CN103922940A - Nitrobenzene production technology - Google Patents
Nitrobenzene production technology Download PDFInfo
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- CN103922940A CN103922940A CN201310630771.4A CN201310630771A CN103922940A CN 103922940 A CN103922940 A CN 103922940A CN 201310630771 A CN201310630771 A CN 201310630771A CN 103922940 A CN103922940 A CN 103922940A
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- mirbane
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- production
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- microtubule reactor
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Abstract
The invention discloses a nitrobenzene production technology. The production technology comprises the following steps: benzene and a gas nitrating agent are used as raw materials for composition of reactants; a metering pump is arranged in the inlet of a micro tube reactor, the feeding ratio of the reactants is controlled to be 1:1.01-1:1.1, and the feeding ratio is molar ratio; the outlet pressure of the metering pump used in the micro tube reactor is greater than 4bar, but is less than the maximum pressure of the micro tube reactor; the reactants are put in the micro tube reactor for continuous flow reaction; the temperature of the reaction process is controlled at in 40-80 DEG C; and the residence time of the reactants in the micro tube reactor is 30s-4h. In the production technology, the reactants are easy to separate, and can be recycled; a production plant covers a small area, the production capacity of the unit plant is large, the production process is short, the operation intensity is low; the energy consumption is low; the production technology does not produce waste acids, is non-pollution to the environment, simplifies the production process, reduces energy consumption, and reduces the cost of nitrobenzene production.
Description
Technical field
The present invention relates to a kind of production technique of industrial chemicals, relate in particular to a kind of production technique of oil of mirbane.
Background technology
Oil of mirbane is a kind of important industrial chemicals, traditional mode of production oil of mirbane be benzene and nitration mixture (vitriol oil+concentrated nitric acid) under violent stirring, reaction generates oil of mirbane, after having reacted, adds water, and isolates oil of mirbane.Separated after oil of mirbane, the concentration of nitration mixture (main component is sulfuric acid) is in 60% left and right.At present, the industrial processing for this intermediate concentration sulfuric acid mainly contains: (1) sulfuric acid concentrate; Concentrate mainly contain two kinds: the one, direct evaporation and concentrating; The shortcoming of evaporation and concentrating is that energy consumption is high, and equipment corrosion is serious, and equipment needs periodic replacement.The 2nd, add SO
3concentrate; In the sulfuric acid of lower concentration, add SO
3although, can improve the concentration of sulfuric acid, also improve the total amount of sulfuric acid simultaneously.In unnecessary sulfuric acid, contain a certain amount of oil of mirbane, its processing is also a difficult problem, easily forms environmental pollution.(2) sulfuric acid of this intermediate concentration is applied to leaching, extraction and the production of valuable metal in ore, but this processing has certain regional limits, has limitation, a small amount of oil of mirbane simultaneously also existing in sulfuric acid, easily forms environmental pollution.
Summary of the invention
In sum, in order to address the above problem, the invention provides a kind of technique of producing oil of mirbane, described processing step is as follows:
A technique of producing oil of mirbane, is characterized in that, described technique comprises the steps:
Using benzene and gas nitrating agent as raw material anabolic reaction thing;
In microtubule Reactor inlet, place arranges volume pump, and the feed ratio of controlling described reactant is 1:1.01-1:1.1, and described feed ratio is mol ratio;
Its top hole pressure of the volume pump using in microtubule reactor is greater than 4bar, and the maximum that is still less than microtubule reactor is withstand voltage;
Described reactant is placed in microtubule reactor and carries out continuous flow reaction;
Temperature in described reaction process is controlled at 40 DEG C-80 DEG C;
The residence time 30s-4h of described reactant in microtubule reactor.
In the technique of described production oil of mirbane, the nitrating agent of gaseous phase can be NO
2, N
2o
5, N
2o
4, NO
2deng one or several;
In the technique of production oil of mirbane, the nitrating agent of described gaseous phase can be also NO
2, N
2o
5, N
2o
4, NO
2deng one or several and O wherein
3mixed gas.
In the technique of described production oil of mirbane, oxynitrides composition gas-liquid mixture contact reacts in microtubule reactor of described benzene and gaseous phase.
In the technique of described production oil of mirbane, described volume pump is ram pump or surge pump.
In the technique of described production oil of mirbane, in order to meet the required pressure of nitration reaction, described ram pump also can adopt the mode of multiple ram pump series connection, and described volume pump adopts the mode of many pump serial connections.
The invention has the beneficial effects as follows:
1, due to the present invention adopt be the nitrating agent of gaseous phase, therefore, reactant be easy to separate, can realize recycle;
2, the production equipment that the present invention adopts is microtubule reactor, and production equipment floor space is little, and the production capacity of unit device is large, and Production Flow Chart is short, and manipulation strength is little;
3, the energy consumption of microtubule reactor its energy consumption compared to traditional production production equipment used is lower;
4, the present invention's employing used be the oxynitrides of gaseous phase as nitrating agent, compared to traditional production, do not produce spent acid, therefore, environment is not polluted, also simplified production technique simultaneously, reduce energy consumption, reduced the production cost of oil of mirbane.
Embodiment
For describing technical scheme of the present invention in detail, and can realize according to the content of this specification sheets, below the invention will be further described.
By the NO of benzene and gaseous phase
2press feed ratio 1:1.01-1:1.1 as raw material anabolic reaction thing, described NO
2as nitrating agent, described feed ratio is mol ratio; The ram pump using in microtubule reactor is set, makes the top hole pressure of institute's ram pump be greater than 4bar, withstand voltage but the peak pressure of ram pump can not exceed the maximum of microtubule reactor.In order to meet pressure requirement, described ram pump also can adopt the mode of multiple ram pump series connection; Described benzene and the NO of gaseous phase
2continuous flow reaction in microtubule reactor; In reaction process, temperature is controlled at 40 DEG C-80 DEG C; The NO of described benzene and gaseous phase
2residence time 30s-4h in microtubule reactor.The technique of the production oil of mirbane described in the present embodiment, the oxynitrides of described gaseous phase is except the NO in the present embodiment
2also can adopt N outward,
2o
5, N
2o
4, NO
2deng one or several; Can also adopt NO
2, N
2o
5, N
2o
4, NO
2deng one or several and O wherein
3mixed gas; What in the present embodiment, adopt is ram pump, also can adopt surge pump.
Above embodiment is exemplary description; not the present invention is done to any pro forma restriction; if not departing from the scope of technical characterictic that the present invention carries, utilize disclosed technology contents to do the local equivalent embodiment that changes or modify, all still belong in the scope of protection of the invention.
Claims (6)
1. a technique of producing oil of mirbane, is characterized in that, described technique comprises the steps:
(1) using benzene and gas nitrating agent as raw material anabolic reaction thing;
(2) at microtubule Reactor inlet place, volume pump is set, the feed ratio of controlling described reactant is 1:1.01-1:1.1, and described feed ratio is mol ratio;
(3) its top hole pressure of volume pump using in microtubule reactor is greater than 4bar, and the maximum that is still less than microtubule reactor is withstand voltage;
(4) described reactant is placed in microtubule reactor and carries out continuous flow reaction;
(5) temperature in described reaction process is controlled at 40 DEG C-80 DEG C;
(6) residence time of described reactant in microtubule reactor is 30s-4h.
2. the technique of production oil of mirbane as claimed in claim 1, is characterized in that, described gas nitrating agent is NO
2, N
2o
5, N
2o
4, NO
2deng one or several.
3. the technique of production oil of mirbane as claimed in claim 1, is characterized in that: the nitrating agent of described gaseous phase is NO
2, N
2o
5, N
2o
4, NO
2deng one or several and O wherein
3mixed gas.
4. the technique of the production oil of mirbane as described in claim as arbitrary in claim 1-3, is characterized in that: described benzene reacts with the continuous flow in microtubule reactor of gas nitrating agent composition gas-liquid mixture.
5. the technique of production oil of mirbane as claimed in claim 1, is characterized in that: described volume pump is ram pump or surge pump.
6. the technique of the production oil of mirbane as described in claim 1 or 5, is characterized in that: described volume pump adopts the mode of many series connections of pumps.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310630771.4A CN103922940B (en) | 2013-12-02 | 2013-12-02 | A kind of technique of producing oil of mirbane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310630771.4A CN103922940B (en) | 2013-12-02 | 2013-12-02 | A kind of technique of producing oil of mirbane |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103922940A true CN103922940A (en) | 2014-07-16 |
| CN103922940B CN103922940B (en) | 2016-04-20 |
Family
ID=51141368
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310630771.4A Expired - Fee Related CN103922940B (en) | 2013-12-02 | 2013-12-02 | A kind of technique of producing oil of mirbane |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103922940B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109180539A (en) * | 2018-09-04 | 2019-01-11 | 浙江工业大学 | Pipelineization prepares the method and device of the chloro- 4- toluenesulfonic acid of 2- nitro -5- |
| CN109232257A (en) * | 2018-09-04 | 2019-01-18 | 浙江工业大学 | Pipeline prepares the method and device of methyl nitrobenzene |
| CN109369453A (en) * | 2018-09-04 | 2019-02-22 | 浙江工业大学 | Pipelineization prepares the method and device of the chloro- 5- nitrobenzonitrile of 2- |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0092372A1 (en) * | 1982-04-16 | 1983-10-26 | Sumitomo Chemical Company, Limited | Process for nitration of benzene |
| CN102432471A (en) * | 2011-11-07 | 2012-05-02 | 常州大学 | Method for undergoing chlorobenzene nitration reaction by using micro-channel reactor |
| CN102838489A (en) * | 2012-09-19 | 2012-12-26 | 辽宁庆阳特种化工有限公司 | Clean production method and device of dinitrotoluene |
-
2013
- 2013-12-02 CN CN201310630771.4A patent/CN103922940B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0092372A1 (en) * | 1982-04-16 | 1983-10-26 | Sumitomo Chemical Company, Limited | Process for nitration of benzene |
| CN102432471A (en) * | 2011-11-07 | 2012-05-02 | 常州大学 | Method for undergoing chlorobenzene nitration reaction by using micro-channel reactor |
| CN102838489A (en) * | 2012-09-19 | 2012-12-26 | 辽宁庆阳特种化工有限公司 | Clean production method and device of dinitrotoluene |
Non-Patent Citations (2)
| Title |
|---|
| 李斌: "微反应器技术在精细化工中的应用", 《精细化工》, vol. 23, no. 1, 31 January 2006 (2006-01-31), pages 1 - 7 * |
| 杨轶: "臭氧介质二氧化氮体系在绿色硝化技术中的应用", 《辽宁化工》, vol. 40, no. 7, 31 July 2011 (2011-07-31), pages 739 - 741 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109180539A (en) * | 2018-09-04 | 2019-01-11 | 浙江工业大学 | Pipelineization prepares the method and device of the chloro- 4- toluenesulfonic acid of 2- nitro -5- |
| CN109232257A (en) * | 2018-09-04 | 2019-01-18 | 浙江工业大学 | Pipeline prepares the method and device of methyl nitrobenzene |
| CN109369453A (en) * | 2018-09-04 | 2019-02-22 | 浙江工业大学 | Pipelineization prepares the method and device of the chloro- 5- nitrobenzonitrile of 2- |
| CN109232257B (en) * | 2018-09-04 | 2021-03-09 | 浙江工业大学 | Method and device for preparing methyl nitrobenzene in pipeline mode |
| CN109180539B (en) * | 2018-09-04 | 2021-03-23 | 浙江工业大学 | Method and device for preparing 2-nitro-5-chloro-4-methylbenzenesulfonic acid through pipelining |
| CN109369453B (en) * | 2018-09-04 | 2021-06-25 | 浙江工业大学 | Method and device for preparing 2-chloro-5-nitrobenzonitrile through pipelining |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103922940B (en) | 2016-04-20 |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CB03 | Change of inventor or designer information |
Inventor after: Liu Fengneng Inventor after: Liu Xiang Inventor after: Su Zhongxing Inventor after: Ma Anping Inventor before: Liu Fengneng Inventor before: Liu Xiang Inventor before: Su Zhongxing |
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