CN112110547B - Microbial carbon source slow-release wax and preparation method and application thereof - Google Patents
Microbial carbon source slow-release wax and preparation method and application thereof Download PDFInfo
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- CN112110547B CN112110547B CN202010953593.9A CN202010953593A CN112110547B CN 112110547 B CN112110547 B CN 112110547B CN 202010953593 A CN202010953593 A CN 202010953593A CN 112110547 B CN112110547 B CN 112110547B
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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
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/105—Phosphorus compounds
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/16—Nitrogen compounds, e.g. ammonia
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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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/06—Nutrients for stimulating the growth of microorganisms
Abstract
The invention relates to the technical field of water treatment, and discloses a microbial carbon source slow-release wax as well as a preparation method and application thereof. The microbial carbon source slow-release wax comprises a waxy carrier, and a water-insoluble microbial carbon source and an auxiliary agent which are distributed in the waxy carrier. The waxy carrier is used for loading the microbial carbon source, so that a growth and propagation place can be provided for beneficial microorganisms, the carbon source is slowly released, the COD (chemical oxygen demand) of a water body is not increased, a continuous, as-needed and controllable carbon source can be provided for the beneficial microorganisms, the carbon nitrogen phosphorus balance is kept, the growth and propagation of the beneficial microorganisms are facilitated, and the water treatment effect can be improved.
Description
Technical Field
The invention relates to the technical field of water treatment, in particular to a microbial carbon source slow-release wax and a preparation method and application thereof.
Background
Nitrogen and phosphorus are important nutrient sources of organisms, and eutrophication of water bodies is easily caused by excessive content of nitrogen and phosphorus in the water bodies. The nitrogen and phosphorus pollution sources are more, and the industrial and mining enterprise wastewater, the livestock and poultry breeding wastewater and the domestic wastewater have higher nitrogen and phosphorus contents. At present, nitrogen and phosphorus pollution becomes an important problem for preventing and treating water pollution.
Microorganisms such as ammonia oxidizing bacteria, nitrosobacteria, nitrifying bacteria and denitrifying bacteria can convert ammonia nitrogen, nitrite nitrogen, nitrate and organic nitrogen in the water body into nitrogen to overflow from the water body, so that the nitrogen content in the water body is reduced; the microorganisms can absorb phosphorus in the normal growth process to meet physiological needs, the microorganisms such as phosphorus accumulating bacteria and the like can absorb the phosphorus in excess to form intracellular polymeric phosphate, and the phosphorus content in the water body can be reduced by utilizing the absorption and conversion of the microorganisms on the phosphorus. Compared with a physical and chemical method, the method for removing nitrogen and phosphorus from the water body by using the microorganisms has the advantages of low treatment cost and less secondary pollution to the environment, is favored by researchers at home and abroad, and is widely applied to sewage treatment and polluted water body treatment.
In the process of microbial nitrogen and phosphorus removal, a large amount of organic carbon sources are consumed for microbial phosphorus uptake, and organic matters with a certain concentration are also required for denitrification to serve as electron donors, but the problem of insufficient carbon sources generally exists in domestic wastewater and polluted water bodies, so that additional carbon sources need to be added to meet the carbon source requirements of microbial phosphorus uptake, denitrification and the like. Chinese patent publication No. CN106830365A discloses a method for biologically decontaminating and purifying water, comprising the following steps: firstly, stirring and separating sludge: adopting movable sludge aeration equipment to re-precipitate sludge at the bottom of the treated rivers and lakes; then, a microorganism survival carrier system is established: putting a carbon source and a microbial bed in the treated rivers and lakes to provide environments for propagation, parasitism and growth of dominant floras; culturing and putting dominant flora: extracting microorganisms with water quality purifying function in river and lake water bodies to form dominant bacterial communities to be thrown into a polluted water body engineering section; installing water body aeration equipment; and finally, the self-purification function of the water body is improved: the dominant flora is rapidly propagated under the action of aeration, nitrifies and degrades sludge and organic matters in water in situ, degrades and converts ammonia, nitrogen and phosphorus pollutants. In the method, the COD in the water body is increased in a short period by directly adding the carbon source, so that the water body is anoxic and the water quality is deteriorated, beneficial microorganisms can grow and reproduce quickly only when the carbon nitrogen phosphorus ratio is in a proper range, and the problems of microorganism metabolism imbalance and the like caused by excessively high early and excessively low later organic carbon content in the water body by directly adding the carbon source are solved, so that the growth and the reproduction of the beneficial microorganisms are not facilitated.
Disclosure of Invention
In order to solve the technical problems, the invention provides a microbial carbon source slow-release wax and a preparation method and application thereof. The microbial carbon source slow-release wax can slowly release the carbon source after being put into the water body to be treated, does not cause the increase of COD (chemical oxygen demand) of the water body, can provide a continuous, as-needed and controllable carbon source for beneficial microorganisms, keeps the balance of carbon, nitrogen and phosphorus, and is beneficial to the growth and the propagation of the beneficial microorganisms.
The specific technical scheme of the invention is as follows:
a microorganism carbon source slow-release wax comprises a wax carrier, and a water-insoluble microorganism carbon source and an auxiliary agent which are distributed in the wax carrier.
After the product is put into a water body to be treated (high nitrogen and high phosphorus), the waxy carrier can be used as a growth and propagation place of beneficial microorganisms (such as bacillus) in the water body, and plays a role in promoting and enriching the beneficial microorganisms; meanwhile, the loaded carbon source is water-insoluble, so that the carbon source can be slowly released in water for a long time, the carbon source substances are complemented with a nitrogen source, a phosphorus source and the like in a water body to serve as a nutrient source of beneficial microorganisms, the growth and the propagation of the beneficial microorganisms are promoted, and finally a layer of microbial film (the number of bacteria cultured on the surface of the waxy carrier can be 9.16 times that of bacteria cultured on the surface of a common filter medium) is formed on the contact surface of the waxy carrier and the water body. The beneficial microorganisms can take nitrogen and phosphorus sources in the water body as nutrient substances in the growth and propagation process, and can effectively reduce indexes such as ammonia nitrogen, total phosphorus and the like in the water body. In addition, a large amount of enzyme is generated after the beneficial microorganisms grow and reproduce, and nitrogen sources and phosphorus sources of macromolecules in the water body can be decomposed into biological nitrate and polyphosphate which can be utilized by nitrobacteria and polyphosphate converting bacteria, so that reactions such as nitrification and denitrification are improved, and indexes such as ammonia nitrogen, total nitrogen and total phosphorus in the water body are reduced. Therefore, the product can be used for water body treatment (such as riverways, ocean lakes, wastewater ponds of factories, culture tail water and the like), and compared with the traditional water body treatment method for directly throwing the carbon source, the product can provide a growth and reproduction place for beneficial microorganisms, the carbon source is slowly released, COD (chemical oxygen demand) in the water body cannot be increased, a continuous, on-demand and controllable carbon source can be provided for the beneficial microorganisms, the carbon-nitrogen-phosphorus balance is kept, and the growth and reproduction of the beneficial microorganisms are facilitated.
Preferably, the waxy carrier comprises the following raw materials in parts by weight: 70-75 parts of soft wax, 20 parts of paraffin wax and 5-10 parts of microcrystalline wax, wherein the total amount is 100 parts; the water-insoluble microbial carbon source comprises the following raw materials: machine oil, PHBV; the mass of the engine oil and the mass of the PHBV are respectively 5-20% and 1-2% of the mass of the waxy carrier; the auxiliary agent comprises the following raw materials: rhamnolipid, water; the rhamnolipid and the water are respectively 1-2% and 1-2% of the mass of the waxy carrier.
Further, the mass of the engine oil, the PHBV, the rhamnolipid and the water is respectively 15%, 1% and 1% of the mass of the waxy carrier.
The PHBV refers to a copolymer of 3-hydroxybutyrate and 3-hydroxyvalerate, and is a microbial degradable material. The PHBV and the engine oil can be used as a microbial carbon source, and the PHBV and the engine oil are combined, so that the method has the following advantages: compared with PHBV, the engine oil is easier to release and is easier to be utilized by microorganisms, so the combination of the engine oil and the PHBV can ensure that the microorganisms have time selectivity when the carbon source is utilized, and is beneficial to the long-acting slow release of the carbon source.
Besides two basic substances, namely a waxy carrier and a carbon source, rhamnolipid can be used as a surfactant, so that the components are better fused; the water can improve the fluidity of the wax liquid, promote the mixing of all the components and enable the porous slow-release wax to better adapt to the water environment.
Preferably, the melting point of the soft wax is 45-50 ℃, the melting point of the paraffin wax is 55-65 ℃, and the melting point of the microcrystalline wax is 60-80 ℃.
Preferably, the microbial carbon source slow-release wax also comprises a calcium alginate fiber net which is distributed in the wax carrier and has a three-dimensional network structure; and the calcium alginate fibers in the calcium alginate fiber net extend to the surface of the waxy carrier and are communicated with the outside; the mass of the calcium alginate fiber net is 30-40% of that of the waxy carrier.
According to the invention, the calcium alginate fiber net with a three-dimensional network structure is arranged in the waxy carrier, after the microbial carbon source slow-release wax is soaked in a solution containing sodium ions, the calcium alginate fibers are subjected to ion exchange and are converted into water-soluble sodium alginate, through three-dimensional network pore passages are formed in the waxy carrier and are communicated with the outside, and water can enter the pore passages to enable beneficial microorganisms in a water body to grow and propagate on the pore walls, so that the contact area of the microorganisms and the water body can be increased, and the water treatment effect is improved.
Although the porosity of the holes prepared by the conventional hole making process (such as air-stirring hole making, hole making agent addition and the like) can be controlled at a high level, the holes are independent from each other and cannot be communicated, so that the water cannot permeate into the waxy carrier, beneficial microorganisms in the water are difficult to enter the holes for growth and propagation, and the microorganisms growing in the holes cannot be in full contact with the water to play a water purifying role. Therefore, compared with the traditional hole making process, the invention can realize the communication between the holes, increase the contact area of the wax carrier and the water body and further improve the water treatment effect. In addition, compared with the traditional hole making process, the method has controllable porosity, can prevent the too high porosity from causing the too fast release of carbon source substances, can prevent the increase of COD (chemical oxygen demand) in the water body and the damage of carbon nitrogen phosphorus balance caused by the carbon source which is not utilized at the initial feeding stage, is not beneficial to the growth and the propagation of beneficial microorganisms, and can also prevent the too low porosity from causing the too small contact area between the waxy carrier and the water body and influencing the water treatment efficiency.
Preferably, the diameter of the calcium alginate fiber is 0.5-1.5 mm.
If the diameter of the calcium alginate fiber is too large, the contact area of the microbial carbon source slow-release wax and a water body after being put into water is too large, carbon source substances are quickly released, and the beneficial microorganisms are not propagated in a large amount at the initial stage of putting, so that COD (chemical oxygen demand) in the water body is increased due to the carbon source which is not utilized, the carbon nitrogen phosphorus balance is damaged, and the growth and the propagation of the beneficial microorganisms are not facilitated; if the diameter of the calcium alginate fiber is too small, the pore channel formed after the fiber is dissolved is too thin, the high-viscosity sodium alginate formed during the fiber dissolution is not easy to dilute into the water body, so that the pore channel is blocked, and impurities in the water body are easy to block the pore channel in the water treatment process, so that water cannot enter the pore channel, and the water treatment effect is influenced.
Preferably, the calcium alginate fiber is a modified calcium alginate fiber, and the preparation method comprises the following steps:
(i) dissolving sodium alginate in water to prepare a sodium alginate solution with the mass fraction of 2-4%; mixing ethanolamine and water according to the volume ratio of 1: 5-8, and adding 1-ethyl- (3-dimethylaminopropyl) carbonyl diimine hydrochloride to prepare a mixed solution; dropwise adding the mixed solution into a sodium alginate solution, wherein the volume ratio of the mixed solution to the sodium alginate solution is 1: 25-30, and stirring for reaction for 3-5 hours to obtain modified sodium alginate;
(ii) dispersing modified sodium alginate and gellan gum into water according to the mass ratio of 1: 0.03-0.05, and adjusting the pH value to 3-4 to obtain a spinning stock solution;
(iii) after the spinning stock solution is sprayed out through a spinneret orifice, the spinning stock solution is solidified into nascent fiber in a calcium chloride solution with the mass fraction of 1-2%;
(iv) and washing and drying the nascent fiber, and then re-twisting to obtain the modified calcium alginate fiber.
Because the diameter of the calcium alginate fiber is smaller, and in the process of dissolving the calcium alginate fiber to enable the waxy carrier to obtain a three-dimensional network pore structure, the ion exchange between the calcium alginate and the sodium ions is a reversible reaction, the calcium ions cannot be completely replaced, so that the formed sodium alginate solution has higher viscosity, and the sodium alginate in the pore cannot be diluted into the water body in time, so that the pore is blocked to isolate the inside of the waxy carrier from the external water body, and the exertion of the pore function is influenced. Therefore, according to the invention, the ethanolamine graft modification is carried out on the sodium alginate, and the carboxyl in the sodium alginate reacts with the amino in the ethanolamine, so that the number of the carboxyl in the sodium alginate is reduced, the combination of calcium ions is reduced, the viscosity of the sodium alginate generated when the fiber is dissolved is reduced, and the pore channel is prevented from being blocked.
The invention blends gellan gum and modified sodium alginate, and has the following functions: 1) the gellan gum has higher viscosity when the pH value is 3-4, can play a role of a thickening agent in wet spinning, and eliminates the influence of ethanolamine graft modification on spinnability; 2) the viscosity of the gellan gum is greatly reduced when the pH value is 5-6, so that the gellan gum can be dissolved in water and flow out of the pore channel by controlling the pH value when the calcium alginate fiber is dissolved, thereby destroying the calcium alginate network structure and being beneficial to the sodium-calcium ion exchange.
Preferably, in the step (i), the mass ratio of the 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride to the sodium alginate is 1: 3.5-5.5.
Preferably, in the step (ii), the mass-to-volume ratio of the modified sodium alginate to the water is 1g: 20-25 mL.
A method for preparing the microbial carbon source slow-release wax, comprising the following steps:
(1) fixing calcium alginate fibers in a mold to form a calcium alginate fiber net with a three-dimensional network structure;
(2) heating and melting soft wax, paraffin wax and microcrystalline wax, adding engine oil and water, stirring uniformly, cooling and agglomerating to obtain wax blocks;
(3) heating the wax block again to melt, fully stirring in the melting process until the wax block is completely melted, adding PHBV and rhamnolipid, and fully mixing to obtain a wax liquid;
(4) pouring the wax liquid into a mold filled with a calcium alginate fiber net, and caking at 0-4 ℃ to obtain the microbial carbon source slow-release wax.
Preferably, in the step (2) and the step (3), the temperature for heating and melting is 60-80 ℃.
A method for water treatment by utilizing the microbial carbon source slow-release wax comprises the following steps: soaking the microbial carbon source slow-release wax in a sodium chloride solution with the pH of 5-6 and the mass fraction of 0.5-2.5%, performing ultrasonic treatment until calcium alginate fibers are completely dissolved, cleaning, and putting into a water body to be treated.
Because the diameter of the calcium alginate fiber is smaller, and the formed sodium alginate solution has higher viscosity in the process of dissolving the calcium alginate fiber to enable the wax carrier to obtain a three-dimensional network pore structure, the sodium alginate in the pore cannot be diluted into a water body in time, and the pore is blocked to isolate the inside of the wax carrier from the outside water body. The invention can increase the temperature of the system and break up the sodium alginate by applying ultrasonic treatment when the fiber is dissolved, thereby accelerating the dissolution of the sodium alginate, reducing the viscosity of the sodium alginate solution and preventing pore channels from being blocked.
Preferably, the power of the ultrasonic treatment is 100-200W.
Compared with the prior art, the invention has the following advantages:
(1) can provide a growth and propagation place for beneficial microorganisms, slowly releases the carbon source, does not cause the increase of COD (chemical oxygen demand) of the water body, can provide a continuous, as-needed and controllable carbon source for the beneficial microorganisms, keeps the balance of carbon, nitrogen and phosphorus, and is beneficial to the growth and propagation of the beneficial microorganisms;
(2) by adding the calcium alginate fiber net into the wax carrier, a through three-dimensional network pore canal can be formed inside the wax block, beneficial microorganisms in the water body can grow and propagate on the pore wall, the contact area of the microorganisms and the water body is increased, and the water treatment efficiency is improved;
(3) by performing ethanolamine graft modification and gellan gum blending on the calcium alginate fibers, the generated sodium alginate can be timely diluted into a water body when the calcium alginate fibers are dissolved, so that the phenomenon that the inside of a waxy carrier is isolated from an external water body due to pore blockage is prevented;
(4) by applying ultrasonic treatment when dissolving the calcium alginate fiber, the dilution of the sodium alginate into water can be accelerated, and the pore channel is prevented from being blocked.
Detailed Description
The present invention will be further described with reference to the following examples.
General examples
A microorganism carbon source slow-release wax comprises a wax carrier, a water-insoluble microorganism carbon source and an auxiliary agent which are distributed in the wax carrier, and a calcium alginate fiber net which is distributed in the wax carrier and has a three-dimensional network structure; the calcium alginate fibers in the calcium alginate fiber net extend to the surface of the waxy carrier and are communicated with the outside.
The waxy carrier comprises the following raw materials in parts by weight: 70-75 parts of soft wax with the melting point of 45-50 ℃, 20 parts of paraffin with the melting point of 55-65 ℃, 5-10 parts of microcrystalline wax with the melting point of 60-80 ℃, and 100 parts of the total amount.
The water-insoluble microbial carbon source comprises the following raw materials: machine oil, PHBV; the mass of the engine oil and the mass of the PHBV are respectively 5-20% and 1-2% of the mass of the waxy carrier.
The auxiliary agent comprises the following raw materials: rhamnolipid, water; the rhamnolipid and the water are respectively 1-2% and 1-2% of the mass of the waxy carrier.
The mass of the calcium alginate fiber net is 30-40% of that of the waxy carrier; the diameter of the calcium alginate fiber is 0.5-1.5 mm.
A method for preparing the microbial carbon source slow-release wax comprises the following steps:
(1) fixing calcium alginate fibers in a mold to form a calcium alginate fiber net with a three-dimensional network structure;
(2) heating and melting soft wax, paraffin wax and microcrystalline wax at 60-80 ℃, adding engine oil and water, stirring uniformly, and cooling and agglomerating to obtain wax blocks;
(3) heating and melting the wax block at 60-80 ℃ again, fully stirring in the melting process until the wax block is completely melted, adding PHBV and rhamnolipid, and fully mixing to obtain wax liquid;
(4) pouring the wax liquid into a mold filled with a calcium alginate fiber net, and caking at 0-4 ℃ to obtain the microbial carbon source slow-release wax.
A method for performing water treatment by using the microbial carbon source slow-release wax comprises the following steps: soaking the microbial carbon source slow-release wax in a sodium chloride solution with the pH of 5-6 and the mass fraction of 0.5-2.5%, performing ultrasonic treatment at 100-200W until calcium alginate fibers are completely dissolved, cleaning, and putting into a water body to be treated.
Optionally, the calcium alginate fiber is a modified calcium alginate fiber, and the preparation method is as follows:
(i) dissolving sodium alginate in water to prepare a sodium alginate solution with the mass fraction of 2-4%; mixing ethanolamine and water according to a volume ratio of 1: 5-8, adding 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride, wherein the mass ratio of the 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride to sodium alginate is 1: 3.5-5.5, and preparing a mixed solution; dropwise adding the mixed solution into a sodium alginate solution, wherein the volume ratio of the mixed solution to the sodium alginate solution is 1: 25-30, and stirring for reaction for 3-5 hours to obtain modified sodium alginate;
(ii) dispersing modified sodium alginate and gellan gum into water according to the mass ratio of 1: 0.03-0.05, wherein the mass volume ratio of the modified sodium alginate to the water is 1g: 20-25 mL, and adjusting the pH value to 3-4 to obtain a spinning stock solution;
(iii) after the spinning stock solution is sprayed out through a spinneret orifice, the spinning stock solution is solidified into nascent fiber in a calcium chloride solution with the mass fraction of 1-2%;
(iv) and washing and drying the nascent fiber, and then re-twisting to obtain the modified calcium alginate fiber.
Example 1
A microorganism carbon source slow-release wax comprises a wax carrier, and a water-insoluble microorganism carbon source and an auxiliary agent which are distributed in the wax carrier.
The waxy carrier comprises the following raw materials in parts by weight: 70 parts of soft wax with the melting point of 45 ℃, 20 parts of paraffin with the melting point of 55 ℃ and 10 parts of microcrystalline wax with the melting point of 60 ℃.
The water-insoluble microbial carbon source comprises the following raw materials: machine oil, PHBV; the mass of the engine oil and the PHBV are respectively 5 percent and 2 percent of the mass of the waxy carrier.
The auxiliary agent comprises the following raw materials: rhamnolipid, water; the weight of the rhamnolipid and the water is 1.5 percent and 2 percent of the weight of the waxy carrier respectively.
A method for preparing the microbial carbon source slow-release wax comprises the following steps:
(1) heating soft wax, paraffin wax and microcrystalline wax at 80 ℃ for melting, adding engine oil and water, stirring uniformly, and cooling for agglomeration to obtain wax blocks;
(2) heating the wax block at 80 ℃ again for melting, fully stirring in the melting process until the wax block is completely melted, adding PHBV and rhamnolipid, and fully mixing to obtain wax liquid;
(3) pouring the wax liquid into a mould, and agglomerating at 0 ℃ to obtain the microbial carbon source slow-release wax.
A method for performing water treatment by using the microbial carbon source slow-release wax comprises the following steps: and putting the microbial carbon source slow-release wax into a water body to be treated.
Example 2
A microorganism carbon source slow-release wax comprises a wax carrier, a water-insoluble microorganism carbon source and an auxiliary agent which are distributed in the wax carrier, and a calcium alginate fiber net which is distributed in the wax carrier and has a three-dimensional network structure; the calcium alginate fibers in the calcium alginate fiber net extend to the surface of the waxy carrier and are communicated with the outside.
The waxy carrier comprises the following raw materials in parts by weight: 70 parts of soft wax with the melting point of 45 ℃, 20 parts of paraffin with the melting point of 55 ℃ and 10 parts of microcrystalline wax with the melting point of 60 ℃.
The water-insoluble microbial carbon source comprises the following raw materials: machine oil, PHBV; the mass of the engine oil and the PHBV are respectively 5 percent and 2 percent of the mass of the waxy carrier.
The auxiliary agent comprises the following raw materials: rhamnolipid, water; the weight of the rhamnolipid and the water is 1.5 percent and 2 percent of the weight of the waxy carrier respectively.
The mass of the calcium alginate fiber net is 30% of that of the waxy carrier; the diameter of the calcium alginate fiber is 0.5 mm.
A method for preparing the microbial carbon source slow-release wax comprises the following steps:
(1) fixing calcium alginate fibers in a die to form a calcium alginate fiber net, wherein the fiber net has a triaxial orthogonal three-dimensional network structure, and the calcium alginate fibers in the three axial directions have equal intervals;
(2) heating soft wax, paraffin wax and microcrystalline wax at 80 ℃ for melting, adding engine oil and water, stirring uniformly, and cooling for agglomeration to obtain wax blocks;
(3) heating the wax block at 80 ℃ again for melting, fully stirring in the melting process until the wax block is completely melted, adding PHBV and rhamnolipid, and fully mixing to obtain wax liquid;
(4) pouring the wax liquid into a mould filled with a calcium alginate fiber net, and caking at 0 ℃ to obtain the microbial carbon source slow-release wax.
A method for performing water treatment by using the microbial carbon source slow-release wax comprises the following steps: soaking the microbial carbon source slow-release wax in a sodium chloride solution with the pH of 5 and the mass fraction of 0.5%, carrying out ultrasonic treatment for 2.5h at 100W, cleaning, and putting into a water body to be treated.
Example 3
A microorganism carbon source slow-release wax comprises a wax carrier, a water-insoluble microorganism carbon source and an auxiliary agent which are distributed in the wax carrier, and a calcium alginate fiber net which is distributed in the wax carrier and has a three-dimensional network structure; the calcium alginate fibers in the calcium alginate fiber net extend to the surface of the waxy carrier and are communicated with the outside.
The waxy carrier comprises the following raw materials in parts by weight: 72 parts of soft wax with the melting point of 48 ℃, 20 parts of paraffin with the melting point of 60 ℃ and 8 parts of microcrystalline wax with the melting point of 70 ℃.
The water-insoluble microbial carbon source comprises the following raw materials: machine oil, PHBV; the mass of the engine oil and the PHBV are respectively 15 percent and 1 percent of the mass of the waxy carrier.
The auxiliary agent comprises the following raw materials: rhamnolipid, water; the weight of the rhamnolipid and the water is 1% and 1% of the weight of the waxy carrier respectively.
The mass of the calcium alginate fiber net is 35% of that of the waxy carrier; the diameter of the calcium alginate fiber is 1 mm.
A method for preparing the microbial carbon source slow-release wax comprises the following steps:
(1) fixing calcium alginate fibers in a die to form a calcium alginate fiber net, wherein the fiber net has a triaxial orthogonal three-dimensional network structure, and the calcium alginate fibers in the three axial directions have equal intervals;
(2) heating soft wax, paraffin wax and microcrystalline wax at 80 ℃ for melting, adding engine oil and water, stirring uniformly, and cooling for agglomeration to obtain wax blocks;
(3) heating the wax block at 80 ℃ again for melting, fully stirring in the melting process until the wax block is completely melted, adding PHBV and rhamnolipid, and fully mixing to obtain wax liquid;
(4) pouring the wax liquid into a mould filled with a calcium alginate fiber net, and caking at 2 ℃ to obtain the microbial carbon source slow-release wax.
A method for performing water treatment by using the microbial carbon source slow-release wax comprises the following steps: soaking the microbial carbon source slow-release wax in a sodium chloride solution with the pH of 5.5 and the mass fraction of 1.5%, carrying out ultrasonic treatment for 2.5h at 150W, cleaning, and putting into a water body to be treated.
Example 4
A microorganism carbon source slow-release wax comprises a wax carrier, a water-insoluble microorganism carbon source and an auxiliary agent which are distributed in the wax carrier, and a calcium alginate fiber net which is distributed in the wax carrier and has a three-dimensional network structure; the calcium alginate fibers in the calcium alginate fiber net extend to the surface of the waxy carrier and are communicated with the outside.
The waxy carrier comprises the following raw materials in parts by weight: 70 parts of soft wax with the melting point of 50 ℃, 20 parts of paraffin with the melting point of 65 ℃, 5 parts of microcrystalline wax with the melting point of 80 ℃, and the total amount is 100 parts.
The water-insoluble microbial carbon source comprises the following raw materials: machine oil, PHBV; the mass of the engine oil and the PHBV are respectively 20 percent and 1.5 percent of the mass of the waxy carrier.
The auxiliary agent comprises the following raw materials: rhamnolipid, water; the weight of the rhamnolipid and the water is 2 percent and 1.5 percent of the weight of the waxy carrier respectively.
The mass of the calcium alginate fiber net is 30-40% of that of the waxy carrier; the diameter of the calcium alginate fiber is 1.5 mm.
A method for preparing the microbial carbon source slow-release wax comprises the following steps:
(1) fixing calcium alginate fibers in a die to form a calcium alginate fiber net, wherein the fiber net has a triaxial orthogonal three-dimensional network structure, and the calcium alginate fibers in the three axial directions have equal intervals;
(2) heating soft wax, paraffin wax and microcrystalline wax at 80 ℃ for melting, adding engine oil and water, stirring uniformly, and cooling for agglomeration to obtain wax blocks;
(3) heating the wax block at 80 ℃ again for melting, fully stirring in the melting process until the wax block is completely melted, adding PHBV and rhamnolipid, and fully mixing to obtain wax liquid;
(4) pouring the wax liquid into a mould filled with a calcium alginate fiber net, and caking at 4 ℃ to obtain the microbial carbon source slow-release wax.
A method for performing water treatment by using the microbial carbon source slow-release wax comprises the following steps: soaking the microbial carbon source slow-release wax in a sodium chloride solution with the pH of 6 and the mass fraction of 2.5%, carrying out ultrasonic treatment for 2.5h at 200W, cleaning, and putting into a water body to be treated.
Example 5
A microorganism carbon source slow-release wax comprises a wax carrier, a water-insoluble microorganism carbon source and an auxiliary agent which are distributed in the wax carrier, and a modified calcium alginate fiber net which is distributed in the wax carrier and has a three-dimensional network structure; the modified calcium alginate fiber in the modified calcium alginate fiber net extends to the surface of the waxy carrier and is communicated with the outside.
The waxy carrier comprises the following raw materials in parts by weight: 70 parts of soft wax with the melting point of 50 ℃, 20 parts of paraffin with the melting point of 65 ℃, 5 parts of microcrystalline wax with the melting point of 80 ℃, and the total amount is 100 parts.
The water-insoluble microbial carbon source comprises the following raw materials: machine oil, PHBV; the mass of the engine oil and the PHBV are respectively 20 percent and 1.5 percent of the mass of the waxy carrier.
The auxiliary agent comprises the following raw materials: rhamnolipid, water; the weight of the rhamnolipid and the water is 2 percent and 1.5 percent of the weight of the waxy carrier respectively.
The mass of the modified calcium alginate fiber net is 30-40% of that of the waxy carrier; the diameter of the modified calcium alginate fiber is 1.5 mm.
The preparation method of the modified calcium alginate fiber comprises the following steps:
(i) dissolving sodium alginate in water to prepare a sodium alginate solution with the mass fraction of 3%; mixing ethanolamine with water according to a volume ratio of 1:6, adding 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride, wherein the mass ratio of the 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride to the sodium alginate is 1:4.5, and preparing a mixed solution; dropwise adding the mixed solution into a sodium alginate solution, wherein the volume ratio of the mixed solution to the sodium alginate solution is 1:27, and stirring for reaction for 4 hours to obtain modified sodium alginate;
(ii) dispersing modified sodium alginate and gellan gum into water according to the mass ratio of 1:0.04, wherein the mass volume ratio of the modified sodium alginate to the water is 1g:25mL, and adjusting the pH value to 3.5 to obtain a spinning stock solution;
(iii) after the spinning solution is sprayed out through a spinneret orifice, the spinning solution is solidified into nascent fiber in a calcium chloride solution with the mass fraction of 1.5%;
(iv) and washing and drying the nascent fiber, and then re-twisting to obtain the modified calcium alginate fiber.
A method for preparing the microbial carbon source slow-release wax comprises the following steps:
(1) fixing the modified calcium alginate fibers in a die to form a modified calcium alginate fiber net, wherein the fiber net has a triaxial orthogonal three-dimensional network structure, and the distances among the modified calcium alginate fibers in the three axial directions are equal;
(2) heating soft wax, paraffin wax and microcrystalline wax at 80 ℃ for melting, adding engine oil and water, stirring uniformly, and cooling for agglomeration to obtain wax blocks;
(3) heating the wax block at 80 ℃ again for melting, fully stirring in the melting process until the wax block is completely melted, adding PHBV and rhamnolipid, and fully mixing to obtain wax liquid;
(4) pouring the wax liquid into a mould filled with the modified calcium alginate fiber net, and caking at 4 ℃ to obtain the microbial carbon source slow-release wax.
A method for performing water treatment by using the microbial carbon source slow-release wax comprises the following steps: soaking the microbial carbon source slow-release wax in a sodium chloride solution with the pH of 6 and the mass fraction of 2.5%, carrying out ultrasonic treatment for 2.5h at 200W, cleaning, and putting into a water body to be treated.
Example 6
A microorganism carbon source slow-release wax comprises a wax carrier, a water-insoluble microorganism carbon source and an auxiliary agent which are distributed in the wax carrier, and a modified calcium alginate fiber net which is distributed in the wax carrier and has a three-dimensional network structure; the modified calcium alginate fiber in the modified calcium alginate fiber net extends to the surface of the waxy carrier and is communicated with the outside.
The waxy carrier comprises the following raw materials in parts by weight: 70 parts of soft wax with the melting point of 50 ℃, 20 parts of paraffin with the melting point of 65 ℃, 5 parts of microcrystalline wax with the melting point of 80 ℃, and the total amount is 100 parts.
The water-insoluble microbial carbon source comprises the following raw materials: machine oil, PHBV; the mass of the engine oil and the PHBV are respectively 20 percent and 1.5 percent of the mass of the waxy carrier.
The auxiliary agent comprises the following raw materials: rhamnolipid, water; the weight of the rhamnolipid and the water is 2 percent and 1.5 percent of the weight of the waxy carrier respectively.
The mass of the modified calcium alginate fiber net is 30-40% of that of the waxy carrier; the diameter of the modified calcium alginate fiber is 1.5 mm.
The preparation method of the modified calcium alginate fiber comprises the following steps:
(i) dissolving sodium alginate in water to prepare a sodium alginate solution with the mass fraction of 3%; mixing ethanolamine with water according to a volume ratio of 1:6, adding 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride, wherein the mass ratio of the 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride to the sodium alginate is 1:4.5, and preparing a mixed solution; dropwise adding the mixed solution into a sodium alginate solution, wherein the volume ratio of the mixed solution to the sodium alginate solution is 1:27, and stirring for reaction for 4 hours to obtain modified sodium alginate;
(ii) dispersing modified sodium alginate into water, wherein the mass-volume ratio of the modified sodium alginate to the water is 1g:25mL, so as to obtain a spinning solution;
(iii) after the spinning solution is sprayed out through a spinneret orifice, the spinning solution is solidified into nascent fiber in a calcium chloride solution with the mass fraction of 1.5%;
(iv) and washing and drying the nascent fiber, and then re-twisting to obtain the modified calcium alginate fiber.
A method for preparing the microbial carbon source slow-release wax comprises the following steps:
(1) fixing the modified calcium alginate fibers in a die to form a modified calcium alginate fiber net, wherein the fiber net has a triaxial orthogonal three-dimensional network structure, and the distances among the modified calcium alginate fibers in the three axial directions are equal;
(2) heating soft wax, paraffin wax and microcrystalline wax at 80 ℃ for melting, adding engine oil and water, stirring uniformly, and cooling for agglomeration to obtain wax blocks;
(3) heating the wax block at 80 ℃ again for melting, fully stirring in the melting process until the wax block is completely melted, adding PHBV and rhamnolipid, and fully mixing to obtain wax liquid;
(4) pouring the wax liquid into a mould filled with the modified calcium alginate fiber net, and caking at 4 ℃ to obtain the microbial carbon source slow-release wax.
A method for performing water treatment by using the microbial carbon source slow-release wax comprises the following steps: soaking the microbial carbon source slow-release wax in a sodium chloride solution with the pH of 6 and the mass fraction of 2.5%, carrying out ultrasonic treatment for 2.5h at 200W, cleaning, and putting into a water body to be treated.
Comparative example 1
A microorganism carbon source slow-release wax comprises a wax carrier, a water-insoluble microorganism carbon source and an auxiliary agent which are distributed in the wax carrier, and a calcium alginate fiber net which is distributed in the wax carrier and has a three-dimensional network structure; the calcium alginate fibers in the calcium alginate fiber net extend to the surface of the waxy carrier and are communicated with the outside.
The waxy carrier comprises the following raw materials in parts by weight: 70 parts of soft wax with the melting point of 45 ℃, 20 parts of paraffin with the melting point of 55 ℃ and 10 parts of microcrystalline wax with the melting point of 60 ℃.
The water-insoluble microbial carbon source comprises the following raw materials: machine oil, PHBV; the mass of the engine oil and the PHBV are respectively 5 percent and 2 percent of the mass of the waxy carrier.
The auxiliary agent comprises the following raw materials: rhamnolipid, water; the weight of the rhamnolipid and the water is 1.5 percent and 2 percent of the weight of the waxy carrier respectively.
The mass of the calcium alginate fiber net is 30% of that of the waxy carrier; the diameter of the calcium alginate fiber is 0.5 mm.
A method for preparing the microbial carbon source slow-release wax comprises the following steps:
(1) fixing calcium alginate fibers in a die to form a calcium alginate fiber net, wherein the fiber net has a triaxial orthogonal three-dimensional network structure, and the calcium alginate fibers in the three axial directions have equal intervals;
(2) heating soft wax, paraffin wax and microcrystalline wax at 80 ℃ for melting, adding engine oil and water, stirring uniformly, and cooling for agglomeration to obtain wax blocks;
(3) heating the wax block at 80 ℃ again for melting, fully stirring in the melting process until the wax block is completely melted, adding PHBV and rhamnolipid, and fully mixing to obtain wax liquid;
(4) pouring the wax liquid into a mould filled with a calcium alginate fiber net, and caking at 0 ℃ to obtain the microbial carbon source slow-release wax.
A method for performing water treatment by using the microbial carbon source slow-release wax comprises the following steps: and soaking the microbial carbon source slow-release wax in a sodium chloride solution with the pH of 5 and the mass fraction of 0.5%, stirring for 2.5h, cleaning, and putting into a water body to be treated.
The sizes of the microbial carbon source slow-release waxes in the examples 1-6 and the comparative example 1 are 35cm multiplied by 25cm, the water source to be treated is culture tail water for culturing Penaeus vannamei Boone, and each 3m of the culture tail water is3Throwing about 1kg of wax block. After the microbial carbon source slow-release wax is put into the water body to be treated for 24 hours and 48 hours, the contents of ammonia nitrogen, nitric acid nitrogen and nitrous acid nitrogen in the water body are respectively measured, and the results are shown in table 1.
TABLE 1
1Blank: no microbial carbon source slow release wax is added;
2directly adding a carbon source: i.e. no waxy carrier is used; the kind and amount of carbon source charged were the same as those of the carbon source in the microbial carbon source sustained-release wax charged in example 1.
From table 1, the content of ammonia nitrogen, nitric acid nitrogen and nitrous acid nitrogen in the water body in example 1 is reduced faster than that of the carbon source directly input, which indicates that the water treatment efficiency can be improved by loading the carbon source with the waxy carrier, because: compared with the traditional water body treatment method for directly feeding the carbon source, the waxy carrier can provide a growth and propagation place for beneficial microorganisms, can slowly release the carbon source, cannot cause the increase of COD (chemical oxygen demand) in the water body, can provide a continuous, on-demand and controllable carbon source for the beneficial microorganisms, keeps the carbon nitrogen phosphorus balance, and is beneficial to the growth and propagation of the beneficial microorganisms.
Based on example 1, example 2 added a polyvinyl alcohol fiber mesh to the microbial carbon source slow release wax. From table 1, the content of ammonia nitrogen, nitrate nitrogen and nitrite nitrogen in the water body in example 2 is reduced faster, which shows that the water treatment efficiency of the microbial carbon source slow-release wax can be effectively improved by adding the calcium alginate fiber in the invention, because: after the calcium alginate fiber mesh is dissolved, interconnected reticular pores are formed in the wax block, the pores are communicated with the outside, and water can enter the pores, so that beneficial microorganisms in the water can grow and propagate on the pore walls, and the contact area between the microorganisms growing in the slow-release wax and the water can be increased, thereby improving the water treatment efficiency.
Based on example 4, example 6 uses ethanolamine to modify calcium alginate fibers. From table 1, the content of ammonia nitrogen, nitrate nitrogen and nitrite nitrogen in the water body in example 6 is reduced faster, which shows that the water treatment efficiency of the microbial carbon source slow-release wax can be improved by using the ethanolamine modified calcium alginate fiber, because: because the diameter of the calcium alginate fiber is smaller, and in the process of dissolving the calcium alginate fiber to enable the waxy carrier to obtain a three-dimensional network pore structure, the ion exchange between the calcium alginate and the sodium ions is a reversible reaction, the calcium ions cannot be completely replaced, so that the formed sodium alginate solution has higher viscosity, and the sodium alginate in the pore cannot be diluted into the water body in time, so that the pore is blocked to isolate the inside of the waxy carrier from the external water body, and the exertion of the pore function is influenced. The ethanolamine graft modification performance is carried out on the sodium alginate, so that the number of carboxyl groups in the sodium alginate is reduced, the combination of calcium ions is reduced, the viscosity of the sodium alginate generated during fiber dissolution is reduced, and pore channels are prevented from being blocked.
Based on example 6, example 5 adopts a method of blending with gellan gum to prepare modified calcium alginate fiber. From table 1, the content of ammonia nitrogen, nitric acid nitrogen and nitrous acid nitrogen in the water body in example 5 is reduced faster, which indicates that the gellan gum blended fabric can improve the water treatment efficiency of the microbial carbon source slow-release wax, because: the gellan gum has higher viscosity when the pH value is 3-4, can play a role of a thickening agent in wet spinning, and eliminates the influence of ethanolamine graft modification on spinnability; the viscosity of the gellan gum is greatly reduced when the pH value is 5-6, and the gellan gum can be dissolved in water and flow out of the pore channel when the calcium alginate fiber is dissolved, so that the calcium alginate network structure is broken, and the sodium-calcium ion exchange is facilitated.
Comparative example 1 no ultrasonic treatment was used to dissolve the calcium alginate fibers, and the dissolution time and the rest of the procedure were the same as in example 2. From table 1, the content of ammonia nitrogen, nitrate nitrogen and nitrite nitrogen in the water body in example 2 is reduced faster, which indicates that the water treatment efficiency of the microorganism carbon source slow-release wax can be improved by adopting ultrasonic treatment when dissolving calcium alginate fibers, because: ultrasonic treatment is applied during fiber dissolution, so that the temperature of the system can be raised, and sodium alginate is scattered, thereby accelerating sodium alginate dissolution, reducing the viscosity of a sodium alginate solution, and preventing pore channel blockage.
The raw materials and equipment used in the invention are common raw materials and equipment in the field if not specified; the methods used in the present invention are conventional in the art unless otherwise specified.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and all simple modifications, alterations and equivalents of the above embodiments according to the technical spirit of the present invention are still within the protection scope of the technical solution of the present invention.
Claims (10)
1. The microbial carbon source slow-release wax is characterized by comprising a waxy carrier, a calcium alginate fiber net which is distributed in the waxy carrier and has a three-dimensional network structure, and a water-insoluble microbial carbon source and an auxiliary agent which are distributed in the waxy carrier; the calcium alginate fibers in the calcium alginate fiber net extend to the surface of the waxy carrier and are communicated with the outside.
2. The microbial carbon source slow release wax of claim 1, wherein:
the waxy carrier comprises the following raw materials in parts by weight: 70-75 parts of soft wax, 20 parts of paraffin wax and 5-10 parts of microcrystalline wax, wherein the total amount is 100 parts;
the water-insoluble microbial carbon source comprises the following raw materials: machine oil, PHBV; the mass of the engine oil and the mass of the PHBV are respectively 5-20% and 1-2% of the mass of the waxy carrier;
the auxiliary agent comprises the following raw materials: rhamnolipid, water; the rhamnolipid and the water are respectively 1-2% and 1-2% of the mass of the waxy carrier.
3. The microbial carbon source slow-release wax as claimed in claim 2, wherein the melting point of the soft wax is 45-50 ℃, the melting point of the paraffin wax is 55-65 ℃, and the melting point of the microcrystalline wax is 60-80 ℃.
4. The microbial carbon source slow-release wax as claimed in claim 2, wherein the mass of the calcium alginate fiber net is 30-40% of the mass of the waxy carrier.
5. The microbial carbon source slow-release wax as claimed in claim 4, wherein the diameter of the calcium alginate fiber is 0.5-1.5 mm.
6. The microbial carbon source slow-release wax of claim 4 or 5, wherein the calcium alginate fiber is a modified calcium alginate fiber, and the preparation method comprises the following steps:
(i) dissolving sodium alginate in water to prepare a sodium alginate solution with the mass fraction of 2-4%; mixing ethanolamine and water according to the volume ratio of 1: 5-8, and adding 1-ethyl- (3-dimethylaminopropyl) carbonyl diimine hydrochloride to prepare a mixed solution; dropwise adding the mixed solution into a sodium alginate solution, wherein the volume ratio of the mixed solution to the sodium alginate solution is 1: 25-30, and stirring for reaction for 3-5 hours to obtain modified sodium alginate;
(ii) dispersing modified sodium alginate and gellan gum into water according to the mass ratio of 1: 0.03-0.05, and adjusting the pH value to 3-4 to obtain a spinning stock solution;
(iii) after the spinning stock solution is sprayed out through a spinneret orifice, the spinning stock solution is solidified into nascent fiber in a calcium chloride solution with the mass fraction of 1-2%;
(iv) and washing and drying the nascent fiber, and then re-twisting to obtain the modified calcium alginate fiber.
7. The microbial carbon source slow-release wax as claimed in claim 6, wherein in the step (i), the mass ratio of the 1-ethyl- (3-dimethylaminopropyl) carbodiimide hydrochloride to the sodium alginate is 1: 3.5-5.5.
8. A method for preparing the microbial carbon source slow-release wax as claimed in any one of claims 4 to 7, which comprises the following steps:
(1) fixing calcium alginate fibers in a mold to form a calcium alginate fiber net with a three-dimensional network structure;
(2) heating and melting soft wax, paraffin wax and microcrystalline wax, adding engine oil and water, stirring uniformly, cooling and agglomerating to obtain wax blocks;
(3) heating the wax block again to melt, fully stirring in the melting process until the wax block is completely melted, adding PHBV and rhamnolipid, and fully mixing to obtain a wax liquid;
(4) pouring the wax liquid into a mold filled with a calcium alginate fiber net, and caking at 0-4 ℃ to obtain the microbial carbon source slow-release wax.
9. A method for water treatment by using the microbial carbon source slow-release wax as claimed in any one of claims 4 to 7, which comprises the following steps: soaking the microbial carbon source slow-release wax in a sodium chloride solution with the pH of 5-6 and the mass fraction of 0.5-2.5%, performing ultrasonic treatment until calcium alginate fibers are completely dissolved, cleaning, and putting into a water body to be treated.
10. The method of claim 9, wherein the power of the sonication is 100-200W.
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