CN205295184U - Multitower continuous rectification, recovery system of first ether of cyclopentyl group - Google Patents
Multitower continuous rectification, recovery system of first ether of cyclopentyl group Download PDFInfo
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- CN205295184U CN205295184U CN201520982294.2U CN201520982294U CN205295184U CN 205295184 U CN205295184 U CN 205295184U CN 201520982294 U CN201520982294 U CN 201520982294U CN 205295184 U CN205295184 U CN 205295184U
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Abstract
The utility model discloses a multitower continuous rectification, recovery system of first ether of cyclopentyl group, the export of CPE vaporizer exports the CPE entry linkage with the raw materials vaporizer with adsorption column entry linkage, adsorption column, the export of methyl alcohol vaporizer is connected with raw materials vaporizer alcohol inlet, the export of raw materials vaporizer is connected with lightness -removing column matter entrance with fixed bed reactor entry linkage, fixed bed reactor export, export of cauldron liquid and CPME rectifier unit entry linkage at the bottom of the lightness -removing column tower, the export of CPME rectifier unit is connected with the CPME storage tank, export of lightness -removing column top of the tower and phase separating groove entry linkage, the CPME rectifier unit establish ties by a CPME rectifying column, the 2nd CPME rectifying column and the 3rd CPME rectifying column and form. The utility model discloses realize the high -efficient separation of result, not the reaction material serialization apply mechanically.
Description
Technical field
This utility model relates to the multitower continuous rectification of a kind of cyclopentyl methyl ether, recovery system.
Background technology
Cyclopentyl methyl ether is a kind of novel environment friendly high-performance hydrophobicity ether solvent, it is called for short CPME, researched and developed by Japanese firm, in October, 2006 lists, it is the ether solvents such as a kind of novel environment friendly high-performance hydrophobicity ether solvent, alternative oxolane, methyltetrahydrofuran, methyl tertiary butyl ether(MTBE) and dioxanes. As reaction dissolvent, can be used for grignard reaction, coupling reaction, coupling aminating reaction, metal reduction reaction, lewis acid reaction and Freed-Kerafyrm thatch reaction etc. are reacted. It is also used for extraction, crystallization, surface treatment and polymerization process simultaneously.
The method of synthesis cyclopentyl methyl ether is relatively more, mainly includes (1): cyclopentenes (is called for short CPE) and methanol addition (EP1405840); (2): Cyclopentane halide replaces (JournaloftheAmericanChemicalSociety with Feldalat NM; Vol.69; (1947); P.2451,2453); Cyclopentane halide herein refers mainly to iodo Pentamethylene. or bromocyclopentane, and the yield of the cyclopentyl methyl ether of this reaction is not high, it is easy to produce to eliminate product (3): Ketocyclopentane and methanol nucleophilic addition (Tetrahedron; Vol.46; Nb.10; (1990); P.3547-3558); (4): cyclopentanol and methylating reagent (ActaChemicaScandinavica; Vol.52; Nb.10; (1998); P.1223-1233), as cyclopentanol reacts with dimethyl sulfate, this synthetic method cost is higher, have employed the material of severe toxicity, and production risk is higher; (5): cyclopentanol sodium replaces (JournaloftheChemicalSociety with halide; (1948); P.1809,1811,1813; ; (1946); P.5066). The synthetic method of industrial more employing cyclopentenes and methanol addition.
Chinese patent literature if publication number is CN104447226A discloses the production method of a kind of cyclopentyl methyl ether, the method comprises the following steps successively: 1) etherificate: cyclopentenes and methanol mixed also carry out etherification reaction by the fixing bed of storng-acid cation exchange resin after heating vaporization and generate cyclopentyl methyl ether, and the volume liquid hourly space velocity (LHSV) control of material is 0.5��4.0hr-1, it is 0.01��0.10MPa that system pressure controls, and feeding temperature is 75��90 DEG C, and the mol ratio of cyclopentenes and methanol is 1: 0.5��0.8;2) regeneration: in etherification reaction, when cyclopentenes conversion ratio is down to below 10.0%, stops charging, catalyst is regenerated, and regeneration condition is: regenerated solvent adopts etherification reaction raw material, and it is 0.1��1.0hr that the volume liquid hourly space velocity (LHSV) of material controls-1, it is 0.3��1.0MPa that system pressure controls, and feeding temperature is 20��90 DEG C, and the recovery time is 10��30 hours. The low conversion rate of the cyclopentenes of this production method, and it is provided without the mode of production of serialization, be not suitable for industrial mass production.
Publication number is the manufacture method that the Chinese patent literature of CN105050994A discloses a kind of cycloalkyl-alkyl ether compound, and it is manufacture formula (1): R1-O-R2(in formula, R1Represent meaning as hereinbefore, R2Expression can have the cyclopenta of substituent group or can have the cyclohexyl of substituent group. ) shown in the method for cycloalkyl-alkyl ether compound, wherein, make the cyclopentenes can with substituent group maybe can have cyclohexene and formula (2): the R of substituent group under the existence of acid-exchange resin1OH(R1Expression can have the alkyl of substituent group and carbon number 1��10 or can have substituent group and the cycloalkyl of carbon number 3��8. ) shown in alcoholic compound react under gaseous state, using specific surface area as acid-exchange resin is 20��50m2/ g, average pore size are 20��70nm and resin that total exchange capacity is 4.8��6.0eq/L-R wet resin.
The seriality of aforementioned production method is not high, does not take into full account the recovery of material.
Utility model content
This utility model solves the technical problem that existing cyclopentyl methyl ether process units serialization degree is not high, it is therefore intended that, it is achieved the high efficiency separation of product, unreacted material serialization is applied mechanically.
The multitower continuous rectification of a kind of cyclopentyl methyl ether, recovery system, it is characterised in that include material carburetion system, fixed bed reactors, product separation system;
Described material carburetion system includes the CPE carburator with CPE entrance, for receiving the adsorption column of CPE after vaporization, with the methyl alcohol vaporizing device of methanol inlet and material carburetor;
Described product separation system includes lightness-removing column, CPME rectifier unit, point phase groove;
CPE vaporizer outlets is connected with adsorption column entrance, and adsorption column outlet is connected with the CPE entrance of material carburetor; The outlet of methyl alcohol vaporizing device is connected with material carburetor methanol inlet; Material carburetor outlet is connected with fixed bed reactors entrance, fixed bed reactors outlet is connected with lightness-removing column material inlet;
Still liquid outlet at the bottom of lightness-removing column tower is connected with CPME rectifier unit entrance, and the outlet of CPME rectifier unit is connected with CPME storage tank; Lightness-removing column tower top outlet is connected with a point phase groove entrance;
Described CPME rectifier unit is in series by a CPME rectifying column, the 2nd CPME rectifying column and the 3rd CPME rectifying column.
Still liquid bottom lightness-removing column, through the multistage CPME rectifying column rectification process of series connection, can be effectively improved the G/C content of cyclopentyl methyl ether.
The entrance of the oneth CPME rectifying column is the entrance of described CPME rectifier unit, the outlet of the oneth CPME rectifying column is connected with the entrance of the 2nd CPME rectifying column, the outlet of the 2nd CPME rectifying column is connected with the entrance of the 3rd CPME rectifying column, the outlet of the 3rd CPME rectifying column is the outlet of described CPME rectifier unit, and the outlet of the 3rd CPME rectifying column is connected with CPME adsorption column entrance.
It is filled with acid-exchange resin in described fixed bed reactors.
As preferably, described acid-exchange resin is one or more of amberlyst15, amberlyst35, amberlyst36.
It is filled with cyclopentadiene resin in described adsorption column.
Cyclopentenes flows through adsorption column after vaporization, the cyclopentadiene resin absorption in post, reducing the content of autopolymer, thus preventing acidic ion exchange resin catalyst poisoning, improving the conversion ratio of cyclopentenes.
Know by experiment, good autopolymer adsorption effect can be obtained at 2-5MPa, 90-110 DEG C, the lifting of CPME purity and the conversion ratio of methanol is favourable.
After catalytic addition completes, reactant liquor enters lightness-removing column, and the still liquid bottom lightness-removing column is flowed into CPME rectifier unit by outlet at bottom, carries out rectification process, prepares cyclopentyl methyl ether.
As preferably, being additionally provided with CPME adsorption column between outlet and the CPME storage tank connecting line of the 3rd CPME rectifying column.
The filler of water sorption it is filled with, as preferably, being filled with molecular sieve in described CPME adsorption column in CPME adsorption column.
As preferably, the outlet of CPME adsorption column and CPME storage tank connecting line being additionally provided with branch road, this branch road is connected with the activation entrance of adsorption column, and activation outlet is incorporated to a CPME rectifying column inlet by pipeline.
After adsorption column uses a period of time, more cyclopentenes oligomer and other impurity can be remained in post, need Regeneration Treatment, by a CPME part for preparation is imported in adsorption column, by CPME eluting adsorption column, carry out activation processing, wash post liquid be directed at again CPME rectifier unit carry out rectification reclaim CPME. The activation frequency of adsorption column can be determined according to practical situation, is usually annually. Improve the adsorption effect of adsorption column by the setting of this branch road, the high efficiency continuously contributing to CPME produces.
The height of the CPME rectifier bottoms still liquid that boils is mainly the material such as oligomeric side-products, a small amount of CPME. The height of each CPME rectifier bottoms boil still liquid outlet merge or be separately added into comprehensive recovery system. Height boil still liquid enter comprehensive recovery system rectification reclaim CPME and dimerization by-product etc.
Lightness-removing column top exit place is provided with two-stage series connection condenser, obtains low boiler cut (light component) and mainly contain cyclopentenes, methanol, water, a small amount of CPME and by-product methyl ether after condensation, and this low boiler cut enters layering in point phase groove; Aqueous phase mainly contains water, methanol and CPE; Enter aqueous phase groove. Oil phase mainly contains CPE, methanol, CPME and minor amount of water composition; Enter oil phase groove.
Product separation system is additionally provided with the CPE knockout tower being connected with oil phase groove, and the outlet of CPE separation column is connected with CPE receiving slit entrance, and the oil phase of CPE receiving slit is by pipeline and CPE vaporizer outlets.
The oil phase of oil phase groove is transferred to CPE knockout tower and carries out second distillation. The top exit of CPE knockout tower is connected with CPE receiving slit entrance, the fraction at top is layered and respectively enters respective storage tank (the second aqueous phase groove and the second oil phase groove) at CPE receiving slit, wherein the material of the second oil phase groove is mainly CPE, the bottom land outlet of this oil phase groove is connected with CPE vaporizer outlets, thus realizing, by unreacted CPE serialization reuse, improving the transformation efficiency of material. Purify through the second-order separation of undue phase groove and CPE receiving slit and can effectively reduce the impurity reclaimed in CPE, it is ensured that the continuous prodution efficiency of product and purity.
Aqueous phase in aqueous phase groove and the second aqueous phase groove mainly contains the materials such as water, methanol and a small amount of CPME, and this aqueous phase accesses comprehensive recovery system in the lump and carries out Methanol Recovery.
Described comprehensive recovery system includes composite distillation tower, composite distillation tower accepts the aqueous phase from CPE receiving slit, aqueous phase groove, boil still liquid with the height bottom CPME rectifier unit and CPE knockout tower, the materials such as methanol, CPME, polymeric rings amylene are reclaimed through composite distillation tower rectification, the methanol reclaimed is transferred in methyl alcohol vaporizing device by pipeline after dried, recovery.
In this utility model, except being batch distillation except comprehensive recovery system, all the other devices are continuous loop and produce.
The method adopting above-mentioned production system continuous prodution cyclopentyl methyl ether, vaporize including by cyclopentenes, filter then through adsorption column, then in material carburetor with methanol mixed, vaporization, enter fixed bed reactors and carry out catalytic addition reaction, reactant liquor distills through lightness-removing column, and light component recovery CPE and methanol, lightness-removing column still liquid obtain cyclopentyl methyl ether through CPME rectifier unit rectification; The temperature of described catalytic addition reaction is 100-105 DEG C, liquid hourly space velocity 0.35-0.55hr-1, gas space speed 110-125hr-1; Pressure is 0.1��0.12Mpa.
The cyclopentenes introduced by cyclopentenes head tank or the second oil phase groove is through the heating vaporization of CPE carburator, described CPE carburator adopts low-pressure steam heating (0.1-0.4MPa, 130-150 DEG C), the cyclopentenes of vaporization flows through adsorption column remove impurity, enter after dewatering in material steam device with the reuse methanol mixed from methanol tank or comprehensive recovery system, then low-pressure steam is adopted to be heated by material carburator, make each mixing of materials, vaporization, the steam pressure of described material carburator is 0.1-0.4MPa, 130-150 DEG C, mixed material after vaporization enters fixed bed reactors and carries out catalytic addition reaction, successive reaction under the cited reaction conditions.
Reactant liquor operating is distilled to lightness-removing column, lightness-removing column adopts pressure to be 0.1-0.4MPa, temperature is the steam of 100-110 DEG C to be heated, bottom lightness-removing column, still liquid mainly contains product CPME and a small amount of oligomeric side-products, enter CPME rectifier unit rectification (0.1-0.4MPa, 110-120 DEG C) carry out refine, collect product frac; CPME rectifier unit is preferably the CPME rectifying column of thtee-stage shiplock, the height of each CPME rectifier bottoms still liquid that boils contains more high boiling material (such as cyclopentenes oligomer) and a small amount of CPME, this height still liquid that boils enters total system, reclaims further CPME and cyclopentenes oligomer.
The square formula 1 of reaction scheme:
Lightness-removing column top exit is light component, is circulated Commercial cultivation through processing recovery CPE, the CPE of recovery through the vaporization of CPE carburator.
The product cut that the outlet of the afterbody CPME rectifying column of CPME rectifier unit is flowed out adsorbs through CPME adsorption column, enters CPME storage tank after drying or directly pack. CPME adsorption column is through absorption after a while, the absorbability of molecular sieve is gradually reduced, slowly lose absorbent function, require over following operation and CPME adsorption column is carried out Regeneration Treatment: CPME adsorption column is warming up to about 200 DEG C, it is filled with nitrogen in post, the water that condensation nitrogen purges out, thus completing the regeneration of CPME adsorption column.
Described acid-exchange resin is one or more of amberlyst15, amberlyst35, amberlyst36.
The resistance to elevated temperatures of above-mentioned acid-exchange resin is better, and methanol conversion is high.
Know by experiment, adopt mixing, specified particle diameter acid-exchange resin can reach ideal effect.
As preferably, the mberlyst-35 of described amberlyst15 and the 20-40wt% that acid-exchange resin is 60-80wt%; The grain warp of described amberlyst15 is 1.2-1.8mm; The grain warp of amberlyst-35 is 0.5-1.2mm.
Particle diameter described herein is the mean diameter of each resin.
Under the catalyst of this proportioning, the conversion ratio of methanol is more than 95%, and in reactant liquor the G/C content of CPME more than 90%; About 1.5-2.5 times is extended with the time limit of single acidic ion exchange resin catalyst.
More preferably, the mberlyst-35 of described amberlyst15 and the 40wt% that acid-exchange resin is 60wt%; The grain warp of described amberlyst15 is 1.2-1.5mm; The grain warp of amberlyst-35 is 0.5-0.8mm.
It is preferred that, under the catalysis of above-mentioned mixing acid-exchange resin, additive reaction temperature is 100-105 DEG C, liquid 0.35hr-1, gas 116hr-1; Pressure is 0.1��0.12Mpa, and in reactant liquor, the conversion ratio of methanol is 97%, and in reactant liquor the G/C content of CPME more than 93%.
Further preferred, the specific surface area of described amberlyst15 is 30-40m2/ g, average pore size are 30-40nm, total heat exchange capacity is 4.8-5.3eq/L-R.
In this utility model, CPE first passes through and reacts with methanol mixed entrance fixed bed reactors after adsorption column processes again, and effectively reduces fixed bed reactor catalyst intoxicating phenomenon; And by unreacted material (CPE and methanol) through post processing recovery, it is achieved that the high efficiency continuously of cyclopentyl methyl ether produces, and improves the conversion ratio of material and the yield of product, effectively reduces the by-products content of catalytic addition reaction.
Accompanying drawing explanation
Fig. 1 is the equipment flowsheet of the continuous production system of a kind of cyclopentyl methyl ether of the present utility model;
Fig. 2 is the process chart of the continuous prodution of cyclopentyl methyl ether of the present utility model.
Detailed description of the invention
Following example are pressed aforesaid operations method and are implemented:
As shown in Figure 1 and Figure 2, a kind of cyclopentyl methyl ether continuous production system, including material carburetion system, fixed bed reactors 7, product separation system; The acid-exchange resin of the amberlyst35 of amberlyst15 and the 40wt% of 60wt% it is filled with in fixed bed reactors 7. Product separation system includes lightness-removing column 8, CPME rectifier unit, point phase groove 9
Material carburetion system includes the CPE carburator 2 with CPE entrance, for receiving the adsorption column 3 of CPE after vaporization, with the methyl alcohol vaporizing device 5 of methanol inlet and material carburetor 6. CPE storage tank 1 is exported and is connected with CPE carburator 2 entrance by pipeline, and CPE carburator 2 outlet is connected with adsorption column 3 entrance, is filled with cyclopentadiene resin in adsorption column 3, and adsorption column 3 outlet is connected with the CPE entrance of material carburetor 6. Methanol tank 4 outlet is connected with methyl alcohol vaporizing device 5 entrance, and methyl alcohol vaporizing device 5 outlet is connected with material carburetor 6 methanol inlet.
Material carburetor 6 outlet is connected with fixed bed reactors 7 entrance, fixed bed reactors 7 outlet is connected with lightness-removing column 8 material inlet.
CPME rectifier unit is that CPME rectifying column the 19, the 2nd CPME rectifying column the 18, the 3rd CPME rectifying column 17 thtee-stage shiplock forms. Still liquid outlet at the bottom of lightness-removing column 8 tower is connected with the entrance of a CPME rectifying column 19, the outlet of the oneth CPME rectifying column 19 is connected with the entrance of the 2nd CPME rectifying column 18, the outlet of the 2nd CPME rectifying column 18 is connected with the entrance of the 3rd CPME rectifying column 17, the outlet of the 3rd CPME rectifying column 17 is connected with CPME adsorption column 25 entrance, is filled with molecular sieve in CPME adsorption column 25.CPME adsorption column 25 outlet is connected with CPME storage tank 26.
Being additionally provided with branch road (Fig. 1 does not mark) on CPME adsorption column 25 outlet and CPME storage tank 26 connecting line, this branch road is connected with the activation entrance of adsorption column 3, and activation outlet is incorporated to CPME rectifying column 19 entrance by pipeline.
Lightness-removing column 8 top exit place is provided with two-stage series connection condenser, and a point phase groove 9 receives condensed fluid. The aqueous phase dividing phase groove 9 enters aqueous phase groove 10, and oil phase enters oil phase groove 11. Product separation system is additionally provided with the CPE knockout tower 13 being connected with oil phase groove 11, CPE knockout tower 13 top exit is connected with CPE receiving slit 14 entrance, the oil phase of oil phase groove 11 is transferred to CPE knockout tower 13 and carries out second distillation, the fraction at top is layered and respectively enters respective storage tank (second aqueous phase groove 15 and the second oil phase groove 16) at CPE receiving slit 14, wherein the material of the second oil phase groove 16 is mainly CPE, the bottom land outlet of the second oil phase groove 16 is connected with CPE carburator 2 outlet, thus realizing unreacted CPE serialization reuse.
The aqueous phase of aqueous phase groove 10 and the second aqueous phase groove 15 enters comprehensive recovery system.
Comprehensive recovery system includes composite distillation tower 20, composite distillation tower 20 accept from aqueous phase groove 10, the second aqueous phase groove 15 aqueous phase, boil still liquid with the height bottom CPME rectifier unit and CPE knockout tower 13, reclaim the materials such as methanol, CPME, polymeric rings amylene, the methanol reclaimed enters Methanol Recovery groove 21 after dried, it is transferred in methyl alcohol vaporizing device 5 by pipeline, recovery.
The height of the CPME rectifier bottoms still liquid that boils is mainly the material such as oligomeric side-products, a small amount of CPME. The still liquid outlet of boiling of the height of each CPME rectifier bottoms of series connection merges or is separately added into comprehensive recovery system, and the CPME that rectification is reclaimed enters CPME accumulator tank 22, and when amount to be recycled is bigger, the unified series connection CPME rectifying column that enters is refined. The dimerization by-product reclaimed and other high refuses enter oligomeric groove 23. Waste water enters wastewater trough 24, is transferred to municipal wastewater and processes system.
In process of production, the cyclopentenes introduced by cyclopentenes head tank or the second oil phase groove 16 heats vaporization through CPE carburator 2, CPE carburator 2 adopts low-pressure steam heating (0.1-0.4MPa, 130-150 DEG C), the cyclopentenes of vaporization flows through adsorption column 3 remove impurity, enter after dewatering in material steam device with the reuse methanol mixed from methanol tank 4 or comprehensive recovery system, then low-pressure steam is adopted to be heated by material carburator, make each mixing of materials, vaporization, the steam pressure of material carburator is 0.1-0.4MPa, 130-150 DEG C, mixed material after vaporization enters fixed bed reactors 7 and carries out catalytic addition reaction.
Reactant liquor operating is distilled to lightness-removing column 8, lightness-removing column 8 adopts pressure to be 0.1-0.4MPa, temperature is the steam of 100-110 DEG C to be heated, bottom lightness-removing column 8, still liquid mainly contains product CPME and a small amount of oligomeric side-products, enter CPME rectifier unit, through a CPME rectifying column 19 (0.1-0.4MPa, 110-120 DEG C), the serialization multitower rectification of the 2nd CPME rectifying column the 18, the 3rd CPME rectifying column 17, product frac is flowed out by the 3rd CPME rectifying column 17, dried then through CPME adsorption column 25, carry out CPME storage tank 26 and store and pack. The height of each CPME rectifier bottoms still liquid that boils contains more high boiling material and a small amount of CPME, and this height still liquid that boils enters total system, reclaims CPME and polymeric rings amylene further.
Lightness-removing column 8 top exit is light component, is circulated Commercial cultivation through aqueous phase groove 10, CPE separator separation and recovery CPE, the CPE of recovery through CPE carburator 2 vaporization.
Amberlyst15, amberlyst35, amberlyst36 of adopting are Rhom and Hass's product.
Embodiment 1
Adopt said system carry out continuous prodution, the CPE of vaporization flow through the pressure of adsorption column be 2MPa, 100 DEG C; The grain warp of the amberlyst15 filled in fixed bed reactors is 1.2-1.8mm; The grain warp of amberlyst-35 is 0.5-1.2mm; The specific surface area of amberlyst15 is 30-40m2/ g, average pore size are 30-40nm, total heat exchange capacity is 4.8-5.3eq/L-R. The mol ratio of cyclopentenes and methanol is 1.6:1, and the temperature of fixed bed reactors is 100-105 DEG C, and liquid hourly space velocity is 0.35hr-1, gas space speed is 110hr-1; Pressure is 0.1Mpa. After continuous prodution terminates, the conversion ratio 96% of methanol, in reactant liquor, the GC purity of product is more than 90% (GC area normalization method purity; Every 30min samples); The purity of cyclopentyl methyl ether prepared by refine is more than 99.5%, and the total recovery of cyclopentyl methyl ether is more than 86%.
Embodiment 2
Adopt said system carry out continuous prodution, the CPE of vaporization flow through the pressure of adsorption column be 2MPa, 100 DEG C; The grain warp of the amberlyst15 filled in fixed bed reactors is 1.2-1.5mm; The grain of amberlyst-35 is 30-40m through the specific surface area for 0.5-0.8mm, amberlyst152/ g, average pore size are 30-40nm, total heat exchange capacity is 4.8-5.3eq/L-R. The mol ratio of cyclopentenes and methanol is 1.6:1, and the temperature of fixed bed reactors is 100-105 DEG C, and liquid hourly space velocity is 0.35hr-1, gas space speed is 116hr-1; Pressure is 0.12Mpa. After continuous prodution terminates, the conversion ratio 97% of methanol, in reactant liquor, the GC purity of product is more than 93% (GC area normalization method purity; Every 30min samples); The purity of cyclopentyl methyl ether prepared by refine is more than 99.5%, and the total recovery of cyclopentyl methyl ether is more than 93%.
Comparative example 1
Compare with embodiment 2, be different in that, in adsorption column, be not filled by cyclopentadiene resin. After continuous prodution terminates, the conversion ratio 73% of methanol, in reactant liquor, the GC purity of product is more than 78% (GC area normalization method purity; Every 30min samples); The purity of cyclopentyl methyl ether prepared by refine is more than 99.5%, and the total recovery of cyclopentyl methyl ether is more than 65%.
Comparative example 2
Compare with embodiment 2, be different in that, adopt single-stage CPME rectifying column that product is refined. After continuous prodution terminates, the conversion ratio 87% of methanol, in reactant liquor, the GC purity of product is more than 90% (GC area normalization method purity; Every 30min samples); The purity of cyclopentyl methyl ether prepared by refine is more than 97.1%, and the total recovery of cyclopentyl methyl ether is more than 73%.
Embodiment 3
Compare with embodiment 1, be different in that, the CPE of vaporization flow through the pressure of adsorption column be 5MPa, 90 DEG C. After continuous prodution terminates, the conversion ratio 95% of methanol, in reactant liquor, the GC purity of product is more than 90% (GC area normalization method purity; Every 30min samples); The purity of cyclopentyl methyl ether prepared by refine is more than 99.5%, and the total recovery of cyclopentyl methyl ether is more than 88%.
Embodiment 4
Compare with embodiment 1, be different in that, fill 80wt% grain in fixed bed reactors through the amberlyst15 for 1.2-1.5mm; The amberlyst-35 acidic resins that 20wt% grain warp is 0.5-0.8mm are as catalyst, after continuous prodution terminates, and the conversion ratio 90% of methanol, in reactant liquor, the GC purity of product is more than 89% (GC area normalization method purity;Every 30min samples); The purity of cyclopentyl methyl ether prepared by refine is more than 99.5%, and the total recovery of cyclopentyl methyl ether is more than 85%.
Embodiment 5
Compare with embodiment 1, be different in that, fill 70wt% grain in fixed bed reactors through the amberlyst15 for 1.2-1.5mm; 20wt% grain is through the amberlyst-35 for 0.5-0.8mm, 10wt% particle diameter be the amberlyst-36 of 0.5-1.5mm as acidic resins as catalyst, after continuous prodution terminates, the conversion ratio 93% of methanol, in reactant liquor, the GC purity of product is more than 87% (GC area normalization method purity; Every 30min samples); The purity of cyclopentyl methyl ether prepared by refine is more than 99.5%, and the total recovery of cyclopentyl methyl ether is more than 83%.
Embodiment 6
Comparing with embodiment 1, be different in that, the mol ratio of cyclopentenes and methanol is 1.05:1, after continuous prodution terminates, and the conversion ratio 95% of methanol, in reactant liquor, the GC purity of product is more than 81% (GC area normalization method purity; Every 30min samples); The purity of cyclopentyl methyl ether prepared by refine is more than 99.5%, and the total recovery of cyclopentyl methyl ether is more than 81%.
Embodiment 7
Comparing with embodiment 1, be different in that, the mol ratio of cyclopentenes and methanol is 2:1, after continuous prodution terminates, and the conversion ratio 96% of methanol, in reactant liquor, the GC purity of product is more than 89% (GC area normalization method purity; Every 30min samples); The purity of cyclopentyl methyl ether prepared by refine is more than 99.5%, and the total recovery of cyclopentyl methyl ether is more than 88%.
Embodiment 8
Said system is adopted to carry out continuous prodution, being distinctive in that, the catalyst of the filling in fixed bed reactors is 100% warp is the amberlyst15 of 1.2-1.5mm, and the mol ratio of cyclopentenes and methanol is 1.6:1, the temperature of fixed bed reactors is 100-105 DEG C, and liquid hourly space velocity is 0.55hr-1, gas space speed is 125hr-1; Pressure is 0.12Mpa. After continuous prodution terminates, the conversion ratio 90% of methanol, in reactant liquor, the GC purity of product is more than 89% (GC area normalization method purity; Every 30min samples); The purity of cyclopentyl methyl ether prepared by refine is more than 99.5%, and the total recovery of cyclopentyl methyl ether is more than 80%.
Claims (7)
1. the multitower continuous rectification of a cyclopentyl methyl ether, recovery system, it is characterised in that include material carburetion system, fixed bed reactors, product separation system;
Described material carburetion system includes the CPE carburator with CPE entrance, for receiving the adsorption column of CPE after vaporization, with the methyl alcohol vaporizing device of methanol inlet and material carburetor;
Described product separation system includes lightness-removing column, CPME rectifier unit, point phase groove;
CPE vaporizer outlets is connected with adsorption column entrance, and adsorption column outlet is connected with the CPE entrance of material carburetor; The outlet of methyl alcohol vaporizing device is connected with material carburetor methanol inlet; Material carburetor outlet is connected with fixed bed reactors entrance, fixed bed reactors outlet is connected with lightness-removing column material inlet;
Still liquid outlet at the bottom of lightness-removing column tower is connected with CPME rectifier unit entrance, and the outlet of CPME rectifier unit is connected with CPME storage tank; Lightness-removing column tower top outlet is connected with a point phase groove entrance;
Described CPME rectifier unit is in series by a CPME rectifying column, the 2nd CPME rectifying column and the 3rd CPME rectifying column;
Being additionally provided with comprehensive recovery system, comprehensive recovery system includes composite distillation tower, and composite distillation tower receives the aqueous phase from CPE receiving slit, aqueous phase groove, and the methanol of recovery is connected with methyl alcohol vaporizing device entrance by pipeline.
2. the multitower continuous rectification of cyclopentyl methyl ether, recovery system as claimed in claim 1, it is characterised in that be filled with cyclopentadiene resin in described adsorption column.
3. the multitower continuous rectification of cyclopentyl methyl ether, recovery system as claimed in claim 2, it is characterised in that be additionally provided with CPME adsorption column between outlet and the CPME storage tank connecting line of the 3rd CPME rectifying column.
4. the multitower continuous rectification of cyclopentyl methyl ether, recovery system as claimed in claim 3, it is characterised in that be filled with molecular sieve in described CPME adsorption column.
5. the multitower continuous rectification of cyclopentyl methyl ether, recovery system as claimed in claim 4, it is characterized in that, the outlet of CPME adsorption column and CPME storage tank connecting line are additionally provided with branch road, this branch road is connected with the activation entrance of adsorption column, and activation outlet is incorporated to a CPME rectifying column inlet by pipeline.
6. the multitower continuous rectification of cyclopentyl methyl ether, recovery system as claimed in claim 5, it is characterized in that, product separation system is additionally provided with the CPE knockout tower being connected with oil phase groove, the outlet of CPE separation column is connected with CPE receiving slit entrance, and the oil phase of CPE receiving slit is by pipeline and CPE vaporizer outlets.
7. the multitower continuous rectification of cyclopentyl methyl ether, recovery system as claimed in claim 6, it is characterised in that be filled with acid-exchange resin in described fixed bed reactors.
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