CN106008190A - Preparation technology of new monosomic plant extract-powdery ethyl vanillin and application of new monosomic plant extract-powdery ethyl vanillin - Google Patents
Preparation technology of new monosomic plant extract-powdery ethyl vanillin and application of new monosomic plant extract-powdery ethyl vanillin Download PDFInfo
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- CN106008190A CN106008190A CN201610360452.XA CN201610360452A CN106008190A CN 106008190 A CN106008190 A CN 106008190A CN 201610360452 A CN201610360452 A CN 201610360452A CN 106008190 A CN106008190 A CN 106008190A
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- C07C45/78—Separation; Purification; Stabilisation; Use of additives
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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- 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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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/34—Alcohols
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- A—HUMAN NECESSITIES
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- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L9/00—Disinfection, sterilisation or deodorisation of air
- A61L9/01—Deodorant compositions
- A61L9/013—Deodorant compositions containing animal or plant extracts, or vegetable material
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/10—Washing or bathing preparations
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q5/00—Preparations for care of the hair
- A61Q5/02—Preparations for cleaning the hair
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
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- C07C45/81—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
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- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
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Abstract
The invention discloses a preparation technology of new monosomic plant extract-powdery ethyl vanillin and application of new monosomic plant extract-powdery ethyl vanillin. The preparation technology of the new monosomic plant extract-powdery ethyl vanillin comprises the following steps: selecting a 2-3-year-old thick and big moso bamboo; drilling a bamboo hole with the diameter of 0.4-1 cm in an interval, which is next to an upper section and a lower section, of an optional section which is away from the ground by less than 20-30 cm, and placing an edible preservative of which the volume is 12%-20% of the total volume in a bamboo section and bamboo leftovers with total amount of 80%-88% in the hole; placing in a closed earth kiln and heating to the temperature of 290-350 DEG C; after 2-3 days, placing collected plant extracts in an underground carrier under the conditions that the room temperature is 18-26 DEG C and the humidity is 60-80 degrees for 5-7 days; naturally dividing into an upper layer and a lower layer; placing a stock solution of the upper layer in a serpentine cooler with stirring and reflux condensing tubes; refluxing, and heating and stirring until the temperature reaches 65-85 DEG C; dropwise adding 6 ml-10 ml of solvent benzol; after 50-60 minutes, adding 2-5 grams of copperas; distilling and performing standing for 3-5 days again; recycling aquiform ethyl vanillin under the condition of separation and purification; drying and atomizing to obtain powdery ethyl vanillin.
Description
Present invention step and the preparation technology of a kind of new solitary plant extract-powdery ethyl vanillin and application thereof.
Background technology
New monomer-the ethyl vanillin of plant extract, traditional is main to be realized by this production method of Nitrosation Process in wood pulp waste liquor, eugenol, guaiacol, safrole.Domestic ethyl vanillin produces main nitroso process and the acetaldehyde acid system etc. of using, but the technique such as nitroso process and acetaldehyde acid system falls behind, seriously polluted, is faced with increasing environmental protection pressure.Therefore, it is necessary to improve.
Summary of the invention
The task of the present invention is to provide preparation technology and the application thereof of a kind of new solitary plant extract-powdery ethyl vanillin, the technical scheme is that such: the new extraction carrier of the present invention is bamboo branch Folium Bambusae and bamboo leftover bits and pieces, by selecting 2～3 years thick bamboo Phyllostachys pubescens Mazei ex H.de Lebaies of life, overhead any internode of below 20-30cm, in close proximity to being the most successively drilled to the bamboo hole of an a diameter of 0.4cm-1cm every place's electric drill, and in hole, load edible antistaling agent and the bamboo leftover bits and pieces of ring inner volume total amount 80%-88% of ring inner volume total amount 12%-20%；Take 5-10cm length, diameter is slightly less than the hollow conduit of hole, hollow tube at one end head inserts in bamboo hole, another termination of hollow conduit outer 0.5 1.5cm of dew bamboo hole, then conduit all seals with charcoal slurry with the conduit mouth of pipe of bamboo hole contact position and another termination of conduit of dew bamboo hole；Afterwards, it is heated up to 290 degree of-350 degree Celsius in being placed on airtight earth kiln, after 2-3 days, takes out conduit, liquid in ring (i.e. plant extract) is poured in sterile barrel.It is 18-26 degree Celsius that plant extract after collecting is placed on room temperature, humidity is underground carrier 5-7 days of 60-80 degree, naturally levels it is divided into, take upper strata stock solution and be placed in equipped with stirring, in the cooling coil(ed) pipe of reflux condensing tube, backflow and heated and stirred 65-85 DEG C dropping solvent benzol 6ml-l0ml, after 50 minutes-60 minutes, chlorination vitriol 2 grams-5 grams is neutrality to reactant. again stand 3-5 days through distillation, then plant extract adds phenethanol 1 gram-3 grams and purifies, become phenethanol and purify liquid, carry out the most again separating decompression distillation, watery ethyl vanillin is reclaimed under the conditions of separating-purifying.Ethyl vanillin drying spraying treatment after reclaiming can obtain powdery ethyl vanillin.
The new solitary plant extract-ethyl vanillin of the present invention by water dilution can by spray application in:
1. the new solitary plant extract-powdery ethyl vanillin by weight 1 of the present invention can be carried out eliminating abnormal flavour, dispel harmful substance by being sprayed in air, increase oxygen content in air than 500-800 water dilution (water 500-800 weight portion).
2. the new solitary plant extract-powdery ethyl vanillin by weight 1 of the present invention can dispel formaldehyde by being sprayed on household than 5-10 water dilution (water 5-10 weight portion), reduces indoor TVOC total content.
3. the new solitary plant extract-powdery ethyl vanillin by weight 1 of the present invention can use field by spray application in Personal hygiene than 15-20 water dilution (water 15-20 weight portion), does not hurts hands, potent decontamination.
4. the new solitary plant extract-powdery ethyl vanillin by weight 1 of the present invention than 750-1000 water dilution (water 750-1000 weight portion) can spray application in crops, reduce insect pest, increase yield, fertile soil.
5. the new solitary plant extract-powdery ethyl vanillin by weight 1 of the present invention is sprayed on body of wall after diluting than 9-11 water, can reduce electromagnetic wave to child and the injury of anemia of pregnant woman's health.
6, with other modes such as smearing after the new solitary plant extract-powdery ethyl vanillin by weight 1 of the present invention dilutes than 9-11 water, utilization skin nursing.
Compared with the prior art, the extraction carrier of the present invention is bamboo leftover bits and pieces and chlorine vitriol, is formed by phenethanol extraction process, and the powdery ethyl vanillin of the present invention has the advantage that feature after above-mentioned process:
1. acid-base reaction: ethyl vanillin dropping liquid contains weak acid, can directly carry out biodegradation, nontoxic.
2. catalytic oxidation: such as mercaptan in the ordinary course of things, it is impossible to react with the oxygen in air, but under the catalysis of ethyl vanillin, can react with the oxygen in air.
3. thermodynamic characteristics.Through the ethyl vanillin drop of atomization, its diameter is below 0.04 millimeter.In this case, the surface of drop can reach 1/3rd and 1/4th of some organic compound bond energys, is to destroy the key in foul smell molecule, makes them unstable, easily decomposes.
4. redox reaction.Such as, formaldehyde has oxidisability, and in ethyl vanillin C9H10O3, weak acid molecule has reproducibility.They can directly react.
Summary characterization experiments analyze, the ethyl vanillin of the present invention can be with gas with foreign flavor in decontamination chamber, by being combined with gas with foreign flavor molecule, and ethyl vanillin dropping liquid generation chemical reaction and be eliminated;It addition, ethyl vanillin can also eliminate chlorine and carbon dioxide, it is by generation corona effect around microgranule, and after corona produces, gas molecule and ethyl vanillin dropping liquid combine thus be removed.
The carrier of the present invention is simple with process of preparing, and carrier of the present invention and preparation technology can break through present Nitrosation Process environmental protection pressure and the bottleneck of acetaldehyde acid system process industry, break international blockade on new techniques.
Accompanying drawing explanation
Fig. 1 is bamboo feeding container used in the present invention;
Fig. 2 is bamboo container facade used in the present invention;
Fig. 3 is that the present invention is reclaimed the ethyl vanillin photo returned.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further described (but not being the restriction to patent of the present invention).
Embodiment
The new extraction carrier of the present invention is bamboo branch Folium Bambusae and bamboo leftover bits and pieces (described bamboo leftover bits and pieces refers to the bamboo saw block differed in size), by selecting 2～3 years thick bamboo Phyllostachys pubescens Mazei ex H.de Lebaies of life, overhead any internode of below 20-30cm, in close proximity to the hole being the most successively drilled to an a diameter of 1cm every place's electric drill, to pierce bamboo wall for degree, and in hole, load the edible antistaling agent of ring inner volume total amount 20% and the bamboo leftover bits and pieces of ring inner volume total amount 80%.Take 6cm length, diameter is slightly less than the hollow conduit of hole, hollow tube at one end head inserts in bamboo hole, another termination of hollow conduit outer 1cm of dew bamboo hole, then conduit all seals with charcoal slurry with the conduit mouth of pipe of bamboo hole contact position and another termination of conduit of dew bamboo hole；350 degree Celsius it are heated up in being placed on airtight earth kiln afterwards, after 3 days, take out conduit, liquid in ring (i.e. plant extract) is poured in sterile barrel, it is 18 degree Celsius that plant extract after collecting is placed on room temperature, humidity is the underground carrier 5 days of 60 degree, naturally levels it is divided into, take upper strata stock solution and be placed in equipped with stirring, in the cooling coil(ed) pipe of reflux condensing tube, solvent benzol l0mL is dripped in about 80 DEG C under backflow and stirring, after 1 hour, chlorination vitriol 5 grams is neutrality to reactant. again stand 3 days through distillation, then plant extract adds phenethanol 1 gram and purifies, become phenethanol and purify liquid, carry out the most again separating decompression distillation, watery ethyl vanillin is reclaimed under the conditions of 60 DEG C；Ethyl vanillin drying spraying treatment after reclaiming can obtain powdery ethyl vanillin.
Experimental data:
| Conduit concentration ppm | Reative cell concentration ppm | Ppm after contact | 5min | 20min | |
| Chlorine | 35 | 35 | 19.2 | 20 | ＜ 0.1 |
| Ammonia | 88 | 88 | 55 | 6 | ＜ 0.1 |
| Carbon dioxide | 3.9 | 3.9 | ＜ 0.02 | 1 | ＜ 0.1 |
Described new solitary plant extract-powdery ethyl vanillin, it can apply as follows:
Air purification field: by weight 1 can carry out air cleaning by being sprayed in air than the dilution of 500-800 weight parts water.New solitary plant extract air purifying process is not only invested low, easy to operate, and the suitability is wide, it is few to take up an area, and need not change, add structures and additional more facility.Employing lasting air purifies and need not consume substantial amounts of electric energy, safe handling is simple, facilitate operative, only need regular replenishment plant extract, and whole system maintenance is cheap with cost of business operation.Air purifying process is applicable not only to the interior space closed, and is more suitable for the exterior space large-scale, superhuge.
Household field: new solitary plant extract-powdery ethyl vanillin by weight 1 can remove abnormal smells from the patient, mycete, greasy dirt etc. than after 5-10 water dilution (water 5-10 weight portion) dilution by sprinkling.Additionally, the use of the new solitary plant extract along with the present invention, the quantity such as fly, mosquito, mouse also can reduce.
Personal hygiene use field: the new solitary plant extract-powdery ethyl vanillin by weight 1 of the present invention is than 15-20(water 15-20 weight portion) dilution after, can by spray application in Personal hygiene.Acetic acid molecule that new solitary plant extract contains and other probioticss, when washing hair, take a shower, doing washing, the new solitary plant extract adding the present invention after dilution can decompose and eliminate the microorganism that human body is harmful, can look after Personal hygiene and reach to maintain to obtain effect.
Crops field: after the new solitary plant extract-powdery ethyl vanillin by weight 1 of the present invention is than 750-1000 water dilution (water 750-1000 weight portion), can be by spray application in crops；Barren soil can be become rich soil after the new solitary plant extract dilution of the present invention.Also can reach simultaneously and reduce insect pest in the case of not using chemical pesticide and increase production.
Family health care field: the new solitary plant extract-powdery ethyl vanillin by weight 1 of the present invention can pass through spray booth inner wall after diluting than 9-11 water, can reduce electromagnetic wave to child and the injury of anemia of pregnant woman's health.
Medical skin is nursed: the new solitary plant extract-powdery ethyl vanillin by weight 1 of the present invention can use, after diluting than 9-11 water, other modes such as smearing, is applied to medical skin nursing.
Below it is only the specific embodiment of the present invention, all similar changes made according to above-mentioned design, the scope of the present invention ought to be belonged to.
Claims (8)
1. the preparation technology of new solitary plant extract-powdery ethyl vanillin, it is characterized in that, new extraction carrier is bamboo branch Folium Bambusae and bamboo leftover bits and pieces, by selecting 2～3 years thick bamboo Phyllostachys pubescens Mazei ex H.de Lebaies of life, overhead any internode of below 20-30cm, in close proximity to being the most successively drilled to the bamboo hole of an a diameter of 0.4cm-1cm every place's electric drill, and in hole, load edible antistaling agent and the bamboo leftover bits and pieces of ring inner volume total amount 80%-88% of ring inner volume total amount 12%-20%；Take 5-10cm length, diameter is slightly less than the hollow conduit of hole, hollow tube at one end head inserts in bamboo hole, another termination of hollow conduit outer 0.5 1.5cm of dew bamboo hole, then conduit all seals with charcoal slurry with the conduit mouth of pipe of bamboo hole contact position and another termination of conduit of dew bamboo hole；It is heated up to 290 degree of-350 degree Celsius in being placed on airtight earth kiln afterwards, after 2-3 days, takes out conduit, ring implants extract is poured in sterile barrel;It is 18-26 degree Celsius that plant extract after collecting is placed on room temperature, humidity is underground carrier 5-7 days of 60-80 degree, naturally levels it is divided into, take upper strata stock solution and be placed in equipped with stirring, in the cooling coil(ed) pipe of reflux condensing tube, backflow and heated and stirred 65-85 DEG C dropping solvent benzol 6ml-l0ml, after 50 minutes-60 minutes, chlorination vitriol 2 grams-5 grams is neutrality to reactant. again stand 3-5 days through distillation, then plant extract adds phenethanol 1 gram-3 grams and purifies, become phenethanol and purify liquid, carry out the most again separating decompression distillation, watery ethyl vanillin is reclaimed under the conditions of separating-purifying；Ethyl vanillin drying spraying treatment after reclaiming can obtain powdery ethyl vanillin.
2. the preparation technology of new solitary plant extract-powdery ethyl vanillin, it is characterized in that, new extraction carrier is bamboo branch Folium Bambusae and bamboo leftover bits and pieces, by selecting 2～3 years thick bamboo Phyllostachys pubescens Mazei ex H.de Lebaies of life, overhead any internode of below 20-30cm, in close proximity to being the most successively drilled to the hole of an a diameter of 1cm every place's electric drill, and in hole, load edible antistaling agent and the bamboo leftover bits and pieces of ring inner volume total amount 80% of ring inner volume total amount 20%；Take 6cm length, diameter is slightly less than the hollow tubing conductor of hole, hollow tubing conductor one termination is inserted in bamboo hole, another termination of hollow tubing conductor outer 1cm of dew bamboo hole, then conduit all seals with charcoal slurry with the conduit mouth of pipe of bamboo hole contact position and another termination of conduit of dew bamboo hole；350 degree Celsius it are heated up in being placed on airtight earth kiln afterwards, after 3 days, take out conduit, ring implants extract is poured in sterile barrel, it is 18 degree Celsius that plant extract after collecting is placed on room temperature, humidity is the underground carrier 5 days of 60 degree, naturally levels it is divided into, take upper strata stock solution and be placed in equipped with stirring, in the cooling coil(ed) pipe of reflux condensing tube, solvent benzol l0mL is dripped in about 80 DEG C under backflow and stirring, after 1 hour, chlorination vitriol 5 grams is neutrality to reactant. again stand 3 days through distillation, then plant extract adds phenethanol 1 gram and purifies, become phenethanol and purify liquid, carry out the most again separating decompression distillation, watery ethyl vanillin is reclaimed under the conditions of 60 DEG C；Ethyl vanillin drying spraying treatment after reclaiming can obtain powdery ethyl vanillin.
The application of new solitary plant extract-powdery ethyl vanillin the most according to claim 1 and 2, is characterized in that, after described new solitary plant extract-powdery ethyl vanillin dilutes than 500-800 weight parts water by 1, is sprayed in air.
The application of new solitary plant extract-powdery ethyl vanillin the most according to claim 1 and 2, is characterized in that, after described new solitary plant extract-powdery ethyl vanillin by weight 1 dilutes than 5-10 water, by being sprayed on household.
The application of new solitary plant extract-powdery ethyl vanillin the most according to claim 1 and 2, is characterized in that, after described new solitary plant extract-powdery ethyl vanillin by weight 1 dilutes than 15-20 water, by spray application in Personal hygiene.
The application of new solitary plant extract-powdery ethyl vanillin the most according to claim 1 and 2, is characterized in that, described new solitary plant extract-powdery ethyl vanillin by weight 1 dilute than 750-1000 water after spray application in crops.
The application of new solitary plant extract-powdery ethyl vanillin the most according to claim 1 and 2, is characterized in that, described new solitary plant extract-powdery ethyl vanillin by weight 1 is sprayed on body of wall after diluting than 9-11 water.
The application of new solitary plant extract-powdery ethyl vanillin the most according to claim 1 and 2, is characterized in that, described new solitary plant extract-powdery ethyl vanillin by weight 1 is applied to skin nursing by the mode of smearing after diluting than 9-11 water.
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| CN201610360452.XA CN106008190A (en) | 2016-05-28 | 2016-05-28 | Preparation technology of new monosomic plant extract-powdery ethyl vanillin and application of new monosomic plant extract-powdery ethyl vanillin |
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| CN201610360452.XA CN106008190A (en) | 2016-05-28 | 2016-05-28 | Preparation technology of new monosomic plant extract-powdery ethyl vanillin and application of new monosomic plant extract-powdery ethyl vanillin |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2062205A (en) * | 1932-03-21 | 1936-11-24 | Boedecker Friedrich | Process of producing the m-alkylethers of protocatechuic aldehyde |
| CN102503788A (en) * | 2011-11-21 | 2012-06-20 | 湖南大学 | Application of 4-(2-methylallyl)-1,2-dihydroxybenzene in preparation of perfume |
| CN105111055A (en) * | 2015-09-23 | 2015-12-02 | 昆明理工大学 | Method for preparing natural p-hydroxy benzaldehyde from bamboo shoots |
-
2016
- 2016-05-28 CN CN201610360452.XA patent/CN106008190A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2062205A (en) * | 1932-03-21 | 1936-11-24 | Boedecker Friedrich | Process of producing the m-alkylethers of protocatechuic aldehyde |
| CN102503788A (en) * | 2011-11-21 | 2012-06-20 | 湖南大学 | Application of 4-(2-methylallyl)-1,2-dihydroxybenzene in preparation of perfume |
| CN105111055A (en) * | 2015-09-23 | 2015-12-02 | 昆明理工大学 | Method for preparing natural p-hydroxy benzaldehyde from bamboo shoots |
Non-Patent Citations (3)
| Title |
|---|
| 易封萍 等主编，: "《合成香料工艺学》", 31 May 2016 * |
| 汪多仁编著: "《现代日用化工》", 31 March 2000, 冶金工业出版社 * |
| 陈朋等: "香兰素抗菌机制研究进展", 《微生物学免疫学进》 * |
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Application publication date: 20161012 |