CN105509507A - Loop jet cooler and method for rapidly cooling isocyanate gas by adopting same - Google Patents
Loop jet cooler and method for rapidly cooling isocyanate gas by adopting same Download PDFInfo
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- CN105509507A CN105509507A CN201610008040.XA CN201610008040A CN105509507A CN 105509507 A CN105509507 A CN 105509507A CN 201610008040 A CN201610008040 A CN 201610008040A CN 105509507 A CN105509507 A CN 105509507A
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- atomizer
- isocyanates
- gas
- reaction tube
- quencher
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F28—HEAT EXCHANGE IN GENERAL
- F28C—HEAT-EXCHANGE APPARATUS, NOT PROVIDED FOR IN ANOTHER SUBCLASS, IN WHICH THE HEAT-EXCHANGE MEDIA COME INTO DIRECT CONTACT WITHOUT CHEMICAL INTERACTION
- F28C3/00—Other direct-contact heat-exchange apparatus
- F28C3/06—Other direct-contact heat-exchange apparatus the heat-exchange media being a liquid and a gas or vapour
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C263/00—Preparation of derivatives of isocyanic acid
- C07C263/10—Preparation of derivatives of isocyanic acid by reaction of amines with carbonyl halides, e.g. with phosgene
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to the field of organic chemical industry, and particularly relates to a loop jet cooler and a method for achieving rapid cooling by means of performing continuous operation on isocyanate gas through the loop jet cooler. According to the cooler, isocyanate gas enters a reaction tube through an isocyanate gas inlet, and a quenching agent enters an inner tube of an atomizer through a quenching agent inlet, is sprayed into the reaction tube through an atomizer nozzle spray hole and an atomizer spraying groove, makes contact with the isocyanate gas mixture and quenches the isocyanate gas. According to the method, corresponding amine and phosgene are subjected to a high-temperature reaction for rapidly cooling the isocyanate gas through the quenching agent, the retention time of the isocyanate gas inside the reaction tube can be adjusted through feeding of the atomizer quenching agent at different positions, side reactions are effectively reduced, and the isocyanate yield is further improved.
Description
Technical field
The invention belongs to organic chemical industry field, be specifically related to a kind of loop spray cooler and utilize it to realize the method for fast cooling to the continued operation of isocyanates gas.
Background technology
Gas phase phosgenation process is that phosgene and amine carry out under the high temperature of 300 ~ 500 DEG C, first generates intermediate product carbamyl chloride, then decomposes further and generates phosgenation product isocyanates.Phosgenation product is gas, and this product is heat-labile at reactor outlet temperature, therefore needs gas to be quickly cooled to uniform temperature, uses liquid quencher that reaction is stopped, to avoid, in quench region, side reaction occurs.Chilling temperature demand fulfillment two conditions: (1), higher than the decomposition temperature of carbamyl chloride, generates product isocyanates to make the carbamyl chloride decomposition completely of part unreacted; (2) because isocyanates is heat sensitive material, temperature can not be too high, and to avoid product isocyanates generation thermosensitive response, general control is between 80 ~ 190 DEG C.Therefore, avoid the generation of side reaction, improve these problems such as the yield of isocyanates is the key problem that puzzlement gas phase phosgenation method produces isocyanates always, and the fast cooling technology of phosgenation reaction material is the emphasis of industrial production technology research and development always.
Patent CN201251375 reports a kind of two phase flow atomized injection cooling device, this injected cool radiator cooler arranges outer cooling water jecket, ectonexine annular gas passage, at chuck mouth and gas passway, nozzle is set respectively, liquids and gases are sprayed by nozzle, mix in mixing chamber, realize the quick cooling of high-temperature gas.This device advantage is that compact conformation, economy and durability, atomization cooling effectiveness are high.And shortcoming is when high-temperature reacting gas is by nozzle, the easy plug nozzle of the solid impurity that gas contains, causes the termination of cooling fast, this device can not be made to run continuously.
Patent US2004/0068137A1 reports the chilled equipment with nozzle, propose and inject cancellation liquid when admixture of gas flows out into cylindrical shape cancellation district, downstream continuously from cylindrical shape reaction zone, wherein cancellation liquid at least two nozzles inject, nozzle is along the equidistant porch being arranged in cancellation district of cancellation district periphery, reacting gas is cooled fast to 150 DEG C, the time of contact of cooling procedure is 0.2 ~ 3s, and quencher is the mixture of inert organic solvents or organic solvent.This patent achieves reactant cessation reaction within the enough short time, but this device cancellation district is FX, effectively can not adjust the time of staying of high-temperature reacting gas in reaction tube, cause reaction not exclusively or excessively complete, the reduction of the product yield that finally induces reaction.
Patent CN101372463B reports a kind of device for ejecting and absorbing, liquid gas jet absorber is set, circulating pump, absorption cell cool fast to high-temperature gas, wherein Jet absorber is arranged on reactor afterbody, the spray-hole of some is evenly set, quencher sprays from spray-hole, and forms certain vacuum.This device absorbs by spraying, make the temperature that the high-temperature gas of discharging from reactor is quickly cooled to product stable, and simultaneously for system course of reaction provides negative pressure, eliminate huge vacuum system, but when containing solid impurity in high-temperature reacting gas, the blocking of Jet absorber can be caused equally, cause the termination of cooling fast, this device can not be made to run continuously.
As can be seen from above-mentioned example, quencher and corresponding equipment can be used to make high-temperature gas realize fast cooling, but all there is the generation that effectively can not reduce side reaction or fast cooling technique is run continuously.Therefore, need to find one and isocyanates gas fast cooling technique can be made to run continuously, and equipment and the method for side reaction generation can be reduced.
Summary of the invention
The object of the invention is to, a kind of loop spray cooler is provided, the quencher with certain pressure is sprayed by spray-hole, promote that quencher mixes with the efficient of isocyanates gas, and can prevent cooler from being reacted solid blocking, realize the continuous fast cooling to isocyanates gas.
For achieving the above object, the technical scheme that the present invention takes is: a kind of loop spray cooler, this cooler is made up of reaction tube and atomizer and atomizer sleeve pipe, atomizer is coaxially connected with atomizer sleeve pipe, and 3-20 atomizer sleeve pipe is that axial Relative distribution is welded on reaction tube in the layering of reaction tube outer surface circumference; Atomizer is made up of pipe, atomizer nozzle and atomizer cap in atomizer, and in atomizer, pipe is coaxially connected with atomizer nozzle and atomizer cap respectively; Isocyanates gas enters in reaction tube by isocyanates gas access N1 mouth, quencher to enter in atomizer after pipe by quencher entrance N2 mouth, spray in reaction tube by atomizer nozzle spray-hole and atomizer cap spray tank, contact with high-temperature reacting gas mixture, cancellation is carried out to isocyanates gas.
Wherein, in described loop spray device, the layering of reaction tube outer surface circumference is that axial Relative distribution is connected with 3-20 atomizer; Atomizer basal spacing is 5-20cm; Each atomizer front end connection control valve, controls quencher and enters reaction tube, adjust reaction tube quench region with this.
Described reaction tube diameter is 6-15 times of atomizer diameter of inner pipe, and atomizer nozzle spray-hole number is 2-6; Its aperture 0.3-0.8mm; Spray-hole length is 0.1-0.5 times of nozzle diameter; Its spray-hole and nozzle plane form inclined angle alpha, and inclination angle is 30 °-75 °, and atomizer cap spray tank footpath is 1-3 times of the atomizer nozzle injection aperture of correspondence.
Another object of the present invention is to, provide a kind of and adopt above-mentioned loop spray cooler to having general formula R (NCO)
nisocyanates gas carry out method fast, and adjust the time of staying of reactant in reaction tube by the atomizer quencher charging of diverse location, effectively reduce the generation of side reaction, improve the yield of isocyanates further.Concrete technical scheme is as follows:
A) in the reactor that temperature is 320-450 DEG C, phosgene with there is general formula R (NH2)
namine reaction generate corresponding isocyanates R (NCO)
n, this isocyanates becomes gaseous state at 320-450 DEG C, and isocyanates gas and solvent chlorobenzene gas flow out from reactor outlet, enter reaction tube through isocyanates gas N1 mouth;
B) each atomizer front end connection control valve, control temperature is that the quencher of 40-100 DEG C enters reaction tube, quencher is after quencher entrance N2, spray in reaction tube by 2-10, reaction tube top atomizer again, quencher fully mixes with isocyanates gas, phosgene, solvent, fast cooling to 120-210 DEG C, before fast cooling, isocyanates gas and excess phosgene are 0.1-0.5s reacting intraductal retention time, obtain the isocyanates of certain yield;
C) quencher is after quencher entrance N2, close loop spray device upper end 2-10 atomizer front end valve, adjusting 1-10 the atomizer making quencher enter loop spray device lower end sprays in reaction tube, quencher fully mixes with isocyanate reaction gas, phosgene, solvent, fast cooling is to 120-210 DEG C, before fast cooling, isocyanate reaction gas and excess phosgene are 0.2-0.8s reacting intraductal retention time, obtain the isocyanates of certain yield;
Wherein said quencher selects the inert organic liquid do not reacted with high-temperature reacting gas, preferred benzene, toluene, ethylbenzene, dimethylbenzene, n-proplbenzene, chlorobenzene, o-dichlorohenzene.
Be the preferred toluene di-isocyanate(TDI) of isocyanates (TDI), methyl diphenylene diisocyanate (MDI), IPDI (IPDI), the hexamethylene diisocyanate (HDI), 4 of gaseous state at 320-450 DEG C, 4-dicyclohexyl methyl hydride diisocyanate (HMDI), to phenyl isocyanate (PPDI), naphthalene diisocyanate (NDI), Methylcyclohexyl diisocyanate (HTDI), Isosorbide-5-Nitrae-cyclohexyl diisocyanate (CHDI), trimethyl hexamethylene diisocyanate (TMDI).
The invention has the beneficial effects as follows: by loop spray cooler, isocyanates gas enters from isocyanates gas access N1 mouth with certain flow, quencher is sprayed in reaction tube by the atomizer that quencher entrance N2 mouth is connected by the axial Relative distribution of layering and realizes quencher and mix with the efficient of isocyanates gas, reaches the fast cooling of isocyanates gas.This process can make corresponding amine photoreactive gas be cooled fast isocyanates gas by quencher after pyroreaction, and the time of staying of isocyanates gas in reaction tube can be adjusted by the atomizer quencher charging of diverse location, the generation of effective reduction side reaction, improves the yield of isocyanates further.
Accompanying drawing explanation
The present invention has 3 width accompanying drawings
Fig. 1 is that loop spray cooler master looks installation diagram
Fig. 2 is that atomizer master looks assembly drawing
Fig. 3 is I-I partial enlarged drawing
Pipe 5-atomizer nozzle 6-atomizer cap 7-nozzle spray-hole 8-atomizer cap spray tank N1-isocyanates gas access N2-quencher entrance in 1-reaction tube 2-atomizer 3-atomizer sleeve pipe 4-atomizer in figure
Detailed description of the invention
Be described principle of the present invention and feature below in conjunction with accompanying drawing, example, only for explaining the present invention, is not intended to limit scope of the present invention.
The present invention is to provide a kind of loop spray cooler, this cooler is made up of reaction tube 1 and atomizer 2 and atomizer sleeve pipe 3, atomizer 2 is coaxially connected with atomizer sleeve pipe 3, and 3-20 atomizer sleeve pipe 3 is that axial Relative distribution is welded on reaction tube 1 in the layering of reaction tube outer surface circumference; Atomizer is made up of pipe in atomizer 4, atomizer nozzle 5 and atomizer cap 6, and in atomizer, pipe 4 is coaxially connected with atomizer nozzle 5 and atomizer cap 6 respectively; Isocyanates gas enters in reaction tube by isocyanates gas N1 entrance, quencher to enter in atomizer after pipe 4 by quencher entrance N2 mouth, spray in reaction tube 1 by atomizer nozzle spray-hole 7 and atomizer cap spray tank 8, with isocyanates gas mixture contacts, cancellation is carried out to isocyanates gas.Wherein, in described loop spray device, the layering of reaction tube outer surface circumference is that axial Relative distribution is connected with 3-20 atomizer; Atomizer basal spacing is 5-20cm; Each atomizer front end connection control valve, controls quencher and enters reaction tube, adjust reaction tube quench region with this.
Described reaction tube diameter is 6-15 times of atomizer diameter of inner pipe, and atomizer nozzle spray-hole number is 2-6; Its aperture 0.3-0.8mm; Spray-hole length is 0.1-0.5 times of nozzle diameter; Its spray-hole and nozzle plane form inclined angle alpha, and inclination angle is 30 °-75 °, and atomizer cap spray tank footpath is 1-3 times of the atomizer nozzle injection aperture of correspondence.
Isocyanates gas cools fast and carries out in above-mentioned loop spray cooler, specifically operates according to the following steps:
A) in the reactor that temperature is 320-450 DEG C, phosgene with there is general formula R (NH
2)
namine reaction generate corresponding isocyanates R (NCO)
n, this isocyanates becomes gaseous state at 320-450 DEG C, and isocyanates gas and solvent chlorobenzene gas flow out from reactor outlet, enter reaction tube through isocyanates gas N1 mouth;
B) each atomizer front end connection control valve, control temperature is that the quencher of 40-100 DEG C enters reaction tube, quencher is after quencher entrance N2, spray in reaction tube 1 by 2-10, reaction tube top atomizer again, quencher fully mixes with isocyanates gas, phosgene, solvent, fast cooling to 120-210 DEG C, before fast cooling, isocyanates gas and excess phosgene are 0.1-0.5s reacting intraductal retention time, obtain the isocyanates of certain yield;
C) quencher is after quencher entrance N2, close loop spray device upper end 2-10 atomizer front end valve, adjusting 1-10 the atomizer making quencher enter loop spray device lower end sprays in reaction tube 1, quencher fully mixes with isocyanates gas, phosgene, solvent, fast cooling is to 120-210 DEG C, before fast cooling, isocyanates gas and excess phosgene are 0.2-0.8s reacting intraductal retention time, obtain the isocyanates of certain yield;
Wherein said quencher selects the inert organic liquid do not reacted with high-temperature reacting gas, preferred benzene, toluene, ethylbenzene, dimethylbenzene, n-proplbenzene, chlorobenzene, o-dichlorohenzene.
Be the preferred toluene di-isocyanate(TDI) of isocyanates (TDI), methyl diphenylene diisocyanate (MDI), IPDI (IPDI), the hexamethylene diisocyanate (HDI), 4 of gaseous state at 320-450 DEG C, 4-dicyclohexyl methyl hydride diisocyanate (HMDI), to phenyl isocyanate (PPDI), naphthalene diisocyanate (NDI), Methylcyclohexyl diisocyanate (HTDI), Isosorbide-5-Nitrae-cyclohexyl diisocyanate (CHDI), trimethyl hexamethylene diisocyanate (TMDI).
In each embodiment cooler parts and processing method technological parameter and require as following table:
Claims (10)
1. a loop spray cooler, it is characterized in that: this cooler is made up of reaction tube (1) and atomizer (2) and atomizer sleeve pipe (3), atomizer (2) is coaxially connected with atomizer sleeve pipe (3), 3 ~ 20 atomizer sleeve pipes (3) are axial Relative distribution in the layering of reaction tube (1) outer surface circumference, are welded on reaction tube (1); Described atomizer (2) is formed by managing (4), atomizer nozzle (5) and atomizer cap (6) in atomizer, and in atomizer, pipe (4) is coaxially connected with atomizer nozzle (5) and atomizer cap (6) respectively; Isocyanates gas enters in reaction tube (1) by isocyanates gas access, quencher is entered in atomizer by quencher entrance and manages after (4), spray in reaction tube (1) by atomizer nozzle spray-hole (7) and atomizer cap spray tank (8), with isocyanates gas mixture contacts, cancellation is carried out to isocyanates gas.
2. a kind of loop spray cooler according to claim 1, it is characterized in that, atomizer (2) basal spacing is 5-20cm, each atomizer (2) front end connection control valve, control quencher and enter reaction tube (1), adjust reaction tube quench region with this.
3. a kind of loop spray cooler according to claim 1, is characterized in that, reaction tube (1) diameter is 6-15 times of atomizer (2) diameter of inner pipe.
4. a kind of loop spray cooler according to claim 1, is characterized in that, atomizer nozzle (5) spray-hole number is 2-6; Its aperture is 0.3-0.8mm; Spray-hole length is 0.1-0.5 times of nozzle diameter; Its spray-hole and nozzle plane form inclined angle alpha, and inclination angle is 30 °-75 °.
5. a kind of loop spray cooler according to claim 1, is characterized in that, atomizer cap spray tank (8) bore open is 1-3 times of atomizer nozzle spray-hole (7) aperture of correspondence.
6. one kind adopts loop spray cooler as described in any one of claim 1-5 to having general formula R (NCO)
nisocyanates gas carry out the method for fast cooling, it is characterized in that, comprise the steps:
A) in the reactor that temperature is 320-450 DEG C, phosgene with there is general formula R (NH
2)
namine reaction generate corresponding isocyanates R (NCO)
n, this isocyanates becomes gaseous state at 320-450 DEG C, and isocyanates gas and solvent chlorobenzene gas flow out from reactor outlet, enter reaction tube through isocyanates gas access;
B) each atomizer front end connection control valve, control temperature is that the quencher of 40-100 DEG C enters reaction tube, quencher is after quencher entrance, spray in reaction tube by 2-10, reaction tube top atomizer again, quencher fully mixes with isocyanates gas, phosgene, solvent, fast cooling to 120-210 DEG C, before fast cooling, isocyanates gas and excess phosgene are 0.1-0.5s reacting intraductal retention time, obtain the isocyanates of certain yield;
C) quencher is after quencher entrance, close loop spray device upper end 2-10 atomizer front end valve, adjusting 1-10 the atomizer making quencher enter loop spray device lower end sprays in reaction tube (1), quencher fully mixes with isocyanate reaction gas, phosgene, solvent, fast cooling is to 120-210 DEG C, before fast cooling, isocyanate reaction gas and excess phosgene are 0.2-0.8s reacting intraductal retention time, obtain isocyanates.
7. method according to claim 6, is characterized in that, described step b), the quencher that c) uses selects the inert organic liquid do not reacted with high-temperature reacting gas.
8. method according to claim 7, is characterized in that, described inert organic liquid is any one in preferred benzene, toluene, ethylbenzene, dimethylbenzene, n-proplbenzene, chlorobenzene or o-dichlorohenzene.
9. method according to claim 6, is characterized in that, described step a), b), c) in isocyanates gas be at 320-450 DEG C of isocyanates in gaseous state.
10. method according to claim 9, is characterized in that, described isocyanates is any one in TDI, MDI, IPDI, HDI, HMDI, PPDI, NDI, HTDI, CHDI, TMDI.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610008040.XA CN105509507B (en) | 2016-01-07 | 2016-01-07 | A kind of loop spray cooler and using its method to isocyanates gas fast cooling |
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| CN201610008040.XA CN105509507B (en) | 2016-01-07 | 2016-01-07 | A kind of loop spray cooler and using its method to isocyanates gas fast cooling |
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| CN105509507B CN105509507B (en) | 2017-07-14 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107899531A (en) * | 2017-12-18 | 2018-04-13 | 甘肃银光聚银化工有限公司 | A kind of spraying cycle reactor and the method for being synthesized by isocyanates |
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| CN1434742A (en) * | 2000-07-03 | 2003-08-06 | 巴斯福股份公司 | Method for reducing byproducts in the mixture of educt trreams |
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