CN101891600A - Preparation method of p-bromoethoxybenzene - Google Patents
Preparation method of p-bromoethoxybenzene Download PDFInfo
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- CN101891600A CN101891600A CN2010102653555A CN201010265355A CN101891600A CN 101891600 A CN101891600 A CN 101891600A CN 2010102653555 A CN2010102653555 A CN 2010102653555A CN 201010265355 A CN201010265355 A CN 201010265355A CN 101891600 A CN101891600 A CN 101891600A
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Abstract
The invention relates to a preparation method of p-bromoethoxybenzene, comprising the following steps: (1) etherification reaction: throwing p-bromophenol and diethyl sulfate into a reaction kettle, stirring, heating, distributing and adding sodium hydroxide to react; (2) washing: adding water to a mixture after etherification reaction, evenly stirring, standing and layering to separate out oily liquid; and (3) rectification: rectifying an oil layer by an efficient rectification tower to obtain the finished product. In the preparation method, the efficient rectification tower is used for rectification instead of the original distillation operation, thus reducing the usage amount of diethyl sulfate and water, keeping the reaction temperature at 30-50 DEG C, saving energy, obtaining high-quality and high-content p-bromoethoxybenzene, achieving high content of p-bromoethoxybenzene up to 99.5% and enhancing the market competitiveness of the product.
Description
Technical field
The invention belongs to the organic compound preparation field, especially a kind of preparation method to Bromoethyl phenyl ether.
Background technology
In the luminous industrial production of chemiluminescence, Bromoethyl phenyl ether had more and more widely application as a kind of important organic compound.Common production method to Bromoethyl phenyl ether is a diazotization reaction, because diazotization reaction needs low temperature to carry out, so need low-temperature freezing facilities, the problem that this type of preparation method exists: 1, owing to need to use expensive refrigerating water pump to realize in the diazotization reaction step, therefore, there is the problem that production unit is many, expense is high in this method, thereby is difficult to reduce cost.2, because the diazotization reaction step is to produce essential in the Bromoethyl phenyl ether process and very consuming time, the production stage of power consumption, therefore, there is the problem that the production time is long, production efficiency is low in this method, is unfavorable for the raising of business economic benefit.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, the preparation method who provides a kind of and can save facility investment, reduces cost, shortens the production time and can enhance productivity to Bromoethyl phenyl ether.
It is to realize by the following technical solutions that the present invention solves its technical problem:
A kind of preparation method to Bromoethyl phenyl ether, this method may further comprise the steps:
(1) etherification reaction step: to one having that heating unit, electricity stir, dropping into p bromophenol, water, ethyl sulfate successively in 50 liters of reactors of thermometer, under agitation be heated to 30 ℃ of-50 ℃ of reactions simultaneously, keep this state of temperature, constantly add sodium hydroxide, sodium hydroxide added the back insulation reaction 1 hour; Stop heating, etherification reaction stops;
(2) water-washing step: will obtain to such an extent that discharge water in the mixed solution behind the etherification reaction, after stirring, standing demix be isolated oil reservoir.
(3) rectification step: oil reservoir is carried out high-efficient spiral-screen column rectifying, and the product that obtains is to the Bromoethyl phenyl ether finished product.
And described p bromophenol: ethyl sulfate: water: the mol ratio of sodium hydroxide is 1: 0.55: 20: 1.1.
And the mol ratio of described water and p bromophenol is 80: 1.
And described rectifying tower is 10 grades of high efficiency separation rectifying tower, uses
The type gauze packing.
Advantage of the present invention and positively effect are:
1, this preparation method uses direct etherification reaction to replace diazotization reaction in synthesis step, and the qualified product that obtain do not need cryogenic freezing diazotization to handle; Prepared quality product meets the technical requirements fully.This preparation method has saved the cryogenic freezing step when producing, avoided the input of refrigerating water pump equipment, therefore, has saved facility investment, reduce production costs,
2, the direct etherification reaction used of this preparation method replaces diazotization reaction, has easy to operately, simplely is convenient to realize suitability for industrialized production, enhances productivity.
3, this preparation method, owing to adopt high-efficient spiral-screen column rectifying, replace original distillation procedure by distillation operation, reduced the charging capacity of ethyl sulfate and water, making temperature of reaction is 30-50 ℃, save energy, and obtain high-quality, high-load to Bromoethyl phenyl ether, can make content reach 99.5%, improve the competitiveness of product in market Bromoethyl phenyl ether.
Embodiment
The invention will be further described below by specific embodiment, and following examples are descriptive, is not determinate, can not limit protection scope of the present invention with this.
Embodiment 1:
A kind of preparation method to Bromoethyl phenyl ether may further comprise the steps:
(1) etherification reaction step: to one having that heating unit, electricity stir, dropping into 10 moles of p bromophenols, 200 moles in water, 5.5 moles of ethyl sulfates successively in 50 liters of reactors of thermometer, under agitation be heated to 35 ± 2 ℃ of reactions simultaneously, keep this state of temperature, constantly add 11 moles in sodium hydroxide, sodium hydroxide added the back insulation reaction 1 hour; Stop heating, etherification reaction stops.
(2) water-washing step: will obtain to such an extent that put 800 mole of water in the mixed solution behind the etherification reaction, after stirring, standing demix be isolated oil reservoir.
(3) rectification step: oil reservoir is carried out high-efficient spiral-screen column rectifying, and this rectifying tower is 10 grades of high efficiency separation rectifying tower, uses
Type gauze packing, the product that obtains are that its content is 99.5% to the Bromoethyl phenyl ether finished product, and color is less than No. 30 (platinum-cobalt colorimetric).
Embodiment 2:
A kind of preparation method to Bromoethyl phenyl ether may further comprise the steps:
(1) etherification reaction step: to one having that heating unit, electricity stir, dropping into 10 moles of p bromophenols, 200 moles in water, 5.5 moles of ethyl sulfates successively in 50 liters of reactors of thermometer, under agitation be heated to 40 ± 2 ℃ of reactions simultaneously, keep this state of temperature, constantly add 11 moles in sodium hydroxide, sodium hydroxide added the back insulation reaction 1 hour; Stop heating, etherification reaction stops.
(2) water-washing step: will obtain to such an extent that put 800 mole of water in the mixed solution behind the etherification reaction, after stirring, standing demix be isolated oil reservoir.
(3) rectification step: oil reservoir is carried out high-efficient spiral-screen column rectifying, and this rectifying tower is 10 grades of high efficiency separation rectifying tower, uses
Type gauze packing, the product that obtains are that its content is 99.5% to the Bromoethyl phenyl ether finished product, and color is less than No. 30 (platinum-cobalt colorimetric).
Embodiment 3:
A kind of preparation method to Bromoethyl phenyl ether may further comprise the steps:
(1) etherification reaction step: to one having that heating unit, electricity stir, dropping into 10 moles of p bromophenols, 200 moles in water, 5.5 moles of ethyl sulfates successively in 50 liters of reactors of thermometer, under agitation be heated to 45 ± 2 ℃ of reactions simultaneously, keep this state of temperature, constantly add 11 moles in sodium hydroxide, sodium hydroxide added the back insulation reaction 1 hour; Stop heating, etherification reaction stops.
(2) water-washing step: will obtain to such an extent that put 800 mole of water in the mixed solution behind the etherification reaction, after stirring, standing demix be isolated oil reservoir.
(3) rectification step: oil reservoir is carried out high-efficient spiral-screen column rectifying, and this rectifying tower is 10 grades of high efficiency separation rectifying tower, uses
Type gauze packing, the product that obtains are that its content is 99.5% to the Bromoethyl phenyl ether finished product, and color is less than No. 30 (platinum-cobalt colorimetric).
Claims (4)
1. the preparation method to Bromoethyl phenyl ether is characterized in that, this method may further comprise the steps:
(1) etherification reaction step: to one having that heating unit, electricity stir, dropping into p bromophenol, water, ethyl sulfate successively in 50 liters of reactors of thermometer, under agitation be heated to 30 ℃ of-50 ℃ of reactions simultaneously, keep this state of temperature, constantly add sodium hydroxide, sodium hydroxide added the back insulation reaction 1 hour; Stop heating, etherification reaction stops;
(2) water-washing step: will obtain to such an extent that discharge water in the mixed solution behind the etherification reaction, after stirring, standing demix be isolated oil reservoir.
(3) rectification step: oil reservoir is carried out high-efficient spiral-screen column rectifying, and the product that obtains is to the Bromoethyl phenyl ether finished product.
2. the preparation method to Bromoethyl phenyl ether according to claim 1 is characterized in that: described p bromophenol: ethyl sulfate: water: the mol ratio of sodium hydroxide is 1: 0.55: 20: 1.1.
3. the preparation method to Bromoethyl phenyl ether according to claim 1 is characterized in that: the mol ratio of described water and p bromophenol is 80: 1.
4. the preparation method to Bromoethyl phenyl ether according to claim 1 is characterized in that: described rectifying tower is 10 grades of high efficiency separation rectifying tower, uses
The type gauze packing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102653555A CN101891600A (en) | 2010-08-28 | 2010-08-28 | Preparation method of p-bromoethoxybenzene |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102653555A CN101891600A (en) | 2010-08-28 | 2010-08-28 | Preparation method of p-bromoethoxybenzene |
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| CN101891600A true CN101891600A (en) | 2010-11-24 |
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| CN2010102653555A Pending CN101891600A (en) | 2010-08-28 | 2010-08-28 | Preparation method of p-bromoethoxybenzene |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108997091A (en) * | 2018-07-10 | 2018-12-14 | 盐城市胜达化工有限公司 | A kind of method of silver bicarbonate activation 2- Bromoethyl phenyl ether |
-
2010
- 2010-08-28 CN CN2010102653555A patent/CN101891600A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108997091A (en) * | 2018-07-10 | 2018-12-14 | 盐城市胜达化工有限公司 | A kind of method of silver bicarbonate activation 2- Bromoethyl phenyl ether |
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Application publication date: 20101124 |