CN102336432A - Separation method for recovering olefin polymerization catalyst mother liquid - Google Patents
Separation method for recovering olefin polymerization catalyst mother liquid Download PDFInfo
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- CN102336432A CN102336432A CN2010102388367A CN201010238836A CN102336432A CN 102336432 A CN102336432 A CN 102336432A CN 2010102388367 A CN2010102388367 A CN 2010102388367A CN 201010238836 A CN201010238836 A CN 201010238836A CN 102336432 A CN102336432 A CN 102336432A
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Abstract
The invention discloses a separation method for recovering olefin polymerization catalyst mother liquid, and the separation method comprises the following working procedures of: (1), sending the catalyst mother liquid into a first fractionating tower C1; (2), returning a titanium tetrachloride gas phase evaporated by a scraped film evaporator to the tower kettle of the first fractionating tower from the top, extracting a high-boiling substance containing titanium tetrachloride at a tower bottom, and discharging the material from the bottom of the scraped film evaporator; and (3), sending the mixture of a hydrocarbon solvent and titanium tetrachloride into a second fractionating tower C2. The method has the following advantages: firstly, process flow is short, the quantity of equipment is reduced and investment in devices ia lowered, and furthermore the problem that the high-boiling substance blocks the towers is solved; secondly, the recovery rate of the titanium tetrachloride is improved, and the emission of wastewater and waste slag is reduced; and thirdly, the repeated condensation and evaporation of titanium tetrachloride are avoided, and the energy consumption of the devices is decreased.
Description
Technical field
The present invention relates to the separation method that a kind of olefin polymerization catalysis mother liquor reclaims, promptly polyolefin catalyst prepares the separation method that contains materials such as hydrocarbon solvent, titanium tetrachloride and high boiling material that produces in the process.
Background technology
Titanium tetrachloride is the important source material of fine chemistry industry, also is the important source material of synthesis of polyolefins catalyzer.Titanium tetrachloride can also be used to make titanium salt, iris agent, olivet, smoke screen, pigment, fabric mordant etc.
The preparation of general polyolefin catalyst is to adopt the solid carrier of liquid phase titanium tetrachloride and magnesium-containing compound or catalyst mix to contact to reach certain hour to obtain highly active Ziegler-Natta catalyst component; Again the ingredient of solid catalyst that obtains is washed with hydrocarbon solvent; To remove the titanium tetrachloride that wherein is not written into; Catalyst slurry is discharged from reactor drum; Produced liquid phase materials such as containing hydrocarbon solvent, titanium tetrachloride and high boiling material simultaneously, be the catalyzer mother liquor, high boiling material mainly comprises high boiling substances such as chlorination alkyl titanium, fat.The at present domestic industrialized technology that from the polyolefin catalyst mother liquor, reclaims hydrocarbon solvent and titanium tetrachloride is following: the mixture that will contain hydrocarbon solvent, titanium tetrachloride and high boiling material is sent in the mother liquor rough segmentation tower; Cat head obtains thick hydrocarbon solvent; At the bottom of the tower titanium tetrachloride and high boiling material; Again respectively through the hydrocarbon solvent rectifying tower with after the titanium tetrachloride rectifying tower separates, hydrocarbon solvent that obtains and titanium tetrachloride product, the material of hydrocarbon solvent rectifying tower and titanium tetrachloride rectifying Tata still get into retort and further distill; The back is separated, neutralized to the raffinate that contains titanium tetrachloride and high boiling material of discharging at the bottom of the retort, the kettle washing water that anhydrates as waste water and waste residue discharge.The shortcoming of this technology is that technical process is complicated; High boiling material in the mother liquor is ability discharge system in the retort of whole flow process end; Can result in blockage to the tower internals of its process, reboiler etc., secondly be that retort is operating as periodical operation, and the material evaporation is through the chuck heat exchange; Efficient is lower, and plant energy consumption is higher; The another one shortcoming is under the recovery condition with higher of titanium tetrachloride; The content of the high boiling material in the tower still material is higher, and high boiling material content when higher material viscosity higher, mobile poor; The coking of still wall can be caused in the following residence time of the condition of high temperature than length, the parking of device will be caused.For fear of blocking up the parking that tower and the coking of still wall cause; Just need guarantee the flowability of material through the recovery that reduces titanium tetrachloride; Titanium tetrachloride content is higher in the raffinate of therefore discharging at the bottom of the mother liquor retort; Not only caused the waste of raw material, also increased three wastes treatment capacity, running cost is higher.
Summary of the invention
Stop up, install material consumption, energy consumption problem of higher, the separation method that the present invention provides a kind of improved olefin polymerization catalysis mother liquor to reclaim for solving the tower that exists in the prior art.
The object of the invention provides the separation method that a kind of improved olefin polymerization catalysis mother liquor reclaims, and includes following operation:
Operation (1):
The catalyzer mother liquor that will contain components such as hydrocarbon solvent, titanium tetrachloride and high boiling material is sent into the first separation column C1; The cat head gas phase is the mixture of hydrocarbon solvent and titanium tetrachloride; After condensing surface E1 condensation, the material of 30%～80% in the condensation liquid phase returns cat head as the backflow of first separation column, and remaining phlegma is from the cat head extraction of first separation column; Get into after-fractionating tower middle part through pump or through modes such as surge tanks, as the charging of after-fractionating tower;
Operation (2):
The first separation column reboiler adopts luwa evaporator B2 and Vertical Thermosyphon Reboiler B1 parallel connection in the operation (1); Perhaps only adopt the reboiler of luwa evaporator B2 as first separation column; The bottoms material gets into luwa evaporator and can send into through pump or potential difference; The titanium tetrachloride gas phase of luwa evaporator evaporation is returned the first fractionation Tata still from the top, extraction is the high boiling material that contains titanium tetrachloride at the bottom of the tower, from the luwa evaporator bottom discharge;
Operation (3):
The hydrocarbon solvent that operation (1) is obtained and the mixture of titanium tetrachloride are sent into after-fractionating tower C2; The cat head gas phase is a hydrocarbon solvent; After condensing surface E2 condensation; The material of 40%～80% in the condensation liquid phase returns cat head as the backflow of after-fractionating tower, and remaining phlegma is to reclaim the cat head extraction of product from the after-fractionating tower as hydrocarbon solvent; Extraction titanium tetrachloride product at the bottom of the tower.
The first separation column C1 can carry out under pressure-fired, also can under vacuum, carry out.Its working pressure scope is at 0.001～0.15MPa, and preferred 0.001～0.12MPa, number of theoretical plate are between 3～80, between preferred 10～50.The scope of weight ratio that gets into hydrocarbon solvent and the titanium tetrachloride of first separation column is 0.002～1, preferable range 0.005～0.5.(under the little situation of ratio than titanium tetrachloride of hydrocarbon solvent, the first separation column bottoms material is more relatively, and this moment is more valuable with the recovery that this stripping technique improves titanium tetrachloride.)
The working pressure scope of after-fractionating tower C2 is at 0.001～0.15MPa, and preferred 0.01～0.12MPa, number of theoretical plate are between 3～80, between preferred 10～50.
The working pressure of luwa evaporator is between 0.001～0.15MPa, and operating temperature range is between 100 ℃～152 ℃, and the thermal medium of luwa evaporator chuck is water vapor or heat conduction wet goods.
The tower still material of first separation column needs from luwa evaporator bottom extraction not directly from the extraction of tower still in this technical process.
Hydrocarbon solvent of the present invention is mainly C6 and/or C7 material from petrochemical complex, preferably hexane, hexanaphthene or heptane.Described high boiling material mainly comprises following several kinds of materials:
Optional conventional electron donor compound is like aliphatics (two) ester and/or aromatics (two) ester and their verivate.
The high boiling material of olefin polymerization catalysis mother liquor generally is the product of one or more titanium tetrachlorides and any electron donor compound be combined into.
Adopt the present invention can reduce the number of devices of device; To compare the heavy-gravity high boiling material separates at first separation column; And tower still reboiler adopts luwa evaporator, and the titanium tetrachloride gas phase of evaporation is returned first separation column, has improved the recovery of titanium tetrachloride; Avoid the evaporation repeatedly and the condensation of titanium tetrachloride in the multitower flow process simultaneously, reduced energy consumption.Discharge system owing to contain the high boiling material of titanium tetrachloride at the bottom of the tower as refuse; Common treatment process is that first water is hydrolyzed; Hydrolyzed product comprises the organism of Ti (OH) 4, HCl and some ester classes; With sodium hydroxide solution acid is neutralized again, finally formed the waste liquid that contains solid slag, as three waste discharge.Therefore the recovery of titanium tetrachloride improves, and the three wastes treatment capacity of whole device will decrease, and like this, the titanium tetrachloride consumption of device reduces, and has practiced thrift the running cost of device, has reduced the pollution of three waste discharge to environment simultaneously.
Sharpest edges of the present invention are that technical process is short, have reduced number of devices, have practiced thrift plant investment, have also solved the problem of the stifled tower of high boiling material; It two is to have improved the titanium tetrachloride recovery, and has reduced the quantity discharged of waste water and waste residue; It three is repeats condensation and evaporations of having avoided titanium tetrachloride, has reduced plant energy consumption.
Description of drawings
Fig. 1 is the separation method schema that olefin polymerization catalysis mother liquor of the present invention reclaims, and containing of the main code name among the figure means:
The C1-first separation column E1-first separation column condensing surface
The C2-after-fractionating tower E2-first separation column condensing surface
The P1-first fractionation Tata still pump B1-first separation column reboiler
B2-luwa evaporator B3-after-fractionating tower reboiler
Embodiment
Below in conjunction with accompanying drawing the separation method that olefin polymerization catalysis mother liquor of the present invention reclaims is done further explanation.
Separation method of the present invention comprises operation (1), operation (2) and operation (3); In operation (1); The catalyzer mother liquor that contains components such as hydrocarbon solvent, titanium tetrachloride and high boiling material is sent into the first separation column C1 through pipeline 1, and the cat head gas phase is the mixture of hydrocarbon solvent and titanium tetrachloride, after pipeline 2 entering overhead condenser E1 condensations; The part that refluxes is returned cat head through pipeline 3, and extraction is partly through the charging of pipeline 4 (or through pump) as after-fractionating tower C2; The first fractionation Tata still material gets into the reboiler heating and gasifying; Return the tower still again; The first separation column reboiler form can adopt luwa evaporator B2 and Vertical Thermosyphon Reboiler B1 parallel connection; Perhaps only adopt the reboiler of luwa evaporator B2 as first separation column, the bottoms material gets into luwa evaporator and can send into through pipeline 6 or potential difference through pump, and the titanium tetrachloride gas phase of luwa evaporator evaporation is returned the first fractionation Tata still from the top through pipeline 7; Extraction W1 contains the high boiling material of titanium tetrachloride at the bottom of the tower, from luwa evaporator bottom through pipeline 8 dischargings; After-fractionating tower C2 is used for separate hydrocarbons solvent and titanium tetrachloride; Hydrocarbon solvent and titanium tetrachloride boiling point differ bigger; Be easier to separate, the cat head extraction is a hydrocarbon solvent, and overhead gas passes through pipeline 9 mutually after condensing surface E2 condensation; The part that refluxes is returned cat head through pipeline 10, and another part S1 is as the solvent product extraction; Extraction S2 is the titanium tetrachloride product that contains micro-hydrocarbon solvent at the bottom of the tower.
Below in conjunction with embodiment, further specify the present invention.
Embodiment 1
A kind of mother liquor of polyolefin catalyst, wherein the content of titanium tetrachloride is 80% (weight), the content of hexane is 15%; The content of heavy constituent high boiling material is 5%, gets into first separation column through pipeline 1, and inlet amount is 1000kg/h; First separation column is a packing tower, and filler is selected the IMTP25# dumped packing for use, and the number of theoretical plate of this tower is 15; Tower top pressure is 105KPa, and the titanium tetrachloride of cat head extraction and hexane fraction are sent into after-fractionating tower C2 through pipeline 4, and the bottoms material gets into luwa evaporator; Gas phase is returned first separation column; Extraction contains the high boiling material of part titanium tetrachloride at the bottom of the luwa evaporator, and high boiling material and titanium tetrachloride weight ratio are 3.61, handles the back as useless discharge at night through hydrolysis etc.The working pressure of after-fractionating tower C2 is 105KPa, and the number of theoretical plate of this tower is 30, cat head extraction hexane fraction S1, extraction titanium tetrachloride S2 at the bottom of the tower.Adopt the inventive method, the water coolant of device, water vapor consumption and the titanium tetrachloride recovery are seen table 1.
Comparative Examples 1
The mixture that will contain hexane, titanium tetrachloride and high boiling material is sent in the mother liquor rough segmentation tower, and wherein the content of titanium tetrachloride is 80% (weight), and the content of hexane is 15%; The content of heavy constituent high boiling material is 5%; Inlet amount is 1000kg/h, and mother liquor rough segmentation cat head obtains thick hexane, is titanium tetrachloride and high boiling material at the bottom of the tower; Again respectively through the hexane rectifying tower with after the titanium tetrachloride rectifying tower separates; Hexane that obtains and titanium tetrachloride product, the material of hexane rectifying tower and titanium tetrachloride rectifying Tata still get into retort and further distill, the raffinate that contains titanium tetrachloride and high boiling material of discharging at the bottom of the retort.The operation of equipment condition adopts this method all with embodiment 1, and the cooling water and steam consumption titanium tetrachloride recovery of device is seen table 1.
Table 1
| Embodiment 1 | Comparative Examples 1 | |
| Steam consumption (kg/h) | 446.4 | 476.74 |
| Cooling water amount (kg/h) | 36106.5 | 39435.9 |
| The titanium tetrachloride recovery | 98.27 | 89.08 |
Can find out that from table 1 steam consumption of embodiment 1 and cooling water amount are starkly lower than steam consumption and the cooling water amount in the Comparative Examples 1, can explain thus and adopt the inventive method and the mother liquor reclaiming method that uses at present to compare, reduce the energy consumption of device.In addition, the recovery of titanium tetrachloride also is significantly improved.
Embodiment 2
A kind of mother liquor of polyolefin catalyst, wherein the content of titanium tetrachloride is 85% (weight), the content of hexane is 10%; The content of heavy constituent high boiling material is 5%, gets into first separation column through pipeline 1, and inlet amount is 1000kg/h; First separation column is a packing tower, and rectifying section is selected IMTP 25# dumped packing for use with profit reduction and reserving Duan Jun, and the number of theoretical plate of this tower is 15; Tower top pressure is 50KPa, and tower bottom pressure is 80KPa, and the titanium tetrachloride of cat head extraction and hexane fraction are sent into after-fractionating tower C2 through pipeline 4; The bottoms material gets into luwa evaporator, and the luwa evaporator working pressure is 60KPa, and the gas phase of luwa evaporator evaporation is returned first separation column; Extraction contains the high boiling material of part titanium tetrachloride from luwa evaporator bottom, handles the back as useless discharge at night through hydrolysis etc.The working pressure of after-fractionating tower C2 is 50KPa, and the number of theoretical plate of this tower is 30, cat head extraction hexane fraction S1, extraction titanium tetrachloride S2 at the bottom of the tower.Adopt the inventive method, its method flow is referring to Fig. 1, and table 2 has provided the mass flow and the composition of each equipment of turnover in present method flow process.Table 2
Claims (7)
1. the separation method that reclaims of an olefin polymerization catalysis mother liquor includes following operation:
Operation (1):
The catalyzer mother liquor that will contain components such as hydrocarbon solvent, titanium tetrachloride and high boiling material is sent into the first separation column C1; The cat head gas phase is the mixture of hydrocarbon solvent and titanium tetrachloride; After condensing surface E1 condensation, the material of 30%～80% in the condensation liquid phase returns cat head as the backflow of first separation column, and remaining phlegma is from the cat head extraction of first separation column; Get into after-fractionating tower middle part, as the charging of after-fractionating tower;
Operation (2):
The first separation column reboiler adopts luwa evaporator B2 and Vertical Thermosyphon Reboiler B1 parallel connection in the operation (1); Perhaps only adopt the reboiler of luwa evaporator B2 as first separation column; The bottoms material gets into luwa evaporator and sends into through pump or potential difference; The titanium tetrachloride gas phase of luwa evaporator evaporation is returned the first fractionation Tata still from the top, extraction is the high boiling material that contains titanium tetrachloride at the bottom of the tower, from the luwa evaporator bottom discharge;
Operation (3):
The hydrocarbon solvent that operation (1) is obtained and the mixture of titanium tetrachloride are sent into after-fractionating tower C2; The cat head gas phase is a hydrocarbon solvent; After condensing surface E2 condensation; The material of 40%～80% in the condensation liquid phase returns cat head as the backflow of after-fractionating tower, and remaining phlegma is to reclaim the cat head extraction of product from the after-fractionating tower as hydrocarbon solvent; Extraction titanium tetrachloride product at the bottom of the tower.
2. separation method according to claim 1, wherein:
The first separation column C1 carries out under pressure-fired or vacuum, and the working pressure scope is at 0.001～0.15MPa, and preferred 0.001～0.12MPa, number of theoretical plate are between 3～80, between preferred 10～50.
3. separation method according to claim 2, wherein:
The first separation column C1 working pressure scope is at 0.001～0.12MPa, and number of theoretical plate is between 10～50.
4. separation method according to claim 1, wherein:
The working pressure scope of after-fractionating tower C2 is at 0.001～0.15MPa, and preferred 0.01～0.12MPa, number of theoretical plate are between 3～80, between preferred 10～50.
5. separation method according to claim 4, wherein:
The working pressure scope of after-fractionating tower C2 is at 0.01～0.12MPa, and number of theoretical plate is between 10～50.
6. separation method according to claim 4, the working pressure of wherein said luwa evaporator are between 0.001～0.15MPa, and operating temperature range is between 100 ℃～152 ℃, and the thermal medium of luwa evaporator chuck is water vapor or thermal oil.
7. separation method according to claim 1, the scope of weight ratio that wherein gets into hydrocarbon solvent and the titanium tetrachloride of first separation column is 0.002～1, preferable range 0.005～0.5.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102897830A (en) * | 2011-07-29 | 2013-01-30 | 中国石油化工股份有限公司 | Recovery method of polyolefin catalyst mother liquid |
| CN104438277A (en) * | 2013-09-16 | 2015-03-25 | 中国石油化工股份有限公司 | Method for producing waste residue by titanium-containing organic catalyst |
| CN105566028A (en) * | 2014-10-13 | 2016-05-11 | 中国石油化工股份有限公司 | Separation system and separation method for mother liquor of polyolefin catalyst |
| CN108635889A (en) * | 2018-07-05 | 2018-10-12 | 中冶焦耐(大连)工程技术有限公司 | A kind of light benzene evaporating column in benzene hydrogenation system and its working method |
| CN108939593A (en) * | 2018-09-30 | 2018-12-07 | 天津中福环保科技股份有限公司 | High-solidification point high viscosity solvent recyclable device, its skid structure and method in a kind of dangerous waste process field |
| CN108939591A (en) * | 2018-09-29 | 2018-12-07 | 天津中福环保科技股份有限公司 | Heavy solvent recyclable device, its skid structure and heavy solvent recovery method in a kind of dangerous waste process field |
| CN111111248A (en) * | 2018-10-30 | 2020-05-08 | 中国石油化工股份有限公司 | Device and method for recovering toluene from organic solvent for preparing polyolefin catalyst |
| CN112704894A (en) * | 2019-10-25 | 2021-04-27 | 中国石油化工股份有限公司 | Catalyst solvent recovery method and titanium-containing solid |
| CN113636592A (en) * | 2020-04-27 | 2021-11-12 | 中国石油化工股份有限公司 | Resourceful treatment equipment and method for polyolefin catalyst mother liquor |
| CN113636906A (en) * | 2020-04-27 | 2021-11-12 | 中国石油化工股份有限公司 | Method for purifying titanium-containing filtrate |
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| CN102897830A (en) * | 2011-07-29 | 2013-01-30 | 中国石油化工股份有限公司 | Recovery method of polyolefin catalyst mother liquid |
| CN104438277A (en) * | 2013-09-16 | 2015-03-25 | 中国石油化工股份有限公司 | Method for producing waste residue by titanium-containing organic catalyst |
| CN104438277B (en) * | 2013-09-16 | 2016-06-29 | 中国石油化工股份有限公司 | A kind of titaniferous organic catalyst produces the processing method of waste residue |
| CN105566028A (en) * | 2014-10-13 | 2016-05-11 | 中国石油化工股份有限公司 | Separation system and separation method for mother liquor of polyolefin catalyst |
| CN108635889A (en) * | 2018-07-05 | 2018-10-12 | 中冶焦耐(大连)工程技术有限公司 | A kind of light benzene evaporating column in benzene hydrogenation system and its working method |
| CN108635889B (en) * | 2018-07-05 | 2023-08-25 | 中冶焦耐(大连)工程技术有限公司 | Light benzene evaporation tower in benzene hydrogenation system and working method thereof |
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| CN111111248A (en) * | 2018-10-30 | 2020-05-08 | 中国石油化工股份有限公司 | Device and method for recovering toluene from organic solvent for preparing polyolefin catalyst |
| CN111111248B (en) * | 2018-10-30 | 2021-10-15 | 中国石油化工股份有限公司 | Device and method for recovering toluene from organic solvent for preparing polyolefin catalyst |
| CN112704894A (en) * | 2019-10-25 | 2021-04-27 | 中国石油化工股份有限公司 | Catalyst solvent recovery method and titanium-containing solid |
| CN113636592A (en) * | 2020-04-27 | 2021-11-12 | 中国石油化工股份有限公司 | Resourceful treatment equipment and method for polyolefin catalyst mother liquor |
| CN113636906A (en) * | 2020-04-27 | 2021-11-12 | 中国石油化工股份有限公司 | Method for purifying titanium-containing filtrate |
| CN113636906B (en) * | 2020-04-27 | 2024-02-02 | 中国石油化工股份有限公司 | Purifying method of titanium-containing filtrate |
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