CN112106786A - Method for extracting pesticide components from biomass raw material based on pasteurization - Google Patents
Method for extracting pesticide components from biomass raw material based on pasteurization Download PDFInfo
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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
- A01N61/00—Biocides, pest repellants or attractants, or plant growth regulators containing substances of unknown or undetermined composition, e.g. substances characterised only by the mode of action
- A01N61/02—Mineral oils; Tar oils; Tar; Distillates, extracts or conversion products thereof
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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- Y02P20/10—Process efficiency
- Y02P20/133—Renewable energy sources, e.g. sunlight
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- Pest Control & Pesticides (AREA)
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Abstract
The invention relates to the technical field of biomass pesticides, in particular to a method for extracting pesticide components from biomass raw materials based on a pasteurization method, which comprises the following steps: carrying out pyrolysis treatment on the biomass raw material, and collecting pyrolysis tar; pretreating the pyrolysis tar to obtain pretreated tar; preparing an alkali washing solution, and performing alkali washing on the pretreated tar under a pasteurization heating condition to obtain a solution containing the pesticide active ingredients; adjusting the pH value to obtain an acidified component solution; carrying out organic extraction to obtain an enriched component organic phase; impurity removal treatment is carried out to obtain an organic phase after impurity removal; and (4) carrying out rotary evaporation treatment on the organic phase obtained by removing impurities to obtain the fine pesticide component. The invention separates and purifies the pesticide components from the biomass raw material, achieves the purpose of fully utilizing the biomass raw material, provides a new way for efficiently utilizing the biomass pyrolysis tar, is used for replacing the prior process for extracting high value-added chemical substances mainly by coal, petroleum and the like, and greatly enhances the extraction effect.
Description
Technical Field
The invention relates to the technical field of biomass pesticides, in particular to a method for extracting pesticide components from a biomass raw material based on a pasteurization method.
Background
The information in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
With the development of industrial technology and the rapid progress of human social civilization, resources such as coal, petroleum and the like are increasingly in short supply, renewable resources capable of replacing petroleum are more and more important to develop, biomass energy is an important component of the renewable resources, and the advantages of being green, cheap and available in raw materials are the utilization advantages of the biomass energy. At present, the utilization technology of biomass mainly comprises modes of direct combustion, pyrolysis, gasification and the like. Among them, biomass pyrolysis is a well-established and relatively reliable utilization technique because it can convert biomass into liquid, solid and gaseous products. The biomass tar has complex components, contains hundreds of chemical substances, contains high-added-value chemical intermediate components such as amines and phenols, and can be widely applied to the industries such as pesticides, medicines, foods and the like.
Meanwhile, the inventor finds that the prior art rarely mentions the extraction of pesticide components from biomass tar and lacks an effective method for extracting pesticide components from biomass tar.
Disclosure of Invention
The invention discloses a method for extracting pesticide components from a biomass raw material based on a pasteurization heating method, which comprises the steps of firstly extracting biomass tar from the biomass raw material, then separating and purifying the pesticide components from the biomass tar to achieve the purpose of fully utilizing the biomass tar, and providing a new way for efficiently utilizing the biomass pyrolysis tar to replace the prior process for extracting high-added-value chemical substances mainly by using non-renewable energy sources such as coal, petroleum and the like.
Specifically, the technical scheme of the invention is as follows:
in a first aspect of the invention, the invention provides a method for extracting pesticide ingredients from a biomass feedstock based on a pasteurization heating process, comprising the steps of: carrying out pyrolysis treatment on the biomass raw material, and collecting pyrolysis tar; carrying out dewatering pretreatment on the pyrolysis tar to obtain pretreated tar; preparing an alkali washing solution, and performing alkali washing on the pretreated tar under a pasteurization heating condition to obtain a solution containing the pesticide active ingredients; adjusting the pH value to obtain an acidified component solution; carrying out organic extraction to obtain an enriched component organic phase; removing impurities to obtain an organic phase after impurity removal; and (4) carrying out rotary evaporation treatment on the organic phase obtained by removing impurities to obtain the fine pesticide component.
Further, the water removal pretreatment operation comprises: and adding anhydrous sodium sulfate solid powder into the pyrolysis tar, performing dewatering treatment, and filtering to obtain the pretreated tar.
Further, the alkali washing treatment step comprises: carrying out stage mixing and pasteurization heating on an alkali washing solution and the pretreated tar, wherein the stage mixing and pasteurization heating conditions are as follows: in the first stage, magnetic stirring is carried out, the temperature is kept at 56-65 ℃ for at least 30 min; in the second stage, the glass rod is stirred, the temperature is kept at 80-83 ℃ and kept for 10 min. And reacting to obtain an alkali washing mixed solution. And (3) carrying out phase layering on the alkali washing mixed solution in a separating funnel to obtain the solution containing the pesticide active ingredients.
Further, the solution pH was adjusted using a 10 wt% sulfuric acid solution.
Further, adopting ethyl acetate as an organic extractant, and obtaining the enriched component organic phase at room temperature and the liquid holding time of the contact reaction of at least 5 min.
Further, the impurity removal operation comprises washing the organic phase with deionized water, adding anhydrous sodium sulfate into the enriched component organic phase to remove moisture, and filtering to remove residual inorganic salt solution, residual moisture and solid residues, thereby obtaining the impurity-removed organic phase.
Further, the organic phase with impurities removed is placed in a rotary evaporator for solvent evaporation, and the evaporation conditions are set as follows: evaporating at 55-60 deg.C under 0.024MPa to about one-quarter atmospheric pressure to obtain fine pesticide component.
In a second aspect of the invention, the invention provides a fine pesticidal composition prepared by the method of the first aspect.
In a third aspect of the invention, the invention provides the use of a fine pesticidal composition according to the second aspect for controlling a plant pest.
The specific embodiment of the invention has the following beneficial effects:
creatively proposes to link the secondary utilization of the biomass tar with the botanical pesticide, and has great popularization value; the method for extracting the pesticide components from the biomass tar is simple to operate, can greatly enrich the effective components, has a wide application range, and provides a new idea for the use of the biomass pyrolysis tar.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. In addition, any methods and materials similar or equivalent to those described herein can be used in the methods of the present invention. The preferred embodiments and materials described herein are intended to be exemplary only.
As discussed in the background, the prior art has been poorly studied for the extraction of pesticide components from biomass and lacks an effective method for extracting pesticide components from biomass feedstock. Aiming at the problems in the prior art, the invention discloses a method for extracting pesticide components from a biomass raw material based on a pasteurization heating method, wherein the pesticide components are separated and purified from the biomass raw material, so that the aim of fully utilizing the biomass raw material is fulfilled, and the extraction method has a good extraction effect.
In one embodiment of the present invention, there is provided a method for extracting pesticide ingredients from a biomass feedstock based on a pasteurization process, comprising the steps of: carrying out pyrolysis treatment on the biomass raw material, and collecting pyrolysis tar; carrying out dewatering pretreatment on the pyrolysis tar to obtain pretreated tar; preparing an alkali washing solution, and performing alkali washing on the pretreated tar under a pasteurization heating condition to obtain a solution containing the pesticide active ingredients; adjusting the pH value to obtain an acidified component solution; carrying out organic extraction to obtain an enriched component organic phase; carrying out impurity removal treatment to obtain an impurity-removed organic phase; and (4) carrying out rotary evaporation treatment on the organic phase obtained by removing impurities to obtain the fine pesticide component.
In a specific embodiment, the operation of the water removal pretreatment is as follows: and adding anhydrous sodium sulfate solid powder into the pyrolysis tar, performing dewatering treatment, and filtering to obtain the pretreated tar.
In a specific embodiment, the alkaline washing treatment step comprises: carrying out stage mixing and pasteurization heating on an alkali washing solution and the pretreated tar, wherein the stage mixing and pasteurization heating conditions are as follows: in the first stage, magnetic stirring is carried out, the temperature is kept at 56-65 ℃ for at least 30 min; in the second stage, the glass rod is stirred, the temperature is kept at 80-83 ℃ and kept for 10 min. Obtaining alkali washing mixed solution after reaction; and (3) carrying out phase layering on the alkali washing mixed solution in a separating funnel to obtain a solution containing the pesticide active ingredients. The pasteurization is carried out by stages, so that the pesticide active ingredients in the pyrolysis tar can react with the solution as far as possible to generate inorganic salt, thereby separating from a tar system, promoting the complete reaction of the active ingredients and greatly improving the extraction efficiency.
In a specific embodiment, the pH of the conditioning solution is a 10 wt% sulfuric acid solution.
In a specific embodiment, the organic extractant used in the organic extraction is ethyl acetate, the liquid holding time of the contact reaction is at least 5min, and the temperature is room temperature, so as to obtain the component-enriched organic phase. The organic solvent is used for extraction, so that the enrichment of effective components is realized, and the higher extraction efficiency is ensured.
In a specific embodiment, the operation of removing impurities comprises washing the organic phase with deionized water, adding anhydrous sodium sulfate to the organic phase enriched with components to remove water, and filtering to remove residual inorganic salt solution, residual water and solid residue, thereby obtaining an organic phase with impurities removed.
In a specific embodiment, the organic phase with impurities removed is placed in a rotary evaporator for solvent evaporation, and the evaporation conditions are set as follows: evaporating at 55-60 deg.C under 0.024MPa to about one-quarter atmospheric pressure to obtain fine pesticide component. The organic solvent can be evaporated out to the maximum extent by rotary evaporation under the condition of about one-fourth atmospheric pressure, so as to obtain fine pesticide components.
In one embodiment of the present invention, there is provided a fine pesticidal component prepared by the above method.
In one embodiment of the present invention, there is provided a use of the above fine pesticide composition for controlling plant diseases and insect pests.
The invention will be further illustrated with reference to the following specific examples.
Example 1
Extracting phenolic pesticide components from pine pyrolysis oil:
crushing and screening pine raw materials, then drying in a drying box, putting the treated pine sample in a pyrolysis furnace for pyrolysis treatment, raising the temperature to 500 ℃ at a heating rate of 20 ℃/min, introducing nitrogen at a rate of 200ml/min, and treating for 60min to obtain pine pyrolysis tar. And adding the pyrolyzed tar into anhydrous sodium sulfate solid powder for dewatering, and filtering to remove impurities. 10g of the pretreated tar was stored to obtain sample 1. Preparing a sodium hydroxide solution with the mass fraction of 10 wt%. Taking 10g of pretreated pine tar and 10g of sodium hydroxide solution, and carrying out staged mixing and pasteurization treatment in a beaker, wherein the heating process comprises the following steps: in the first stage, magnetic stirring is carried out, the temperature is kept at 60 ℃ for 30 min; in the second stage, the glass rod is stirred, the temperature is kept at 80 ℃ and kept for 10 min. After the reaction is finished, putting the solution into a separating funnel, separating a lower phase, and then adding a sulfuric acid solution with the mass fraction of 10 wt% to adjust the PH to be 2; then, extracting the organic phase by ethyl acetate in a fractional manner to obtain a solution enriched with phenolic compound components; washing the solution with deionized water to remove residual inorganic salt, adding anhydrous sodium sulfate, and removing residual water; the residue was filtered through a funnel to remove residual solid impurities. And (3) placing the treated impurity-removed organic phase in a rotary evaporator, and performing solvent evaporation operation at the heating temperature of 60 ℃ and the pressure of 0.024MPa for 20min to obtain the fine phenolic compound. An appropriate amount of methylene chloride was added to the obtained fine phenolic compound to dilute it, thereby obtaining sample 2. The specific composition of the phenolic compounds in sample 2 was obtained by GC/MS analysis as follows:
| serial number | Name of substance | 2 percent/% (solvent removal) of sample |
| 1 | Phenol and its preparation | 2.76 |
| 2 | P-methylphenol | 1.34 |
| 3 | 3-methylphenol | 2.05 |
| 4 | P-methoxyphenol | 7.21 |
| 5 | Maltol | 3.12 |
| 6 | 2-methoxy-5-methylphenol | 5.43 |
| 7 | Resorcinol | 1.87 |
| 8 | 2-methoxy-4-ethylphenol | 2.49 |
| 9 | 4-Methylresorcinol | 1.07 |
| 10 | 2, 6-dimethoxyphenol | 9.35 |
| 11 | 5-tert-butyl pyrogallol | 3.38 |
| 12 | 2-methyl-4-ethoxyphenol | 2.76 |
Example 2
Extracting phenolic pesticide components from safflower pyrolysis oil:
crushing and screening a safflower raw material, then drying in a drying box, putting a treated safflower sample in a pyrolysis furnace for pyrolysis treatment, raising the temperature to 500 ℃ at a heating rate of 20 ℃/min, introducing nitrogen at a rate of 200ml/min, and treating for 60min to obtain safflower pyrolysis tar. And adding the pyrolyzed tar into anhydrous sodium sulfate solid powder for dewatering, and filtering to remove impurities. Taking 10g of the pretreated tar oil for storage to obtain a sample 3; taking 10g of pretreated safflower tar and 10g of sodium hydroxide solution with the mass fraction of 10 wt%, and carrying out staged mixing and pasteurization treatment in a beaker, wherein the heating process comprises the following steps: in the first stage, magnetic stirring is carried out, the temperature is kept at 65 ℃ and 30 min; in the second stage, the glass rod is stirred, the temperature is kept at 80 ℃ and kept for 10 min. After the reaction is finished, putting the solution into a separating funnel, separating a lower phase, and then adding a sulfuric acid solution with the mass fraction of 10 wt% to adjust the PH to be 2; then, extracting the organic phase by ethyl acetate in a fractional manner to obtain a solution enriched with phenolic compound components; washing the solution with deionized water to remove residual inorganic salt, adding anhydrous sodium sulfate, and removing residual water; the residue was filtered through a funnel to remove residual solid impurities. And (3) placing the treated impurity-removed organic phase in a rotary evaporator, and performing solvent evaporation operation at the heating temperature of 60 ℃ and the pressure of 0.024MPa for 20min to obtain the fine phenolic compound. An appropriate amount of methylene chloride was added to the obtained fine phenolic compound to dilute it, to obtain sample 4. The specific composition of the phenolic compounds in sample 4 was obtained by GC/MS analysis as follows:
experimental example: test of insecticidal Effect of the Fine pesticidal ingredients prepared in examples 1 and 2
In the experiment, diamondback moth larvae (2 years old) are selected, 3 suitable culture dishes are selected, filter paper covers the bottoms of the culture dishes, and deionized water is dripped to keep the filter paper moist. Cutting cabbage leaves into proper sizes, cleaning one in each culture dish, removing wax, soaking the cut cabbage leaves in 5ml of clear water, 5ml of pine sample 2 and 5ml of safflower sample 4 liquid medicine for 10s respectively by using forceps, and taking back the leaves to the culture dishes 1, 2 and 3. The plates were then dried in a cool and ventilated place and 18 healthy moth larvae (2 instar) per plate were inoculated with soft brushes. After the larvae are inoculated, the culture dish is placed in an incubator at 27 ℃, and a layer of moist gauze is covered on the culture dish to ensure a moist environment of 30% -40% for the growth of the larvae. After treatment for 3d, the number of live and dead insects treated was recorded. The record shows that the insecticidal rate of the clear water culture medium 1 is 12.5 percent, the insecticidal rate of the pine culture medium 2 is 66.67 percent, and the insecticidal rate of the safflower culture medium is 61.2 percent.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for extracting pesticide ingredients from a biomass raw material based on a pasteurization method, characterized in that the method comprises the following steps:
carrying out pyrolysis treatment on the biomass raw material, and collecting pyrolysis tar;
carrying out dewatering pretreatment on the pyrolysis tar to obtain pretreated tar;
preparing a sodium hydroxide solution with a certain mass fraction to obtain a standby alkaline washing solution;
carrying out alkali washing on the pretreated tar by using the standby alkali washing solution under a pasteurization heating condition to obtain a solution containing pesticide active ingredients;
adjusting the pH value of the pesticide active ingredient-containing solution to obtain an acidified ingredient solution;
carrying out organic extraction on the acidified component solution to obtain an enriched component organic phase;
removing impurities from the enriched component organic phase to obtain an impurity-removed organic phase;
and carrying out rotary evaporation on the impurity-removed organic phase to obtain the fine pesticide component.
2. The pasteurization-based heating method for extracting pesticide ingredients from biomass raw materials according to claim 1, characterized in that the pretreatment operation comprises: and adding anhydrous sodium sulfate solid powder into the pyrolysis tar, performing dewatering treatment, and filtering to obtain the pretreated tar.
3. The pasteurization-based heating method for extracting agricultural chemical ingredients from biomass raw material as claimed in claim 1, wherein the step of alkali washing comprises: carrying out stage mixing on the alkaline washing solution and the pretreated tar, carrying out pasteurization heating, and reacting to obtain an alkaline washing mixed solution; carrying out phase layering on the alkali washing mixed solution in a separating funnel to obtain the pesticide-containing effective component solution;
preferably, the mass fraction of sodium hydroxide in the alkaline washing solution is 10 wt%.
4. The pasteurization-based heating process for extracting pesticide ingredients from biomass feedstock as recited in claim 3, wherein the stage mixing and pasteurization heating conditions are: in the first stage, magnetic stirring is carried out, the temperature is kept at 56-65 ℃ for at least 30 min; and in the second stage, stirring by a glass rod, keeping the temperature at 80-83 ℃ for 10 min.
5. The pasteurization-based heating method for extracting agricultural chemicals from biomass feedstock as recited in claim 1, wherein the step of adjusting the PH comprises: and carrying out reverse reaction on the dilute sulfuric acid solution and the pesticide effective component solution to obtain the acidified component solution.
6. The pasteurization-based heating method for extracting pesticide ingredients from biomass raw materials as claimed in claim 1, characterized in that the organic extractant used in the organic extraction is ethyl acetate, the duration of the contact reaction is at least 5min, and the temperature is room temperature, so as to obtain an ingredient-enriched organic phase.
7. The pasteurization-based heating method for extracting pesticide ingredients from biomass raw materials as claimed in claim 1, wherein the impurity removal operation comprises washing the organic phase with deionized water, adding anhydrous sodium sulfate into the ingredient-enriched organic phase to remove water, and filtering to obtain the impurity-removed organic phase.
8. The pasteurisation heating based method for extracting agricultural chemicals from biomass feedstock according to claim 1, wherein the rotary evaporation conditions are set as: the water bath temperature is 60 deg.C, the evaporation pressure is 0.024Mpa, and the evaporation time is at least 20 min.
9. A fine pesticidal component produced by the method of extracting a pesticidal component from a biomass feedstock based on pasteurization based on any one of claims 1 to 8.
10. Use of the fine pesticidal component of claim 9 for controlling plant pests.
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