CN104292080B - The continuous distillation method of two-(2-chloro isopropyl) ether is extracted from epoxy propane slop - Google Patents
The continuous distillation method of two-(2-chloro isopropyl) ether is extracted from epoxy propane slop Download PDFInfo
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- CN104292080B CN104292080B CN201410479709.4A CN201410479709A CN104292080B CN 104292080 B CN104292080 B CN 104292080B CN 201410479709 A CN201410479709 A CN 201410479709A CN 104292080 B CN104292080 B CN 104292080B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/34—Separation; Purification; Stabilisation; Use of additives
- C07C41/40—Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation
- C07C41/42—Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation by distillation
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Abstract
A kind of continuous distillation method extracting two-(2-chloro isopropyl) ether from epoxy propane slop of the present invention, step is as follows: (1) preheating, (2) rectifying removal of impurities, (3) mixing steam cooling are reclaimed; (4) backflow, (5) target product rectifying: described lights column kettle material is delivered to product tower 10 by lights column column bottoms pump 9 and carries out rectifying.The tower reactor of described product tower is heated by product tower reboiler 11.Controlling product tower top working pressure is 0.1 ~ 101.33KPa, reflux ratio 0.1-10, bottom temperature 80-200 DEG C, tower top temperature 60-180 DEG C, and tower top distillates two-(2-chloro isopropyl) ether steam; (6) target product condensation, (7) product reflux, (8) tower bottom are managed.Method provided by the invention extracts the method for two-(2-chloro isopropyl) ether from epoxy propane slop, adopts continuous rectificating technique, does not need to add entrainer water, avoid the problem of equipment corrosion.
Description
Technical field
The invention belongs to rectifying field, relate to the recovery method of effective constituent in a kind of waste liquid, the invention particularly relates to a kind of continuous distillation method extracting two-(2-chloro isopropyl) ether from epoxy propane slop.
Background technology
At present, China's production of propylene oxide mainly adopts chlorohydrination, the by product that this process produces contains 50-85% (wt) 1,2-propylene dichloride and 5-20% (wt) two-(2-chloro isopropyl) ether, in addition, also component is planted containing a small amount of propylene oxide, propylene chlorohydrin, allyl group chlorine water and some unknown aldehyde, ketone etc. more than 30.Because this byproduct compounds is complicated, separating difficulty is large, and yellowish, irritating smell are comparatively large, and most domestic production of propylene oxide producer can only it can be used as low side solvent sell or burn.Along with the fierceness day by day that environmental requirement increasingly stringent and Enterprise business are competed, some scholars and research institution are studied extracting propylene dichloride from epoxy propane slop, but the research of extracting two-(2-chloro isopropyl) ether from epoxy propane slop is less.
Two-(2-chloro isopropyl) ether solubility property is better than propylene dichloride, it is the senior solvent being used as rubber and resin and ethyl cellulose etc., there is very high added value, extract from epoxy propane slop reclaim by product two-(2-chloro isopropyl) ether, pollution can be greatly reduced, reduce raw material and energy consumption, thus strengthen the competitive power of enterprise.
Chinese patent CN1513826A discloses a kind of method that azeotropic distillation extracts two-(2-chloro isopropyl) ether from epoxy propane slop, other entrainer in addition to water that the method provides is difficult to be separated with two-(2-chloro isopropyl) ether, is difficult to obtain practical application.And when adopting water to be entrainer, a large amount of chlorine-containing compounds in waste liquid can be hydrolyzed production hydrochloric acid at rectification temperature 90-115 DEG C, serious to equipment corrosion, azeotropic distillation also can produce a large amount of waste water simultaneously.At present, there is no the report of the continuous rectification separation method extracting two-(2-chloro isopropyl) ether from propylene oxide by chlorohydrination waste liquid.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art part, provide one to provide and can realize automatic control, run continuously, process cost is low, without equipment corrosion, simple, the efficient a kind of continuous distillation method extracting two-(2-chloro isopropyl) ether from epoxy propane slop of extraction element.
The object of the invention is to be achieved through the following technical solutions:
A kind of continuous distillation method extracting two-(2-chloro isopropyl) ether from epoxy propane slop, step is as follows:
(1) preheating: the epoxy propane slop A extracting propylene dichloride sends into epoxy propane slop preheater 2 by waste drains pump 1, the heavy constituent heat exchange of extraction at the bottom of waste liquid and product tower tower in this preheater.
(2) rectifying removal of impurities: the waste liquid after preheating enters lights column 3 and carries out rectifying, and the tower reactor of described lights column is heated by lights column reboiler 4; Controlling tower top working pressure is 0.1 ~ 101.33KPa, and reflux ratio is 0.1-20, and bottom temperature is 80-190 DEG C, and tower top temperature is 30-100 DEG C, and tower top distillates the mixing steam containing propylene dichloride, propylene chlorohydrin etc.;
(3) mixing steam cooling is reclaimed: the described mixing steam containing propylene dichloride, propylene chlorohydrin etc. enters lights column first-stage condenser 5 water coolant partial condensation, and liquid phase enters lights column return tank 7 by gravity; Uncooled vapour phase enters the lights column secondary condenser 6 5-10 DEG C of whole condensation of refrigerated water, and liquid phase enters light constituent storage tank V1 by gravity.The vapor phase exit temperature of described lights column first-stage condenser controls at 35-45 DEG C, and the liquid-phase outlet temperature of described lights column secondary condenser controls at 25-35 DEG C;
(4) reflux: lights column reflux pump 8 (or by gravity) is by the reflux ratio of the material in described lights column return tank according to regulation, and a part sends lights column backflow back to, and another part extraction is to light constituent storage tank V1;
(5) target product rectifying: described lights column kettle material is delivered to product tower 10 by lights column column bottoms pump 9 and carries out rectifying.The tower reactor of described product tower is heated by product tower reboiler 11.Controlling product tower top working pressure is 0.1 ~ 101.33KPa, reflux ratio 0.1-10, bottom temperature 80-200 DEG C, tower top temperature 60-180 DEG C, and tower top distillates two-(2-chloro isopropyl) ether steam;
(6) target product condensation: described two-(2-chloro isopropyl) ether steam enters product tower first-stage condenser 12 and uses water coolant partial condensation, liquid phase enters product tower return tank 14 by gravity; Uncooled vapour phase enters product tower secondary condenser 13, and with the 5-10 DEG C of whole condensation of refrigerated water, liquid phase enters lights column return tank by gravity.The vapor phase exit temperature of described product tower first-stage condenser controls at 50-120 DEG C, and the liquid-phase outlet temperature of described product tower secondary condenser controls at 35-45 DEG C;
(7) product reflux: product tower reflux pump 15 (or by gravity) is by the reflux ratio of the material in described product tower return tank according to regulation, part thing sends the backflow of product tower back to, another part sends into two-(2-chloro isopropyl) ether storage tank V2 after delivering to two-(2-chloro isopropyl) ether water cooler 16 water quench to 45 DEG C;
(8) tower bottom reason: described product tower tower reactor heavy constituent, by after the extraction of product tower column bottoms pump 17, is delivered to after described epoxy propane slop preheater 2 is cooled to 45 DEG C, sent into heavy constituent storage tank V3.
Advantage of the present invention and positively effect are:
1, method provided by the invention extracts the method for two-(2-chloro isopropyl) ether from epoxy propane slop, adopts continuous rectificating technique, does not need to add entrainer water, avoid the problem of equipment corrosion.
2, the rectifying related in method provided by the invention runs continuously, and production efficiency is high, constant product quality, and energy and propylene oxide by chlorohydrination full scale plant run continuously.
3, method provided by the invention is suitable for suitability for industrialized production, and obtain two-(2-chloro isopropyl) ether product water white transparency after separation, have no irritating odor, purity can reach 95-98% (wt), yield 90-95%.
Accompanying drawing explanation
Fig. 1 operational flowchart of the present invention.
Embodiment
Below in conjunction with embodiment, the present invention is further described; Following embodiment is illustrative, is not determinate, can not limit protection scope of the present invention with following embodiment.
Of the present invention extract from propylene oxide by chlorohydrination waste liquid two-(2-chloro isopropyl) ether continuous distillation method, it comprises the following steps:
(1) preheating: the epoxy propane slop A extracting propylene dichloride sends into epoxy propane slop preheater 2 by waste drains pump 1, the heavy constituent heat exchange of extraction at the bottom of waste liquid and product tower tower in this preheater.
(2) rectifying removal of impurities: the waste liquid after preheating enters lights column 3 and carries out rectifying, and the tower reactor of described lights column is heated by lights column reboiler 4; Controlling tower top working pressure is 0.1 ~ 101.33KPa, and reflux ratio is 0.1-20, and bottom temperature is 80-190 DEG C, and tower top temperature is 30-100 DEG C, and tower top distillates the mixing steam containing propylene dichloride, propylene chlorohydrin etc.;
(3) mixing steam cooling is reclaimed: the described mixing steam containing propylene dichloride, propylene chlorohydrin etc. enters lights column first-stage condenser 5 water coolant partial condensation, and liquid phase enters lights column return tank 7 by gravity; Uncooled vapour phase enters the lights column secondary condenser 6 5-10 DEG C of whole condensation of refrigerated water, and liquid phase enters light constituent storage tank V1 by gravity.The vapor phase exit temperature of described lights column first-stage condenser controls at 35-45 DEG C, and the liquid-phase outlet temperature of described lights column secondary condenser controls at 25-35 DEG C;
(4) reflux: lights column reflux pump 8 (or by gravity) is by the reflux ratio of the material in described lights column return tank according to regulation, and a part sends lights column backflow back to, and another part extraction is to light constituent storage tank V1;
(5) target product rectifying: described lights column kettle material is delivered to product tower 10 by lights column column bottoms pump 9 and carries out rectifying.The tower reactor of described product tower is heated by product tower reboiler 11.Controlling product tower top working pressure is 0.1 ~ 101.33KPa, reflux ratio 0.1-10, bottom temperature 80-200 DEG C, tower top temperature 60-180 DEG C, and tower top distillates two-(2-chloro isopropyl) ether steam;
(6) target product condensation: described two-(2-chloro isopropyl) ether steam enters product tower first-stage condenser 12 and uses water coolant partial condensation, liquid phase enters product tower return tank 14 by gravity; Uncooled vapour phase enters product tower secondary condenser 13, and with the 5-10 DEG C of whole condensation of refrigerated water, liquid phase enters lights column return tank by gravity.The vapor phase exit temperature of described product tower first-stage condenser controls at 50-120 DEG C, and the liquid-phase outlet temperature of described product tower secondary condenser controls at 35-45 DEG C;
(7) product reflux: product tower reflux pump 15 (or by gravity) is by the reflux ratio of the material in described product tower return tank according to regulation, part thing sends the backflow of product tower back to, another part sends into two-(2-chloro isopropyl) ether storage tank V2 after delivering to two-(2-chloro isopropyl) ether water cooler 16 water quench to 45 DEG C;
(8) tower bottom reason: described product tower tower reactor heavy constituent, by after the extraction of product tower column bottoms pump 17, is delivered to after described epoxy propane slop preheater 2 is cooled to 45 DEG C, sent into heavy constituent storage tank V3.
Embodiment 1
A kind of continuous distillation method extracting two-(2-chloro isopropyl) ether from epoxy propane slop, step is as follows:
(1) preheating: by the extraction of 500kg/h the epoxy propane slop of propylene dichloride sent into the heavy constituent heat exchange of extraction at the bottom of waste liquid preheater and product tower tower by waste drains pump.
(2) rectifying removal of impurities: the epoxy propane slop after preheating enters lights column and carries out rectifying.Controlling lights column tower top working pressure is 0.1KPa, and reflux ratio is 0.1.Bottom temperature 80 DEG C, tower top temperature is 30 DEG C.
(3) mixing steam cooling is reclaimed: after the mixing steam of the propylene dichloride, propylene chlorohydrin etc. of tower top enters lights column first-stage condenser water coolant partial condensation, liquid phase enters lights column return tank by gravity; Uncooled vapour phase enters lights column secondary condenser with after 5 DEG C of whole condensations of refrigerated water, and liquid phase enters light constituent storage tank by gravity.
(4) reflux: 20kg/h material returns lights column in, by 200kg/h material extraction to light constituent storage tank by lights column by gravity according to the reflux ratio of regulation by the material in lights column return tank.
(5) the lights column kettle material of target product rectifying: 300kg/h is delivered to product tower by lights column column bottoms pump and carries out rectifying.Controlling product column overhead working pressure is 0.1KPa, reflux ratio 0.1, bottom temperature 80 DEG C, tower top temperature 60 DEG C.
(6) target product condensation: tower top distillate two-after (2-chloro isopropyl) ether steam enters product tower first-stage condenser water coolant partial condensation, liquid phase enters product tower return tank by gravity; Uncooled vapour phase enters product tower secondary condenser with after 5 DEG C of whole condensations of refrigerated water, and liquid phase enters product tower return tank by gravity.
(7) product reflux: the material of 25kg/h returns in product tower according to the reflux ratio of regulation by gravity by the material in product tower return tank, the material of 250kg/h is delivered to two-(2-chloro isopropyl) ether water cooler, with after water quench to 45 DEG C, send into two-(2-chloro isopropyl) ether storage tank.
(8) tower bottom reason: the product tower tower reactor heavy constituent of 50kg/h, by delivering to after epoxy propane slop preheater cools after the extraction of product tower column bottoms pump, sends into heavy constituent storage tank.Products obtained therefrom purity 95%, yield 90%.
Embodiment 2
A kind of continuous distillation method extracting two-(2-chloro isopropyl) ether from epoxy propane slop, step is as follows:
(1) preheating: by the extraction of 1000kg/h the epoxy propane slop of propylene dichloride sent into the heavy constituent heat exchange of extraction at the bottom of waste liquid preheater and product tower tower by waste drains pump.
(2) rectifying removal of impurities: the epoxy propane slop after preheating enters lights column and carries out rectifying.Controlling lights column tower top working pressure is 50KPa, and reflux ratio is 10, bottom temperature 190 DEG C, and tower top temperature is 50 DEG C.
(3) mixing steam cooling is reclaimed: after the mixing steam of the propylene dichloride, propylene chlorohydrin etc. of tower top enters lights column first-stage condenser water coolant partial condensation, liquid phase enters lights column return tank by gravity; Uncooled vapour phase enters lights column secondary condenser with after 5 DEG C of whole condensations of refrigerated water, and liquid phase enters light constituent storage tank by gravity.
(4) reflux: 4000kg/h material returns lights column in, by 400kg/h material extraction to light constituent storage tank by lights column by gravity according to the reflux ratio of regulation by the material in lights column return tank.
(5) the lights column kettle material of target product rectifying: 600kg/h is delivered to product tower by lights column column bottoms pump and carries out rectifying.Controlling product column overhead working pressure is 50KPa, reflux ratio 5.Bottom temperature 150 DEG C, tower top temperature 140 DEG C.
(6) target product condensation: tower top distillate two-after (2-chloro isopropyl) ether steam enters product tower first-stage condenser water coolant partial condensation, liquid phase enters product tower return tank by gravity; Uncooled vapour phase enters product tower secondary condenser with after 5 DEG C of whole condensations of refrigerated water, and liquid phase enters product tower return tank by gravity.
(7) product reflux: the material of 2750kg/h returns in product tower according to the reflux ratio of regulation by gravity by the material in product tower return tank, the material of 550kg/h is delivered to two-(2-chloro isopropyl) ether water cooler, with after water quench to 45 DEG C, send into two-(2-chloro isopropyl) ether storage tank.
(8) tower bottom reason: the product tower tower reactor heavy constituent of 50kg/h, by delivering to after epoxy propane slop preheater cools after the extraction of product tower column bottoms pump, sends into heavy constituent storage tank.Products obtained therefrom purity 97%, yield 94%.
Embodiment 3
A kind of continuous distillation method extracting two-(2-chloro isopropyl) ether from epoxy propane slop, step is as follows:
(1) preheating: by the extraction of 3000kg/h the epoxy propane slop of propylene dichloride sent into the heavy constituent heat exchange of extraction at the bottom of waste liquid preheater and product tower tower by waste drains pump.
(2) rectifying removal of impurities: the epoxy propane slop after preheating enters lights column and carries out rectifying.Controlling lights column tower top working pressure is 101.33KPa, and reflux ratio is 20, bottom temperature 130 DEG C, and tower top temperature is 100 DEG C.
(3) mixing steam cooling is reclaimed: after the mixing steam of the propylene dichloride, propylene chlorohydrin etc. of tower top enters lights column first-stage condenser water coolant partial condensation, liquid phase enters lights column return tank by gravity; Uncooled vapour phase enters lights column secondary condenser with after 5 DEG C of whole condensations of refrigerated water, and liquid phase enters light constituent storage tank by gravity.
(4) reflux: 24000kg/h material returns lights column in, by 1200kg/h material extraction to light constituent storage tank by lights column by gravity according to the reflux ratio of regulation by the material in lights column return tank.
(5) the lights column kettle material of target product rectifying: 1800kg/h is delivered to product tower by lights column column bottoms pump and carries out rectifying.Controlling product column overhead working pressure is 101.33KPa, reflux ratio 10.Bottom temperature 200 DEG C, tower top temperature 187 DEG C.
(6) target product condensation: tower top distillate two-after (2-chloro isopropyl) ether steam enters product tower first-stage condenser water coolant partial condensation, liquid phase enters product tower return tank by gravity; Uncooled vapour phase enters product tower secondary condenser with after 5 DEG C of whole condensations of refrigerated water, and liquid phase enters product tower return tank by gravity.
(7) product reflux: the material of 17500kg/h returns in product tower according to the reflux ratio of regulation by gravity by the material in product tower return tank, the material of 1750kg/h is delivered to two-(2-chloro isopropyl) ether water cooler, with after water quench to 45 DEG C, send into two-(2-chloro isopropyl) ether storage tank.
(8) tower bottom reason: the product tower tower reactor heavy constituent of 50kg/h, by delivering to after epoxy propane slop preheater cools after the extraction of product tower column bottoms pump, sends into heavy constituent storage tank.Products obtained therefrom purity 98%, yield 95%.
Claims (1)
1. from epoxy propane slop, extract the continuous distillation method of two-(2-chloro isopropyl) ether, it is characterized in that: step is as follows:
(1) preheating: the epoxy propane slop A extracting propylene dichloride sends into epoxy propane slop preheater by waste drains pump, the heavy constituent heat exchange of extraction at the bottom of waste liquid and product tower tower in this preheater;
(2) rectifying removal of impurities: the waste liquid after preheating enters lights column and carries out rectifying, the tower reactor of described lights column is heated by lights column reboiler; Controlling tower top working pressure is 0.1 ~ 101.33KPa, and reflux ratio is 0.1-20, and bottom temperature is 80-190 DEG C, and tower top temperature is 30-100 DEG C, and tower top distillates the mixing steam containing propylene dichloride, propylene chlorohydrin;
(3) mixing steam cooling is reclaimed: the described mixing steam containing propylene dichloride, propylene chlorohydrin enters lights column first-stage condenser water coolant partial condensation, and liquid phase enters lights column return tank by gravity; Uncooled vapour phase enters the 5-10 DEG C of whole condensation of refrigerated water of lights column secondary condenser, liquid phase enters light constituent storage tank V1 by gravity, the vapor phase exit temperature of described lights column first-stage condenser controls at 35-45 DEG C, and the liquid-phase outlet temperature of described lights column secondary condenser controls at 25-35 DEG C;
(4) reflux: lights column reflux pump is by the reflux ratio of the material in described lights column return tank according to regulation, and a part sends lights column backflow back to, and another part extraction is to light constituent storage tank V1;
(5) target product rectifying: described lights column kettle material is delivered to product tower by lights column column bottoms pump and carries out rectifying, the tower reactor of described product tower is heated by product tower reboiler, controlling product tower top working pressure is 0.1 ~ 101.33KPa, reflux ratio 0.1-10, bottom temperature 80-200 DEG C, tower top temperature 60-180 DEG C, tower top distillates two-(2-chloro isopropyl) ether steam;
(6) target product condensation: described two-(2-chloro isopropyl) ether steam enters product tower first-stage condenser water coolant partial condensation, liquid phase enters product tower return tank by gravity; Uncooled vapour phase enters product tower secondary condenser, with the 5-10 DEG C of whole condensation of refrigerated water, liquid phase enters lights column return tank by gravity, the vapor phase exit temperature of described product tower first-stage condenser controls at 50-120 DEG C, and the liquid-phase outlet temperature of described product tower secondary condenser controls at 35-45 DEG C;
(7) product reflux: product tower reflux pump is by the reflux ratio of the material in described product tower return tank according to regulation, part thing sends the backflow of product tower back to, another part sends into two-(2-chloro isopropyl) ether storage tank V2 after delivering to two-(2-chloro isopropyl) ether water cooler water quench to 45 DEG C;
(8) tower bottom reason: described product tower tower reactor heavy constituent, by after the extraction of product tower column bottoms pump, is delivered to after described epoxy propane slop preheater 2 is cooled to 45 DEG C, sent into heavy constituent storage tank V3.
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| CN201410479709.4A CN104292080B (en) | 2014-09-19 | 2014-09-19 | The continuous distillation method of two-(2-chloro isopropyl) ether is extracted from epoxy propane slop |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1513826A (en) * | 2002-12-31 | 2004-07-21 | 中国石油化工股份有限公司 | Method of extracting bi-(2-chloroisopropyl) ether |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1513826A (en) * | 2002-12-31 | 2004-07-21 | 中国石油化工股份有限公司 | Method of extracting bi-(2-chloroisopropyl) ether |
Non-Patent Citations (2)
| Title |
|---|
| 8万t/a环氧丙烷塔底废水中二氯异丙醚(DCIP)含量的测定;满鑫;《氯碱工业》;20020831(第8期);第37-38页 * |
| Recovery of Bis(2-chloroisopropyl) Ether and 1,2-Dichloropropane from the Waste Water from Propylene Oxide Production;E. MILCHERT et al.;《Chem. Papers》;19961231;第50卷(第5期);第283-287页 * |
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