CN107188838A - A kind of processing method of garlic oil - Google Patents
A kind of processing method of garlic oil Download PDFInfo
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- CN107188838A CN107188838A CN201710476061.9A CN201710476061A CN107188838A CN 107188838 A CN107188838 A CN 107188838A CN 201710476061 A CN201710476061 A CN 201710476061A CN 107188838 A CN107188838 A CN 107188838A
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- processing method
- garlic oil
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- garlic
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C319/00—Preparation of thiols, sulfides, hydropolysulfides or polysulfides
- C07C319/22—Preparation of thiols, sulfides, hydropolysulfides or polysulfides of hydropolysulfides or polysulfides
- C07C319/24—Preparation of thiols, sulfides, hydropolysulfides or polysulfides of hydropolysulfides or polysulfides by reactions involving the formation of sulfur-to-sulfur bonds
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C319/00—Preparation of thiols, sulfides, hydropolysulfides or polysulfides
- C07C319/26—Separation; Purification; Stabilisation; Use of additives
- C07C319/28—Separation; Purification
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention discloses a kind of processing method of garlic oil, chloropropene is used for raw material, and the garlic oil using diallyl trithioether as main component is made through vulcanization, condensation, physical layering separation；Processing method provided by the present invention is without using organic solvents such as toluene, ether, and processing technology is simple, and easy to operate, Diallytrisin content >=50%, is suitable for large-scale promotion application in the product of acquisition.
Description
Technical field
The present invention relates to feed additive field, particularly a kind of processing method of garlic oil.
Background technology
Garlic oil is a kind of natural antimicrobial substance extracted by certain processing technology from garlic, is described as in soil
Longer broad-spectrum antibiotic, has suppression or killing action to many parasites, bacterium, virus.Because it has stronger resist
Cancer, antiviral, antibacterial activity, can strengthen matrix immunity, wide in livestock breeding industry as a kind of feed addictive
General application.In Feed Manufacturing, garlic oil has natural fragrance, and high temperature resistant, easily granulation do not develop immunity to drugs, in vivo without residual
Stay, it is nontoxic.In addition, with clear pest, removing toxic substances, function promoting blood circulation and removing blood stasis, can significantly reduce noxious material in feed, energy insect prevention is removed
Evil, protects feed quality, with high application value.
Main component material in garlic extract includes diallyl sulfide（DS）, diallyl disulphide（DDS）、
Diallytrisin（DTS）With the thioether of diallyl four（DTTS）Deng wherein based on trithioether.But such product is from garlic
The yield of middle extraction is extremely low, and temperature requirement is high less than 0.2%, and when extracting for existing garlic oil recovery rate, and the time is long, and activity is variable,
Needed for can not meet research and daily use, it has also become the technical barrier urgently to be resolved hurrily at present of this area.
The content of the invention
The garlic oil obtained for current biological extraction method yields poorly, and the present invention provides a kind of processing method of garlic oil,
The recovery rate of garlic oil is improved, what the present invention was realized in：
A kind of processing method of garlic oil, it is comprised the following steps that：
（1）The synthesis of polysulfide
Vulcanization reaction：First reactor is rinsed well with running water, a certain amount of running water is added into reactor, stirring is started,
Akali sulphide is added into reactor, while adding steam into chuck, material in kettle is warming up to 60-68 DEG C, is delayed into reactor
Slowly a certain amount of sulphur is added, device is covered tightly after adding, 85 ~ 90 DEG C, the transparent dark-brown of solution, 85 ~ 90 are continuously heating to
DEG C isothermal reaction 1 hour, is then cooled to 30-35 DEG C gradually；
Wherein, the mass ratio for adding akali sulphide and sulphur is 45-51:25；
Condensation reaction：Keep 30-35 DEG C of temperature constant, be slowly added to chloropropene to reactor, chlorination propylene can not be too fast, adds
Keeping temperature continues stirring reaction half an hour afterwards, then adds steam that material is heated up into 40-45 DEG C of constant temperature stirring reaction 2 to chuck
Hour, open cooling water and material is cooled to less than 35 DEG C, stop static 1 hour of stirring；
Wherein, the mass ratio for adding chloropropene and akali sulphide is 50-68:45-51；
（2）Separating-purifying
Material layering is waited after standing 1 hour, dereaction liquid bottom mother liquor is put.There is black material to release application bucket reception when seeing
Remove water；Edible vegetable oil or it is oily received with other mixture releasings with bucket, washing removes impurity and takes edible vegetable oil barrelling to deposit, as garlic
Oil.
Further, in the processing method of garlic oil that the present invention is provided, the akali sulphide of selection is vulcanized sodium, its content >=
60%；Sodium sulfite content≤2.0, sodium thiosulfate≤2.0.
Compared with prior art, garlic oil processing method of the invention possesses following advantage：
1st, simplify synthesis technique operation, do not use the organic solvents such as toluene or ether in technical solution of the present invention reaction, reduce into
This, shortens activity time, increases economic benefit.
2nd, the akali sulphide that the present invention is selected, principal component content >=60%；Sodium sulfite content≤2.0, sodium thiosulfate≤
2.0。
3rd, the garlic oily product obtained, wherein total active constituent content ＞ 97%, Diallytrisin content >=50%.
Brief description of the drawings
Fig. 1 is the process chart of garlic oil processing method of the present invention.
Embodiment
It is an object of the invention to provide a kind of processing technology of garlic oil.Further illustrated below by the mode of embodiment
The present invention, but therefore do not limit the present invention within described scope of embodiments.
Embodiment 1
（1）The synthesis of polysulfide
Vulcanization reaction：First reactor is rinsed well with running water, 2000kg running water is added into reactor, stirring is started,
By 450kg vulcanized sodium（Wherein sodium sulfide content >=60%；Sodium sulfite content≤2.0, sodium thiosulfate≤2.0））Add reaction
Kettle, while adding steam into chuck, is warming up to 60 DEG C of temperature by material in kettle, 250kg sulphur is slowly added into reactor,
Device is covered tightly after adding, 85 DEG C are continuously heating to, then the transparent dark-brown of solution, isothermal reaction 1 hour is cooled to gradually
30 DEG C of temperature.
Condensation reaction：Constant 30 DEG C of keeping temperature, 500kg chloropropenes are slowly added to reactor, and chlorination propylene can not mistake
It hurry up, keep 30 DEG C of temperature to continue stirring reaction half an hour after adding, then add steam that material is heated up into 40 DEG C and permanent to chuck
Warm stirring reaction 2 hours, then opens cooling water and material is cooled into less than 35 DEG C, stopping is stirred and mixed static 1 hour.
（2）Separating-purifying
1 hour is stood, material layering is waited, puts dereaction liquid bottom mother liquor, have black material when seeing（Contain the miscellaneous of garlic oil
Matter）Release application bucket and receive removing water；Edible vegetable oil or it is oily received with other mixture releasings with bucket, washing remove impurity（Add water and stir
Mix after static layering）Take edible vegetable oil（Weak yellow liquid）Barrelling is deposited.Garlic oil yield 97.2%
In obtained garlic oil product, 51% is accounted for chromatography detection Diallytrisin content.
The preparation flow technique of the present embodiment is as shown in Figure 1.
Embodiment 2
（1）The synthesis of polysulfide
Vulcanization reaction：First reactor is rinsed well with running water, 2200kg running water is added into reactor, stirring is started,
By 490kg vulcanized sodium（Wherein sodium sulfide content >=60%；Sodium sulfite content≤2.0, sodium thiosulfate≤2.0）Add reaction
Kettle, while adding steam into chuck, is warming up to 65 DEG C of temperature by material in kettle, 250kg sulphur is slowly added into reactor,
Device is covered tightly after adding, 88 DEG C are continuously heating to, then the transparent dark-brown of solution, isothermal reaction 1 hour is cooled to gradually
35 DEG C of temperature.
Condensation reaction：35 DEG C of keeping temperature is constant, and 650kg chloropropenes are slowly added to reactor, and chlorination propylene can not mistake
It hurry up, add rear keeping temperature and continue to react half an hour, then add steam that material is heated up into 45 DEG C of isothermal reactions 2 to chuck small
When, open cooling water and material is cooled to less than 35 DEG C, stop static 1 hour of stirring.
（2）Separating-purifying
1 hour is stood, material layering is waited, puts dereaction liquid bottom mother liquor.There is black material to release application bucket reception when seeing
Remove water；Edible vegetable oil or it is oily received with other mixture releasings with bucket, washing remove impurity take edible vegetable oil barrelling deposit.
In obtained garlic oil product, Diallytrisin content accounts for 52.1%.
Embodiment 3
（1）The synthesis of polysulfide
Vulcanization reaction：First reactor is rinsed well with running water, 2400kg running water is added into reactor, stirring is started,
By 510kg vulcanized sodium（Wherein sodium sulfide content >=60%；Sodium sulfite content≤2.0, sodium thiosulfate≤2.0）Add reaction
Kettle, while adding steam into chuck, is warming up to 68 DEG C of temperature by material in kettle, 250kg sulphur is slowly added into reactor,
Device is covered tightly after adding, 90 DEG C are continuously heating to, then the transparent dark-brown of solution, isothermal reaction 1 hour is cooled to gradually
30 DEG C of temperature.
Condensation reaction：30 DEG C of keeping temperature is constant, and 680kg chloropropenes are slowly added to reactor, and chlorination propylene can not mistake
It hurry up, add rear 30 DEG C of keeping temperature and continue to react half an hour, then add steam that material is heated up into 42 DEG C of isothermal reactions 2 to chuck
Hour, open cooling water and material is cooled to less than 35 DEG C, stop static 1 hour of stirring.
（2）Separating-purifying
1 hour is stood, material layering is waited, puts dereaction liquid bottom mother liquor.There is black material to release application bucket reception when seeing
Remove water；Edible vegetable oil or it is oily received with other mixture releasings with bucket, washing remove impurity take edible vegetable oil barrelling deposit.
In obtained garlic oil product, Diallytrisin content accounts for 51.6%.
The explanation of above example is only intended to the method and its core concept for helping to understand the present invention.It is described above to be only
The preferred embodiment of the present invention, it is noted that due to the finiteness of literal expression, and objectively there is unlimited specific knot
Structure, for those skilled in the art, under the premise without departing from the principles of the invention, can also make some
Improve, retouch or change, above-mentioned technical characteristic can also be by rights combined；These improve retouching, change or
Combination, or the not improved guarantor that the design of invention and technical scheme are directly applied into other occasions, the present invention is regarded as
Protect scope.
Claims (4)
1. a kind of processing method of garlic oil, it is characterised in that comprise the following steps that：
The synthesis of polysulfide
Water and akali sulphide are added into reactor, 60-68 DEG C is warming up to, sulphur is added, 85-90 DEG C, then constant temperature stirring is warming up to
Reaction 1 hour, is then naturally cooling to 30-35 DEG C and keeps the temperature constant, and chloropropene is added into reactor, continues to stir
Half an hour is reacted, 40-45 DEG C is then heated to, stirring reaction 2 hours, it is subsequently cooled to less than 35 DEG C, it is quiet to 1 hour；
Separating-purifying
Material layering is waited after standing 1 hour, upper strata edible vegetable oil is garlic oil.
2. the processing method of garlic oil according to claim 1, it is characterised in that step（1）Middle added chloropropene and vulcanization
The mass ratio of alkali is 50-68:45-51.
3. the processing method of garlic oil according to claim 2, it is characterised in that step（1）Middle added akali sulphide and sulphur
Mass ratio be 45-51:25.
4. according to the processing method of one of the claim 1-3 garlic oils, it is characterised in that the akali sulphide is vulcanized sodium.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710476061.9A CN107188838A (en) | 2017-06-21 | 2017-06-21 | A kind of processing method of garlic oil |
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| CN201710476061.9A CN107188838A (en) | 2017-06-21 | 2017-06-21 | A kind of processing method of garlic oil |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101037406A (en) * | 2006-03-16 | 2007-09-19 | 北京资源亚太动物药品有限公司 | Synthesizing method of garlic oil |
| CN101265223A (en) * | 2008-05-05 | 2008-09-17 | 唐永锋 | Green non-pollution synthesis technology for garlic oil |
| CN101337917A (en) * | 2008-08-08 | 2009-01-07 | 淮阴工学院 | Method for catalytic synthesis of garlic oil of different combinations by phase-transfer method |
| CN101691346A (en) * | 2009-09-08 | 2010-04-07 | 北京资源亚太饲料科技有限公司 | Separation and purification method of synthetic garlic oil |
| CN105693576A (en) * | 2016-03-30 | 2016-06-22 | 洛阳和梦科技有限公司 | Preparation method of diallyl polythioether compounds |
-
2017
- 2017-06-21 CN CN201710476061.9A patent/CN107188838A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101037406A (en) * | 2006-03-16 | 2007-09-19 | 北京资源亚太动物药品有限公司 | Synthesizing method of garlic oil |
| CN101265223A (en) * | 2008-05-05 | 2008-09-17 | 唐永锋 | Green non-pollution synthesis technology for garlic oil |
| CN101337917A (en) * | 2008-08-08 | 2009-01-07 | 淮阴工学院 | Method for catalytic synthesis of garlic oil of different combinations by phase-transfer method |
| CN101691346A (en) * | 2009-09-08 | 2010-04-07 | 北京资源亚太饲料科技有限公司 | Separation and purification method of synthetic garlic oil |
| CN105693576A (en) * | 2016-03-30 | 2016-06-22 | 洛阳和梦科技有限公司 | Preparation method of diallyl polythioether compounds |
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Application publication date: 20170922 |