CN110015678B - Production process of concentrated polyaluminum chloride - Google Patents
Production process of concentrated polyaluminum chloride Download PDFInfo
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Abstract
The invention discloses a production process of concentrated polyaluminium chloride, and particularly relates to the field of water purification materials. The water film dedusting process removes reaction impurities and sulfides in the mixed solution, improves the purity of the concentrated polyaluminum chloride, reaches the drinking water purification standard, adopts a multi-stage spraying process, effectively utilizes the tail gas heat energy of a drying tower, saves energy, reduces consumption, concentrates the liquid polyaluminum chloride, improves the production efficiency, gradually concentrates the liquid concentration, finally finely adjusts the concentration, facilitates the concentration control and prevents crystallization.
Description
Technical Field
The invention relates to the field of water purification materials, in particular to a production process of novel concentrated polyaluminum chloride.
Background
The liquid polyaluminium chloride is an inorganic polymer flocculant, and inorganic polymers with large molecular weight and high charge are generated through the action of hydroxyl ion functional groups and polyvalent anion polymerization functional groups. The polyaluminium chloride has a large molecular structure, strong adsorption capacity, small using amount and low treatment cost; the dissolubility is good, the activity is high, the alumen ustum formed by coagulation in the water body is large, the sedimentation is fast, and the purification capacity is 2-3 times larger than that of other inorganic flocculants; the adaptability is strong, the influence by the PH value and the temperature of the water body is small, the raw water reaches the national water reference standard after being purified, the water quality after being treated is low in medium cation and anion content, and the ion exchange treatment and the preparation of high-purity water are facilitated; the method has the advantages of low corrosivity and simple and convenient operation, can improve the labor intensity and labor conditions of the chemical dosing process, and can be widely applied to the fields of industrial water purification, municipal sewage treatment and recovery of useful substances in industrial wastewater and waste residues.
The conventional polyaluminium chloride production process adopts a primary water film dedusting process to remove dust and cool, and adopts water spraying, so that the utilization of heat energy of a drying tower is zero, liquid polyaluminium chloride cannot be concentrated, the production efficiency is low, and the purification performance of a product needs to be improved.
Therefore, it is necessary to invent a new production process of concentrated polyaluminium chloride.
Disclosure of Invention
In order to overcome the defects in the prior art, the embodiment of the invention provides a novel production process of concentrated polyaluminium chloride, reaction impurities and sulfides in mixed liquor are removed through a water film dust removal process, the purity of the concentrated polyaluminium chloride is improved, the drinking water purification standard is reached, a multi-stage spraying process is adopted, the tail gas heat energy of a drying tower is effectively utilized, the energy is saved, the consumption is reduced, the liquid polyaluminium chloride is concentrated, the production efficiency is improved, the liquid concentration is concentrated step by step, the concentration is finally finely adjusted, the concentration control is convenient, and the crystallization is prevented.
In order to achieve the purpose, the invention provides the following technical scheme: a production process of novel concentrated polyaluminum chloride comprises the following specific steps:
the method comprises the following steps: preparing 1-3 parts of aluminum hydroxide and 3-8 parts of hydrochloric acid, reacting the active aluminum hydroxide and the hydrochloric acid at high temperature and high pressure to generate an aluminum chloride aqueous solution, and adding deionized water into the aqueous solution to dilute the solution to prepare polymeric liquid polyaluminum chloride for later use;
step two: adding sodium hydroxide, sodium carbonate and lime into the polymeric liquid polyaluminium chloride prepared in the step one for reaction, increasing the content of OH ions in the polymeric liquid polyaluminium chloride, and adjusting the basicity and the acidity-basicity of the polymeric liquid polyaluminium chloride;
step three: heating and pressurizing the polymerized liquid polyaluminium chloride in the step two for atomization, introducing into a spiral-flow type water film dust remover, and removing reaction impurities and sulfides in the mixed liquid through a water film dust removal process;
step four: and (3) introducing the high-purity polymeric liquid polyaluminium chloride processed in the third step into a drying tower for heating treatment, and concentrating the polymeric liquid polyaluminium chloride by adopting a multi-stage spraying process, wherein the method comprises the following specific steps:
first-stage spray concentration, pressurizing the polyaluminum chloride liquid by a high-pressure pump, spraying atomized particles from an atomizing nozzle, heating the atomized particles, mixing and reacting tail gas of a drying tower with the atomized particles, improving the heating efficiency, and cooling the polyaluminum chloride liquid after a period of time;
performing secondary spray concentration, namely pressurizing the primarily concentrated polymeric liquid polyaluminium chloride by a high-pressure pump, spraying atomized particles from an atomizing nozzle, heating the atomized particles, mixing and reacting the tail gas of the drying tower with the atomized particles, improving the heating efficiency, and cooling the polymeric liquid polyaluminium chloride after a period of time;
three-stage spraying fine adjustment, namely pressurizing and atomizing the secondary concentrated polymerization liquid polyaluminium chloride according to the liquid concentration of the secondary concentrated polymerization liquid polyaluminium chloride, and spraying atomized steam to uniformly mix the steam and the secondary concentrated polymerization liquid polyaluminium chloride;
step five: condensing and liquefying the concentrated polymerization liquid polyaluminum chloride uniformly mixed in the step four, and sealing and storing by using a glass container.
Preferably, in the first step, the reaction temperature is set to be 70-150 ℃, the reaction pressure is set to be 0.5-0.8MPa, and the mass ratio of the deionized water to the aluminum chloride water is set to be 1: 3-5.
Preferably, the polyaluminum chloride liquid prepared in the first step has a concentration of 13.6-14%, a basicity of 40.2-43.5% and a pH of 4.2-4.6.
Preferably, the molar ratio of the polymeric aluminum to the sodium hydroxide, the sodium carbonate and the limewater in the polymeric liquid polyaluminum chloride in the second step is 1:1-1.05, 1:0.5-1 and 1:0.5-1 respectively, the basicity of the polymeric liquid polyaluminum chloride after the reaction in the second step is 73.9-88.2% and the pH value is 4.8-5.0.
Preferably, the heating temperature of the first-stage spray concentration drying tower in the fourth step is set to be 120 ℃ and 150 ℃, and the concentration of the liquid after the first-stage concentration is 17-18%.
Preferably, the heating temperature of the second-stage spray concentration drying tower in the fourth step is set to be 150 ℃ and 180 ℃, and the liquid concentration after the second-stage concentration is 18-19%.
Preferably, the heating temperature of the third-stage spraying fine-tuning drying tower in the fourth step is set to be 110 ℃, the concentration of the liquid after the third-stage fine tuning is 18.3-18.7%, and the pH value is 4.9-5.1.
The invention has the technical effects and advantages that:
1. reaction impurities and sulfides in the mixed solution are removed through a water film dedusting process, the purity of the concentrated polyaluminium chloride is improved, the drinking water purification standard is reached, a multi-stage spraying process is adopted, the tail gas heat energy of a drying tower is effectively utilized, the energy is saved, the consumption is reduced, the liquid polyaluminium chloride is concentrated, the production efficiency is improved, the liquid concentration is concentrated step by step, the concentration is finally finely adjusted, the concentration control is convenient, and the crystallization is prevented;
2. by adding a proper amount of sodium hydroxide, sodium carbonate and lime to react with the polyaluminum chloride liquid, the OH ion content in the polyaluminum chloride liquid is increased, the basicity and the acidity-basicity of the polyaluminum chloride liquid are adjusted, the purification efficiency and the use safety of the concentrated polyaluminum chloride are improved, and the sterilization and purification effects are better.
Detailed Description
The following will clearly and completely describe the technical solutions in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all 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 provides a production process of novel concentrated polyaluminum chloride, which comprises the following specific steps:
the method comprises the following steps: preparing 1 part of aluminum hydroxide and 3 parts of hydrochloric acid, reacting the active aluminum hydroxide and the hydrochloric acid at a high temperature and a high pressure to generate an aluminum chloride aqueous solution, adding deionized water into the aqueous solution to dilute the solution to obtain polymeric liquid polyaluminum chloride for later use, wherein the reaction temperature is set to 70 ℃, the reaction pressure is set to 0.5MPa, the mass ratio of the deionized water to the aluminum chloride aqueous solution is set to 1:3, the concentration of the obtained polymeric liquid polyaluminum chloride liquid is 13.6%, the basicity is 40.2%, and the pH value is 4.2;
step two: adding sodium hydroxide, sodium carbonate and lime into the polymerized liquid polyaluminium chloride prepared in the first step for reaction, increasing the content of OH ions in the polymerized liquid polyaluminium chloride, and adjusting the basicity and the acidity-basicity of the polymerized liquid polyaluminium chloride, wherein the molar ratios of the polymerized aluminium in the polymerized liquid polyaluminium chloride to the sodium hydroxide, the sodium carbonate and the limewater are respectively 1:1, 1:0.5 and 1:0.5, the basicity after the reaction is 73.9 percent, and the pH value is 4.8;
step three: heating and pressurizing the polymerized liquid polyaluminium chloride in the step two for atomization, introducing into a spiral-flow type water film dust remover, and removing reaction impurities and sulfides in the mixed liquid through a water film dust removal process;
step four: and (3) introducing the high-purity polymeric liquid polyaluminium chloride processed in the third step into a drying tower for heating treatment, and concentrating the polymeric liquid polyaluminium chloride by adopting a multi-stage spraying process, wherein the method comprises the following specific steps:
first-stage spray concentration, namely pressurizing the polyaluminum chloride liquid by a high-pressure pump, spraying atomized particles from an atomizing nozzle, heating the atomized particles, mixing and reacting tail gas of a drying tower with the atomized particles, setting the heating temperature to be 120 ℃, cooling the polyaluminum chloride liquid after a period of time, and performing first-stage concentration to obtain a liquid with the concentration of 17%;
performing secondary spray concentration, namely pressurizing the primarily concentrated polymeric liquid polyaluminium chloride by a high-pressure pump, spraying atomized particles from an atomizing nozzle, heating the atomized particles, mixing and reacting tail gas of a drying tower with the atomized particles, setting the heating temperature to be 150 ℃, cooling the polymeric liquid polyaluminium chloride after a period of time, and performing secondary concentration to obtain a liquid with the concentration of 18%;
three-stage spraying fine adjustment, namely pressurizing and atomizing the secondary concentrated polymerization liquid polyaluminium chloride according to the liquid concentration of the secondary concentrated polymerization liquid polyaluminium chloride, spraying atomized steam to uniformly mix the steam and the secondary concentrated polymerization liquid polyaluminium chloride, setting the heating temperature to be 100 ℃, and adjusting the liquid concentration to be 18.3% and the pH value to be 4.9 after three-stage fine adjustment;
step five: condensing and liquefying the concentrated polymerization liquid polyaluminum chloride uniformly mixed in the step four, and sealing and storing by using a glass container.
The concentrated polyaluminium chloride prepared in the embodiment has high liquid concentration, less impurity content, high purity, high hydroxide ion content, strong adsorption capacity, good flocculation effect and convenience for purified water use, in addition, the performance detection and purification test are carried out on the prepared concentrated polyaluminium chloride, the result shows that the liquid concentration is 18.3%, no crystallization is generated, the total content of arsenic, lead, cadmium, mercury and hexavalent chromium in the polyaluminium chloride is less than 0.00012%, the effective purification rate is 90%, the unit usage amount is 5g/L, and the purification efficiency is general.
Example 2
The invention provides a production process of novel concentrated polyaluminum chloride, which comprises the following specific steps:
the method comprises the following steps: preparing 2 parts of aluminum hydroxide and 5.5 parts of hydrochloric acid, reacting the active aluminum hydroxide and the hydrochloric acid at a high temperature and a high pressure to generate an aluminum chloride aqueous solution, adding deionized water into the aqueous solution to dilute the solution to obtain polymeric liquid polyaluminum chloride for later use, wherein the reaction temperature is set to 110 ℃, the reaction pressure is set to 0.7MPa, the mass ratio of the deionized water to the aluminum chloride aqueous solution is set to 1:4, the concentration of the obtained polymeric liquid polyaluminum chloride liquid is 13.8%, the basicity is 43%, and the pH value is 4.4;
step two: adding sodium hydroxide, sodium carbonate and lime into the polymerized liquid polyaluminium chloride prepared in the first step for reaction, increasing the content of OH ions in the polymerized liquid polyaluminium chloride, and adjusting the basicity and the acidity and basicity of the polymerized liquid polyaluminium chloride, wherein the molar ratios of the polymerized aluminium in the polymerized liquid polyaluminium chloride to the sodium hydroxide, the sodium carbonate and the limewater are respectively 1:1.03, 1:0.8 and 1:0.8, the basicity after the reaction is 80%, and the pH value is 4.9;
step three: heating and pressurizing the polymerized liquid polyaluminium chloride in the step two for atomization, introducing into a spiral-flow type water film dust remover, and removing reaction impurities and sulfides in the mixed liquid through a water film dust removal process;
step four: and (3) introducing the high-purity polymeric liquid polyaluminium chloride processed in the third step into a drying tower for heating treatment, and concentrating the polymeric liquid polyaluminium chloride by adopting a multi-stage spraying process, wherein the method comprises the following specific steps:
first-stage spray concentration, namely pressurizing the polyaluminum chloride liquid by a high-pressure pump, spraying atomized particles from an atomizing nozzle, heating the atomized particles, mixing and reacting tail gas of a drying tower with the atomized particles, setting the heating temperature to be 125 ℃, cooling the polyaluminum chloride liquid after a period of time, and performing first-stage concentration to obtain liquid with the concentration of 17.5%;
performing secondary spray concentration, namely pressurizing the primarily concentrated polymeric liquid polyaluminium chloride by a high-pressure pump, spraying atomized particles from an atomizing nozzle, heating the atomized particles, mixing and reacting tail gas of a drying tower with the atomized particles, setting the heating temperature to be 165 ℃, cooling the polymeric liquid polyaluminium chloride after a period of time, and controlling the liquid concentration to be 18.5% after the secondary concentration;
three-stage spraying fine adjustment, namely pressurizing and atomizing the secondary concentrated polymerization liquid polyaluminium chloride according to the liquid concentration of the secondary concentrated polymerization liquid polyaluminium chloride, spraying atomized steam to uniformly mix the steam and the secondary concentrated polymerization liquid polyaluminium chloride, setting the heating temperature to be 105 ℃, setting the liquid concentration after the three-stage fine adjustment to be 18.5 percent, and setting the pH value to be 5.0;
step five: condensing and liquefying the concentrated polymerization liquid polyaluminum chloride uniformly mixed in the step four, and sealing and storing by using a glass container.
Compared with the embodiment 1, the concentrated polyaluminium chloride prepared in the embodiment has high liquid concentration, less impurity content, high purity, high hydroxide ion content, strong adsorption capacity, good flocculation effect and convenience for purified water use, in addition, the embodiment performs performance detection and purification test on the prepared concentrated polyaluminium chloride, and the result shows that the liquid concentration is 18.5 percent, no crystallization is generated, the total content of arsenic, lead, cadmium, mercury and hexavalent chromium in the polyaluminium chloride is less than 0.00010 percent, the effective purification rate is 98 percent, the unit usage amount is 3g/L, and the purification efficiency is high.
Example 3
The invention provides a production process of novel concentrated polyaluminum chloride, which comprises the following specific steps:
the method comprises the following steps: preparing 3 parts of aluminum hydroxide and 8 parts of hydrochloric acid, reacting the active aluminum hydroxide and the hydrochloric acid at a high temperature and a high pressure to generate an aluminum chloride aqueous solution, adding deionized water into the aqueous solution to dilute the solution to obtain polymeric liquid polyaluminum chloride for later use, wherein the reaction temperature is set to 150 ℃, the reaction pressure is set to 0.8MPa, the mass ratio of the deionized water to the aluminum chloride aqueous solution is set to 1:5, the concentration of the obtained polymeric liquid polyaluminum chloride liquid is 14%, the basicity is 43.5%, and the pH value is 4.6;
step two: adding sodium hydroxide, sodium carbonate and lime into the polymerized liquid polyaluminium chloride prepared in the step one for reaction, increasing the content of OH ions in the polymerized liquid polyaluminium chloride, and adjusting the basicity and the acidity and basicity of the polymerized liquid polyaluminium chloride, wherein the molar ratios of the polymerized aluminium in the polymerized liquid polyaluminium chloride to the sodium hydroxide, the sodium carbonate and the limewater are respectively 1:1.05, 1:1 and 1:1, the basicity after the reaction is 88.2 percent, and the pH value is 5.0;
step three: heating and pressurizing the polymerized liquid polyaluminium chloride in the step two for atomization, introducing into a spiral-flow type water film dust remover, and removing reaction impurities and sulfides in the mixed liquid through a water film dust removal process;
step four: and (3) introducing the high-purity polymeric liquid polyaluminium chloride processed in the third step into a drying tower for heating treatment, and concentrating the polymeric liquid polyaluminium chloride by adopting a multi-stage spraying process, wherein the method comprises the following specific steps:
first-stage spray concentration, namely pressurizing the polyaluminum chloride liquid by a high-pressure pump, spraying atomized particles from an atomizing nozzle, heating the atomized particles, mixing and reacting tail gas of a drying tower with the atomized particles, setting the heating temperature to be 150 ℃, cooling the polyaluminum chloride liquid after a period of time, and performing first-stage concentration to obtain liquid with the concentration of 18%;
performing secondary spray concentration, namely pressurizing the primarily concentrated polymeric liquid polyaluminium chloride by a high-pressure pump, spraying atomized particles from an atomizing nozzle, heating the atomized particles, mixing and reacting tail gas of a drying tower with the atomized particles, setting the heating temperature to be 180 ℃, cooling the polymeric liquid polyaluminium chloride after a period of time, and controlling the liquid concentration to be 19% after the secondary concentration;
three-stage spraying fine adjustment, namely pressurizing and atomizing the secondary concentrated polymerization liquid polyaluminium chloride according to the liquid concentration of the secondary concentrated polymerization liquid polyaluminium chloride, spraying atomized steam to uniformly mix the steam and the secondary concentrated polymerization liquid polyaluminium chloride, setting the heating temperature to be 110 ℃, and adjusting the liquid concentration to be 18.7% and the pH value to be 5.1 after three-stage fine adjustment;
step five: condensing and liquefying the concentrated polymerization liquid polyaluminum chloride uniformly mixed in the step four, and sealing and storing by using a glass container.
Comparing example 1 and 2, the concentrated polyaluminium chloride liquid concentration that prepares in this embodiment is high, and impurity content is few, and purity is high, and the hydroxide ion content is high, and adsorption efficiency is strong, and it is effectual to flocculate, and the water use of being convenient for, in addition this embodiment carries out performance detection and purification test to the concentrated polyaluminium chloride who prepares, and the result shows that the liquid concentration is 18.7%, and no crystallization produces, and the total content of arsenic, lead, cadmium, mercury and hexavalent chromium is less than 0.00011% in the polyaluminium chloride liquid, and effective purification rate is 97%, and the unit use amount is 3g/L, and purification efficiency is high.
The following table is obtained according to examples 1 to 3:
as can be seen from the above table, in example 2, the raw materials have a moderate proportion, the processing temperature is moderate, the prepared concentrated polyaluminum chloride has the best use effect, and a proper amount of sodium hydroxide, sodium carbonate and lime are added for reaction, so that the content of OH ions in the polyaluminum chloride liquid is increased, the basicity and the acidity and basicity of the polyaluminum chloride liquid are adjusted, the purification efficiency and the use safety of the concentrated polyaluminum chloride are improved, the sterilization and purification effects are better, the reaction impurities and the sulfides in the mixed liquid are removed through the water film dust removal process, the purity of the concentrated polyaluminum chloride is improved, the drinking water purification standard is reached, the multi-stage spraying process is adopted, the tail gas heat energy of the drying tower is effectively utilized, the energy is saved, the consumption is reduced, the liquid polyaluminum chloride is concentrated, the production efficiency is improved, the liquid concentration.
Finally, it should be noted that: the above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that are within the spirit and principle of the present invention are intended to be included in the scope of the present invention.
Claims (4)
1. A production process of concentrated polyaluminium chloride is characterized in that: the method comprises the following specific steps:
the method comprises the following steps: preparing 1-3 parts of aluminum hydroxide and 3-8 parts of hydrochloric acid, reacting the active aluminum hydroxide and the hydrochloric acid at high temperature and high pressure to generate an aluminum chloride aqueous solution, and adding deionized water into the aqueous solution to dilute the solution to prepare polymeric liquid polyaluminum chloride for later use;
step two: adding sodium hydroxide, sodium carbonate and lime into the polymeric liquid polyaluminium chloride prepared in the step one for reaction, increasing the content of OH ions in the polymeric liquid polyaluminium chloride, and adjusting the basicity and the acidity-basicity of the polymeric liquid polyaluminium chloride;
step three: heating and pressurizing the polymerized liquid polyaluminium chloride in the step two for atomization, introducing into a spiral-flow type water film dust remover, and removing reaction impurities and sulfides in the mixed liquid through a water film dust removal process;
step four: and (3) introducing the high-purity polymeric liquid polyaluminium chloride processed in the third step into a drying tower for heating treatment, and concentrating the polymeric liquid polyaluminium chloride by adopting a multi-stage spraying process, wherein the method comprises the following specific steps:
first-stage spray concentration, pressurizing the polyaluminum chloride liquid by a high-pressure pump, spraying atomized particles from an atomizing nozzle, heating the atomized particles, mixing and reacting tail gas of a drying tower with the atomized particles, improving the heating efficiency, and cooling the polyaluminum chloride liquid after a period of time;
performing secondary spray concentration, namely pressurizing the primarily concentrated polymeric liquid polyaluminium chloride by a high-pressure pump, spraying atomized particles from an atomizing nozzle, heating the atomized particles, mixing and reacting the tail gas of the drying tower with the atomized particles, improving the heating efficiency, and cooling the polymeric liquid polyaluminium chloride after a period of time;
three-stage spraying fine adjustment, namely pressurizing and atomizing the secondary concentrated polymerization liquid polyaluminium chloride according to the liquid concentration of the secondary concentrated polymerization liquid polyaluminium chloride, and spraying atomized steam to uniformly mix the steam and the secondary concentrated polymerization liquid polyaluminium chloride;
step five: condensing and liquefying the concentrated polymerization liquid polyaluminium chloride uniformly mixed in the step four, and sealing and storing by using a glass container;
the molar ratios of the polymeric aluminum to the sodium hydroxide, the sodium carbonate and the lime water in the polymeric liquid polyaluminium chloride in the second step are respectively 1:1-1.05, 1:0.5-1 and 1:0.5-1, the basicity of the polymeric liquid polyaluminium chloride after reaction in the second step is 73.9-88.2 percent, and the pH value is 4.8-5.0;
the heating temperature of the first-stage spray concentration drying tower in the fourth step is set to be 120-;
the heating temperature of the second-stage spray concentration drying tower in the fourth step is set to be 150-;
the heating temperature of the third-stage spraying fine-tuning drying tower in the fourth step is set to be 110 ℃, the concentration of the liquid after the third-stage fine tuning is 18.3-18.7%, and the pH value is 4.9-5.1.
2. The process according to claim 1, wherein the process comprises the following steps: in the first step, the reaction temperature is set to be 70-150 ℃, the reaction pressure is set to be 0.5-0.8MPa, and the mass ratio of the deionized water to the aluminum chloride aqueous solution is set to be 1: 3-5.
3. The process according to claim 1, wherein the process comprises the following steps: the concentration of the polyaluminum chloride liquid prepared in the first step is 13.6-14%, the basicity is 40.2-43.5%, and the pH value is 4.2-4.6.
4. Concentrated polyaluminium chloride obtainable by the process of any one of claims 1 to 3.
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CN112266004A (en) * | 2020-10-19 | 2021-01-26 | 四川海明源环保科技有限公司 | Production method of polyaluminum chloride in sewage treatment agent |
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