CN205616821U - Serialization production system of first ether of cyclopentyl group - Google Patents
Serialization production system of first ether of cyclopentyl group Download PDFInfo
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- CN205616821U CN205616821U CN201520984203.9U CN201520984203U CN205616821U CN 205616821 U CN205616821 U CN 205616821U CN 201520984203 U CN201520984203 U CN 201520984203U CN 205616821 U CN205616821 U CN 205616821U
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Abstract
The utility model discloses a first ether serialization production system 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 utility model discloses in, CPE reacts with methyl alcohol mixed admission fixed bed reactor after the adsorption column is handled earlier again, has effectively reduced the fixed bed reactor catalyst poisoning phenomenon, and reaction material (CPE and methyl alcohol) does not retrieve through the aftertreatment and applies mechanically, has realized the high -efficient serialization production of first ether of cyclopentyl group.
Description
Technical field
This utility model relates to the continuous production system of a kind of cyclopentyl methyl ether.
Background technology
Cyclopentyl methyl ether is a kind of novel environment friendly high-performance hydrophobicity ether solvent, being called for short CPME, Japanese firm research and develop, 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.Being also used for extraction, crystallization, surface processes and polymerization process simultaneously.
The method of synthesis cyclopentyl methyl ether is the most, mainly includes (1): cyclopentenes (being called for short CPE) and methanol addition (EP1405840)；(2): Cyclopentane halide replaces (Journal of the American Chemical Society 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 the highest, easily produces and eliminates product (3): Ketocyclopentane and methanol nucleophilic addition (Tetrahedron；vol.46；nb.10；(1990)；p.3547-3558)；(4): cyclopentanol and methylating reagent (Acta Chemica Scandinavica；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 (Journal of the Chemical Society with halide；(1948)；p.1809,1811,1813；；(1946)；p.5066).Industrial more employing cyclopentenes and the synthetic method of methanol addition.
As the Chinese patent literature of Publication No. 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 storng-acid cation exchange resin fixed bed 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 cyclopentenes is 1: 0.5～0.8 with the mol ratio of methanol；2) regeneration: in etherification reaction, when cyclopentenes conversion ratio is down to below 10.0%, stops charging, regenerates catalyst, and regeneration condition is: regenerated solvent uses 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 conversion ratio of the cyclopentenes of this production method is low, and is provided without the mode of production of serialization, is not suitable for industrial mass production.
The Chinese patent literature of Publication No. CN105050994A discloses the manufacture method of 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.The method of the cycloalkyl-alkyl ether compound shown in), wherein, makes the cyclopentenes can with substituent group maybe can have cyclohexene and formula (2): the R of substituent group in the presence of acid-exchange resin1OH(R1Expression can have substituent group and the alkyl of carbon number 1～10 or can have substituent group and the cycloalkyl of carbon number 3～8.Alcoholic compound shown in) reacts under gaseous state, and using specific surface area as acid-exchange resin is 20～50m2The resin that/g, average pore size are 20～70nm and total exchange capacity is 4.8～6.0eq/L-R wet resin.
The seriality of aforementioned production method is the highest, does not takes 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 the highest, it is therefore intended that, improve the conversion ratio of material, improve production efficiency.
The continuous production system of a kind of cyclopentyl methyl ether, including material carburetion system, fixed bed reactors, product separation system；
Described material carburetion system include the CPE carburator with CPE entrance, after receiving vaporization the adsorption column of CPE, with the methyl alcohol vaporizing device of methanol inlet and material carburetor；
Described product separation system includes lightness-removing column, CPME rectifier unit, split-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 split-phase groove 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, reduces the content of autopolymer, thus prevents acidic ion exchange resin catalyst to be poisoned, improves the conversion ratio of cyclopentenes.
Being known by experiment, can obtain preferable autopolymer adsorption effect at 2-5MPa, 90-110 DEG C, the lifting to 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, between the outlet of CPME rectifier unit and CPME storage tank connecting line, it is additionally provided with CPME adsorption column.The outlet of CPME rectifier unit is connected with CPME adsorption column entrance, and the outlet of CPME adsorption column is connected with CPME reservoir inlet.
It is filled with the filler of water sorption in CPME adsorption column, as preferably, in described CPME adsorption column, is filled with molecular sieve.
As preferably, the outlet of CPME adsorption column is additionally provided with branch road on CPME storage tank connecting line, and this branch road is connected with the activation entrance of adsorption column, and activation outlet is incorporated to CPME rectifier unit entrance 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.
As preferably, described CPME rectifier unit is that multistage CPME rectifying column is in series.
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.
Further preferably, described CPME rectifier unit is in series by a CPME rectifying column, the 2nd CPME rectifying column and the 3rd CPME rectifying column.
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 that outlet is described CPME rectifier unit of the 3rd CPME rectifying column, the outlet of the 3rd CPME rectifying column is connected with CPME adsorption column entrance.
The high boiling still liquid of CPME rectifier bottoms is mainly the material such as oligomeric side-products, a small amount of CPME.The high boiling still liquid outlet of each CPME rectifier bottoms merges or is separately added into comprehensive recovery system.High boiling still liquid enters comprehensive recovery system rectification and reclaims CPME and dimerization by-product etc..
Being provided with two-stage series connection condenser at lightness-removing column top exit, obtain low boiler cut (light component) and mainly contain cyclopentenes, methanol, water, a small amount of CPME and by-product methyl ether after condensation, this low boiler cut enters in split-phase groove and is layered；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 realize, by unreacted CPE serialization reuse, improving the transformation efficiency of material.The second-order separation through split-phase groove and CPE receiving slit purifies 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 from CPE receiving slit, the aqueous phase of aqueous phase groove, with the high boiling still liquid 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, in addition to comprehensive recovery system is batch distillation, remaining device is continuous prodution.
The method using above-mentioned production system continuous prodution cyclopentyl methyl ether, vaporize including by cyclopentenes, filter through adsorption column again, 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 uses low-pressure steam heating (0.1-0.4MPa, 130-150 DEG C), the cyclopentenes of vaporization flows through adsorption column remove impurity, except enter after water in material steam device with the reuse methanol mixed from methanol tank or comprehensive recovery system, then low-pressure steam is used to be heated by material carburator, each material is made to mix, 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, the steam that lightness-removing column uses pressure to be 0.1-0.4MPa, temperature is 100-110 DEG C heats, 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 high boiling still liquid of each CPME rectifier bottoms contains more high boiling material (such as cyclopentenes oligomer) and a small amount of CPME, this height boiling still liquid enters total system, reclaims CPME and cyclopentenes oligomer further.
The square formula of reaction scheme 1:
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 through the absorption of CPME adsorption column, dried entrance CPME storage tank or is directly packed.CPME adsorption column is through absorption after a while, the absorbability of molecular sieve is gradually reduced, slowly lose absorbent function, need, by following operation, CPME adsorption column carries out Regeneration Treatment: CPME adsorption column is warming up to about 200 DEG C, nitrogen it is filled with in post, the water that condensation nitrogen purges out, thus complete 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 preferable, and methanol conversion is high.
Being known by experiment, employing mixes, the acid-exchange resin of specified particle diameter can reach ideal effect.
As preferably, described acid-exchange resin is the mberlyst-35 of amberlyst15 Yu 20-40wt% of 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 90% more than the G/C content of CPME in 95%, and reactant liquor；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 amberlyst15 Yu 40wt% that described 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.
Further preferably, 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 during in reactant liquor, the conversion ratio of methanol is 97%, and reactant liquor, the G/C content of CPME is 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 conversion ratio and the yield of product of material, 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
As shown in Figure 1 and Figure 2, the continuous production system of a kind of cyclopentyl methyl ether, including material carburetion system, fixed bed reactors 7, product separation system；The acid-exchange resin of the amberlyst35 of amberlyst15 and 40wt% of 60wt% it is filled with in fixed bed reactors 7.Product separation system includes lightness-removing column 8, CPME rectifier unit, split-phase groove 9
Material carburetion system include the CPE carburator 2 with CPE entrance, after receiving vaporization the adsorption column 3 of CPE, 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.
CPME adsorption column 25 outlet is additionally provided with branch road (Fig. 1 does not marks) on CPME storage tank 26 connecting line, and 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.
Being provided with two-stage series connection condenser at lightness-removing column 8 top exit, split-phase groove 9 receives condensed fluid.The aqueous phase of split-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 realizes 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, with the high boiling still liquid 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 high boiling still liquid of CPME rectifier bottoms is mainly the material such as oligomeric side-products, a small amount of CPME.The high boiling still liquid outlet 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 refines.The dimerization by-product reclaimed and other high refuses enter oligomeric groove 23.Waste water enters wastewater trough 24, is transferred to municipal wastewater processing 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 uses low-pressure steam to heat (0.1-0.4MPa, 130-150 DEG C), the cyclopentenes of vaporization flows through adsorption column 3 remove impurity, except enter after water in material steam device with the reuse methanol mixed from methanol tank 4 or comprehensive recovery system, then low-pressure steam is used to be heated by material carburator, each material is made to mix, 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, the steam that lightness-removing column 8 uses pressure to be 0.1-0.4MPa, temperature is 100-110 DEG C heats, 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 through CPME adsorption column 25 again, carry out CPME storage tank 26 and store and pack.The high boiling still liquid of each CPME rectifier bottoms contains more high boiling material and a small amount of CPME, and this height boiling still liquid 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 using are Rhom and Hass's product.
Embodiment 1
Using said system to carry out continuous prodution, the CPE of vaporization flows through the pressure of adsorption column and is
2MPa、100℃；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.Cyclopentenes is 1.6:1 with the mol ratio of methanol, 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 sampling)；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
Use 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.Cyclopentenes is 1.6:1 with the mol ratio of methanol, 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 sampling)；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
Comparing with embodiment 2, difference is, is not filled by cyclopentadiene resin in adsorption column.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 sampling)；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
Comparing with embodiment 2, difference is, uses single-stage CPME rectifying column to refine product.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 sampling)；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
Comparing with embodiment 1, difference is, 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 sampling)；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
Comparing with embodiment 1, difference is, fills 80wt% grain through the amberlyst15 for 1.2-1.5mm in fixed bed reactors；20wt% grain is through the amberlyst-35 acidic resins for 0.5-0.8mm as catalyst, and 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 sampling)；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
Comparing with embodiment 1, difference is, fills 70wt% grain through the amberlyst15 for 1.2-1.5mm in fixed bed reactors；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 sampling)；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, difference is, cyclopentenes is 1.05:1 with the mol ratio of methanol, and after continuous prodution terminates, 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 sampling)；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, difference is, cyclopentenes is 2:1 with the mol ratio of methanol, and after continuous prodution terminates, 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 sampling)；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 used to carry out continuous prodution, difference is, the catalyst of the filling in fixed bed reactors be 100% warp be the amberlyst15 of 1.2-1.5mm, 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 sampling)；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 (8)
1. the continuous production system of a cyclopentyl methyl ether, it is characterised in that include material carburetion system, fixed bed reactors, product separation system；
Described material carburetion system include the CPE carburator with CPE entrance, after receiving vaporization the adsorption column of CPE, with the methyl alcohol vaporizing device of methanol inlet and material carburetor；
Described product separation system includes lightness-removing column, CPME rectifier unit, split-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 split-phase groove entrance.
2. the continuous production system of cyclopentyl methyl ether as claimed in claim 1, it is characterised in that be filled with cyclopentadiene resin in described adsorption column.
3. the continuous production system of cyclopentyl methyl ether as claimed in claim 1, it is characterised in that be filled with acid-exchange resin in described fixed bed reactors.
4. the continuous production system of cyclopentyl methyl ether as claimed in claim 3, it is characterised in that be additionally provided with CPME adsorption column between the outlet of CPME rectifier unit and CPME storage tank connecting line.
5. the continuous production system of cyclopentyl methyl ether as claimed in claim 4, it is characterised in that be filled with molecular sieve in described CPME adsorption column.
6. the continuous production system of cyclopentyl methyl ether as claimed in claim 5, it is characterized in that, the outlet of CPME adsorption column is additionally provided with branch road on CPME storage tank connecting line, and this branch road is connected with the activation entrance of adsorption column, and activation outlet is incorporated to CPME rectifier unit entrance by pipeline.
7. the continuous production system of cyclopentyl methyl ether as claimed in claim 6, it is characterised in that described CPME rectifier unit is in series by multistage CPME rectifying column.
8. the continuous production system of cyclopentyl methyl ether as claimed in claim 7, it is characterized in that, 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.
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