CN111109299A - Preparation method of algistat containing ginkgo endophyte - Google Patents
Preparation method of algistat containing ginkgo endophyte Download PDFInfo
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- CN111109299A CN111109299A CN201911345276.2A CN201911345276A CN111109299A CN 111109299 A CN111109299 A CN 111109299A CN 201911345276 A CN201911345276 A CN 201911345276A CN 111109299 A CN111109299 A CN 111109299A
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
- A01N37/36—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a singly bound oxygen or sulfur atom attached to the same carbon skeleton, this oxygen or sulfur atom not being a member of a carboxylic group or of a thio analogue, or of a derivative thereof, e.g. hydroxy-carboxylic acids
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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
- C02F1/50—Treatment of water, waste water, or sewage by addition or application of a germicide or by oligodynamic treatment
Abstract
The invention discloses a preparation method of an algistat containing ginkgo endophyte, belonging to the technical field of water body treatment. The invention extracts ginkgo endophyte from ginkgo bark and leaves and attaches the ginkgo endophyte to the algistat component, the ginkgo endophyte has good sterilization and bacteriostasis capability, the pollution of the algistat to the environment can be reduced by utilizing the ginkgo endophyte, simultaneously, components such as plant fiber, lignin and the like are extracted from ginkgo tree bark and leaves, carbonized fiber is generated in the subsequent carbonization process, meanwhile, carbonized particles formed by carbonizing sugar molecules are embedded in the fiber, the algae removal efficiency of the algae inhibitor is enhanced, the effect is fast, a silicon dioxide component is introduced into the fiber component, a silicate component is adsorbed in the plant fiber, after the pH value is adjusted and the high-temperature treatment is carried out, the silicon dioxide nanometer molecules are generated in the carbon fiber structure again, the roughness of the surface of the carbon fiber is improved, meanwhile, the carbon fibers are coated and protected to a certain extent, so that the growth environment of the ginkgo endophyte is protected, and the algae removal aging of the algae inhibitor is improved.
Description
Technical Field
The invention discloses a preparation method of an algistat containing ginkgo endophyte, belonging to the technical field of water body treatment.
Background
With the development of economy and the increase of human activities, the eutrophication of water bodies in lakes and reservoirs is becoming more and more serious. The algal bloom phenomenon caused by water eutrophication not only brings serious harm to an ecological system, but also seriously threatens the health and survival of human beings, increases the treatment and maintenance cost of the water body, causes the imbalance of the water ecological environment and becomes one of the important challenges in the field of water resource environment.
Algal blooms are a disaster phenomenon frequently occurring in seawater and fresh water areas at present, and are called red tides in the sea and water blooms in the fresh water. The algae capable of forming bloom are mainly of the cyanobacteria and chlorophyta species. In eutrophic fresh water bodies, microcystis aeruginosa and anabaena sarcina are the most common.
In the emergency treatment method of blue-green algae outbreak, adding a chemical agent and a biological agent is a more applied technology. Although the addition of oxidants such as potassium permanganate and sodium hypochlorite in the water body can directly kill the algae, the indigenous biological ecological environment with the background having the restoration function is damaged. In order to avoid the failure of the biological ecological restoration measures, the starting of the water body biological ecological restoration system must be prolonged to the point that the oxidant fails, the starting time of the system is prolonged, and the initial restoration effect of the system is also influenced. The salts containing copper ions, such as copper sulfate and the like, mainly kill algae by depending on the toxicity of heavy metals, and also destroy the background biological ecosystem, and the method is more dangerous because the method introduces the heavy metal ions into the water body. In comparison, the flocculating agent is relatively mild, takes effect for a short time and has good water body clarification effect, but the flocculating agent can only realize the flocculation precipitation algae removal of the overlying water and cannot realize the long-acting algae inhibition of the water body.
The current algae control technologies mainly include the following: physical methods such as isolation method, air-float method, ultrasonic method, activated carbon adsorption, micro-filter algae removal, etc.; chemical methods such as chemical oxidation, addition of chemical algaecide, strengthening of flocculation precipitation agent, etc.; biological methods such as ecological wetland technology and utilization of plant allelochemicals. Among them, the physical method has poor effect of killing the bottom layer or low density algae, the cost is high, and the large area use is difficult. The chemical method has the characteristic of rapidness and effectiveness, and is most widely applied. However, the chemical agent is easy to cause secondary pollution, has the defects of high cost, difficult control, easy damage to ecological environment and the like, and endangers the safety of aquatic organisms and even human beings. Because of its high efficiency, fast speed and good ecological safety, allelochemicals are widely concerned by scholars at home and abroad.
The algistat can quickly exert the algae-inhibiting effect to relieve the water bloom, so that the algistat becomes one of the emergency treatment methods of the water bloom. The algistats can be classified into physical algistats, chemical algistats and biochemical algistats, and the properties of the algistats are as follows: physical algistat: the algae inhibiting effect is obvious, but the algae inhibiting effect can be achieved only after a long time, and metal ions such as iron, aluminum and the like can be introduced into the water body, and the pollution is still caused although the pollution is low; chemical algistat: the composition has quick response, has toxicity to aquatic organisms while killing algae, and often has the hidden trouble of secondary pollution; biological algistat: low toxicity and low cost.
Therefore, the invention of the algistat with quick effect and long failure is necessary to the technical field of water body treatment.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: aiming at the defects of slow effect and short algae removal time effect of the existing algae inhibitor, the preparation method of the algae inhibitor containing the gingko endophyte is provided.
In order to solve the technical problems, the invention adopts the technical scheme that:
a preparation method of an algistat containing gingko endophyte comprises the following steps:
putting the filtrate and a citric acid solution with the mass fraction of 6-10% into a beaker, stirring for 30-40 min at the rotating speed of 1200-1300 r/min by using a stirrer to prepare an organic solvent, putting the organic solvent and a carbonized base material into a stirring kettle, stirring for 50-60 min at the rotating speed of 60-80 r/min, standing for 3-5 days after stirring, filtering after standing to obtain a modified filter cake, putting the filter cake into an oven for drying, and grinding and crushing to obtain the gingko endophyte-containing algistat;
the concrete preparation steps of the carbonized base material are as follows:
(1) putting the heat treatment reaction liquid into a three-neck flask, putting the three-neck flask into a water bath kettle with a water bath temperature of 90-100 ℃, dropwise adding an acetic acid solution with the mass fraction of 6-10% into the three-neck flask to adjust the pH value, stirring for 40-50 min at the constant temperature by using a stirring device at the rotating speed of 500-600 r/min, filtering after stirring to obtain a filter cake, and cleaning the filter cake for 3-5 times by using distilled water to obtain a prefabricated product;
(2) placing the prefabricated product in a muffle furnace, raising the temperature in the muffle furnace to 80-90 ℃, preheating for 30-40 min, filling argon into the muffle furnace after preheating, raising the temperature in the muffle furnace, reacting at constant temperature for 60-80 min, putting the reaction product into a planetary ball mill, and performing ball-material ratio of 10 at a rotating speed of 60-80 r/min: grinding for 30-40 min under the condition of 1 to prepare carbonized base stock;
the specific preparation steps of the heat treatment reaction liquid are as follows:
(1) putting ginkgo tree barks and ginkgo leaves into a grinder to be ground to obtain a mixture, putting the mixture into an oven, drying for 2-3 hours at the temperature of 40-50 ℃ to obtain a dried material, and mixing the dried material with absolute ethyl alcohol according to the mass ratio of 1:10, putting the beaker into a beaker, placing the beaker into a shaking table, shaking and soaking for 3-4 h, and performing suction filtration and separation after soaking to obtain filter residue and filtrate;
(2) putting the filter residue into a reaction kettle, soaking the filter residue in hydrochloric acid with the mass fraction of 3-6%, sealing the reaction kettle, raising the temperature in the reaction kettle to 60-70 ℃, stirring the mixture for 2-3 hours at the constant temperature by using a stirrer at the rotating speed of 400-500 r/min, dropwise adding a sodium hydroxide solution with the mass fraction of 10-15% into a beaker after stirring, and adjusting the pH value to prepare an alkaline mixed solution;
(3) and putting the alkaline mixed solution and silicon dioxide powder into a reaction kettle, filling nitrogen into the reaction kettle to increase the pressure in the reaction kettle to 1.2-1.4 MPa, increasing the temperature in the reaction kettle to 150-170 ℃, reacting for 1-2 h at constant temperature and constant pressure, and stirring for 80-100 min at the rotating speed of 600-700 r/min by using a stirrer after reaction to prepare the heat treatment reaction solution.
The mass ratio of the filtrate to the citric acid solution with the mass fraction of 6-10% is 1: 10.
The mass ratio of the organic solvent to the carbonized base material is 10: 1.
Specifically, the pH value adjusted by dripping an acetic acid solution with the mass fraction of 6-10% in the step (1) for preparing the carbonized base material is 6.0-6.5.
And (3) specifically preparing the carbonized base material, wherein the temperature in the muffle furnace is increased to 350-400 ℃.
The mass ratio of the ginkgo tree bark to the ginkgo tree leaves in the specific preparation step (1) of the heat treatment reaction liquid is 5: 1.
The mass ratio of the dry material to the absolute ethyl alcohol in the specific preparation step (1) of the heat treatment reaction liquid is 1: 10.
specifically, in the step (2) for preparing the heat treatment reaction liquid, the pH value adjusted by dropwise adding a sodium hydroxide solution with the mass fraction of 10-15% is 10-12.
The mass ratio of the alkaline mixed solution to the silica powder in the specific preparation step (3) of the heat-treated reaction solution is 20: 1.
The beneficial technical effects of the invention are as follows:
firstly, mixing ginkgo bark and ginkgo leaves, crushing and drying, soaking the ginkgo bark and the ginkgo leaves in absolute ethyl alcohol after drying, leaching to obtain filter residue and filtrate after soaking, then soaking the filter residue in hydrochloric acid, adding alkali liquor after heating at high temperature to prepare alkaline mixed liquor, then adding silicon dioxide powder into the alkaline mixed liquor to perform high-temperature high-pressure reaction to prepare heat treatment reaction liquid, then dropwise adding acetic acid into the heat treatment reaction liquid, stirring and filtering to obtain a prefabricated product, then putting the prefabricated product into a muffle furnace to perform high-temperature treatment to prepare a carbonized base material, finally mixing the filtrate with citric acid solution, then adding the carbonized base material into the mixture to soak, filtering, drying and grinding to obtain the ginkgo endophyte algicide contained in the ginkgo, the ginkgo endophyte extracted from the ginkgo bark and the ginkgo leaves is attached to the algicide component, and has good sterilization and bacteriostasis capacity, the ginkgo endophyte is utilized to reduce the pollution of the algistat to the environment, simultaneously components such as plant fiber, lignin and the like are extracted from ginkgo tree barks and leaves, fiber components, lignin and other organic components are hydrolyzed under high temperature and high pressure and an alkali liquor environment, molecular chains are broken to generate micromolecular fiber components and carbohydrate compounds, the improvement of the decomposition degree of the organic components is beneficial to the increase of the contact area of each organic component and the surrounding environment, the specific surface area of the organic components is improved, carbonized fiber is generated in the subsequent carbonization process, simultaneously carbonized particles formed by the carbonization of sugar molecules are embedded in the carbonized fiber, covalent bonds are formed between the carbonized fiber and the surrounding components in the carbonization process, the structural strength of the carbonized fiber is further improved, the carbonized fiber can bond the ginkgo endophyte, the ginkgo endophyte can be generated in a carbonized structure as a substrate material, and simultaneously has good adsorption effect on algae organisms in water, the algaecide has the advantages that the algaecide is enhanced in algae removal efficiency, the effect is fast, the silicon dioxide component is introduced into the fiber component, the silicate component is adsorbed in the plant fiber, the silicon dioxide nano molecules are generated in the carbon fiber structure again after the pH value is adjusted and the high-temperature treatment is carried out, the surface roughness of the carbon fiber is improved, meanwhile, the carbon fiber is coated and protected to a certain extent, the growth environment of the gingko endophyte is protected, the algae removal aging of the algaecide is improved, and the algaecide has a wide application prospect.
Detailed Description
Putting ginkgo tree barks and ginkgo leaves into a grinder according to a mass ratio of 5:1 to be ground to obtain a mixture, putting the mixture into an oven, drying for 2-3 hours at the temperature of 40-50 ℃ to obtain a dried material, and mixing the dried material with absolute ethyl alcohol according to a mass ratio of 1:10, putting the beaker into a beaker, placing the beaker into a shaking table, shaking and soaking for 3-4 h, and performing suction filtration and separation after soaking to obtain filter residue and filtrate for later use; putting the filter residues into a reaction kettle, soaking the filter residues in hydrochloric acid with the mass fraction of 3-6%, sealing the reaction kettle, raising the temperature in the reaction kettle to 60-70 ℃, stirring the mixture for 2-3 hours at the constant temperature by using a stirrer at the rotating speed of 400-500 r/min, dropwise adding a sodium hydroxide solution with the mass fraction of 10-15% into a beaker after stirring, and adjusting the pH value to 10-12 to prepare an alkaline mixed solution; putting the alkaline mixed solution and silicon dioxide powder into a reaction kettle according to the mass ratio of 20:1, filling nitrogen into the reaction kettle to increase the pressure in the reaction kettle to 1.2-1.4 MPa, increasing the temperature in the reaction kettle to 150-170 ℃, reacting for 1-2 h at constant temperature and constant pressure, and stirring for 80-100 min at the rotating speed of 600-700 r/min by using a stirrer after reaction to prepare a heat treatment reaction solution; putting the heat treatment reaction liquid into a three-neck flask, putting the three-neck flask into a water bath kettle with a water bath temperature of 90-100 ℃, dropwise adding an acetic acid solution with the mass fraction of 6-10% into the three-neck flask to adjust the pH value to 6.0-6.5, stirring for 40-50 min at the constant temperature by using a stirring device at the rotating speed of 500-600 r/min, filtering after stirring to obtain a filter cake, and cleaning the filter cake for 3-5 times by using distilled water to obtain a prefabricated product; placing the prefabricated product in a muffle furnace, raising the temperature in the muffle furnace to 80-90 ℃, preheating for 30-40 min, filling argon into the muffle furnace after preheating, raising the temperature in the muffle furnace to 350-400 ℃, reacting at a constant temperature for 60-80 min, putting the reaction product into a planetary ball mill, and performing ball-material ratio of 10 at a rotating speed of 60-80 r/min: grinding for 30-40 min under the condition of 1 to prepare carbonized base stock; putting the standby filtrate and 6-10% citric acid solution into a beaker according to the mass ratio of 1:10, stirring the mixture by using a stirrer at the rotating speed of 1200-1300 r/min for 30-40 min to prepare an organic solvent, putting the organic solvent and the carbonized base material into a stirring kettle according to the mass ratio of 10:1, stirring the mixture for 50-60 min under the condition that the rotating speed is 60-80 r/min, standing the mixture for 3-5 days after stirring, filtering the mixture to obtain a modified filter cake, putting the modified filter cake into an oven for drying, and grinding and crushing the dried filter cake to obtain the gingko endophyte algistat.
Example 1
Preparation of heat treatment reaction liquid:
putting ginkgo tree barks and ginkgo leaves into a pulverizer according to the mass ratio of 5:1, pulverizing to obtain a mixture, putting the mixture into an oven, drying for 2 hours at the temperature of 40 ℃ to obtain a dried material, and mixing the dried material with absolute ethyl alcohol according to the mass ratio of 1:10, putting the beaker into a shaking table, shaking and soaking for 3 hours, and performing suction filtration and separation after soaking to obtain filter residue and filtrate for later use;
putting the filter residues into a reaction kettle, soaking the filter residues in hydrochloric acid with the mass fraction of 3%, sealing the reaction kettle, raising the temperature in the reaction kettle to 60 ℃, stirring the mixture for 2 hours at the constant temperature by using a stirrer at the rotating speed of 400r/min, dropwise adding a sodium hydroxide solution with the mass fraction of 10% into a beaker after stirring, and adjusting the pH value to 10 to obtain an alkaline mixed solution;
putting the alkaline mixed solution and silicon dioxide powder into a reaction kettle according to the mass ratio of 20:1, filling nitrogen into the reaction kettle to increase the air pressure in the reaction kettle to 1.2MPa, increasing the temperature in the reaction kettle to 150 ℃, carrying out constant-temperature and constant-pressure reaction for 1h, and stirring the mixture for 80min at the rotating speed of 600r/min by using a stirrer after the reaction to prepare a heat treatment reaction solution;
preparing a carbonized base material:
putting the heat treatment reaction liquid into a three-neck flask, putting the three-neck flask into a water bath kettle with the water bath temperature of 90 ℃, dropwise adding an acetic acid solution with the mass fraction of 6% into the three-neck flask to adjust the pH value to 6.0, stirring for 40min at the constant temperature by using a stirring device at the rotating speed of 500r/min, filtering after stirring to obtain a filter cake, and cleaning the filter cake for 3 times by using distilled water to obtain a prefabricated product;
placing the prefabricated product in a muffle furnace, raising the temperature in the muffle furnace to 80 ℃, preheating for 30min, filling argon into the muffle furnace after preheating, raising the temperature in the muffle furnace to 350 ℃, reacting at constant temperature for 60min, putting the reaction product into a planet ball mill, and performing ball-material ratio of 10 at a rotating speed of 60 r/min: grinding for 30min under the condition of 1 to prepare carbonized base stock;
the preparation of the algistat containing the gingko endophyte comprises the following steps:
putting the standby filtrate and 6% citric acid solution into a beaker according to the mass ratio of 1:10, stirring for 30min at the rotating speed of 1200r/min by using a stirrer to prepare an organic solvent, putting the organic solvent and the carbonized base material into a stirring kettle according to the mass ratio of 10:1, stirring for 50min at the rotating speed of 60r/min, standing for 3 days after stirring, filtering to obtain a modified filter cake, putting the filter cake into an oven for drying, grinding and crushing to obtain the gingko endophyte-containing algistat.
Example 2
Preparation of heat treatment reaction liquid:
putting ginkgo tree barks and ginkgo leaves into a pulverizer according to the mass ratio of 5:1, pulverizing to obtain a mixture, putting the mixture into an oven, drying for 2.5 hours at the temperature of 45 ℃ to obtain a dried material, and mixing the dried material with absolute ethyl alcohol according to the mass ratio of 1:10 putting the mixture into a beaker, placing the beaker into a shaking table, shaking and soaking for 3.5 hours, and performing suction filtration and separation after soaking to obtain filter residue and filtrate for later use;
putting the filter residues into a reaction kettle, soaking the filter residues in hydrochloric acid with the mass fraction of 5%, sealing the reaction kettle, raising the temperature in the reaction kettle to 65 ℃, stirring the mixture for 2.5 hours at the constant temperature by using a stirrer at the rotating speed of 450r/min, dropwise adding a sodium hydroxide solution with the mass fraction of 12% into a beaker after stirring, and adjusting the pH value to 11 to obtain an alkaline mixed solution;
putting the alkaline mixed solution and silicon dioxide powder into a reaction kettle according to the mass ratio of 20:1, filling nitrogen into the reaction kettle to increase the air pressure in the reaction kettle to 1.3MPa, increasing the temperature in the reaction kettle to 160 ℃, carrying out constant-temperature and constant-pressure reaction for 1.5h, and stirring for 90min at the rotating speed of 650r/min by using a stirrer after the reaction to prepare a heat treatment reaction solution;
preparing a carbonized base material:
putting the heat treatment reaction liquid into a three-neck flask, putting the three-neck flask into a water bath kettle with the water bath temperature of 95 ℃, dropwise adding an acetic acid solution with the mass fraction of 8% into the three-neck flask to adjust the pH value to 6.2, stirring for 45min at the constant temperature by using a stirring device at the rotating speed of 550r/min, filtering after stirring to obtain a filter cake, and cleaning the filter cake for 4 times by using distilled water to obtain a prefabricated product;
placing the prefabricated product in a muffle furnace, raising the temperature in the muffle furnace to 85 ℃, preheating for 35min, filling argon into the muffle furnace after preheating, raising the temperature in the muffle furnace to 370 ℃, reacting at constant temperature for 70min, putting the reaction product into a planet ball mill, and performing ball-material ratio of 10 at a rotating speed of 70 r/min: grinding for 35min under the condition of 1 to prepare carbonized base stock;
the preparation of the algistat containing the gingko endophyte comprises the following steps:
putting the standby filtrate and 8% citric acid solution into a beaker according to the mass ratio of 1:10, stirring the mixture for 35min at the rotating speed of 1250r/min by using a stirrer to prepare an organic solvent, putting the organic solvent and the carbonized base material into a stirring kettle according to the mass ratio of 10:1, stirring the mixture for 55min at the rotating speed of 70r/min, standing the mixture for 4 days after stirring, filtering the mixture after standing to obtain a modified filter cake, putting the modified filter cake into an oven to dry, grinding and crushing the dried filter cake to obtain the gingko endophyte-containing algistat.
Example 3
Preparation of heat treatment reaction liquid:
putting ginkgo tree barks and ginkgo leaves into a pulverizer according to the mass ratio of 5:1, pulverizing to obtain a mixture, putting the mixture into an oven, drying for 3 hours at the temperature of 50 ℃ to obtain a dried material, and mixing the dried material with absolute ethyl alcohol according to the mass ratio of 1:10, putting the beaker into a shaking table, shaking and soaking for 4 hours, and performing suction filtration and separation after soaking to obtain filter residue and filtrate for later use;
putting the filter residues into a reaction kettle, soaking the filter residues in hydrochloric acid with the mass fraction of 6%, sealing the reaction kettle, raising the temperature in the reaction kettle to 70 ℃, stirring the mixture for 3 hours at the constant temperature by using a stirrer at the rotating speed of 500r/min, dropwise adding a sodium hydroxide solution with the mass fraction of 15% into a beaker after stirring, and adjusting the pH value to 12 to obtain an alkaline mixed solution;
putting the alkaline mixed solution and silicon dioxide powder into a reaction kettle according to the mass ratio of 20:1, filling nitrogen into the reaction kettle to increase the air pressure in the reaction kettle to 1.4MPa, increasing the temperature in the reaction kettle to 170 ℃, carrying out constant-temperature and constant-pressure reaction for 2 hours, and stirring the mixture for 100 minutes by using a stirrer at the rotating speed of 700r/min after the reaction to obtain a heat treatment reaction solution;
preparing a carbonized base material:
putting the heat treatment reaction liquid into a three-neck flask, putting the three-neck flask into a water bath kettle with a water bath temperature of 100 ℃, dropwise adding an acetic acid solution with the mass fraction of 10% into the three-neck flask to adjust the pH value to 6.5, stirring for 50min at a constant temperature by using a stirring device at a rotating speed of 600r/min, filtering after stirring to obtain a filter cake, and washing the filter cake for 5 times by using distilled water to obtain a prefabricated product;
placing the prefabricated product in a muffle furnace, raising the temperature in the muffle furnace to 90 ℃, preheating for 40min, filling argon into the muffle furnace after preheating, raising the temperature in the muffle furnace to 400 ℃, reacting at a constant temperature for 80min, putting the reaction product into a planet ball mill, and performing ball-material ratio of 10 at a rotating speed of 80 r/min: grinding for 40min under the condition of 1 to prepare carbonized base stock;
the preparation of the algistat containing the gingko endophyte comprises the following steps:
putting the standby filtrate and a citric acid solution with the mass fraction of 10% into a beaker according to the mass ratio of 1:10, stirring for 40min at the rotating speed of 1300r/min by using a stirrer to prepare an organic solvent, putting the organic solvent and the carbonized base material into a stirring kettle according to the mass ratio of 10:1, stirring for 60min at the rotating speed of 80r/min, standing for 5 days after stirring, filtering to obtain a modified filter cake, putting the filter cake into an oven for drying, grinding and crushing to obtain the gingko endophyte-containing algistat.
Comparative example 1: the procedure was essentially the same as in example 2, except that the alkaline mixture was absent.
Comparative example 2: essentially the same procedure as in example 2 was followed except that the carbonising binder was absent.
Comparative example 3: an algistat containing ginkgo endophyte produced by a company of Welsh city, Anhui province.
And (3) performance testing: the algistats obtained in examples and comparative examples were added to four groups of microcystis aeruginosa solutions (diluted so that the initial algal cell density of the microcystis aeruginosa solution was 1.7 × 106cells/mL), the density of the algae cells in the microcystis aeruginosa solution is calculated every 24 hours and is continuously calculated for 3 days. Microcystis aeruginosa liquid: culturing Microcystis aeruginosa PCC7806 (purchased from algal seed bank of aquatic organism research institute of Chinese academy of sciences) in a culture medium to obtain Microcystis aeruginosa liquid under the culture conditions of: the illumination intensity is 4000lx, the light-dark ratio is 12 h: and (3) shaking for 3-5 times every day at the temperature of 24-26 ℃ for 12h, and culturing for 7 days to obtain the microcystis aeruginosa liquid.
Table 1: result of measuring performance of algistat
| Detecting items | Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Algal cell number after 24h (× 10)6cells/mL） | 1.3 | 1.2 | 1.2 | 1.8 | 1.8 | 1.6 |
| Algal cell number after 48h (× 10)6cells/mL） | 1.1 | 0.9 | 0.9 | 1.7 | 1.6 | 1.4 |
| Number of algal cells after 72h (× 10)6cells/mL） | 0.7 | 0.7 | 0.6 | 1.9 | 1.8 | 1.5 |
In summary, it can be seen from Table 1 that the algistat of the present invention acts quickly, and the number of algal cells after 24 hours is reduced to 1.2 × 106cells/mL, long time effect, good algae removal effect after 72 hours, and wide application prospect.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, but rather as the subject matter of the invention is to be construed in all aspects and as broadly as possible, and all changes, equivalents and modifications that fall within the true spirit and scope of the invention are therefore intended to be embraced therein.
Claims (9)
1. A preparation method of an algistat containing gingko endophyte is characterized by comprising the following specific preparation steps:
putting the filtrate and a citric acid solution with the mass fraction of 6-10% into a beaker, stirring for 30-40 min at the rotating speed of 1200-1300 r/min by using a stirrer to prepare an organic solvent, putting the organic solvent and a carbonized base material into a stirring kettle, stirring for 50-60 min at the rotating speed of 60-80 r/min, standing for 3-5 days after stirring, filtering after standing to obtain a modified filter cake, putting the filter cake into an oven for drying, and grinding and crushing to obtain the gingko endophyte-containing algistat;
the concrete preparation steps of the carbonized base material are as follows:
(1) putting the heat treatment reaction liquid into a three-neck flask, putting the three-neck flask into a water bath kettle with a water bath temperature of 90-100 ℃, dropwise adding an acetic acid solution with the mass fraction of 6-10% into the three-neck flask to adjust the pH value, stirring for 40-50 min at the constant temperature by using a stirring device at the rotating speed of 500-600 r/min, filtering after stirring to obtain a filter cake, and cleaning the filter cake for 3-5 times by using distilled water to obtain a prefabricated product;
(2) placing the prefabricated product in a muffle furnace, raising the temperature in the muffle furnace to 80-90 ℃, preheating for 30-40 min, filling argon into the muffle furnace after preheating, raising the temperature in the muffle furnace, reacting at constant temperature for 60-80 min, putting the reaction product into a planetary ball mill, and performing ball-material ratio of 10 at a rotating speed of 60-80 r/min: grinding for 30-40 min under the condition of 1 to prepare carbonized base stock;
the specific preparation steps of the heat treatment reaction liquid are as follows:
(1) putting ginkgo tree barks and ginkgo leaves into a grinder to be ground to obtain a mixture, putting the mixture into an oven, drying for 2-3 hours at the temperature of 40-50 ℃ to obtain a dried material, and mixing the dried material with absolute ethyl alcohol according to the mass ratio of 1:10, putting the beaker into a beaker, placing the beaker into a shaking table, shaking and soaking for 3-4 h, and performing suction filtration and separation after soaking to obtain filter residue and filtrate;
(2) putting the filter residue into a reaction kettle, soaking the filter residue in hydrochloric acid with the mass fraction of 3-6%, sealing the reaction kettle, raising the temperature in the reaction kettle to 60-70 ℃, stirring the mixture for 2-3 hours at the constant temperature by using a stirrer at the rotating speed of 400-500 r/min, dropwise adding a sodium hydroxide solution with the mass fraction of 10-15% into a beaker after stirring, and adjusting the pH value to prepare an alkaline mixed solution;
(3) and putting the alkaline mixed solution and silicon dioxide powder into a reaction kettle, filling nitrogen into the reaction kettle to increase the pressure in the reaction kettle to 1.2-1.4 MPa, increasing the temperature in the reaction kettle to 150-170 ℃, reacting for 1-2 h at constant temperature and constant pressure, and stirring for 80-100 min at the rotating speed of 600-700 r/min by using a stirrer after reaction to prepare the heat treatment reaction solution.
2. The method for preparing an algistat containing endophytes of ginkgo according to claim 1, wherein the algistat comprises: the mass ratio of the filtrate to the citric acid solution with the mass fraction of 6-10% is 1: 10.
3. The method for preparing an algistat containing endophytes of ginkgo according to claim 1, wherein the algistat comprises: the mass ratio of the organic solvent to the carbonized base material is 10: 1.
4. The method for preparing an algistat containing endophytes of ginkgo according to claim 1, wherein the algistat comprises: specifically, the pH value adjusted by dripping an acetic acid solution with the mass fraction of 6-10% in the step (1) for preparing the carbonized base material is 6.0-6.5.
5. The method for preparing an algistat containing endophytes of ginkgo according to claim 1, wherein the algistat comprises: and (3) specifically preparing the carbonized base material, wherein the temperature in the muffle furnace is increased to 350-400 ℃.
6. The method for preparing an algistat containing endophytes of ginkgo according to claim 1, wherein the algistat comprises: the mass ratio of the ginkgo tree bark to the ginkgo tree leaves in the specific preparation step (1) of the heat treatment reaction liquid is 5: 1.
7. The method for preparing an algistat containing endophytes of ginkgo according to claim 1, wherein the algistat comprises: the mass ratio of the dry material to the absolute ethyl alcohol in the specific preparation step (1) of the heat treatment reaction liquid is 1: 10.
8. the method for preparing an algistat containing endophytes of ginkgo according to claim 1, wherein the algistat comprises: specifically, in the step (2) for preparing the heat treatment reaction liquid, the pH value adjusted by dropwise adding a sodium hydroxide solution with the mass fraction of 10-15% is 10-12.
9. The method for preparing an algistat containing endophytes of ginkgo according to claim 1, wherein the algistat comprises: the mass ratio of the alkaline mixed solution to the silica powder in the specific preparation step (3) of the heat-treated reaction solution is 20: 1.
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