CN102993128B - Device and method for recovering epoxypropane from epoxypropane-carbon dioxide copolymer washing liquid - Google Patents
Device and method for recovering epoxypropane from epoxypropane-carbon dioxide copolymer washing liquid Download PDFInfo
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- CN102993128B CN102993128B CN201210488862.4A CN201210488862A CN102993128B CN 102993128 B CN102993128 B CN 102993128B CN 201210488862 A CN201210488862 A CN 201210488862A CN 102993128 B CN102993128 B CN 102993128B
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Abstract
The invention discloses a device and a method for recovering epoxypropane from epoxypropane-carbon dioxide copolymer washing liquid; the device is characterized in that a liquid-solid separator is connected with an inlet arranged in the middle of a rough epoxypropane rectifying tower; an outlet arranged at the top of the rough epoxypropane rectifying tower is connected with an inlet arranged at the lower part of an extraction rectifying tower; an outlet arranged at the bottom of the rough epoxypropane rectifying tower is connected with an inlet of a methanol recovery tower; an outlet arranged at the top of the extraction rectifying tower is connected with a molecular sieve absorption tower; an outlet arranged at the bottom of the extraction rectifying tower is connected with an inlet arranged in the middle of an extraction water recovery tower; an outlet arranged at the top of the extraction water recovery tower is connected with the inlet arranged in the middle of the rough epoxypropane rectifying tower; and the epoxypropane-carbon dioxide copolymer washing liquid is sequentially sent into the liquid-solid separator, the rough epoxypropane rectifying tower, the extraction rectifying tower and the molecular sieve absorption tower, so as to obtain high-purity epoxypropane which has the purity being higher than 99.96wt% and reaches the polymer grade requirement. The device and the method have the advantages that energy consumption is low, few side reactions and side products are generated and the recovered epoxypropane has high purity.
Description
Technical field
The present invention relates to a kind of propylene oxide recovery process and equipment, especially relate to a kind of Apparatus for () and method therefor reclaiming propylene oxide from propylene oxide-carbon dioxide multipolymer washings.
Background technology
One of main raw material of synthesis carbonic acid gas one epoxy propane copolymer, carbonic acid gas is the CO that many field of industrial productions produce
2waste gas, is discharged in atmospheric layer and not only causes environmental pollution, and is the waste of carbon resource.Carbonic acid gas, under catalyst action, during by activation to higher degree, with epoxide generation copolyreaction, generates carbonic acid gas one epoxy propane copolymer, through aftertreatment, just obtains carbonic acid gas resin material.Can by CO by the synthesis of carbonic acid gas one epoxy propane copolymer
2resource immobilization, this not only opens new carbon resource, alleviates the shortage of petrochemical materials, and can protect the ecotope of the mankind.On the other hand, the complete biodegradable characteristic of carbonic acid gas one epoxy propane copolymer, the nonbiodegradable common plastics of replacement of use, can be widely used in wrapping material, table ware, daily use Sundry goods, disposable medical material, the aspects such as operation stitching.Also important meaning is had for solution " white pollution ".
Existing carbon dioxide-epoxypropane copolymer is by by carbonic acid gas (CO
2) be placed in synthesis reaction vessel with propylene oxide (PO), control the temperature and pressure in kettle, under the effect of catalyzer, directly carry out Reactive Synthesis.The carbon dioxide-epoxypropane copolymer surface adhesion be obtained by reacting has the propylene oxide of a large amount of non-complete reaction, therefore need by cohesion washing process, the propylene oxide sticking to the non-complete reaction of solid polymer surfaces to be separated completely with solid polymer, but the washings that propylene oxide-carbon dioxide multipolymer cohesion washing process is discharged contains methyl alcohol, propylene oxide, methylcarbonate, 2-methoxy-1-propanol, 1-methoxy-2-propanol and a small amount of low-molecular(weight)polymer, glycerine, granules of catalyst simultaneously also containing inactivation, containing a large amount of propylene oxide in cohesion washings, these propylene oxide need to reclaim with recycling.Therefore, from so complicated mixed solution, obtain that to reach the propylene oxide that polymerization quality requires very difficult.
Because methyl alcohol and propylene oxide are after temperature is more than 90 DEG C, can react, generate oligopolymer, simultaneously after working pressure is more than 0.3MPag, methyl alcohol and propylene oxide can form azeotrope.Therefore, methyl alcohol must select suitable operational condition with being separated of propylene oxide, and takes multiple means, just can avoid the generation of oligopolymer, azeotrope, reclaims the high purity propylene oxide obtaining and meet polymerization and require simultaneously.In view of above factor, existing cohesion washings takes rectification under vacuum to carry out purifies and separates to propylene oxide usually, and ensures that system is carried out under low operating temperature.But adopt rectification under vacuum system, need to consume high-grade cold, will arrange vaccum-pumping equipment, energy consumption is high, and the purity of the propylene oxide obtained is for can only reach 99.5% simultaneously, directly can't gets back to polyreaction and utilize.
Summary of the invention
Technical problem to be solved by this invention be to provide a kind of energy consumption low, from propylene oxide-carbon dioxide multipolymer washings, reclaim the Apparatus for () and method therefor that propene oxide purity reaches polymerization-grade requirement.
The present invention solves the problems of the technologies described above adopted technical scheme: a kind of equipment reclaiming propylene oxide from propylene oxide-carbon dioxide multipolymer washings, comprise liquid-solid separator, crude propene oxide rectifying tower, methanol distillation column, extractive distillation column, extraction water recovery tower and adsorbing tower with molecular sieve, described liquid-solid separator is connected with the centre inlet of described crude propene oxide rectifying tower, the tower top outlet of described crude propene oxide rectifying tower is connected with the lower inlet of described extractive distillation column, the tower bottom outlet of described crude propene oxide rectifying tower is connected with the import of described methanol distillation column, the tower top outlet of described extractive distillation column is connected with described adsorbing tower with molecular sieve, the tower bottom outlet of described extractive distillation column is connected with the centre inlet of described extraction water recovery tower, the tower top outlet of described extraction water recovery tower is connected with the centre inlet of described crude propene oxide rectifying tower, the tower bottom outlet of described extraction water recovery tower is connected with the centre inlet of described extractive distillation column.
The tower top of the tower top of described crude propene oxide rectifying tower, the tower top of described methanol distillation column, described extractive distillation column and the tower top of described extraction water recovery tower are connected with overhead condenser, return tank, reflux pump respectively in turn.
At the bottom of the tower of described crude propene oxide rectifying tower, at the bottom of the tower of methanol distillation column, at the bottom of the tower of described extractive distillation column, at the bottom of the tower of described extraction water recovery tower, be connected to tower bottom reboiler.
Pressure pump is respectively arranged with between the tower bottom outlet of described crude propene oxide rectifying tower and the import of described methanol distillation column, between the tower top outlet of described extractive distillation column and described adsorbing tower with molecular sieve, between the tower bottom outlet of described extractive distillation column and the centre inlet of described extraction water recovery tower and between the tower bottom outlet of described extraction water recovery tower and the centre inlet of described extractive distillation column.
The tower bottom outlet of described extraction water recovery tower is connected with de-salted water inlet ductwork.
From propylene oxide-carbon dioxide multipolymer washings, reclaim a method for propylene oxide, concrete steps are as follows:
(1) propylene oxide-carbon dioxide multipolymer washings is sent into liquid-solid separator and remove most of granules of catalyst, obtain washing supernatant liquor;
(2) supernatant liquor will be washed and send into crude propene oxide rectifying tower, control tower top temperature is 35 ~ 45 DEG C, tower top pressure is 101 ~ 130kpa, be separated through crude propene oxide rectifying tower, tower top obtains the crude propene oxide that purity is 95 ~ 98wt%, obtains the mixing solutions containing methyl alcohol at the bottom of tower;
(3) crude propene oxide is sent into extractive distillation column, controlling tower top temperature is 35 ~ 45 DEG C, and tower top pressure is 101 ~ 130kpa, is separated through extractive distillation column, tower top obtains the propylene oxide of purity higher than 99.95wt%, obtains the aqueous solution containing propylene oxide and methyl alcohol at the bottom of tower;
(4) methanol distillation column is sent being separated the mixing solutions containing methyl alcohol obtained through crude propene oxide rectifying tower into, controlling tower top temperature is 60 ~ 70 DEG C, tower top pressure 101 ~ 130kpa, be separated through methanol distillation column, tower top obtains the methyl alcohol of purity more than 99%, discharges the high boiling mixture matter containing oligopolymer, methoxypropanol at the bottom of tower;
(5) adsorbing tower with molecular sieve is sent into being separated the purity obtained through extractive distillation column higher than the propylene oxide of 99.95wt%, by a small amount of methyl alcohol of containing in molecular sieve adsorption removing propylene oxide, obtain purity higher than 99.96wt% and meet the high pure propylene oxide of polymerization-grade requirement;
(6) extraction water recovery tower is sent being separated the aqueous solution containing propylene oxide and methyl alcohol obtained through extractive distillation column into, control tower top temperature is 40 ~ 50 DEG C, tower top pressure is 101 ~ 130kpa, be separated through extraction water recovery tower, tower top obtains methyl alcohol and propylene oxide mixture, water is extracted at the bottom of tower, described methyl alcohol and propylene oxide mixture are delivered to crude propene oxide rectifying tower and are separated, deliver to extractive distillation column and recycle as extraction solvent after described extraction water and the de-salted water supplemented are mixed in proportion;
(7) repeat above-mentioned steps (1) and carry out cyclical operation to (6).
Described liquid-solid separator is whizzer or cyclone separator.
Described adsorbing tower with molecular sieve is built with 4A molecular sieve.A small amount of methyl alcohol that can contain in absorbing ring Ethylene Oxide.
Recirculation cooler is provided with in described adsorbing tower with molecular sieve.This recirculation cooler can ensure that adsorbing tower with molecular sieve operates at low temperatures, thus ensures the dealcoholysis effect of propylene oxide.
Compared with prior art, the invention has the advantages that: the present invention reclaims the Apparatus for () and method therefor of propylene oxide from propylene oxide-carbon dioxide multipolymer washings, whole process system top temperature is no more than 65 DEG C, pressure is no more than 0.05MPag, therefore low temperature, the low voltage operated limited generation avoiding methyl alcohol and propylene oxide side reaction, thus improve the rate of recovery of methyl alcohol, propylene oxide; Do not need high-grade cold and pumped vacuum systems, energy consumption is low, and process cost is little simultaneously; By taking the optimum combination of the multiple chemical engineering unit operations such as solid-liquor separation, extracting rectifying, molecular sieve adsorption, effectively achieve high purity and the high-recovery of the propylene oxide of recovery.
Accompanying drawing explanation
Fig. 1 is equipment flowsheet schematic diagram of the present invention.
Embodiment
Below in conjunction with accompanying drawing embodiment, the present invention is described in further detail.
Embodiment one
A kind of equipment reclaiming propylene oxide from propylene oxide-carbon dioxide multipolymer washings of the present invention, as shown in Figure 1, comprise liquid-solid separator 1, crude propene oxide rectifying tower 2, methanol distillation column 3, extractive distillation column 4, extraction water recovery tower 5 and adsorbing tower with molecular sieve 6, liquid-solid separator 1 is connected with the centre inlet of crude propene oxide rectifying tower 2, the tower top outlet of crude propene oxide rectifying tower 2 is connected with the lower inlet of extractive distillation column 4, the tower bottom outlet of crude propene oxide rectifying tower 2 is connected with the import of methanol distillation column 3, the tower top outlet of extractive distillation column 4 is connected with adsorbing tower with molecular sieve 6, the tower bottom outlet of extractive distillation column 4 is connected with the centre inlet of extraction water recovery tower 5, the tower top outlet of extraction water recovery tower 5 is connected with the centre inlet of crude propene oxide rectifying tower 2, the tower bottom outlet of extraction water recovery tower 5 is connected with the centre inlet of extractive distillation column 4.
In this particular embodiment, the tower top of the tower top of crude propene oxide rectifying tower 2, the tower top of methanol distillation column 3, the tower top of extractive distillation column 4 and extraction water recovery tower 5 is connected with overhead condenser 7, return tank 8 and reflux pump 9 respectively in turn; Tower bottom reboiler 10 is connected at the bottom of the tower of crude propene oxide rectifying tower 2, at the bottom of the tower of methanol distillation column 3, at the bottom of the tower of extractive distillation column 4 and at the bottom of the tower of extraction water recovery tower 5.
In this particular embodiment, between the tower bottom outlet of crude propene oxide rectifying tower 2 and the import of methanol distillation column 3, between the tower top outlet of extractive distillation column 4 and adsorbing tower with molecular sieve 6, pressure pump 11 is respectively arranged with between the tower bottom outlet of extractive distillation column 4 and the centre inlet of extraction water recovery tower 5 and between the tower bottom outlet of extraction water recovery tower 5 and the centre inlet of extractive distillation column 4; The tower bottom outlet of extraction water recovery tower 5 is connected with de-salted water inlet ductwork 12.
Embodiment two
A kind of method reclaiming propylene oxide from propylene oxide-carbon dioxide multipolymer washings of the present invention, as shown in Figure 1, concrete steps are as follows:
(1) propylene oxide-carbon dioxide multipolymer washings is sent into liquid-solid separator 1 and remove most of granules of catalyst, obtain clear liquid;
(2) clear liquid is sent into crude propene oxide rectifying tower 2, control that tower top temperature is 40 DEG C, tower top pressure is 103kpa, be separated through crude propene oxide rectifying tower 2, tower top obtains the crude propene oxide that purity is 96.5wt%, obtains the mixing solutions containing methyl alcohol at the bottom of tower;
(3) crude propene oxide is sent into extractive distillation column 3, controlling tower top temperature is 39 DEG C, and tower top pressure is 103kpa, is separated through extractive distillation column 3, and tower top obtains the propylene oxide of purity higher than 99.95wt%, obtains the aqueous solution containing propylene oxide and methyl alcohol at the bottom of tower;
(4) methanol distillation column 3 is sent being separated the mixing solutions containing methyl alcohol obtained through crude propene oxide rectifying tower 2 into, controlling tower top temperature is 65 DEG C, tower top pressure 103kpa, be separated through methanol distillation column 3, tower top obtains the methyl alcohol of purity more than 99%, discharges the high boiling mixture matter containing oligopolymer, methoxypropanol at the bottom of tower;
(5) adsorbing tower with molecular sieve 6 is sent into being separated the purity obtained through extractive distillation column 3 higher than the propylene oxide of 99.95wt%, by a small amount of methyl alcohol of containing in molecular sieve adsorption removing propylene oxide, obtain purity higher than 99.96wt% and meet the high pure propylene oxide of polymerization-grade requirement;
(6) extraction water recovery tower 5 is sent being separated the aqueous solution containing propylene oxide and methyl alcohol obtained through extractive distillation column 3 into, control tower top temperature is 46 DEG C, tower top pressure is 103kpa, be separated through extraction water recovery tower 5, tower top obtains methyl alcohol and propylene oxide mixture, water is extracted at the bottom of tower, methyl alcohol and propylene oxide mixture are delivered to crude propene oxide rectifying tower 2 and are separated, deliver to extractive distillation column 3 and recycle as extraction solvent after extraction water and the de-salted water supplemented are mixed in proportion;
(7) repeat above-mentioned steps (1) and carry out cyclical operation to (6).
In this particular embodiment, liquid-solid separator 1 is whizzer or cyclone separator, washings is first by the granules of catalyst of liquid-solid separator (whizzer, cyclone separator etc.) the removing overwhelming majority, these granules of catalyst remove from washings, can alleviate the degree that propylene oxide and methyl alcohol react; Adsorbing tower with molecular sieve 6, built with 4A molecular sieve, is provided with recirculation cooler (not shown) in this adsorbing tower with molecular sieve.This recirculation cooler can ensure that adsorbing tower with molecular sieve operates at low temperatures, thus ensures the dealcoholysis effect of propylene oxide.
Embodiment three
With embodiment two, its difference is: step (2) middle control tower top temperature is 35 DEG C, tower top pressure is 101kpa, and be separated through crude propene oxide rectifying tower 2, tower top obtains the crude propene oxide that purity is 95wt%; Controlling tower top temperature in step (3) is 35 DEG C, and tower top pressure is 101kpa, is separated through extractive distillation column 3, and tower top obtains the propylene oxide of purity higher than 99.95wt%; Controlling tower top temperature in step (4) is 60 DEG C, tower top pressure 101kpa, and be separated through methanol distillation column 3, tower top obtains the methyl alcohol of purity more than 99%; Step (6) middle control tower top temperature is 40 DEG C, tower top pressure is 101kpa.
Embodiment four
With embodiment two, its difference is: step (2) middle control tower top temperature is 45 DEG C, tower top pressure is 130kpa, and be separated through crude propene oxide rectifying tower 2, tower top obtains the crude propene oxide that purity is 98wt%; Controlling tower top temperature in step (3) is 45 DEG C, and tower top pressure is 130kpa, is separated through extractive distillation column 3, and tower top obtains the propylene oxide of purity higher than 99.95wt%; Controlling tower top temperature in step (4) is 70 DEG C, tower top pressure 130kpa, and be separated through methanol distillation column 3, tower top obtains the methyl alcohol of purity more than 99%; Step (6) middle control tower top temperature is 50 DEG C, tower top pressure is 130kpa.
Certainly, above-mentioned explanation is not limitation of the present invention, and the present invention is also not limited to above-mentioned citing.Those skilled in the art are in essential scope of the present invention, and the change made, remodeling, interpolation or replacement, also should belong to protection scope of the present invention.
Claims (5)
1. one kind is reclaimed the equipment of propylene oxide from propylene oxide-carbon dioxide multipolymer washings, it is characterized in that: comprise liquid-solid separator, crude propene oxide rectifying tower, methanol distillation column, extractive distillation column, extraction water recovery tower and adsorbing tower with molecular sieve, described liquid-solid separator is connected with the centre inlet of described crude propene oxide rectifying tower, the tower top outlet of described crude propene oxide rectifying tower is connected with the lower inlet of described extractive distillation column, the tower bottom outlet of described crude propene oxide rectifying tower is connected with the import of described methanol distillation column, the tower top outlet of described extractive distillation column is connected with described adsorbing tower with molecular sieve, the tower bottom outlet of described extractive distillation column is connected with the centre inlet of described extraction water recovery tower, the tower top outlet of described extraction water recovery tower is connected with the centre inlet of described crude propene oxide rectifying tower, the tower bottom outlet of described extraction water recovery tower is connected with the centre inlet of described extractive distillation column, the tower top of described crude propene oxide rectifying tower, the tower top of described methanol distillation column, the tower top of described extractive distillation column and the tower top of described extraction water recovery tower are connected with overhead condenser in turn respectively, return tank, reflux pump, at the bottom of the tower of described crude propene oxide rectifying tower, at the bottom of the tower of methanol distillation column, at the bottom of the tower of described extractive distillation column, tower bottom reboiler is connected at the bottom of the tower of described extraction water recovery tower, between the tower bottom outlet of described crude propene oxide rectifying tower and the import of described methanol distillation column, between the tower top outlet of described extractive distillation column and described adsorbing tower with molecular sieve, pressure pump is respectively arranged with between the tower bottom outlet of described extractive distillation column and the centre inlet of described extraction water recovery tower and between the tower bottom outlet of described extraction water recovery tower and the centre inlet of described extractive distillation column, the tower bottom outlet of described extraction water recovery tower is connected with de-salted water inlet ductwork.
2. the method reclaiming propylene oxide from propylene oxide-carbon dioxide multipolymer washings according to claim 1, is characterized in that concrete steps are as follows:
(1) propylene oxide-carbon dioxide multipolymer washings is sent into liquid-solid separator and remove most of granules of catalyst, obtain washing supernatant liquor;
(2) supernatant liquor will be washed and send into crude propene oxide rectifying tower, control tower top temperature is 35 ~ 45 DEG C, tower top pressure is 101 ~ 130kpa, be separated through crude propene oxide rectifying tower, tower top obtains the crude propene oxide that purity is 95 ~ 98%, obtains the mixing solutions containing methyl alcohol at the bottom of tower;
(3) crude propene oxide is sent into extractive distillation column, controlling tower top temperature is 35 ~ 45 DEG C, and tower top pressure is 101 ~ 130kpa, is separated through extractive distillation column, tower top obtains the propylene oxide of purity higher than 99.95wt%, obtains the aqueous solution containing propylene oxide and methyl alcohol at the bottom of tower;
(4) methanol distillation column is sent being separated the mixing solutions containing methyl alcohol obtained through crude propene oxide rectifying tower into, controlling tower top temperature is 60 ~ 70 DEG C, tower top pressure 101 ~ 130kpa, be separated through methanol distillation column, tower top obtains the methyl alcohol of purity more than 99%, discharges the high boiling mixture matter containing oligopolymer, methoxypropanol at the bottom of tower;
(5) adsorbing tower with molecular sieve is sent into being separated the purity obtained through extractive distillation column higher than the propylene oxide of 99.95wt%, by a small amount of methyl alcohol of containing in molecular sieve adsorption removing propylene oxide, obtain purity higher than 99.96wt% and meet the high pure propylene oxide of polymerization-grade requirement;
(6) extraction water recovery tower is sent being separated the aqueous solution containing propylene oxide and methyl alcohol obtained through extractive distillation column into, control tower top temperature is 40 ~ 50 DEG C, tower top pressure is 101 ~ 130kpa, be separated through extraction water recovery tower, tower top obtains methyl alcohol and propylene oxide mixture, water is extracted at the bottom of tower, described methyl alcohol and propylene oxide mixture are delivered to crude propene oxide rectifying tower and are separated, deliver to extractive distillation column and recycle as extraction solvent after described extraction water and the de-salted water supplemented are mixed in proportion;
(7) repeat above-mentioned steps (1) and carry out cyclical operation to (6).
3. the method reclaiming propylene oxide from propylene oxide-carbon dioxide multipolymer washings according to claim 2, is characterized in that: described liquid-solid separator is whizzer or cyclone separator.
4. the method reclaiming propylene oxide from propylene oxide-carbon dioxide multipolymer washings according to claim 2, is characterized in that: described adsorbing tower with molecular sieve is built with 4A molecular sieve.
5. the method reclaiming propylene oxide from propylene oxide-carbon dioxide multipolymer washings according to claim 4, is characterized in that: be provided with recirculation cooler in described adsorbing tower with molecular sieve.
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| CN201210488862.4A CN102993128B (en) | 2012-11-26 | 2012-11-26 | Device and method for recovering epoxypropane from epoxypropane-carbon dioxide copolymer washing liquid |
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| CN201210488862.4A CN102993128B (en) | 2012-11-26 | 2012-11-26 | Device and method for recovering epoxypropane from epoxypropane-carbon dioxide copolymer washing liquid |
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| CN102993128B true CN102993128B (en) | 2015-01-28 |
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