficult to treat, and is directly discharged into the nature to cause rapid deterioration of water quality of a water source, so that great threat is brought to the continuous and stable development of the society. In recent years, the fundamental reason of the outbreak of algae in many watersheds is the serious overproof of the phosphorus content in water. Nitrogen and phosphorus are essential elements for plant growth, are easy to be utilized by aquatic organisms, and along with the use of a large amount of pesticides and detergents, phosphorus-containing wastewater enters lakes and rivers through discharge, water bodies are eutrophicated, and salts stimulate the mass propagation of algae and cover and gather on the surface of the water bodies, so that the water quality is deteriorated.
However, the algae cells in the water body have the characteristics of high negative charge, small density, strong stability, difficult coagulation and the like, which greatly increase the water treatment and purification difficulty of the algae-containing wastewater, and the algae removal technology commonly used in the water plant at present mainly comprises methods such as pre-chlorination, air flotation and the like. The most common method is pre-chlorination, but in the pre-chlorination process, chlorine and organic matters in water react to generate a plurality of harmful halogenated matters, and meanwhile, the pre-chlorination destroys algae cells in water, so that algae toxins leak, and potential safety hazards are caused to the water.
Disclosure of Invention
The invention aims to provide a preparation process of a high-performance polyaluminium chloride flocculating agent, which solves the following technical problems:
in the prior art, the algae cells in the water body are treated by using the pre-chlorination, so that chlorine and organic matters in the water body react to generate halogenated matters in the operation process, the algae cells in the water body are damaged in the pre-chlorination process to cause leakage of algae toxins, and the residual halogenated matters and the algae toxins in the treated water body have potential safety hazards.
The purpose of the invention can be realized by the following technical scheme:
a preparation process of a high-performance polyaluminum chloride flocculating agent comprises the following steps:
(1) adding diatomite and a hydrochloric acid solution into a reaction kettle, carrying out heat preservation reaction, filtering and washing, drying at low temperature, drying and grinding, and calcining in a muffle furnace to obtain activated diatomite;
(2) adding activated diatomite, acrylamide and deionized water into a reaction bottle, adding acryloyloxyethyl trimethyl ammonium chloride and 2-vinylpyridine, mechanically stirring uniformly, adding an initiator under the nitrogen atmosphere and normal temperature condition, reacting for 9-15h under heat preservation, discharging, drying, crushing and sieving to obtain modified diatomite;
(3) adding aluminum chloride, deionized water and modified diatomite into a reaction bottle, mechanically stirring uniformly, dropwise adding a NaOH solution into a constant-pressure dropping funnel, keeping the temperature, standing, curing, drying and grinding to obtain the flocculant.
As a further scheme of the invention: in the step (1), the temperature is raised to 70-90 ℃ in a water bath, and the reaction is carried out for 1-2h under the condition of heat preservation.
As a further scheme of the invention: in the step (1), the hydrochloric acid solution is 5-10% of hydrochloric acid aqueous solution by mass fraction, and the solid-to-liquid ratio (g/mL) of the diatomite to the hydrochloric acid solution is 1: 4-6.
As a further scheme of the invention: in the step (1), the temperature of the muffle furnace is raised to 350 ℃ for calcining for 1-1.5h, and is continuously raised to 450 ℃ for calcining for 0.5-1 h.
As a further scheme of the invention: activating diatomite in the step (2): acrylamide: acryloyloxyethyltrimethyl ammonium chloride: 2-vinylpyridine: the mass ratio of the initiator is 150-200: 100: 30-45: 1-2: 0.1-0.2.
As a further scheme of the invention: the initiator is prepared by mixing an azo initiator and potassium persulfate in a mass ratio of 4-6:2, wherein the azo initiator is any one of azodiisobutyronitrile and azodiisoheptanonitrile.
As a further scheme of the invention: aluminum chloride in the step (3): deionized water: the mass ratio of the modified diatomite is 3: 40-90: 60-100.
As a further scheme of the invention: in the step (3), the curing temperature is 80-95 ℃, and the curing time is 12-18 h.
As a further scheme of the invention: in the step (3), 0.4-0.5mol/L NaOH aqueous solution is dripped to 75-85% of basicity.
The invention has the beneficial effects that:
(1) the method comprises the steps of firstly activating diatomite, polymerizing the activated diatomite with acrylamide, acryloyloxyethyl trimethyl ammonium chloride and 2-vinylpyridine, grafting cationic polyacrylamide on the surface of the diatomite to obtain modified diatomite, and loading polyaluminum chloride on the modified diatomite to obtain the flocculant. According to the invention, a large number of bulges and holes are generated by grafting the copolymer on the surface of the diatomite, the whole structure is looser, the order degree and the crystal structure of the diatomite structure are damaged by the grafted polyacrylamide molecular chain, the original specific surface area and adsorption capacity are greatly increased, the bridging and flocculating capacities are improved, the electropositivity of the surface of the modified diatomite is higher under an acidic condition, and the electric neutralization capacity exerted in the flocculation algae removal process is stronger. The polyacrylamide is grafted on the surface of the diatomite to increase the substrate distance and the potential value of the diatomite and improve the adsorption capacity of the diatomite and algae cells, the modified diatomite is electropositive in a water body and electronegative in the water body, the concentration of coagulated nuclei for coagulation and flocculation in water is increased due to electric attraction and aggregation, in the process of out-phase flocculation, not only is the effective collision among particles increased, but also the algae cells and the like are coagulated with the modified diatomite into flocculating constituents with higher density, the algae cells in the water body are effectively removed, the ammonia nitrogen and cations on the surface of the modified diatomite are subjected to ion exchange, the phosphorus in the water exists in the form of phosphate, and the flocculating constituents have good adsorption effect on the total phosphorus.
(2) In the rapid stirring process of the flocculant, the concentration of coagulated nuclei in water is rapidly increased, and alum floc with larger density and volume is formed under the action of polyaluminium chloride, so that the coagulation and precipitation are promoted. The polyaluminium chloride is loaded in the pore canal of the modified diatomite and slowly released into the wastewater in the stirring process, so that the problem that the polyaluminium chloride is firstly hydrolyzed in water and forms alumen ustum to cause that zeolite powder and algal cells are difficult to coalesce to form a new flocculating constituent is effectively avoided. In the flocculation process, water and aluminum complex ions are hydrolyzed to generate mononuclear hydroxyl aluminum ions, and then the mononuclear hydroxyl aluminum ions are hydrolyzed step by step, the mononuclear hydroxyl aluminum ions form polynuclear hydroxyl complexes due to collision, and the complexes adsorb suspended matters and colloid particles with negative charge in water to form [ Al (OH) with a net structure 3 ]m (m is more than or equal to 13) is precipitated.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the invention relates to a preparation process of a high-performance polyaluminum chloride flocculant, which comprises the following steps:
(1) adding 200g of diatomite and 800mL of hydrochloric acid aqueous solution with the mass fraction of 5% into a reaction kettle, heating to 70 ℃ in a water bath, carrying out heat preservation reaction for 1 hour, filtering, washing, drying at low temperature, drying, grinding, heating to 300 ℃ in a muffle furnace, calcining for 1 hour, continuously heating to 400 ℃, and calcining for 0.5 hour to obtain activated diatomite;
(2) adding 150g of activated diatomite, 100g of acrylamide and deionized water into a reaction bottle, adding 30g of acryloyloxyethyl trimethyl ammonium chloride and 1g of 2-vinylpyridine, mechanically stirring uniformly, adding 0.075g of azodiisobutyronitrile and 0.025g of potassium persulfate under the conditions of nitrogen atmosphere and normal temperature, carrying out heat preservation reaction for 9 hours, discharging, drying, crushing and sieving to obtain modified diatomite;
(3) adding 6g of aluminum chloride, 80g of deionized water and 120g of modified diatomite into a reaction bottle, mechanically stirring uniformly, dropwise adding 0.5mol/L NaOH solution into a constant-pressure dropping funnel until the basicity is 85%, heating to 80 ℃, curing for 12h, drying and grinding to obtain the flocculant.
Example 2:
the invention relates to a preparation process of a high-performance polyaluminium chloride flocculating agent, which comprises the following steps:
(1) adding 200g of diatomite and 1000mL of hydrochloric acid aqueous solution with the mass fraction of 5% into a reaction kettle, heating to 75 ℃ in a water bath, carrying out heat preservation reaction for 1.5h, filtering, washing, drying at low temperature, drying, grinding, heating to 310 ℃ in a muffle furnace, calcining for 1.2h, continuously heating to 410 ℃, and calcining for 0.6h to obtain activated diatomite;
(2) adding 150g of activated diatomite, 100g of acrylamide and deionized water into a reaction bottle, adding 32g of acryloyloxyethyl trimethyl ammonium chloride and 1.2g of 2-vinylpyridine, mechanically stirring uniformly, adding 0.075g of azodiisobutyronitrile and 0.025g of potassium persulfate under the conditions of nitrogen atmosphere and normal temperature, carrying out heat preservation reaction for 9-15h, discharging, drying, crushing and sieving to obtain modified diatomite;
(3) adding 3g of aluminum chloride, 50g of deionized water and 70g of modified diatomite into a reaction bottle, mechanically stirring uniformly, dripping 0.5mol/L of NaOH solution into a constant-pressure dropping funnel until the basicity is 85%, heating to 85 ℃, curing for 12 hours, drying and grinding to obtain the flocculant.
Example 3:
the invention relates to a preparation process of a high-performance polyaluminium chloride flocculating agent, which comprises the following steps:
(1) adding 200g of diatomite and 1050mL of hydrochloric acid aqueous solution with the mass fraction of 5% into a reaction kettle, heating to 75 ℃ in a water bath, carrying out heat preservation reaction for 1.5h, filtering, washing, drying at low temperature, drying, grinding, heating to 320 ℃ in a muffle furnace, calcining for 1.2h, continuously heating to 420 ℃, and calcining for 0.7h to obtain activated diatomite;
(2) adding 170g of activated diatomite, 100g of acrylamide and deionized water into a reaction bottle, adding 41g of acryloyloxyethyl trimethyl ammonium chloride and 1.5g of 2-vinylpyridine, mechanically stirring uniformly, adding 0.075g of azobisisobutyronitrile and 0.025g of potassium persulfate under the conditions of nitrogen atmosphere and normal temperature, carrying out heat preservation reaction for 12 hours, discharging, drying, crushing and sieving to obtain modified diatomite;
(3) adding 3g of aluminum chloride, 70g of deionized water and 80g of modified diatomite into a reaction bottle, mechanically stirring uniformly, dropwise adding 0.5mol/L NaOH solution into a constant-pressure dropping funnel until the basicity is 85%, heating to 90 ℃, curing for 15h, drying, and grinding to obtain the flocculant.
Example 4:
the invention relates to a preparation process of a high-performance polyaluminium chloride flocculating agent, which comprises the following steps:
(1) adding 200g of diatomite and 1100mL of hydrochloric acid aqueous solution with the mass fraction of 5% into a reaction kettle, heating to 80 ℃ in a water bath, carrying out heat preservation reaction for 1.5h, filtering, washing, drying at low temperature, drying, grinding, heating to 320 ℃ in a muffle furnace, calcining for 1.4h, continuously heating to 420 ℃, and calcining for 0.8h to obtain activated diatomite;
(2) adding 190g of activated diatomite, 100g of acrylamide and deionized water into a reaction bottle, adding 42g of acryloyloxyethyl trimethyl ammonium chloride and 1.8g of 2-vinylpyridine, mechanically stirring uniformly, adding 0.075g of azobisisobutyronitrile and 0.025g of potassium persulfate under the conditions of nitrogen atmosphere and normal temperature, carrying out heat preservation reaction for 14 hours, discharging, drying, crushing and sieving to obtain modified diatomite;
(3) adding 3g of aluminum chloride, 80g of deionized water and 90g of modified diatomite into a reaction bottle, mechanically stirring uniformly, dropwise adding 0.5mol/L NaOH solution into a constant-pressure dropping funnel until the basicity is 85%, heating to 90 ℃, curing for 15h, drying, and grinding to obtain the flocculant.
Example 5:
the invention relates to a preparation process of a high-performance polyaluminium chloride flocculating agent, which comprises the following steps:
(1) adding 200g of diatomite and 1200mL of hydrochloric acid aqueous solution with the mass fraction of 5% into a reaction kettle, heating to 90 ℃ in a water bath, carrying out heat preservation reaction for 2 hours, filtering, washing, drying at low temperature, drying, grinding, heating to 350 ℃ in a muffle furnace, calcining for 1.5 hours, continuously heating to 450 ℃, and calcining for 1 hour to obtain activated diatomite;
(2) adding 200g of activated diatomite, 100g of acrylamide and deionized water into a reaction bottle, adding 45g of acryloyloxyethyl trimethyl ammonium chloride and 2g of 2-vinylpyridine, mechanically stirring uniformly, adding 0.075g of azodiisobutyronitrile and 0.025g of potassium persulfate under the conditions of nitrogen atmosphere and normal temperature, carrying out heat preservation reaction for 15 hours, discharging, drying, crushing and sieving to obtain modified diatomite;
(3) adding 3g of aluminum chloride, 90g of deionized water and 100g of modified diatomite into a reaction bottle, mechanically stirring uniformly, dropwise adding 0.5mol/L NaOH solution into a constant-pressure dropping funnel until the basicity is 85%, heating to 95 ℃, curing for 18h, drying and grinding to obtain the flocculant.
Comparative example 1:
the preparation process of the flocculant comprises the following steps:
(1) adding 200g of diatomite, 100g of acrylamide and deionized water into a reaction bottle, adding 45g of acryloyloxyethyl trimethyl ammonium chloride and 2g of 2-vinylpyridine, uniformly stirring by a machine, adding 0.075g of azodiisobutyronitrile and 0.025g of potassium persulfate under the conditions of nitrogen atmosphere and normal temperature, reacting for 15 hours while keeping the temperature, discharging, drying, crushing and sieving to obtain modified diatomite;
(2) adding 3g of aluminum chloride, 90g of deionized water and 100g of modified diatomite into a reaction bottle, mechanically stirring uniformly, dropwise adding 0.5mol/L NaOH solution into a constant-pressure dropping funnel until the basicity is 85%, heating to 95 ℃, curing for 18h, drying and grinding to obtain the flocculant.
Comparative example 2:
the preparation process of the flocculant comprises the following steps:
(1) adding 200g of diatomite and 1200mL of hydrochloric acid aqueous solution with the mass fraction of 5% into a reaction kettle, heating to 90 ℃ in a water bath, carrying out heat preservation reaction for 2 hours, filtering, washing, drying at low temperature, drying, grinding, heating to 350 ℃ in a muffle furnace, calcining for 1.5 hours, continuously heating to 450 ℃, and calcining for 1 hour to obtain activated diatomite;
(2) adding 3g of aluminum chloride, 90g of deionized water and 100g of activated diatomite into a reaction bottle, mechanically stirring uniformly, dropwise adding 0.5mol/L NaOH solution into a constant-pressure dropping funnel until the basicity is 85%, heating to 95 ℃, curing for 18h, drying, and grinding to obtain the flocculant.
Comparative example 3:
the preparation process of the flocculant comprises the following steps:
(1) adding 200g of diatomite and 1200mL of hydrochloric acid aqueous solution with the mass fraction of 5% into a reaction kettle, heating to 90 ℃ in a water bath, carrying out heat preservation reaction for 2 hours, filtering, washing, drying at low temperature, drying, grinding, heating to 350 ℃ in a muffle furnace, calcining for 1.5 hours, continuously heating to 450 ℃, and calcining for 1 hour to obtain activated diatomite;
(2) adding 200g of activated diatomite, 100g of acrylamide and deionized water into a reaction bottle, adding 45g of acryloyloxyethyl trimethyl ammonium chloride and 2g of 2-vinylpyridine, mechanically stirring uniformly, adding 0.075g of azodiisobutyronitrile and 0.025g of potassium persulfate under the conditions of nitrogen atmosphere and normal temperature, carrying out heat preservation reaction for 15 hours, discharging, drying, crushing and sieving to obtain the flocculant.
Comparative example 4:
the preparation process of the flocculant comprises the following steps:
adding 3g of aluminum chloride and 90g of deionized water into a reaction bottle, mechanically stirring uniformly, dropwise adding 0.5mol/L NaOH solution into a constant-pressure dropping funnel until the basicity is 85%, heating to 95 ℃, curing for 18h, drying, and grinding to obtain the flocculant.
And (3) performance detection:
and (3) adding a pH regulator into the wastewater to be treated in a reactor to adjust the pH to 6, adding the flocculant prepared in the embodiment 1-3, wherein the addition amount of the flocculant is 50mg/L, mechanically stirring at 300r/min for 10-20min, standing for precipitation, and taking supernatant to measure related data.
(1) Algae removal rate: measuring the cell density of algae by a microscopic counting method: and (3) adding 7.5mL of Luge reagent into 500mL of supernatant, standing and precipitating for 1d in a dark place, extracting the supernatant by using a siphon tube, taking 10mL of turbid liquid, transferring the turbid liquid into a colorimetric tube, sucking 0.1mL of turbid liquid, injecting the turbid liquid into an algae technical frame, counting by using a microscope, repeating the steps for three times, taking an average value, calculating the algae cell content and the algae removal rate in the supernatant, and obtaining a calculation result shown in Table 1.
(2) Turbidity removal rate: the turbidity of the water sample was measured by means of a model WGZ-200 turbidity meter, and the turbidity removal rate was calculated, the calculation results are shown in Table 1.
(3) And phosphorus removal rate: the total phosphorus was measured by ammonium molybdate spectrophotometry, and the results are shown in table 1.
(4) Ammonia nitrogen removal rate: the ammonia nitrogen concentration in the sewage is measured by adopting a nano spectrophotometry, and the detection result is shown in table 1.
Table 1:
as can be seen from Table 1, the flocculant prepared by the invention has good adsorption and sedimentation effects on algal cells, total phosphorus and ammonia nitrogen in wastewater.
The embodiments of the present invention have been described in detail, but the description is only for the preferred embodiments of the present invention and should not be construed as limiting the scope of the present invention. All equivalent changes and modifications made within the scope of the present invention shall fall within the scope of the present invention.
Claims (9)
1. A preparation process of a high-performance polyaluminium chloride flocculant is characterized by comprising the following steps:
(1) adding diatomite and a hydrochloric acid solution into a reaction kettle, carrying out heat preservation reaction, filtering and washing, drying at low temperature, drying and grinding, and calcining in a muffle furnace to obtain activated diatomite;
(2) adding activated diatomite, acrylamide and deionized water into a reaction bottle, adding acryloyloxyethyl trimethyl ammonium chloride and 2-vinylpyridine, mechanically stirring uniformly, adding an initiator under the nitrogen atmosphere and normal temperature condition, reacting for 9-15h under heat preservation, discharging, drying, crushing and sieving to obtain modified diatomite;
(3) adding aluminum chloride, deionized water and modified diatomite into a reaction bottle, mechanically stirring uniformly, dropwise adding a NaOH solution into a constant-pressure dropping funnel, keeping the temperature, standing, curing, drying and grinding to obtain the flocculant.
2. The preparation process of the high-performance polyaluminum chloride flocculating agent according to claim 1, wherein the temperature of the water bath in the step (1) is raised to 70-90 ℃, and the reaction is carried out for 1-2 hours under the condition of heat preservation.
3. The preparation process of the high-performance polyaluminum chloride flocculating agent according to claim 1, wherein the hydrochloric acid solution in the step (1) is 5-10% by mass of hydrochloric acid aqueous solution, and the solid-to-liquid ratio (g/mL) of the diatomite to the hydrochloric acid solution is 1: 4-6.
4. The preparation process of the high-performance polyaluminum chloride flocculating agent according to claim 1, wherein the muffle furnace is heated to 350 ℃ for 1-1.5h, and is further heated to 450 ℃ for 0.5-1h in the step (1).
5. The preparation process of the high-performance polyaluminum chloride flocculating agent according to claim 1, wherein the diatomite is activated in the step (2): acrylamide: acryloyloxyethyltrimethyl ammonium chloride: 2-vinylpyridine: the mass ratio of the initiator is 150-200: 100: 30-45: 1-2: 0.1-0.2.
6. The preparation process of the high-performance polyaluminum chloride flocculating agent according to claim 1, wherein the initiator is prepared by mixing an azo initiator with a mass ratio of 4-6:2 and potassium persulfate, and the azo initiator is any one of azobisisobutyronitrile and azobisisoheptonitrile.
7. The preparation process of the high-performance polyaluminum chloride flocculating agent according to claim 1, wherein in the step (3), the ratio of aluminum chloride: deionized water: the mass ratio of the modified diatomite is 3: 40-90: 60-100.
8. The preparation process of the high-performance polyaluminum chloride flocculating agent according to claim 1, wherein in the step (3), the aging temperature is 80-95 ℃ and the aging time is 12-18 h.
9. The process for preparing a high-performance polyaluminum chloride flocculating agent according to claim 1, wherein in the step (3), 0.4 to 0.5mol/L NaOH aqueous solution is added dropwise until the salinity is 75 to 85 percent.
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| AU2020104225A4 (en) * | 2020-11-02 | 2021-03-11 | Jiangxi Academy Of Environmental Sciences | Kaolin-based water purifying material, preparation method and use thereof |
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| CN107902736A (en) * | 2017-11-14 | 2018-04-13 | 中冶华天工程技术有限公司 | The preparation method and composite flocculation algae-inhibiting agent of composite flocculation algae-inhibiting agent |
| CN108314759A (en) * | 2018-02-11 | 2018-07-24 | 南京工业大学 | Preparation method of chitosan modified algae removal flocculating agent |
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| AU2020104225A4 (en) * | 2020-11-02 | 2021-03-11 | Jiangxi Academy Of Environmental Sciences | Kaolin-based water purifying material, preparation method and use thereof |
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