CN1554571A - Low temperature liquid phase one-step synthesizing bromine chloride - Google Patents
Low temperature liquid phase one-step synthesizing bromine chloride Download PDFInfo
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- CN1554571A CN1554571A CNA2003101178501A CN200310117850A CN1554571A CN 1554571 A CN1554571 A CN 1554571A CN A2003101178501 A CNA2003101178501 A CN A2003101178501A CN 200310117850 A CN200310117850 A CN 200310117850A CN 1554571 A CN1554571 A CN 1554571A
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Abstract
The present invention relates to bromine chloride synthesizing technology. Liquid bromine and chlorine gas are pretreated via drying and reacted at low temperature of -10 to -20 deg.c in a reactor to synthesize bromine chloride. The pre-treatment of the material can reduce side reactions, and the synthesizing temperature below the boiling point of bromine chloride ensures the synthesis of bromine chloride in single liquid phase. Chlorine gas is introduced into bromine container homogeneously to ensure the high conversion rate and high material utilization. The bromine chloride synthesizing process of the present invention is simple, easy in operation, maintenance and management and the product has purity over 99% and needs no refining.
Description
Technical field
The present invention relates to a kind of synthetic technology of interhalogen compounds, particularly relate to the synthetic technology of bromine chloride (BrCl).
Background technology
Bromine chloride is a kind of interhalogen compounds, since the great attention of finding just to have caused since it has many monopolizing characteristics and extensive use people.Therefore, the synthetic technology of bromine chloride becomes the important research project of field of inorganic chemical engineering.
The synthetic technology of existing bromine chloride has similar substantially technology, has all that cost height, energy consumption are big, preparing product is still needed the purified problem, is not suitable for expanding examination and scale production.With Japanese Patent and domestic public technology is that example illustrates existing lifting synthesis technique for bromine chloride:
Japanese Patent is clear-54-9195: and in the reactor that fills the liquid bromine, feed chlorine continuously, and temperature of reaction is controlled in 30-70 ℃ the scope.Because the boiling point of bromine is 58.5 ℃, therefore, synthesizing in gas-liquid two-phase of bromine chloride carried out.Behind synthetic the finishing, according to the boiling point of bromine chloride, bromine and chlorine, remove the contained bromine of product, chlorine in the differing temps scope, removing the resulting product bromine chloride in back also needs further refining.Therefore, utilize the synthesizing chlorinated bromine cost of this patented technology height, energy consumption is big, technical process is long, treating process also can produce pollution.
" produce the shop experiment of bromine chloride " (sea lake salt and chemical industry, 1998, the 3rd phase): except that stock liquid bromine, chlorine being carried out drying and control synthesizing chlorinated bromine temperature 40-42 ℃, remaining Technology is identical with above-mentioned Japanese Patent technology, and the product of this technology system also needs to make with extra care.Therefore, there are same problem in it and Japanese Patent technology.
Summary of the invention
For solving the problem that exists in the existing lifting synthesis technique for bromine chloride, the present invention releases the technology of a kind of low temperature, the synthesizing chlorinated bromine of liquid phase one-step, has avoided prior art synthetic existing inversion of phases problem in gas-liquid two-phase, does not also need treating process, save energy.
Lifting synthesis technique for bromine chloride involved in the present invention is through synthesizing bromine chloride in-10--20 ℃ temperature range after the super-dry pre-treatment in reactor with liquid bromine and chlorine.
According to 5 ℃ of the boiling points of bromine chloride, the synthesis temperature of determining is below the boiling point of bromine chloride, to guarantee that synthesizing chlorinated bromine is mainly in liquid phase.For making the synthetic high product purity, in synthesizing chlorinated bromine forward reaction device, feed the exsiccant air as protection gas, avoid side reaction to take place; And dry preprocessing process is the drying process of being removed major impurity water in stock liquid bromine and the chlorine by the vitriol oil.
The concrete steps of the synthesizing chlorinated bromine of low temperature liquid phase single stage method are as follows:
(1) in reactor, feeds the exsiccant air;
(2) with the liquid bromine through vitriol oil drying, the water content that makes bromine places reactor with bromine again less than 50ppm, and reactor temperature is transferred to-10--20 ℃;
(3) with chlorine through vitriol oil drying, the water content that makes chlorine is less than 50ppm, adopts the bottom to have the tubule of uniform small pores that chlorine is fed at a slow speed in the reactor of containing bromine again, the bottom of tubule places below the bromine liquid level;
(4) when the mole number of chlorine is 1-1.2 times of bromine mole number, stop to feed chlorine, liquid bromine and chlorine promptly synthesize the bromine chloride product.
The synthesizing chlorinated bromine technology of low temperature liquid phase single stage method involved in the present invention use the exsiccant air as shielding gas, and raw material has reduced the side reaction generation through pre-treatment.Synthesis temperature guarantees the synthetic mainly synthetic in single phase-liquid phase of bromine chloride below the boiling point of bromine chloride.Adopt the bottom to have the tubule of uniform small pores chlorine to be fed in the reactor of containing bromine, guarantee the even feeding of chlorine and farthest transform the raw material availability height.Lifting synthesis technique for bromine chloride involved in the present invention, technical process is simple, easy operation, maintenance and management, sintetics purity need not treating process greater than 99%, save energy.
Embodiment
Embodiment 1
Take by weighing the liquid bromine of 155 grams, place the separating funnel that fills 30 milliliters of vitriol oils, left standstill after shaking up 15 minutes, separate, the reactor after the dried bromine of the vitriol oil places the feeding dry air; Chlorine cylinder is connected in the vitriol oil drying bottle, chlorine feeds in the above-mentioned reactor after with the drying bottle of flow velocity through filling 50 milliliters of vitriol oils of 0.70 Grams Per Minute again, and the temperature of controlling reactor is-10 ℃; When the feeding amount of chlorine is 82.5 grams, stop to feed, obtain product bromine chloride 223 grams, purity is 99.01%, the rate of recovery of chlorine is 83.73%.
Embodiment 2
Take by weighing the liquid bromine of 132 grams, place the separating funnel that fills 25 milliliters of vitriol oils, left standstill after shaking up 15 minutes, separate, the reactor after the dried bromine of the vitriol oil places the feeding dry air; Chlorine cylinder is connected in the vitriol oil drying bottle, chlorine feeds in the above-mentioned reactor after with the drying bottle of flow velocity through filling 40 milliliters of vitriol oils of 0.47 Grams Per Minute again, and the temperature of controlling reactor is-15 ℃; When the feeding amount of chlorine is 65.6 grams, stop to feed, obtain product bromine chloride 190 grams, purity is 99.10%, the rate of recovery of chlorine is 88.41%.
Embodiment 3
Take by weighing the liquid bromine of 108 grams, place the separating funnel that fills 20 milliliters of vitriol oils, left standstill after shaking up 15 minutes, separate, the reactor after the dried bromine of the vitriol oil places the feeding dry air; Chlorine cylinder is connected in the vitriol oil drying bottle, chlorine feeds in the above-mentioned reactor after with the drying bottle of flow velocity through filling 32 milliliters of vitriol oils of 0.22 Grams Per Minute again, and the temperature of controlling reactor is-20 ℃; When the feeding amount of chlorine is 52.5 grams, stop to feed, obtain product bromine chloride 155 grams, purity is 99.19%, the rate of recovery of chlorine is 91.83%.
Claims (5)
1, the technology of the synthesizing chlorinated bromine of a kind of low temperature liquid phase single stage method is characterized in that liquid bromine and chlorine through synthesizing bromine chloride in-10--20 ℃ temperature range after the super-dry pre-treatment in reactor.
2, the technology of the synthesizing chlorinated bromine of low temperature liquid phase single stage method according to claim 1 is characterized in that liquid bromine and chlorine through vitriol oil drying, and dried liquid bromine and chlorine water content are all less than 50ppm.
3, the technology of the synthesizing chlorinated bromine of low temperature liquid phase single stage method according to claim 1 is characterized in that the tubule that adopts the bottom that uniform small pores is arranged feeds chlorine at a slow speed in the reactor of containing bromine, and the speed that chlorine feeds is the 0.22-0.70 Grams Per Minute.
4, the technology of the synthesizing chlorinated bromine of low temperature liquid phase single stage method according to claim 4, the bottom that it is characterized in that feeding the tubule of chlorine places below the bromine liquid level.
When 5, the synthesizing chlorinated bromine technology of low temperature liquid phase single stage method according to claim 4, the mole number that it is characterized in that feeding chlorine are 1-1.2 times of bromine mole number, stop to feed chlorine.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2003101178501A CN1554571A (en) | 2003-12-22 | 2003-12-22 | Low temperature liquid phase one-step synthesizing bromine chloride |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2003101178501A CN1554571A (en) | 2003-12-22 | 2003-12-22 | Low temperature liquid phase one-step synthesizing bromine chloride |
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| CN1554571A true CN1554571A (en) | 2004-12-15 |
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| CNA2003101178501A Pending CN1554571A (en) | 2003-12-22 | 2003-12-22 | Low temperature liquid phase one-step synthesizing bromine chloride |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104477850A (en) * | 2014-12-02 | 2015-04-01 | 中国船舶重工集团公司第七一八研究所 | Preparation method and device of chlorine trifluoride |
| CN109438168A (en) * | 2018-11-13 | 2019-03-08 | 大连奇凯医药科技有限公司 | The preparation method of five bromofluorobenzenes |
-
2003
- 2003-12-22 CN CNA2003101178501A patent/CN1554571A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104477850A (en) * | 2014-12-02 | 2015-04-01 | 中国船舶重工集团公司第七一八研究所 | Preparation method and device of chlorine trifluoride |
| CN104477850B (en) * | 2014-12-02 | 2016-08-24 | 中国船舶重工集团公司第七一八研究所 | The preparation method of a kind of chlorine trifluoride and device |
| CN109438168A (en) * | 2018-11-13 | 2019-03-08 | 大连奇凯医药科技有限公司 | The preparation method of five bromofluorobenzenes |
| CN109438168B (en) * | 2018-11-13 | 2021-06-11 | 大连奇凯医药科技有限公司 | Preparation method of bromopentafluorobenzene |
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