CN105503597A - Preparation method of environmental methyl salicylate - Google Patents
Preparation method of environmental methyl salicylate Download PDFInfo
- Publication number
- CN105503597A CN105503597A CN201511012669.3A CN201511012669A CN105503597A CN 105503597 A CN105503597 A CN 105503597A CN 201511012669 A CN201511012669 A CN 201511012669A CN 105503597 A CN105503597 A CN 105503597A
- Authority
- CN
- China
- Prior art keywords
- leaves
- preparation
- leaf
- tuberose
- solvent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C67/54—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/58—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention relates to a preparation method of environmental methyl salicylate. The preparation method comprises the steps of weighing acacia leaves, tuberose leaves and holly leaves; soaking the acacia leaves, the tuberose leaves and the holly leaves for 1 to 2 hours by using warm water with temperature of 30 to 50 DEG C, taking out and airing, grinding the aired acacia leaves, the tuberose leaves and the holly leaves into a muddy mixture; uniformly mixing ethyl alcohol and glacial acetic acid to be a solvent; adding the muddy mixture and the solvent into a Soxhlet extractor, and extracting to obtain an original extract solution of the methyl salicylate; adding the original extract solution of the methyl salicylate into a distiller, steaming out the most part of solvent, and remaining distillate; standing the distillate for 3 to 5 hours; separating out a oil layer when the oil layer occurs in the distillate; adding the oil layer into the distiller for rectification; collecting cut fraction, namely, the methyl salicylate is obtained, the yield of the methyl salicylate prepared by using the preparation method can reach 12 percent or more, and the production cost is reduced.
Description
Technical field
The present invention relates to field of fine chemical, especially a kind of preparation method of wintergreen oil of environmental protection.
Background technology
Wintergreen oil extensively exists at nature, is wintergreen, little of medicine main body of oil.Also be present in the essential oil of Tuberose, Quercetin tree, Yi Lanyilan, cloves, tea etc.; Be mainly used in pharmaceutical products and sanitary product as toothpaste, tooth powder, collutory, toilet powder shui, wind dispelling wet goods, also can be used for the perfuming of industrial goods as glue, sticking tape, board subsides, paste etc., also can be used for food flavour, if strawberry, grape, English walnut, spearmint, pungent essence are as special blue or green gas.
Existing wintergreen oil is generally assisted by Whitfield's ointment and methyl alcohol and is prepared with catalyzer, and the wintergreen oil adopting this preparation method to obtain easily produces pollution, and cost is higher.
Summary of the invention
The object of the invention is the preparation method of the wintergreen oil in order to provide a kind of environmental protection, the wintergreen oil productive rate using the method to prepare reaches more than 12%, and cost reduces.
For solving the problems of the technologies described above, technical scheme of the present invention is:
A preparation method for the wintergreen oil of environmental protection, its preparation method is as follows:
(1) by (2-3): (2-3): the ratio of weight and number of (4-5) takes Acacia leaf, Tuberose leaf and the leaves of purpurea, the warm water soaking 1-2h of Acacia leaf, Tuberose leaf and the leaves of purpurea 30-50 DEG C is taken out and dries, Acacia leaf, Tuberose leaf and the leaves of purpurea after drying are ground to form pureed mixture;
(2) by (1-3): ethanol mixes as solvent with Glacial acetic acid by the ratio of weight and number of (2-5), the pureed mixture prepare step (1) and solvent add in apparatus,Soxhlet's to extract and obtain carrying solution at the beginning of wintergreen oil, Extracting temperature is 85 DEG C, extracts 6-8h;
(3) add in distiller steamed carrying solution at the beginning of wintergreen oil by most of solvent, remainder slips out liquid, and temperature is 95 DEG C;
(4) will slip out after liquid leaves standstill 3-5h, and slip out in liquid and occur oil reservoir, isolate oil reservoir, oil reservoir is added in distiller and carry out rectifying, collect cut, be wintergreen oil.
The preparation method of the wintergreen oil of above-mentioned a kind of environmental protection, wherein, the temperature of described rectifying is 200 DEG C.
Beneficial effect of the present invention is:
The present invention adopts Acacia leaf, Tuberose leaf and the leaves of purpurea using rational proportion as starting material, and prepare wintergreen oil by each step, output can reach more than 12%, and cost reduces 20%; Ethanol and Glacial acetic acid are mixed as solvent, improves the amount of dissolving in of wintergreen oil, decrease the demand of solvent, saved cost.
Specific embodiment
Below by way of specific embodiment, the specific embodiment of the present invention is described in further detail.
Example one
A preparation method for the wintergreen oil of environmental protection, its preparation method is as follows:
(1) Acacia leaf, Tuberose leaf and the leaves of purpurea is taken by the ratio of weight and number of 2:3:4, Acacia leaf, Tuberose leaf and the leaves of purpurea are taken out with the warm water soaking 2h of 50 DEG C and dries, Acacia leaf, Tuberose leaf and the leaves of purpurea after drying are ground to form pureed mixture;
(2) mix as solvent using ethanol with Glacial acetic acid by the ratio of weight and number of 2:3, the pureed mixture prepare step (1) and solvent add in apparatus,Soxhlet's to extract and obtain carrying solution at the beginning of wintergreen oil, and Extracting temperature is 85 DEG C, extract 8h;
(3) add in distiller steamed carrying solution at the beginning of wintergreen oil by most of solvent, remainder slips out liquid, and temperature is 95 DEG C;
(4) will slip out after liquid leaves standstill 5h, and slip out in liquid and occur oil reservoir, isolate oil reservoir, oil reservoir is added in distiller and carry out rectifying, collect cut, be wintergreen oil.
Example two
A preparation method for the wintergreen oil of environmental protection, its preparation method is as follows:
(1) Acacia leaf, Tuberose leaf and the leaves of purpurea is taken by the ratio of weight and number of 3:2:5, Acacia leaf, Tuberose leaf and the leaves of purpurea are taken out with the warm water soaking 2h of 40 DEG C and dries, Acacia leaf, Tuberose leaf and the leaves of purpurea after drying are ground to form pureed mixture;
(2) mix as solvent using ethanol with Glacial acetic acid by the ratio of weight and number of 1:4, the pureed mixture prepare step (1) and solvent add in apparatus,Soxhlet's to extract and obtain carrying solution at the beginning of wintergreen oil, and Extracting temperature is 85 DEG C, extract 8h;
(3) add in distiller steamed carrying solution at the beginning of wintergreen oil by most of solvent, remainder slips out liquid, and temperature is 95 DEG C;
(4) will slip out after liquid leaves standstill 5h, and slip out in liquid and occur oil reservoir, isolate oil reservoir, oil reservoir is added in distiller and carry out rectifying, collect cut, be wintergreen oil.
Example three
A preparation method for the wintergreen oil of environmental protection, its preparation method is as follows:
(1) Acacia leaf, Tuberose leaf and the leaves of purpurea is taken by the ratio of weight and number of 3:2.5:4, Acacia leaf, Tuberose leaf and the leaves of purpurea are taken out with the warm water soaking 2h of 30 DEG C and dries, Acacia leaf, Tuberose leaf and the leaves of purpurea after drying are ground to form pureed mixture;
(2) by the ratio of weight and number of 1.5:3.2, ethanol is mixed as solvent with Glacial acetic acid, the pureed mixture prepare step (1) and solvent add in apparatus,Soxhlet's to extract and obtain carrying solution at the beginning of wintergreen oil, Extracting temperature is 85 DEG C, extracts 8h;
(3) add in distiller steamed carrying solution at the beginning of wintergreen oil by most of solvent, remainder slips out liquid, and temperature is 95 DEG C;
(4) will slip out after liquid leaves standstill 5h, and slip out in liquid and occur oil reservoir, isolate oil reservoir, oil reservoir is added in distiller and carry out rectifying, collect cut, be wintergreen oil.
Here description of the invention and application is illustrative, not wants by scope restriction of the present invention in the above-described embodiments, and therefore, the present invention is not by the restriction of the present embodiment, and the technical scheme that any employing equivalence replacement obtains is all in the scope of protection of the invention.
Claims (2)
1. a preparation method for the wintergreen oil of environmental protection, is characterized by, and its preparation method is as follows:
By (2-3): (2-3): the ratio of weight and number of (4-5) takes Acacia leaf, Tuberose leaf and the leaves of purpurea, the warm water soaking 1-2h of Acacia leaf, Tuberose leaf and the leaves of purpurea 30-50 DEG C is taken out and dries, Acacia leaf, Tuberose leaf and the leaves of purpurea after drying are ground to form pureed mixture;
By (1-3): ethanol mixes as solvent with Glacial acetic acid by the ratio of weight and number of (2-5), the pureed mixture prepare step (1) and solvent add in apparatus,Soxhlet's to extract and obtain carrying solution at the beginning of wintergreen oil, Extracting temperature is 85 DEG C, extracts 6-8h;
Add in distiller steamed carrying solution at the beginning of wintergreen oil by most of solvent, remainder slips out liquid, and temperature is 95 DEG C;
To slip out after liquid leaves standstill 3-5h, and slip out in liquid and occur oil reservoir, isolate oil reservoir, oil reservoir is added in distiller and carry out rectifying, collect cut, be wintergreen oil.
2. the preparation method of the wintergreen oil of a kind of environmental protection as claimed in claim 1, is characterized by, and the temperature of described rectifying is 200 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201511012669.3A CN105503597A (en) | 2015-12-31 | 2015-12-31 | Preparation method of environmental methyl salicylate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201511012669.3A CN105503597A (en) | 2015-12-31 | 2015-12-31 | Preparation method of environmental methyl salicylate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105503597A true CN105503597A (en) | 2016-04-20 |
Family
ID=55711972
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201511012669.3A Pending CN105503597A (en) | 2015-12-31 | 2015-12-31 | Preparation method of environmental methyl salicylate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105503597A (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB476898A (en) * | 1936-06-24 | 1937-12-17 | Howards And Sons Ltd | Manufacture of esters of salicylic acid |
| CN101225045A (en) * | 2008-01-31 | 2008-07-23 | 浙江科技学院 | Micro-wave synthetic method for preparing methyl salicylate |
-
2015
- 2015-12-31 CN CN201511012669.3A patent/CN105503597A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB476898A (en) * | 1936-06-24 | 1937-12-17 | Howards And Sons Ltd | Manufacture of esters of salicylic acid |
| CN101225045A (en) * | 2008-01-31 | 2008-07-23 | 浙江科技学院 | Micro-wave synthetic method for preparing methyl salicylate |
Non-Patent Citations (2)
| Title |
|---|
| 李仁全: "从冬青树叶中提取水杨酸甲酯的探讨", 《四川职业技术学院学报》 * |
| 郭鹏 等: "从冬青叶中提取冬青油的工艺探讨", 《信阳师范学院学报》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102659743A (en) | Extraction rectification method of anthocyanin in mulberry | |
| CN104306443B (en) | A kind of method of oil camphor tree leaf comprehensive utilization | |
| CN104371026A (en) | Cellulose acetate butyrate mixed ester with high butyryl content, and preparation method thereof | |
| CN103087828B (en) | A kind of Yunnan black tea essential oil and preparation method thereof | |
| CN104726250B (en) | The brewage process of chestnut flower boy's wine | |
| CN110747234A (en) | Preparation method of sophora flower extractum | |
| CN106332998A (en) | Making method for Fuzhuan tea with dried tangerine or orange peel aroma | |
| WO2010026021A3 (en) | Combination of extracts of various plants for improving the symptoms of dementia disorders | |
| CN102772521B (en) | Method for extracting coffee polyphenols from coffee bean | |
| CN102863477A (en) | Method for extracting plant polyphenol from walnut shells by using ionic liquid | |
| CN102942637B (en) | Method for increasing extraction rate of wide cactus polysaccharide | |
| CN110151810A (en) | A method of safflower extract is prepared using eutectic solvent | |
| CN103146473A (en) | Method for simultaneously extracting Australian tea tree essential oil and flavonoid glycosides | |
| CN105503597A (en) | Preparation method of environmental methyl salicylate | |
| CN102260587A (en) | Method for extracting grape seed oil and proantho cyanidins | |
| CN105153096A (en) | Method for extracting procyanidins (OPC) from grape seeds | |
| CN101444474A (en) | Rhodiola root extract with senile-resistant efficacy and preparation method thereof | |
| CN107163679B (en) | Preparation method of gravure ink without benzene | |
| CN104099204A (en) | Brewing method of resveratrol wild grape wine | |
| CN104497287A (en) | Alkyd resin and preparation method thereof | |
| CN101473880A (en) | Method for extracting and separating thearubigins from black tea | |
| CN103845396A (en) | Hickory sterol extractive and preparation method and application thereof | |
| CN104824245A (en) | Preparation process of Liupao tea extract capable of preventing and improving fatty liver | |
| CN102813686B (en) | Method for extracting active ingredients from hibiscus sabdariffa calyx | |
| CN105037313A (en) | Method for simply separating myricetrin and catechin in bark of waxberry tree |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20160420 |
|
| RJ01 | Rejection of invention patent application after publication |