CN105693576A - Preparation method of diallyl polythioether compounds - Google Patents
Preparation method of diallyl polythioether compounds Download PDFInfo
- Publication number
- CN105693576A CN105693576A CN201610187957.0A CN201610187957A CN105693576A CN 105693576 A CN105693576 A CN 105693576A CN 201610187957 A CN201610187957 A CN 201610187957A CN 105693576 A CN105693576 A CN 105693576A
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- CN
- China
- Prior art keywords
- diallyl
- sodium
- polysulfide
- production
- chloropropene
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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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/22—Alkali metal sulfides or polysulfides
- C01B17/34—Polysulfides of sodium or potassium
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a preparation method of diallyl polythioether compounds. The preparation method comprises the following steps: carrying out reaction on a sodium sulfide water solution and a simple substance sulfur in a closed reaction vessel to generate a sodium polysulfide solution, and adding chloropropene into the sodium polysulfide water solution, thereby preparing the diallyl polythioether compounds. The simple substance sulfur and sodium sulfide react to generate the sodium polysulfide water solution, and the sodium polysulfide water solution reacts with the chloropropene to prepare the diallyl polythioether compounds. Thus, the method has the advantages of optimized technical process and simple after-treatment, avoids waste of resources, and reduces the environmental pollution.
Description
Technical field
The present invention relates to diallyl polysulfide compounds process for production thereof, belong to technical field of fine。
Background technology
Diallyl polysulfide compound is the main component of Bulbus Allii quintessence oil, and Bulbus Allii quintessence oil has special garlic taste, it is possible to preventing and treating multiple infectious disease, is a kind of broad spectrum antibiotic。There is multiple very strong biological function, such as anti-cancer, regulate blood pressure, stomach invigorating, antiviral etc.。The biological characteristics of Bulbus Allii quintessence oil uniqueness, for having antibiotic effect without antibiotic side effect, does not find extended residual phenomenon in the tissue yet。Now it is widely used in medicine, veterinary drug, pesticide and food additive。
There are natural extract and chemosynthesis two kinds in the source of Bulbus Allii quintessence oil, and the Bulbus Allii quintessence oil of natural extract limits it widely use owing to being subject to the impact of the factors such as raw material is in short supply, yield poorly。
Chinese patent CN88105457.7 describes the synthetic method of a kind of Oleum Bulbus Allii, adopts sodium thiosulfate, sodium sulfide and chloropropene to do raw material, and it is long that this method exists the response time, and yield is low, has the shortcomings such as sewage discharge。
The synthetic method of a kind of Oleum Bulbus Allii disclosed in Chinese patent 200610057594.5, the same with Chinese patent CN88105457.7 raw material, but introduce substantial amounts of organic solvent in the reaction as reaction medium simultaneously, bring solvent recovery problem, also result in the waste of ample resources, safety in production hidden danger。
Chinese patent 200810015851.8 is with sodium hydroxide for catalyst, sodium sulfide and chloropropene are reacted in aqueous medium in reaction vessel, generate diallyl sulfide, continue to be obtained by reacting Oleum Bulbus Allii after then adding sulfur with sodium thiosulfate for catalyst again。
Summary of the invention
Present invention aim to overcome that the deficiency of existing synthetic technology, it is provided that there is process optimization, the simple advantage of post processing, it is to avoid the waste of resource, decrease environmental pollution。
Technical scheme is as follows:
1, diallyl polysulfide compound and preparation method, it is characterised in that: diallyl polysulfide compounds process for production thereof is to prepare according to below step, the first step, and sodium sulfide solution and elemental sulfur react generation sodium polysulfide solution in closed reaction vessel；Second step, adds chloropropene aqueous sodium polysulfide and prepares diallyl polysulfide compound。
2, diallyl polysulfide compounds process for production thereof according to claim 2, it is characterised in that: sodium sulfide and elemental sulfur synthesize the mol ratio of sodium polysulphide more than 1, less than 4。
3, diallyl polysulfide compounds process for production thereof according to claim 2, it is characterised in that: chloropropene and sodium polysulphide synthesize the mol ratio of diallyl polysulfide compound more than 0.8, less than 1.2。
The invention has the beneficial effects as follows:
1, the diallyl polysulfide compounds process for production thereof of the present invention simplifies technological process, it is possible in a reactor, disposable completing prepares diallyl polysulfide compound；
2, the diallyl polysulfide compounds process for production thereof byproduct of reaction of the present invention is that byproduct of reaction can recycle through concentration, separating treatment, alleviates environmental pollution containing sodium chloride and part material。
Detailed description of the invention
Following instance is only further illustrate the present invention, is not restriction the scope of protection of the invention。
Embodiment diallyl disulphide Diallytrisin preparation method of mixture
1,500 milliliters of four-hole boiling flasks are with thermometer, spherical cooling tube, constant pressure funnel, are placed on 500 milliliters of electric heating covers。
2, adding in 500 milliliters of four-hole boiling flasks by 240.2 grams of analytical pure nine water cure sodium (1.0mol), 100 grams, 48 grams analytical pure Cosans (1.5mol) of deionized water, under stirring, heating-up temperature is in 90?95 ° of C, react 60 minutes, prepare the trisulfides sodium water solution mixture of sodium disulfide。
3, trisulfides for above-mentioned sodium disulfide sodium water solution mixture is cooled to 40 ° of C standby；Adding 75 grams of analytical pure chloropropenes (0.98mol) to constant pressure funnel, chloropropene is added dropwise under stirring the trisulfides sodium water solution mixed solution of sodium disulfide, controlling drip reacting temperature is 40-45 ° of C, and time for adding controlled at 30-45 minute；After being added dropwise to complete, control reaction temperature 50-60 ° of C, react 2 hours, complete synthesis diallyl disulphide Diallytrisin mixture reaction。
4, with 500ml separatory funnel separation diallyl disulphide Diallytrisin mixture solution, top is that pale yellowish oil liquid is diallyl disulphide Diallytrisin mixture。
Diallyl disulphide Diallytrisin mixture density (25 ° of C): 1.106, index of refraction (20 ° of C): 1.590。
Claims (3)
1. diallyl polysulfide compounds process for production thereof, it is characterised in that: diallyl polysulfide compounds process for production thereof is to prepare according to below step, the first step, and sodium sulfide solution and elemental sulfur react generation aqueous sodium polysulfide in closed reaction vessel；Second step, adds chloropropene aqueous sodium polysulfide and prepares diallyl polysulfide compound。
2. diallyl polysulfide compounds process for production thereof according to claim 1, it is characterised in that: the mol ratio that sodium sulfide synthesizes sodium polysulphide with elemental sulfur is greater than 1, less than 4。
3. diallyl polysulfide compounds process for production thereof according to claim 1, it is characterised in that: the mol ratio that chloropropene synthesizes diallyl polysulfide compound with sodium polysulphide is greater than 0.8, less than 1.2。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610187957.0A CN105693576A (en) | 2016-03-30 | 2016-03-30 | Preparation method of diallyl polythioether compounds |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610187957.0A CN105693576A (en) | 2016-03-30 | 2016-03-30 | Preparation method of diallyl polythioether compounds |
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| Publication Number | Publication Date |
|---|---|
| CN105693576A true CN105693576A (en) | 2016-06-22 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610187957.0A Pending CN105693576A (en) | 2016-03-30 | 2016-03-30 | Preparation method of diallyl polythioether compounds |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107188838A (en) * | 2017-06-21 | 2017-09-22 | 宜兴市天石饲料有限公司 | A kind of processing method of garlic oil |
| CN107235877A (en) * | 2017-06-23 | 2017-10-10 | 洛阳和梦科技有限公司 | Diallyl polysulfide compound for catalysis preparation method |
Citations (4)
| 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 |
| 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 |
| CN103073569A (en) * | 2013-02-05 | 2013-05-01 | 景德镇宏柏化学科技有限公司 | Production process of organosilane polysulfide |
-
2016
- 2016-03-30 CN CN201610187957.0A patent/CN105693576A/en active Pending
Patent Citations (4)
| 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 |
| 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 |
| CN103073569A (en) * | 2013-02-05 | 2013-05-01 | 景德镇宏柏化学科技有限公司 | Production process of organosilane polysulfide |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107188838A (en) * | 2017-06-21 | 2017-09-22 | 宜兴市天石饲料有限公司 | A kind of processing method of garlic oil |
| CN107235877A (en) * | 2017-06-23 | 2017-10-10 | 洛阳和梦科技有限公司 | Diallyl polysulfide compound for catalysis preparation method |
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Application publication date: 20160622 |
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