CN103657121B - A kind of renovation process of extracting, rectifying and separating phenylethylene solvent for use - Google Patents
A kind of renovation process of extracting, rectifying and separating phenylethylene solvent for use Download PDFInfo
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Abstract
A kind of renovation process of extracting, rectifying and separating phenylethylene process solvent for use, comprise and will pass in the middle part of extractive distillation column containing cinnamic hydrocarbon mixture, extraction distillation solvent passes into extractive distillation column top and carries out extracting rectifying, be rich in cinnamic rich solvent and enter solvent recovery tower from the discharge of extracting rectifying tower bottom, the lean solvent part that solvent recovery tower flows out returns extractive distillation column, another part passes in the heat exchanger tube of falling film evaporator, solvent and low-boiling point material evaporation is made to enter solvent regeneration tower by decompression falling film evaporation, in solvent regeneration tower, high-boiling-point impurity is in a liquid state and is discharged by bottom line, the regenerated solvent of gas phase is discharged by overhead line, pressure in described falling film evaporator heat exchanger tube is 10 ~ 30kPa, temperature is 120 ~ 145 DEG C.This method effectively can remove the high-boiling-point impurity in lean solvent at a lower temperature, prevents cinnamic high temperature polymerization, extends the cycle of operation of extracting, rectifying and separating phenylethylene device.
Description
Technical field
The present invention relates to a kind of renovation process of separation of extractive distillation hydrocarbon product solvent for use, specifically, is a kind of renovation process of extracting, rectifying and separating phenylethylene solvent for use.
Background technology
Extraction and extracting rectifying are widely used in aromatics separation (benzene,toluene,xylene), styrene and butadiene from hydrocarbon mixture.In extraction process, keep the long-period stable operation of the product of extractant confrontation raising separation and recovery product purity, the rate of recovery and device all extremely important.
From without separating phenylethylene the drippolene of hydrogenation, feasible method adopts extracting rectifying.Extracting rectifying process has two key problem in technology, and one is solvent, and the performance of solvent comprises selective, boiling point, thermo-chemical stability and solvent to cinnamic polymerization inhibition performance etc., has vital impact to process technology economic indicator.Next how effectively to suppress styrene polymerization, and this is related to that can device long-period stable operation.In order to suppress styrene polymerization, except screening high-efficiency polymerization inhibitor, the problem how removing high boiling substance in solvent reclamation process at a lower temperature to be solved exactly.
In aromatic hydrocarbons, cinnamic extraction or extracting rectifying process, the method except the high-boiling-point impurity in desolventizing generally adopted at present adopts decompression distillation, concrete operation method is: solvent to be regenerated and steam are passed into one and be provided with in the container of plug-in type reboiler and carry out reduction vaporization regeneration, due to the easy scale effect heating effect of plug-in type reboiler, just need to stop cleaning once fouling, not only bother, and affect the long-period stable operation of whole device.Particularly to the material that this kind of temperature-sensitive of styrene is easily polymerized, if the higher boiling polymer in solvent can not be removed continuously, whole extractive distillation device will be forced normally to run.
CN1077560C discloses one extraction fractional distillation from drippolene, reclaims cinnamic method, feature adds water in extractant, its method for regenerating solvent is exactly the common decompression distillation adding water vapour and carry out, due to the pressure influence of the hydrostatic column of existence at the bottom of the regenerator of plug-in type heating, cause temperature drift at the bottom of regenerator, the easy fouling of heater, affects the power of regeneration of solvent and the long-term operation of device.
CN200910135880.2 discloses a kind of renovation process of extracting solvent for extracting, rectifying and separating styrene, comprise top extracting, rectifying and separating phenylethylene being passed into after the part and water mixing of solvent recovery gained lean solvent cleaning by solvent tower, cleaning by solvent agent is as C
8aromatic hydrocarbons enters cleaning by solvent tower by bottom, moisture lean solvent after purification is discharged from cleaning by solvent tower bottom pipeline, enter the bottom of extracting, rectifying and separating phenylethylene solvent recovery tower, the cleaning by solvent agent of being rich in styrene polymer is discharged by cleaning by solvent top of tower, enter the middle part of cleaning by solvent agent recovery tower, the cleaning by solvent agent removing styrene polymer is discharged from tower top, and styrene polymer is discharged from the bottom of cleaning by solvent agent recovery tower.This method uses the polymer in cleanser extraction lean solvent by the method for back extraction, thus the polymer in removing lean solvent, realize solvent reclamation.This method is relatively applicable to the oligomer removed in lean solvent, relatively poor to the removal effect of high polymer and water-soluble high impurity.
Summary of the invention
The object of this invention is to provide a kind of renovation process of extracting, rectifying and separating phenylethylene process solvent for use, the method effectively can remove the high-boiling-point impurity in lean solvent at a lower temperature, prevent cinnamic high temperature polymerization, extend the cycle of operation of extracting, rectifying and separating phenylethylene device.
The renovation process of extracting, rectifying and separating phenylethylene solvent for use provided by the invention, comprise and will pass in the middle part of extractive distillation column containing cinnamic hydrocarbon mixture, extraction distillation solvent passes into extractive distillation column top and carries out extracting rectifying, be rich in cinnamic rich solvent and enter solvent recovery tower from the discharge of extracting rectifying tower bottom, the lean solvent part that solvent recovery tower flows out returns extractive distillation column, another part passes in the heat exchanger tube of falling film evaporator, make lean solvent by the falling film evaporation under reducing pressure and enter solvent regeneration tower lower than the low-boiling point material evaporation of lean solvent boiling point, in solvent regeneration tower, high-boiling-point impurity higher than lean solvent boiling point is in a liquid state and is discharged by bottom line, the regenerate lean solvent of gas phase is discharged by overhead line, pressure in described falling film evaporator heat exchanger tube is 10 ~ 30kPa, temperature is 120 ~ 145 DEG C.
The present invention uses falling film evaporator to replace the plug-in type reboiler of existing solvent reclamation tower bottom to carry out heating evaporation to lean solvent to be regenerated, owing to eliminating the impact of liquid level static pressure needed for traditional plug-in type reboiler, under identical solvent reclamation pressure tower, effectively can reduce the temperature of solvent reclamation tower bottom, thus effectively remove the high-boiling-point impurity high compared with extractant boiling point, cinnamic polymerization can be prevented, the running time of extension fixture simultaneously.
Accompanying drawing explanation
Fig. 1 is that the inventive method uses a falling film evaporator to carry out the schematic flow sheet of solvent reclamation.
Fig. 2 is that the inventive method uses two falling film evaporators to switch the schematic flow sheet carrying out solvent reclamation.
Fig. 3 is the partial enlarged drawing that falling film evaporator of the present invention is connected with solvent regeneration tower.
Fig. 4 is the structural representation that in prior art, solvent regeneration tower uses plug-in type reboiler.
Detailed description of the invention
The inventive method uses falling film evaporator to make lean solvent evaporation under reduced pressure to be regenerated, make under controlled pressure by the temperature controlled in falling film evaporator heat exchanger tube, low-boiling point material lower than lean solvent boiling point evaporates with lean solvent, and be in a liquid state higher than the high-boiling-point impurity of lean solvent boiling point, after entering solvent regeneration tower, high-boiling-point impurity (polymer) is sunken at the bottom of solvent regeneration tower, discharged by bottom line, thus high-boiling-point impurity is removed from lean solvent, the lean solvent of gas phase is then discharged from regeneration overhead, is regenerated solvent.Compared with the method for regenerating solvent of existing employing plug-in type reboiler, reboiler is not set at the bottom of solvent regeneration tower of the present invention heating evaporation is carried out to solvent, thus there is not the liquid of submergence reboiler, thus the impact that the static pressure eliminating the generation of this part liquid produces lean solvent evaporation, can be at the same pressure, make solvent reclamation column bottom temperature reduce by 5 ~ 15 DEG C, styrene can be prevented at high temperature to be polymerized, also farthest can make the impurity higher than solvent boiling point and separated from solvent.In addition, and due to the distribution of gas in falling film evaporator heat exchanger tube even, heat exchanger tube inwall is less scaling, can remove high-boiling-point impurity in lean solvent by continous-stable, guarantee the device long-period stable operation of extracting, rectifying and separating phenylethylene.
The inventive method adopts falling film evaporator to evaporate lean solvent to be regenerated, described falling film evaporator comprises housing and is placed in the heat exchanger tube in housing, the upper end of housing or side are equipped with the end socket being uniformly distributed and flowing into material in heat exchanger tube, during use, heat medium, by the housing of falling film evaporator, namely walks shell side, heats the heat exchanger tube in housing, lean solvent to be regenerated enters the heat exchanger tube interior (walking tube side) of falling film evaporator, carries out falling film evaporation.In the heat exchanger tube of falling film evaporator, lean solvent forms liquid film along tube wall flowing, and lean solvent evaporates and becomes gas phase on liquid film, and liquid film flows downward under gravity, namely forms falling film evaporation.
In the inventive method, the pressure in falling film evaporator heat exchanger tube is preferably 12 ~ 25kPa, temperature preferably 125 ~ 140 DEG C.
For making lean solvent more easily evaporate in falling film evaporation process, preferably in the heat exchanger tube of falling film evaporator, passing into water vapour, making the mass ratio of lean solvent and water vapour be 0.2 ~ 1.0, preferably 0.3 ~ 0.6.
Described water vapour and lean solvent can enter in the heat exchanger tube of falling film evaporator by same position or diverse location, are preferably entered in the heat exchanger tube of falling film evaporator by diverse location.
In the methods of the invention, two falling film evaporators, in turn handover operations can be set.When after a falling film evaporator fouling evaporating solvent deleterious, another falling film evaporator can be changed and carry out solvent reclamation, and dirty removing processing is carried out to the falling film evaporator of fouling, after another falling film evaporator fouling, reuse the falling film evaporator through dirty removing processing again, and dirty removing processing is carried out to the falling film evaporator of fouling, handover operation two falling film evaporators so in turn.
Heat transferring medium preferred water steam in described falling film evaporator shell side.
In the inventive method, the lean solvent carrying out regenerating process accounts for 0.5 ~ 5 quality % of lean solvent total amount, preferably 1.0 ~ 2.5 quality %.Regenerated by a part of lean solvent, removing higher boiling polymer wherein, both can ensure the normal operating of extractive distillation device, can ensure again the quality of lean solvent used.
One or more in the present invention, in the preferred sulfone compound of described extraction distillation solvent, glycols compound and glycol ether.The preferred sulfolane of described sulfone compound, dimethyl sulfone or 3-methyl sulfolane.The described preferred diethylene glycol (DEG) of glycols compound, triethylene glycol, tetraethylene glycol or five glycol.The described preferred diethylene glycol monomethyl ether of glycol ether, triethylene glycol monomethyl ether, tetraethylene glycol monomethyl ether or five glycol monomethyl ethers.
For increasing the effect of extracting, rectifying and separating phenylethylene, the water of above-mentioned extraction distillation solvent preferably containing 0.2 ~ 0.8 quality %.After extracting, rectifying and separating phenylethylene, the water separated from extract remainder and extract can be reused for the falling film evaporation process of lean solvent.
Of the present invention containing the preferred drippolene C of cinnamic hydrocarbon mixture
8cut, wherein containing the styrene of 20 ~ 60 quality %, the C of 38 ~ 78 quality %
8aromatic hydrocarbons, all the other are toluene, C
9aromatic hydrocarbons and non-aromatics.Described C
8aromatic hydrocarbons is ethylbenzene, paraxylene, meta-xylene and ortho-xylene.
Below in conjunction with accompanying drawing, the present invention is described.
In Fig. 1, entered the middle part of extractive distillation column by pipeline 1 containing cinnamic hydrocarbon mixture, extractive distillation column 102 is entered by pipeline 2 from middle part after heat exchanger 101 heat exchange, extraction distillation solvent enters extractive distillation column 102 by pipeline 15 by top, and through extracting rectifying, raffinate is discharged by extractive distillation column overhead line 3, enter return tank 103, by the isolated oil phase of return tank, a part is passed back into the top of extractive distillation column 102 by pipeline 4, another part is then discharged by pipeline 5.Be rich in cinnamic rich solvent to discharge by bottom extractive distillation column 102, solvent recovery tower 104 is entered from middle part by pipeline 7, extract and water are discharged by overhead line 8 and are entered return tank 105, the extract part of discharging from return tank 105 passes back into solvent recovery tower 104 by pipeline 9, and another part is then discharged from pipeline 10 as styrene product.The water of discharging from return tank 103 and return tank 105 is discharged by pipeline 6 and pipeline 11 respectively, through heat exchanger 106 and from after the lean solvent heat exchange at solvent recovery tower 104 end, water is vaporized and enters in falling film evaporator 107 top inflow falling film evaporator 107 heat exchanger tube through pipeline 12, also enter in heat exchanger tube after the end socket that the lean solvent part gone out from solvent recovery tower 104 underflow enters falling film evaporator after pipeline 13 mixes with the solvent-laden material 18 from solvent regeneration tower 108 end is uniformly distributed, heat medium enters the shell side of falling film evaporator 107, by the temperature regulating the temperature of heat medium to control heat exchanger tube, described heat medium is water vapour.In heat exchanger tube, having lean solvent under water vapour existent condition to flow down along tube wall in heat exchanger tube, form liquid film, liquid film is while flowing down, and low-boiling point material evaporates with lean solvent, namely carries out falling film evaporation.Stream passes via line 16 after falling film evaporation enters bottom solvent regeneration tower 108, lean solvent and the steam of gasification are discharged from the pipeline 17 at solvent regeneration tower 108 top, return to solvent recovery tower 104 end, unevaporated high-boiling-point impurity discharges solvent regeneration tower 108 by bottom, a part is mixed with the lean solvent from pipeline 13 by pipeline 18, another portion is discharged by pipeline 19, thus high-boiling-point impurity is discharged extractive distillation device, completes the regenerative process of solvent.
Fig. 2 and Fig. 1 is substantially identical, unlike being provided with two falling film evaporators 107, when a wherein falling film evaporator generation fouling, after the decay of evaporating solvent function, solid line can be switched to the position of dotted line mark, switch to another falling film evaporator and carry out lean solvent falling film evaporation, to ensure solvent reclamation ability better.
Fig. 3 is the partial enlarged drawing that in Fig. 1, falling film evaporator is connected with solvent regeneration tower.Can be clear that by Fig. 3, falling film evaporator 107 forms primarily of housing 32 and the heat exchanger tube 31 be placed in housing.Water vapour is entered the end socket 33 of falling film evaporator 107 respectively by pipeline 13 by pipeline 12, lean solvent to be regenerated, after being evenly distributed, entering in the heat exchanger tube of falling film evaporator 107, walk tube side, entered the bottom of solvent regeneration tower 108 after falling film evaporation by pipeline 16.Heat medium enters in the shell of falling film evaporator by pipeline 20, walks shell side, discharges falling film evaporator by pipeline 21.Heat exchanger tube is connected with solvent regenerator 108, and the two pressure is identical, by the temperature regulating the amount entering the heat medium of shell side can control falling film evaporator heat exchanger tube.In solvent regeneration tower, high-boiling-point impurity is discharged by solvent reclamation tower bottom, and a part is mixed with lean solvent to be regenerated by pipeline 18, and all the other are discharged by pipeline 19.
Fig. 4 is the structural representation of the plug-in type depressurized solvent regenerator generally used in prior art, its method of carrying out solvent reclamation is: heat medium enters plug-in type reboiler 23 by pipeline 24 and heats it, then flowed out by pipeline 25, heat medium preferred water steam, lean solvent enters the middle part of solvent regeneration tower 108 by pipeline 13, water vapour enters solvent regeneration tower 108 by pipeline 12 from bottom, in solvent regeneration tower 108, solvent flashes to gas, discharged from top by pipeline 17, high boiling impurity is discharged from bottom line 19.In Fig. 4, at the plug-in type reboiler 23 that solvent reclamation tower bottom is arranged, the easy fouling of its outer surface, and the liquid level in solvent regeneration tower must flood plug-in type reboiler 23, the temperature that the static pressure that this liquid level produces can cause solvent to evaporate raises, and namely solvent regeneration tower operating temperature significantly raises.
Further describe the present invention below by example, but the present invention is not limited to this.
Example 1
With drippolene C
8cut is extracting rectifying raw material, and its composition is in table 1.By the flow process shown in Fig. 1, extracting rectifying and solvent reclamation are carried out to described raw material, reclaim styrene wherein, extraction distillation solvent used contains the water of 99.5 quality % sulfolane and 0.5 quality %, add composite polymerzation inhibitor wherein, composite polymerzation inhibitor consists of: the 4-hydroxyl-2 of 55 quality %, 2,6,6-tetramethyl piperidine nitrogen oxygen free radical (OH-TEMPO), 4, the 6-dinitro-2-sec-butyl phenols (DNBP) of 25 quality %, the N of 20 quality %, N-diethyl hydroxylamine, the composite polymerzation inhibitor of injection and the mass ratio of extracting rectifying raw material are 300 μ g/g.
Solvent reclamation adopts the method for decompression falling film evaporation, and the mass ratio controlling the lean solvent/steam entered in falling film evaporator heat exchanger tube is 0.33, and the lean solvent carrying out regenerating accounts for 1.7 quality % of lean solvent total amount.Pressure in falling film evaporator heat exchanger tube is that 20kPa(is equal with solvent reclamation tower top pressure), heat exchanger tube outlet temperature is 132 DEG C (equal with solvent reclamation column bottom temperature), and each tower operating condition and extracting rectifying and solvent reclamation the results are shown in Table 2.
Comparative example 1
By the method for Fig. 4, adopt the solvent regeneration tower arranging plug-in type reboiler at the bottom of conventional tower to carry out decompression regeneration to solvent, extracting rectifying raw material used and composite polymerzation inhibitor are with example 1, and the lean solvent carrying out regenerating accounts for 1.7 quality % of lean solvent total amount.Each tower operating condition and extracting rectifying and solvent reclamation the results are shown in Table 2.
Table 1
Table 2
As shown in Table 2, under identical solvent reclamation tower top pressure, the conventional method that the inventive method adopts compared with comparative example 1, regeneration column bottom temperature reduces 13 DEG C.In 180 days of trial run, the present invention clears up solvent regeneration tower without the need to shut-down operation, regenerated solvent amount comparatively comparative example 1 adds 13%, and adopt conventional plug-in type reboiler to carry out the method for solvent reclamation, because reboiler fouling cannot normally run, need the operation stopping solvent regeneration tower, 4 scale removal cleaning is carried out to solvent regeneration tower, due to the impact of solvent regeneration tower shut-down operation, in lean solvent after regeneration, polymer content increases 0.2 quality %, comparatively the inventive method, is equivalent to the polymer adding 15% in regenerated solvent.Also can be found out by table 2, because in the inventive method lean solvent, polymer concentration is lower, also comparatively comparative example 1 is slightly high to reclaim cinnamic purity.
Example 2
By the method for example 1 with drippolene C
8cut is extracting rectifying raw material, reclaims styrene wherein, unlike extraction distillation solvent used containing 80.0 quality % sulfolane, the triethylene glycol of 19.5 quality % and the water of 0.5 quality %.Each tower operating condition and extracting rectifying and solvent reclamation the results are shown in Table 3.
Comparative example 2
By the method for Fig. 4, adopt the solvent regeneration tower arranging plug-in type reboiler at the bottom of conventional tower to carry out decompression to solvent and regenerate, extracting rectifying raw material used and composite polymerzation inhibitor are with example 2, and each tower operating condition and extracting rectifying and solvent reclamation the results are shown in Table 3.
Table 3
As shown in Table 3, the inventive method is than comparative example 2, and under same solvent reclamation tower top pressure, solvent reclamation column bottom temperature reduces 11 DEG C.In 180 days of trial run, the inventive method is cleared up solvent regeneration tower without the need to shut-down operation, regenerated solvent amount comparatively comparative example 2 adds 15%, and adopt the method for regenerating solvent of common plug-in type reboiler, because reboiler fouling cannot run well, need the operation stopping solvent regeneration tower, 5 scale removal cleaning is carried out to solvent regeneration tower, due to the impact that solvent regeneration tower is stopped work, polymer build-up 0.5 quality % in lean solvent after regeneration, comparatively the inventive method, is equivalent to the polymer adding 23% in regenerated solvent.Also can be found out by table 3, because in the inventive method lean solvent, polymer content is lower, reclaim styrene product purity also comparatively comparative example 2 improve.
Claims (12)
1. the renovation process of an extracting, rectifying and separating phenylethylene solvent for use, comprise and will pass in the middle part of extractive distillation column containing cinnamic hydrocarbon mixture, extraction distillation solvent passes into extractive distillation column top and carries out extracting rectifying, be rich in cinnamic rich solvent and enter solvent recovery tower from the discharge of extracting rectifying tower bottom, the lean solvent part that solvent recovery tower flows out returns extractive distillation column, another part passes in the heat exchanger tube of falling film evaporator, make solvent by the falling film evaporation under reducing pressure and enter solvent regeneration tower lower than the low-boiling point material evaporation of lean solvent boiling point, in solvent regeneration tower, high-boiling-point impurity higher than lean solvent boiling point is in a liquid state and is discharged by bottom line, the regenerate lean solvent of gas phase is discharged by overhead line, pressure in described falling film evaporator heat exchanger tube is 10 ~ 30kPa, temperature is 120 ~ 145 DEG C, described falling film evaporator comprises housing and is placed in the heat exchanger tube in housing, the upper end of housing or side are equipped with the end socket being uniformly distributed and flowing into material in heat exchanger tube.
2. in accordance with the method for claim 1, it is characterized in that the pressure in falling film evaporator heat exchanger tube is 12 ~ 25kPa, temperature is 125 ~ 140 DEG C.
3. according to the method described in claim 1 or 2, it is characterized in that passing into water vapour in the heat exchanger tube of falling film evaporator, make the mass ratio of lean solvent and water vapour be 0.2 ~ 1.0.
4. in accordance with the method for claim 3, it is characterized in that the mass ratio of lean solvent and water vapour is 0.2 ~ 1.0.
5. in accordance with the method for claim 3, it is characterized in that described water vapour and lean solvent are entered in the heat exchanger tube of falling film evaporator by same position or diverse location.
6. in accordance with the method for claim 1, it is characterized in that described extraction distillation solvent is selected from sulfone compound, glycols compound and glycol ether any one or a few.
7. in accordance with the method for claim 6, it is characterized in that described sulfone compound is selected from sulfolane, dimethyl sulfone or 3-methyl sulfolane.
8. in accordance with the method for claim 6, it is characterized in that described glycols compound is diethylene glycol (DEG), triethylene glycol, tetraethylene glycol or five glycol.
9. in accordance with the method for claim 6, it is characterized in that described glycol ether is diethylene glycol monomethyl ether, triethylene glycol monomethyl ether, tetraethylene glycol monomethyl ether or five glycol monomethyl ethers.
10. in accordance with the method for claim 1, it is characterized in that arranging two falling film evaporators handover operation in turn.
11. in accordance with the method for claim 1, it is characterized in that the heat transferring medium in falling film evaporator shell side is water vapour.
12. in accordance with the method for claim 1, it is characterized in that described is drippolene C containing cinnamic hydrocarbon mixture
8cut, wherein containing the styrene of 20 ~ 60 quality %, the C of 38 ~ 78 quality %
8aromatic hydrocarbons, all the other are toluene, C
9aromatic hydrocarbons and non-aromatics.
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| RU2767422C1 (en) * | 2021-06-21 | 2022-03-17 | Федеральное государственное бюджетное образовательное учреждение высшего образования «Казанский национальный исследовательский технологический университет» (ФГБОУ ВО «КНИТУ») | Method of producing styrene by liquid-phase dehydration of methylphenylcarbinol-containing raw material |
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| CN109422613B (en) * | 2017-08-29 | 2021-06-11 | 中国石油化工股份有限公司 | Method and device for decoloring crude styrene separated from pyrolysis gasoline |
| CN109422615B (en) * | 2017-08-29 | 2022-03-11 | 中国石油化工股份有限公司 | Method and device for decoloring crude styrene separated from pyrolysis gasoline |
| US11465953B2 (en) * | 2018-01-12 | 2022-10-11 | China Petroleum & Chemical Corporation | Method for purification of a solvent for separation of styrene by extractive distillation and for separation of styrene |
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| CN1322005A (en) * | 2000-04-28 | 2001-11-14 | 松下环境空调工程技术株式会社 | Method and device for regeneration of waste solvent |
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| RU2767422C1 (en) * | 2021-06-21 | 2022-03-17 | Федеральное государственное бюджетное образовательное учреждение высшего образования «Казанский национальный исследовательский технологический университет» (ФГБОУ ВО «КНИТУ») | Method of producing styrene by liquid-phase dehydration of methylphenylcarbinol-containing raw material |
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