CN101337860A - Method and device for recovering low-boiling-point compound from heavy tar of phenylethene - Google Patents
Method and device for recovering low-boiling-point compound from heavy tar of phenylethene Download PDFInfo
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- CN101337860A CN101337860A CNA2008100421166A CN200810042116A CN101337860A CN 101337860 A CN101337860 A CN 101337860A CN A2008100421166 A CNA2008100421166 A CN A2008100421166A CN 200810042116 A CN200810042116 A CN 200810042116A CN 101337860 A CN101337860 A CN 101337860A
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Abstract
The invention provides a method and a device for recovering low-boiling-point materials from a heavy tar of styrene. The method comprises the following steps: feeding a mixture containing styrene and a heavy component into a fine styrene rectification tower; separating styrene from the top of the fine styrene rectification tower; discharging the heavy tar composed of the heavy component and the styrene from the bottom of the tower; pumping to the top of a stripping tower by a heavy tar transfer pump; evaporating light components including the styrene in the heavy tar to the vapor phase by the rising vapor in the stripping tower, and returning to the fine styrene rectification tower from the top of the stripping tower; and condensing the heavy components in the heavy tar to obtain a liquid-phase tar residual liquid, flowing to the bottom of the tower directly, compressing and recycling the tar residual liquid to an evaporator from the bottom of the stripping tower by a tar residual liquid recycle pump, heating and returning to the bottom of the tower, and discharging a portion of the tar residual liquid at the same time. The method can improve the recovery rate of the low-boiling-point materials by 10 to 50% and reduce the content of useful products in the discharge material of the tar residual liquid to achieve larger economic benefit.
Description
Technical field
The present invention relates to a kind of method and apparatus that from the vinylbenzene heavy tar, reclaims low-boiling-point substance.
Background technology
In chemical industry and petrochemical complex, a large amount of producing various polymerization single polymerization monomers, for example, divinyl pentadiene vinylbenzene Vinylstyrene vinyl toluene vinyl acetate between to for plastic acrylate vinylformic acid hydroxyl ester methacrylic ester hydroxyethyl methacrylate ester or the like, in these monomeric rectifying production processes, the capital runs into the problem of monomer autohemagglutination, the speed of autohemagglutination is closely related with rectification temperature. for the supplies consumption of avoiding autohemagglutination to cause as far as possible, the normal engineering treatment method that adopts mainly contains two, the one, adopt rectification under vacuum, reduce rectification temperature as far as possible; The 2nd, add various stoppers, prevent the monomer polymerization loss.The basic demand of stopper has significant inhibition and separates with the purpose product easily, so high boiling chemical commonly used.The high boiling substance of other that bring in the self-aggregate in the monomer rectifying process, polymer, stopper and the production process, these components have just constituted our usually said heavy tar.
Heavy tar for the phenyl ethylene rectification device produces often is called the vinylbenzene heavy tar.This vinylbenzene heavy tar generally has high boiling point, high viscosity, and carried the lower boiling styrene monomer of content 10%-60%, in order to guarantee the operation of rectifier unit continous-stable, in order to reduce the loss of material of purpose product styrene monomer, must solve the problem that reclaims low-boiling-point substance in the heavy tar.
The method of industrial normal employing at present has two kinds, and the one, evaporate extracting heavy tar out by thin-film evaporator, reclaim low boiling component wherein.In production practice, find to evaporate extracting heavy tar out, because thin-film evaporator has rotatable parts with thin-film evaporator, in rectification under vacuum, the sealing of rotatable parts is problems, thereby makes that the reliability of equipment is relatively poor, is difficult to satisfy the requirement of continuous operation and production; The 2nd, evaporate extracting heavy tar out by adiabatic flash, reclaim low boiling component wherein.For example described the method for utilizing adiabatic flash in Chinese patent 02155115.4 and the Chinese patent 02111311.4 and evaporated, reclaimed the cinnamic method and apparatus of low boiling component wherein extracting heavy tar out.But adopt adiabatic flash efficient too low, its mass transfer theory level generally has only 0.3-0.7 less than 1, makes the internal circulating load of vinylbenzene heavy tar heighten, the 30-100 that is almost the thin film evaporation technology doubly, the content of styrene monomer is difficult to drop to and is lower than 10% in the vinylbenzene heavy tar raffinate simultaneously; Be generally 12-16%, the loss of material is bigger, and one 100,000 tons/year styrene device is produced vinylbenzene heavy tar 1000-1500 ton per year, causes to such an extent that the styrene monomer loss has the 120-288 ton, thereby has caused the financial loss of 130-300 ten thousand.
Summary of the invention
The objective of the invention is to propose from the vinylbenzene heavy tar, to reclaim the method and apparatus of low-boiling-point substance,, satisfy the industrial sector needs to overcome the above-mentioned defective that prior art exists.
Method of the present invention comprises the steps:
The mixture that contains vinylbenzene and heavy component enters the refining benzene ethylene rectification tower, isolate vinylbenzene at refining benzene ethylene distillation cat head, discharge the heavy tar that constitutes by heavy constituent and vinylbenzene at the tower still, deliver to carry by the heavy tar transferpump then and heat up in a steamer top of tower, heat up in a steamer in the tower carrying, the steam raising that cinnamic light constituent is risen that comprises in the heavy tar enters vapour phase, heats up in a steamer column overhead and returns the refining benzene ethylene rectification tower by carrying; Heavy constituent condensation in the heavy tar enters liquid phase, is the tar raffinate, through tower still, and the tar raffinate heats up in a steamer tower still bottom and sends out through tar raffinate recycle pump pressurized circulation is heated to vaporizer after and return the tower still, while discharge section tar raffinate by carrying;
The temperature of phenyl ethylene rectification column overhead is 80～100 ℃, and the temperature at the bottom of the phenyl ethylene rectification Tata is 90～120 ℃;
Carry the tower top pressure 12～18kPa that heats up in a steamer tower, temperature is 98～108 ℃, and tower still pressure is that 16～24kPa, temperature are 142～168 ℃, and tar raffinate internal circulating load is 10-50 times of discharge tar content weight;
Contain in the mixture of vinylbenzene and heavy component, cinnamic weight content is 94～99%, the αJia Jibenyixi weight content is 0.01～1%, styrene dimer body weight content is 0.5～1.5%, all the other are other heavy constituent, as vinylbenzene tripolymer and other polymers, stopper nitrophenyl phenolic compounds, for example 2,6-dinitrobenzene-4-tert.-butyl phenol, ditane or diphenylethane etc.; (down together)
In the heavy tar that described refining benzene ethylene distillation Tata still obtains, cinnamic weight content is 10%-60%, and the αJia Jibenyixi weight content is 0.1～10%, and styrene dimer body weight content is 10～60%, and all the other are other heavy constituent;
Carry and heat up in a steamer column overhead and return in the logistics of refining benzene ethylene rectification tower, the vinylbenzene weight content is 40～80%, and the αJia Jibenyixi weight content is 2～10%, and styrene dimer body weight content is 1～8%, and all the other are other heavy constituent;
The vinylbenzene weight content is 0.5～5% in the tar raffinate, and the αJia Jibenyixi weight content is 1～3%, styrene dimer body weight content is 30～68%, other reorganization are divided into 10～26%.
The present invention has adopted a kind of cat head not have carrying of pump circulation heating with condenser, tower still to heat up in a steamer tower and come styrene monomer in the Separation and Recovery vinylbenzene heavy tar raffinate, improve the lower boiling material rate of recovery and improved 10-50%, greatly reduced the content of useful products in the tar raffinate discharge material, cinnamic weight content is reduced to 3% by 12-16%, has bigger economic benefit.Compared with prior art, one 100,000 tons/year styrene device is produced vinylbenzene heavy tar 1000-1500 ton per year, uses present technique and can reduce vinylbenzene loss 100-230 ton, thereby create the economic benefit of 100-230 ten thousand.
Description of drawings
Fig. 1 is device and the schematic flow sheet that reclaims low-boiling-point substance from the vinylbenzene heavy tar.
Embodiment
Referring to Fig. 1, be used to realize that the device of method of the present invention comprises:
Refining benzene ethylene rectification tower 1, heavy tar transferpump 2, carry and heat up in a steamer tower 3, tar raffinate recycle pump 4 and vaporizer 5;
Owing to reclaimed the heavy tar behind the light constituent, viscosity is big, mobile relatively poor, heats up in a steamer in the tower 3 so carry, and is provided with the filler that the strong anti-coking of handling capacity stops up, such as the mellagrid filler of Sulzer company.
The present invention is described further by the following examples.
Adopt device and the flow process of Fig. 1, wherein: carry and heating up in a steamer in the tower 3, be provided with the mellagrid filler of Sulzer company, packed height is 4 meters, carries the vapor phase exit that heats up in a steamer tower 3 cats head and is connected by the stripping section of pipeline with refining benzene ethylene rectification tower 1.
Raw material and processing parameter are as follows:
Contain in the mixture of vinylbenzene and heavy component, cinnamic weight content is 97%, the αJia Jibenyixi weight content is 0.2%, styrene dimer body weight content is 1%, all the other are other heavy constituent, as vinylbenzene tripolymer and other polymers, stopper 2,6-dinitrobenzene-4-tert.-butyl phenol, ditane or diphenylethane etc.;
The temperature of phenyl ethylene rectification column overhead is 80 ℃, and the temperature at the bottom of the phenyl ethylene rectification Tata is 104 ℃;
Carry the tower top pressure 18kPa that heats up in a steamer tower, temperature is 108 ℃, and tower still pressure is that 24kPa, temperature are 158 ℃, and tar raffinate internal circulating load is 10 times of discharge tar content weight;
In the heavy tar that described refining benzene ethylene distillation Tata still obtains, cinnamic weight content is 40%, and the αJia Jibenyixi weight content is 6%, and styrene dimer body weight content is 39.6%, and all the other are other heavy constituent;
Carry and heat up in a steamer column overhead and return in the logistics of refining benzene ethylene rectification tower, the vinylbenzene weight content is 80%, and the αJia Jibenyixi weight content is 10%, and styrene dimer body weight content is 8%, and all the other are other heavy constituent;
The vinylbenzene weight content is 3% in the tar raffinate, and the αJia Jibenyixi weight content is 3%, styrene dimer body weight content is 68%, and other reorganization are divided into 26%.
Adopt above-mentioned processing condition, handle 100,000 tons/year 1000 tons of heavy tars that styrene device produced, can reduce 100 tons of vinylbenzene losses, thereby create 1,000,000 economic benefit.
Adopt device and the flow process of Fig. 1, wherein: carry and heating up in a steamer in the tower 3, be provided with the mellagrid filler of Sulzer company, packed height is 3 meters, carries the vapor phase exit that heats up in a steamer tower 3 cats head and is connected with the tower still of refining benzene ethylene rectification tower 1 by pipeline.
Raw material and processing parameter are as follows:
Contain in the mixture of vinylbenzene and heavy component, cinnamic weight content is 99%, the αJia Jibenyixi weight content is 0.1%, styrene dimer body weight content is 0.6%, all the other are other heavy constituent, as vinylbenzene tripolymer and other polymers, stopper 2,6-dinitrobenzene-4-tert.-butyl phenol, ditane or diphenylethane etc.
The temperature of phenyl ethylene rectification column overhead is 76 ℃, and the temperature at the bottom of the phenyl ethylene rectification Tata is 100 ℃;
Carry the tower top pressure 18kPa that heats up in a steamer tower, temperature is 108 ℃, and tower still pressure is that 24kPa, temperature are 158 ℃, and tar raffinate internal circulating load is 50 times of discharge tar content weight;
In the heavy tar that described refining benzene ethylene distillation Tata still obtains, cinnamic weight content is 60%, and the αJia Jibenyixi weight content is 4%, and styrene dimer body weight content is 26.6%, and all the other are other heavy constituent;
Carry and heat up in a steamer column overhead and return in the logistics of refining benzene ethylene rectification tower, the vinylbenzene weight content is 80%, and the αJia Jibenyixi weight content is 10%, and styrene dimer body weight content is 8%, and all the other are other heavy constituent;
The vinylbenzene weight content is 0.5% in the tar raffinate, and the αJia Jibenyixi weight content is 2.6%, styrene dimer body weight content is 69%, and other reorganization are divided into 27%.
Adopt above-mentioned processing condition, handle 100,000 tons/year 1500 tons of heavy tars that styrene device produced, can reduce 230 tons of vinylbenzene losses, thereby create 2,300,000 economic benefit.
Claims (8)
1. from the vinylbenzene heavy tar, reclaim the method for low-boiling-point substance, it is characterized in that, comprise the steps: that the mixture that contains vinylbenzene and heavy component enters the refining benzene ethylene rectification tower, isolate vinylbenzene at refining benzene ethylene distillation cat head, discharge the heavy tar that constitutes by heavy constituent and vinylbenzene at the tower still, deliver to carry by the heavy tar transferpump then and heat up in a steamer top of tower, heat up in a steamer in the tower carrying, the steam raising that cinnamic light constituent is risen that comprises in the heavy tar enters vapour phase, heats up in a steamer column overhead and returns the refining benzene ethylene rectification tower by carrying; Heavy constituent condensation in the heavy tar enters liquid phase, is the tar raffinate, through tower still, and the tar raffinate heats up in a steamer tower still bottom and sends out through tar raffinate recycle pump pressurized circulation is heated to vaporizer after and return the tower still, while discharge section tar raffinate by carrying.
2. method according to claim 1 is characterized in that, the temperature of phenyl ethylene rectification column overhead is 80～100 ℃, and the temperature at the bottom of the phenyl ethylene rectification Tata is 90～120 ℃;
3. method according to claim 1 is characterized in that, carries the tower top pressure 12～18kPa that heats up in a steamer tower, and temperature is 98～108 ℃, and tower still pressure is that 16～24kPa, temperature are 142～168 ℃,, tar raffinate internal circulating load is 10-50 times of discharge tar content weight.
4. method according to claim 1 is characterized in that, contains in the mixture of vinylbenzene and heavy component, cinnamic weight content is 94～99%, the αJia Jibenyixi weight content is 0.01～1%, and styrene dimer body weight content is 0.5～1.5%, and all the other are other heavy constituent.
5. method according to claim 1, it is characterized in that, in the heavy tar that described refining benzene ethylene distillation Tata still obtains, cinnamic weight content is 10%-60%, the αJia Jibenyixi weight content is 0.1～10%, styrene dimer body weight content is 10～60%, and all the other are other heavy constituent.
6. method according to claim 1 is characterized in that, carries heating up in a steamer column overhead and returning in the logistics of refining benzene ethylene rectification tower, the vinylbenzene weight content is 40～80%, the αJia Jibenyixi weight content is 2～10%, and styrene dimer body weight content is 1～8%, and all the other are other heavy constituent.
7. method according to claim 1 is characterized in that, the vinylbenzene weight content is 0.5～5% in the tar raffinate, and the αJia Jibenyixi weight content is 1～3%, styrene dimer body weight content is 30～68%, other reorganization are divided into 10～26%.
8. realize the device of each described method of claim 1～7, it is characterized in that, comprise refining benzene ethylene rectification tower (1), heavy tar transferpump (2), carry and heat up in a steamer tower (3), tar raffinate recycle pump (4) and vaporizer (5);
Heavy tar transferpump (2) is connected by pipeline with the tower still of described refining benzene ethylene rectification tower (1), the outlet of described heavy tar transferpump (2) is carried the liquid inlet (301) of heating up in a steamer tower 3 cats head and is connected with being arranged on by pipeline, carrying the vapor phase exit that heats up in a steamer tower (3) cat head is connected with the stripping section or the tower still of described refining benzene ethylene rectification tower (1) by pipeline, carrying the tower still that heats up in a steamer tower (3) is connected by the inlet of pipeline with tar raffinate recycle pump (4), the inlet of vaporizer (5) is connected by the outlet of pipeline with tar raffinate recycle pump (4), the outlet of vaporizer (5) by pipeline be arranged on the circulation fluid inlet (302) of carrying the tower still that heats up in a steamer tower (3) and be connected.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2008100421166A CN101337860B (en) | 2008-08-27 | 2008-08-27 | Method and device for recovering low-boiling-point compound from heavy tar of phenylethene |
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| CN2008100421166A CN101337860B (en) | 2008-08-27 | 2008-08-27 | Method and device for recovering low-boiling-point compound from heavy tar of phenylethene |
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| CN103550946A (en) * | 2013-11-15 | 2014-02-05 | 上海赛科石油化工有限责任公司 | Crude styrene separating method for reducing scale formation of crude styrene separation tower still |
| CN104744206A (en) * | 2013-12-30 | 2015-07-01 | 中国石油化工股份有限公司 | Method for extractive distillation recovery of styrene from pyrolysis gasoline C8 fraction |
| CN109438162A (en) * | 2018-10-29 | 2019-03-08 | 江苏常青树新材料科技有限公司 | A kind of divinylbenzene tar recovery system and recovery process |
| CN111056905A (en) * | 2019-12-17 | 2020-04-24 | 安徽昊源化工集团有限公司 | System for recovering effective components in styrene byproduct tar |
| CN113511950A (en) * | 2021-06-29 | 2021-10-19 | 中国石油化工股份有限公司 | Method for efficiently recovering styrene in styrene tar |
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| CN1227197C (en) * | 2002-04-10 | 2005-11-16 | 中国石油化工股份有限公司 | Styrene separation process |
| CN1187300C (en) * | 2002-12-17 | 2005-02-02 | 中国石油化工股份有限公司 | Negative pressure adiabatic flash tank and adiabatic flash vaporizaiton method for tar phenylethylene recovery |
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| CN103550946A (en) * | 2013-11-15 | 2014-02-05 | 上海赛科石油化工有限责任公司 | Crude styrene separating method for reducing scale formation of crude styrene separation tower still |
| CN103550946B (en) * | 2013-11-15 | 2017-02-08 | 上海赛科石油化工有限责任公司 | Crude styrene separating method for reducing scale formation of crude styrene separation tower still |
| CN104744206A (en) * | 2013-12-30 | 2015-07-01 | 中国石油化工股份有限公司 | Method for extractive distillation recovery of styrene from pyrolysis gasoline C8 fraction |
| CN104744206B (en) * | 2013-12-30 | 2016-08-17 | 中国石油化工股份有限公司 | From drippolene C8in fraction, cinnamic method is reclaimed in extractive distillation |
| CN109438162A (en) * | 2018-10-29 | 2019-03-08 | 江苏常青树新材料科技有限公司 | A kind of divinylbenzene tar recovery system and recovery process |
| CN111056905A (en) * | 2019-12-17 | 2020-04-24 | 安徽昊源化工集团有限公司 | System for recovering effective components in styrene byproduct tar |
| CN113511950A (en) * | 2021-06-29 | 2021-10-19 | 中国石油化工股份有限公司 | Method for efficiently recovering styrene in styrene tar |
| CN113511950B (en) * | 2021-06-29 | 2024-05-28 | 中国石油化工股份有限公司 | Method for efficiently recycling styrene in styrene tar |
| CN113599856A (en) * | 2021-08-11 | 2021-11-05 | 安徽晟捷新能源科技有限公司 | Equipment for recycling tar at bottom of NMP (N-methyl pyrrolidone) rectifying tower |
| US20240026231A1 (en) * | 2022-07-22 | 2024-01-25 | T.En Process Technology, Inc. | Systems and methods for enhancing the recovery of styrene |
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Address after: 201102 602, room 41, Lane 1458, long Ming Road, Minhang District, Shanghai. Co-patentee after: CHANGZHOU RUIHUA CHEMICAL ENG & TECH Co.,Ltd. Patentee after: Xu Zhigang Address before: 201102 602, room 41, Lane 1458, long Ming Road, Minhang District, Shanghai. Co-patentee before: CHANGZHOU RUIHUA CHEMICAL ENG&TECH CO.,LTD. Patentee before: Xu Zhigang |
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