CN102060295B - Production technology of high purity phosgene with low hydrogen chloride content - Google Patents
Production technology of high purity phosgene with low hydrogen chloride content Download PDFInfo
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- YGYAWVDWMABLBF-UHFFFAOYSA-N Phosgene Chemical compound ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 title claims abstract description 128
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 229910000041 hydrogen chloride Inorganic materials 0.000 title claims abstract description 34
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 18
- 238000005516 engineering process Methods 0.000 title abstract description 13
- 238000010521 absorption reaction Methods 0.000 claims abstract description 36
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229910002091 carbon monoxide Inorganic materials 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 28
- 239000012535 impurity Substances 0.000 claims abstract description 11
- 238000010992 reflux Methods 0.000 claims abstract description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Natural products CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 20
- 241000282326 Felis catus Species 0.000 claims description 15
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 claims description 14
- 238000012856 packing Methods 0.000 claims description 13
- 239000002904 solvent Substances 0.000 claims description 11
- RFFLAFLAYFXFSW-UHFFFAOYSA-N 1,2-dichlorobenzene Chemical compound ClC1=CC=CC=C1Cl RFFLAFLAYFXFSW-UHFFFAOYSA-N 0.000 claims description 4
- 239000000945 filler Substances 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 229910000975 Carbon steel Inorganic materials 0.000 claims description 2
- 239000010962 carbon steel Substances 0.000 claims description 2
- 238000004064 recycling Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 125000003944 tolyl group Chemical group 0.000 claims 1
- 239000007789 gas Substances 0.000 abstract description 47
- 239000007791 liquid phase Substances 0.000 abstract description 6
- 239000004417 polycarbonate Substances 0.000 abstract description 5
- 229920000515 polycarbonate Polymers 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000012948 isocyanate Substances 0.000 abstract 1
- 150000002513 isocyanates Chemical class 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 15
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 8
- 229910052757 nitrogen Inorganic materials 0.000 description 8
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 7
- 235000011089 carbon dioxide Nutrition 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 6
- 150000002148 esters Chemical class 0.000 description 6
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 5
- 239000000460 chlorine Substances 0.000 description 5
- 229910052801 chlorine Inorganic materials 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 238000000926 separation method Methods 0.000 description 5
- 238000009833 condensation Methods 0.000 description 4
- 230000005494 condensation Effects 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- -1 U.S. Pat 60012021 Chemical compound 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 description 2
- 238000005660 chlorination reaction Methods 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000007086 side reaction Methods 0.000 description 2
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 150000005826 halohydrocarbons Chemical class 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Abstract
The invention relates to a production technology of high purity phosgene with low hydrogen chloride content. The production technology comprises the following operation steps: the mixed gas with rich phosgene, unreacted excessive carbon monoxide and other impurities enters at least one rectifying tower, the top of each rectifying tower is provided with a fractional condenser, the liquid phase is used for refluxing, most of hydrogen chloride is discharged from the top of the rectifying tower along with CO and high purity phosgene is obtained at the bottom of the rectifying tower; and the gas discharged from the top of the rectifying tower passes through at least one absorption tower to wash away and recycle phosgene. The production technology in the invention has simple process flow and low production cost and is convenient to operate; and the hydrogen chloride content of the obtained phosgene product is greatly reduced, the purity of phosgene is more than 99.90% and the obtained phosgene can be used for the products using phosgene as a raw material such as isocyanate and polycarbonate and the like.
Description
Technical field:
The present invention relates to a kind of production technique of high-purity phosgene of low hydrogen chloride content, remove hydrogenchloride, the method for purification phosgene the mixture of the phosgene that especially generates from carbon monoxide and chlorine reaction.
Background technology:
Phosgene is a kind of important organic intermediate, and many purposes, the important source material of especially producing isocyanic ester, polycarbonate are all arranged in agricultural chemicals, medicine, engineering plastics, polyurethane material and military affairs.
Usually reacted in the presence of catalyzer by carbon monoxide (CO) and chlorine in the industry and obtain phosgene, this method the earliest can be referring to Ullmann ' s Encyclopedia of Industrial Chemistry (the 5th edition, A19 volume, the 413rd page).Reaction mechanism is following:
The content of the phosgene impurities of producing in this way changes according to the processing condition difference.Impurity derives from the phosgene building-up process some and does not hope the side reaction that takes place, and major impurity has: the tetracol phenixin that the chlorination reaction of CO perchlorizing, gac and methane generates; The hydrogenchloride that the chlorination reaction of unavoidable impurities hydrogen generates in the raw material (CO and chlorine) etc.
Content in order to tetracol phenixin in the phosgene of top method preparation is generally 250-2000ppm, and hydrogen chloride content is generally 200-5000ppm.Because halohydrocarbon is harmful to environment; People have carried out many-sided research to the tetracol phenixin that how to reduce in the phosgene; Like U.S. Pat 60012021, German patent DE 19848668.5 and Japanese Patent JP88-156040 and JP80-014044 have proposed to reduce the method for the tetracol phenixin in the phosgene respectively.The existence of hydrogenchloride has reduced the purity of phosgene in the phosgene; Generate at phosgene in the downstream application such as isocyanic ester, polycarbonate; Side reaction taking place, also might meet water and generate hydrochloric acid to equipment generation corrosion, therefore should in the phosgene product, reduce the content of hydrogenchloride as far as possible.German patent DE 102004044592.3 has been described a kind of method of separating hydrogen chloride photoreactive gas, and the described mixture of this method only contains two kinds of components of hydrogenchloride photoreactive gas.German patent DE 10260084.8 has been described a kind of hydrogenchloride photoreactive gas separating mixture; The described mixture of this method comprises hydrogenchloride, phosgene, possible solvent, low-boiling-point substance and the inert composition that generally obtains in the process for preparing isocyanic ester through amine and phosgene reaction; This method main purpose is through with rare gas element such as nitrogen the hydrogenchloride in the phosgene being removed, and will obtain phosgene or phosgene solution is recycled to isocyanic ester synthetic conversion zone.
At present; The method of traditional separation purification phosgene is to utilize the mode of multi-stage condensing to become liquid to a large amount of phosgene condensations in the mixed gas; Thereby realize that phosgene separates with non-condensable gas with excessive CO in the reactor drum, its technical process is: the mixed gas that is rich in phosgene and contains the intact excessive carbon monoxide of unreacted and other impurity that comes from phosgene reactor passes through first-stage condenser and secondary condenser, and the most phosgene condensations in the mixed gas are got off; Through knockout drum; The tank deck logistics is rich in the intact excessive carbon monoxide of unreacted and other non-condensable gas, handles through going other operation behind the solvent recuperation phosgene wherein, promptly obtains the product phosgene in jar.In the phosgene synthesis reactor, complete in order to make chlorine reaction, generally add excessive CO.The shortcoming of this method is that most of hydrogenchloride can be along with phosgene condensation together.
Summary of the invention:
The production technique that the purpose of this invention is to provide the lower high purity phosgene of a kind of hydrogen chloride content; Promptly from the mixture of carbon monoxide and chlorine reaction generation phosgene, remove hydrogenchloride, purification phosgene; This technology can significantly reduce the content of HCl in the phosgene of preparation, and the phosgene of being produced can be used for isocyanic ester, polycarbonate and other is the product of raw material with the phosgene.
In order to realize the foregoing invention purpose; The production technique of high-purity phosgene of a kind of low hydrogen chloride content provided by the invention; Operate according to following steps: (1) gets at least one rectifying tower from the mixed gas that is rich in phosgene and contains the intact excessive carbon monoxide of unreacted and other impurity that phosgene reactor comes, and rectifying tower top has partial condenser, and liquid phase provides backflow; Let most of hydrogenchloride discharge with CO, obtain highly purified phosgene at the bottom of the rectifying tower simultaneously by rectifying tower top; What (2) rectifying tower top was discharged is that main gas passes through at least one absorption tower washing and recycling phosgene wherein again with CO.
Rectifying tower proposed by the invention is packing tower or the tray column that has reflux exchanger, and the material of its tower body and internals is carbon steel or stainless steel, and preferred filler tower, filler are structured packing or dumped packing, and optimum is the stainless steel dumped packed column.The number of theoretical plate of tower is generally 3～10, and preferred 5～8, working pressure is generally 0.3～0.6MPa, preferred 0.4～0.5MPa.
Rectifying tower top has partial condenser, saturated total reflux, and reflux ratio is generally 18～24 (quality), is preferably 19～21.
The extraction of partial condenser gas phase gets into the phosgene of carrying under one's arms with solvent recuperation CO in the absorption tower.
With solvent absorbing phosgene wherein, the absorption tower is packing tower or tray column to the tail gas that the rectifying tower cat head is discharged, the preferred filler tower through the absorption tower.Working pressure is 0.3～0.6MPa, and preferred 0.4～0.5MPa, number of theoretical plate are 3～10, preferred 5～8.
The used solvent in absorption tower is the organic solvent good to the phosgene solubility property, comprises toluene, chlorobenzene, orthodichlorobenzene, YLENE, o-Xylol, DEIP etc., preferred toluene and chlorobenzene.The mass ratio that reclaims solvent load and non-condensable gas amount is 2～5, preferred 2.5～3.0.
Compared with prior art, the production technique of high-purity phosgene of a kind of low hydrogen chloride content of the present invention has following advantage:
(1) the present invention has replaced condensed in two stages and one-level gas-liquid separation in the existing Technology with a rectifying tower that has dephlegmator of top of the tower, has reduced the phosgene producing apparatus, has simplified technical process.
(2) phosgene that at the bottom of rectifying tower, obtained of the present invention, under the almost constant situation of the cold that consumes, hydrogen chloride content reduces greatly, is reduced to 200PPM by the existing general 2000PPM of technology.
(3) phosgene that at the bottom of rectifying tower, obtained of the present invention; Under the almost constant situation of the cold that consumes; The CO content of carrying under one's arms simultaneously reduces greatly; Be reduced to 100PPM by the existing general 1000PPM of technology, the purity of phosgene is brought up to more than 99.90% by the existing general 99.50%-99.60% of technology.
Description of drawings:
Fig. 1 is the technological process of production figure of high-purity phosgene of low hydrogen chloride content of the present invention.
Embodiment:
Through specific embodiment and with the correlated Comparative Examples of traditional technology production technique of the present invention is done further to set forth below.
Embodiment 1-3 technical process is as shown in Figure 1; Be rich in phosgene and contain the intact excessive carbon monoxide of unreacted and the mixed gas S1 of other impurity from what phosgene reactor came, this mixed gas S1 is through rectifying tower 1, and rectifying tower 1 cat head has partial condenser 2; Liquid phase provides backflow; Gas phase S3 is rich in the intact excessive carbon monoxide of unreacted and other non-condensable gas, handles through going other operation behind the solvent recuperation phosgene wherein, promptly obtains product phosgene S2 at the bottom of rectifying tower 1 tower.
Comparative Examples 1-3 technical process is: be rich in phosgene and contain the intact excessive carbon monoxide of unreacted and the mixed gas S1 of other impurity from what phosgene reactor came; This mixed gas S1 is through first-stage condenser and secondary condenser; Most phosgene condensations in the mixed gas are got off, and through knockout drum, the tank deck logistics is rich in the intact excessive carbon monoxide of unreacted and other non-condensable gas; Through going other operation to handle behind the solvent recuperation phosgene wherein, promptly obtain phosgene in jar.
In embodiment and the Comparative Examples in each stream strand percentage composition form and all to be meant mass percent.
Embodiment 1,
Rectifying tower 1 is a packing tower, and number of theoretical plate is 3.The mixed gas S1 flow that is rich in phosgene that comes from phosgene reactor is that 50kg/h, temperature are that 65 ℃, pressure are 0.5MPa, consists of: phosgene 97.16%, carbon monoxide 2.23%; Hydrogenchloride 0.21%; Nitrogen 0.21%, carbonic acid gas 0.14% and other rare gas element 0.05%, S1 gets into from the 3rd block of plate of rectifying tower 1; Rectifying tower 1 cat head working pressure is 0.45MPa, and reflux ratio is 20.Promptly obtain phosgene product S2 at the bottom of rectifying tower 1 tower.
Rectifying tower 1 cat head has partial condenser 2; Liquid phase provides backflow, and mixed gas S3 is through the absorption tower 3, and absorption tower 3 is a packing tower; Number of theoretical plate is 3; Further reclaim phosgene wherein with toluene, the exhaust S6 of absorption tower 3 cats head send vent gas treatment, and the phosgene solution S5 that reclaims at the bottom of 3 towers of absorption tower can or destroy and handle according to the further purification of arts demand.Absorption tower 3 tower top pressures are 0.4MPa, toluene consumption 50kg/h.
The phosgene product result that obtains sees table 1 and table 2.
Comparative Examples 1,
The mixed gas S1 flow that is rich in phosgene that comes from phosgene reactor is that 50kg/h, temperature are that 65 ℃, pressure are 0.5MPa, consists of: phosgene 97.16%, carbon monoxide 2.23%; Hydrogenchloride 0.21%; Nitrogen 0.21%, carbonic acid gas 0.14% and other rare gas element 0.05%, S1 is cooled to 40 ℃ through first-stage condenser; Pass through the secondary condenser deep cooling again to-10 ℃, get into knockout drum.Promptly obtain product phosgene S2 in the knockout drum.
The logistics of gas-liquid separation tank deck is through the absorption tower; Packing tower is adopted on the absorption tower, and number of theoretical plate is 3, further reclaims phosgene wherein with toluene; Vent gas treatment is sent in the exhaust that absorbs cat head, and the phosgene solution that reclaims at the bottom of the tower can further be purified perhaps to destroy and handled according to arts demand.The absorption tower tower top pressure is 0.4MPa, toluene consumption 50kg/h.
The Comparative Examples 1 phosgene product result that obtains sees table 1 and table 2.
Embodiment 2,
Rectifying tower 1 is a packing tower, and number of theoretical plate is 5.The mixed gas S1 flow that is rich in phosgene that comes from phosgene reactor is that 50kg/h, temperature are that 65 ℃, pressure are 0.5MPa, consists of phosgene 97.16%, carbon monoxide 2.23%; Hydrogenchloride 0.21%; Nitrogen 0.21%, carbonic acid gas 0.14% and other rare gas element 0.05%, S1 gets into from the 5th block of plate of rectifying tower 1; Rectifying tower 1 cat head working pressure is 0.45MPa, and reflux ratio is 24.Promptly obtain phosgene product S2 at the bottom of rectifying tower 1 tower.
Rectifying tower 1 cat head has partial condenser 2; Liquid phase provides backflow; Mixed gas S3 is through the absorption tower 3, and absorption tower 3 number of theoretical plates are 10, further reclaim phosgene wherein with chlorobenzene; The exhaust S6 of absorption tower 3 cats head send vent gas treatment, and the phosgene solution S5 that reclaims at the bottom of 3 towers of absorption tower can further purify perhaps to destroy and handle according to arts demand.Absorption tower 3 tower top pressures are 0.4MPa, chlorobenzene consumption 75kg/h.
The phosgene product result that obtains sees table 1 and table 2.
Comparative Examples 2,
The mixed gas S1 flow that is rich in phosgene that comes from phosgene reactor is that 50kg/h, temperature are that 65 ℃, pressure are 0.5MPa, consists of: phosgene 97.16%, carbon monoxide 2.23%; Hydrogenchloride 0.21%; Nitrogen 0.21%, carbonic acid gas 0.14% and other rare gas element 0.05%, S1 is cooled to 40 ℃ through first-stage condenser; Pass through the secondary condenser deep cooling again to-10 ℃, get into knockout drum.Promptly obtain product phosgene S2 in the knockout drum.
The logistics of gas-liquid separation tank deck is through the absorption tower, and the absorption tower number of theoretical plate is 10, further reclaims phosgene wherein with chlorobenzene, and vent gas treatment is sent in the exhaust of absorption cat head, and the phosgene solution of recovery can further be purified or the destruction processing according to arts demand at the bottom of the tower.The absorption tower tower top pressure is 0.4MPa, chlorobenzene consumption 75kg/h.
The Comparative Examples 2 phosgene product result that obtains sees table 1 and table 2.
Embodiment 3,
Rectifying tower 1 is a packing tower, and number of theoretical plate is 10.The mixed gas S1 flow that is rich in phosgene that comes from phosgene reactor is that 50kg/h, temperature are that 65 ℃, pressure are 0.5MPa, consists of: phosgene 97.16%, carbon monoxide 2.23%; Hydrogenchloride 0.21%; Nitrogen 0.21%, carbonic acid gas 0.14% and other rare gas element 0.05%, S1 gets into from the 10th block of plate of rectifying tower 1; Rectifying tower 1 cat head working pressure is 0.45MPa, and reflux ratio is 18.Promptly obtain phosgene product S2 at the bottom of rectifying tower 1 tower.
Rectifying tower 1 cat head has partial condenser 2; Liquid phase provides backflow; Mixed gas S3 is through the absorption tower 3, and absorption tower 3 number of theoretical plates are 10, further reclaim phosgene wherein with methylene dichloride; The exhaust S6 of absorption tower 3 cats head send vent gas treatment, and the phosgene solution S5 that reclaims at the bottom of 3 towers of absorption tower can further purify perhaps to destroy and handle according to arts demand.Absorption tower 3 tower top pressures are 0.4MPa, methylene dichloride consumption 50kg/h.
The phosgene product result that obtains sees table 1 and table 2.
Comparative Examples 3,
The mixed gas S1 flow that is rich in phosgene that comes from phosgene reactor is that 50kg/h, temperature are that 65 ℃, pressure are 0.5MPa, consists of: phosgene 97.16%, carbon monoxide 2.23%; Hydrogenchloride 0.21%; Nitrogen 0.21%, carbonic acid gas 0.14% and other rare gas element 0.05%, S1 is cooled to 40 ℃ through first-stage condenser; Pass through the secondary condenser deep cooling again to-10 ℃, get into knockout drum.Promptly obtain product phosgene S2 in the knockout drum.
The logistics of gas-liquid separation tank deck is through the absorption tower, and the absorption tower number of theoretical plate is 10, further reclaims phosgene wherein with methylene dichloride, and vent gas treatment is sent in the exhaust of absorption cat head, and the phosgene solution of recovery can further be purified or the destruction processing according to arts demand at the bottom of the tower.The absorption tower tower top pressure is 0.4MPa, methylene dichloride consumption 50kg/h.
The phosgene product result that Comparative Examples 3 is obtained sees table 1 and table 2.
Visible by the data in table 1 and the table 2; Technology and existing technology ratio that the present invention proposes; The phosgene product gas purity is brought up to more than 99.93% by original 99.60%, and the content of impurity CO drops to 100ppm by 1000ppm, and hydrogen chloride content is reduced to below the 200ppm by 1600ppm; Prepared phosgene is applicable to preparation tolylene diisocyanate (TDI), diphenylmethanediisocyanate isocyanic ester such as (MDI), especially is suitable for the preparation polycarbonate.
Table 1 embodiment and Comparative Examples obtain result's contrast of phosgene product
| Charging | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative Examples | |
| S1 | S2 | S2 | S2 | S2 | |
| Phosgene | 97.16％ | 99.93％ | 99.94％ | 99.94％ | 99.60％ |
| CO | 2.23％ | 0.01％ | 0.01％ | 0.01％ | 0.10％ |
| Hydrogenchloride | 0.21％ | 0.02％ | 0.017％ | 0.017％ | 0.16％ |
| Nitrogen | 0.21％ | 0.001％ | 0.001％ | 0.001％ | 0.01％ |
| Carbonic acid gas | 0.14％ | 0.01％ | 0.0085％ | 0.0085％ | 0.10％ |
| Rare gas element | 0.05％ | 0.029％ | 0.02％ | 0.02％ | 0.03％ |
| Flow kg/h | 50 | 48.4 | 48.2 | 48.8 | 48.6 |
Result's contrast of table 2 embodiment and Comparative Examples solvent recuperation phosgene
| Embodiment 1 | Comparative Examples 1 | Embodiment 2 | Comparative Examples 2 | Embodiment 3 | Comparative Examples 3 | |
| Phosgene amount among the S3, kg/h | 5.938 | 5.422 | 8.078 | 5.422 | 1.3799 | 5.422 |
| Reclaim phosgene amount, kg/h among the S5 | 5.920 | 5.411 | 8.078 | 5.422 | 1.3799 | 5.422 |
| The phosgene recovery, % | 99.70％ | 99.80％ | 100％ | 100％ | 100％ | 100％ |
Claims (5)
1. the production technique of the phosgene of purifying; It is characterized in that operating according to following steps: the mixed gas that is rich in phosgene and contains the intact excessive carbon monoxide of unreacted and other impurity that comes from phosgene reactor gets at least one rectifying tower; Let most of hydrogenchloride discharge with CO, obtain highly purified phosgene at the bottom of the rectifying tower simultaneously by rectifying tower top; What rectifying tower top was discharged is that main gas passes through at least one absorption tower washing and recycling phosgene wherein again with CO.
2. the production technique of a kind of phosgene of purifying according to claim 1 is characterized in that rectifying tower is packing tower or the tray column that has reflux exchanger, and the material of its tower body and internals is carbon steel or stainless steel, and filler is structured packing or dumped packing; The number of theoretical plate of tower is 3～10, and working pressure is 0.3～0.6MPa.
3. the production technique of a kind of phosgene of purifying according to claim 1 is characterized in that rectifying tower top has partial condenser, and reflux ratio is 18～24.
4. the production technique of a kind of phosgene of purifying according to claim 1; It is characterized in that tail gas that the rectifying tower cat head discharges through the absorption tower with solvent absorbing phosgene wherein; The absorption tower is packing tower or tray column, and working pressure is 0.3～0.6MPa, and number of theoretical plate is 3～10.
5. the production technique of a kind of phosgene of purifying according to claim 4 is characterized in that the used solvent in absorption tower is toluene, chlorobenzene, orthodichlorobenzene, YLENE.
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| CN103877829B (en) * | 2013-12-18 | 2016-07-06 | 西安近代化学研究所 | The absorption process of ethylenediamine rectifying column tail gas and device |
| TWI511771B (en) * | 2013-12-31 | 2015-12-11 | Ind Tech Res Inst | Method and system for treating gas |
| CN105197931A (en) * | 2014-11-10 | 2015-12-30 | 青岛科技大学 | Low-consumption environment-friendly efficient phosgene synthesis technology |
| WO2020132936A1 (en) | 2018-12-26 | 2020-07-02 | 万华化学集团股份有限公司 | Method for preparing isocyanate in gaseous phase |
| CN109704993A (en) * | 2018-12-26 | 2019-05-03 | 万华化学集团股份有限公司 | A method of preparing isocyanates in the gas phase |
| CN112390729A (en) * | 2020-11-10 | 2021-02-23 | 宁夏瑞泰科技股份有限公司 | Method for co-producing n-butyl isocyanate by chloroformic acid-2-ethylhexyl ester |
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| JPH0629129B2 (en) * | 1988-06-25 | 1994-04-20 | 出光石油化学株式会社 | Method for producing phosgene |
| US5672747A (en) * | 1996-05-17 | 1997-09-30 | Stauffer; John E. | Phosgene process |
| DE10260084A1 (en) * | 2002-12-19 | 2004-07-01 | Basf Ag | Separation of a mixture of hydrogen chloride and phosgene |
| JP2006137669A (en) * | 2005-12-05 | 2006-06-01 | Sumitomo Chemical Co Ltd | Method for producing phosgene |
| DE102006024542A1 (en) * | 2006-05-23 | 2007-11-29 | Bayer Materialscience Ag | Process for the separation of carbon monoxide from a hydrogen chloride-containing gas |
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