CN103570557B - Continuous still reaction produces method and the device of 3,4 dichlorphenamide bulk powders - Google Patents
Continuous still reaction produces method and the device of 3,4 dichlorphenamide bulk powders Download PDFInfo
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- CN103570557B CN103570557B CN201310550210.3A CN201310550210A CN103570557B CN 103570557 B CN103570557 B CN 103570557B CN 201310550210 A CN201310550210 A CN 201310550210A CN 103570557 B CN103570557 B CN 103570557B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
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Abstract
The invention belongs to chemical production field, particularly the continuous still reaction of one produces method and the device of 3,4 dichlorphenamide bulk powders.This continuous still reaction produces method and the device of 3,4 dichlorphenamide bulk powders, with 3,4-dichloronitrobenzene for raw material, it is characterized in that: 3,4-dichloronitrobenzene and methyl alcohol enter reactor a continuously respectively by nitro compounds pump and methanol pump; There is catalytic hydrogenation reaction in 3,4-dichloronitrobenzene, generate 3,4-DCA under the effect of catalyzer, anti-dechlorinating agent; The pressure of reactor a is 0.8 ~ 0.95MPa, and temperature is 60 ~ 70 DEG C; Material utilize the high potential difference between each reactor successively overflow enter reactor b and reactor c, finally enter in subsider and be separated decaying catalyst; Non-decaying catalyst reenters reactor a recycle, and decaying catalyst strainer reclaims, and final product enters the storage of product groove.The present invention is applicable to large-scale commercial production, easily automatically controls, simple to operate, saves manpower, and stablizes, operational safety, be suitable for wide popularization and application.
Description
Technical field
The invention belongs to chemical production field, particularly the continuous still reaction of one produces method and the device of 3,4 dichlorphenamide bulk powders.
Background technology
3,4-DCA is the intermediate of multiple dyestuff, pigment, medicine, agricultural chemicals and fine chemical product.The production method of 3,4-DCA has iron reduction method and catalytic hydrogenating reduction method.It is a kind of eco-friendly production technique that catalytic hydrogenating reduction method produces 3,4-DCA, has reduction reaction time short, the advantage such as temperature is low, pressure is low.At present, catalytic hydrogenating reduction method production 3,4-DCA adopts batch tank to produce mostly.
Need in batch tank production process to carry out the non-productive operation such as charging and discharging, easily cause the loss of material and energy, improve production cost, extend the production cycle, and quality product is not easily stablized.Particularly conventional at present catalytic hydrogenating reduction method need of production uses volatile organic solvent, and batch tank produces the volatilization easily causing poisonous, inflammable, explosive solvent, causes certain influence to HUMAN HEALTH and safety in production.Batch tank is produced and is not suitable for being applied to scale operation.
Summary of the invention
The present invention, in order to make up the defect of prior art, provides method and the device of continuous still reaction production 3,4 dichlorphenamide bulk powders that a kind of technological operation is simple, production cost is low.
The present invention is achieved through the following technical solutions:
A kind of still reaction continuously produces the method for 3,4 dichlorphenamide bulk powders, with 3,4-dichloronitrobenzene is raw material, it is characterized in that: 3,4-dichloronitrobenzene and methyl alcohol 1:2 in mass ratio, respectively by nitro compounds pump and methanol pump pressure-raising to 1.5MPa, and enter reactor a continuously; There is catalytic hydrogenation reaction in 3,4-dichloronitrobenzene, generate 3,4-DCA under the effect of catalyzer, anti-dechlorinating agent; The pressure of reactor a is 0.8 ~ 0.95MPa, and temperature is 60 ~ 70 DEG C; Material utilize the high potential difference between each reactor successively overflow enter reactor b and reactor c, finally enter in subsider and be separated decaying catalyst; Non-decaying catalyst reenters reactor a recycle, and decaying catalyst strainer reclaims, and final product enters the storage of product groove.
Described catalyzer and the charging before 3,4-dichloronitrobenzene and methanol feeding of anti-dechlorinating agent, add-on is 1% ~ 5% of 3,4-dichloronitrobenzene quality.
Continuous still reaction of the present invention produces 3, the device of 4 dichlorphenamide bulk powders, it is characterized in that: comprise nitro compounds pump and methanol pump, nitro compounds pump and methanol pump are all connected with reactor a, reactor a, reactor b and reactor c connect mutually, reactor c outlet is connected with subsider, and subsider top is connected with strainer, and strainer lower part outlet is connected with product groove.
Described reactor a, reactor b and reactor c are provided with whipping appts, external jacket and inner coil pipe; Whipping appts can improve hydrogenation reaction speed, and external jacket and inner coil pipe then can realize the heating and cooling to material, guarantees to react safe operation.
Described reactor a, reactor b and reactor c level attitude reduce 8% ~ 25% of each reactor oneself height successively.
Be provided with the Venturi squirt pump being communicated with methanol feeding pipe below described subsider, non-decaying catalyst by Venturi squirt pump with entering hydriding reactor a after methanol mixed.
Described reactor a, reactor b, reactor c and subsider top are provided with pressure equalizing pipe, each reactor pressure is consistent, thus reaches the object of continuous hydrogenation.
Described strainer adopts material to be 316L metal agglomeration filter core, is provided with automatic back blow and press dry and automatic clinker-removing device, all can reclaim catalyzer, alleviate labor intensity, reduces catalyst consumption; Filtering accuracy is 0.1 μm, and decaying catalyst can all retain.
The invention has the beneficial effects as follows: present invention achieves 3, the high efficiente callback of 4 dichloronitrobenzene by-product hydrochloric acids utilizes, and technological operation is simple, automatic control level is high, to the impurity existed in dusty gas and p-Nitrophenyl chloride treatment effect good, be suitable for wide popularization and application.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the present invention is further illustrated.
Accompanying drawing 1 is structural representation of the present invention;
In figure, 1 reactor a, 2 reactor b, 3 reactor c, 4 subsiders, 5 strainers, 6 methanol pump, 7 nitro compounds pumps, 8 Venturi squirt pumps, 9 external jackets, 10 inner coil pipes, 11 whipping apptss, 12 pan tanks, 13 pressure equalizing pipes, 14 methanol feeding pipes.
Embodiment
Accompanying drawing is a kind of specific embodiment of the present invention.Continuous still reaction of the present invention produces the device of 3,4 dichlorphenamide bulk powders, and comprise nitro compounds pump 7 and methanol pump 6, nitro compounds pump 7 is all connected with reactor a1 with methanol pump 6; Reactor a1, reactor b2 and reactor c3 connect mutually, and its level attitude reduces 13% of each reactor oneself height successively; Reactor c3 outlet is connected with subsider 4, and reactor a1, reactor b2, reactor c3 and subsider 4 top are provided with pressure equalizing pipe 13; Subsider 4 top is connected with strainer 5, and strainer 5 lower part outlet is connected with product groove 12; The Venturi squirt pump 8 being communicated with methanol feeding pipe 14 is provided with below subsider 4.
Described reactor a1, reactor b2 and reactor c3 are provided with whipping appts 11, external jacket 9 and inner coil pipe 10; Whipping appts 11 can improve hydrogenation reaction speed, and external jacket 9 and inner coil pipe 10 then can realize the heating and cooling to material, guarantees to react safe operation.
Described strainer 5 adopts material to be 316L metal agglomeration filter core, is provided with automatic back blow and press dry and automatic clinker-removing device, all can reclaim catalyzer, alleviate labor intensity, reduces catalyst consumption; Filtering accuracy is 0.1 μm, and decaying catalyst can all retain.
3,4-dichloronitrobenzene and methyl alcohol 1:2 in mass ratio, respectively by nitro compounds pump 7 and methanol pump 6 pressure-raising to 1.5MPa, then enters reactor a1 continuously.Catalyzer and the charging before 3,4-dichloronitrobenzene and methanol feeding of anti-dechlorinating agent, add-on is 3% of 3,4-dichloronitrobenzene quality.There is catalytic hydrogenation reaction in 3,4-dichloronitrobenzene, generate 3,4-DCA under the effect of catalyzer, anti-dechlorinating agent.Pressure in reactor a1 is 0.9MPa, and temperature is 66 DEG C.Material utilize the high potential difference between each reactor successively overflow enter reactor b2 and reactor c3, finally enter in subsider 4 and be separated decaying catalyst, pressure equalizing pipe 13 can make the pressure of each reactor and subsider 4 be consistent, thus reaches the object of continuous hydrogenation.The principle that subsider 4 adopts gravity settling and centrifugal settling to combine, namely mixed solution enters the eddy current producing and rotate from the side, in uphill process, rely on gravity and subsider 4 top overflow separator tank to carry out separate and subside to non-decaying catalyst, decaying catalyst tiny on a small quantity enters subsider 4 top separator tank.Non-decaying catalyst is by Venturi squirt pump 8 with entering hydriding reactor a1 recycle after methanol mixed, decaying catalyst strainer 5 reclaims, and final product enters product groove 12 and stores.
Claims (5)
1. the method for continuous still reaction production 3,4 dichlorphenamide bulk powders, with 3,4-dichloronitrobenzene is raw material, it is characterized in that: 3,4-dichloronitrobenzene and methyl alcohol 1:2 in mass ratio, respectively by nitro compounds pump (7) and methanol pump (6) pressure-raising to 1.5MPa, and enter reactor a(1 continuously); There is catalytic hydrogenation reaction in 3,4-dichloronitrobenzene, generate 3,4-DCA under the effect of catalyzer, anti-dechlorinating agent; Described catalyzer and the charging before 3,4-dichloronitrobenzene and methanol feeding of anti-dechlorinating agent, add-on is 1% ~ 5% of 3,4-dichloronitrobenzene quality, reactor a(1) pressure be 0.8 ~ 0.95MPa, temperature is 60 ~ 70 DEG C; Material utilize the high potential difference between each reactor successively overflow enter reactor b(2) and reactor c(3), finally enter in subsider (4) and be separated decaying catalyst; Non-decaying catalyst reenters reactor a(1) recycle, decaying catalyst strainer (5) reclaims, and final product enters product groove (12) storage.
2. continuous still reaction according to claim 1 produces 3, the device of 4 dichlorphenamide bulk powders, it is characterized in that: comprise nitro compounds pump (7) and methanol pump (6), nitro compounds pump (7) and methanol pump (6) all with reactor a(1) be connected, reactor a(1), reactor b(2) and reactor c(3) mutually connect, reactor c(3) outlet be connected with subsider (4), subsider (4) top is connected with strainer (5), strainer (5) lower part outlet is connected with product groove (12), described reactor a(1), reactor b(2), reactor c(3) be provided with pressure equalizing pipe (13) with subsider (4) top, described reactor a(1), reactor b(2) and reactor c(3) be provided with external jacket (9), inner coil pipe (10) and whipping appts (11).
3. continuous still reaction according to claim 2 produces the device of 3,4 dichlorphenamide bulk powders, it is characterized in that: described reactor a(1), reactor b(2) with reactor c(3) level attitude reduces 8% ~ 25% of each reactor oneself height successively.
4. continuous still reaction according to claim 2 produces the device of 3,4 dichlorphenamide bulk powders, it is characterized in that: described subsider (4) below is provided with the Venturi squirt pump (8) being communicated with methanol feeding pipe (14).
5. continuous still reaction according to claim 2 produces the device of 3,4 dichlorphenamide bulk powders, it is characterized in that: described strainer (5) adopts material to be 316L metal agglomeration filter core, and be provided with automatic back blow and press dry and automatic clinker-removing device, filtering accuracy is 0.1 μm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310550210.3A CN103570557B (en) | 2013-11-08 | 2013-11-08 | Continuous still reaction produces method and the device of 3,4 dichlorphenamide bulk powders |
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| CN201310550210.3A CN103570557B (en) | 2013-11-08 | 2013-11-08 | Continuous still reaction produces method and the device of 3,4 dichlorphenamide bulk powders |
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| CN103570557A CN103570557A (en) | 2014-02-12 |
| CN103570557B true CN103570557B (en) | 2015-10-28 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105418433A (en) * | 2015-11-17 | 2016-03-23 | 山东沾化天九化工有限公司 | Method and device for producing 3,4-dichloronitrobenzene through continuous kettle type reaction |
| CN108658791A (en) * | 2017-03-31 | 2018-10-16 | 北京颖泰嘉和生物科技股份有限公司 | The device and method of continuous autoclave production amidogen ether |
| CN107138101A (en) * | 2017-06-27 | 2017-09-08 | 查都（上海）科技有限公司 | A kind of system of acetylene and formaldehyde deep reaction |
| CN114917836B (en) * | 2021-07-23 | 2023-07-14 | 南通江山农药化工股份有限公司 | Hydrogenation kettle non-pressure-relief hydrogenation device and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103342650A (en) * | 2013-07-30 | 2013-10-09 | 青岛科技大学 | Method for continuously producing 3,4-dichloroaniline |
| CN103360265A (en) * | 2012-04-06 | 2013-10-23 | 浙江龙盛化工研究有限公司 | Method for continuous hydrogenation of dinitrobenzene and recycling of reaction heat thereof |
| CN203866230U (en) * | 2013-11-08 | 2014-10-08 | 山东沾化天九化工有限公司 | Device for producing 3, 4-dichloroaniline through continuous kettle reaction |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103360265A (en) * | 2012-04-06 | 2013-10-23 | 浙江龙盛化工研究有限公司 | Method for continuous hydrogenation of dinitrobenzene and recycling of reaction heat thereof |
| CN103342650A (en) * | 2013-07-30 | 2013-10-09 | 青岛科技大学 | Method for continuously producing 3,4-dichloroaniline |
| CN203866230U (en) * | 2013-11-08 | 2014-10-08 | 山东沾化天九化工有限公司 | Device for producing 3, 4-dichloroaniline through continuous kettle reaction |
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Effective date of registration: 20201119 Address after: No. 169, Jieyong Road, Lunan high tech chemical industry park, Mushi Town, Tengzhou City, Zaozhuang City, Shandong Province Patentee after: Shandong zhennuo Chemical Co., Ltd Address before: 256800 Chengbei Industrial Zone, Zhanhua County, Shandong, Binzhou Patentee before: SHANDONG ZHANHUA TIANJIU CHEMICAL Co.,Ltd. |
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