CN115161056A - Stable crude wood vinegar and preparation method thereof - Google Patents

Stable crude wood vinegar and preparation method thereof Download PDF

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CN115161056A
CN115161056A CN202210740568.1A CN202210740568A CN115161056A CN 115161056 A CN115161056 A CN 115161056A CN 202210740568 A CN202210740568 A CN 202210740568A CN 115161056 A CN115161056 A CN 115161056A
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wood vinegar
polyoxyethylene ether
surfactant
crude
parts
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张鹏
张宗俭
张春华
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BEIJING GRAND AGROCHEM Ltd
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BEIJING GRAND AGROCHEM Ltd
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
    • C10C5/00—Production of pyroligneous acid distillation of wood, dry distillation of organic waste
    • 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
    • A01N25/02—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 liquids as carriers, diluents or solvents
    • A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
    • 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
    • A01N25/22—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 ingredients stabilising the active ingredients
    • 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
    • A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/90—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
    • 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
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
    • A01P7/00—Arthropodicides
    • A01P7/04—Insecticides
    • 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
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E50/00—Technologies for the production of fuel of non-fossil origin
    • Y02E50/10—Biofuels, e.g. bio-diesel

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  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • Wood Science & Technology (AREA)
  • General Health & Medical Sciences (AREA)
  • Environmental Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Zoology (AREA)
  • Pest Control & Pesticides (AREA)
  • Plant Pathology (AREA)
  • Dentistry (AREA)
  • Agronomy & Crop Science (AREA)
  • Toxicology (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Dispersion Chemistry (AREA)
  • Insects & Arthropods (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The invention relates to stable crude wood vinegar and a preparation method thereof, belonging to the technical field of agricultural and forestry waste processing. The stable crude wood vinegar liquid consists of the following components in parts by weight: 75-99 parts of crude wood vinegar; 1-20 parts of surfactant; 0-5 parts of an antifreezing agent. The crude wood vinegar liquid can be placed for a long time and has uniform appearance, and wood tar cannot be separated out; can be directly used as raw materials for producing and processing downstream products such as soil conditioners, pesticide additives, fertilizer additives, sanitary disinfectants and the like.

Description

Stable crude wood vinegar and preparation method thereof
Technical Field
The invention relates to the technical field of agricultural and forestry waste processing, and particularly provides stable crude wood vinegar and a preparation method thereof.
Background
The pyroligneous liquor is an organic liquid component obtained by condensing, recovering and separating gas generated in the pyrolysis and carbonization processes of biomass. The components mainly comprise organic acids, phenols, ketones, alcohols and aldehydes, and also comprise heterocyclic compounds, trace elements and the like. The wood vinegar can be classified into wood vinegar using branches as a main raw material, bamboo vinegar using bamboo as a main raw material, grass vinegar using grass as a main raw material, and the like, depending on the source of the raw material. The pyroligneous acid can be classified into crude pyroligneous acid, precipitated pyroligneous acid, distilled pyroligneous acid, etc. according to differences in production processes.
The wood vinegar is a byproduct generated in the charcoal firing process, the yield is high, and generally 200-300 kg of crude wood vinegar can be generated in the process of preparing charcoal by one ton of wood. The collection process can be roughly divided into three stages: the temperature is lower than 150 ℃ in the pre-carbonization stage of the wood, and the main components collected in the condensed flue gas are light oil with low boiling point and small specific gravity in the bark part of the wood. The temperature is between 150 ℃ and 300 ℃ which is the wood carbonization stage, cellulose, hemicellulose, lignin and the like in the wood begin to be pyrolyzed, and the main component collected in the condensed flue gas is wood vinegar mainly containing organic acid. The temperature is 300 ℃ to 400 ℃ as a rapid carbonization stage, and the main component collected in the condensed flue gas is wood tar. In the actual production process, the collected crude wood vinegar is a complex mixture of multiple components, when the wood vinegar is used, the wood tar in the crude wood vinegar is mainly organic acids, the wood tar in the crude wood vinegar is gradually precipitated along with the prolonging of the storage time, and the precipitated wood tar can affect the appearance quality of the wood vinegar product, such as oily precipitates formed on the wall or the bottom of a container; on the other hand, the use of pyroligneous liquor is affected, for example, wood tar easily blocks a spray head during spraying, so that crude pyroligneous liquor usually needs to be refined before further use.
The common refining and separating method of the crude pyroligneous acid comprises the following steps: standing, distilling, adsorbing, electrolyzing, freezing and thawing at low temperature, filtering, enzymolysis, and distributing, and is mainly used for further purifying the crude wood vinegar to remove harmful substances such as wood tar, solid impurities, and heavy metals. Depending on the specific application scenario and the target, the requirements for refining and purifying the crude pyroligneous acid are different, for example, the requirements for refining food or cosmetics are high, and the requirements for refining in the agricultural field are relatively low.
The existing wood vinegar refining method has the problems of long treatment time, high cost, complex process, large equipment investment, secondary pollutant generation and the like. For example, the standing method usually requires standing for 3 to 6 months, and the pyroligneous liquor of a 10 ten thousand ton/year charcoal producing plant is produced at a yield of 6 to 9 ten thousand ton/year, so that the storage space and facilities are required for such a large number of pyroligneous liquor standing treatments. The distillation method has high energy consumption and low value of the generated by-product, and the downstream product is prepared after the treatment by the method, so the cost of the prepared product is not dominant. The adsorption method mostly adopts activated carbon to adsorb and remove wood tar in the wood vinegar, and has the defects of secondary waste generation and incomplete adsorption.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides stable crude wood vinegar and a preparation method thereof, and the crude wood vinegar can be placed for a long time and has uniform appearance without precipitating wood tar; can be directly used as raw materials for producing and processing downstream products such as soil conditioners, pesticide additives, fertilizer additives, sanitary disinfectants and the like.
In order to solve the technical problems, the invention provides the following technical scheme:
on one hand, the invention provides stable crude wood vinegar which comprises the following components in parts by weight:
75-99 parts of crude wood vinegar;
1-20 parts of surfactant;
0-5 parts of an antifreezing agent.
Preferably, the stable crude wood vinegar consists of the following components in parts by weight:
80-99 parts of crude wood vinegar;
10-20 parts of a surfactant;
0-5 parts of antifreeze.
Further, the surfactant comprises a surfactant A with HLB being more than or equal to 10.
Preferably, the surfactant A is one or more of sodium dodecyl benzene sulfonate, tristyrylphenol polyoxyethylene ether and phosphate ester or sulfonate thereof, castor oil polyoxyethylene ether, alkylphenol polyoxyethylene ether and phosphate ester or ammonium salt thereof, tristyrylphenol polyoxyethylene polyoxypropylene ether, fatty alcohol polyoxyethylene ether and sodium salt or ammonium salt thereof, plant polyene phenol polyoxyethylene ether and phosphate ester salt thereof, high-molecular block polyether, polyoxyethylene sorbitan fatty acid ester, alkyl glycoside, alkyl betaine or cocamido betaine, fatty alcohol ethylene oxide condensate, tallow amine polyoxyethylene ether, alkylphenol formaldehyde resin polyoxyethylene ether sulfate, maleic acid diisooctyl sulfonate, benzyl dimethyl phenol polyoxyethylene ether, alkylphenol formaldehyde resin polyoxyethylene ether, fluorocarbon and fluorosilicone surfactant. For example, tristyrylphenol polyoxyethylene ether and its phosphate or sulfonate: 601. 602, 603, 604, 605, 601P, 601SA, etc.; castor oil polyoxyethylene ether: EL-40; alkylphenol ethoxylates and phosphate esters or ammonium salts thereof: OP-7, OP-10, OP-15, OP-10P, NP-10, NP-10P, etc.; tristyrylphenol polyoxyethylene polyoxypropylene ether: 1601. 1602, etc.; fatty alcohol polyoxyethylene ether and sodium salt or ammonium salt thereof: AEO-5, AEO-7, AEO-9, AEO-3P, AES, and the like; plant polyene phenol polyoxyethylene ether and phosphate, ammonium salt or sulfonate thereof: NSF-10, NSF-10E, NSN3004A, NSN3004C, NSN3015; high-molecular block polyether: g5000, D800, 10500, etc.; polyoxyethylene sorbitan fatty acid ester: tween20, tween40, tween 60, tween 80, and the like; alkyl glycoside: APG50, APG70, etc.; alkyl betaines or cocamide betaines: BS-12, CAB35, etc.; fatty alcohol ethylene oxide condensate: o-10, O-15, O-20, etc.; tallow amine polyoxyethylene ether: AC1810, AC1815, etc.; alkylphenol formaldehyde resin polyoxyethylene ether sulfate: s270, M270 and the like; diisooctyl maleate sulfonate: a rapid penetrant T; benzyl dimethylphenol polyoxyethylene ether: farm milks 400#, 401#, 402#, etc.; alkylphenol formaldehyde resin polyoxyethylene ether: farm milks 700#, 701#, 702#, etc.; fluorocarbon, fluorosilicon surfactants: YM-313, FC-922, etc.
Further, the surfactant also comprises a surfactant B with HLB less than 10.
Preferably, the surfactant B is one or more of calcium dodecyl benzene sulfonate, ammonium dodecyl benzene sulfonate, castor oil polyoxyethylene ether EL-20, alkylphenol polyoxyethylene OP-4, NP-4, plant polyene phenol polyoxyethylene ether NSF-3, NSF-5, sorbitan fatty acid ester (Span 20, span40, span60, span 80), tallow amine polyoxyethylene ether 1805 and silicone polyether (GY-S903, RH-208 and Silwet 408).
Furthermore, the mass ratio of the surfactant B to the surfactant A is less than or equal to 1.4.
For example, the lipophilic emulsifier monomer OP-4 is used in combination with the hydrophilic emulsifier monomer OP-10, and when the amount of OP-10 is 5 parts by weight, the amount of OP-4 is not more than 7 parts by weight. If three or more different types of surfactant monomers are used in combination, the ratio of the sum of all lipophilic surfactant monomers to the sum of all hydrophilic surfactant monomers is also not higher than 1.4.
Further, the crude wood vinegar refers to a complex mixture of organic acids, alcohols, phenols, ketones, aldehydes, wood tar and other substances generated in the pyrolysis process of wood (or grass), and includes common wood vinegar, bamboo vinegar, grass vinegar and the like.
Preferably, the antifreeze is ethylene glycol, propylene glycol or urea.
On the other hand, the invention also provides a preparation method of the stable crude wood vinegar, which is to uniformly mix the crude wood vinegar, the surfactant and the antifreezing agent.
The instability of crude pyroligneous liquor in long-term storage is mainly due to the wood tar contained therein. The main component of the wood tar is wood impure phenol, and also contains acids, esters, alcohols, ketones, aldehydes, hydrocarbons, heterocycles, carbohydrates and the like, and the wood tar is a complex mixture. The wood tar is denser than the pyroligneous liquor and is immiscible with the pyroligneous liquor, so that it precipitates from the pyroligneous liquor during long-term storage to form an oil which sticks to the wall or bottom of the pyroligneous liquor storage container.
Suitable surfactants for the two immiscible liquids may be selected to stabilize and uniformly mix the incompatible two phases together by emulsification, dispersion, solubilization, and the like. The surfactant has amphiphilicity due to the fact that the surfactant contains hydrophilic groups and lipophilic groups, wherein the lipophilic groups are easy to combine with an oil phase, and the hydrophilic groups are easy to combine with a water phase. By adjusting the proportion of two immiscible liquids and the three phases of the added surfactant, one phase of the liquid can be wrapped into tiny emulsion droplets to be uniformly dispersed into the other phase, but in the practical application process, due to the fact that the types of the surfactants are multiple, the difference between the structures and the hydrophilicity and the lipophilicity is large, the difference between the compound use performances of the surfactants of different types and proportions is obvious, and the like, the application technology of the surfactants is always the key technology for preparing emulsions, microemulsions and the like. The wood tar and pyroligneous liquor system of the invention is a mixed system with complex components, and the wood tar in the crude pyroligneous liquor is uniformly and stably dispersed under the action of a specific surfactant, so that the aim of avoiding the occurrence of ointment-like precipitates after long-term storage is fulfilled. Can be directly used as raw materials for producing and processing downstream products such as soil conditioners, pesticide additives, fertilizer additives, sanitary disinfectants and the like.
The method for treating the wood vinegar has the following remarkable advantages: firstly, compared with a standing precipitation method, the method is efficient, and the treatment time of the crude pyroligneous liquor can be greatly shortened; compared with distillation and rectification methods, the method has the advantages of low cost, energy conservation, low carbon and environmental protection; thirdly, compared with an adsorption method, the method is environment-friendly, and does not generate secondary wastes such as adsorption waste residues and the like; fourthly, the treated wood vinegar has good long-term storage stability and does not have the problems of layering, precipitation and the like. The wood vinegar liquid after being processed can be used for deep processing products in different fields, such as pesticide synergist, soil processing agent, fertilizer additive, feed additive, water treatment agent, industrial cleaning agent, sanitary disinfectant and the like.
Detailed Description
In order to make the technical problems, technical solutions and advantages to be solved by the present invention clearer, the following detailed description is given with reference to specific embodiments.
The reagents and materials used in the examples and comparative examples were commercially available unless otherwise specified.
The invention provides stable crude wood vinegar and a preparation method thereof, and specific examples are as follows.
Example 1
A method for preparing stable crude wood vinegar liquid comprises: taking 900g of crude pyroligneous liquor, 70g of sodium dodecyl benzene sulfonate and 30g of glycol, and uniformly stirring in a 1000ml beaker, and recording as S1; the crude pyroligneous is pyroligneous.
Example 2
A method for preparing stable crude wood vinegar liquid comprises: putting 950g of crude pyroligneous liquor and 601 50g of tristyrylphenol polyoxyethylene ether agricultural emulsion in a 1000ml beaker, and uniformly stirring, and recording as S2; the crude wood vinegar is wood vinegar.
Example 3
A method for preparing stable crude wood vinegar liquid comprises: taking 750g of crude pyroligneous liquor, 200g of octyl phenol polyoxyethylene ether OP-10 and 50g of propylene glycol, and placing the raw pyroligneous liquor, the octyl phenol polyoxyethylene ether OP-10 and the propylene glycol in a 1000ml beaker to be uniformly stirred, and marking as S3; the crude wood vinegar is wood vinegar.
Example 4
A method for preparing stable crude wood vinegar liquid comprises: taking 940g of crude pyroligneous liquor, 10g of plant source polyalkenyl phenol polyoxyethylene ether NSF and 30g of urea, and placing in a 1000ml beaker to stir uniformly, and marking as S4; the crude wood vinegar is wood vinegar.
Example 5
A method for preparing stable crude wood vinegar liquid comprises: putting 880g of crude pyroligneous liquor, 10g of plant source polyalkenyl phenol polyoxyethylene ether NSF, 30g of sodium dodecyl benzene sulfonate and 20g of ethylene glycol into a 1000ml beaker, and uniformly stirring, wherein the weight is marked as S5; the crude wood vinegar is grass vinegar.
Example 6
A method for preparing stable crude wood vinegar liquid comprises: putting 850g of crude wood vinegar, 140g of diisooctyl maleate sulfonate and 10g of organic silicon surfactant GY-S903 in a 1000ml beaker, and uniformly stirring to obtain S6; the crude wood vinegar is wood vinegar.
Example 7
A method for preparing stable crude wood vinegar liquid comprises: putting 950g of crude wood vinegar, 1810 40g of Niu Zhian polyoxyethylene ether and 10g of ethylene glycol into a 1000ml beaker, and uniformly stirring, and recording as S7; the crude wood vinegar is bamboo vinegar.
Example 8
A method for preparing stable crude wood vinegar liquid comprises: taking 800g of crude pyroligneous liquor, 80 30g of sorbitan fatty acid ester span, 18032.5 g of Niu Zhian polyoxyethylene ether, 87.5g of rapid penetrating agent T and 50g of propylene glycol, and placing the crude pyroligneous liquor, the sorbitan fatty acid ester span, the Niu Zhian polyoxyethylene ether and the propylene glycol in a 1000ml beaker to be uniformly stirred, wherein the weight of the rapid penetrating agent is marked as S8; the crude wood vinegar is wood vinegar.
Example 9
A method for preparing stable crude wood vinegar liquid comprises: 990g of crude pyroligneous liquor, 4g of castor oil polyoxyethylene ether EL-20 and 6g of benzyl dimethyl phenol polyoxyethylene ether agricultural emulsion No. 400 are taken and placed in a 1000ml beaker to be uniformly stirred, and the mixture is marked as S9; the crude pyroligneous is pyroligneous.
Example 10
A method for preparing stable crude wood vinegar liquid comprises: placing 850g of crude pyroligneous liquor, OP-4 65g of alkylphenol polyoxyethylene ether, 50g of alkyl glycoside APG, 700#35g of alkylphenol formaldehyde resin polyoxyethylene ether agricultural emulsion and 20g of glycol in a 1000ml beaker, and uniformly stirring to obtain S10; the crude wood vinegar is wood vinegar.
Example 11
A method for preparing stable crude wood vinegar liquid comprises: putting 900g of crude pyroligneous liquor, 10g of calcium dodecyl benzene sulfonate, 20g of alkylphenol polyoxyethylene NP-4, 20g of polyoxyethylene sorbitan fatty acid ester Tween and 10g of urea in a 1000ml beaker, and uniformly stirring, wherein the weight is marked as S11; the crude wood vinegar is wood vinegar.
Example 12
A method for preparing stable crude wood vinegar liquid comprises: placing 850g of crude pyroligneous liquor, 601P 65g of tristyrylphenol polyoxyethylene ether sulfonate, 65g of calcium dodecylbenzene sulfonate and 20g of ethylene glycol in a 1000ml beaker, and uniformly stirring, wherein the weight is marked as S12; the crude wood vinegar is wood vinegar.
Example 13
A method for preparing stable crude wood vinegar liquid comprises: placing 850g of crude pyroligneous liquor, 601SA 65g of triphenylvinyl phenol polyoxyethylene ether phosphate, 65g of calcium dodecylbenzene sulfonate and 20g of ethylene glycol in a 1000ml beaker, and uniformly stirring, wherein the weight is marked as S13; the crude wood vinegar is wood vinegar.
Example 14
A method for preparing stable crude wood vinegar liquid comprises: placing 850g of crude pyroligneous liquor, 65g of plant polyene phenol polyoxyethylene ether phosphate NSN3004A, 65g of calcium dodecyl benzene sulfonate and 20g of ethylene glycol in a 1000ml beaker, and uniformly stirring, and marking as S14; the crude pyroligneous is pyroligneous.
Example 15
A method for preparing stable crude wood vinegar liquid comprises: placing 850g of crude pyroligneous liquor, 65g of plant polyene phenol polyoxyethylene ether phosphate NSN3004A, 65g of calcium dodecylbenzene sulfonate and 20g of ethylene glycol in a 1000ml beaker, and uniformly stirring, wherein the weight is marked as S15; the crude wood vinegar is wood vinegar.
Example 16
A method for preparing stable crude wood vinegar liquid comprises: placing 850g of crude wood vinegar, 65g of plant polyene phenol polyoxyethylene ether ammonium salt NSN3004C, 65g of calcium dodecyl benzene sulfonate and 20g of ethylene glycol in a 1000ml beaker, and uniformly stirring, wherein the weight is marked as S16; the crude wood vinegar is wood vinegar.
Example 17
A method for preparing stable crude wood vinegar liquid comprises: placing 850g of crude wood vinegar, 3015 g of plant polyene phenol polyoxyethylene ether sulfonate NSN, 65g of calcium dodecylbenzene sulfonate and 20g of ethylene glycol in a 1000ml beaker, and uniformly stirring, wherein the weight is marked as S17; the crude wood vinegar is wood vinegar.
Example 18
A method for preparing stable crude wood vinegar liquid comprises: putting 850g of crude pyroligneous liquor, 1810 g of tallow amine polyoxyethylene ether AC, 65g of calcium dodecyl benzene sulfonate and 20g of ethylene glycol into a 1000ml beaker, and uniformly stirring, and recording as S18; the crude wood vinegar is wood vinegar.
Example 19
A method for preparing stable crude wood vinegar liquid comprises: placing 850g of crude pyroligneous liquor, 1815 g of tallow amine polyoxyethylene ether AC1815 g, 65g of calcium dodecyl benzene sulfonate and 20g of ethylene glycol in a 1000ml beaker, and uniformly stirring to obtain S19; the crude pyroligneous is pyroligneous.
To further illustrate the advantageous effects of the present invention, comparative examples were constructed as follows.
Comparative example 1
A method for preparing crude wood vinegar comprises: taking 800g of crude pyroligneous liquor, 1306 150g of isomeric alcohol polyoxyethylene ether and 50g of ethylene glycol, and placing the crude pyroligneous liquor, 1306 150g of isomeric alcohol polyoxyethylene ether and 50g of ethylene glycol in a 1000ml beaker for uniformly stirring, and marking as D1; the crude pyroligneous is pyroligneous.
Comparative example 2
A method for preparing crude wood vinegar comprises: placing 850g of crude pyroligneous liquor, 30g of glycol and 30g of fatty alcohol alkoxylate CEREWIN6400 in a 1000ml beaker, and uniformly stirring to obtain D2; the crude wood vinegar is wood vinegar.
Comparative example 3
A method for preparing crude wood vinegar comprises: placing 850g of crude pyroligneous liquor, 10g of plant source polyalkenylphenol polyoxyethylene ether NSF, 40g of polyethylene glycol 400 monostearate PEG400MS and 30g of ethylene glycol in a 1000ml beaker, and uniformly stirring to obtain D3; the crude wood vinegar is wood vinegar.
Comparative example 4
A method for preparing crude wood vinegar comprises: putting 855g of crude pyroligneous liquor, 10g of plant source polyalkenyl phenol polyoxyethylene ether NSF, 75g of calcium dodecylbenzenesulfonate and 20g of ethylene glycol into a 1000ml beaker, and uniformly stirring, wherein the weight is marked as D4; the crude wood vinegar is wood vinegar.
Comparative example 5
A method for preparing crude wood vinegar comprises: taking 900g of crude pyroligneous liquor and 100g of ethylene glycol, and uniformly stirring in a 1000ml beaker, and marking as D5; the crude pyroligneous is pyroligneous.
Comparative example 6
Taking 1000g of crude pyroligneous liquor, and recording as D6; the crude pyroligneous is pyroligneous.
Comparative example 7
The alkyl glycoside APG50 and the alkylphenol formaldehyde resin polyoxyethylene ether agricultural emulsion 700# are replaced by the same amount of alkylphenol polyoxyethylene ether OP-4, and the rest conditions are the same as the example 10 and are marked as D7.
Comparative example 8
The alkylphenol formaldehyde resin polyoxyethylene ether agricultural emulsion 700# is replaced by the same amount of alkylphenol polyoxyethylene ether OP-4, and the rest conditions are the same as the example 10 and are marked as D8.
The samples prepared in the above examples and comparative examples were charged into a 1L transparent plastic bottle and sealed, and the empty bottle weight and the charged amount of each sample were weighed. The samples were stored according to GB/T19136-2003 determination method for thermal storage stability of pesticides and GB/T19137-2003 determination method for low temperature stability of pesticides, and the appearance change of the samples was observed and recorded. The stored sample bottles were opened and left upright for 10 minutes until the liquid inside did not drip, and the bottle weight change was weighed and recorded. The wood tar precipitation rate was calculated as follows:
ω(％)＝(m 1 -m 2 )/m*100％；
wherein: omega is the precipitation rate of wood tar; m is 1 Bottle weight after hot or cold storage; m is 2 The weight of the empty bottle without the sample; m is the weight of the wood vinegar sample filled in the bottle. The test results are shown in tables 1-2.
TABLE 1 storage stability test results for the samples of the examples
Figure BDA0003717800710000091
Figure BDA0003717800710000101
As can be seen from Table 1, the present invention has good hot and cold storage stability by the combined action of the specific surfactant and the crude pyroligneous liquor, is convenient for long-term storage, and can be directly used as an additive for application.
The combination of surfactant a and surfactant B (examples 6 and 8-11) effectively reduced the precipitation rate of wood tar compared to surfactant a alone (examples 1-5 and 7), while the combination of specific surfactant a and surfactant B (examples 12-19) further reduced the precipitation rate of wood tar.
TABLE 2 comparative example sample storage stability test results
Figure BDA0003717800710000102
As can be seen from Table 2, the wood vinegar obtained by replacing the type of the surfactant or changing the amount ratio of the surfactant has a high wood tar precipitation rate after hot or cold storage.
The test method for the low-temperature and thermal storage stability of the pesticide is an accelerated test method, and can simulate and reflect the performance change of the pesticide preparation in two-year storage. The stability of the crude wood vinegar liquid added with the surfactant is detected by referring to a test method for testing the low-temperature and thermal storage stability of the pesticide, and the result shows that the crude wood vinegar liquid treated by the surfactant has good stability and always keeps a uniform state and does not generate ointment-like precipitates when being stored at low temperature and under thermal storage. The crude wood vinegar samples treated or not treated by other surfactants have obvious phenomenon of ointment-like precipitates in accelerated storage tests, and are difficult to meet the requirement of subsequent processing and use.
The stable crude wood vinegar prepared by the method can be directly used as a raw material for producing and processing downstream products such as a soil conditioner, a pesticide additive, a fertilizer additive, a sanitary disinfectant and the like, and is concretely as follows.
The crude pyroligneous acid of example 10, examples 12 to 19 and comparative examples 1 to 8 of the present invention was used as an adjuvant to be added to a pesticide, and the specific formulation of the pesticide was as follows:
TABLE 3.7% Emamectin benzoate SC formulation components
Raw materials Percentage content
Emamectin benzoate original drug 5.7%, book Bai
GY-W07 2％
GY-1287 6％
Ethylene glycol 3％
Magnesium aluminum silicate 1％
Xanthan gum 0.16％
GY-B15 0.16％
GY-X60 0.3％
Crude wood vinegar Make up to 100%
500g of the components are fully stirred in a beaker until the components are uniformly mixed, and then a vertical sand mill is adopted for grinding. The grinding conditions were: the bead ratio is 1.5, the rotating speed is 1600rpm, and the grinding time is 1.5h. Then the sample is filtered and collected, and is filled in a 100ml transparent plastic sample bottle, the bottle is sealed, and the cold storage test and the hot storage test are respectively carried out. The stability of the recorded sample was observed and the particle size of the tested sample was varied, the results are shown in tables 4-5.
TABLE 4 results of SC storage stability test of 5.7% emamectin benzoate containing crude pyroligneous liquid of example
Figure BDA0003717800710000121
TABLE 5 results of SC storage stability test for 5.7% emamectin benzoate containing comparative example crude pyroligneous acid
Figure BDA0003717800710000122
Figure BDA0003717800710000131
As can be seen from tables 4-5, when the crude pyroligneous acid treated by the scheme of the present invention is added as a synergistic component to a pesticide preparation, the preparation performance is stable and is not affected by the disadvantage of instability of the crude pyroligneous acid. When the crude wood vinegar processed by the scheme of the invention is added into a pesticide preparation, the problems of oil separation, layering, caking, creaming and the like easily occur during storage of the preparation.
The prepared emamectin benzoate SC is used for carrying out field test on the cabbage plutella xylostella, and the control effect is 88.6 percent in 14 days after the treatment by using the emamectin benzoate SC prepared in the embodiment 10 of the invention; when the emamectin benzoate SC prepared in examples 12-19 is used for treatment, the control effect is 93.6-99.7% in 14 days after the treatment; the control effect is 64.2 to 81.5 percent after 14 days of treatment by using emamectin benzoate SC prepared in comparative examples 1 to 8. The crude wood vinegar prepared by the method disclosed by the invention is proved to be capable of improving the stability of the prepared emamectin benzoate SC and improving the insecticidal effect of the emamectin benzoate SC to a certain extent.
In conclusion, the problem that wood tar is separated out after the crude pyroligneous liquor is stored for a long time can be effectively solved by treating the crude pyroligneous liquor by using the surfactant type screened by the invention and the specific treatment method. Compared with the conventional common method, the treatment method is simple and effective, has low cost and no secondary pollutant, and is a feasible scheme for treating the crude pyroligneous liquor.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined in the appended claims.

Claims (10)

1. The stable crude wood vinegar is characterized by comprising the following components in parts by weight:
75-99 parts of crude wood vinegar;
1-20 parts of surfactant;
0-5 parts of an antifreezing agent.
2. The stable crude wood vinegar as claimed in claim 1, which is composed of the following components in parts by weight:
80-99 parts of crude wood vinegar;
10-20 parts of a surfactant;
0-5 parts of antifreeze.
3. The stable crude pyroligneous acid as claimed in claim 1 or 2, wherein said surfactant comprises surfactant A having HLB of 10 or more.
4. The stable crude wood vinegar of claim 3, wherein the surfactant A is one or more of sodium dodecylbenzene sulfonate, tristyrylphenol polyoxyethylene ether and phosphate ester or sulfonate thereof, castor oil polyoxyethylene ether, alkylphenol polyoxyethylene ether and phosphate ester or ammonium salt thereof, tristyrylphenol polyoxyethylene polyoxypropylene ether, fatty alcohol polyoxyethylene ether and sodium salt or ammonium salt thereof, plant polyene phenol polyoxyethylene ether and phosphate ester salt thereof, high molecular block polyether, polyoxyethylene sorbitan fatty acid ester, alkyl glycoside, alkyl betaine or cocamide betaine, fatty alcohol ethylene oxide condensate, tallow amine polyoxyethylene ether, alkylphenol formaldehyde resin polyoxyethylene ether sulfate, diisooctyl maleate sulfonate, benzyl dimethyl phenol polyoxyethylene ether, alkylphenol formaldehyde resin polyoxyethylene ether, fluorocarbon, fluorosilicone surfactant.
5. The stable crude wood vinegar as claimed in claim 4, wherein said surfactant further comprises a surfactant B having HLB < 10.
6. The stable crude pyroligneous acid according to claim 5 wherein said surfactant B is one or more selected from the group consisting of calcium dodecylbenzene sulfonate, ammonium dodecylbenzene sulfonate, castor oil polyoxyethylene ether, alkylphenol polyoxyethylene ether, plant polyene phenol polyoxyethylene ether, sorbitan fatty acid ester, tallow amine polyoxyethylene ether, silicone polyether.
7. The stable crude wood vinegar as claimed in claim 6, wherein the mass ratio of the surfactant B to the surfactant A is 1.4 or less.
8. The stable crude wood vinegar according to claim 1 or 2, wherein said crude wood vinegar is wood vinegar, bamboo vinegar or grass vinegar.
9. The stable crude wood vinegar according to claim 1 or 2, wherein the anti-freezing agent is ethylene glycol, propylene glycol or urea.
10. The method for preparing stable crude pyroligneous acid as claimed in any one of claims 1 to 9, wherein the crude pyroligneous acid, the surfactant and the anti-freezing agent are uniformly mixed.
CN202210740568.1A 2022-06-28 2022-06-28 Stable crude wood vinegar and preparation method thereof Pending CN115161056A (en)

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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH11269469A (en) * 1998-03-24 1999-10-05 Kaihatsu Koji Kk Production of high-quality pyroligneous acid material
JP2002020762A (en) * 2000-07-07 2002-01-23 Shoji Kurosawa Method for stabilizing solution property of smoking liquid
CN102503667A (en) * 2011-10-21 2012-06-20 北京雷力农用化学有限公司 Foliage fertilizer and preparation method thereof
CN104798824A (en) * 2015-02-15 2015-07-29 抚顺市世纪东方生物质综合技术开发有限公司 Botanical fungicide as well as preparation, use and storage methods thereof
CN105340969A (en) * 2015-12-04 2016-02-24 成都新朝阳作物科学有限公司 Natural herbicide composition and application thereof
CN108949214A (en) * 2018-08-08 2018-12-07 唐山市新雅诺生物科技有限公司 A kind of single flash wood vinegar, purification wood tar, for killing paste for removing and inhibiting psoriasis mushroom and preparation method thereof
CN110746232A (en) * 2019-12-11 2020-02-04 武汉天颖环境工程股份有限公司 Preparation method of pyroligneous foliar fertilizer with lasting fertilizer effect
CN114009431A (en) * 2021-12-08 2022-02-08 中化化工科学技术研究总院有限公司 Novel herbicide synergist and preparation and use methods thereof

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH11269469A (en) * 1998-03-24 1999-10-05 Kaihatsu Koji Kk Production of high-quality pyroligneous acid material
JP2002020762A (en) * 2000-07-07 2002-01-23 Shoji Kurosawa Method for stabilizing solution property of smoking liquid
CN102503667A (en) * 2011-10-21 2012-06-20 北京雷力农用化学有限公司 Foliage fertilizer and preparation method thereof
CN104798824A (en) * 2015-02-15 2015-07-29 抚顺市世纪东方生物质综合技术开发有限公司 Botanical fungicide as well as preparation, use and storage methods thereof
CN105340969A (en) * 2015-12-04 2016-02-24 成都新朝阳作物科学有限公司 Natural herbicide composition and application thereof
CN108949214A (en) * 2018-08-08 2018-12-07 唐山市新雅诺生物科技有限公司 A kind of single flash wood vinegar, purification wood tar, for killing paste for removing and inhibiting psoriasis mushroom and preparation method thereof
CN110746232A (en) * 2019-12-11 2020-02-04 武汉天颖环境工程股份有限公司 Preparation method of pyroligneous foliar fertilizer with lasting fertilizer effect
CN114009431A (en) * 2021-12-08 2022-02-08 中化化工科学技术研究总院有限公司 Novel herbicide synergist and preparation and use methods thereof

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