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CN102258935A - Recovery and utilization method of phosgene in phosgenation reaction tail gas - Google Patents

Recovery and utilization method of phosgene in phosgenation reaction tail gas Download PDF

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CN102258935A
CN102258935A CN2011101012604A CN201110101260A CN102258935A CN 102258935 A CN102258935 A CN 102258935A CN 2011101012604 A CN2011101012604 A CN 2011101012604A CN 201110101260 A CN201110101260 A CN 201110101260A CN 102258935 A CN102258935 A CN 102258935A
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phosgene
reaction tower
phosgenation
product
tail gas
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徐建平
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Gu Weiwen
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Gu Weiwen
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Abstract

The invention relates to a recovery and utilization method of phosgene in phosgenation reaction tail gas. According to the method, phosgene tail gas containing 5.5% of phosgene is delivered to a first phosgene recovering reaction tower, a recycling liquid in a first circulation vessel is delivered to the first phosgene recovering reaction tower through a first circulation pump, such that a phosgenated product is produced through a reaction between the phosgene tail gas and the recycling liquid, and the product is delivered to the first circulation vessel; gas delivered from the first phosgene recovering reaction tower is delivered to a second phosgene recovering reaction tower, a recycling liquid in a second circulation vessel is delivered to the second phosgene recovering reaction tower through a second circulation pump, such that a phosgenated product is produced through a reaction between the phosgene tail gas and the recycling liquid, and the product is delivered to the second circulation vessel; When the concentration of the phosgenated product in the first circulation vessel reaches 98%, the phosgenated product in the first circulation vessel is delivered to a deacidification vessel. When a nitrogen blowing standard is reached, the finished phosgenated product is obtained. Phosgenation tail gas containing 0.5% of phosgene is delivered from the second phosgene recovering reaction tower to a condenser, and then delivered to a phosgenation tail gas system containing 0.5% of phosgene through a buffer. According to the invention, a phosgenated product is produced from phosgene in phosgenation tail gas, and phosgene content is reduced from 5.5% to 0.5%.

Description

The recoverying and utilizing method of phosgene in the phosgenation reaction tail gas
Technical field
The present invention relates to the recoverying and utilizing method of phosgene in a kind of phosgenation reaction tail gas.
Background technology
At present, the tail gas treatment process of all phosgenation products behind logical phosgene reaction all adopts following technical process: at first phosgene tail gas sponges the hydrogen chloride that produces in the photochemical reaction through water and reclaims hydrochloric acid, enter three grades of SN-7501 molecular sieve filling towers then and carry out hot water catalysis destruction, phosgene is broken to hydrogen chloride and carbon dioxide recovery hydrochloric acid, and then enter caustic wash tower and destroy remaining phosgene with NaOH, simultaneously behind the absorbing carbon dioxide, by being higher than the emptying of the high row of 40m exhaust duct.The destruction of this technology phosgene tail gas, concentration of emission, rate of discharge can satisfy " discharge standard of air pollutants ".But only solved the destruction of phosgene tail gas, and failed to utilize the phosgene in the tail gas.If the generation operation is unexpected in logical light process of producing product, perhaps generation hot water catalysis destruction is not thorough when handling the higher concentration phosgene, just the discharging that can exceed standard causes environmental pollution, personnel is damaged.
Summary of the invention
The objective of the invention is to overcome the deficiency that prior art exists, the recoverying and utilizing method of phosgene in a kind of phosgenation reaction tail gas is provided.
Purpose of the present invention is achieved through the following technical solutions:
The recoverying and utilizing method of phosgene in the phosgenation reaction tail gas, characteristics are: recycling system comprises that first phosgene reclaims reaction tower, second phosgene reclaims reaction tower, first recirculating still, second recirculating still, first circulating pump, second circulating pump and depickling still, reclaim reaction tower at first phosgene, second phosgene reclaims reaction tower, drop in first recirculating still and second recirculating still and reclaim liquid, come the phosgene tail gas that contains phosgene 5.5% of self-contained phosgene 5.5% phosgene exhaust system to enter first phosgene recovery reaction tower, by first circulating pump recovery liquid in first recirculating still is delivered to first phosgene and reclaim reaction tower, the phosgene that reclaims in the liquid and first phosgene recovery reaction tower reacts generation phosgenation product, the phosgenation product exports first recirculating still to, along with circulation and temperature control, the phosgenation product design constantly raises in first recirculating still;
The gas that comes out from first phosgene recovery reaction tower enters second phosgene recovery reaction tower, second circulating pump is delivered to second phosgene with the recovery liquid in second recirculating still and is reclaimed reaction tower, the phosgene that reclaims in the liquid and second phosgene recovery reaction tower reacts generation phosgenation product, the phosgenation product exports second recirculating still to, along with circulation and temperature control, the phosgenation product design constantly raises in second recirculating still;
The phosgenation product design reaches at 98% o'clock in first recirculating still, and the phosgenation transferred product in first recirculating still to the depickling still, is carried out nitrogen by nitrogen pot and blown drum back up to standard acquisition phosgenation product, and the phosgenation product is delivered to phosgenation product holding vessel;
Phosgenation product in first recirculating still will continue circular response in phosgenation transferred product to the first recirculating still in second recirculating still after shifting, it is 40~50% that second recirculating still shifts the phosgenation product design of coming; When second recirculating still is empty, replenish the new recovery liquid of adding by reclaiming flow container to second recirculating still, so repeatedly;
Second phosgene reclaims the phosgene tail gas that reaction tower output contains phosgene 0.5%, and the phosgene tail gas that contains phosgene 0.5% enters to deliver to through buffer after the condenser condenses again and contains phosgene 0.5% phosgene exhaust system.
The recoverying and utilizing method of phosgene in the above-mentioned phosgenation reaction tail gas, described first phosgene reclaim reaction tower and second phosgene recovery reaction tower is the tower reaction tower of film absorption.
The invention has the advantages that:
The present invention is provided with recycling system by enter the destruction tower at phosgene tail gas before, the phosgene that makes full use of in the phosgene tail gas is made the phosgenation product, effectively reduce the phosgene amount that contains that enters phosgene tail gas breaking plant, be reduced to 0.5% with containing the phosgene amount in the phosgene tail gas from 5.5%, reduced the load of the system that destroys, utilize phosgene manufacturing in the phosgene tail gas to obtain quality and reclaim product greater than 98% phosgene, effectively reduce and enter phosgene content in the classical phosgene exhaust gas processing device, under any circumstance all guaranteed the qualified discharge of phosgene tail gas, thoroughly stopped environmental pollution and to the generation of personnel's injury accident, improve security, prevented the accident generation.This process economics benefit and social effect are remarkable, can be rated as have novelty, the good technology of creativeness, practicality.
Description of drawings
Fig. 1: the organigram of recycling system of the present invention.
The implication of each Reference numeral among the figure:
1-contains phosgene 5.5% phosgene exhaust system; 2-first phosgene reclaims reaction tower; 3-second phosgene reclaims reaction tower; The 4-condenser; 5-contains phosgene 0.5% phosgene exhaust system; The 6-surge tank; 7-reclaims flow container; 8-depickling still; 9-first recirculating still; 10-second recirculating still; 11-first circulating pump; 12-second circulating pump; 13-phosgenation product holding vessel; The 14-nitrogen pot.
The specific embodiment
The recoverying and utilizing method of phosgene in the phosgenation reaction tail gas, as shown in Figure 1, recycling system comprises that first phosgene reclaims reaction tower 2, second phosgene reclaims reaction tower 3, first recirculating still 9, second recirculating still 10, first circulating pump 11, second circulating pump 12 and depickling still 8, reclaim reaction tower 2 at first phosgene, second phosgene reclaims reaction tower 3, drop in first recirculating still 9 and second recirculating still 10 and reclaim liquid, come the phosgene tail gas that contains phosgene 5.5% of self-contained phosgene 5.5% phosgene exhaust system 1 to enter first phosgene recovery reaction tower 2, by first circulating pump 11 the recovery liquid in first recirculating still 9 is delivered to first phosgene and reclaim reaction tower 2, the phosgene that reclaims in the liquid and first phosgene recovery reaction tower 2 reacts generation phosgenation product, the phosgenation product exports first recirculating still 9 to, along with circulation and temperature control, the phosgenation product design constantly raises in first recirculating still 9;
The gas that comes out from first phosgene recovery reaction tower 2 enters second phosgene recovery reaction tower 3, second circulating pump 12 is delivered to second phosgene with the recovery liquid in second recirculating still 10 and is reclaimed reaction tower 3, the phosgene that reclaims in the liquid and second phosgene recovery reaction tower 3 reacts generation phosgenation product, the phosgenation product exports second recirculating still 10 to, along with circulation and temperature control, the phosgenation product design constantly raises in second recirculating still 10;
When the phosgenation product design reaches 98% in first recirculating still 9, with the phosgenation transferred product in first recirculating still 9 to depickling still 8, carry out nitrogen by nitrogen pot 14 and blow drum back up to standard acquisition phosgenation product, the phosgenation product is delivered to phosgenation product holding vessel 13;
Phosgenation product in first recirculating still 9 will continue circular response in phosgenation transferred product to the first recirculating still 9 in second recirculating still 10 after shifting, it is 40~50% that second recirculating still 10 shifts the phosgenation product design of coming; When second recirculating still, 10 skies, replenish the new recovery liquid of adding by reclaiming flow container 7 to second recirculating still 10, so repeatedly;
Second phosgene reclaims the phosgene tail gas that reaction tower 3 outputs contain phosgene 0.5%, and the phosgene tail gas that contains phosgene 0.5% enters to deliver to through buffer 6 after condenser 4 condensations again and contains phosgene 0.5% phosgene exhaust system 5.
Wherein, first phosgene recovery reaction tower 2 and second phosgene recovery reaction tower 3 are the tower reaction tower of film absorption.First recirculating still 9 and second recirculating still 10 are recirculating stills that low-speed agitator and cooling system are installed, and material is determined with the requirement of phosgenation product.
The actual consumption data contrast on the methylchloroformate production line of process of the present invention and traditional handicraft method is as follows:
Figure BSA00000479002300041
The present invention is provided with recycling system by enter the destruction tower at phosgene tail gas before, the phosgene that makes full use of in the phosgene tail gas is made the phosgenation product, effectively reduce the phosgene amount that contains that enters phosgene tail gas breaking plant, be reduced to 0.5% with containing the phosgene amount in the phosgene tail gas from 5.5%, reduced the load of the system that destroys, utilize phosgene manufacturing in the phosgene tail gas to obtain quality and reclaim product greater than 98% phosgene, effectively reduce and enter phosgene content in the classical phosgene exhaust gas processing device, under any circumstance all guaranteed the qualified discharge of phosgene tail gas, thoroughly stopped environmental pollution and to the generation of personnel's injury accident, improve security, prevented the accident generation.
The above only is a preferred implementation of the present invention, for those skilled in the art, under the prerequisite that does not break away from the principle of the invention, can also make some improvements and modifications, and these improvements and modifications also should be considered as protection scope of the present invention.

Claims (2)

1. the recoverying and utilizing method of phosgene in the phosgenation reaction tail gas, it is characterized in that: recycling system comprises that first phosgene reclaims reaction tower (2), second phosgene reclaims reaction tower (3), first recirculating still (9), second recirculating still (10), first circulating pump (11), second circulating pump (12) and depickling still (8), reclaim reaction tower (2) at first phosgene, second phosgene reclaims reaction tower (3), drop in first recirculating still (9) and second recirculating still (10) and reclaim liquid, come the phosgene tail gas that contains phosgene 5.5% of self-contained phosgene 5.5% phosgene exhaust system (1) to enter first phosgene recovery reaction tower (2), by first circulating pump (11) the recovery liquid in first recirculating still (9) is delivered to first phosgene and reclaim reaction tower (2), the phosgene that reclaims in the liquid and first phosgene recovery reaction tower (2) reacts generation phosgenation product, the phosgenation product exports first recirculating still (9) to, along with circulation and temperature control, the phosgenation product design constantly raises in first recirculating still (9);
The gas that comes out from first phosgene recovery reaction tower (2) enters second phosgene recovery reaction tower (3), second circulating pump (12) is delivered to second phosgene with the recovery liquid in second recirculating still (10) and is reclaimed reaction tower (3), the phosgene that reclaims in the liquid and second phosgene recovery reaction tower (3) reacts generation phosgenation product, the phosgenation product exports second recirculating still (10) to, along with circulation and temperature control, the phosgenation product design constantly raises in second recirculating still (10);
The phosgenation product design reaches at 98% o'clock in first recirculating still (9), with the phosgenation transferred product in first recirculating still (9) to depickling still (8), carry out nitrogen by nitrogen pot (14) and blow drum back up to standard acquisition phosgenation product, the phosgenation product is delivered to phosgenation product holding vessel (13);
Phosgenation product in first recirculating still (9) will continue circular response in phosgenation transferred product to the first recirculating still (9) in second recirculating still (10) after shifting, it is 40~50% that second recirculating still (10) shifts the phosgenation product design of coming; When second recirculating still (10) is empty, replenish the new recovery liquid of adding by reclaiming flow container (7) to second recirculating still (10), so repeatedly;
Second phosgene reclaims the phosgene tail gas that reaction tower (3) output contains phosgene 0.5%, and the phosgene tail gas that contains phosgene 0.5% enters to deliver to through buffer (6) after condenser (4) condensation again and contains phosgene 0.5% phosgene exhaust system (5).
2. the recoverying and utilizing method of phosgene in the phosgenation reaction tail gas according to claim 1 is characterized in that: described first phosgene reclaims reaction tower (2) and second phosgene recovery reaction tower (3) is the tower reaction tower of film absorption.
CN2011101012604A 2011-04-22 2011-04-22 Recovery and utilization method of phosgene in phosgenation reaction tail gas Pending CN102258935A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105289247A (en) * 2015-10-20 2016-02-03 安徽广信农化股份有限公司 Stearoyl chloride phosgene recovery method
CN106008268A (en) * 2016-05-18 2016-10-12 江苏蓝丰生物化工股份有限公司 Method for recycling phosgene in tail gas produced through thermo-optical reaction for synthesis of 3,5-dichlorophenyl isocyanate
CN111686556A (en) * 2020-07-31 2020-09-22 济宁康盛彩虹生物科技有限公司 Industrial treatment system and treatment method for solid light tail gas in process of synthesizing fluorinated phase transfer catalyst

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1547482A (en) * 1975-07-15 1979-06-20 Basf Ag Removal of phosgene from off-gas
CN101018596A (en) * 2004-09-13 2007-08-15 巴斯福股份公司 Method for separating hydrogen chloride and phosgene
CN101348252A (en) * 2008-04-25 2009-01-21 甘肃银光化学工业集团有限公司 Phosgene recovery method for toluene diisocyanate production process
CN101348446A (en) * 2008-04-25 2009-01-21 甘肃银光化学工业集团有限公司 Phosgene removing method for TDI production
US20090104099A1 (en) * 2007-10-17 2009-04-23 Au-Yeung Patrick H Rich gas absorption apparatus and method
CN101671273A (en) * 2009-09-18 2010-03-17 天津大学 Method for recycling phosgene in continuous production process of toluene di-isocyanate

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1547482A (en) * 1975-07-15 1979-06-20 Basf Ag Removal of phosgene from off-gas
CN101018596A (en) * 2004-09-13 2007-08-15 巴斯福股份公司 Method for separating hydrogen chloride and phosgene
US20090104099A1 (en) * 2007-10-17 2009-04-23 Au-Yeung Patrick H Rich gas absorption apparatus and method
CN101348252A (en) * 2008-04-25 2009-01-21 甘肃银光化学工业集团有限公司 Phosgene recovery method for toluene diisocyanate production process
CN101348446A (en) * 2008-04-25 2009-01-21 甘肃银光化学工业集团有限公司 Phosgene removing method for TDI production
CN101671273A (en) * 2009-09-18 2010-03-17 天津大学 Method for recycling phosgene in continuous production process of toluene di-isocyanate

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105289247A (en) * 2015-10-20 2016-02-03 安徽广信农化股份有限公司 Stearoyl chloride phosgene recovery method
CN106008268A (en) * 2016-05-18 2016-10-12 江苏蓝丰生物化工股份有限公司 Method for recycling phosgene in tail gas produced through thermo-optical reaction for synthesis of 3,5-dichlorophenyl isocyanate
CN111686556A (en) * 2020-07-31 2020-09-22 济宁康盛彩虹生物科技有限公司 Industrial treatment system and treatment method for solid light tail gas in process of synthesizing fluorinated phase transfer catalyst

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Application publication date: 20111130