CN108128906B - High-temperature industrial wastewater treating agent - Google Patents
High-temperature industrial wastewater treating agent Download PDFInfo
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- CN108128906B CN108128906B CN201711430912.2A CN201711430912A CN108128906B CN 108128906 B CN108128906 B CN 108128906B CN 201711430912 A CN201711430912 A CN 201711430912A CN 108128906 B CN108128906 B CN 108128906B
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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
- C02F3/00—Biological treatment of water, waste water, or sewage
- C02F3/34—Biological treatment of water, waste water, or sewage characterised by the microorganisms used
- C02F3/342—Biological treatment of water, waste water, or sewage characterised by the microorganisms used characterised by the enzymes used
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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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
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- C02F1/42—Treatment of water, waste water, or sewage by ion-exchange
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Abstract
The invention provides a high-temperature industrial wastewater treating agent which comprises the following raw materials in parts by weight: 20-25 parts of activated carbon, 10-12 parts of nano ferroferric oxide, 45-50 parts of lipase liquid, 5-8 parts of sepiolite powder, 5-8 parts of zeolite powder, 5-8 parts of medical stone powder, 5-8 parts of vermiculite, 5-8 parts of perlite, 10-12 parts of chitosan, 3-5 parts of sodium humate, 10-12 parts of sodium carboxymethyl starch, 8-10 parts of polyaluminium chloride and 0.5-0.7 part of tea polyphenol. The raw material components for preparing the high-temperature industrial wastewater treatment agent are nontoxic and harmless, secondary pollution after adsorption treatment cannot be caused, and the raw material components can be better promoted and matched with each other by matching with a specific preparation method, so that the excellent water purification effect can be cooperatively exerted, and heavy metal ions and harmful organic substances in the high-temperature industrial wastewater can be well removed.
Description
Technical Field
The invention relates to the technical field of sewage treatment, in particular to a high-temperature industrial wastewater treating agent.
Background
With the development of economy, chemical plants in various places are more and more, the treatment of industrial sewage becomes a hot point concerned by various circles, and the adsorption treatment by adopting activated carbon is a common treatment method, but the adsorption amount of the activated carbon to heavy metal ions and organic matters in wastewater is very small, a large amount of activated carbon is required to be used each time the wastewater is treated, and the cost is high. In the prior art, the activated carbon can be modified by lipase liquid secreted by bacteria, so that the adsorption capacity of the activated carbon on heavy metals and organic matters is improved, but the lipase used for modifying the activated carbon has temperature sensitivity, and loses the activity thereof at high temperature, thereby losing the modification effect of the lipase on the activated carbon. As is known, when industrial wastewater is generated, higher temperature is often accompanied, and therefore, if the existing lipase is used for modifying activated carbon, the prepared modified activated carbon treating agent still has difficulty in achieving excellent treatment effect in high-temperature wastewater; if the industrial wastewater is firstly cooled and then treated by the active carbon treating agent, the treatment cost is greatly increased.
Therefore, it is necessary to develop a high-temperature industrial wastewater treatment agent using activated carbon as a main raw material, so as to improve the adsorption capacity of the activated carbon on organic matters and heavy metal ions in high-temperature wastewater, and simultaneously, fully exert the mutual synergistic effect of the activated carbon and other raw materials, improve the adsorption rate of the treatment agent, reduce the cost and improve the economic benefit.
Disclosure of Invention
In view of the above, the invention provides an environment-friendly and efficient high-temperature industrial wastewater treatment agent with high adsorption rate and low cost.
The invention provides a high-temperature industrial wastewater treating agent which comprises the following raw materials in parts by weight: 20-25 parts of activated carbon, 10-12 parts of nano ferroferric oxide, 45-50 parts of lipase liquid, 5-8 parts of sepiolite powder, 5-8 parts of zeolite powder, 5-8 parts of medical stone powder, 5-8 parts of vermiculite, 5-8 parts of perlite, 10-12 parts of chitosan, 3-5 parts of sodium humate, 10-12 parts of sodium carboxymethyl starch, 8-10 parts of polyaluminium chloride and 0.5-0.7 part of tea polyphenol;
further, the lipase liquid is a lipase liquid secreted by mixed fermentation culture of pseudomonas stutzeri, pseudomonas aeruginosa and aspergillus niger;
further, the pseudomonas stutzeri, pseudomonas aeruginosa and aspergillus niger are mixed according to the proportion of 1: 1: 2 inoculating the mixture into a culture medium for mixed fermentation culture;
further, the total inoculation amount of the pseudomonas stutzeri, the pseudomonas aeruginosa and the aspergillus niger is 8-10% of the volume of a culture medium for fermentation culture;
further, the culture conditions are: the pH value of the culture medium is 7.0-7.2, the culture temperature is 23-28 ℃, the rotating speed of a shaking table is 150-;
further, the preparation method of the culture medium for fermentation culture comprises the following steps: taking 30 parts of beef extract, 15 parts of peptone and 15 parts of sodium chloride according to the parts by weight, dissolving in 1000 parts of distilled water, adjusting the pH to 7.0-7.2 by using 0.1mol/L NaOH solution, and placing in a sterilization pot for sterilization at 121 ℃ for 5 minutes;
further, the treating agent comprises the following raw materials in parts by weight: 22 parts of activated carbon, 11 parts of nano ferroferric oxide, 48 parts of lipase liquid, 7 parts of sepiolite powder, 6 parts of zeolite powder, 6 parts of medical stone powder, 7 parts of vermiculite, 6 parts of perlite, 11 parts of chitosan, 4 parts of sodium humate, 11 parts of sodium carboxymethyl starch, 9 parts of polyaluminium chloride and 0.6 part of tea polyphenol;
further, the particle size of the active carbon is 0.7-0.8 mm; the particle size of the medical stone powder is 100-120 meshes; the particle size of the sepiolite powder is 150-200 meshes; the particle size of the zeolite powder is 100-120 meshes; the particle size of the vermiculite is 2-4 mm; the particle size of the perlite is 2-4 mm;
further, the content of humic acid dry basis in the sodium humate is more than or equal to 55 percent; the content of effective substances in the sodium carboxymethyl starch is more than or equal to 99 percent; the content of alumina in the polyaluminium chloride is more than or equal to 30 percent; the content of the chitosan is more than or equal to 99 percent, and the degree of deacetylation is more than 90 percent;
further, the preparation method of the high-temperature industrial wastewater treatment agent comprises the following steps:
(1) mixing activated carbon, nano ferroferric oxide, lipase liquid and tea polyphenol, adjusting the pH of the mixture to 7.0, then placing the mixture in a shaking table with the rotation speed of 150 plus 155r/min, and treating the mixture for 4 to 5 hours at the temperature of about 25 ℃;
(2) and (2) adding sodium humate and chitosan into the mixture obtained in the step (1), continuously stirring for 30-45min, adding sepiolite powder, zeolite powder, medical stone powder, vermiculite, perlite, sodium carboxymethyl starch and polyaluminium chloride, and mixing and stirring for 1-1.5 h.
The invention has the beneficial effects that:
the raw material components for preparing the high-temperature industrial wastewater treatment agent are nontoxic and harmless, secondary pollution after adsorption treatment cannot be caused, the raw material components have excellent adsorption functions, and the raw material components can be better promoted and matched with each other by matching with a specific preparation method, so that the water purification effect can be exerted synergistically, finally, the prepared treatment agent can be directly used for the high-temperature industrial wastewater, heavy metal ions and harmful organic substances in the high-temperature industrial wastewater can be well removed, and the high-temperature industrial wastewater treatment agent is good in adsorption effect, high in purification efficiency, low in cost and stable in quality.
In the invention, the activated carbon has a certain adsorption rate on heavy metal and organic matters, and the nano ferroferric oxide can also adsorb a certain amount of heavy metal ions; after being mixed, the raw materials can be mutually matched to react with heavy metal ions in industrial wastewater, such as complexation, ion exchange and the like, so that the heavy metal ions can be stably adsorbed, the adsorption stability can be improved, a water-insoluble precipitate can be formed, and the raw materials can be compatible with and adsorbed by organic compounds in the wastewater to form hydrogen bonds and the like, so that harmful substances such as the heavy metal ions and the organic compounds can be simultaneously adsorbed; the lipase liquid is secreted by pseudomonas stutzeri, pseudomonas aeruginosa and aspergillus niger mixed fermentation culture, the lipase liquid can still keep high activity under the high-temperature condition, and has high-temperature stability, the lipase liquid has good adsorption effect on heavy metal ions and organic matters, and meanwhile, the activity of the lipase can be greatly improved by adding tea polyphenol; in the embodiment, the raw material components are fully mixed by a specific preparation method, magnetic nano ferroferric oxide is introduced into the activated carbon, active groups of lipase with high-temperature enzyme activity are introduced into the surfaces of the activated carbon and the nano ferroferric oxide, and the mutual synergy and mutual coordination effect of the raw material components can be well played; due to the bridging action of hydroxide ions and the polymerization action of polyvalent anions, the polyaluminium chloride has larger relative molecular mass and higher charge, and can realize high-degree electric neutralization and bridging action on colloids and particles in the wastewater, thereby powerfully removing heavy metals, colloids, radioactive toxic substances and the like in the wastewater; the medical stone powder, the sepiolite powder and the zeolite powder have higher specific surface area and surface activity due to the own specific loose porous structure, and can increase the contact area with the wastewater, so the medical stone powder, the sepiolite powder and the zeolite powder have unique adsorption, screening, cation and anion exchange and catalytic performances, and can adsorb harmful substances such as organic compounds, heavy metal ions and the like in the wastewater; vermiculite has higher layer charge number, so the vermiculite has higher cation exchange capacity and stronger cation exchange adsorption capacity; the perlite can play a good role in purifying water.
Detailed Description
The embodiment provides a high-temperature industrial wastewater treating agent, which comprises the following raw materials in parts by weight: 20-25 parts of activated carbon, 10-12 parts of nano ferroferric oxide, 45-50 parts of lipase liquid, 5-8 parts of sepiolite powder, 5-8 parts of zeolite powder, 5-8 parts of medical stone powder, 5-8 parts of vermiculite, 5-8 parts of perlite, 10-12 parts of chitosan, 3-5 parts of sodium humate, 10-12 parts of sodium carboxymethyl starch, 8-10 parts of polyaluminium chloride and 0.5-0.7 part of tea polyphenol; the lipase liquid is secreted by pseudomonas stutzeri, pseudomonas aeruginosa and aspergillus niger mixed fermentation culture;
preferably, the treating agent comprises the following raw materials in parts by weight: 22 parts of activated carbon, 11 parts of nano ferroferric oxide, 48 parts of lipase liquid, 7 parts of sepiolite powder, 6 parts of zeolite powder, 6 parts of medical stone powder, 7 parts of vermiculite, 6 parts of perlite, 11 parts of chitosan, 4 parts of sodium humate, 11 parts of sodium carboxymethyl starch, 9 parts of polyaluminium chloride and 0.6 part of tea polyphenol;
the raw material components used for preparing the high-temperature industrial wastewater treatment agent in the embodiment are nontoxic and harmless, secondary pollution after adsorption treatment cannot be caused, the raw material components have excellent adsorption functions, and the raw material components can be better promoted and matched with each other by matching with a specific preparation method, so that the water purification effect can be exerted synergistically, finally, the prepared treatment agent can be directly used for high-temperature industrial wastewater, heavy metal ions and harmful organic substances in the high-temperature industrial wastewater can be well removed, and the high-temperature industrial wastewater treatment agent is good in adsorption effect, high in purification efficiency, low in cost and stable in quality. The activated carbon has a certain adsorption rate on heavy metal and organic matters, and the nano ferroferric oxide can also adsorb a certain amount of heavy metal ions; after being mixed, the raw materials can be mutually matched to react with heavy metal ions in industrial wastewater, such as complexation, ion exchange and the like, so that the heavy metal ions can be stably adsorbed, the adsorption stability can be improved, a water-insoluble precipitate can be formed, and the raw materials can be compatible with and adsorbed by organic compounds in the wastewater to form hydrogen bonds and the like, so that harmful substances such as the heavy metal ions and the organic compounds can be simultaneously adsorbed; the lipase liquid is secreted by pseudomonas stutzeri, pseudomonas aeruginosa and aspergillus niger mixed fermentation culture, the lipase liquid can still keep high activity under the high-temperature condition, and has high-temperature stability, the lipase liquid has good adsorption effect on heavy metal ions and organic matters, and meanwhile, the activity of the lipase can be greatly improved by adding tea polyphenol; in the embodiment, the raw material components are fully mixed by a specific preparation method, magnetic nano ferroferric oxide is introduced into the activated carbon, active groups of lipase with high-temperature enzyme activity are introduced into the surfaces of the activated carbon and the nano ferroferric oxide, and the mutual synergy and mutual coordination effect of the raw material components can be well played; due to the bridging action of hydroxide ions and the polymerization action of polyvalent anions, the polyaluminium chloride has larger relative molecular mass and higher charge, and can realize high-degree electric neutralization and bridging action on colloids and particles in the wastewater, thereby powerfully removing heavy metals, colloids, radioactive toxic substances and the like in the wastewater; the medical stone powder, the sepiolite powder and the zeolite powder have higher specific surface area and surface activity due to the own specific loose porous structure, and can increase the contact area with the wastewater, so the medical stone powder, the sepiolite powder and the zeolite powder have unique adsorption, screening, cation and anion exchange and catalytic performances, and can adsorb harmful substances such as organic compounds, heavy metal ions and the like in the wastewater; vermiculite has higher layer charge number, so the vermiculite has higher cation exchange capacity and stronger cation exchange adsorption capacity; the perlite can play a good role in purifying water.
In the embodiment, the pseudomonas stutzeri, pseudomonas aeruginosa and aspergillus niger are mixed according to the proportion of 1: 1: 2, inoculating the bacillus subtilis and the pseudomonas aeruginosa and the aspergillus niger in a culture medium for mixed fermentation culture, wherein the total inoculation amount of the pseudomonas stutzeri, the pseudomonas aeruginosa and the aspergillus niger is 8-10% of the volume of the culture medium for fermentation culture; the culture conditions are as follows: the pH value of the culture medium is 7.0-7.2, the culture temperature is 23-28 ℃, the rotating speed of a shaking table is 150-; the lipase liquid secreted by the pseudomonas stutzeri, pseudomonas aeruginosa and aspergillus niger which are subjected to synergistic fermentation culture under specific conditions according to a certain proportion can still keep high activity under high temperature conditions, and the lipase liquid has a very good adsorption effect on heavy metal ions and organic matters, and the wastewater treatment agent prepared by the synergistic cooperation of the lipase liquid with the characteristics, activated carbon, ferroferric oxide and the like has excellent high temperature resistance and high adsorption capacity.
In this embodiment, the method for activating pseudomonas stutzeri and pseudomonas aeruginosa comprises:
(1) preparing a culture medium for fermenting and culturing beef extract: weighing 30g of beef extract, 15g of peptone and 15g of sodium chloride, dissolving in 1000mL of distilled water, adjusting pH to 7.0-7.2 by using 0.1mol/L NaOH solution, and then sterilizing in a sterilization pot at 121 ℃ for 5 minutes to obtain the beef extract;
(2) activation of freeze-dried powder: adding the freeze-dried powder into a culture medium for beef extract fermentation culture, slightly shaking to uniformly mix the freeze-dried powder and the beef extract to prepare a bacterial suspension, slightly cooling a sterilized LB solid culture medium to prepare a slant culture medium, transplanting part of the bacterial suspension onto the slant culture medium, culturing in a constant-temperature incubator at 37 ℃ to increase the number of bacterial colonies, selecting and culturing robust bacterial colonies from the slant culture medium, inoculating the robust bacterial colonies onto a new slant culture medium for culturing, and repeating the steps for 2-3 times until a well-grown bacterial strain is obtained.
In this embodiment, the activation method of aspergillus niger is:
(1) preparing an improved martin culture medium: respectively dissolving 5g of peptone, 1.0g of dipotassium phosphate, 2.0g of yeast extract powder and 0.5g of magnesium sulfate in 1000ml of distilled water, adjusting the pH to be about 6.8 by using 0.1mol/L NaOH solution, boiling, adding 20g of glucose for dissolving, shaking up, filtering by using gauze, and adjusting the pH value to be 6.4 +/-0.2;
(2) activation of aspergillus niger freeze-dried powder: and (3) inoculating the preserved aspergillus niger into an improved martin culture medium, performing shaking culture at 23-28 ℃ for about 5-6 days, then scribing the activated bacterial liquid onto an improved martin agar inclined plane (prepared by adding agar into the improved martin culture medium), and performing standing culture at 23-28 ℃ for 6-7 days.
In this embodiment, the preparation method of the culture medium for fermentation culture comprises: taking 30 parts of beef extract, 15 parts of peptone and 15 parts of sodium chloride according to the parts by weight, dissolving in 1000 parts of distilled water, adjusting the pH to 7.0-7.2 by using 0.1mol/L NaOH solution, and placing in a sterilization pot for sterilization at 121 ℃ for 5 minutes; is beneficial to the secretion of high-activity enzyme after mixed culture of pseudomonas stutzeri, pseudomonas aeruginosa and aspergillus niger.
In this embodiment, the method for extracting lipase liquid includes the following steps:
(1) extracting a crude enzyme solution: collecting fermentation liquor, and centrifuging at 4000r/min for 15min to obtain supernatant, i.e. crude enzyme solution;
(2) extracting lipase liquid: taking 3mL of the solution with the concentration of 0.0667 mol.L-1Putting phosphate buffer solution and 1mL of oleic acid into a conical flask, uniformly mixing, putting into a constant-temperature water bath kettle at 37 ℃, preheating for at least 5min, then adding 0.1mL of crude enzyme liquid obtained by extraction in the step (1), stirring for reacting for 10min, immediately adding 8mL of toluene (analytically pure), continuously stirring for reacting for 2min, and stopping the reaction; and centrifuging the solution obtained after the treatment in the steps for at least 10min at 3000r/min, and taking the upper organic mixed solution as lipase liquid.
In this example, the amounts of the phosphate buffer solution, oleic acid, and toluene were adjusted in proportion to the amount of the crude enzyme solution to be extracted.
In the embodiment, the particle size of the activated carbon is 0.7-0.8 mm; the particle size of the medical stone powder is 100-120 meshes; the particle size of the sepiolite powder is 150-200 meshes; the particle size of the zeolite powder is 100-120 meshes; the particle size of the vermiculite is 2-4 mm; the particle size of the perlite is 2-4 mm; is convenient for dispersion and improves the adsorption effect.
In the embodiment, the content of humic acid dry basis in the sodium humate is more than or equal to 55 percent; the content of effective substances in the sodium carboxymethyl starch is more than or equal to 99 percent; the content of alumina in the polyaluminium chloride is more than or equal to 30 percent; the content of the chitosan is more than or equal to 99 percent, and the degree of deacetylation is more than 90 percent; ensuring the number of active groups and improving the adsorption effect.
In this embodiment, the preparation method of the high-temperature industrial wastewater treatment agent includes the following steps:
(1) mixing activated carbon, nano ferroferric oxide, lipase liquid and tea polyphenol, adjusting the pH of the mixture to 7.0, then placing the mixture in a shaking table with the rotation speed of 150 plus 155r/min, and treating the mixture for 4 to 5 hours at the temperature of about 25 ℃;
(2) adding sodium humate and chitosan into the mixture obtained in the step (1), continuously stirring for 30-45min, adding sepiolite powder, zeolite powder, medical stone powder, vermiculite, perlite, sodium carboxymethyl starch and polyaluminium chloride, and mixing and stirring for 1-1.5 h; the preparation method is simple and easy to operate, and by mixing the lipase liquid with high-temperature activity, the tea polyphenol, the activated carbon and the nano ferroferric oxide, the magnetic nano ferroferric oxide can be introduced into the activated carbon, and meanwhile, active groups are introduced into the surfaces of the activated carbon and the nano ferroferric oxide and then are mixed with other raw material components, so that the mutual synergistic effect among the raw material components can be better exerted, and the excellent high-temperature water purification effect is achieved.
The following are specific examples:
example one
The high-temperature industrial wastewater treatment agent provided by the embodiment comprises the following raw materials in parts by weight: 20 parts of activated carbon, 10 parts of nano ferroferric oxide, 45 parts of lipase liquid, 5 parts of sepiolite powder, 5 parts of zeolite powder, 5 parts of medical stone powder, 5 parts of vermiculite, 5 parts of perlite, 10 parts of chitosan, 3 parts of sodium humate, 10 parts of sodium carboxymethyl starch, 8 parts of polyaluminium chloride and 0.5 part of tea polyphenol;
wherein the lipase liquid is prepared from pseudomonas stutzeri, pseudomonas aeruginosa and aspergillus niger according to the proportion of 1: 1: 2 inoculating the lipase liquid into a culture medium for mixed fermentation culture to produce secreted lipase liquid; the total inoculation amount of the pseudomonas stutzeri, the pseudomonas aeruginosa and the aspergillus niger is 10 percent of the volume of a culture medium for fermentation culture; the culture conditions are as follows: the pH value of the culture medium is 7.0, the culture temperature is 23 ℃, the rotating speed of a shaking table is 150r/min, and the culture time is 42 h.
In this embodiment, the method for activating pseudomonas stutzeri and pseudomonas aeruginosa comprises:
(1) preparing a culture medium for fermenting and culturing beef extract: weighing 30g of beef extract, 15g of peptone and 15g of sodium chloride, dissolving in 1000mL of distilled water, adjusting pH to 7.0-7.2 by using 0.1mol/L NaOH solution, and then sterilizing in a sterilization pot at 121 ℃ for 5 minutes to obtain the beef extract;
(2) activation of freeze-dried powder: adding the freeze-dried powder into a culture medium for beef extract fermentation culture, slightly shaking to uniformly mix the freeze-dried powder and the beef extract to prepare a bacterial suspension, slightly cooling a sterilized LB solid culture medium to prepare a slant culture medium, transplanting part of the bacterial suspension onto the slant culture medium, culturing in a constant-temperature incubator at 37 ℃ to increase the number of bacterial colonies, selecting and culturing robust bacterial colonies from the slant culture medium, inoculating the robust bacterial colonies onto a new slant culture medium for culturing, and repeating the steps for 2-3 times until a well-grown bacterial strain is obtained.
In this embodiment, the activation method of aspergillus niger is:
(1) preparing an improved martin culture medium: respectively dissolving 5g of peptone, 1.0g of dipotassium phosphate, 2.0g of yeast extract powder and 0.5g of magnesium sulfate in 1000ml of distilled water, adjusting the pH to be about 6.8 by using 0.1mol/L NaOH solution, boiling, adding 20g of glucose for dissolving, shaking up, filtering by using gauze, and adjusting the pH value to be 6.4 +/-0.2;
(2) activation of aspergillus niger freeze-dried powder: and (3) inoculating the preserved aspergillus niger into an improved martin culture medium, performing shaking culture at 23-28 ℃ for about 5-6 days, then scribing the activated bacterial liquid onto an improved martin agar inclined plane (prepared by adding agar into the improved martin culture medium), and performing standing culture at 23-28 ℃ for 6-7 days.
In this embodiment, the preparation method of the culture medium for fermentation culture comprises: 30 parts of beef extract, 15 parts of peptone and 15 parts of sodium chloride are taken according to the parts by weight and dissolved in 1000 parts of distilled water, then the pH is adjusted to 7.0-7.2 by 0.1mol/L NaOH solution, and the beef extract is placed in a sterilization pot to be sterilized for 5 minutes at the temperature of 121 ℃.
In this embodiment, the method for extracting lipase liquid includes the following steps:
(1) extracting a crude enzyme solution: collecting fermentation liquor, and centrifuging at 4000r/min for 15min to obtain supernatant, i.e. crude enzyme solution;
(2) extracting lipase liquid: taking 3mL of the solution with the concentration of 0.0667 mol.L-1Putting phosphate buffer solution and 1mL of oleic acid into a conical flask, uniformly mixing, putting into a constant-temperature water bath kettle at 37 ℃, preheating for at least 5min, then adding 0.1mL of crude enzyme liquid obtained by extraction in the step (1), stirring for reacting for 10min, immediately adding 8mL of toluene (analytically pure), continuously stirring for reacting for 2min, and stopping the reaction; and centrifuging the solution obtained after the treatment in the steps for at least 10min at 3000r/min, and taking the upper organic mixed solution as lipase liquid.
In this example, the amounts of the phosphate buffer solution, oleic acid, and toluene were adjusted in proportion to the amount of the crude enzyme solution to be extracted.
In the embodiment, the particle size of the activated carbon is 0.7-0.8 mm; the particle size of the medical stone powder is 100-120 meshes; the particle size of the sepiolite powder is 150-200 meshes; the particle size of the zeolite powder is 100-120 meshes; the particle size of the vermiculite is 2-4 mm; the particle size of the perlite is 2-4 mm.
In the embodiment, the content of humic acid dry basis in the sodium humate is more than or equal to 55 percent; the content of effective substances in the sodium carboxymethyl starch is more than or equal to 99 percent; the content of alumina in the polyaluminium chloride is more than or equal to 30 percent; the content of the chitosan is more than or equal to 99 percent, and the degree of deacetylation is more than 90 percent.
In this embodiment, the preparation method of the high-temperature industrial wastewater treatment agent includes the following steps:
(1) mixing activated carbon, nano ferroferric oxide, lipase liquid and tea polyphenol, adjusting the pH of the mixture to 7.0, then placing the mixture in a shaking table with the rotation speed of 150r/min, and treating the mixture for 4 hours at about 25 ℃;
(2) and (2) adding sodium humate and chitosan into the mixture obtained in the step (1), continuously stirring for 30min, adding sepiolite powder, zeolite powder, medical stone powder, vermiculite, perlite, sodium carboxymethyl starch and polyaluminium chloride, and mixing and stirring for 1 h.
Example two
The high-temperature industrial wastewater treatment agent provided by the embodiment comprises the following raw materials in parts by weight: 22 parts of activated carbon, 11 parts of nano ferroferric oxide, 48 parts of lipase liquid, 7 parts of sepiolite powder, 6 parts of zeolite powder, 6 parts of medical stone powder, 7 parts of vermiculite, 6 parts of perlite, 11 parts of chitosan, 4 parts of sodium humate, 11 parts of sodium carboxymethyl starch, 9 parts of polyaluminium chloride and 0.6 part of tea polyphenol;
wherein the lipase liquid is prepared from pseudomonas stutzeri, pseudomonas aeruginosa and aspergillus niger according to the proportion of 1: 1: 2 inoculating the lipase liquid into a culture medium for mixed fermentation culture to produce secreted lipase liquid; the total inoculation amount of the pseudomonas stutzeri, the pseudomonas aeruginosa and the aspergillus niger is 9 percent of the volume of a culture medium for fermentation culture; the culture conditions are as follows: the pH value of the culture medium is 7.2, the culture temperature is 25 ℃, the rotating speed of a shaking table is 155r/min, and the culture time is 48 h.
In this embodiment, the method for activating pseudomonas stutzeri and pseudomonas aeruginosa and the method for activating aspergillus niger are the same as those in the first embodiment; the preparation method of the culture medium for fermentation culture is the same as that of the first embodiment; the extraction method of the lipase liquid is the same as the first embodiment.
In the embodiment, the particle size of the activated carbon is 0.7-0.8 mm; the particle size of the medical stone powder is 100-120 meshes; the particle size of the sepiolite powder is 150-200 meshes; the particle size of the zeolite powder is 100-120 meshes; the particle size of the vermiculite is 2-4 mm; the particle size of the perlite is 2-4 mm.
In the embodiment, the content of humic acid dry basis in the sodium humate is more than or equal to 55 percent; the content of effective substances in the sodium carboxymethyl starch is more than or equal to 99 percent; the content of alumina in the polyaluminium chloride is more than or equal to 30 percent; the content of the chitosan is more than or equal to 99 percent, and the degree of deacetylation is more than 90 percent.
In this embodiment, the preparation method of the high-temperature industrial wastewater treatment agent includes the following steps:
(1) mixing activated carbon, nano ferroferric oxide, lipase liquid and tea polyphenol, adjusting the pH of the mixture to 7.0, then placing the mixture in a shaking table with the rotating speed of 155r/min, and treating the mixture for 4.5 hours at about 25 ℃;
(2) and (2) adding sodium humate and chitosan into the mixture obtained in the step (1), continuously stirring for 40min, adding sepiolite powder, zeolite powder, medical stone powder, vermiculite, perlite, sodium carboxymethyl starch and polyaluminium chloride, and mixing and stirring for 1 h.
EXAMPLE III
The high-temperature industrial wastewater treatment agent provided by the embodiment comprises the following raw materials in parts by weight: 25 parts of activated carbon, 12 parts of nano ferroferric oxide, 50 parts of lipase liquid, 8 parts of sepiolite powder, 8 parts of zeolite powder, 8 parts of medical stone powder, 8 parts of vermiculite, 8 parts of perlite, 12 parts of chitosan, 5 parts of sodium humate, 12 parts of sodium carboxymethyl starch, 10 parts of polyaluminium chloride and 0.7 part of tea polyphenol;
wherein the lipase liquid is prepared from pseudomonas stutzeri, pseudomonas aeruginosa and aspergillus niger according to the proportion of 1: 1: 2 inoculating the lipase liquid into a culture medium for mixed fermentation culture to produce secreted lipase liquid; the total inoculation amount of the pseudomonas stutzeri, the pseudomonas aeruginosa and the aspergillus niger is 10 percent of the volume of a culture medium for fermentation culture; the culture conditions are as follows: the pH of the culture medium is 7.2, the culture temperature is 28 ℃, the rotating speed of the shaking table is 155r/min, and the culture time is 54 h.
In this embodiment, the method for activating pseudomonas stutzeri and pseudomonas aeruginosa and the method for activating aspergillus niger are the same as those in the first embodiment; the preparation method of the culture medium for fermentation culture is the same as that of the first embodiment; the extraction method of the lipase liquid is the same as the first embodiment.
In the embodiment, the particle size of the activated carbon is 0.7-0.8 mm; the particle size of the medical stone powder is 100-120 meshes; the particle size of the sepiolite powder is 150-200 meshes; the particle size of the zeolite powder is 100-120 meshes; the particle size of the vermiculite is 2-4 mm; the particle size of the perlite is 2-4 mm.
In the embodiment, the content of humic acid dry basis in the sodium humate is more than or equal to 55 percent; the content of effective substances in the sodium carboxymethyl starch is more than or equal to 99 percent; the content of alumina in the polyaluminium chloride is more than or equal to 30 percent; the content of the chitosan is more than or equal to 99 percent, and the degree of deacetylation is more than 90 percent.
In this embodiment, the preparation method of the high-temperature industrial wastewater treatment agent includes the following steps:
(1) mixing activated carbon, nano ferroferric oxide, lipase liquid and tea polyphenol, adjusting the pH of the mixture to 7.0, then placing the mixture in a shaking table with the rotating speed of 155r/min, and treating the mixture for 5 hours at about 25 ℃;
(2) and (2) adding sodium humate and chitosan into the mixture obtained in the step (1), continuously stirring for 45min, adding sepiolite powder, zeolite powder, medical stone powder, vermiculite, perlite, sodium carboxymethyl starch and polyaluminium chloride, and mixing and stirring for 1.5h to obtain the product.
Example four
The high-temperature industrial wastewater treatment agent provided by the embodiment comprises the following raw materials in parts by weight: 20 parts of activated carbon, 12 parts of nano ferroferric oxide, 45 parts of lipase liquid, 8 parts of sepiolite powder, 5 parts of zeolite powder, 8 parts of medical stone powder, 5 parts of vermiculite, 8 parts of perlite, 10 parts of chitosan, 5 parts of sodium humate, 10 parts of sodium carboxymethyl starch, 10 parts of polyaluminium chloride and 0.6 part of tea polyphenol;
wherein the lipase liquid is prepared from pseudomonas stutzeri, pseudomonas aeruginosa and aspergillus niger according to the proportion of 1: 1: 2 inoculating the lipase liquid into a culture medium for mixed fermentation culture to produce secreted lipase liquid; the total inoculation amount of the pseudomonas stutzeri, the pseudomonas aeruginosa and the aspergillus niger is 10 percent of the volume of a culture medium for fermentation culture; the culture conditions are as follows: the pH value of the culture medium is 7.0, the culture temperature is 25 ℃, the rotating speed of a shaking table is 155r/min, and the culture time is 48 h.
In this embodiment, the method for activating pseudomonas stutzeri and pseudomonas aeruginosa and the method for activating aspergillus niger are the same as those in the first embodiment; the preparation method of the culture medium for fermentation culture is the same as that of the first embodiment; the extraction method of the lipase liquid is the same as the first embodiment.
In the embodiment, the particle size of the activated carbon is 0.7-0.8 mm; the particle size of the medical stone powder is 100-120 meshes; the particle size of the sepiolite powder is 150-200 meshes; the particle size of the zeolite powder is 100-120 meshes; the particle size of the vermiculite is 2-4 mm; the particle size of the perlite is 2-4 mm.
In the embodiment, the content of humic acid dry basis in the sodium humate is more than or equal to 55 percent; the content of effective substances in the sodium carboxymethyl starch is more than or equal to 99 percent; the content of alumina in the polyaluminium chloride is more than or equal to 30 percent; the content of the chitosan is more than or equal to 99 percent, and the degree of deacetylation is more than 90 percent.
In this embodiment, the preparation method of the high-temperature industrial wastewater treatment agent includes the following steps:
(1) mixing activated carbon, nano ferroferric oxide, lipase liquid and tea polyphenol, adjusting the pH of the mixture to 7.0, then placing the mixture in a shaking table with the rotation speed of 150r/min, and treating the mixture for 4 hours at about 25 ℃;
(2) and (2) adding sodium humate and chitosan into the mixture obtained in the step (1), continuously stirring for 30min, adding sepiolite powder, zeolite powder, medical stone powder, vermiculite, perlite, sodium carboxymethyl starch and polyaluminium chloride, and mixing and stirring for 1 h.
EXAMPLE five
The high-temperature industrial wastewater treatment agent provided by the embodiment comprises the following raw materials in parts by weight: 25 parts of activated carbon, 10 parts of nano ferroferric oxide, 50 parts of lipase liquid, 5 parts of sepiolite powder, 8 parts of zeolite powder, 5 parts of medical stone powder, 8 parts of vermiculite, 5 parts of perlite, 12 parts of chitosan, 3 parts of sodium humate, 12 parts of sodium carboxymethyl starch, 8 parts of polyaluminium chloride and 0.7 part of tea polyphenol;
wherein the lipase liquid is prepared from pseudomonas stutzeri, pseudomonas aeruginosa and aspergillus niger according to the proportion of 1: 1: 2 inoculating the lipase liquid into a culture medium for mixed fermentation culture to produce secreted lipase liquid; the total inoculation amount of the pseudomonas stutzeri, the pseudomonas aeruginosa and the aspergillus niger is 10 percent of the volume of a culture medium for fermentation culture; the culture conditions are as follows: the pH of the culture medium is 7.0, the culture temperature is 25 ℃, the rotating speed of the shaking table is 155r/min, and the culture time is 54 h.
In this embodiment, the method for activating pseudomonas stutzeri and pseudomonas aeruginosa and the method for activating aspergillus niger are the same as those in the first embodiment; the preparation method of the culture medium for fermentation culture is the same as that of the first embodiment; the extraction method of the lipase liquid is the same as the first embodiment.
In the embodiment, the particle size of the activated carbon is 0.7-0.8 mm; the particle size of the medical stone powder is 100-120 meshes; the particle size of the sepiolite powder is 150-200 meshes; the particle size of the zeolite powder is 100-120 meshes; the particle size of the vermiculite is 2-4 mm; the particle size of the perlite is 2-4 mm.
In the embodiment, the content of humic acid dry basis in the sodium humate is more than or equal to 55 percent; the content of effective substances in the sodium carboxymethyl starch is more than or equal to 99 percent; the content of alumina in the polyaluminium chloride is more than or equal to 30 percent; the content of the chitosan is more than or equal to 99 percent, and the degree of deacetylation is more than 90 percent.
In this embodiment, the preparation method of the high-temperature industrial wastewater treatment agent includes the following steps:
(1) mixing activated carbon, nano ferroferric oxide, lipase liquid and tea polyphenol, adjusting the pH of the mixture to 7.0, then placing the mixture in a shaking table with the rotating speed of 155r/min, and treating the mixture for 5 hours at about 25 ℃;
(2) and (2) adding sodium humate and chitosan into the mixture obtained in the step (1), continuously stirring for 45min, adding sepiolite powder, zeolite powder, medical stone powder, vermiculite, perlite, sodium carboxymethyl starch and polyaluminium chloride, and mixing and stirring for 1.5h to obtain the product.
In the above examples, the raw materials were all available on the market.
Putting the treating agent prepared in the first to fifth embodiments into simulated high-temperature industrial wastewater at 50 ℃, wherein the ratio of the treating agent to the wastewater is 10 g: 1L, adjusting the pH value of the wastewater to 6.5 +/-0.5, treating the wastewater for 2 hours at the rotating speed of 150rpm, and testing the COD value before and after treatment and the concentration of contained heavy metal ions, wherein the results are shown in the following table 1.
As can be seen from the above table, the treatment agent prepared by the invention can achieve better purification and removal effects on heavy metal ions and organic pollutants in simulated high-temperature industrial wastewater, and is suitable for treating the high-temperature industrial wastewater; if a better water purification effect is required, the dosage of the treating agent can be increased according to actual needs.
And (3) determining the activity of the lipase liquid:
inoculating pseudomonas stutzeri, pseudomonas aeruginosa and aspergillus niger into the fermentation culture medium for culture, wherein the total inoculation amount is 10% of the volume of the fermentation culture medium, performing fermentation enzyme production culture at 25 ℃ and 150r/min for 42h, extracting lipase liquid according to the extraction method, and determining the activity of the lipase liquid at 35 ℃, 40 ℃, 42 ℃, 45 ℃, 50 ℃ and 55 ℃, wherein the results are shown in the following table 2.
The enzyme activity test method comprises the following steps:
taking 2 100mL triangular bottles, respectively adding 4mL of PVA olive oil emulsion (olive oil and polyvinyl alcohol solution are mixed according to the ratio of l:3, emulsifying for 5min for 3 times by a high-speed emulsifying machine) and 5mL of 0.025mol/LpH 7.5.5 phosphate buffer (the emulsion attached to the bottle wall should be washed down) into a blank bottle (A) and a sample bottle (B), and adding 15mL of 95% ethanol into the bottle A. Preheating in water bath at different temperatures for 5 minutes, adding lipase liquid lmL into each bottle, immediately recording, reacting for 15 minutes, immediately adding 95% ethanol 15mL into bottle B, stopping reaction, adding phenolphthalein indicator 3 drops, titrating with 0.05mol/L standard NaOH to reddish, and respectively adopting V1 and V2 as two groups of consumed NaOH solutions. Ethanol for the control sample should be added before the enzyme solution.
The lipase activity unit (U) is defined as: under the test conditions, the enzyme solution per ml per minute catalyzes the substrate to release 1 μmol of free fatty acid, which is defined as a unit of lipase activity (U), and the calculation formula is as follows:
and V sample: volume of NaOH consumed in the sample bottle at the end of titration (mL)
V, empty: volume of NaOH consumed in control bottle (mL) at the end of titration
TABLE 2
As can be seen from Table 2, the lipase liquid secreted by the mixed fermentation of the Pseudomonas stutzeri, the Pseudomonas aeruginosa and the Aspergillus niger on the fermentation medium can still keep high activity under high temperature, has high temperature stability, and can be used for modifying raw materials such as activated carbon, ferroferric oxide and the like to prepare the treating agent suitable for high-temperature industrial wastewater.
Finally, the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all of them should be covered in the claims of the present invention.
Claims (9)
1. A high-temperature industrial wastewater treating agent is characterized in that: the treating agent comprises the following raw materials in parts by weight: 20-25 parts of activated carbon, 10-12 parts of nano ferroferric oxide, 45-50 parts of lipase liquid, 5-8 parts of sepiolite powder, 5-8 parts of zeolite powder, 5-8 parts of medical stone powder, 5-8 parts of vermiculite, 5-8 parts of perlite, 10-12 parts of chitosan, 3-5 parts of sodium humate, 10-12 parts of sodium carboxymethyl starch, 8-10 parts of polyaluminium chloride and 0.5-0.7 part of tea polyphenol;
the lipase liquid is secreted by pseudomonas stutzeri, pseudomonas aeruginosa and aspergillus niger mixed fermentation culture.
2. A high temperature industrial wastewater treatment agent according to claim 1, wherein: the pseudomonas stutzeri, the pseudomonas aeruginosa and the aspergillus niger are mixed according to the proportion of 1: 1: 2 inoculating the mixture into a culture medium for mixed fermentation culture.
3. A high temperature industrial wastewater treatment agent according to claim 2, wherein: the total inoculation amount of the pseudomonas stutzeri, the pseudomonas aeruginosa and the aspergillus niger is 8-10% of the volume of a culture medium for fermentation culture.
4. A high temperature industrial wastewater treatment agent according to claim 3, wherein: the culture conditions are as follows: the pH value of the culture medium is 7.0-7.2, the culture temperature is 23-28 ℃, the rotation speed of a shaking table is 150-155r/min, and the culture time is at least 42 h.
5. A high temperature industrial wastewater treatment agent according to claim 4, wherein: the preparation method of the culture medium for fermentation culture comprises the following steps: 30 parts of beef extract, 15 parts of peptone and 15 parts of sodium chloride are taken according to the parts by weight and dissolved in 1000 parts of distilled water, then the pH is adjusted to 7.0-7.2 by 0.1mol/L NaOH solution, and the beef extract is placed in a sterilization pot to be sterilized for 5 minutes at the temperature of 121 ℃.
6. A high temperature industrial wastewater treatment agent according to claim 5, wherein: the treating agent comprises the following raw materials in parts by weight: 22 parts of activated carbon, 11 parts of nano ferroferric oxide, 48 parts of lipase liquid, 7 parts of sepiolite powder, 6 parts of zeolite powder, 6 parts of medical stone powder, 7 parts of vermiculite, 6 parts of perlite, 11 parts of chitosan, 4 parts of sodium humate, 11 parts of sodium carboxymethyl starch, 9 parts of polyaluminium chloride and 0.6 part of tea polyphenol.
7. A high temperature industrial wastewater treatment agent according to claim 1, wherein: the particle size of the active carbon is 0.7-0.8 mm; the particle size of the medical stone powder is 100-120 meshes; the particle size of the sepiolite powder is 150-200 meshes; the particle size of the zeolite powder is 100-120 meshes; the particle size of the vermiculite is 2-4 mm; the particle size of the perlite is 2-4 mm.
8. A high temperature industrial wastewater treatment agent according to claim 1, wherein: the content of humic acid dry basis in the sodium humate is more than or equal to 55 percent; the content of effective substances in the sodium carboxymethyl starch is more than or equal to 99 percent; the content of alumina in the polyaluminium chloride is more than or equal to 30 percent; the content of the chitosan is more than or equal to 99 percent, and the degree of deacetylation is more than 90 percent.
9. A high temperature industrial wastewater treatment agent according to claim 1, wherein: the preparation method of the high-temperature industrial wastewater treating agent comprises the following steps:
(1) mixing activated carbon, nano ferroferric oxide, lipase liquid and tea polyphenol, adjusting the pH of the mixture to 7.0, then placing the mixture in a shaking table with the rotation speed of 150 plus 155r/min, and treating for 4-5h at 25 ℃;
(2) and (2) adding sodium humate and chitosan into the mixture obtained in the step (1), continuously stirring for 30-45min, adding sepiolite powder, zeolite powder, medical stone powder, vermiculite, perlite, sodium carboxymethyl starch and polyaluminium chloride, and mixing and stirring for 1-1.5 h.
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| CN106135648A (en) * | 2015-04-17 | 2016-11-23 | 兰瑛 | Lipase compositions and application thereof |
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| CN106925218A (en) * | 2017-04-11 | 2017-07-07 | 安徽博硕科技有限公司 | A kind of kitchen oil stain adsorbent and preparation method thereof |
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