CN1049491A - A kind of novel process of refining haloalkane simply - Google Patents
A kind of novel process of refining haloalkane simply Download PDFInfo
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- CN1049491A CN1049491A CN 90107912 CN90107912A CN1049491A CN 1049491 A CN1049491 A CN 1049491A CN 90107912 CN90107912 CN 90107912 CN 90107912 A CN90107912 A CN 90107912A CN 1049491 A CN1049491 A CN 1049491A
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- haloalkane
- alcohol
- phosphotidic
- reagent
- refining
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
- C07C17/395—Separation; Purification; Stabilisation; Use of additives by treatment giving rise to a chemical modification of at least one compound
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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
A kind of novel process of refining haloalkane simply, its process is with containing the haloalkane of alcohol, with the system of phosphotidic reagent mixed liquor, place under the certain temperature, behind the stirring reaction certain hour, add lower alcohol or do not add lower alcohol, directly underpressure distillation can get the higher haloalkane of purity.
Description
The present invention relates to a kind of novel process of refining haloalkane simply, and implement this novel process detailed process.
Haloalkane of the present invention can be represented by following general formula:
R-（X）n
R can be a straight chain, and side chain or cyclic alkyl also can be saturated or undersaturated, and its carbonatoms is in the 2-20 scope.X is a halogen atom, can be fluorine, chlorine, bromine and iodine, and halogen atom is counted n in the 1-10 scope, is preferably in the 1-3 scope.With the several halogen atoms in a part can be identical or inequality.
The example of haloalkane of the present invention is as follows, but be not limited to this: 1,2-ethylene dichloride, monobromethane, chlorobutane and isomer thereof, n-butyl bromide, bromooctane, chloro or bromocyclohexane, bromododecane, chlorinated dodecane, bromo or chloro or iodohexadecane and octadecane, and isomer.The present invention is to the refining particularly practical of bromododecane, and this product has a wide range of applications in chemical industries such as pharmacy, and its purity has very big influence to the quality of many Chemicals.
Generally speaking, many haloalkanes are that alcohol by its corresponding carbonatoms gets through halogenating reaction.Especially unreacted higher alcohols in the haloalkane product adopts the method for distillation or rectifying under many circumstances, is difficult for separating fully with corresponding haloalkane, and is that have even basic branch is too busy to get away.Its energy consumption of rectifying tower of employing high tray-number and installation cost and process cost are all higher, can increase product cost undoubtedly.In addition, another kind of common method of separating alcohol in the haloalkane is that halohydrocarbon and a certain amount of vitriol oil that will contain alcohol mixes, at a certain temperature, sulfuric acid and alcohol wherein form Monosulfate, through a large amount of water washing of repeated multiple times, after sulfuric ester removed, do not contained the product of alcohol again through distillation.The shortcoming of this method is, easily produces emulsion during washing, is difficult for layering, and time of repose is long, and complex operation also will consume a large amount of soda acids simultaneously, and itself produces a large amount of acid-base waste fluids inevitably its technology, brings serious pollution to environment.
In order to overcome the defective of above-mentioned existing technology, the objective of the invention is to: by easy operation, determine a kind of processing method of separating the alcohol in the haloalkane, the haloalkane of higher degree is provided, thereby reduce production costs, reduce environmental pollution, to satisfy the heavy demand of chemical industry such as pharmacy to haloalkane.
The inventor finds: form phosphoric acid or phosphorous acid ester with the alcohol in phosphotidic reagent and the haloalkane, need not washing, directly through underpressure distillation, alcohol can be removed, avoided fatty alcohol sulfate to thermally labile, decompose because of being heated, produce multiple pair of product.Fatty alcohol phosphate among the present invention is more stable to heat, and its boiling point is higher than corresponding haloalkane far away, only utilizes simple underpressure distillation, can separate fully with haloalkane.Haloalkane for its suitability for industrialized production higher degree has improved favourable condition.The selected phosphotidic reagent source of the present invention is easy, does not have particular requirement.As Vanadium Pentoxide in FLAKES, phosphorus pentachloride, phosphorus oxychloride, phosphorus trichloride, phosphorus tribromide etc.These phosphotidic reagent also can be got by on-site preparation, add bromine and red phosphorus and generate phosphorus tribromide in the haloalkane crude product.The consumption of the phosphotidic reagent of technology of the present invention can decide by the content of alcohol in the haloalkane, generally can be greater than the equivalent of alcohol in the haloalkane, can excessive 0.1-1 doubly, best excessive 0.2-0.5 times.If haloalkane is refining less demanding, also can be lower than the equivalents of alcohol, the temperature of reaction of its phosphotidic is decided according to the active degree of phosphotidic reagent and alcohol, generally between 10-300 ℃, is preferably in normal temperature between the boiling point of required purified haloalkane.Its reaction times is depended on the activity and the determined temperature of reaction of used phosphotidic reagent, generally between 0.5-24 hour, is preferably between 0.5-5 hour.
The inventor also finds, adopts a certain amount of low-carbon alcohol, as methyl alcohol, ethanol, propyl alcohol, Virahol or butanols etc., acts on the reacted residual phosphorus esterifying reagent of phosphotidic, carries out direct underpressure distillation again, improves the purity of haloalkane even more ideally.
Following embodiment will further specify the present invention, but be not limited to this scope.
Embodiment 1
Containing the 21%(weight percent with 8 liters) its purity of 1-bromododecane (industrial goods) of lauryl alcohol is about 78%, mixed solution with 500 milliliters of phosphorus tribromides, place 80 ℃ to stir 3.5 hours down, under 0.06 crust (45mmHg) normal atmosphere, 175-180 ℃ of fraction collected in underpressure distillation then, get 5.6 liters of 1-bromododecanes, through day island proper Tianjin GC-9A, the 6%SE-80 chromatographic column detects, and its purity brings up to 92.7%.
Embodiment 2
With the 1-bromododecane industrial goods of 10 liters of embodiment 1 and the mixed solution of 1000 milliliters of phosphorus pentachlorides, place 90 ℃ to stir after 4 hours down, so go into 300 milliliter of 75% ethanol, continue stirring and stopped in 1 hour, all the other operational conditions such as embodiment 1, getting 1-bromododecane purity is 94%.
Embodiment 3
With the 1-bromododecane industrial goods of 10 liters of embodiment 1 and the mixture of 700 gram Vanadium Pentoxide in FLAKESs, place 85 ℃ to stir 5 hours down, all the other operational conditions such as embodiment 1, getting 1-bromododecane purity is 97.5%.
Claims (6)
- A kind of novel process of refining haloalkane simply
- 1, a kind of refining simply haloalkane technology is characterized in that: will contain the haloalkane of alcohol and the system of phosphotidic reagent mixed liquor, place under the certain temperature, and the stirring reaction certain hour, directly underpressure distillation can obtain the higher haloalkane of purity.
- 2, by 1 a described technology, its haloalkane can be used R-(X) the n general formula represents that R can be side chain, straight chain or cyclic alkyl, can also be saturated or undersaturated, its carbonatoms is between 2-20.X is a halogen atom, and its number n is preferably in the 1-3 scope between 1-10, and wherein haloalkane is a bromo, and haloalkanes such as the pentane of chloro or iodo, octane, dodecane or n-Hexadecane are the most suitable.
- 3, by the described technology of claim 1-2, wherein phosphide can be selected Vanadium Pentoxide in FLAKES, phosphorus oxychloride, phosphorus pentachloride, trichlorine or phosphorus tribromide for use for reagent, and above-mentioned phosphotidic agent also can be got by on-site preparation.
- 4, by the described technology of claim 1-3, the consumption of phosphotidic reagent can more than or equal to or less than the equivalent of alcohol in the haloalkane, best excessive 0.2-0.5 doubly.Temperature of reaction is preferably in normal temperature between the boiling point that will make with extra care haloalkane between 10-300 ℃.Reaction times was preferably between 0.5-5 hour between 0.5-24 hour.
- 5, by the described technology of claim 1-4, after the phosphotidic reaction finishes, can add lower alcohol, as the phosphotidic reagent of methyl alcohol, ethanol, propyl alcohol, Virahol or butanols effect remnants, it is even more ideal to carry out direct underpressure distillation again.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 90107912 CN1049491A (en) | 1990-09-26 | 1990-09-26 | A kind of novel process of refining haloalkane simply |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 90107912 CN1049491A (en) | 1990-09-26 | 1990-09-26 | A kind of novel process of refining haloalkane simply |
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| Publication Number | Publication Date |
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| CN1049491A true CN1049491A (en) | 1991-02-27 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 90107912 Pending CN1049491A (en) | 1990-09-26 | 1990-09-26 | A kind of novel process of refining haloalkane simply |
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| CN (1) | CN1049491A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109678647A (en) * | 2018-08-22 | 2019-04-26 | 浙江万盛股份有限公司 | A kind of preparation method of high-purity 1- chlorine normal butane |
-
1990
- 1990-09-26 CN CN 90107912 patent/CN1049491A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109678647A (en) * | 2018-08-22 | 2019-04-26 | 浙江万盛股份有限公司 | A kind of preparation method of high-purity 1- chlorine normal butane |
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