CN103044261A - Safe production method of nitro-compound - Google Patents
Safe production method of nitro-compound Download PDFInfo
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- CN103044261A CN103044261A CN2013100199133A CN201310019913A CN103044261A CN 103044261 A CN103044261 A CN 103044261A CN 2013100199133 A CN2013100199133 A CN 2013100199133A CN 201310019913 A CN201310019913 A CN 201310019913A CN 103044261 A CN103044261 A CN 103044261A
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Abstract
The invention provides a production method of nitro-compound. The production method comprises the steps of: continuously feeding a mixed acid solution from a heavy-phase inlet of a first centrifugal extraction separation device of a nitration separation system disclosed by the invention, and continuously feeding a raw material to be nitrified from a light-phase inlet of a final centrifugal extraction separation device at the same time, wherein the reaction temperature inside each centrifugal extraction separation device is controlled at 10-160 DEG C, and the rotating speed of each centrifugal extraction separation device is controlled at 800-2000 r/min; after multi-stage continuous nitration reaction, discharging final coarse nitride from a light-phase outlet of the first centrifugal extraction separation device, and discharging final waste acid from a heavy-phase outlet of the final centrifugal extraction separation device; and carrying out common alkali washing and water washing on the coarse nitride, and distilling the coarse nitride to obtain the refined nitro-compound product. According to the method disclosed by the invention, the nitration reaction is continuously carried out; the device is compact, easy to achieve automatic control, large in operation elasticity, and high in production efficiency; and as the reaction product and the waste acid are separated from each other at the same time inside the same reactor, the contact time of the reaction product and the waste acid is greatly shortened, side reaction is effectively avoided, energy consumption and material consumption are greatly reduced, and the security of the nitration reaction process is fundamentally ensured.
Description
Technical field
The invention belongs to hydrocarbon compound and nitric acid and under the effect of an acidic catalyst, carry out nitration reaction, the technical field of nitric acid synthesis based compound, what be specifically related to is production equipment and the production method that a kind of nitration reaction is produced nitro-compound.
Background technology
Nitration reaction is particularly to introduce the chemical reaction that nitro generates nitro-compound in the arene compounds to hydrocarbon compound, and the purposes of nitro-compound is very extensive.The nitro compound the production of material all adopts the method production take nitration mixture as nitrating agent for a long time.At first in nitrator, carry out nitration reaction, then with thick nitration product with nitrated after spent acid separate, thick nitration product obtains nitrated product through washing, alkali cleaning.Whether nitration reaction is divided into intermittently nitrated and continuous nitrification continuously by production process, whether takes out nitration reaction heat by reaction process and is divided into the nitrated and adiabatic nitration of heat-obtaining.No matter be intermittently nitrated or continuous nitrification, heat-obtaining is nitrated or adiabatic nitration, the used reactor of nitration reaction Industrial processes mainly is the kettle type nitrating reactor with whipping appts at present.When kettle type nitrating reactor is used for heat-obtaining nitration reaction production process, its heat transmission is mainly undertaken by the still external jacket, need when the kettle type nitrating reactor chuck can not meet the demands that heat transfer coils is set and increase heat transfer area in still, setting up heat transfer coils makes stirrer diameter be forced to reduce, weakened mixed effect, reduced heat transfer coefficient, therefore kettle type nitrating reactor overall heat transfer poor effect; When kettle type nitrating reactor was used for intermittently nitration reaction, the general employing dripped charging, and it is inhomogeneous that concentration distribution can appear in local superheating and the still in the charging position, and then caused the not high and throughput of quality product to be restricted; When kettle type nitrating reactor is used for the continuous nitrification reaction process, need to adopt many stills series connection, material residence time in still is uneven, and production process is itrated compound and to cross itrated compound wayward not, and production process is complicated; Material stock is many in the kettle type nitrating reactor, in case it is greatly destructive to blast.
Chinese patent CN102432410A and Chinese patent CN1789235A have proposed a kind of tubular type nitrator, with static mixer as nitrator, make nitration mixture and treat that nitrated raw material flows at the tubular reactor inner edge, mix on the limit, the limit reaction, conduct heat in the limit, although this nitrator has certain progress than kettle type nitrating reactor, but its reaction mass is the same side from tubular reactor to be entered and jointly flows out from opposite side, along with the carrying out of flowing and reacting, reaction mass is far away apart from material inlet, the concentration of reactant is lower and concentration product is higher, the impellent of reaction is less, might cause reaction to be carried out thoroughly or causes the side reaction odds to increase; Reacting in addition also needs after complete special separating device with nitration product and spent acid separately, the operation relative complex.
Summary of the invention
The object of the invention is to propose a kind of nitration reaction method, the method not only has very high yield, and the conversion process of reaction and the sepn process of reacted product and spent acid are finished in same reactor simultaneously, method of the present invention is aided with the automatic continuous production that DCS can realize nitro-compound.
Above-mentioned purpose of the present invention is achieved through the following technical solutions:
At first, a kind of multistage nitration reaction separation system for the nitro compound the production of material is provided, it is the multistage continuous nitration reaction separation system that is made of the series connection of the Centrifugical extraction separating device more than 2, the heavy out of every Centrifugical extraction separating device connects the heavy liquid inlet of next Centrifugical extraction separating device, and the light phase entrance of every Centrifugical extraction separating device connects the light phase export of next Centrifugical extraction separating device; Each gangway that links to each other connects by pipeline.
In the multistage nitration reaction separation system of the present invention, the Centrifugical extraction separating device that is in the series devices two ends can relatively be called the first, last platform mutually, namely when wherein the equipment of an end is called " first Centrifugical extraction separating device ", the equipment of the other end then is called as " last platform Centrifugical extraction separating device ", and vice versa.
Described multistage nitration reaction separation system preferably is made of the series connection of 2-4 platform Centrifugical extraction separating device; Most preferably consisted of by 4 Centrifugical extraction separating device series connection.
Centrifugal extraction equipment described in the inventive method can be that commercially available various Centrifugical extraction separators, centrifugal extractor or other can be called by those skilled in the art the mechanical means of " Centrifugical extraction separating device ", disclosed centrifugal extraction equipment among the HL-125 centrifugal extractor of Beijing extraction application technical institute development, U.S. CINC V2 multifunctional centrifugal separating and extracting device, Chinese patent literature CN201949682U, the CN200977420Y for example, etc.
On this basis, the present invention also provides a kind of production method of nitro-compound, may further comprise the steps:
1) make the mixed acid solution Accessory Right that contains sulfuric acid and nitric acid require the heavy liquid inlet continuously feeding of first Centrifugical extraction separating device of 1 described multistage nitration reaction separation system, treat that simultaneously nitrated raw material is from the light phase entrance continuously feeding of last platform Centrifugical extraction separating device, control the interior temperature of reaction of every Centrifugical extraction separating device at 10～160 ℃, and the rotating speed of control Centrifugical extraction separating device is at 800-2000 rev/min; In every Centrifugical extraction separating device, under the effect of centrifugal force, finish simultaneously nitration reaction and and react rear thick itrated compound and remain separating of nitration mixture, thick itrated compound after the separation is discharged from through the light phase export of every Centrifugical extraction separating device, and again enter the upper level of nitration reaction separation system through the light phase entrance of a upper Centrifugical extraction separating device, nitration mixture after separating then flows out through the heavy out of every Centrifugical extraction separating device, and enters the next stage of nitration reaction separation system through the heavy liquid inlet of next Centrifugical extraction separating device;
2) after the multistage continuous nitration reaction of step 1), discharge final thick itrated compound from the light phase export of first Centrifugical extraction separating device, from the final spent acid of heavy out outflow of last platform Centrifugical extraction separating device; With thick itrated compound through conventional alkali cleaning and the washing after, the nitro-compound product that obtains making with extra care through rectifying again.
Described nitrated raw material preferred aromatic hydrocarbons or the polyvalent alcohol treated of step 1).
Described aromatic hydrocarbons is benzene, toluene or chlorobenzene more preferably;
The further preferred glycerol of described polyvalent alcohol or BT.
The described mixed acid solution of step 1) by weight percentage, preferably contains the sulfuric acid of 20-80% and the nitric acid of 2-40%, and surplus is water.
Temperature of reaction in the described Centrifugical extraction separating device of step 1) preferably is controlled at 15-150 ℃.
The rotating speed of the described Centrifugical extraction separating device of step 1) preferably is controlled at 1000-1800 rev/min.
Step 2) spent acid of described last platform Centrifugical extraction separating device outflow is preferably prepared nitration mixture for step 1) as raw material again after concentrated.
The production method of nitro-compound of the present invention both had been applicable to the nitrated and adiabatic nitration of heat-obtaining, also was applicable to nitric acid excessive or treat the reaction that itrated compound is excessive.Two kinds of reactants mix continuously, react, conduct heat, separate in nitration reaction separation system of the present invention, thereby have obtained high yield and effect cheaply.Compare with the technique of tubular type nitrator with using kettle type nitrating reactor in the prior art, the present invention has advantages of following concrete:
1, method of the present invention selects centrifugal extraction equipment as the nitration reaction separator, the nitration reaction thing can mix moment because its unique structure and centrifugal action make, moment separates, contact fully and evenly, and the quick effective separation of reacted spent acid and the thick itrated compound of purpose product, in the whole process material duration of contact short, sufficient reacting, avoid side reaction that Long Term Contact causes and the decomposition reaction of product, guaranteed quality, improved yield.
2, compare with traditional tank reactor, the present invention as reactor, dwindles the size of reactor with centrifugal extractor greatly, in the situation that identical production capacity, the material amount of holding of inside reactor of the present invention only has traditional reactor to hold the 0.6-1% of material amount.Less holds the material amount so that the hazard level of reactive system reduces greatly, and meet with catastrophic failure (as have a power failure, cut off the water, the miscellaneous equipment fault) time the rapid intrasystem material of emptying, the generation of having stopped the security incidents such as material spray, blast.
3, adopt static mixing different from the tubular type nitrator, the nitration reaction separator among the present invention is because have whipping appts so that reactant can be more rapidly, mix fully, and then so that nitration reaction can carry out sooner; Compare with tubular type nitrator following current technique, nitration reaction separator internal reaction material nitration mixture of the present invention and treat that nitrated material is counter current contact, all keep the reaction density of maximum poor when reaction mass contacts in the nitration reaction separator everywhere, thereby nitration reaction to carry out ground rapider more thorough, side reaction is still less; Need other outfit product separation equipment different from the tubular type nitrator, nitration reaction separator of the present invention has possessed the function of product separation simultaneously, has simplified operation, has saved investment.
4, among the present invention, centrifugal extractor is as the application of nitration reaction separator, so that start time and the idle time of producing become very short, so not only reduced pending amount with treating the aftertreatment material, also reduced start and stop transport during technological fluctuation, and then reduced quality and security risk.
5, method of the present invention can be aided with at an easy rate DCS and realizes that automatization controls, and reduces manning.
6, among the present invention take centrifugal extractor as the nitration reaction separator increase so that conversion unit is controlled the scope of adjusting, throughput can be regulated arbitrarily between 20-100%.
7, method of the present invention both had been applicable to the nitrated and adiabatic nitration of heat-obtaining also to be applicable to nitric acid excessive or treat the reaction that itrated compound is excessive.
Description of drawings
Fig. 1 is the schematic flow sheet of the production method of nitro compounds described in the specific embodiment of the invention.
Among Fig. 1: 1 is the nitration mixture basin, 2 for treating the itrated compound basin, 3 is the nitration mixture volume pump, 4 for treating the itrated compound volume pump, 5 is the nitration mixture interchanger, and 6 for treating the itrated compound interchanger, and 7,8,9,10 are nitration reaction separator (being the Centrifugical extraction separating device), and platform Centrifugical extraction separating device headed by 7,10 is last platform Centrifugical extraction separating device.
Embodiment
Technical solution of the present invention can be carried out according to following embodiment:
1) as shown in Figure 1, with 4 Centrifugical extraction separating device series connection, form multistage continuous nitration reaction separation system, series system is the heavy liquid inlet that the heavy out of every Centrifugical extraction separating device connects next Centrifugical extraction separating device, and the light phase entrance of every Centrifugical extraction separating device connects the light phase export of next Centrifugical extraction separating device; Each gangway that links to each other connects by pipeline; From the nitration mixture of nitration mixture basin 1 with nitration mixture volume pump 3 by the heavy liquid inlet continuously feeding by first Centrifugical extraction separating device 7 through 5 heating of nitration mixture interchanger or after being cooled to suitable temp of certain flow, meanwhile until itrated compound from until itrated compound basin 2 usefulness until itrated compound volume pump 4 by certain flow through until 6 heating of itrated compound interchanger or after being cooled to suitable temp by the light phase entrance continuously feeding of last platform Centrifugical extraction separating device 10.In every Centrifugical extraction separating device, under the effect of centrifugal force, finish simultaneously nitration reaction and and react rear thick itrated compound and remain separating of nitration mixture, thick itrated compound after the separation is discharged from through the light phase export of every Centrifugical extraction separating device, and enter the upper level of nitration reaction separation system through the light phase entrance of a upper Centrifugical extraction separating device, nitration mixture after separating then flows out through the heavy out of every Centrifugical extraction separating device, and enter the next stage of nitration reaction separation system through the heavy liquid inlet of next Centrifugical extraction separating device, thus, reactant is constantly carrying out mixing fully in the nitration reaction separation system, reaction, conduct heat, sepn process, the final thick itrated compound that generates of reaction is flowed out by the light phase export of first Centrifugical extraction separating device 7, reacts final remaining spent acid by the heavy out outflow of last platform Centrifugical extraction separating device 10.
2) the thick itrated compound that flows out is after conventional alkali cleaning and washing, the nitro-compound product that obtains making with extra care through rectifying, the spent acid that flows out the nitration reaction separator can turn back to the nitration mixture preparation process and again prepare nitration mixture as raw material after concentrating, redundance enters the spent acid hold-up vessel.
Embodiment 1 prepares the method for oil of mirbane
Concrete steps comprise:
1) take the HL-50 centrifugal extractor of Beijing extraction application technical institute development as the nitration reaction separator, according to the method for describing in the above-mentioned embodiment four separators are connected, make according to water: the mixed acid solution of the part by weight preparation of nitric acid: sulfuric acid=7:45:48 is from the heavy liquid inlet charging of the first nitration reaction separator, make benzene from the light phase entrance charging of the 4th nitration reaction separator, mixed acid solution and the benzene pump that is measured is sent into the nitration reaction separator continuously simultaneously, wherein the raw materials components mole ratio of benzene and nitric acid is 1:1.02, and mixing acid and benzene carry out nitration reaction under the rotating speed of 60-80 ℃ temperature and 1100-1300 rev/min; 2) in every nitration reaction separator, under the effect of centrifugal force, finish simultaneously the nitration reaction of benzene and separating of the afterwards thick oil of mirbane of reaction and residue nitration mixture, thick oil of mirbane after the separation is discharged from through the light phase export of every nitration reaction separator, and enter the upper level of nitration reaction separation system through the light phase entrance of a upper nitration reaction separator, nitration mixture after separating then flows out through the heavy out of every nitration reaction separator, and enters the next stage of nitration reaction separation system through the heavy liquid inlet of next nitration reaction separator; The final thick oil of mirbane that generates is flowed out by the light phase export of first nitration reaction separator 7, reacts final remaining spent acid by the heavy out outflow of last platform nitration reaction separator 10.
3) rectifying after washing, alkali cleaning of thick oil of mirbane gets oil of mirbane, and spent acid circulates after flash concentration and prepares nitration mixture.
The oil of mirbane product purity that the present embodiment obtains is 99.5%, and yield is 98.5%.
Embodiment 2 prepares the method for oil of mirbane
Process is with embodiment 1, and change nitration mixture and consist of water: nitric acid: sulfuric acid=30:4:66, the raw materials components mole ratio of benzene and nitric acid are 1.1:1.0, and mixing acid and benzene carry out nitration reaction under the rotating speed of 136 ℃ temperature and 900 rev/mins;
The oil of mirbane product purity that the present embodiment obtains is 99.5%, and yield is 99.1%.
Process is with embodiment 1, and changing the nitration mixture proportioning is water: nitric acid: sulfuric acid=20:56:24, the raw materials components mole ratio of benzene and nitric acid are 1.0:1.05, and mixing acid and toluene carry out nitration reaction under the rotating speed of 50 ℃ temperature and 1000 rev/mins; React complete after, thick itrated compound gets Ortho Nitro Toluene, para-nitrotoluene and meta-nitrotoluene through rectifying.
The nitrotoluene product purity that the present embodiment obtains is 98%, and total recovery is 94.5%.
Embodiment 4 prepares the method for nitro-chlorobenzene
Process is with embodiment 1, and changing the nitration mixture proportioning is water: nitric acid: sulfuric acid=20:10:70, the raw materials components mole ratio of chlorobenzene and nitric acid are 1.1:1.0, and mixing acid and toluene carry out nitration reaction under the rotating speed of 90 ℃ temperature and 1400 rev/mins; React complete after, thick itrated compound gets o-Nitrochlorobenzene and p-Nitrophenyl chloride through crystallization, rectifying.
The o-Nitrochlorobenzene that the present embodiment obtains and p-Nitrophenyl chloride product purity are 97.5%, and total recovery is 97%.
Embodiment 5 prepares the method for nitroglycerine and BT trinitrate mixture
Process is with embodiment 1, and changing the nitration mixture proportioning is water: nitric acid: sulfuric acid=10:30:60, the raw materials components mole ratio of alcohol mixture and nitric acid are 1.0:1.05, and mixing acid and alcohol mixture carry out nitration reaction under the rotating speed of 50 ℃ temperature and 1000 rev/mins;
The nitroglycerine that the present embodiment obtains and BT trinitrate mixture total content 98.8%, yield is 96.7%.
Claims (10)
1. multistage nitration reaction separation system that is used for the nitro compound the production of material, it is characterized in that: it is made of the series connection of the Centrifugical extraction separating device more than 2, the heavy out of every Centrifugical extraction separating device connects the heavy liquid inlet of next Centrifugical extraction separating device, and the light phase entrance of every Centrifugical extraction separating device connects the light phase export of next Centrifugical extraction separating device; Each gangway that links to each other connects by pipeline.
2. multistage nitration reaction separation system claimed in claim 1 is characterized in that: it is made of the series connection of 2-4 platform Centrifugical extraction separating device.
3. the production method of a nitro-compound may further comprise the steps:
1) make the mixed acid solution Accessory Right that contains sulfuric acid and nitric acid require the heavy liquid inlet continuously feeding of first Centrifugical extraction separating device of 1 described multistage nitration reaction separation system, treat that simultaneously nitrated raw material is from the light phase entrance continuously feeding of last platform Centrifugical extraction separating device, control the interior temperature of reaction of every Centrifugical extraction separating device at 10～160 ℃, and the rotating speed of control Centrifugical extraction separating device is at 800-2000 rev/min; In every Centrifugical extraction separating device, under the effect of centrifugal force, finish simultaneously nitration reaction and and react rear thick itrated compound and remain separating of nitration mixture, thick itrated compound after the separation is discharged from through the light phase export of every Centrifugical extraction separating device, and again enter the upper level of nitration reaction separation system through the light phase entrance of a upper Centrifugical extraction separating device, nitration mixture after separating then flows out through the heavy out of every Centrifugical extraction separating device, and enters the next stage of nitration reaction separation system through the heavy liquid inlet of next Centrifugical extraction separating device;
2) after the multistage continuous nitration reaction of step 1), discharge final thick itrated compound from the light phase export of first Centrifugical extraction separating device, from the final spent acid of heavy out outflow of last platform Centrifugical extraction separating device; With thick itrated compound through conventional alkali cleaning and the washing after, the nitro-compound product that obtains making with extra care through rectifying again.
4. the production method of nitro-compound claimed in claim 3, it is characterized in that: step 1) is described treats that nitrated raw material is aromatic hydrocarbons or polyvalent alcohol.
5. the production method of nitro-compound claimed in claim 4, it is characterized in that: described aromatic hydrocarbons is benzene, toluene or chlorobenzene.
6. the production method of nitro-compound claimed in claim 4, it is characterized in that: described polyvalent alcohol is glycerol or BT.
7. the production method of nitro-compound claimed in claim 3 is characterized in that: the described mixed acid solution of step 1), by weight percentage, contain the sulfuric acid of 20-80% and the nitric acid of 2-40%, and surplus is water.
8. the production method of nitro-compound claimed in claim 3 is characterized in that: the temperature of reaction in the described Centrifugical extraction separating device of step 1) is controlled at 15-150 ℃.
9. the production method of nitro-compound claimed in claim 3, it is characterized in that: the rotating speed of the described Centrifugical extraction separating device of step 1) is controlled at 1000-1800 rev/min.
10. the production method of nitro-compound claimed in claim 3 is characterized in that: step 2) spent acid that flows out of described last platform Centrifugical extraction separating device prepares nitration mixture for step 1) again as raw material after concentrated.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107033005A (en) * | 2015-07-14 | 2017-08-11 | 北京化工大学苏州（相城）研究院 | A kind of nitration method of aromatic compound |
| CN108586256A (en) * | 2018-03-20 | 2018-09-28 | 淮海工学院 | A kind of method of continuous flow upstream nitrification production dinitrobenzene |
| CN110845373A (en) * | 2019-11-29 | 2020-02-28 | 浙江嘉福新材料科技有限公司 | Method for continuously preparing 2-nitro-4-methylsulfonyl toluene |
| CN111559737A (en) * | 2020-05-27 | 2020-08-21 | 河南洛染股份有限公司 | Method for continuously extracting nitration waste acid |
| CN113000232A (en) * | 2021-03-02 | 2021-06-22 | 西安近代化学研究所 | Liquid nitrate post-treatment system and process |
| CN113372280A (en) * | 2021-05-25 | 2021-09-10 | 黄冈银河阿迪药业有限公司 | 2-methylimidazole continuous nitration reaction system and continuous nitration process |
| CN114588850A (en) * | 2022-03-03 | 2022-06-07 | 清华大学 | Integrated micro-reactor for liquid-liquid heterogeneous exothermic reaction and use method |
| WO2024001054A1 (en) * | 2022-06-28 | 2024-01-04 | 宁夏信广和新材料科技有限公司 | Production method for nitrobenzene |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU955580A1 (en) * | 1981-02-05 | 1988-08-23 | Предприятие П/Я Р-6476 | Centrifugal extractor |
| CN1789235A (en) * | 2004-12-13 | 2006-06-21 | 沈阳化工学院 | Apparatus and method for preparing nitrobenzene by nitration of tubular benzene |
| CN102070457A (en) * | 2011-02-15 | 2011-05-25 | 河南洛染股份有限公司 | Method for continuously preparing dinitrochlorobenzene |
| CN102432471A (en) * | 2011-11-07 | 2012-05-02 | 常州大学 | Method for undergoing chlorobenzene nitration reaction by using micro-channel reactor |
| CN102675118A (en) * | 2012-04-25 | 2012-09-19 | 中国石油化工股份有限公司 | Washing and separation method of nitrobenzene |
-
2013
- 2013-01-18 CN CN201310019913.3A patent/CN103044261B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU955580A1 (en) * | 1981-02-05 | 1988-08-23 | Предприятие П/Я Р-6476 | Centrifugal extractor |
| CN1789235A (en) * | 2004-12-13 | 2006-06-21 | 沈阳化工学院 | Apparatus and method for preparing nitrobenzene by nitration of tubular benzene |
| CN102070457A (en) * | 2011-02-15 | 2011-05-25 | 河南洛染股份有限公司 | Method for continuously preparing dinitrochlorobenzene |
| CN102432471A (en) * | 2011-11-07 | 2012-05-02 | 常州大学 | Method for undergoing chlorobenzene nitration reaction by using micro-channel reactor |
| CN102675118A (en) * | 2012-04-25 | 2012-09-19 | 中国石油化工股份有限公司 | Washing and separation method of nitrobenzene |
Non-Patent Citations (1)
| Title |
|---|
| 段五华等: "微型离心萃取器在萃取工艺实验研究中的应用", 《现代化工》 * |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107033005A (en) * | 2015-07-14 | 2017-08-11 | 北京化工大学苏州（相城）研究院 | A kind of nitration method of aromatic compound |
| CN107033005B (en) * | 2015-07-14 | 2020-08-11 | 北京化工大学苏州（相城）研究院 | Nitration method of aromatic compound |
| CN108586256A (en) * | 2018-03-20 | 2018-09-28 | 淮海工学院 | A kind of method of continuous flow upstream nitrification production dinitrobenzene |
| CN110845373A (en) * | 2019-11-29 | 2020-02-28 | 浙江嘉福新材料科技有限公司 | Method for continuously preparing 2-nitro-4-methylsulfonyl toluene |
| CN111559737A (en) * | 2020-05-27 | 2020-08-21 | 河南洛染股份有限公司 | Method for continuously extracting nitration waste acid |
| CN113000232A (en) * | 2021-03-02 | 2021-06-22 | 西安近代化学研究所 | Liquid nitrate post-treatment system and process |
| CN113000232B (en) * | 2021-03-02 | 2022-08-19 | 西安近代化学研究所 | Liquid nitrate post-treatment system and process |
| CN113372280A (en) * | 2021-05-25 | 2021-09-10 | 黄冈银河阿迪药业有限公司 | 2-methylimidazole continuous nitration reaction system and continuous nitration process |
| CN114588850A (en) * | 2022-03-03 | 2022-06-07 | 清华大学 | Integrated micro-reactor for liquid-liquid heterogeneous exothermic reaction and use method |
| WO2024001054A1 (en) * | 2022-06-28 | 2024-01-04 | 宁夏信广和新材料科技有限公司 | Production method for nitrobenzene |
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