CN115414702A - Device and method for removing aluminum trichloride catalyst from carbon five petroleum resin - Google Patents
Device and method for removing aluminum trichloride catalyst from carbon five petroleum resin Download PDFInfo
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- 229920005989 resin Polymers 0.000 title claims abstract description 121
- 239000011347 resin Substances 0.000 title claims abstract description 121
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 52
- 239000003054 catalyst Substances 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 51
- 239000003208 petroleum Substances 0.000 title claims abstract description 39
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 title claims abstract description 38
- 238000000605 extraction Methods 0.000 claims abstract description 156
- 239000007788 liquid Substances 0.000 claims abstract description 125
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 92
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 41
- 230000008569 process Effects 0.000 claims abstract description 23
- 239000003513 alkali Substances 0.000 claims abstract description 20
- 238000002347 injection Methods 0.000 claims abstract description 8
- 239000007924 injection Substances 0.000 claims abstract description 8
- 238000003809 water extraction Methods 0.000 claims abstract description 8
- 230000003068 static effect Effects 0.000 claims abstract description 7
- 230000018044 dehydration Effects 0.000 claims abstract description 5
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 5
- 239000002351 wastewater Substances 0.000 claims description 12
- 239000000945 filler Substances 0.000 claims description 9
- 239000010865 sewage Substances 0.000 claims description 6
- 238000003795 desorption Methods 0.000 claims description 4
- UNSWNZFTRPSXHQ-UHFFFAOYSA-N penta-1,2,3,4-tetraene Chemical compound C=C=C=C=C UNSWNZFTRPSXHQ-UHFFFAOYSA-N 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 238000004945 emulsification Methods 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 238000005406 washing Methods 0.000 description 19
- 239000000243 solution Substances 0.000 description 10
- 230000000694 effects Effects 0.000 description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 8
- 238000003756 stirring Methods 0.000 description 8
- 238000006555 catalytic reaction Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 229920000642 polymer Polymers 0.000 description 5
- 239000004215 Carbon black (E152) Substances 0.000 description 4
- 229930195733 hydrocarbon Natural products 0.000 description 4
- 150000002430 hydrocarbons Chemical class 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 238000000622 liquid--liquid extraction Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000004062 sedimentation Methods 0.000 description 3
- 238000000638 solvent extraction Methods 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 2
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000009849 deactivation Effects 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 238000010907 mechanical stirring Methods 0.000 description 2
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- 238000012986 modification Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- PMJHHCWVYXUKFD-SNAWJCMRSA-N (E)-1,3-pentadiene Chemical group C\C=C\C=C PMJHHCWVYXUKFD-SNAWJCMRSA-N 0.000 description 1
- 229910000975 Carbon steel Inorganic materials 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 239000004831 Hot glue Substances 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 239000004820 Pressure-sensitive adhesive Substances 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000010962 carbon steel Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000010538 cationic polymerization reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- PMJHHCWVYXUKFD-UHFFFAOYSA-N piperylene Natural products CC=CC=C PMJHHCWVYXUKFD-UHFFFAOYSA-N 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0426—Counter-current multistage extraction towers in a vertical or sloping position
- B01D11/043—Counter-current multistage extraction towers in a vertical or sloping position with stationary contacting elements, sieve plates or loose contacting elements
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0488—Flow sheets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0492—Applications, solvents used
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
A device and a method for removing an aluminum trichloride catalyst from carbon five petroleum resin belong to the technical field of carbon five petroleum resin production. The device is characterized in that: the device comprises a first extraction tower (2), a second extraction tower (6) and a resin liquid settling tank (9), wherein the bottom of the second extraction tower (6) is connected to the upper part of the first extraction tower (2) through a first extraction tower water inlet line (5), and a dilute alkali liquid injection line (12) is further connected to the first extraction tower water inlet line (5). The method is characterized in that: carbon penta polymerization liquid from a polymerization unit sequentially and continuously enters a first extraction tower (2) and a second extraction tower (6) for alkaline water extraction and deoxygenated water extraction; the clear resin liquid after the two-step continuous extraction enters a resin liquid settling tank (9) for static settling dehydration. The polymerization liquid in the invention is in countercurrent contact with water, and the water consumption is low. And the process equipment is static equipment such as a tower and the like, so that the emulsification risk is avoided.
Description
Technical Field
A device and a method for removing an aluminum trichloride catalyst from carbon five petroleum resin belong to the technical field of carbon five petroleum resin production.
Background
The carbon five petroleum resin is also called C5 petroleum resin, and is a thermoplastic resin mainly prepared by taking piperylene concentrated solution obtained by separating and purifying byproduct carbon five fraction of ethylene cracking as a raw material and carrying out catalytic polymerization by aluminum trichloride. The weight average molecular weight (Mw) is about 2000, and the modified polyvinyl alcohol is mainly used as tackifying resin to be applied to the fields of hot melt adhesive, pressure-sensitive adhesive, rubber tires, road marking paint and the like.
The production process of the carbon five petroleum resin is a continuous cationic polymerization process, and the catalyst adopts anhydrous aluminum trichloride to produce the m-pentadiene resin.
The production process unit comprises four process units of polymerization, catalyst removal, flash evaporation and granulation.
At present, when most carbon five petroleum resin manufacturers remove a catalyst aluminum trichloride unit, the adopted process scheme is that alkaline water is simply mixed with a polymerization solution, the catalyst aluminum trichloride is converted into aluminum hydroxide which enters a water phase, then the aluminum hydroxide is washed by water to remove the residual alkaline solution in the polymerization solution, and waste water is directly discharged after standing. The alkaline washing unit equipment comprises an alkaline washing kettle and an alkaline washing settling tank, and the water washing unit equipment comprises a water washing kettle and a one-stage or multi-stage water washing settling tank. The materials used included: the water treatment agent comprises alkaline water and hot water, wherein the alkaline water is dilute sodium hydroxide aqueous solution, dilute ammonia water and the like, and the hot water is deionized water, deoxygenated water and the like.
In the scheme, in the alkali washing stirring process, in order to ensure a good washing effect, the stirring frequency needs to be increased, so that the alkali water and the catalyst aluminum trichloride in the polymerization solution are fully mixed, the reaction of the aluminum trichloride and the alkali water is facilitated, and the removal of the catalyst is realized. When the stirring frequency is too high, the system is easy to emulsify, so that water and oil are not uniformly layered to form an emulsifying layer, and drainage carries oil to cause environmental pollution; when the stirring frequency of the alkaline washing kettle is too low, water and the polymerization liquid can not be fully mixed, a large amount of catalyst is remained in the polymerization liquid, the catalysis removing effect of the system is poor, the catalyst residue in the product is increased, the product is dark in color, the ash content is high, and the product quality is influenced.
The invention patent 201410601984.9 of China provides a continuous washing method in the catalysis removing process, which sequentially adopts alkaline water, clean water and ammonia water for washing, wherein the washing temperature is 47-53 ℃, so that the continuous catalysis removing process of petroleum resin is realized, but 2% of sodium hydroxide aqueous solution is still used for washing in the first alkali washing process, and the phenomena of emulsification and incomplete washing cannot be avoided.
The utility model patent 201520574795.7 in China provides a C5 petroleum resin catalyst deactivation and desorption system, does not wash with alkali, adopts washing kettle and tertiary corrosion-resistant material's washing jar, through polymer liquid and hot water mixture, catalyst and water fully react, make the catalyst deactivation, subside through the tertiary, and the catalyst that realizes in the polymer liquid obtains getting rid of completely, but this scheme equipment is many to all need adopt corrosion-resistant material, the investment is great.
The utility model Chinese patent 201920980319.3 has increased vertical water-oil mixer and circulating pump on the basis of patent 201520574795.7, mixes through the circulation many times, increases the mixed effect of hot water and polymerization liquid, but this scheme adopts corrosion-resistant material except that the settling cask, and the blender volume that increases in addition is great, and inside is equipped with the filler, and the material transport pressure drop is great, has increased the circulating pump, has increased equipment investment and consumption of power.
The method ensures the de-catalysis effect in the process of removing the carbon five petroleum resin catalyst and effectively prevents the emulsification phenomenon from generating important significance for the production of the carbon five petroleum resin.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: overcomes the defects of the prior art, and provides a device and a method for removing the aluminum trichloride catalyst from the carbon five petroleum resin, which ensure the catalyst removal effect and effectively prevent the emulsification phenomenon.
The technical scheme adopted by the invention for solving the technical problems is as follows: this device of desorption aluminium trichloride catalyst in five petroleum resin of carbon, its characterized in that:
including first extraction tower, second extraction tower and resin liquid settling cask, the sub-unit connection of first extraction tower have five polymerization liquid lines of carbon, the resin liquid line connection is passed through to the lower part of second extraction tower at first extraction tower top, second extraction tower top is passed through second extraction tower top resin liquid line connection resin liquid settling cask, the upper portion of second extraction tower is connected with the deoxidization water injection line, the bottom of second extraction tower is connected to first extraction tower upper portion through first extraction tower inlet line, still be connected with the dilute alkali liquor injection line on the first extraction tower inlet line.
The invention relates to a continuous extraction device, which utilizes the liquid-liquid extraction principle and can respectively utilize dilute alkaline water and deoxygenated hot water to carry out continuous countercurrent extraction on inorganic aluminum salt in resin liquid by two extraction towers so as to realize the removal of catalyst aluminum trichloride of carbon five resin polymerization liquid. The inside of the whole catalyst removal device is not provided with power consumption equipment such as a pump and stirring equipment; two stages of extraction towers are connected in series, the first stage of extraction tower can recycle the second stage of hot water, and the water consumption is greatly reduced; no forced stirring facility is provided, the risk of water-oil emulsification is eliminated, the equipment can adopt common carbon steel equipment to achieve good removal effect of the catalyst in the resin liquid, the overall investment of the equipment is small, and the economic benefit is good.
The preferable device for removing the aluminum trichloride catalyst from the hydrocarbon-containing petroleum resin is characterized in that a tower internal part of the first extraction tower is a filler, and an oil phase redistributor is arranged among the fillers. The carbon five petroleum resin can be more uniformly dispersed in the dilute alkali liquor, and the extraction efficiency is increased.
The preferable device for removing the aluminum trichloride catalyst from the hydrocarbon-penta petroleum resin is characterized in that a tower internal part of the second extraction tower is a high-efficiency tower plate which is arranged in a sectional manner, and the high-efficiency tower plate is a sieve plate or a floating valve plate. The extraction requirement can be met by passing through the tower plate in the second extraction tower.
The device of desorption aluminium trichloride catalyst in foretell five petroleum resin of carbon of preferred, resin liquid settling cask in be equipped with the coalescer of the free water that condenses, resin liquid settling cask bottom is connected with resin liquid settling cask drainage line, the well lower part of resin liquid settling cask is connected with settling cask resin liquid and is adopted the line. The coalescer is arranged in the resin liquid settling tank, so that trace water in the resin liquid can be well coalesced, and the excessive water is prevented from entering the subsequent process.
A method for removing an aluminum trichloride catalyst in the production of carbon five petroleum resin by using the device is characterized in that:
carbon penta polymerization liquid from a polymerization unit sequentially and continuously enters a first extraction tower and a second extraction tower to carry out alkaline water extraction and deoxygenated water extraction; the clear resin liquid after two-step continuous extraction enters a resin liquid settling tank for static settling dehydration;
the alkaline water extraction is to mix dilute alkaline liquid and hot water from the bottom of the second extraction tower to form mixed alkaline water; the mixed alkaline water is continuously fed from top to bottom in the first extraction tower, the carbon pentamer liquid is fed from bottom to top in the first extraction tower, and the two are in countercurrent contact to carry out extraction mass transfer; wherein the alkali water after mixing is a continuous phase, and the carbon pentapolymer liquid is a dispersed phase;
the deoxygenated water extracted at the temperature of 60-80 ℃ continuously flows down in the second extraction tower from top to bottom, and clear polymerization liquid continuously extracted from the top of the first extraction tower flows up in the second extraction tower from bottom to top; the clear polymerization liquid floats upwards depending on the density of the clear polymerization liquid, and the clear polymerization liquid are in cross flow contact on a tower tray for extraction mass transfer; wherein the deoxygenated water is a continuous phase, and the clear polymerization liquid is a dispersed phase.
The invention adopts a brand new catalyst removal process scheme, utilizes the liquid-liquid extraction principle, and utilizes dilute alkaline water and hot deoxygenated water to respectively carry out continuous countercurrent extraction on inorganic aluminum salt in resin liquid through two extraction towers, thereby realizing the removal of the catalyst aluminum trichloride in the carbon five resin polymerization liquid. Power consumption equipment such as an inorganic pump, stirring and the like in the whole de-catalysis process after the carbon five polymerization solution is contacted with the extraction water; the two extraction towers are connected in series for operation, the first extraction tower recycles the hot water of the second extraction tower, and the water consumption is greatly reduced; the process has no forced stirring process, eliminates the risk of water-oil emulsification, and can achieve good removal effect of the catalyst in the resin liquid.
Preferably, in the method for removing the aluminum trichloride catalyst from the hydrocarbon-containing petroleum resin, the clear polymer solution extracted by the first extraction tower passes through the resin liquid line from the top of the tower and then enters the middle lower part of the tower bottom of the second extraction tower. The clear polymer liquid automatically floats upwards in the dilute alkali liquid and is spontaneously discharged from the top of the tower, and the clear polymer liquid flows into the middle lower part of the tower kettle of the second extraction tower under the action of gravity, so that a power pump is not needed in the process.
Preferably, in the method for removing the aluminum trichloride catalyst from the hydrocarbon-containing petroleum resin, the alkaline waste water of the raffinate in the first extraction tower enters the tower bottom of the first extraction tower and is discharged to subsequent sewage treatment through a wastewater discharge line. And the raffinate waste alkaline water is continuously discharged from the bottom of the tower, so that smooth feeding above the tower is ensured.
Preferably, in the method for removing the aluminum trichloride catalyst from the carbon five petroleum resin, the raffinate wastewater in the second extraction tower enters the tower kettle of the second extraction tower, is mixed with the dilute alkali liquor, and then enters the top of the first extraction tower through the water inlet line of the first extraction tower to serve as the extractant of the first extraction tower. The extraction is completed in the first extraction tower after the raffinate wastewater in the second extraction tower is mixed with the dilute alkali liquor, so that the consumption of hot water can be reduced, and the treatment capacity and the treatment cost of the raffinate wastewater can be reduced.
Preferably, in the method for removing the aluminum trichloride catalyst from the carbon five petroleum resin, the free water condensed in the resin liquid settling tank enters the bottom of the resin liquid settling tank for aggregation, and is discharged to sewage treatment through a drainage line at the bottom of the resin liquid settling tank. The condensed free water spontaneously enters the bottom of the resin liquid sedimentation tank to be accumulated under the action of gravity and can be discharged through simple discharging.
Preferably, in the method for removing the aluminum trichloride catalyst from the carbon five petroleum resin, the carbon five resin liquid after the free water is separated by settling in the resin liquid settling tank is extracted by a resin liquid extraction line of the settling tank to a subsequent process unit for treatment.
Compared with the prior art, the method for removing the aluminum trichloride catalyst in the production of the carbon five petroleum resin has the beneficial effects that:
1. the two-step extraction of the invention adopts a liquid-liquid extraction process, wherein the water phase is a continuous phase, and the polymerization liquid is a dispersed phase; ensuring that the aluminum trichloride catalyst in the polymerization liquid can be fully extracted by the water phase.
2. The invention adopts two stages of extraction towers to be operated in series, wherein the first stage of extraction tower adopts alkaline washing, and the second stage of extraction tower adopts water washing; the extraction is carried out by using dilute alkaline water and hot deoxygenated water in sequence, so that the extraction effect is more thorough. The hot water can be reused before and after the hot water is used, and the water consumption is reduced.
3. The polymerization liquid and the water phase in the two-stage extraction tower are in continuous countercurrent contact, the utilization rate of the water phase as the extraction liquid is high, and the total consumption is low.
4. The two-stage extraction tower process equipment is static equipment such as a tower and the like, rapid forced mechanical stirring is not needed, and the emulsification risk is avoided in the extraction process.
5. The core equipment of the invention adopts the unique sectional design of the internal parts of the extraction tower, the mass transfer effect is good, and the catalyst removal rate is high.
Drawings
The technical solutions of the present invention will be described in further detail below with reference to the accompanying drawings and examples, but it should be understood that these drawings are designed for illustrative purposes only and thus do not limit the scope of the present invention. Furthermore, unless otherwise indicated, the drawings are intended to be illustrative of the structural configurations described herein and are not necessarily drawn to scale.
FIG. l is a schematic diagram of a device for removing the aluminum trichloride catalyst from the hydrocarbon-containing petroleum resin.
The system comprises a carbon five polymerization liquid line 1, a first extraction tower 3, a resin liquid line 4, a wastewater discharge line 5, a first extraction tower water inlet line 6, a second extraction tower 7, a second extraction tower top resin liquid line 8, a deoxygenated water injection line 9, a resin liquid settling tank 10, a resin liquid settling tank water discharge line 11, a settling tank resin liquid extraction line 12 and a dilute alkali liquid injection line.
Detailed Description
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments according to the present application. As used herein, the singular forms "a", "an", and "the" are intended to include the plural forms as well, and furthermore, the terms "comprises" and "having", and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict.
The present invention is further illustrated by the following examples.
Examples
Referring to figure 1:
the device for removing the aluminum trichloride catalyst from the hydrocarbon-penta petroleum resin comprises a first extraction tower 2, a second extraction tower 6 and a resin liquid settling tank 9; the tower internals of the first extraction tower 2 are fillers, and a redistributor of the oil phase is arranged among the fillers; the tower internals of the second extraction tower 6 are high-efficiency tower plates arranged in sections; a coalescer for condensing free water is arranged in the resin liquid settling tank 9, the bottom of the resin liquid settling tank 9 is connected with a drainage line 10 of the resin liquid settling tank, and the middle lower part of the resin liquid settling tank 9 is connected with a resin liquid extraction line 11 of the settling tank.
The sub-unit connection of first extraction tower 2 has five polymerization liquid lines of carbon 1, 2 tops of first extraction tower are connected to the lower part of second extraction tower 6 through resin liquid line 3, 6 tops of second extraction tower pass through second extraction tower top of the tower resin liquid line 7 and connect resin liquid settling cask 9, the upper portion of second extraction tower 6 is connected with deoxidization water and injects the line 8, the bottom of second extraction tower 6 is connected to 2 upper portions of first extraction tower through first extraction tower inlet line 5, still be connected with diluted alkali lye on the first extraction tower inlet line 5 and inject line 12.
The process of removing the aluminum trichloride catalyst by using the device comprises the following steps:
carbon five resin polymerization liquid from a polymerization unit enters a first extraction tower 2 from the bottom of the first extraction tower 2 through a carbon five polymerization liquid line 1, and a pumped dilute alkali liquid is mixed with hot water from the bottom of a second extraction tower 6 through a dilute alkali liquid injection line 12 and a first extraction tower water inlet line 5 and then enters the top of the first extraction tower 2.
The mixed alkaline water continuously flows from top to bottom in the first extraction tower 2, the carbon pentamer solution floats upwards from bottom to top in the first extraction tower 2 and is in countercurrent contact with the carbon pentamer solution for extraction mass transfer without mechanical stirring in the process; wherein, the internal parts of the first extraction tower 2 are high-efficiency fillers, an oil phase redistributor is arranged among the fillers, water is a continuous phase, the polymerization liquid is a dispersed phase, and the extracted clear polymerization liquid passes through the resin liquid line 3 from the top of the first extraction tower 2 and then enters the middle lower part of the tower kettle of the second extraction tower 6. And the raffinate waste alkaline water enters the tower kettle of the first extraction tower 2, is discharged by self-flowing through a waste water discharge line 4, and is subjected to subsequent sewage treatment.
Carbon five resin liquid from the top of the first extraction tower 2 automatically flows into the middle lower part of a tower kettle of a second extraction tower 6 through a resin liquid line 3, and deoxygenated water with pumping pressure and the temperature of 60-80 ℃ enters the second extraction tower 6 from the upper part of the second extraction tower 6 through a deoxygenated water injection line 8. The hot water flows down from top to bottom in the second extraction tower 6, the carbon five resin liquid rises from bottom to top in the second extraction tower 6 depending on the density of the carbon five resin liquid, and the carbon five resin liquid are in cross flow contact on a tower tray to carry out extraction mass transfer. Wherein, the tower internal parts of the second extraction tower 6 are high-efficiency tower plates which are arranged in a sectional way, the type of the tower plates is a sieve plate, water is a continuous phase, and the resin liquid is a dispersed phase.
The extracted clear resin liquid enters a resin liquid settling tank 9 from a resin liquid line 7 at the top of the second extraction tower for static settling and dehydration. The raffinate wastewater in the second extraction tower 6 enters the tower kettle of the second extraction tower 6 and enters the tower top of the first extraction tower 2 through a water inlet line 5 of the first extraction tower to be used as an extractant of the former tower. The carbon five resin liquid from the top of the second extraction tower 6 enters a resin liquid settling tank 9 through a resin liquid line 7 at the top of the second extraction tower for static settling and dehydration. A micro water coalescer is arranged in the tank, condensed free water enters the bottom of the resin liquid settling tank 9 for gathering and is discharged to sewage treatment through a drainage line 10 of the resin liquid settling tank. The resin liquid of the carbon five after the free water is separated by sedimentation is extracted to a subsequent process unit for treatment through a resin liquid extraction line 11 of the sedimentation tank.
The foregoing is directed to preferred embodiments of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow. However, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the protection scope of the technical solution of the present invention.
Claims (10)
1. The utility model provides a device of desorption aluminium trichloride catalyst in five petroleum resin of carbon which characterized in that:
including first extraction tower (2), second extraction tower (6) and resin liquid settling cask (9), the sub-unit connection of first extraction tower (2) have five polymerization liquid lines of carbon (1), resin liquid line (3) are connected to the lower part of second extraction tower (6) are passed through at first extraction tower (2) top, second extraction tower (6) top is passed through second extraction tower top resin liquid line (7) and is connected resin liquid settling cask (9), the upper portion of second extraction tower (6) is connected with deoxidization water and injects line (8), the bottom of second extraction tower (6) is connected to first extraction tower (2) upper portion through first extraction tower water inlet line (5), still be connected with diluted alkali liquid injection line (12) on first extraction tower water inlet line (5).
2. The device for removing the aluminum trichloride catalyst from the carbon five petroleum resin according to claim 1, which is characterized in that:
the tower internals of the first extraction tower (2) are fillers, and an oil phase redistributor is arranged among the fillers.
3. The device for removing the aluminum trichloride catalyst from the carbon five petroleum resin according to claim 1, which is characterized in that:
the tower internals of the second extraction tower (6) are high-efficiency tower plates arranged in a segmented mode, and the high-efficiency tower plates are sieve plates or floating valve plates.
4. The device for removing the aluminum trichloride catalyst from the carbon five petroleum resin according to claim 1, which is characterized in that:
the resin liquid settling tank (9) in be equipped with the coalescer of the free water that condenses, resin liquid settling tank (9) bottom is connected with resin liquid settling tank drain line (10), the well sub-unit connection of resin liquid settling tank (9) has settling tank resin liquid to adopt line (11).
5. A method for removing aluminum trichloride catalyst from carbopenta petroleum resin using the apparatus of any of claims 1~4, comprising:
carbon penta polymerization liquid from a polymerization unit sequentially and continuously enters a first extraction tower (2) and a second extraction tower (6) for alkaline water extraction and deoxygenated water extraction; the clear resin liquid after the two-step continuous extraction enters a resin liquid settling tank (9) for static settling and dehydration;
the alkaline water extraction is to mix dilute alkaline liquid and hot water from the bottom of the second extraction tower (6) to form mixed alkaline water; the mixed alkaline water continuously flows from top to bottom in the first extraction tower (2), the carbon pentamer liquid flows from bottom to top in the first extraction tower (2), and the two are in countercurrent contact for extraction mass transfer; wherein the alkali water after mixing is a continuous phase, and the carbon pentapolymer liquid is a dispersed phase;
the deoxygenated water extracted at the temperature of 60-80 ℃ continuously flows down in the second extraction tower (6) from top to bottom, and clear polymerization liquid continuously extracted from the top of the first extraction tower (2) flows up in the second extraction tower (6); the clear polymerization liquid floats upwards depending on the density of the clear polymerization liquid, and the clear polymerization liquid are in cross flow contact on a tower tray for extraction mass transfer; wherein, the deoxygenated hot water is a continuous phase, and the clear polymerization liquid is a dispersed phase.
6. The method for removing the aluminum trichloride catalyst from the carbon five petroleum resin as claimed in claim 5, wherein the method comprises the following steps:
and the clear polymerization liquid extracted by the first extraction tower (2) enters the middle lower part of the tower kettle of the second extraction tower (6) from the top of the tower through a resin liquid line (3).
7. The method for removing the aluminum trichloride catalyst from the carbon five petroleum resin as claimed in claim 5, wherein the method comprises the following steps:
and the raffinate alkali waste water of the first extraction tower (2) enters the tower kettle of the first extraction tower (2) and is discharged to subsequent sewage treatment through a waste water discharge line (4).
8. The method for removing the aluminum trichloride catalyst from the carbon five petroleum resin as claimed in claim 5, wherein the method comprises the following steps:
and the raffinate wastewater in the second extraction tower (6) enters the tower kettle of the second extraction tower (6), is mixed with dilute alkali liquor and then enters the top of the first extraction tower (2) through a first extraction tower water inlet line (5) to be used as an extracting agent of the first extraction tower (2).
9. The method for removing the aluminum trichloride catalyst from the carbon five petroleum resin as claimed in claim 5, wherein the method comprises the following steps:
and the free water condensed in the resin liquid settling tank (9) enters the bottom of the resin liquid settling tank (9) for gathering and is discharged to sewage treatment through a drainage line (10) of the resin liquid settling tank.
10. The method for removing the aluminum trichloride catalyst from the carbon five petroleum resin as claimed in claim 5, wherein the method comprises the following steps:
and the carbon five resin liquid obtained after the free water is settled and separated by the resin liquid settling tank (9) is extracted to a subsequent process unit for treatment through a resin liquid extraction line (11) of the settling tank.
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| CN202211381375.8A CN115414702A (en) | 2022-11-07 | 2022-11-07 | Device and method for removing aluminum trichloride catalyst from carbon five petroleum resin |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB797386A (en) * | 1956-04-25 | 1958-07-02 | Exxon Research Engineering Co | Petroleum resins from solvent extracted fractions |
| US3198777A (en) * | 1959-06-10 | 1965-08-03 | Stamicarbon | Process for purifying polymers |
| GB1010302A (en) * | 1961-06-06 | 1965-11-17 | Hibernia Chemie G M B H | Improvements in or relating to a process for the purification of poly-olefins |
| US5206358A (en) * | 1991-03-14 | 1993-04-27 | Maruzen Petrochemical Co., Ltd. | Process for manufacturing petroleum resin |
| CN102816280A (en) * | 2012-08-29 | 2012-12-12 | 宁波甬华树脂有限公司 | Preparation method of diisobutylene modified C5 petroleum resin |
| CN112827215A (en) * | 2020-12-31 | 2021-05-25 | 华东理工大学 | Cyclone extraction method and device for C5 petroleum resin polymerization liquid |
-
2022
- 2022-11-07 CN CN202211381375.8A patent/CN115414702A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB797386A (en) * | 1956-04-25 | 1958-07-02 | Exxon Research Engineering Co | Petroleum resins from solvent extracted fractions |
| US3198777A (en) * | 1959-06-10 | 1965-08-03 | Stamicarbon | Process for purifying polymers |
| GB1010302A (en) * | 1961-06-06 | 1965-11-17 | Hibernia Chemie G M B H | Improvements in or relating to a process for the purification of poly-olefins |
| US5206358A (en) * | 1991-03-14 | 1993-04-27 | Maruzen Petrochemical Co., Ltd. | Process for manufacturing petroleum resin |
| CN102816280A (en) * | 2012-08-29 | 2012-12-12 | 宁波甬华树脂有限公司 | Preparation method of diisobutylene modified C5 petroleum resin |
| CN112827215A (en) * | 2020-12-31 | 2021-05-25 | 华东理工大学 | Cyclone extraction method and device for C5 petroleum resin polymerization liquid |
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