CN112042680A - Environment-friendly preservative and preparation method thereof - Google Patents
Environment-friendly preservative and preparation method thereof Download PDFInfo
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- CN112042680A CN112042680A CN202010962561.5A CN202010962561A CN112042680A CN 112042680 A CN112042680 A CN 112042680A CN 202010962561 A CN202010962561 A CN 202010962561A CN 112042680 A CN112042680 A CN 112042680A
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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
- A01N27/00—Biocides, pest repellants or attractants, or plant growth regulators containing hydrocarbons
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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
- A01N33/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds
- A01N33/02—Amines; Quaternary ammonium compounds
- A01N33/12—Quaternary ammonium compounds
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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
- A01N35/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having two bonds to hetero atoms with at the most one bond to halogen, e.g. aldehyde radical
- A01N35/04—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having two bonds to hetero atoms with at the most one bond to halogen, e.g. aldehyde radical containing aldehyde or keto groups, or thio analogues thereof, directly attached to an aromatic ring system, e.g. acetophenone; Derivatives thereof, e.g. acetals
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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
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/02—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms
- A01N43/04—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom
- A01N43/14—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom six-membered rings
- A01N43/16—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom six-membered rings with oxygen as the ring hetero atom
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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
- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
- A01N47/40—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having a double or triple bond to nitrogen, e.g. cyanates, cyanamides
- A01N47/42—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having a double or triple bond to nitrogen, e.g. cyanates, cyanamides containing —N=CX2 groups, e.g. isothiourea
- A01N47/44—Guanidine; Derivatives 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
- A01N55/00—Biocides, pest repellants or attractants, or plant growth regulators, containing organic compounds containing elements other than carbon, hydrogen, halogen, oxygen, nitrogen and sulfur
- A01N55/08—Biocides, pest repellants or attractants, or plant growth regulators, containing organic compounds containing elements other than carbon, hydrogen, halogen, oxygen, nitrogen and sulfur containing boron
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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
- A01N63/00—Biocides, pest repellants or attractants, or plant growth regulators containing microorganisms, viruses, microbial fungi, animals or substances produced by, or obtained from, microorganisms, viruses, microbial fungi or animals, e.g. enzymes or fermentates
- A01N63/10—Animals; Substances produced thereby or obtained therefrom
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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
- A01N65/08—Magnoliopsida [dicotyledons]
- A01N65/32—Ranunculaceae [Buttercup family], e.g. hepatica, hydrastis or goldenseal
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
- B27K3/34—Organic impregnating agents
- B27K3/50—Mixtures of different organic impregnating agents
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/32—Polymers modified by chemical after-treatment
- C08G65/329—Polymers modified by chemical after-treatment with organic compounds
- C08G65/333—Polymers modified by chemical after-treatment with organic compounds containing nitrogen
- C08G65/33379—Polymers modified by chemical after-treatment with organic compounds containing nitrogen containing nitro group
- C08G65/33386—Polymers modified by chemical after-treatment with organic compounds containing nitrogen containing nitro group cyclic
- C08G65/33389—Polymers modified by chemical after-treatment with organic compounds containing nitrogen containing nitro group cyclic aromatic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/32—Polymers modified by chemical after-treatment
- C08G65/329—Polymers modified by chemical after-treatment with organic compounds
- C08G65/337—Polymers modified by chemical after-treatment with organic compounds containing other elements
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G81/00—Macromolecular compounds obtained by interreacting polymers in the absence of monomers, e.g. block polymers
Abstract
The invention discloses an environment-friendly preservative which is characterized by comprising the following components in parts by weight: 3-6 parts of salicylaldehyde norbornadiene ionized co-modified methoxy poly (ethylene glycol) amine lignosulfonate, 2-4 parts of diazo alkyl urea, 1-2 parts of 1-thianthrene boric acid, 0.5-1.5 parts of 1-ethyl-3-guanidino thiourea hydrochloride, 5-8 parts of antibacterial Chinese herbal medicine extract, 15-25 parts of ethanol and 150 parts of deionized water. The invention also provides a preparation method of the environment-friendly preservative. The environment-friendly preservative disclosed by the invention is good in corrosion prevention effect, good in environment-friendly performance, antibacterial and broad-spectrum, and excellent in performance stability.
Description
Technical Field
The invention relates to the technical field of preservatives, and particularly relates to an environment-friendly preservative and a preparation method thereof.
Background
In recent years, with the rapid increase of economy in China, the living standard of people is improved year by year, and the spiritual civilization construction is rapidly developed while the material civilization is pursued, so that the desire for improving the home environment is more and more urgent. Furniture has been expected to be more important as an important member of home environment. They want to achieve original and natural novelty through furniture. Under the situation, the furniture made of the wood and bamboo is generally accepted by people, the natural texture of the wood and bamboo is maintained, and the furniture is fresh, elegant, beautiful and comfortable, and not only maintains the inherent excellent characteristics of the wood and bamboo, such as high density, toughness, strength and the like.
The furniture made of wood and bamboo is made of wood and bamboo, various nutrient substances required by the growth of microorganisms are rich in the tissue structure of the wood and bamboo, the growth of the microorganisms easily causes the mildew and color change of the wood and the products thereof, the use value of the wood and the products is reduced, and the wood and the products are not beneficial to subsequent processing and utilization, so the mildew-proof and corrosion-proof technology of the wood and the bamboo is always concerned, and the mildew-proof and corrosion-proof technology is an important way and means for prolonging the service life of the wood and the bamboo, improving the utilization level of the wood and the bamboo and saving the wood resources.
To date, the most common methods of protection against mold and corrosion are chemical agents, leakage and exudation of the preservative during production and use, and disposal and burning of the preservative treated wood can have adverse effects on the environment and harm human health. As environmental concerns become more and more of a concern, the choice of preservative is also critical. The wood preservative commonly used in the world at present mainly comprises copper, chromium, arsenic, copper amine quaternary ammonium salt, copper azole and the like, and arsenic and chromium in copper, chromium and arsenic are toxic substances, so that the wood preservative is easy to damage human bodies, and particularly has greater harm to the human bodies when used indoors. The wood protective agent in the prior art is prepared by adding ammonia or amine solvent into a sterilization protective component, and the ammonia or amine solvent is necessary for dissolving copper compounds and achieving the sterilization protective effect, so that a large amount of solvent is consumed, and the environment is polluted because the amine or the amine solvent is easy to volatilize. In addition, the volatilization of the solvent can bring out partial components of the preservative, thereby affecting the fixing performance of the preservative and reducing the sterilization effect.
The Chinese patent with application number 200910147579.3 discloses a novel wood preservative. Comprises the following raw materials: cnidium monnieri, radix sophorae flavescentis, fructus kochiae, radix stemonae and rhizoma smilacis glabrae. Root and bark of Melia azedarach L. Has the advantages that: the wood preservative prepared by adopting the traditional Chinese medicine formula has antibacterial and insect-proof effects, also has a certain inhibiting effect on wood rot fungi, and is completely a green and environment-friendly material: the traditional Chinese medicine is low in price, and compared with a chemical agent, the cost can be reduced by preparing the wood preservative; the preparation process of the traditional Chinese medicine is simple, and the energy consumption can be saved. The traditional Chinese medicine preparation is mainly prepared by decocting, and the required equipment is simpler; the traditional Chinese medicine has good antiseptic effect; the traditional Chinese medicine is an absolute green resource, and has higher safety to the environment compared with a chemical preservative. However, the preservative of pure traditional Chinese medicines has limited preservative property, slow effect and insufficient broad spectrum.
Therefore, the development of an environment-friendly preservative with good corrosion prevention effect, good environment-friendly performance, broad antibacterial spectrum and excellent performance stability is very important.
Disclosure of Invention
In view of the above, the invention aims to provide an environment-friendly preservative and a preparation method thereof, wherein the preparation method is simple and easy to implement, has high preparation efficiency, has low requirements on reaction conditions and equipment, and is suitable for continuous large-scale production; the prepared environment-friendly preservative has the advantages of good corrosion prevention effect, good environment-friendly performance, broad antibacterial spectrum and excellent performance stability.
In order to achieve the purpose, the invention adopts the technical scheme that:
the environment-friendly preservative is characterized by comprising the following components in parts by weight: 3-6 parts of salicylaldehyde norbornadiene ionized co-modified methoxy poly (ethylene glycol) amine lignosulfonate, 2-4 parts of diazo alkyl urea, 1-2 parts of 1-thianthrene boric acid, 0.5-1.5 parts of 1-ethyl-3-guanidino thiourea hydrochloride, 5-8 parts of antibacterial Chinese herbal medicine extract, 15-25 parts of ethanol and 150 parts of deionized water.
Preferably, the preparation method of the salicylaldehyde norbornadiene ionized co-modified methoxy poly (ethylene glycol) amine lignosulfonate comprises the following steps:
step S1, adding methoxy poly (ethylene glycol) amine, 7-chloronorbornadiene and 3-chloromethyl-5-nitro salicylaldehyde into a high-boiling-point solvent, stirring and reacting for 8-10 hours at 70-80 ℃, and then performing rotary evaporation to remove the solvent to obtain salicylaldehyde norbornadiene ionized co-modified methoxy poly (ethylene glycol) amine;
and S2, adding the salicylaldehyde norbornadiene ionized co-modified methoxy poly (ethylene glycol) amine and sodium lignosulfonate prepared in the step S1 into water, stirring and reacting at 50-60 ℃ for 6-8 hours, pouring the obtained solution into a dialysis bag, dialyzing in deionized water for 10-20 hours, and then performing rotary evaporation on the solution in the dialysis bag to remove water to obtain the salicylaldehyde norbornadiene ionized co-modified methoxy poly (ethylene glycol) amine lignosulfonate.
Preferably, the molar ratio of the methoxy poly (ethylene glycol) amine, the 7-chloronorbornadiene, the 3-chloromethyl-5-nitro salicylaldehyde and the high-boiling-point solvent in the step S1 is 1:1:2 (15-25).
Preferably, the high boiling point solvent is at least one of dimethyl sulfoxide, N-dimethylformamide, N-dimethylacetamide and N-methylpyrrolidone.
Preferably, the molar ratio of the salicylaldehyde norbornadiene ionized co-modified methoxy poly (ethylene glycol) amine, the sodium lignosulfonate and the water in the step S2 is 2:1 (20-30).
Preferably, the methoxypoly (ethylene glycol) amine has a weight average molecular weight of 2000.
Preferably, the antibacterial Chinese herbal medicine extract is prepared from the following raw material medicines in parts by weight: 1-3 parts of Chinese pulsatilla root, 2-4 parts of verbena, 1-4 parts of desmodium, 1-3 parts of folium isatidis, 2-5 parts of Chinese violet, 1-2 parts of musk, 1-3 parts of subprostrate sophora and 2-4 parts of bitter gourd.
Preferably, the preparation method of the antibacterial Chinese herbal medicine extract comprises the following steps: mixing the above materials uniformly to obtain a mixture, adding water into the mixture, decocting at 80-90 deg.C for 2-4 hr, filtering to remove residue, collecting filtrate, and removing water by rotary evaporation to obtain Chinese medicinal extract.
Preferably, the mass ratio of the mixed material to the water is 1 (6-12).
The invention also aims to provide a preparation method of the environment-friendly preservative, which is characterized by comprising the following steps: the components are uniformly mixed according to the parts by weight, stirred and reacted for 3-5 hours at the temperature of 60-80 ℃, and then cooled to room temperature, so that the environment-friendly preservative is obtained.
Adopt the produced beneficial effect of above-mentioned technical scheme to lie in:
(1) the preparation method of the environment-friendly preservative provided by the invention is simple and feasible, has high preparation efficiency, has low requirements on reaction conditions and equipment, and is suitable for continuous large-scale production.
(2) The environment-friendly preservative provided by the invention overcomes the defects that the traditional preservative is easy to damage human bodies due to leakage and seepage in the production and use processes, and the fixation performance of the preservative is influenced and the sterilization and disinfection effects are reduced due to the fact that partial components of the preservative are often brought out by volatilization of a solvent, and has the advantages of good preservative effect, good environment-friendly performance, broad antibacterial spectrum and excellent performance stability.
(3) According to the environment-friendly preservative provided by the invention, salicylaldehyde norbornadiene ionized co-modified methoxy poly (ethylene glycol) amine lignosulfonate is added, and the excellent preservative performance of salicylaldehyde, norbornadiene, methoxy poly (ethylene glycol) amine and lignosulfonate is combined, so that high osmotic pressure can be generated when the antiseptic acts with protein, and the protein is rapidly dehydrated in a large amount; in addition, a protective layer can be formed on the surface of the protein to prevent the surface of bacteria from absorbing invasion and degrading enzyme, so that the bacteriostatic effect is achieved. The active ingredients are connected into a whole in a chemical bond form, so that the active ingredients can better play a synergistic effect, the performance of the preservative is more stable, the quaternary ammonium salt structure is introduced into the molecular chain through modification, the antibacterial and anticorrosive performance can be further improved, different structures have different anticorrosive principles, and the anticorrosive functional groups of different principles have synergistic effect, so that the antibacterial and anticorrosive broad spectrum is effectively improved.
(4) The environment-friendly preservative provided by the invention has the synergistic effect of diazoalkyl urea, 1-thianthrene boric acid and 1-ethyl-3-guanidino thiourea hydrochloride, so that the preservative effect is improved. The 1-thianthrene boric acid is easily connected with quaternary ammonium salt cationic groups on salicylaldehyde norbornadiene ionized co-modified methoxy poly (ethylene glycol) amine lignosulfonate in an ionic bond form through ion exchange, so that the performance is more stable.
(5) According to the environment-friendly preservative provided by the invention, the antibacterial Chinese herbal medicine extract is added, and the raw material medicines are reasonably compatible and cooperate, so that the preservative effect is further improved, and the raw material medicines are natural, non-toxic and harmless to the environment, and more environment-friendly.
Detailed Description
In order to make the technical solutions of the present invention better understood and make the above features, objects, and advantages of the present invention more comprehensible, the present invention is further described with reference to the following examples. The examples are intended to illustrate the invention only and are not intended to limit the scope of the invention.
In the embodiment of the invention, the raw materials are all purchased commercially.
Example 1
The environment-friendly preservative is characterized by comprising the following components in parts by weight: 3 parts of salicylaldehyde norbornadiene ionized co-modified methoxy poly (ethylene glycol) amine lignosulfonate, 2 parts of diazoalkyl urea, 1 part of 1-thianthrene boric acid, 0.5 part of 1-ethyl-3-guanidino thiourea hydrochloride, 5 parts of antibacterial Chinese herbal medicine extract, 15 parts of ethanol and 120 parts of deionized water.
The preparation method of the salicylaldehyde norbornadiene ionized co-modified methoxy poly (ethylene glycol) amine lignosulfonate comprises the following steps:
step S1, adding methoxy poly (ethylene glycol) amine, 7-chloronorbornadiene and 3-chloromethyl-5-nitro salicylaldehyde into a high-boiling-point solvent, stirring and reacting for 8 hours at 70 ℃, and then performing rotary evaporation to remove the solvent to obtain salicylaldehyde norbornadiene ionized co-modified methoxy poly (ethylene glycol) amine;
and S2, adding the salicylaldehyde norbornadiene ionized co-modified methoxy poly (ethylene glycol) amine and sodium lignosulfonate prepared in the step S1 into water, stirring and reacting at 50 ℃ for 6 hours, pouring the obtained solution into a dialysis bag, dialyzing in deionized water for 10 hours, and performing rotary evaporation on the solution in the dialysis bag to remove water to obtain the salicylaldehyde norbornadiene ionized co-modified methoxy poly (ethylene glycol) amine lignosulfonate.
In the step S1, the molar ratio of the methoxy poly (ethylene glycol) amine, the 7-chloronorbornadiene, the 3-chloromethyl-5-nitro salicylaldehyde and the high-boiling-point solvent is 1:1:2: 15; the high boiling point solvent is dimethyl sulfoxide.
In the step S2, the molar ratio of the salicylaldehyde norbornadiene ionized co-modified methoxy poly (ethylene glycol) amine to the sodium lignosulfonate to the water is 2:1: 20.
The methoxypoly (ethyleneglycol) amine has a weight average molecular weight of 2000.
The antibacterial Chinese herbal medicine extract is prepared from the following raw material medicines in parts by weight: 1 part of Chinese pulsatilla root, 2 parts of verbena, 1 part of desmodium, 1 part of folium isatidis, 2 parts of Chinese violet, 1 part of musk, 1 part of subprostrate sophora and 2 parts of balsam pear.
The preparation method of the antibacterial Chinese herbal medicine extract comprises the following steps: mixing the raw materials uniformly to obtain a mixed material, adding water into the mixed material, decocting at 80 ℃ for 2 hours, filtering to remove residues, taking the filtrate, and removing water by rotary evaporation to obtain a Chinese herbal medicine extract; the mass ratio of the mixed material to the water is 1: 6.
The preparation method of the environment-friendly preservative is characterized by comprising the following steps of: the components are uniformly mixed according to the parts by weight, stirred and reacted for 3 hours at the temperature of 60 ℃, and then cooled to room temperature, so that the environment-friendly preservative is obtained.
Example 2
The environment-friendly preservative is characterized by comprising the following components in parts by weight: 4 parts of salicylaldehyde norbornadiene ionized co-modified methoxy poly (ethylene glycol) amine lignosulfonate, 2.5 parts of diazoalkyl urea, 1.2 parts of 1-thianthrene boric acid, 0.7 part of 1-ethyl-3-guanidino thiourea hydrochloride, 6 parts of antibacterial Chinese herbal medicine extract, 17 parts of ethanol and 130 parts of deionized water.
The preparation method of the salicylaldehyde norbornadiene ionized co-modified methoxy poly (ethylene glycol) amine lignosulfonate comprises the following steps:
step S1, adding methoxy poly (ethylene glycol) amine, 7-chloronorbornadiene and 3-chloromethyl-5-nitro salicylaldehyde into a high-boiling-point solvent, stirring and reacting for 8.5 hours at 73 ℃, and then performing rotary evaporation to remove the solvent to obtain salicylaldehyde norbornadiene ionized co-modified methoxy poly (ethylene glycol) amine;
and S2, adding the salicylaldehyde norbornadiene ionized co-modified methoxy poly (ethylene glycol) amine and sodium lignosulfonate prepared in the step S1 into water, stirring and reacting at 52 ℃ for 6.5 hours, pouring the obtained solution into a dialysis bag, dialyzing in deionized water for 13 hours, and then performing rotary evaporation on the solution in the dialysis bag to remove water, so as to obtain the salicylaldehyde norbornadiene ionized co-modified methoxy poly (ethylene glycol) amine lignosulfonate.
In the step S1, the molar ratio of the methoxy poly (ethylene glycol) amine, the 7-chloronorbornadiene, the 3-chloromethyl-5-nitro salicylaldehyde and the high-boiling-point solvent is 1:1:2: 17; the high boiling point solvent is N, N-dimethylformamide.
In the step S2, the molar ratio of the salicylaldehyde norbornadiene ionized co-modified methoxy poly (ethylene glycol) amine to the sodium lignosulfonate to the water is 2:1: 23.
The methoxypoly (ethyleneglycol) amine has a weight average molecular weight of 2000.
The antibacterial Chinese herbal medicine extract is prepared from the following raw material medicines in parts by weight: 1.5 parts of Chinese pulsatilla root, 2.5 parts of verbena, 2 parts of desmodium, 1.5 parts of dyers woad leaf, 3 parts of Chinese violet, 1.2 parts of musk, 1.5 parts of subprostrate sophora and 2.5 parts of balsam pear.
The preparation method of the antibacterial Chinese herbal medicine extract comprises the following steps: mixing the raw materials uniformly to obtain a mixed material, adding water into the mixed material, decocting at 83 deg.C for 2.5 hr, filtering to remove residue, collecting filtrate, and removing water by rotary evaporation to obtain Chinese herbal medicine extract; the mass ratio of the mixed material to the water is 1: 8.
The preparation method of the environment-friendly preservative is characterized by comprising the following steps of: the components are uniformly mixed according to the parts by weight, stirred and reacted for 3.5 hours at the temperature of 65 ℃, and then cooled to room temperature, so that the environment-friendly preservative is obtained.
Example 3
The environment-friendly preservative is characterized by comprising the following components in parts by weight: 4.5 parts of salicylaldehyde norbornadiene ionized co-modified methoxy poly (ethylene glycol) amine lignosulfonate, 3 parts of diazo alkyl urea, 1.5 parts of 1-thianthrene boric acid, 1 part of 1-ethyl-3-guanidino thiourea hydrochloride, 6.5 parts of antibacterial Chinese herbal medicine extract, 20 parts of ethanol and 135 parts of deionized water.
The preparation method of the salicylaldehyde norbornadiene ionized co-modified methoxy poly (ethylene glycol) amine lignosulfonate comprises the following steps:
step S1, adding methoxy poly (ethylene glycol) amine, 7-chloronorbornadiene and 3-chloromethyl-5-nitro salicylaldehyde into a high-boiling-point solvent, stirring and reacting for 9 hours at 75 ℃, and then performing rotary evaporation to remove the solvent to obtain salicylaldehyde norbornadiene ionized co-modified methoxy poly (ethylene glycol) amine;
and S2, adding the salicylaldehyde norbornadiene ionized co-modified methoxy poly (ethylene glycol) amine and sodium lignosulfonate prepared in the step S1 into water, stirring and reacting at 55 ℃ for 7 hours, pouring the obtained solution into a dialysis bag, dialyzing in deionized water for 15 hours, and performing rotary evaporation on the solution in the dialysis bag to remove water to obtain the salicylaldehyde norbornadiene ionized co-modified methoxy poly (ethylene glycol) amine lignosulfonate.
In the step S1, the molar ratio of the methoxy poly (ethylene glycol) amine, the 7-chloronorbornadiene, the 3-chloromethyl-5-nitro salicylaldehyde and the high-boiling-point solvent is 1:1:2: 20; the high boiling point solvent is N, N-dimethylacetamide.
In the step S2, the molar ratio of the salicylaldehyde norbornadiene ionized co-modified methoxy poly (ethylene glycol) amine to the sodium lignosulfonate to the water is 2:1: 25; the methoxypoly (ethyleneglycol) amine has a weight average molecular weight of 2000.
The antibacterial Chinese herbal medicine extract is prepared from the following raw material medicines in parts by weight: 2 parts of Chinese pulsatilla root, 3 parts of verbena, 2.5 parts of desmodium, 2 parts of dyers woad leaf, 3.5 parts of Chinese violet, 1.5 parts of musk, 2 parts of subprostrate sophora and 3 parts of balsam pear.
The preparation method of the antibacterial Chinese herbal medicine extract comprises the following steps: mixing the raw materials uniformly to obtain a mixed material, adding water into the mixed material, decocting at 85 ℃ for 3 hours, filtering to remove residues, taking the filtrate, and removing water by rotary evaporation to obtain a Chinese herbal medicine extract; the mass ratio of the mixed material to the water is 1: 9.
The preparation method of the environment-friendly preservative is characterized by comprising the following steps of: the components are uniformly mixed according to the parts by weight, stirred and reacted for 4 hours at the temperature of 70 ℃, and then cooled to room temperature, so as to obtain the environment-friendly preservative.
Example 4
The environment-friendly preservative is characterized by comprising the following components in parts by weight: 5.5 parts of salicylaldehyde norbornadiene ionized co-modified methoxy poly (ethylene glycol) amine lignosulfonate, 3.5 parts of diazo alkyl urea, 1.8 parts of 1-thianthrene boric acid, 1.4 parts of 1-ethyl-3-guanidino thiourea hydrochloride, 7.5 parts of antibacterial Chinese herbal medicine extract, 24 parts of ethanol and 145 parts of deionized water.
The preparation method of the salicylaldehyde norbornadiene ionized co-modified methoxy poly (ethylene glycol) amine lignosulfonate comprises the following steps:
step S1, adding methoxy poly (ethylene glycol) amine, 7-chloronorbornadiene and 3-chloromethyl-5-nitro salicylaldehyde into a high-boiling-point solvent, stirring and reacting for 9.5 hours at 78 ℃, and then performing rotary evaporation to remove the solvent to obtain salicylaldehyde norbornadiene ionized co-modified methoxy poly (ethylene glycol) amine;
and S2, adding the salicylaldehyde norbornadiene ionized co-modified methoxy poly (ethylene glycol) amine and sodium lignosulfonate prepared in the step S1 into water, stirring and reacting at 58 ℃ for 7.5 hours, pouring the obtained solution into a dialysis bag, dialyzing in deionized water for 19 hours, and then performing rotary evaporation on the solution in the dialysis bag to remove water, so as to obtain the salicylaldehyde norbornadiene ionized co-modified methoxy poly (ethylene glycol) amine lignosulfonate.
In the step S1, the molar ratio of the methoxy poly (ethylene glycol) amine, the 7-chloronorbornadiene, the 3-chloromethyl-5-nitro salicylaldehyde and the high-boiling-point solvent is 1:1:2: 24; the high boiling point solvent is formed by mixing dimethyl sulfoxide, N-dimethylformamide, N-dimethylacetamide and N-methylpyrrolidone according to a mass ratio of 1:2:2: 3.
In the step S2, the molar ratio of the salicylaldehyde norbornadiene ionized co-modified methoxy poly (ethylene glycol) amine to the sodium lignosulfonate to the water is 2:1: 28; the methoxypoly (ethyleneglycol) amine has a weight average molecular weight of 2000.
The antibacterial Chinese herbal medicine extract is prepared from the following raw material medicines in parts by weight: 2.5 parts of Chinese pulsatilla root, 3.5 parts of verbena, 3.5 parts of desmodium, 2.5 parts of dyers woad leaf, 4.5 parts of Chinese violet, 1.8 parts of musk, 2.5 parts of subprostrate sophora and 3.5 parts of balsam pear.
The preparation method of the antibacterial Chinese herbal medicine extract comprises the following steps: mixing the raw materials uniformly to obtain a mixed material, adding water into the mixed material, decocting at 88 ℃ for 3.5 hours, filtering to remove residues, taking the filtrate, and removing water by rotary evaporation to obtain a Chinese herbal medicine extract; the mass ratio of the mixed material to the water is 1: 11.
The preparation method of the environment-friendly preservative is characterized by comprising the following steps of: the components are uniformly mixed according to the parts by weight, stirred and reacted for 4.5 hours at 78 ℃, and then cooled to room temperature, so as to obtain the environment-friendly preservative.
Example 5
The environment-friendly preservative is characterized by comprising the following components in parts by weight: 6 parts of salicylaldehyde norbornadiene ionized co-modified methoxy poly (ethylene glycol) amine lignosulfonate, 4 parts of diazo alkyl urea, 2 parts of 1-thianthrene boric acid, 1.5 parts of 1-ethyl-3-guanidino thiourea hydrochloride, 8 parts of an antibacterial Chinese herbal medicine extract, 25 parts of ethanol and 150 parts of deionized water.
The preparation method of the salicylaldehyde norbornadiene ionized co-modified methoxy poly (ethylene glycol) amine lignosulfonate comprises the following steps:
step S1, adding methoxy poly (ethylene glycol) amine, 7-chloronorbornadiene and 3-chloromethyl-5-nitro salicylaldehyde into a high-boiling-point solvent, stirring and reacting for 10 hours at 80 ℃, and then performing rotary evaporation to remove the solvent to obtain salicylaldehyde norbornadiene ionized co-modified methoxy poly (ethylene glycol) amine;
and S2, adding the salicylaldehyde norbornadiene ionized co-modified methoxy poly (ethylene glycol) amine prepared in the step S1 and sodium lignosulfonate into water, stirring and reacting for 8 hours at 60 ℃, pouring the obtained solution into a dialysis bag, dialyzing for 20 hours in deionized water, and performing rotary evaporation on the solution in the dialysis bag to remove water to obtain the salicylaldehyde norbornadiene ionized co-modified methoxy poly (ethylene glycol) amine lignosulfonate.
In the step S1, the molar ratio of the methoxy poly (ethylene glycol) amine, the 7-chloronorbornadiene, the 3-chloromethyl-5-nitro salicylaldehyde and the high-boiling-point solvent is 1:1:2: 25; the high boiling point solvent is N-methyl pyrrolidone.
In the step S2, the molar ratio of the salicylaldehyde norbornadiene ionized co-modified methoxy poly (ethylene glycol) amine to the sodium lignosulfonate to the water is 2:1: 30; the methoxypoly (ethyleneglycol) amine has a weight average molecular weight of 2000.
The antibacterial Chinese herbal medicine extract is prepared from the following raw material medicines in parts by weight: 3 parts of Chinese pulsatilla root, 4 parts of verbena, 4 parts of desmodium, 3 parts of folium isatidis, 5 parts of Chinese violet, 2 parts of musk, 3 parts of subprostrate sophora and 4 parts of balsam pear.
The preparation method of the antibacterial Chinese herbal medicine extract comprises the following steps: mixing the raw materials uniformly to obtain a mixed material, adding water into the mixed material, decocting at 90 ℃ for 4 hours, filtering to remove residues, taking the filtrate, and removing water by rotary evaporation to obtain a Chinese herbal medicine extract; the mass ratio of the mixed material to the water is 1: 12.
The preparation method of the environment-friendly preservative is characterized by comprising the following steps of: the components are uniformly mixed according to the parts by weight, stirred and reacted for 5 hours at the temperature of 80 ℃, and then cooled to room temperature, so that the environment-friendly preservative is obtained.
Comparative example 1
This example provides an environmentally friendly preservative having the same formulation and preparation method as example 1, except that no salicylaldehyde norbornadiene ionized co-modified methoxy poly (ethylene glycol) amine lignosulfonate was added.
Comparative example 2
This example provides an environmentally friendly preservative formulation and method of preparation similar to example 1 except that no diazolidinyl urea is added.
Comparative example 3
This example provides an environmentally friendly preservative formulation and method of preparation similar to example 1 except that 1-thianthrene boronic acid and 1-ethyl-3-guanidinothiourea hydrochloride were not added.
Comparative example 4
This example provides an environmentally friendly preservative having the same formulation and preparation method as example 1, except that no antibacterial herbal extract is added.
In order to further illustrate the beneficial technical effects of the embodiments of the present invention, the environmental protection preservatives described in the embodiments 1 to 5 and the comparative examples 1 to 4 are subjected to related performance tests, the test method refers to the forestry industry standard LY/T1283-1998 "laboratory test method for toxicity of wood preservative on decay fungi", hairy poplar is used as a test material, each preservative is used for treating the sample, an indoor corrosion resistance test is performed, and the average weight loss rate of the white decay sample and the average weight loss rate of the brown decay sample are respectively calculated, and the results are shown in table 1.
TABLE 1
| Item | Average weight loss ratio (%) of white rot sample | Average weight loss ratio (%) |
| Examples1 | 5.14 | 4.20 |
| Example 2 | 5.09 | 4.14 |
| Example 3 | 5.03 | 4.10 |
| Example 4 | 4.96 | 4.03 |
| Example 5 | 4.90 | 3.97 |
| Comparative example 1 | 6.70 | 5.88 |
| Comparative example 2 | 6.62 | 5.81 |
| Comparative example 3 | 6.56 | 5.79 |
| Comparative example 4 | 6.58 | 5.90 |
As can be seen from Table 1, the environmentally friendly preservative disclosed in the examples of the present invention has better preservative performance for both white rot fungi and brown rot fungi, which is the result of the synergistic effect of the components.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. The environment-friendly preservative is characterized by comprising the following components in parts by weight: 3-6 parts of salicylaldehyde norbornadiene ionized co-modified methoxy poly (ethylene glycol) amine lignosulfonate, 2-4 parts of diazo alkyl urea, 1-2 parts of 1-thianthrene boric acid, 0.5-1.5 parts of 1-ethyl-3-guanidino thiourea hydrochloride, 5-8 parts of antibacterial Chinese herbal medicine extract, 15-25 parts of ethanol and 150 parts of deionized water.
2. The environment-friendly preservative according to claim 1, wherein the preparation method of the salicylaldehyde norbornadiene ionized co-modified methoxy poly (ethylene glycol) amine lignosulfonate comprises the following steps:
step S1, adding methoxy poly (ethylene glycol) amine, 7-chloronorbornadiene and 3-chloromethyl-5-nitro salicylaldehyde into a high-boiling-point solvent, stirring and reacting for 8-10 hours at 70-80 ℃, and then performing rotary evaporation to remove the solvent to obtain salicylaldehyde norbornadiene ionized co-modified methoxy poly (ethylene glycol) amine;
and S2, adding the salicylaldehyde norbornadiene ionized co-modified methoxy poly (ethylene glycol) amine and sodium lignosulfonate prepared in the step S1 into water, stirring and reacting at 50-60 ℃ for 6-8 hours, pouring the obtained solution into a dialysis bag, dialyzing in deionized water for 10-20 hours, and then performing rotary evaporation on the solution in the dialysis bag to remove water to obtain the salicylaldehyde norbornadiene ionized co-modified methoxy poly (ethylene glycol) amine lignosulfonate.
3. The environment-friendly preservative according to claim 2, wherein the molar ratio of the methoxy poly (ethylene glycol) amine, the 7-chloronorbornadiene, the 3-chloromethyl-5-nitro salicylaldehyde and the high-boiling-point solvent in the step S1 is 1:1:2 (15-25).
4. The environmentally friendly preservative according to claim 2, wherein the high boiling point solvent is at least one of dimethylsulfoxide, N-dimethylformamide, N-dimethylacetamide and N-methylpyrrolidone.
5. The environment-friendly preservative according to claim 2, wherein the molar ratio of the salicylaldehyde norbornadiene ionized co-modified methoxy poly (ethylene glycol) amine, the sodium lignosulfonate and the water in the step S2 is 2:1 (20-30).
6. The environmentally friendly preservative of claim 2, wherein the methoxypoly (ethyleneglycol) amine has a weight average molecular weight of 2000.
7. The environment-friendly preservative according to claim 1, wherein the antibacterial Chinese herbal medicine extract is prepared from the following raw material medicines in parts by weight: 1-3 parts of Chinese pulsatilla root, 2-4 parts of verbena, 1-4 parts of desmodium, 1-3 parts of folium isatidis, 2-5 parts of Chinese violet, 1-2 parts of musk, 1-3 parts of subprostrate sophora and 2-4 parts of bitter gourd.
8. The environment-friendly preservative according to claim 7, wherein the preparation method of the antibacterial Chinese herbal medicine extract comprises the following steps: mixing the above materials uniformly to obtain a mixture, adding water into the mixture, decocting at 80-90 deg.C for 2-4 hr, filtering to remove residue, collecting filtrate, and removing water by rotary evaporation to obtain Chinese medicinal extract.
9. The environment-friendly preservative according to claim 8, wherein the mass ratio of the mixed material to the water is 1 (6-12).
10. The environment-friendly preservative according to any one of claims 1 to 9, wherein the preparation method of the environment-friendly preservative comprises the following steps: the components are uniformly mixed according to the parts by weight, stirred and reacted for 3-5 hours at the temperature of 60-80 ℃, and then cooled to room temperature, so that the environment-friendly preservative is obtained.
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