CN106083517A - The preparation method of high-purity longifolene - Google Patents
The preparation method of high-purity longifolene Download PDFInfo
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- CN106083517A CN106083517A CN201610479845.2A CN201610479845A CN106083517A CN 106083517 A CN106083517 A CN 106083517A CN 201610479845 A CN201610479845 A CN 201610479845A CN 106083517 A CN106083517 A CN 106083517A
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- longifolene
- molecular sieve
- zeolite molecular
- purity
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/148—Purification; Separation; Use of additives by treatment giving rise to a chemical modification of at least one compound
- C07C7/17—Purification; Separation; Use of additives by treatment giving rise to a chemical modification of at least one compound with acids or sulfur oxides
- C07C7/171—Sulfuric acid or oleum
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/04—Purification; Separation; Use of additives by distillation
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- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Water Supply & Treatment (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention discloses the preparation method of a kind of high-purity longifolene, method particularly includes: longifolene crude product is added in reactor, add zeolite molecular sieve, be warming up to 100 DEG C～120 DEG C, insulation reaction 30 minutes～1 hour, filter, remove zeolite molecular sieve, then add concentrated sulphuric acid, be warming up to 120 DEG C～130 DEG C, insulation reaction 30 minutes～40 minutes, adds aqueous slkali regulation pH value of solution to neutral；Decompression distillation, discharging, obtain high-purity longifolene；Gained longifolene high purity more than 85% of the present invention.
Description
Technical field
The present invention relates to Oleum Terebinthinae deep process technology field, the preparation method of a kind of high-purity longifolene.
Background technology
Longifolene is a kind of natural perfume material extracted from heavy duty Oleum Terebinthinae, has special chemism, is synthesis
The raw material of resin, synthetic perfume, flotation agent and organic synthesis, utilizes longifolene can manufacture isolonglifolene, Isolongifolenone
Deng product, the allotment for essence can replace some expensive spice.
When heavy turpentine purifies longifolene, often due to longifolene is close with caryophyllene boiling point in heavy turpentine, system
The longifolene product obtained usually contains the caryophyllene of 10%～12% so that the purity of longifolene is less than 70%, significantly
Reduce the use value of longifolene.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of high-purity longifolene, the soluble problem of this method.
In order to solve the problems referred to above, the technical solution used in the present invention is:
The preparation method of this high-purity longifolene is: added by longifolene crude product in reactor, adds zeolite molecular sieve, mixing
Uniformly, it is warming up to 100 DEG C～120 DEG C, insulation reaction 30 minutes～1 hour, filters, removes zeolite molecular sieve, then add
Concentrated sulphuric acid, is warming up to 120 DEG C～130 DEG C, insulation reaction 30 minutes～40 minutes, adds aqueous slkali regulation pH value of solution to neutral；
Decompression distillation, discharging, obtain high-purity longifolene；Wherein, the addition of zeolite molecular sieve is longifolene crude product gross weight
0.1%～0.2%；The addition of concentrated sulphuric acid is the 0.03%～0.1% of longifolene crude product gross weight.
In technique scheme, more specifically technical scheme is it may also is that zeolite molecular sieve is sodium type zeolite molecular sieves.
Further, the preparation method of zeolite molecular sieve is: is added in sodium salt solution by kieselguhr 5A molecular sieve, is warming up to
50 DEG C～70 DEG C, insulation reaction 2 hours, make a diameter of 2 millimeters of spheroidal particle, at 170 DEG C～180 DEG C, dry 2 hours,
Calcine 1 hour～2 hours at 450 DEG C～500 DEG C again.
Owing to have employed technique scheme, the present invention compared with prior art has the advantages that
The present invention is sequentially added into sodium type zeolite molecular sieves, concentrated sulphuric acid, makes the most of caryophyllene isomerization in longifolene crude product, institute
Obtain longifolene high purity more than 85%.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described:
Embodiment 1
The preparation method of the present embodiment high-purity longifolene is: is added in sodium salt solution by kieselguhr 5A molecular sieve, is warming up to 50
DEG C～55 DEG C, insulation reaction 2 hours, make a diameter of 2 millimeters of spheroidal particle, at 172 DEG C～175 DEG C, dry 2 hours, then
Calcine 2 hours at 450 DEG C～460 DEG C, obtain sodium type zeolite molecular sieves；Then longifolene crude product is added in reactor, add
Enter sodium type zeolite molecular sieves, mix homogeneously, be warming up to 100 DEG C～120 DEG C, insulation reaction 50 minutes, filters, removes na-pretreated zeolite
Molecular sieve, then adds concentrated sulphuric acid, is warming up to 120 DEG C～130 DEG C, insulation reaction 30 minutes, adds aqueous slkali regulation solution
PH is to neutral；Decompression distillation, discharging, obtain high-purity longifolene；
The present embodiment sodium type zeolite molecular sieves addition is the 0.2% of longifolene crude product gross weight；The addition of concentrated sulphuric acid is for long
The 0.03% of leaf alkene crude product gross weight.
The purity of the present embodiment longifolene is 86.2%.
Embodiment 2
The preparation method of the present embodiment high-purity longifolene is: is added in sodium salt solution by kieselguhr 5A molecular sieve, is warming up to 60
DEG C～63 DEG C, insulation reaction 2 hours, make a diameter of 2 millimeters of spheroidal particle, at 176 DEG C～180 DEG C, dry 2 hours, then
Calcine 1 hour at 495 DEG C～500 DEG C, obtain sodium type zeolite molecular sieves；Then longifolene crude product is added in reactor, add
Enter sodium type zeolite molecular sieves, mix homogeneously, be warming up to 100 DEG C～120 DEG C, insulation reaction 1 hour, filters, removes na-pretreated zeolite
Molecular sieve, then adds concentrated sulphuric acid, is warming up to 120 DEG C～130 DEG C, insulation reaction 35 minutes, adds aqueous slkali regulation solution
PH is to neutral；Decompression distillation, discharging, obtain high-purity longifolene；
The present embodiment sodium type zeolite molecular sieves addition is the 0.15% of longifolene crude product gross weight；The addition of concentrated sulphuric acid is for long
The 0.1% of leaf alkene crude product gross weight.
The purity of the present embodiment longifolene is 87.3%.
Embodiment 3
The preparation method of the present embodiment high-purity longifolene is: is added in sodium salt solution by kieselguhr 5A molecular sieve, is warming up to 68
DEG C～70 DEG C, insulation reaction 2 hours, make a diameter of 2 millimeters of spheroidal particle, at 170 DEG C～175 DEG C, dry 2 hours, then
Calcine 1.5 hours at 470 DEG C～478 DEG C, obtain sodium type zeolite molecular sieves；Then longifolene crude product is added in reactor,
Add sodium type zeolite molecular sieves, mix homogeneously, be warming up to 100 DEG C～120 DEG C, insulation reaction 30 minutes, filters, removes sodium form boiling
Stone molecular sieve, then adds concentrated sulphuric acid, is warming up to 120 DEG C～130 DEG C, insulation reaction 40 minutes, adds aqueous slkali regulation molten
Liquid pH is to neutral；Decompression distillation, discharging, obtain high-purity longifolene；
The present embodiment sodium type zeolite molecular sieves addition is the 0.1% of longifolene crude product gross weight；The addition of concentrated sulphuric acid is for long
The 0.05% of leaf alkene crude product gross weight.
The purity of the present embodiment longifolene is 85.4%.
Claims (3)
1. the preparation method of a high-purity longifolene, it is characterised in that comprise the following steps: longifolene crude product is added reaction
In still, add zeolite molecular sieve, mix homogeneously, be warming up to 100 DEG C～120 DEG C, insulation reaction 30 minutes～1 hour, filters, removes
Remove zeolite molecular sieve, then add concentrated sulphuric acid, be warming up to 120 DEG C～130 DEG C, insulation reaction 30 minutes～40 minutes, add
Aqueous slkali regulation pH value of solution is to neutral；Decompression distillation, discharging, obtain high-purity longifolene；
Wherein, the addition of zeolite molecular sieve is the 0.1%～0.2% of longifolene crude product gross weight；The addition of concentrated sulphuric acid is
The 0.03%～0.1% of longifolene crude product gross weight.
The preparation method of high-purity longifolene the most according to claim 1, it is characterised in that: described zeolite molecular sieve is sodium
Type zeolite molecular sieve.
The preparation method of high-purity longifolene the most according to claim 1 and 2, it is characterised in that described zeolite molecular sieve
Preparation method is: is added in sodium salt solution by kieselguhr 5A molecular sieve, is warming up to 50 DEG C～70 DEG C, and insulation reaction 2 hours is made
A diameter of 2 millimeters of spheroidal particle, at 170 DEG C～180 DEG C, dry 2 hours, then calcine 1 hour～2 at 450 DEG C～500 DEG C
Hour.
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| CN201610479845.2A CN106083517A (en) | 2016-06-28 | 2016-06-28 | The preparation method of high-purity longifolene |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1095704A (en) * | 1993-05-26 | 1994-11-30 | 中国林业科学研究院林产化学工业研究所 | Process for preparing beta-caryophyllenol |
| CN101568503A (en) * | 2006-12-21 | 2009-10-28 | 纳幕尔杜邦公司 | Hydrogenation of caryophyllene |
| CN103449954A (en) * | 2013-08-27 | 2013-12-18 | 梧州市松桦化学品有限公司 | Preparation method of high-purity longifolene |
| CN104193579A (en) * | 2014-07-25 | 2014-12-10 | 广西梧州松脂股份有限公司 | Purification method for longifolene |
| CN104909976A (en) * | 2015-05-27 | 2015-09-16 | 梧州市嘉盈树胶有限公司 | Longifolene purification method |
| CN104961616A (en) * | 2015-05-27 | 2015-10-07 | 梧州市嘉盈树胶有限公司 | Longifolene purifying method |
-
2016
- 2016-06-28 CN CN201610479845.2A patent/CN106083517A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1095704A (en) * | 1993-05-26 | 1994-11-30 | 中国林业科学研究院林产化学工业研究所 | Process for preparing beta-caryophyllenol |
| CN101568503A (en) * | 2006-12-21 | 2009-10-28 | 纳幕尔杜邦公司 | Hydrogenation of caryophyllene |
| CN103449954A (en) * | 2013-08-27 | 2013-12-18 | 梧州市松桦化学品有限公司 | Preparation method of high-purity longifolene |
| CN104193579A (en) * | 2014-07-25 | 2014-12-10 | 广西梧州松脂股份有限公司 | Purification method for longifolene |
| CN104909976A (en) * | 2015-05-27 | 2015-09-16 | 梧州市嘉盈树胶有限公司 | Longifolene purification method |
| CN104961616A (en) * | 2015-05-27 | 2015-10-07 | 梧州市嘉盈树胶有限公司 | Longifolene purifying method |
Non-Patent Citations (2)
| Title |
|---|
| 刘红: "提取高纯度长叶烯新技术工业化问题的剖析", 《化学工程与装备》 * |
| 历阳等: "沸石分子筛的绿色合成路线", 《化学进展》 * |
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