CN102675127A - Method and device for preparing 3,4-dichloroaniline without solvent - Google Patents
Method and device for preparing 3,4-dichloroaniline without solvent Download PDFInfo
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- CN102675127A CN102675127A CN2012101657558A CN201210165755A CN102675127A CN 102675127 A CN102675127 A CN 102675127A CN 2012101657558 A CN2012101657558 A CN 2012101657558A CN 201210165755 A CN201210165755 A CN 201210165755A CN 102675127 A CN102675127 A CN 102675127A
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Abstract
The invention belongs to the field of chemical processing, and particularly discloses a method and a device for preparing 3,4-dichloroaniline without solvent. The method includes using 3,4-dichloronitrobenzene as a raw material, adding an assistant and a novel catalyst into the 3,4-dichloronitrobenzene, feeding hydrogen into a hydrogenation kettle to react continuously under certain pressure and at certain temperature, and collecting reacted hydrogenated liquid into a hydrogenated liquid tank via a filter; and blowing a filtered catalyst into the hydrogenation kettle to be reused via the filter. The method and the device have the advantages that a process is simple in operation, production cost is low, automatic control degree is high, yield of product is also high, quality is good, side reaction is little, reaction conditions are moderate, security is guaranteed, labor intensity of workers is low, and the method and the device are suitable for wide popularization and application.
Description
(1) technical field
The invention belongs to chemical production field, particularly a kind of solvent-free production 3, the method for 4-dichlorphenamide bulk powder and device.
(2) background technology
Along with reform and opening-up; National economy develops rapidly, and fine chemistry industry industries such as medicine, fuel, agricultural chemicals, daily-use chemical industry have quantitatively ranked among great powers in the world's ranks in scale, but still there are bigger gap in state of the art and developed country; Quality product is not high; Material consumption and energy consumption are higher, and particularly disposal of three wastes imperfection has seriously restricted further developing of fine chemistry industry.China's shortening technology had all had important breakthrough in technological development with promoting the use of in recent years, and the shortening technology not only is widely used in petrochemical complex, refining of petroleum, on fine chemistry industry, has also obtained continually developing and using.
At present; The many enterprises of China still generally adopt method of reducing such as the iron powder, Sodium Sulphide, Hydrazine Hydrate 80 in five sixties and hydrogenating reduction method tissue to produce on Aniline Production, and the former progressively eliminates because of seriously polluted at present, and latter's production technique is more advanced; But use methyl alcohol etc. makes to need in the solvent reaction process to drip the nitro thing; Through reaction color control reaction effect, often occur judging the inaccurate phenomenon that influences reaction effect because of color, influence the lifting of single still load; Have methyl alcohol, hydrogen existence and working pressure to increase at the above operational safety coefficient of 1.0Mpa in addition in the reaction kettle, reaction back end hydrogenation liquid need propose methyl alcohol through rectifying tower, causes consuming cost to increase.
(3) summary of the invention
The present invention provides the solvent-free production 3 that a kind of technological operation is simple, production cost is low, the method and apparatus of 4-dichlorphenamide bulk powder in order to remedy the deficiency of prior art.
The present invention realizes through following technical scheme:
A kind of solvent-free production 3, the method for 4-dichlorphenamide bulk powder is with 3; The 4-dichloronitrobenzene is a raw material; It is characterized in that: 3, interpolation morpholine and parts by weight are 1% platinum carbon catalyst in the 4-dichloronitrobenzene, under 0.5 ~ 0.7M pressure, 95 ~ 105 ℃ of temperature, feed hydrogen successive reaction in the hydrogenation still; Reacted hydride is collected in the hydrogenation liquid bath through strainer, and the catalyzer after the filtration gets into the hydrogenation still through the strainer blowback and reuses.
Behind the catalyzer of the present invention remodeling, intensity is higher, can be because of reaction kettle stirring problem does not cause catalyst loss, prolong catalyzer work-ing life, and in catalytic reaction process, except that producing product and water, can not produce other by products, have excellent economy; Reactant need not to add solvent, reduces and utilizes the space because of solvent takies the hydrogenation still, improves the reaction kettle utilization ratio; New catalyst and production technique can not saved the solvent distillation device because of boring concentration just influences catalyst activity simultaneously.
More excellent scheme of the present invention is:
For preventing to occur the dechlorination phenomenon in the reaction process, said hydrogenation still to wherein adding anti-dechlorination suppressor factor, is guaranteed to react back end hydrogenation liquid dechlorination amount and is controlled at below the per mille before feeding intake, and solves in the reaction process and causes corrosion on Equipment because of serious dechlorination.
The filtration of said strainer and regeneration are all carried out under pressure-fired, use hydrogen that the blowback of strainer inner catalyst is reused to hydrogenation still bottom, reduce hydrogen consumption.
Solvent-free production 3 of the present invention, the device of 4-dichlorphenamide bulk powder comprises the magnetic force hydrogenation still that is communicated with the hydrogen inlet pipe, and hydrogenation still, hydrogen inlet pipe all are communicated with strainer, and strainer is communicated with subsider.
The pipeline visor is installed on the connecting pipe of said strainer and subsider, is convenient in time grasp the situation of pipeline inner fluid, reach the purpose of timely feedback response information.
Said hydrogenation still bottom is equipped with thief hole, is convenient to sample circuit and discharges waste material at the bottom of the still.
Said filter element is a metal powder sintered filter element, and filter type is the chimney filter inner filtration, has solved the problem that exists of filtering.
Technological operation of the present invention is simple, production cost is low, and the automatic control level is high, and product yield is high, quality is good, side reaction seldom, reaction conditions is gentle, security is protected, labor strength is low, is suitable for wide popularization and application.
(4) description of drawings
Below in conjunction with accompanying drawing the present invention is further described.
Fig. 1 is a structural representation of the present invention.
Among the figure, 1 hydrogenation still, 2 strainers, 3 subsiders, 4 pipeline visors, 5 hydrogen inlet pipes, 6 thief holes.
(5) embodiment
Fig. 1 is a kind of specific embodiment of the present invention.This embodiment comprises the magnetic force hydrogenation still 1 that is communicated with hydrogen inlet pipe 5, and hydrogenation still 1, hydrogen inlet pipe 5 all are communicated with strainer 2, and strainer 2 is communicated with subsider 3; On the connecting pipe of said strainer 2 and subsider 3 pipeline visor 4 is installed; Said hydrogenation still 1 bottom is equipped with thief hole 6.
Before feeding intake; In hydrogenation still 1, add anti-dechlorination suppressor factor, in hydrogenation still 1, throw in 3 then, 4-dichloronitrobenzene, morpholine and parts by weight are 1% platinum carbon catalyst; Under certain pressure and temperature, feed hydrogen; Successive reaction in the hydrogenation still, the qualified back of hydrogenation mixed solution is through strainer 2 filtering catalysts, and filtrate is further confirmed the catalyst filtration effect through pipeline visor 4; Qualified filtered liq gets into subsider 3 and carries out branch water, and the catalyzer after the filtration gets into hydrogenation still 1 through strainer 2 blowbacks and reuses; The filtration of said strainer 2 and regeneration are all carried out under pressure-fired.
Claims (7)
1. solvent-free production 3; The method of 4-dichlorphenamide bulk powder, with 3, the 4-dichloronitrobenzene is a raw material; It is characterized in that:: 3; Interpolation morpholine and parts by weight are 1% platinum carbon catalyst in the 4-dichloronitrobenzene, under 0.5 ~ 0.7M pressure, 95 ~ 105 ℃ of temperature, feed hydrogen successive reaction in the hydrogenation still, and reacted hydride is collected in the hydrogenation liquid bath through strainer; Catalyzer after the filtration gets into the hydrogenation still through the strainer blowback and reuses.
2. solvent-free production 3 according to claim 1, the method for 4-dichlorphenamide bulk powder is characterized in that: said hydrogenation still is before feeding intake, to wherein adding anti-dechlorination suppressor factor.
3. solvent-free production 3 according to claim 1, the method for 4-dichlorphenamide bulk powder is characterized in that: the filtration of said strainer and regeneration are all carried out under pressure-fired.
4. solvent-free production 3 according to claim 1; The device of 4-dichlorphenamide bulk powder; It is characterized in that: comprise the magnetic force hydrogenation still (1) that is communicated with hydrogen inlet pipe (5), hydrogenation still (1), hydrogen inlet pipe (5) all are communicated with strainer (2), and strainer (2) is communicated with subsider (3).
5. solvent-free production 3 according to claim 4, the device of 4-dichlorphenamide bulk powder is characterized in that: on the connecting pipe of said strainer (2) and subsider (3) pipeline visor (4) is installed.
6. solvent-free production 3 according to claim 4, the device of 4-dichlorphenamide bulk powder is characterized in that: said hydrogenation still (1) bottom is equipped with thief hole (6).
7. solvent-free production 3 according to claim 4, the device of 4-dichlorphenamide bulk powder is characterized in that: said filter element (2) is a metal powder sintered filter element, and filter type is the chimney filter inner filtration.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101657558A CN102675127A (en) | 2012-05-25 | 2012-05-25 | Method and device for preparing 3,4-dichloroaniline without solvent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101657558A CN102675127A (en) | 2012-05-25 | 2012-05-25 | Method and device for preparing 3,4-dichloroaniline without solvent |
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| CN102675127A true CN102675127A (en) | 2012-09-19 |
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| CN2012101657558A Pending CN102675127A (en) | 2012-05-25 | 2012-05-25 | Method and device for preparing 3,4-dichloroaniline without solvent |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103113233A (en) * | 2013-01-11 | 2013-05-22 | 山东富原化工有限公司 | Production method for preparing chlorinated aniline via chlorination of nitrobenzene hydrogenation by utilizing solvent-free process |
| CN103387498A (en) * | 2013-07-20 | 2013-11-13 | 王一如 | Method and device for producing o-chloroaniline without solvent |
| CN103694124A (en) * | 2012-09-28 | 2014-04-02 | 中国石油化工股份有限公司 | Method for high-selectivity preparation of 3,4-dichloroaniline |
| CN105330548A (en) * | 2015-10-20 | 2016-02-17 | 安徽广信农化股份有限公司 | Diuron-intermediate production waste residue treatment technology |
| CN108911991A (en) * | 2018-08-17 | 2018-11-30 | 济南和润化工科技有限公司 | A kind of method of solvent-free catalytic hydrogenation production 2,3,4- trifluoromethyl aniline |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103694124A (en) * | 2012-09-28 | 2014-04-02 | 中国石油化工股份有限公司 | Method for high-selectivity preparation of 3,4-dichloroaniline |
| CN103113233A (en) * | 2013-01-11 | 2013-05-22 | 山东富原化工有限公司 | Production method for preparing chlorinated aniline via chlorination of nitrobenzene hydrogenation by utilizing solvent-free process |
| CN103387498A (en) * | 2013-07-20 | 2013-11-13 | 王一如 | Method and device for producing o-chloroaniline without solvent |
| CN105330548A (en) * | 2015-10-20 | 2016-02-17 | 安徽广信农化股份有限公司 | Diuron-intermediate production waste residue treatment technology |
| CN108911991A (en) * | 2018-08-17 | 2018-11-30 | 济南和润化工科技有限公司 | A kind of method of solvent-free catalytic hydrogenation production 2,3,4- trifluoromethyl aniline |
| CN108911991B (en) * | 2018-08-17 | 2021-03-23 | 济宁市金泰利华化工科技有限公司 | Method for producing 2,3, 4-trifluoroaniline by solvent-free catalytic hydrogenation method |
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Application publication date: 20120919 |