CN106588730A - Preparation method of diallyl trisulfide - Google Patents
Preparation method of diallyl trisulfide Download PDFInfo
- Publication number
- CN106588730A CN106588730A CN201611096479.9A CN201611096479A CN106588730A CN 106588730 A CN106588730 A CN 106588730A CN 201611096479 A CN201611096479 A CN 201611096479A CN 106588730 A CN106588730 A CN 106588730A
- Authority
- CN
- China
- Prior art keywords
- parts
- preparation
- product
- sodium hydrosulfide
- sodium
- 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.)
- Granted
Links
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- UBAXRAHSPKWNCX-UHFFFAOYSA-N diallyl trisulfide Chemical compound C=CCSSSCC=C UBAXRAHSPKWNCX-UHFFFAOYSA-N 0.000 title abstract description 8
- HYHCSLBZRBJJCH-UHFFFAOYSA-M sodium hydrosulfide Chemical compound [Na+].[SH-] HYHCSLBZRBJJCH-UHFFFAOYSA-M 0.000 claims abstract description 18
- 150000003839 salts Chemical class 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000000047 product Substances 0.000 claims abstract description 11
- 239000012043 crude product Substances 0.000 claims abstract description 9
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims abstract description 8
- 235000019345 sodium thiosulphate Nutrition 0.000 claims abstract description 8
- OWXJKYNZGFSVRC-NSCUHMNNSA-N (e)-1-chloroprop-1-ene Chemical compound C\C=C\Cl OWXJKYNZGFSVRC-NSCUHMNNSA-N 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 239000012467 final product Substances 0.000 claims description 4
- 238000007493 shaping process Methods 0.000 claims description 4
- 239000000463 material Substances 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- 238000000034 method Methods 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 3
- 239000008213 purified water Substances 0.000 abstract 1
- 238000005292 vacuum distillation Methods 0.000 abstract 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- 229910052979 sodium sulfide Inorganic materials 0.000 description 3
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 3
- OSDWBNJEKMUWAV-UHFFFAOYSA-N Allyl chloride Chemical compound ClCC=C OSDWBNJEKMUWAV-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000010189 synthetic method Methods 0.000 description 2
- 230000002159 abnormal effect Effects 0.000 description 1
- 239000003674 animal food additive Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- ZLCCLBKPLLUIJC-UHFFFAOYSA-L disodium tetrasulfane-1,4-diide Chemical compound [Na+].[Na+].[S-]SS[S-] ZLCCLBKPLLUIJC-UHFFFAOYSA-L 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 230000035943 smell Effects 0.000 description 1
- SRRKNRDXURUMPP-UHFFFAOYSA-N sodium disulfide Chemical compound [Na+].[Na+].[S-][S-] SRRKNRDXURUMPP-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C381/00—Compounds containing carbon and sulfur and having functional groups not covered by groups C07C301/00 - C07C337/00
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a preparation method of diallyl trisulfide. The preparation method has simple processes, utilizes easily available raw materials, has few reaction processes and realizes high finished product content. The preparation method comprises 1) taking 50 parts of sodium hydrosulfide and 100 parts of water and preparing a sodium hydrosulfide solution with a concentration of 0.6mol, 2) taking a three-mouth flask having a volume of 1000ml, adding 280 parts of purified water, 300 parts of 1.2mol of sodium thiosulfate and 92 parts of 1.2mol of chloropropene into the three-mouth flask and preparing a Bunte salt, 3) controlling a temperature in a range of 30 to 50 DEG C, adding 150 parts of 0.6mol of the sodium hydrosulfide solution into the Bunte salt drop by drop along with stirring to decompose the Bunte salt, 4) standing the decomposed product for 2 to 6h for layering so that a crude product is obtained, and 5) putting the crude product into a rectifying still, and carrying out vacuum distillation under control of a bottom temperature of 90 to 110 DEG C and a collecting gas temperature of 62 to 64 DEG C/100Pa so that the diallyl trisulfide product is obtained.
Description
Technical field：
Present invention relates particularly to a kind of preparation method of Diallytrisin, belongs to chemical technology field.
Background technology：
Diallytrisin is a kind of yellow liquid, with disgusting abnormal smells from the patient, 112～120 DEG C of boiling point (2133Pa), or
95～97 DEG C (667Pa) or 70 DEG C (133Pa), water insoluble and ethanol are miscible in ether.Main usess be medicine intermediate,
Food additive, feed additive.The preparation method of existing Diallytrisin is by 2 using S and Na2S:1 synthesis
Na2S3, then Na2S3 and allyl chloride press 1:2 reactions；Due to synthesize sodium sulfide be based on Na2S3 and containing Na2S,
The mixture of Na2S2, Na2S4 etc., after process, crude product composition is more miscellaneous, main peak content about 40%.
The content of the invention：
In view of this, the invention provides a kind of synthetic method is simple, raw material is easy to get, and reactions steps are few, finished product content it is high two
The preparation method of diallyl trisulfide ether.
For achieving the above object, the technical solution used in the present invention is：
A kind of preparation method of Diallytrisin, is prepared from by following raw material Jing special process：280 parts of pure water,
300 parts of the sodium hyposulfite of 1.2mol, 92 parts of the chloropropene of 1.2mol, 150 parts of the sodium hydrosulfide of 0.6 mol.
A kind of preparation method of Diallytrisin, comprises the following steps：
1）Take 50 parts of NaHS standby with the sodium hydrosulfide that 100 parts of water make 0.6 mol；
2）Take 1000ml there-necked flasks, add 280 parts of pure water, 300 parts of the sodium hyposulfite of 1.2mol, 92 parts of the chloropropene of 1.2mol,
Make Bunte salt；
3）30 ~ 50 DEG C of temperature control, the lower Deca step 1 of stirring）150 parts of the sodium hydrosulfide of 0.6 prepared mol, decomposes
Bunte salt；
4）2-6 hours are stood, 86 parts of crude product, content 82.5% after layered shaping, is obtained final product;
5）Carry out rectification under vacuum with 100ml there-necked flasks, shunt head, 90 ~ 110 DEG C of bottom temperature of control, collect 62 ~ 64 DEG C of temperature/
100Pa, obtains the Diallytrisin product of 66 parts of contents 92%.
The invention has the beneficial effects as follows：Synthetic method is simple, and raw material is easy to get, and low production cost, reactions steps are few, and finished product contains
Amount is high, is adapted to large-scale production.
Specific embodiment:
To further elucidate this programme, the preferred embodiments of the invention are described with reference to specific embodiment, these descriptions
It is intended merely to further illustrate advantages of the present invention, rather than limiting to the claimed invention.
Embodiment 1
A kind of preparation method of Diallytrisin, comprises the following steps：
1）Take NaHS 50g and 100g water make 0.6 mol sodium hydrosulfide it is standby；
2）1000ml there-necked flasks are taken, pure water 280g, the sodium hyposulfite 300g of 1.2mol, the chloropropene 92g of 1.2mol, system is added
Into Bunte salt；
3）40 ~ 50 DEG C of temperature control, the lower Deca step 1 of stirring）The sodium hydrosulfide 150g of 0.6 prepared mol, decomposes Bunte
Salt；
4）5 hours are stood, crude product 86g, content 82.5% after layered shaping, is obtained final product;
5）Carry out rectification under vacuum with 100ml there-necked flasks, shunt head, 90 ~ 110 DEG C of bottom temperature of control, collect 62 ~ 64 DEG C of temperature/
100Pa, obtains the Diallytrisin product of 66g contents 92%.
Embodiment 2
A kind of preparation method of Diallytrisin, comprises the following steps：
1）Take NaHS 50kg and 100kg water make 0.6 mol sodium hydrosulfide it is standby；
2）Pure water 280kg, the sodium hyposulfite 300kg of 1.2mol, the chloropropene 92kg of 1.2mol are added in reactor, is made
Bunte salt；
3）45 ~ 50 DEG C of temperature control, the lower Deca step 1 of stirring）The sodium hydrosulfide 150kg of 0.6 prepared mol, decomposes
Bunte salt；
4）6 hours are stood, crude product 86kg, content 82.5% after layered shaping, is obtained final product;
5）By step 4）Gained crude product 86kg is put in 100L rectifying stills, carries out rectification under vacuum, 90 ~ 110 DEG C of bottom temperature of control, collection
62 ~ 64 DEG C/100Pa of temperature, obtains the Diallytrisin product of 66kg contents 92%.
Then the present invention uses quantitative NaHS using allyl chloride and sodium hyposulfite quantitative response, controlled syntheses Bunte salt
Decompose Bunte salt, what is obtained is relatively simple ideal product, therefore product yield and quality are higher.
The above is only the preferred embodiment of the present invention, above-mentioned preferred implementation is not construed as limitation of the present invention,
Protection scope of the present invention should be defined by claim limited range.For those skilled in the art come
Say, without departing from the spirit and scope of the present invention, the protection that some improvements and modifications also should be regarded as the present invention can also be made
Scope.
Claims (1)
1. a kind of preparation method of Diallytrisin, it is characterised in that：It is prepared from the following materials：280 parts of pure water,
300 parts of the sodium hyposulfite of 1.2mol, 92 parts of the chloropropene of 1.2mol, 150 parts of the sodium hydrosulfide of 0.6 mol, including following
Step：
1）Take 50 parts of NaHS standby with the sodium hydrosulfide that 100 parts of water make 0.6 mol；
2）Take 1000ml there-necked flasks, add 280 parts of pure water, 300 parts of the sodium hyposulfite of 1.2mol, 92 parts of the chloropropene of 1.2mol,
Make Bunte salt；
3）30 ~ 50 DEG C of temperature control, the lower Deca step 1 of stirring）150 parts of the sodium hydrosulfide of 0.6 prepared mol, decomposes
Bunte salt；
4）2-6 hours are stood, crude product after layered shaping, is obtained final product；
5）Step 4 gained crude product is put in rectifying still, rectification under vacuum, 90 ~ 110 DEG C of bottom temperature of control, collection temperature 62 ~ 64 is carried out
DEG C/100Pa, obtain Diallytrisin product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611096479.9A CN106588730B (en) | 2016-12-02 | 2016-12-02 | A kind of preparation method of Diallytrisin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611096479.9A CN106588730B (en) | 2016-12-02 | 2016-12-02 | A kind of preparation method of Diallytrisin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106588730A true CN106588730A (en) | 2017-04-26 |
| CN106588730B CN106588730B (en) | 2019-01-11 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611096479.9A Active CN106588730B (en) | 2016-12-02 | 2016-12-02 | A kind of preparation method of Diallytrisin |
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| Country | Link |
|---|---|
| CN (1) | CN106588730B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116102476A (en) * | 2023-01-10 | 2023-05-12 | 滕州市天水生物科技有限公司 | A kind of preparation method of dipropyl trisulfide |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020198410A1 (en) * | 2001-03-28 | 2002-12-26 | Indian Institute Of Technology | Process for the preparation of diorganotrisulfide |
| 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 |
-
2016
- 2016-12-02 CN CN201611096479.9A patent/CN106588730B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020198410A1 (en) * | 2001-03-28 | 2002-12-26 | Indian Institute Of Technology | Process for the preparation of diorganotrisulfide |
| 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 |
Non-Patent Citations (1)
| Title |
|---|
| 于雅霜等: "大蒜新素合成的探讨", 《牡丹江医学院学报》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116102476A (en) * | 2023-01-10 | 2023-05-12 | 滕州市天水生物科技有限公司 | A kind of preparation method of dipropyl trisulfide |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106588730B (en) | 2019-01-11 |
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