CN110655156B - Catalytic flue gas desulfurization wastewater flocculant and preparation method thereof - Google Patents
Catalytic flue gas desulfurization wastewater flocculant and preparation method thereof Download PDFInfo
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- CN110655156B CN110655156B CN201910993324.2A CN201910993324A CN110655156B CN 110655156 B CN110655156 B CN 110655156B CN 201910993324 A CN201910993324 A CN 201910993324A CN 110655156 B CN110655156 B CN 110655156B
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- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
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Abstract
The invention belongs to the technical field of industrial wastewater treatment, and particularly relates to a catalytic flue gas desulfurization wastewater flocculant and a preparation method thereof. The flocculant is compounded by a polymeric organic flocculant and an inorganic flocculant, wherein the polymeric organic flocculant is a mixture of poly dimethyl diallyl ammonium chloride and cationic polyacrylamide, and the inorganic flocculant is a mixture of zinc sulfate, magnesium sulfate and polymeric aluminum silicate sulfate. The method has the advantages of wide applicable water quality range, high efficiency, reduced dosage, convenient and environment-friendly field use, no toxicity or corrosion, no corrosion to equipment, no adverse effect on the process, no increase of raw water COD, high temperature resistance, and acid and alkali resistance. When the pH value is 6.5-8.0, the concentration of suspended matters in wastewater is 1000-5000 mg/L and the water temperature is 45-60 ℃, 200-400 mg/L of the flocculating agent is added, the suspended matters in the effluent of the sedimentation tank are less than or equal to 40mg/L, the removal rate of the suspended matters is more than 98.5 percent, and the flocculation effect is obviously better than that of the existing PAM.
Description
Technical Field
The invention belongs to the technical field of industrial wastewater treatment, and particularly relates to a catalytic flue gas desulfurization wastewater flocculant and a preparation method thereof.
Background
The water treatment flocculant has long history and various varieties, mainly takes an inorganic flocculant, an organic flocculant and a microbial flocculant as main materials, but still cannot meet the technical requirements of industrial sewage and urban sewage treatment in recent years.
As early as 90 s, developed countries in the world have made great technical progress in flue gas desulfurization, and flue gas desulfurization modification work has been basically completed in 2000, such as America, germany, japan and the like. With the rapid development of economy in China, national governments and local governments continuously strengthen environmental protection prevention and treatment measures and successively develop various environmental protection policy rules and regulations. Since the implementation of GB31571-2015 discharge Standard for pollutants for petrochemical industry in 7 months of 2015, all domestic refinery catalytic devices and power plants are continuously reconstructed or newly built with environmental protection facilities for flue gas desulfurization and denitration to meet the requirements of national environmental protection policies. The flue gas desulfurization process mainly takes a wet method, a dry method and a semi-dry method as the leading positions, wherein the wet flue gas desulfurization technology is a desulfurization technology widely applied in the world and has mature process technology and SO removal 2 The method has the characteristics of high efficiency, reliable operation, simple operation, low cost and the like, the installed capacity of the wet flue gas desulfurization process accounts for 85 percent of the total capacity of the existing industrial flue gas desulfurization device, and meanwhile, the wet flue gas desulfurization technology is also a technology which is mainly developed in the country in recent years. However, the wet desulphurization process also brings about some problems, especially the treatment of catalytic flue gas desulphurization waste water. The components of the catalytic flue gas desulfurization wastewater are very complex, the main components of the catalytic flue gas desulfurization wastewater are various catalysts for catalytic cracking, and the catalytic cracking wastewater contains various nickel, vanadium, cerium and copperAluminum, iron, sodium, calcium and the like.
The external drainage standard of the foreign factor device is low, a PAM flocculating agent is mainly adopted, and suspended matters are more than 120mg/L; PAC (forbidden due to serious corrosion of equipment) and PAM are mainly adopted in China, and suspended matters are more than 80mg/L. The existing flocculating agent has the problems of poor treatment effect of suspended matters, serious corrosion of chloride ions on white steel process equipment, filter blockage caused by a high-content organic flocculating agent, inconvenience in field use, environmental friendliness and the like in industrial application. Therefore, it is urgent to develop a high-efficiency flocculant for treating catalytic cracking flue gas desulfurization wastewater.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: overcomes the defects of the prior art and provides the flocculating agent for catalyzing the flue gas desulfurization wastewater. The flocculation effect is greatly increased, the applicable water quality range is wide, the efficiency is high, the advantages of reduced dosage, no toxicity and corrosion, convenient and environment-friendly field use are achieved, the SS of the treated wastewater is reduced, no corrosion is caused to equipment, no adverse effect is caused to the process, the COD of the raw water is not increased, and the raw water is resistant to high temperature and acid and alkali; the invention also provides a preparation method thereof.
The catalytic flue gas desulfurization wastewater flocculant is prepared by compounding a high-molecular organic flocculant and an inorganic flocculant, wherein the high-molecular organic flocculant is a mixture of poly dimethyl diallyl ammonium chloride and cationic polyacrylamide, and the inorganic flocculant is a mixture of zinc sulfate, magnesium sulfate and polymerized aluminum silicate sulfate.
Preferably, the catalytic flue gas desulfurization wastewater flocculant provided by the invention comprises the following raw materials in percentage by weight:
wherein:
the preparation process of the polyaluminium silicate sulfate controls aluminum: the molar ratio of silicon is 10.
The preparation method of the polymeric aluminum silicate sulfate comprises the following steps: dropwise adding a water glass solution into a 25wt% sulfuric acid solution, continuously stirring for 30 minutes, controlling the pH of a reaction system to be less than 2, reacting to obtain polysilicic acid, then adding an aluminum sulfate solution into the polysilicic acid, stirring for 2 hours, and curing for 24 hours to obtain the polyaluminum silicate sulfate solution.
When the polymeric aluminum silicate sulfate is prepared, the purpose of controlling the pH value of a reaction system to be less than 2 is to avoid the phenomenon of jelly and gelation.
According to the preparation method of the catalytic flue gas desulfurization wastewater flocculant, zinc sulfate and magnesium sulfate are added into a polymeric aluminum silicate sulfate solution, the mixture is stirred and dissolved, then cationic polyacrylamide is added, the mixture is continuously stirred until the mixture is fully dissolved and no fish eye phenomenon occurs, and finally, poly dimethyl diallyl ammonium chloride emulsion is added, and the mixture is uniformly stirred to obtain a final product.
The stirring speed is required to be controlled within 150r/min in the preparation process of the catalytic flue gas desulfurization wastewater flocculant.
Preferably, the preparation method of the catalytic flue gas desulfurization wastewater flocculant provided by the invention comprises the steps of adding 4 parts of zinc sulfate and 1 part of magnesium sulfate into 90 parts of polymerized aluminum silicate sulfate solution, stirring and dissolving, adding 1 part of cationic polyacrylamide, continuously stirring until the cationic polyacrylamide is fully dissolved and no fish eye phenomenon exists, and finally adding 4 parts of polydimethyldiallyl ammonium chloride emulsion, and uniformly stirring to obtain a final product.
The catalytic flue gas desulfurization wastewater flocculant provided by the invention is colorless to light green viscous liquid in appearance, the solid content is more than or equal to 20.0%, and the kinematic viscosity (25 ℃) is less than or equal to 80mm 2 S, density (20 ℃) is more than or equal to 1.20g/cm 3 The pH value is 2.0-4.0.
The catalytic flue gas desulfurization wastewater flocculant is a novel composite flocculant compounded by more than two inorganic and organic flocculants after being modified and synthesized by chemical reaction under specific conditions, and different flocculants are compounded to complement the advantages, so that the defects of using a single flocculant are overcome. The polymerized aluminum silicate sulfate solution has the electrical neutralization and net laying characteristics of the inorganic flocculant, the organic flocculant poly dimethyl diallyl ammonium chloride and the cationic polyacrylamide have excellent adsorption and bridging characteristics, and the polymerized aluminum silicate sulfate, the zinc sulfate and the magnesium sulfate perform chemical reaction in the system wastewater to play the electrical neutralization role of the inorganic flocculant and form a net-shaped adsorption floc, so that the effect of decoloring and adsorbing colloidal particles can be well played, and the precipitation speed of flocculated alum flocs is accelerated. The flocculating agent has the advantages of good synergistic effect between various inorganic and organic flocculating agents, greatly increased flocculating effect, wide applicable water quality range, high efficiency, reduced dosage, no toxicity or corrosion, convenient field use and environmental protection. The industrial application results show that: the concentration of suspended matters in the catalytic flue gas desulfurization wastewater treated by adding 200-400 mg/L of the flocculant is reduced from 1000-5000 mg/L to 20-40 mg/L, the removal rate of the suspended matters reaches more than 98.5%, the technical problems that the suspended matters do not reach the standard and a filter is blocked after the catalytic desulfurization wastewater is treated at present are thoroughly solved, the technical index requirements are completely met, no adverse effect is caused to equipment and process, and the field use is convenient and environment-friendly.
The invention relates to a catalytic flue gas desulfurization wastewater flocculant, which is applied to the field of industrial wastewater treatment.
Compared with the prior art, the invention has the following beneficial effects:
(1) The catalytic flue gas desulfurization wastewater flocculant is a novel composite flocculant compounded by more than two inorganic and organic flocculants after being modified and synthesized through chemical reaction under specific conditions, different flocculants are compounded to have complementary advantages, the defects of using a single flocculant are overcome, the catalytic flue gas desulfurization wastewater flocculant has the functions of electrical neutralization of the inorganic flocculant and adsorption bridging of the organic flocculant, the flocculation effect is greatly increased, the applicable water quality range is wide, the efficiency is high, the dosage is reduced, the on-site use is convenient and environment-friendly, and the wastewater treated by the catalytic flue gas desulfurization flocculant has the advantages of no toxicity and no corrosion, the SS of the treated wastewater is reduced to 20-40 mg/L, the catalytic flue gas desulfurization wastewater flocculant does not corrode equipment, has no adverse effect on the process, does not increase the COD of raw water, is high temperature resistant, and is acid and alkali resistant.
(2) The catalytic flue gas desulfurization wastewater flocculant provided by the invention is characterized in that after 200-400 mg/L of the flocculant is injected, the numerical value of suspended matters in effluent of a sedimentation tank is less than or equal to 40mg/L, the removal rate of the suspended matters is more than 98.5%, and the flocculation effect is obviously better than that of the existing PAM when the pH is 6.5-8.0, the concentration of suspended matters in wastewater is 1000-5000 mg/L, and the water temperature is 45-60 ℃. The industrial application result shows that: the content of suspended matters in the wastewater treated by the flocculant is reduced from more than 3000mg/L to 20-40 mg/L, the process index requirements are met, no adverse effect is caused on equipment and processes, and the flocculant is convenient to use on site and environment-friendly.
Drawings
FIG. 1 is a process flow diagram for preparing a polyaluminum silicate sulfate solution according to the present invention.
Detailed Description
The present invention is further described below with reference to examples.
Example 1
The catalytic flue gas desulfurization wastewater flocculant comprises the following raw materials in percentage by weight:
wherein:
preparation process of polyaluminum silicate sulfate aluminum: the molar ratio of silicon is 10.
The preparation method of the poly aluminum silicate sulfate comprises the following steps: dropwise adding a water glass solution into a 25wt% sulfuric acid solution, continuously stirring for 30 minutes, controlling the pH of a reaction system to be less than 2 to avoid the phenomenon of jelly and glue formation, reacting to obtain polysilicic acid, then adding an aluminum sulfate solution into the polysilicic acid, stirring for 2 hours, and curing for 24 hours to obtain the poly aluminum sulfate silicate solution.
The preparation method of the catalytic flue gas desulfurization wastewater flocculant described in this embodiment 1 includes adding 4 parts of zinc sulfate and 1 part of magnesium sulfate to 90 parts of polymeric aluminum silicate sulfate solution, stirring for dissolution, adding 1 part of cationic polyacrylamide, continuously stirring until the mixture is fully dissolved and no fish eye phenomenon occurs, and finally adding 4 parts of polydimethyldiallyl ammonium chloride emulsion, and uniformly stirring to obtain a final product; the stirring speed is controlled at 140r/min in the preparation process.
Table 1 physicochemical indexes of the flocculant for catalytic flue gas desulfurization wastewater prepared in example 1
| Serial number | Item | Index (es) |
| 1 | Appearance of the product | Colorless viscous liquid |
| 2 | Solid content (%) | 28 |
| 3 | Kinematic viscosity (25 ℃, mm) 2 /s) | 52 |
| 4 | Density (20 ℃, g/cm) 3 ) | 1.31 |
| 5 | pH value | 3.1 |
The industrial application condition of the flue gas desulfurization and denitrification unit of the Qilu petrochemical 2.60Mt/a catalytic device is as follows:
table 2 example 1 operating parameters of a flue gas desulfurization and denitration unit of a catalytic apparatus
| Parameter name | Operating parameters |
| Operating temperature of clarification tank (. Degree. C.) | 54～60 |
| The retention amount of water (m) in the clarification tank 3 ) | 120 |
| Amount of treated Water (t/h) | 30 |
| Salt content of wastewater (%) | 1.8 |
| Concentration of wastewater suspended matter (mg/L) | 3000 |
| pH value | 7.0～8.0 |
Application effects
After the flocculant is added into the tank, the value of suspended matters in the effluent of the clarification tank is not more than 40mg/L, the removal rate of the suspended matters is more than 98.6 percent, the COD of the wastewater is increased, and the technical requirement that the value of suspended matters in the effluent of the process is not more than 40mg/L is met. The phenomena of corrosion leakage of process equipment pipelines and filter blockage do not occur in the industrial application process of one year, the dissolution and compounding are not needed on the site, and the additive is directly added into a medicine adding tank and injected into a mixing tank, so that the use is convenient and the environment is protected.
Example 2
The catalytic flue gas desulfurization wastewater flocculant comprises the following raw materials in percentage by weight:
wherein:
the preparation process of the polyaluminium silicate sulfate controls aluminum: the molar ratio of silicon is 10.
The preparation method of the poly aluminum silicate sulfate comprises the following steps: dropwise adding a water glass solution into a 25wt% sulfuric acid solution, continuously stirring for 30 minutes, controlling the pH of a reaction system to be less than 2, avoiding the occurrence of a jelly and glue phenomenon, reacting to obtain polysilicic acid, then adding an aluminum sulfate solution into the polysilicic acid, stirring for 2 hours, and curing for 24 hours to obtain the polyaluminum silicate sulfate solution.
In the preparation method of the catalytic flue gas desulfurization wastewater flocculant described in this embodiment 2, 2 parts of zinc sulfate and 1 part of magnesium sulfate are added to 93.2 parts of polyaluminum silicate sulfate solution, stirred and dissolved, then 0.8 part of cationic polyacrylamide is added, and continuously stirred until the mixture is fully dissolved without a fish eye phenomenon, and finally 3 parts of poly dimethyl diallyl ammonium chloride emulsion is added and stirred uniformly to obtain a final product; the stirring speed is controlled at 140r/min in the whole preparation process.
Table 3 physicochemical indexes of the flocculant for catalytic flue gas desulfurization wastewater prepared in example 2
| Serial number | Item | Index (I) |
| 1 | Appearance of the product | Colorless viscous liquid |
| 2 | Solid content (%) | 29 |
| 3 | Kinematic viscosity (25 ℃, mm) 2 /s) | 46 |
| 4 | Density (20 ℃, g/cm) 3 ) | 1.30 |
| 5 | pH value | 3.1 |
Operational parameters of the 1.80Mt/a catalytic unit PTU unit of the Malachite petrochemical:
table 4 example 2 catalytic unit PTU unit operating parameters
| Parameter name | Operating parameters |
| Operating temperature of clarification tank (. Degree. C.) | 50～57 |
| The retention amount of water (m) in the clarification tank 3 ) | 240 |
| Amount of treated Water (t/h) | 10 |
| Salt content of wastewater (%) | 1.5 |
| Concentration of wastewater suspended matter (mg/L) | 3500 |
| pH value | 7.2 |
Application effects
After 300mg/L of the flocculating agent is added, the value of suspended matters in effluent of the clarification tank is not more than 40mg/L, the removal rate of the suspended matters is more than 98.8 percent, COD (chemical oxygen demand) of wastewater is not increased, and the technical requirement that the value of suspended matters in process effluent is not more than 40mg/L is met. The phenomena of corrosion leakage of process equipment pipelines and blockage of filters do not occur in the industrial application process of one year, and the use is convenient and environment-friendly.
Example 3
The catalytic flue gas desulfurization wastewater flocculant comprises the following raw materials in percentage by weight:
wherein:
the preparation process of the polyaluminium silicate sulfate controls aluminum: the molar ratio of silicon is 10.
The preparation method of the polymeric aluminum silicate sulfate comprises the following steps: dropwise adding a water glass solution into a 25% sulfuric acid solution (mass concentration) and continuously stirring for 30 minutes, controlling the pH of a reaction system to be less than 2 so as to avoid the phenomenon of jelly and gel formation, reacting to obtain polysilicic acid, then adding an aluminum sulfate solution into the polysilicic acid, stirring for 2 hours and then curing for 24 hours to obtain the polyaluminum silicate sulfate solution.
In the preparation method of the catalytic flue gas desulfurization wastewater flocculant described in this embodiment 3, 2 parts of zinc sulfate and 1 part of magnesium sulfate are added to 93.2 parts of polyaluminum silicate sulfate solution, stirred and dissolved, then 0.8 part of cationic polyacrylamide is added, and continuously stirred until the mixture is fully dissolved without the fish eye phenomenon, and finally 3 parts of poly dimethyl diallyl ammonium chloride emulsion is added and stirred uniformly to obtain a final product; the stirring speed is controlled at 140r/min in the whole preparation process.
TABLE 5 physicochemical indices of the flocculant for catalytic flue gas desulfurization wastewater prepared in example 3
| Serial number | Item | Index (es) |
| 1 | Appearance of the product | Colorless viscous liquid |
| 2 | Solid content (%) | 29 |
| 3 | Kinematic viscosity (25 ℃, mm) 2 /s) | 46 |
| 4 | Density (20 ℃, g/cm) 3 ) | 1.30 |
| 5 | pH value | 3.1 |
Operating parameters of PTU unit of Jiangsu Xinhaishi 1.20Mt/a catalytic device:
table 6 example 3 catalytic unit PTU unit operating parameters
Application effects
After the flocculating agent is added for 350mg/L, the value of suspended matters in the effluent of the clarification tank does not exceed 40mg/L, the removal rate of the suspended matters is more than 98.8 percent, the COD of the wastewater is not increased, and the technical requirement that the value of the suspended matters in the process effluent is less than or equal to 40mg/L is met. The phenomena of corrosion leakage of process equipment pipelines and blockage of filters do not occur in the industrial application process, and the use is convenient and environment-friendly.
Example 4
The catalytic flue gas desulfurization wastewater flocculant comprises the following raw materials in percentage by weight:
wherein:
the preparation process of the polyaluminium silicate sulfate controls aluminum: the molar ratio of silicon is 10.
The preparation method of the poly aluminum silicate sulfate comprises the following steps: dropwise adding a water glass solution into a 25% sulfuric acid solution (mass concentration) and continuously stirring for 30 minutes, controlling the pH of a reaction system to be less than 2 so as to avoid the phenomenon of jelly and gel formation, reacting to obtain polysilicic acid, then adding an aluminum sulfate solution into the polysilicic acid, stirring for 2 hours and then curing for 24 hours to obtain the polyaluminum silicate sulfate solution.
In the preparation method of the catalytic flue gas desulfurization wastewater flocculant described in this embodiment 4, 4 parts of zinc sulfate and 1 part of magnesium sulfate are added to 90 parts of polyaluminum silicate sulfate solution, stirred and dissolved, then 1 part of cationic polyacrylamide is added, and stirred continuously until the mixture is fully dissolved without the fish eye phenomenon, and finally 4 parts of poly dimethyl diallyl ammonium chloride emulsion is added and stirred uniformly to obtain a final product; the stirring speed is controlled at 140r/min in the whole preparation process.
Table 7 physicochemical indexes of the flocculant for catalytic flue gas desulfurization wastewater prepared in example 4
| Serial number | Item | Index (I) |
| 1 | Appearance of the product | Colorless viscous liquid |
| 2 | Solid content (%) | 28 |
| 3 | Kinematic viscosity (25 ℃, mm) 2 /s) | 52 |
| 4 | Density (20 ℃, g/cm) 3 ) | 1.31 |
| 5 | pH value | 3.1 |
The industrial application situation of the flue gas desulfurization and denitrification unit of a catalytic device of 3.50Mt/a refining in Qinzhou, guangxi:
table 8 example 4 operating parameters of flue gas desulfurization and denitration unit of catalytic apparatus
| Parameter name | Operating parameters |
| Operating temperature of clarification tank (. Degree. C.) | 55～60 |
| The retention amount of water (m) in the clarification tank 3 ) | 120 |
| Amount of treated Water (t/h) | 25 |
| Salt content of wastewater (%) | 1.2 |
| Concentration of wastewater suspended matter (mg/L) | 2500 |
| pH value | 7.0～8.0 |
Application effects
After the flocculating agent is added for 400mg/L, the value of suspended matters in effluent of the clarification tank is not more than 35mg/L, the removal rate of the suspended matters is more than 98.6 percent, COD (chemical oxygen demand) of wastewater is not increased, and the technical requirement that the value of suspended matters in process effluent is not more than 40mg/L is met. The phenomena of corrosion leakage of process equipment pipelines and filter blockage do not occur in the industrial application process of one year, the dissolution and compounding are not needed on the site, and the additive is directly added into a medicine adding tank and injected into a mixing tank, so that the use is convenient and the environment is protected.
Claims (5)
1. The catalytic flue gas desulfurization wastewater flocculant is characterized in that: the flocculant is prepared by compounding a polymeric organic flocculant and an inorganic flocculant, wherein the polymeric organic flocculant is a mixture of poly dimethyl diallyl ammonium chloride and cationic polyacrylamide, and the inorganic flocculant is a mixture of zinc sulfate, magnesium sulfate and polymeric aluminum silicate sulfate; the catalytic flue gas desulfurization wastewater flocculant comprises the following raw materials in percentage by weight:
2 to 6 percent of poly dimethyl diallyl ammonium chloride
0.5 to 2 percent of cationic polyacrylamide
2 to 5 percent of zinc sulfate
0.5 to 2 percent of magnesium sulfate
85 to 95 percent of polymeric aluminum silicate sulfate;
the preparation process of the polyaluminium silicate sulfate controls aluminum: the molar ratio of silicon is 10;
the preparation method of the poly aluminum silicate sulfate comprises the following steps: dropwise adding a water glass solution into a 25wt% sulfuric acid solution, continuously stirring for 30 minutes, controlling the pH of a reaction system to be less than 2, reacting to obtain polysilicic acid, then adding an aluminum sulfate solution into the polysilicic acid, stirring for 2 hours, and curing for 24 hours to obtain the polyaluminum silicate sulfate solution.
2. The catalytic flue gas desulfurization wastewater flocculant of claim 1, characterized in that: the appearance is colorless to light green viscous liquid, the solid content is more than or equal to 20.0 percent, and the kinematic viscosity (25 ℃) is less than or equal to 80mm 2 S, density (20 ℃) is more than or equal to 1.20g/cm 3 The pH value is 2.0-4.0.
3. The preparation method of the catalytic flue gas desulfurization wastewater flocculant of claim 1, characterized by comprising the following steps: adding zinc sulfate and magnesium sulfate into the polymeric aluminum silicate sulfate solution, stirring for dissolving, adding cationic polyacrylamide, continuously stirring until the cationic polyacrylamide is fully dissolved, and finally adding the poly dimethyl diallyl ammonium chloride emulsion, and uniformly stirring to obtain a final product.
4. The preparation method of the catalytic flue gas desulfurization wastewater flocculant according to claim 3, characterized in that: the stirring speed in the preparation process is controlled within 150 r/min.
5. The preparation method of the catalytic flue gas desulfurization wastewater flocculant according to claim 3, characterized in that: adding 4 parts of zinc sulfate and 1 part of magnesium sulfate into 90 parts of poly aluminum silicate sulfate solution, stirring and dissolving, adding 1 part of cationic polyacrylamide, continuously stirring until the cationic polyacrylamide is fully dissolved, and finally adding 4 parts of poly dimethyl diallyl ammonium chloride emulsion, and uniformly stirring to obtain a final product.
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