CN101367708A - Preparation of chloro-cyclohexane under nitrogen protection - Google Patents
Preparation of chloro-cyclohexane under nitrogen protection Download PDFInfo
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- CN101367708A CN101367708A CNA2008101392974A CN200810139297A CN101367708A CN 101367708 A CN101367708 A CN 101367708A CN A2008101392974 A CNA2008101392974 A CN A2008101392974A CN 200810139297 A CN200810139297 A CN 200810139297A CN 101367708 A CN101367708 A CN 101367708A
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Abstract
The invention relates to a preparation method of chlorocyclohexane under the protection of nitrogen; the method is characterized in that the mixture of nitrogen and chlorine continuously is filled from the side opening of the lower part of a reactor, and cyclohexane is filled from the lower port of the reactor; the chlorine is pre-dispersed by the nitrogen, and then evenly mixed with the cyclohexane in the mixing area of the reactor, and enters into the reacting area of the reactor and reacts rapidly under the priming of the green ray to produce chlorocyclohexane which flows out of a overflow pipe, thereby improving the selectivity and the yield of the chlorocyclohexane. The nitrogen is continuously filled, so the reactor can be always in the state of nitrogen filling, which effectively prevents explosion accident.
Description
Technical field
The invention belongs to the synthesis technique of organic chemical industry's product, a kind of specifically novel process of safety preparation chlorocyclohexane.
Background technology
Chlorocyclohexane is a kind of basic raw material of organic synthesis, also is a kind of important fine chemical product.It is mainly used in the intermediate of products such as rubber anti-chark agent CTP, medical artane, agricultural chemicals cyhexatin; Also can be used for the polyurethane foam catalyst n, N-dimethylcyclohexylamine, rust-preventive agent etc. synthetic.
In numerous chlorocyclohexane preparation methods, the hexanaphthene light chlorination process has overcome the shortcoming of hexalin hydrogenchloride method of substitution, hexanaphthene chlorine method of substitution, tetrahydrobenzene hydrogenchloride additive process, low because of its temperature of reaction, speed of response is fast, adopts light source to avoid plurality of advantages such as catalyst contamination as initiator and had an optimistic view of by the entrepreneur.Patent 200410041630.X adopts reactor and rectifying tower coupled technology to improve transformation efficiency, improves selectivity on original basis.But because the inlet of hexanaphthene and chlorine has just begun reaction all at reaction zone when material also has little time to mix, because the part exists chlorine gas concentration too high, so still there is the drawback of consecutive chlorination reaction.In addition, just there is safety problem in original hexanaphthene light chlorination process, if reactor and rectifying tower are coupled, tower still temperature can reach 140～150 ℃, has more increased unsafe factor.
Summary of the invention
The object of the present invention is to provide that a kind of chlorination selectivity is good, cyclohexane conversion is high and the hexanaphthene light chlorination process of good operation safety prepares the method for chlorocyclohexane.
The present invention is achieved in that
Chlorine and nitrogen is 1:(0.5～1 by volume) carry out pre-mixing, gas mixture feeds continuously from the side mouth of the reactor lower part amount of chlorine with 70～80kg/h, and hexanaphthene feeds from the reactor bottom port continuously with the speed of 320～340L/h.The bottom of reactor is the mixing of materials district, and hexanaphthene and chlorine nitrogen mixed gas arrive reactor top through the thorough mixing of mixing zone, and the initiation light source is arranged here, are the reaction zones of reactor.Under the effect of certain temperature and initiation light source, chlorine and hexanaphthene react rapidly, generate chlorocyclohexane, with unreacted hexanaphthene from vertical discharger track overflow, enter crude steam kettle continuously and carry out continuous still battery, remove most of hexanaphthene, form the crude product chlorocyclohexane.The crude product chlorocyclohexane is squeezed into rectifying still again and is purified, and obtains the high-purity chloro hexanaphthene.
Advantage of the present invention mainly is presented as:
1. chlorine enters before the reactor, uses nitrogen dilution, and the uniform distribution of chlorine in hexanaphthene played pre-dispersed effect.
2. enter the nitrogen of reactor with chlorine,, in reactor, reactive system has been played provide protection, effectively prevented the generation of explosion hazard, do not have side reaction again and take place as rare gas element.
3. adopt the mode of underfeed, make hexanaphthene and chlorine before reaction, sufficient mixing time and space are arranged, effectively prevented the consecutive chlorination reaction, ensured the selectivity of chlorocyclohexane.
4. after chlorocyclohexane generates, in time overflow from overflow spout, short in the reaction zone residence time, effectively prevented the consecutive chlorination reaction.
5. the mode that adopts simple distillation and smart distillation to engage in the thick steaming stage, steams a large amount of hexanaphthenes with lower temperature, carries out reuse.Steam the stage in essence, obtain the high purity chlorocyclohexane, accomplished reasonable energy utilization, improve the purity of chlorocyclohexane with underpressure distillation.
Description of drawings
Accompanying drawing 1 is a process flow sheet
Accompanying drawing 2 is the reactor synoptic diagram
Embodiment:
Below in conjunction with embodiment the present invention is elaborated.
Feed hexanaphthene from the reactor bottom port continuously with the speed of 320～340L/h, open steam valve and make the temperature of reactor rise to 50-60 ℃.Chlorine and nitrogen are 1:(0.5～1 by volume) mixes the back and feed continuously from reactor bottom side mouth, the adjusting flow valve, the feeding speed that makes chlorine is 70～80kg/h.Chlorine carries out thorough mixing at the mixing zone and the hexanaphthene of reactor lower part behind nitrogen dilution, arrive the reaction zone (reactor top) that causes light source is housed, and reacts rapidly under the initiation that causes light, generates chlorocyclohexane.Reaction plays important provide protection to the nitrogen that feeds to security of system.The chlorocyclohexane that generates in time overflows from overflow spout, enters into thick steaming system continuously, the hexanaphthene that steams reuse after condensation, and the purity of the crude product chlorocyclohexane that overflows by equilibration tube can reach about 95%, and the content of polychloride is less than 3%.The crude product chlorocyclohexane is squeezed in the rectifying still by vacuum, carries out underpressure distillation, can get purity greater than 99.5% chlorocyclohexane finished product, and the yield of chlorocyclohexane reaches more than 90%.Front-end volatiles mainly contain hexanaphthene and carry out reuse.In the reaction process, the hydrogen chloride gas of formation absorbs through the last water of multi-stage condensing, forms hydrochloric acid and sells or utilization as by product.
Claims (8)
1. the preparation technology of chloro-cyclohexane under nitrogen protection is characterized in that: nitrogen mixes the back and feeds continuously from the side mouth of reactor lower part with chlorine, hexanaphthene feeds continuously from the reactor lower port.Chlorine is earlier pre-dispersed through nitrogen, then at the mixing zone and the hexanaphthene thorough mixing of reactor, gas-liquid mixture enters reaction zone reaction rapidly under the initiation that causes light, in time flow out from upflow tube after generating chlorocyclohexane, enter thick steaming system continuously and carry out continuously thick the steaming, become the finished product chlorocyclohexane after the crude product chlorocyclohexane rectification and purification.Nitrogen feeds continuously, reactive system is in all the time fills the nitrogen state, has effectively prevented the generation of explosion hazard.
2. preparation technology according to claim 1 is characterized in that: chlorination reaction is continuously feeding, successive reaction, discharging continuously.
3. preparation technology according to claim 1 is characterized in that: chlorine and nitrogen are with volume ratio 1:(0.5～1) mix.
4. preparation technology according to claim 1 is characterized in that: feed reactor again after nitrogen and the chlorine pre-mixing and mix with hexanaphthene.
5. preparation technology according to claim 1 is characterized in that: the feeding speed of chlorine is 70～80kg/h, and the feeding speed of hexanaphthene is 320～340L/h.
6. preparation technology according to claim 1 is characterized in that: chlorine and hexanaphthene all adopt the bottom reinforced, help gas-liquid and mix mutually, prevent the generation of consecutive chlorination reaction.
7. preparation technology according to claim 1 is characterized in that: the thick steaming is continuously feeding, continuous still battery, discharging continuously.
8. preparation technology according to claim 1 is characterized in that: reactor is in all the time and fills under the nitrogen state, prevents the generation of explosion hazard.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2008101392974A CN101367708B (en) | 2008-08-27 | 2008-08-27 | Preparation of chloro-cyclohexane under nitrogen protection |
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| CN2008101392974A CN101367708B (en) | 2008-08-27 | 2008-08-27 | Preparation of chloro-cyclohexane under nitrogen protection |
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| CN101367708A true CN101367708A (en) | 2009-02-18 |
| CN101367708B CN101367708B (en) | 2011-02-02 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106824005A (en) * | 2017-02-12 | 2017-06-13 | 江苏诚信药业有限公司 | Prepare the process system of ebutol |
| CN108484351A (en) * | 2018-04-19 | 2018-09-04 | 北京阳光欣禾科技有限公司 | A kind of efficient chlorination process method producing chlorocyclohexane |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1279009C (en) * | 2004-08-09 | 2006-10-11 | 南京工业大学 | Method for producing chlorocyclohexane through coupling between chlorination reactor and rectification tower |
| CN1291957C (en) * | 2004-12-30 | 2006-12-27 | 锦化化工（集团）有限责任公司 | Method for preparing chlorocyclohexane |
| JP5118645B2 (en) * | 2005-11-03 | 2013-01-16 | ハネウェル・インターナショナル・インコーポレーテッド | Method for producing a fluorinated organic compound |
-
2008
- 2008-08-27 CN CN2008101392974A patent/CN101367708B/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106824005A (en) * | 2017-02-12 | 2017-06-13 | 江苏诚信药业有限公司 | Prepare the process system of ebutol |
| CN108484351A (en) * | 2018-04-19 | 2018-09-04 | 北京阳光欣禾科技有限公司 | A kind of efficient chlorination process method producing chlorocyclohexane |
| CN108484351B (en) * | 2018-04-19 | 2020-10-30 | 北京阳光欣禾科技有限公司 | Efficient chlorination reaction process method for producing chlorocyclohexane |
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| CN101367708B (en) | 2011-02-02 |
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Owner name: SHANDONG YANGGU HUATAI CHEMICAL INDUSTRY CO., LTD. Free format text: FORMER OWNER: WANG ZHUANHUA Effective date: 20091204 |
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Effective date of registration: 20091204 Address after: 217#, 217, Qinghe West Road, Yanggu County, Shandong, Liaocheng, China: 252300 Applicant after: Shandong Yanggu Huatai Chemical Co., Ltd. Address before: Shandong, Yanggu, Huatai Chemical Co., Ltd., Yanggu County, Yanggu County, Liaocheng, Shandong Province, China Code: 252300 Applicant before: Wang Chuanhua |
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