CN101264864A - Automatic pressure-lifting synthesis technique for bromine chloride by one-step method - Google Patents
Automatic pressure-lifting synthesis technique for bromine chloride by one-step method Download PDFInfo
- Publication number
- CN101264864A CN101264864A CNA2008100528854A CN200810052885A CN101264864A CN 101264864 A CN101264864 A CN 101264864A CN A2008100528854 A CNA2008100528854 A CN A2008100528854A CN 200810052885 A CN200810052885 A CN 200810052885A CN 101264864 A CN101264864 A CN 101264864A
- Authority
- CN
- China
- Prior art keywords
- chlorine
- bromine
- reactor
- pressure
- step method
- 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.)
- Pending
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a self-boosted one-step bromine chloride synthesis technology, which is characterized in that the synthesis reaction of the liquid bromine processed by dried pretreatment and the decompressed high purity chlorine is processed in a airtight medium pressure reactor, wherein the chlorine charging speed is 0.35 to 0.60 gram per minute. While the chlorine is charged and the synthesis reaction of bromine and chlorine is processed, the pressure in the reactor is increasing, and the temperature is rising; the pressure can be as high as 10 atm, the temperature ca be as high as 70 DEG C. When the ratio of the mole numbers of chlorine and bromine in the reactor reaches to 1.00-1.02 :1, the charging of chlorine in medium pressure reactor is stopped. After stopping the charging of chlorine, the materials in the reactor is kept to stir in 15 to 20 minutes, and the high purity bromine chloride product is obtained. The self-boosted one-step bromine chloride synthesis technology has the advantages of simple technological process, no three wastes, no need for refining process, little control point, easy operation, convenient maintenance and management and energy saving, and the synthesis product purity is more than 99.70%.
Description
Technical field
The present invention relates to the synthetic technology of interhalogen compounds, particularly relate to the technology of utilizing liquid bromine and chlorine synthesizing chlorinated bromine (BrCl) in middle-pressure reactor.
Background technology
Bromine chloride is a kind of interhalogen compounds as industrial disinfection agent and bromizating agent application, since it has many monopolizing characteristics and extensive use since discovery, has just caused people's great attention.Therefore, the synthetic technology of bromine chloride becomes the important research project of field of inorganic chemical engineering.
Problems such as the bromine chloride synthetic method of prior art generally adopts the non-closed reactor that is communicated with atmosphere, and it is refining to exist that cost height, energy consumption are big, preparing product is still needed are not suitable for expanding examination and scale production.For example:
Japanese Patent is clear-54-9195: and in the reactor that fills the liquid bromine, feed chlorine continuously, and reaction is controlled in 30～70 ℃ the temperature range.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, in the differing temps scope, product contained bromine and chlorine are removed again, also need resulting bromine chloride product further refining after removing.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 3 phases): 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.Described bromine chloride preparation technique synthetic product also needs to make with extra care.Therefore, there are same problem in it and Japanese Patent technology.
" the synthesizing chlorinated bromine technology of low temperature liquid phase single stage method " (sea lake salt and chemical industry, 1999, the 6th phase) and " Study On Pilot Scale Technology of Bromine Chloride " (sea lake salt and chemical industry, 2005, the 6th phase): synthesizing in liquid phase of bromine chloride carried out, and reactor pressure is a normal pressure, and the reaction synthesis temperature is-10 ℃～-20 ℃, resulting bromine chloride product does not need further treating process, and bromine chloride purity reaches 99.00%.But this technology adopts low temperature liquid phase synthetic method, needs powerful refrigerator, and equipment, piping insulation facility are perfect, therefore, have problems such as big, the synthesizing chlorinated bromine cost of energy consumption height.
Summary of the invention
Bromine chloride synthetic method at prior art exists problems such as quality is lower, cost is high, energy consumption is big, the present invention releases a kind of from boosting the synthesizing chlorinated bromine technology of single stage method, its purpose is to utilize liquid bromine and chlorine to react synthesizing chlorinated bromine under middle pressure condition, meet the physical properties that bromine chloride exists and reacts at gas-liquid two-phase, when reducing energy consumption, obtained high purity chlorination bromine.
Automatic pressure-lifting synthesis technique for bromine chloride by one-step method involved in the present invention will carry out building-up reactions through the pretreated liquid bromine of super-dry and high-purity chlorine in airtight middle-pressure reactor.Chlorine feeds from the opening for feed of the reactor that fills the liquid bromine, and feeding speed is 0.35～0.60 Grams Per Minute.The opening for feed of reactor is equipped with tetrafluoro aperture grid distributor, and hole diameter Φ 1mm can be evenly distributed to chlorine in the reactor of containing bromine.Along with the feeding of chlorine and the carrying out of chlorine and bromine building-up reactions, reactor pressure increases, temperature raises.Chlorine feeds the pressure, temperature variation in the speed control reactor, and pressure can reach 10atm, and temperature can reach 70 ℃.When feeding chlorine, the material in the reactor is stirred.The ratio of the mole number of the mole number of chlorine and bromine reaches at 1.00～1.02: 1 o'clock in the middle-pressure reactor, stops to feed in middle-pressure reactor chlorine.After stopping logical chlorine, keep the material in the reactor is continued to stir 15～20 minutes, can obtain highly purified bromine chloride product.
The concrete steps of automatic pressure-lifting synthesis technique for bromine chloride by one-step method are as follows:
(1) in reactor, feeds inert nitrogen gas or exsiccant air;
(2) with the liquid bromine through vitriol oil drying, the water content that makes bromine places reactor with bromine again less than 30ppm;
(3) with high-purity liquid chlorine decompression becoming chlorine, its water content is less than 30ppm, and the tetrafluoro aperture grid distributor that adopts the reactor feed mouth to install is passed into chlorine in the reactor, and logical chlorine speed is 0.35～0.60 Grams Per Minute;
(4) when carrying out building-up reactions, the material in the reactor is stirred to reactor feeding chlorine and with the liquid bromine;
(5) ratio when plain mole number of chlorine in the reactor and bromine mole number reaches 1.00～1.02: in the time of 1, stop to feed chlorine in reactor;
(6) stop to feed chlorine after, keep the material in the reactor is continued to stir 15～20 minutes.
Certainly the synthesizing chlorinated bromine technology of the single stage method of boosting involved in the present invention, liquid bromine and chlorine react under middle pressure condition, meet bromine chloride in the physical properties that gas-liquid two-phase exists, and have quickened the speed of reaction of bromine chloride at gas-liquid two-phase.The tetrafluoro aperture grid distributor that adopts the reactor feed mouth to install is passed into chlorine in the reactor of containing bromine, guarantees all even maximum conversion of chlorine, the raw material availability height.Use inert nitrogen gas or exsiccant air and reactor is carried out pre-cleaning, and remove moisture after the pre-treatment of stock liquid bromine process, reduced the generation of side reaction as shielding gas.Certainly the synthesizing chlorinated bromine technology of the single stage method of boosting involved in the present invention, technical process is simple, and sintetics purity is greater than 99.70%, and the no three wastes need not treating process, and the reference mark is few and easy to operate, easy care and management, save energy.
Embodiment
Embodiment 1
Take by weighing the liquid bromine of 150.80 grams, place the separating funnel that fills 30 milliliters of vitriol oils, left standstill 20 minutes after mixing shakes up, separate, the reactor after the dried bromine of the vitriol oil places the feeding dry air; With the feeding mouth that is connected to after high-purity liquid chlorine decompression on the reactor, chlorine feeds in the described reactor with the flow velocity of 0.6 Grams Per Minute again, and the pressure in the reactor is up to 10atm, and reactor temperature rises to 70 ℃; When the feeding amount of chlorine is 67.60 grams, stop logical chlorine.Continue reaction 15 minutes, obtain product 218.00 grams, bromine chloride purity 99.78%, the rate of recovery 98.93% of chlorine.
Embodiment 2
Take by weighing the liquid bromine of 147.00 grams, place the separating funnel that fills 28 milliliters of vitriol oils, left standstill 20 minutes after mixing shakes up, separate, the reactor after the dried bromine of the vitriol oil places the feeding dry air; With the feeding mouth that is connected to after high-purity liquid chlorine decompression on the reactor, chlorine feeds in the above-mentioned reactor with the flow velocity of 0.5 Grams Per Minute again, and the pressure in the reactor rises to 8atm, and reactor temperature rises to 65 ℃; When the feeding amount of chlorine is 66.00 grams, stop logical chlorine; Continue reaction 15 minutes, obtain product 212.80 grams, bromine chloride purity 99.85%, chlorine yield 99.09%.
Embodiment 3
Take by weighing the liquid bromine of 129.00 grams, place the separating funnel that fills 25 milliliters of vitriol oils, mix and shook up the back refining 20 minutes, separate, place the reactor that feeds rare gas element nitrogen through the dried bromine of the vitriol oil, with the feeding mouth that is connected to after high-purity liquid chlorine decompression on the reactor, chlorine feeds in the above-mentioned reactor with the flow velocity of 0.43 Grams Per Minute again; Pressure in the reactor rises to 5.8atm, and reactor temperature rises to 52 ℃; When the feeding amount of chlorine was 57.80 grams, logical chlorine stopped, and continues reaction 20 minutes, obtained product 186.50 grams, bromine chloride purity 99.89%, chlorine yield 99.32%.
Claims (6)
1, a kind of automatic pressure-lifting synthesis technique for bromine chloride by one-step method, utilize liquid bromine and chlorine synthesizing chlorinated bromine in reactor, it is characterized in that high-purity chlorine that will feed carries out building-up reactions in airtight middle-pressure reactor after pretreated liquid bromine of super-dry and decompression; The speed that feeds chlorine to middle-pressure reactor is 0.35～0.60 Grams Per Minute, and the ratio of chlorine mole number and bromine mole number reaches at 1.00～1.02: 1 o'clock in the middle-pressure reactor, stops chlorine and feeds.
2, automatic pressure-lifting synthesis technique for bromine chloride by one-step method according to claim 1 is characterized in that, the liquid bromine is through vitriol oil drying, and the water content of dry back liquid bromine is less than 30ppm.
3, automatic pressure-lifting synthesis technique for bromine chloride by one-step method according to claim 1 is characterized in that, the chlorine of employing is high-purity liquid chlorine, and its water content is less than 30ppm.
4, automatic pressure-lifting synthesis technique for bromine chloride by one-step method according to claim 1 is characterized in that, chlorine feeds from the opening for feed of reactor, and the opening for feed of reactor is equipped with tetrafluoro aperture grid distributor, chlorine can be evenly distributed in the reactor of containing bromine.
5, automatic pressure-lifting synthesis technique for bromine chloride by one-step method according to claim 1 is characterized in that, when carrying out building-up reactions to reactor feeding chlorine and with the liquid bromine, the material in the reactor is stirred.
6, automatic pressure-lifting synthesis technique for bromine chloride by one-step method according to claim 5 is characterized in that, after stopping to feed chlorine, keeps the material in the reactor is continued to stir 15～20 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100528854A CN101264864A (en) | 2008-04-25 | 2008-04-25 | Automatic pressure-lifting synthesis technique for bromine chloride by one-step method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100528854A CN101264864A (en) | 2008-04-25 | 2008-04-25 | Automatic pressure-lifting synthesis technique for bromine chloride by one-step method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101264864A true CN101264864A (en) | 2008-09-17 |
Family
ID=39987592
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2008100528854A Pending CN101264864A (en) | 2008-04-25 | 2008-04-25 | Automatic pressure-lifting synthesis technique for bromine chloride by one-step method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101264864A (en) |
Cited By (3)
| 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 |
| CN112794286A (en) * | 2021-03-26 | 2021-05-14 | 大连海惠博科技有限公司 | Continuous flow method synthesis system and synthesis process of bromine chloride |
-
2008
- 2008-04-25 CN CNA2008100528854A patent/CN101264864A/en active Pending
Cited By (5)
| 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 |
| CN112794286A (en) * | 2021-03-26 | 2021-05-14 | 大连海惠博科技有限公司 | Continuous flow method synthesis system and synthesis process of bromine chloride |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| EP1690980A1 (en) | Process and apparatus for conversion of biomass | |
| TW366336B (en) | Process for producing highly pure terephthalic acid | |
| WO1990013514A1 (en) | Gaseous generator system for preparing chlorine dioxide | |
| CN102690218A (en) | Method for synthesizing xanthate | |
| CN101264864A (en) | Automatic pressure-lifting synthesis technique for bromine chloride by one-step method | |
| CN110877914A (en) | Method for preparing high-purity high-white calcium carbonate by mineralizing and fixing carbon dioxide with phosphogypsum | |
| CN101863496A (en) | Method for preparing battery grade lithium carbonate by purifying industrial grade lithium carbonate | |
| KR0138587B1 (en) | Novel method for the production of methanol | |
| CN102627306B (en) | Novel method for preparing solid aluminum sulfate by using waste | |
| CN107406401B (en) | Process for the manufacture of furan-2, 5-dicarboxylic acid (FDCA) from solid salts | |
| CN108047208A (en) | A kind of method for reducing Losartan dimer impurity | |
| CN109422641B (en) | Continuous production method for preparing calcium formate from yellow phosphorus tail gas | |
| CN104610045A (en) | Method for producing dimer acid, and production apparatus automatically enforcing method | |
| CN109896503B (en) | Solvent system and method for producing hydrogen peroxide by anthraquinone process | |
| CN101709055A (en) | Method for synthesizing ionic liquid | |
| CN108484423A (en) | A method of isolating and purifying l-Alanine from l-Alanine zymotic fluid | |
| CN111217718B (en) | Sulfur-free 2-bromo-4-fluoroacetanilide synthesis method | |
| WO2023019666A1 (en) | Preparation process for depleted anhydrous zinc acetate | |
| CN107473271A (en) | A kind of preparation method of PAFS | |
| CN103804162B (en) | Method for preparing high-purity 9-fluorenone from high-purity fluorene | |
| CA1097478A (en) | Production of chlorine dioxide | |
| US4049785A (en) | Production of chlorine dioxide with product slurry metathesis | |
| CN104098722B (en) | Dehydration and replacement device and method for seed bed of polyethylene device reactor | |
| JP6274838B2 (en) | Method for producing alkali metal sulfide | |
| CN1554571A (en) | Low temperature liquid phase one-step synthesizing bromine chloride |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20080917 |