CN102120729B - Industrial method for producing iminostilbene through catalytic dehydrogenation of iminodibenzyl - Google Patents
Industrial method for producing iminostilbene through catalytic dehydrogenation of iminodibenzyl Download PDFInfo
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Abstract
The invention provides an industrial method for producing iminostilbene through catalytic dehydrogenation of iminodibenzyl. The method comprises the process flows that: a reactant material is heated, melted, and mixed with high-temperature water vapor, and the mixture enters a dehydrogenation reactor; dehydrogenation reaction is performed in an axial or a radial fixed bed reactor which comprises at least two catalyst beds; the high-temperature water vapor is arranged between the two catalyst beds to indirectly or directly heat a reactant flow; the reactant flow which gets out of the reactor passes through a heat exchanger for heat exchange and heat recovery, and subsequently enters an absorption tower which is provided with the heat exchanger and is an bubbling absorption tower or a spray absorption tower; and a solvent which absorbs a reaction product is subjected to evaporation, crystallization and the like to obtain a product iminostilbene. The method has the characteristics of high reactivity, low consumption of raw materials, low energy consumption, environmentally-friendly process and the like.
Description
Technical field
The invention belongs to the chemical reaction engineering technical field, specifically, relate to a kind of catalytic dehydrogenation industrialized preparing process of medicine intermediate iminostilbene.
Background technology
Iminostilbene (IS) is a kind of important medicinal intermediates, is mainly used in the synthetic of Carbamzepine and O'Casey equality medicine.
(10,11-dihydro-IS, IDB) synthetic imido stilbene is the method for industrial extensive employing, mainly contains bromination method, liquid-phase catalysis dehydriding and vapor catalytic dehydrogenation method with iminodibenzyl.Bromination method is the commercial run of production iminostilbene the earliest; iminodibenzyl prepares the method for iminostilbene through multisteps such as acidylate, bromination, dehydrobromination, deacylated tRNAs; this method exists that low conversion rate, dopant species are many, the drawback such as waste time and energy, and quality product is not high.The defectives such as catalytic dehydrogenation prepares the imido stilbene under the iminodibenzyl liquid-phase condition, and temperature of reaction is low, and product yield is higher, but exist to adopt noble metal catalyst and loss serious, consumes hydrogen acceptor, and product postprocessing is more loaded down with trivial details.The iminodibenzyl vapor catalytic dehydrogenation prepares imido stilbene method, has a technical process simple, and the by product kind is few, easily separated, and quality product is high, can be used for producing without advantages such as bromine Carbamzepines, and be the best approach of producing iminostilbene.
A kind of Catalysts and its preparation method is disclosed among the document CN 100453175C, and the application of this catalyzer in producing iminostilbene, the catalyzer that has proposed to adopt the metal oxide by molybdenum, tin and iron to form utilizes the iminodibenzyl gas-phase dehydrogenation to produce the method for iminostilbene.The method is dissolved in iminodibenzyl in the aromatic hydrocarbon solvent with concentration 5-30% (W/W), evaporates in vaporizer under 300-375 ℃, and in 350～480 ℃ of lower reactions, the direct condensation of reacted material is reclaimed in isothermal tube reactor.The method exists a large amount of solvents to pass through catalyzer with reactant, causes catalyst life greatly to reduce, and is difficult to satisfy the requirement of long period stably manufactured in the industry; Reactor diameter 23mm only only belongs to laboratory testing rig in addition.
A kind of chemical synthesis process of iminostilbene is disclosed among the document CN 101307021A, adopt fixed-bed reactor, electrically heated makes the catalytic bed temperature be increased to 400-600 ℃, the iminodibenzyl of melting is brought catalytic bed into by high-pressure water vapor, enter the device that water coolant is housed after the reaction, recrystallization obtains product behind the mixed solution evaporate to dryness moisture content that obtains.The method adopts the electrically heated catalytic bed, and energy consumption is very high when using in the industry; Adopt water vapor to carry raw material and advance reactor, the raw material inlet amount is regulated difficulty; Reactor diameter 30mm only can't directly apply to industrial production in addition, and catalytic bed is one section only, and reaction efficiency is low, does not implement heat transfer reactor between the multistage, and system also operates under normal pressure, belongs to laboratory testing rig.
A kind of production technique of iminostilbene is disclosed in the document US 3531466, the base metal dehydrogenation catalyst has been proposed, adopt tubular reactor, temperature of reaction is between 300～700 ℃, normal pressure or negative-pressure operation utilize water vapor to carry raw material, and reduce the dividing potential drop of iminodibenzyl by adding nitrogen, the whole condensations of reaction after product, mixed solution obtains product through recrystallization.The method employing water vapor carries raw material and advances reactor, and the raw material inlet amount is regulated difficulty; Adopt nitrogen conditioned reaction thing dividing potential drop, caused the dehydrogenated tail gas calorific value significantly to descend, under the negative-pressure operation condition so that the load of tail-gas compressor increase; Reactor diameter 30mm only belongs to laboratory testing rig in addition.
Disclose a kind of production method of imido stilbene in the document JP 55017330, prepared compound metal oxide catalyst, use temperature 350-650 ℃, reaction system can be carried out under normal pressure or reduced pressure.Reactor diameter 16mm adopts electrically heated, only belongs to laboratory testing rig.
In sum, the method of iminostilbene is produced in above-mentioned iminodibenzyl catalytic dehydrogenation, mostly for developing the catalyzer of iminodibenzyl catalytic dehydrogenation iminostilbene processed, its iminostilbene production method is the preparation method in laboratory, production technique when all not proposing industrial scale production, and there is production energy consumption high, the short deficiency that waits of catalyst life.
Summary of the invention
The present inventor is by research, produce iminostilbene for the iminodibenzyl catalytic dehydrogenation, find a kind of industrialized production method, the technical process of present method is: reaction mass is through entering dehydrogenation reactor after the heat fused with after high-temperature water vapor mixes, dehydrogenation reaction is to comprise axially or in the radial fixed-bed reactor carrying out of at least two catalytic bed at one, high-temperature water vapor is set indirectly or the direct heating reactant flow between two catalytic bed, carry out heat exchange from reactor logistics out through an interchanger and reclaim heat, enter subsequently the absorption tower with interchanger, through cooling, after cooling and the absorption, its solvent that is rich in reaction product takes out, through pervaporation, crystallizations etc. obtain the product iminostilbene.Present method has realized the highly selective of catalytic dehydrogenating reaction by heat transfer technology between multistage catalysis and bed; Employing absorbs the product of easy crystallization with organic solvent with the absorption tower of interchanger; Process water recycles, and has implemented zero release; Dehydrogenated tail gas directly enters process furnace and burns, and has both obtained the calorific value of hydrogen, has reduced again discharging.Present method has overcome the technological deficiencies such as energy consumption is high in the prior art, catalyst life is short, meets simultaneously the environmental requirement of energy-saving and emission-reduction, can implement large-scale industrial production.
Therefore, primary and foremost purpose of the present invention just is to provide a kind of iminodibenzyl vapor catalytic dehydrogenation to produce the method for iminostilbene.
The technical issues that need to address of the present invention are:
(1) production technique that provides a kind of industrial feasible iminodibenzyl vapor catalytic dehydrogenation to produce iminostilbene, the catalytic dehydrogenating reaction of realization highly selective;
When (2) carrying out industrial-scale production, for the requirement of environmental protection and energy saving, must consider the comprehensive utilization of energy and the discharging of the reduction three wastes;
(3) pre-treatment of product and aftertreatment technology must consider that the raw material of easy crystallization and product hold susceptible to plugging problem in equipment, meet to produce actual needs;
Therefore, design of the present invention is such:
1, adopts negative pressure technique, meet the feature that the iminodibenzyl catalytic dehydrogenation increases volumetric reaction, can improve the equilibrium conversion of reaction, more be conducive to the raising of reaction preference;
2, adopting water vapor is thermophore, provides dehydrogenation reaction needed heat, and the dividing potential drop effect that reduces raw material is also arranged simultaneously.In addition, the adding of water vapor can effectively advance water-gas reaction, has avoided the coking of catalyzer, significantly improves the life-span of catalyzer;
3, adopt the multistage reaction process, can reduce the inlet temperature of raw material, to avoid the excessive shortcoming of single hop adiabatic reaction temperature drop amplitude, thereby the selectivity of reaction and the yield of reaction have been improved, also can reduce significantly the charge ratio of water vapor and raw material on the other hand, thereby reduce the energy consumption of device;
4, adopt the radial reactor technology, or adopt thin bed axial flow reactor technology, effectively reduce bed pressure drop, more meet the negative dehydrogenation processing requirement;
5, adopt bubble absorbing tower, liquid phase solvent is dissolved in the reaction product that very easily forms crystallization in the fast cooling process fully in the tower, has removed fast again the heat of reactant flow simultaneously, and its device absorption and heat transfer efficiency are high, also is difficult for being stopped up by reaction product;
6, adopt spray absorber, the organic solvent that reaction product and unreacted raw material are sprayed absorbs fully; Heat is discharged by the outer solvent interchanger of tower, and its device assimilated efficiency is high, and pressure drop is low, also is difficult for being stopped up by reaction product;
7, process water has reclaimed heat through interchanger and water treating device, has implemented recycle;
8, dehydrogenated tail gas is delivered to the process furnace burning, both eliminated the disposal of pollutants of reactive system, can be used as again the fuel of process furnace.
According to above-mentioned design, the present invention proposes following technical scheme:
The method of iminostilbene is produced in a kind of iminodibenzyl catalytic dehydrogenation, dehydrogenation reaction is to carry out in a dehydrogenation reactor that comprises at least two catalytic bed, a mixing tank is set before the reactor, reaction mass is squeezed in the mixing tank by pump after being heated fusing, mix with high-temperature water vapor, reactant flow enters reactor after being raised to temperature of reaction; Settle interchanger between two catalytic bed in the reactor, enter next catalyst bed reaction after in heat-exchanger rig, being reheated temperature of reaction from the reaction mass of a upper catalytic bed; Carry out heat exchange from reactor material out through an interchanger and reclaim heat, enter subsequently the absorption tower, absorption liquid is processed through pervaporation, crystallization etc. and is obtained the product iminostilbene.Extracted out by compressor as dehydrogenated tail gas after the interchanger condensation from top, absorption tower gas out, deliver to the process furnace burning.
Iminodibenzyl catalytic dehydrogenation of the present invention is produced in the method for iminostilbene, dehydrogenation reactor adopts radial reactor or the axial flow reactor of multistage, fill the base metal dehydrogenation catalyst take ferric oxide as main active ingredient in the bed, interchanger is set between the catalytic bed.Reactant flow is entered by reactor head, flows out from reactor bottom.Dehydrogenation reaction of the present invention can adopt the dehydrogenation catalyst take ferric oxide as main active component.
Iminodibenzyl catalytic dehydrogenation of the present invention is produced in the method for iminostilbene, the multistage reaction process is adopted in catalytic dehydrogenation, can reduce the inlet temperature of raw material, thereby improved the selectivity of reaction, also can significantly reduce on the other hand the charge ratio of water vapor and raw material, thereby reduced the energy consumption of device, be the low-carbon (LC) production technique.
Iminodibenzyl catalytic dehydrogenation of the present invention is produced in the method for iminostilbene, and the weight space velocity of iminodibenzyl is 0.01～2.0h
-1The mol ratio of water vapor and iminodibenzyl is 10～300, and temperature of reaction is 300～650 ℃, and the absolute pressure mean value in the reactor is between 0.02～0.10Mpa, the transformation efficiency of reactant iminodibenzyl is 60～90%, and the selectivity of reaction product iminostilbene is 65～90%; In addition, catalysis dehydrogenation reaction of the present invention also can operate under normal pressure.
Iminodibenzyl catalytic dehydrogenation of the present invention is produced in the method for iminostilbene, the intermediate heat that arrives first in the reactor from process furnace high-temperature water vapor out carries out heat exchange, and then enter mixing tank and mix with the raw material iminodibenzyl, the intermediate heat that perhaps arrives first in the reactor from process furnace high-temperature water vapor out carries out heat exchange, then get back to and enter again mixing tank after process furnace reheats and mix with the raw material iminodibenzyl, the high temperature pipe of front a kind of method is shorter, and the temperature of the furnace outlet water vapor of rear a kind of method is lower.
Iminodibenzyl catalytic dehydrogenation of the present invention is produced in the method for iminostilbene, adopt bubble absorbing tower or spray absorber to carry out the aftertreatment of reaction product, be specially with the dissolution with solvents very easily reactant of crystallization and reaction product in the reactant flow in the fast cooling process, obtained the liquid phase solvent that mainly contains reaction product; Or heat exchange component is set in tower, effectively rapid moving is walked heat, makes the reactant in the reactant flow enter oil phase from gas phase fast, has reclaimed simultaneously heat; Or the solvent interchanger is set outside tower, out Partial Liquid Phase solvent is by solvent interchanger cooling from the absorption tower, and then circulation enters top, absorption tower; In tower, be provided with the gas distributor of reactant flow charging and the liquid phase distributor of solvent, thereby guaranteed the abundant contact of vapour-liquid.Adopt bubble absorbing tower or spray absorber, its good absorbing effect, device is difficult for stopping up for crystallisate.
Iminodibenzyl catalytic dehydrogenation of the present invention is produced in the method for iminostilbene, and the heat exchange component of described bubble absorbing tower and spray absorber, gas distributor and liquid distributor are the common type of putting down in writing in the chemical engineering unit operation handbook.
Iminodibenzyl catalytic dehydrogenation of the present invention is produced in the method for iminostilbene, the solvent that adopt on the absorption tower is the organic solvent of water insoluble energy solubilizing reaction product and raw material, such as benzene,toluene,xylene etc., absorption tower oil phase liquid out obtains the product iminostilbene by separation means such as evaporation, crystallizations, and unreacted iminodibenzyl then returns head tank.
Iminodibenzyl catalytic dehydrogenation of the present invention is produced in the method for iminostilbene, and dehydrogenated tail gas is delivered to the process furnace burning, and water recycles through behind the treater, and three-waste free discharge under the normal condition of production of whole reactive system is eco-friendly production technique.
Any dehydrogenation reactor all can be used to implement processing method of the present invention, but better with the use radial reactor under the negative-pressure operation condition.
Description of drawings
The schematic flow sheet of iminostilbene method is produced in the dehydrogenation of Fig. 1 iminodibenzyl two-stage catalytic of the present invention.
The schematic flow sheet of iminostilbene method is produced in three sections catalytic dehydrogenations of Fig. 2 iminodibenzyl of the present invention.
Specific implementation method
The present invention is described further below in conjunction with accompanying drawing.
In Fig. 1: fresh iminodibenzyl is sent into head tank 1, is melted under the heating of water vapor, then is transported to mixing tank 3 by volume pump 2; Water is heated to be high-temperature water vapor in process furnace 4, at first carry out heat exchange in the resuperheater 14 in the reactor 5, the reactant flow that heating is flowed out from the first bed, then entering mixing tank 3 mixes with raw material, the mol ratio of water vapor and raw material is 10～300, and mixed reaction mass temperature is between 300-650 ℃; Enter reactor 5 from mixing tank 3 reactant flow out, reactor 5 is the axial flow reactor pattern of two sections thermal insulation, resuperheat, reactant flow is at first by the first bed, along with the temperature of carrying out reactant flow of reacting reduces gradually, the reactant flow that flows out from the first bed enters the reaction of the second catalytic bed by resuperheater 14 after its temperature is thus lifted between 300～650 ℃ again; Enter interchanger 6 to reclaim heat from reactor 5 reactant flow out, enter subsequently absorption tower 7, this absorption tower is bubble absorbing tower; Absorption tower 7 internal reaction logistics at first enter in the liquid phase solvent by gas distributor, then by solvent condenses, absorption, gas flows out from cat head, the water that condensation is got off is discharged at the bottom of tower, 7 top adds by liquid distributor solvent from the absorption tower, the solvent phase that has absorbed reaction product and reactant is discharged from the bottom of tower, water tank type interchanger 13 is set, with sensible heat and the condensation latent heat of removing reactant flow in the liquid on absorption tower 7; 7 bottom is extracted the solvent phase that contains reaction product out by pump 12 from the absorption tower, processes obtaining product imido stilbene through pervaporation, crystallization etc.; The water of condensation that flow out 7 bottom from the absorption tower is through water treating device 8, recycles after removing the impurity such as micro-content organism and inorganic salt; The logistics out of 7 cats head at first by condenser 9 coolings, then enters vapour liquid separator 10 and carries out gas-liquid separation from the absorption tower, and tail gas enters compressor 11, and phlegma returns absorption tower 7; Compressor 11 provides system needed pressure, is sent to process furnace 4 from compressor 11 tail gas out and burns.
In Fig. 2 flow process: fresh iminodibenzyl is sent into head tank 1, is melted under the heating of water vapor, then is transported to mixing tank 3 by volume pump 2; Water is heated to be high-temperature water vapor in process furnace 4, at first carry out heat exchange in the resuperheater 15 in the reactor 5 and the resuperheater 14, heat respectively from the reactant flow of the second bed and the outflow of the first bed, then entering mixing tank 3 mixes with raw material, the mol ratio of water vapor and raw material is 10～300, and mixed reaction mass temperature is between 300-650 ℃; Enter reactor 5 from mixing tank 3 reactant flow out, reactor 5 is the radial reactor pattern of three sections thermal insulation, two sections resuperheats, reactant flow is at first by the first bed, along with the temperature of carrying out reactant flow of reacting reduces gradually, the reactant flow that flows out from the first bed is by resuperheater 14, after being thus lifted between 300～650 ℃ again, its temperature enters the reaction of the second catalytic bed, the reactant flow that flows out from the second bed enters the reaction of the 3rd catalytic bed by resuperheater 15 after its temperature is thus lifted between 300～650 ℃ again; Enter interchanger 6 to reclaim heat from reactor 5 reactant flow out, enter subsequently absorption tower 7, this absorption tower is spray absorber; Absorption tower 7 internal reaction logistics at first enter in the tower by gas distributor, then by solvent condenses, absorption, gas flows out from cat head, the water that condensation is got off is discharged at the bottom of tower, 7 top adds by liquid distributor solvent from the absorption tower, the solvent phase that has absorbed reaction product and reactant is discharged from the bottom of tower, and 7 the external solvent interchanger 16 on the absorption tower is with sensible heat and the condensation latent heat of removing reactant flow; 7 bottom is extracted the solvent phase that contains reaction product out by pump 12 from the absorption tower, and part is processed through pervaporation, crystallization etc. and obtained product imido stilbene, and remaining solvent by 16 coolings of solvent interchanger, then returns to 7 tops, absorption tower mutually; The water of condensation that flow out 7 bottom from the absorption tower is through water treating device 8, recycles after removing the impurity such as micro-content organism and inorganic salt; , then enter vapour liquid separator 10 and carry out gas-liquid separation at first by condenser 9 coolings from the logistics out of bubble absorbing tower 7 cats head, tail gas enters compressor 11, and phlegma returns bubble absorbing tower 7; Compressor 11 provides system needed pressure, is sent to process furnace 4 from compressor 11 tail gas out and burns.
In the present invention, catalyzer can adopt commercially available broad variety dehydrogenation catalyst, also can adopt the catalyzer of the various iminodibenzyl vapor catalytic dehydrogenations of reporting such as document.The iminodibenzyl weight space velocity is 0.01～2.0h
-1
[embodiment 1]
The iminodibenzyl vapor catalytic dehydrogenation carries out with the technical process of Fig. 1, reactor is the axial flow reactor pattern of two sections thermal insulation, resuperheat, the mol ratio of water vapor and iminodibenzyl is 140, the temperature of reactant flow in each reaction bed ingress is respectively 550 ℃ and 530 ℃, absolute pressure mean value in the reactor is at 0.050Mpa, and the iminodibenzyl weight space velocity is 0.20h
-1, catalyzer adopts the C105 dehydrogenation catalyst.Adopting benzene in the bubble absorbing tower is that solvent reclaims.Reaction result sees Table 1.
[embodiment 2]
The iminodibenzyl vapor catalytic dehydrogenation carries out with the technical process of Fig. 2, reactor is the radial reactor pattern of three sections thermal insulation, resuperheat, the mol ratio of water vapor and iminodibenzyl is 160, the temperature of reactant flow in each reaction bed ingress is 530 ℃, absolute pressure mean value in the reactor is at 0.030Mpa, and the iminodibenzyl weight space velocity is 0.10h
-1, catalyzer adopts the LH315 dehydrogenation catalyst.Adopting toluene in the spray absorber is that solvent reclaims.Reaction result sees Table 1.
[embodiment 3]
The iminodibenzyl vapor catalytic dehydrogenation carries out with the technical process of Fig. 2, reactor is the radial reactor pattern of three sections thermal insulation, resuperheat, the mol ratio of water vapor and iminodibenzyl is 200, the temperature of reactant flow in each reaction bed ingress is 530 ℃, absolute pressure mean value in the reactor is at 0.150Mpa, and the iminodibenzyl weight space velocity is 0.15h
-1, catalyzer adopts the GS08 dehydrogenation catalyst.Adopting dimethylbenzene in the spray absorber is that solvent reclaims.Reaction result sees Table 1.
Table 1:
Adopt method of the present invention, compared with prior art have the following advantages:
1. reactivity worth is good, adopts heat exchange and negative-pressure operation between multistage catalyzed reaction technique, bed, has improved reactivity worth, and raw material consumption is lower, and the yield of reaction product iminostilbene is 60～65%;
2. energy consumption is lower, adopts multistage catalyzed reaction technique, and the mol ratio of water vapor and iminodibenzyl is down to about 100～200 by 300, and produced simultaneously dehydrogenated tail gas directly advances process furnace and burns to obtain calorific value.Thereby whole technique belongs to energy-saving.
3. what the iminodibenzyl vapor catalytic dehydrogenation was produced is the imido stilbene that does not contain the impurity such as Bromide compound, is high-quality pharmaceutical intermediate;
4. catalyst life is long, and the life-span of carrying the feeding manner catalyzer of raw material with respect to solvent increases more than 3～10 times;
5. the tail gas of whole reaction process generation directly burns and obtains calorific value, and three-waste free discharge is environmentally friendly;
6. by pre-treatment and aftertreatment technology, the raw material and the product that have solved easy crystallization hold susceptible to plugging problem in equipment.
Claims (9)
1. the method for iminostilbene is produced in an iminodibenzyl catalytic dehydrogenation, it is characterized in that, dehydrogenation reaction is to carry out in a dehydrogenation reactor that comprises at least two catalytic bed, fills the dehydrogenation catalyst take ferric oxide as main active ingredient in the described catalytic bed; A mixing tank is set before the reactor, and reaction mass is squeezed in the mixing tank by pump after heat fused and is mixed with high-temperature water vapor, and its reactant flow enters dehydrogenation reactor after being raised to temperature of reaction; Settle interchanger between two catalytic bed in the reactor, enter next catalyst bed reaction after in heat-exchanger rig, being reheated temperature of reaction from the reactant flow of a upper catalytic bed; Carry out heat exchange from reactor logistics out through an interchanger and reclaim heat, enter subsequently the absorption tower, reactant flow is lowered the temperature and solvent absorbing, and the solvent that has absorbed afterwards reaction product obtains the product iminostilbene through pervaporation and crystallization treatment again.
2. the method for claim 1 is characterized in that, described dehydrogenation reactor is axial restraint bed bioreactor or radial fixed-bed reactor.
3. such as each described method of claim 1-2, it is characterized in that, processing condition are: the mol ratio of water vapor and iminodibenzyl is 10～300, reactant flow is heated to 300～650 ℃ at described each reactor inlet place, absolute pressure in the reactor is 0.02～0.10Mpa or normal pressure, adopts simultaneously 0.01～2.0h
-1The iminodibenzyl weight space velocity.
4. the method for claim 1, it is characterized in that, carry out resuperheat between the catalytic bed, to improve the reactant flow temperature, wherein reheating method is for arranging intermediate heat, by the high-temperature water vapor indirect heating, or directly add reactant flow by the high-temperature water vapor that process furnace is drawn, carry out direct heating.
5. the method for claim 1, it is characterized in that, described absorption tower is bubble absorbing tower, heat exchange inner member and reactant flow sparger are set in the tower, and reactant flow enters the liquid phase layer that is full of solvent through sparger, and reaction product and unreacted raw material are absorbed, water vapor is condensed in the reactant flow, incoagulability tail gas is discharged by cat head, and solvent is added by tower top, and solvent phase logistics outlet is in the bottom of bubble absorbing tower.
6. the method for claim 1, it is characterized in that, described absorption tower is spray absorber, and reactant flow sparger and solvent sparger are set in the tower, reactant flow is in sparger enters tower, absorbed by the solvent under by upper spray, and water vapor is condensed in the reactant flow, incoagulability tail gas is discharged by cat head, the solvent phase logistics is discharged by the tower bottom, after the solvent interchanger heat exchange cooling, with fresh solvent, the top of spray absorber is sent in recirculation to part outside tower.
7. such as claim 1,5 or 6 described methods, it is characterized in that, the solvent on described absorption tower is benzene, toluene or dimethylbenzene.
8. the method for claim 1, it is characterized in that, after flow through water treating device from absorption tower aqueous-phase material out, with carry out entering process furnace after heat is reclaimed in heat exchange through an interchanger from reactor logistics out, the intermediate heat that the high-temperature water vapor that produces arrives first in the reactor carries out heat exchange, enter the temperature of reaction of next bed to improve reaction mass, and then enter mixing tank and mix with the raw material iminodibenzyl.
9. the method for claim 1 is characterized in that, the tail gas that dehydrogenation reaction produces is delivered to the process furnace burning.
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| CN102432539B (en) * | 2011-10-25 | 2013-11-13 | 华东理工大学 | Crystallization separation method in process of producing iminostilbene through catalytic dehydrogenation of iminodibenzyl |
| CN102432538A (en) * | 2011-10-25 | 2012-05-02 | 华东理工大学 | Integrated industrial production method for producing iminostilbene by continuous catalytic deamination and catalytic dehydrogenation of 2,2'-diamino-bibenzyl |
| CN105439954A (en) * | 2014-09-25 | 2016-03-30 | 中国石油化工股份有限公司 | One-step synthesis method of iminostilbene |
| CN111217751B (en) * | 2020-03-16 | 2021-06-08 | 浙江华洲药业有限公司 | Synthesis method of iminostilbene |
| CN115057817B (en) * | 2022-06-15 | 2023-09-08 | 浙江华洋药业有限公司 | Production process of iminostilbene |
| CN116726636A (en) * | 2023-08-14 | 2023-09-12 | 北京海望氢能科技有限公司 | Gas water scrubber and gas separation system |
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