CN107235831A - The method that dicyclohexyl ether is reclaimed from cyclohexanol rectifying column kettle liquid - Google Patents
The method that dicyclohexyl ether is reclaimed from cyclohexanol rectifying column kettle liquid Download PDFInfo
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- CN107235831A CN107235831A CN201710532096.XA CN201710532096A CN107235831A CN 107235831 A CN107235831 A CN 107235831A CN 201710532096 A CN201710532096 A CN 201710532096A CN 107235831 A CN107235831 A CN 107235831A
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- storage tank
- rectifying column
- kettle liquid
- cyclohexanol
- extractant
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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
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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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- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of method that dicyclohexyl ether is reclaimed in rectifying column kettle liquid from cyclohexanol, belong to chemical technology field.This method reclaims dicyclohexyl ether under double tower pattern by extractant of water from cyclohexanol rectifying column kettle liquid.Kettle liquid is pumped into first rectifying column first, extractant is made with water, rectification under vacuum is to be sufficiently separated out dicyclohexyl ether and part heavy constituent, then its kettle liquid is pumped into Second distillation column and makees extractant with water, carry out rectification under vacuum, overhead distillate, which is stood, divides a liquid, and the distillate of upper strata cut and first rectifying column is incorporated at one, and heavy constituent is obtained from Second distillation column tower reactor.Present invention water makees extractant, by rectification under vacuum, has not only obtained the dicyclohexyl ether of high-purity, and distillate upper strata dicyclohexyl ether content reaches 95%.And provide possibility more to reclaim cyclohexanol.Water is economical and practical as extractant environmental protection, temperature needed for reducing distillation process, improves economic benefit.
Description
Technical field
The present invention relates to a kind of method that dicyclohexyl ether is reclaimed in rectifying column kettle liquid from cyclohexanol, belong to Chemical Engineering Technology neck
Domain.
Background technology
Cyclohexanol is generally industrially prepared using cyclohexane oxidation process and cyclohexene hydration method at present, inevitably
The accessory substances such as dicyclohexyl ether, cyclohexylidene hexamethylene and 1- cyclohexyl ring hexenes can be produced, in the bottom liquid of synthesizing cyclohexanol
Dicyclohexyl ether accounts for nearly 9%.Prior art obtains the cyclohexanol of part high-purity, part cyclohexanol and heavy constituent by rectifying
Constitute kettle liquid.Dicyclohexyl ether and cyclohexanol are rich in kettle liquid, wherein dicyclohexyl ether is high economic value product, must so having
Dicyclohexyl ether is reclaimed.Twice laid is realized, environmental pollution is reduced.
The content of the invention
For the purpose of fully reclaiming the dicyclohexyl ether in cyclohexanol rectifying column kettle liquid, the present invention provides a kind of from cyclohexanol
The method that dicyclohexyl ether is reclaimed in rectifying column kettle liquid.
To realize the purpose of the present invention, the present invention propose double tower be used in conjunction, rectification under vacuum, the method for making with water extractant.
Realized especially by following technical scheme：
Dicyclohexyl ether retracting device is used first, and the device includes rectifying column, storage tank and cooler, it is characterised in that rectifying
Tower uses double tower, is connected in series by pump and storage tank A；Complete condenser A is connected by pipeline at the top of first rectifying column, complete condenser A connects
Meet storage tank B, storage tank B connection storage tanks G；Complete condenser B, complete condenser B connection storage tank C, storage are connected by pipeline at the top of Second distillation column
Tank C is connected in parallel storage tank G, storage tank D and storage tank F simultaneously by valve, and storage tank F connects first rectifying column and second by parallel connection of pumps
Rectifying column；Complete condenser B is connected in parallel complete condenser A and vavuum pump simultaneously；Second distillation column bottom connects discharging pump, discharging pump respectively
Connect storage tank E.
Each rectifying column inner top is provided with cooler.Bottom connects dehvery pump.
Rectifying column is using ceramic raschig rings as filler in described device.Extractant is deionized water in described device.
Cyclohexanol rectifying tower reactor liquid pump is entered into first rectifying column, while being pumped into the deionized water of kettle liquid weight 35%, stirred,
Tower reactor is gradually heated to 60-70 DEG C, and now tower top is 40-50 DEG C, cooler control backflow.Light component is liquefied by complete condenser A
Flow into first rectifying column and distillate liquid storage tank B, stand a point liquid, lower floor's water flows into extractant storage tank F by gravity, and upper strata light component is flowed into
First rectifying column distillate upper strata storage tank G.Kettle liquid is pumped into intermediate storage tank A, because two tower reaction time are different with temperature, the storage tank
Play cooling and cushioning effect；Then the kettle liquid in the storage tank is pumped into Second distillation column, at the same be pumped into kettle liquid weight 45% go from
Sub- water, stirring, tower reactor is gradually heated to 80-90 DEG C, and now tower top is 50-60 DEG C, cooler control backflow, passes through complete condenser B
Flow into Second distillation column and distillate liquid storage tank C, stood in the storage tank, separation water flows into extractant storage tank F, extractant is pumped into
First rectifying column is recycled, and upper strata flows into dicyclohexyl ether storage tank D by gravity, merges with storage tank G components, kettle liquid is pumped into second
Rectifying tower reactor liquid storage tank E.
It is preferred that：First rectifying column tower top chiller water is cooled down, and temperature control is in 50 DEG C, Second distillation column tower top cooler
It is water-cooled, temperature control is at 60 DEG C.
The principle of the invention and innovative point are：
1st, first rectifying column tower top cooler plays a part of backflow heavy constituent purification light component, and light component is flowed into by complete condenser
Storage tank B, kettle liquid is pumped into storage tank A, because two tower reaction time are different with temperature, and storage tank A plays cooling and cushioning effect.
2nd, two rectifying columns are using water as extractant, first rectifying column reclaimed water and cyclohexanol formation azeotropic mixture, its low boiling point
The azeotropic mixture of the boiling point of other compositions and water formation azeotropic mixture in kettle liquid, water and cyclohexanol is preferentially distillated；In Second distillation column
Go out dicyclohexyl ether also with water and dicyclohexyl ether formation Azeotrope separation.Water is cheap and easy to get, and with cyclohexanol and two rings
Hexyl ether is substantially immiscible, distillates component and is easily layered.
The invention has the advantages that：This method is cheap and easy to get using water as extractant, to environment non-hazardous, and simple to operate,
Required temperature is low in the process of running, so reducing energy consumption, input cost is low, and cyclohexanol rectifying tower reactor can be reclaimed well
Dicyclohexyl ether in liquid, reclaims dicyclohexyl ether purity up to more than 92%, and dicyclohexyl ether total recovery is up to more than 82%.Can be very well
Realize the recovery of the dicyclohexyl ether and cyclohexanol in cyclohexanol rectifying column kettle liquid, economic and environmental protection in ground.
Brief description of the drawings
Fig. 1 is apparatus of the present invention structural representation, in figure, 1- first rectifying columns, 2- coolers A, 3- complete condenser A, 4- storage
Tank B, 5- storage tank G, 6- Second distillation column, 7- coolers B, 8- complete condenser B, 9- storage tank C, 10- storage tank D, 11- vavuum pump, 12- storages
Tank F, 13- extractant delivery pump, 14- storage tanks E, 15- discharging pump, 16- delivery pumps A, 17- storage tank A, 18- delivery pump B, 19- is defeated
Send pump C, 20- storage tank H.
Fig. 2 carries out the gas chromatogram of before processing cyclohexanol rectifying column kettle liquid for the present invention.
Fig. 3 is the gas chromatogram that the embodiment of the present invention 1 carries out kettle liquid after cyclohexanol recovery.
Fig. 4 is the gas chromatogram that the embodiment of the present invention 1 reclaims light component.
Specific embodiment
For the present invention is better described, it is described in detail with reference to accompanying drawing.
Embodiment 1
Device such as accompanying drawing 1, first rectifying column (1) is entered by cyclohexanol rectifying tower reactor liquid pump, at the same be pumped into kettle liquid weight 35% go from
Sub- water, stirs 1h, and negative pressure 0.1MPa, tower reactor is gradually heated to 60 DEG C, and now tower top is 44 DEG C, cooler A (2) control backflows,
Improve light component purity.Light component flows into first rectifying column by complete condenser A (3) liquefaction and distillates liquid storage tank B (4), obtains hexamethylene
Alcohol, stands a point liquid, and lower floor's water flows into extractant storage tank F (12) by gravity, and upper strata light component is flowed on first rectifying column distillate
Layer storage tank G (5), obtains dicyclohexyl ether.Kettle liquid is pumped into intermediate storage tank A (17), because two tower reaction time are different with temperature, should
The kettle liquid that storage tank is risen in cooling and cushioning effect, the storage tank is pumped into Second distillation column (6), while being pumped into going for kettle liquid weight 45%
Ionized water, stirs 1h, and negative pressure 0.1MPa, tower reactor is gradually heated to 80 DEG C, and now tower top is 56 DEG C, and cooler B (7) is controlled back
Stream, improves distillate purity, and flowing into Second distillation column by complete condenser B (8) distillates liquid storage tank C (9), obtains quiet in the storage tank
Put, obtain cyclohexanol, separation water flows into extractant storage tank F (12), and extractant is pumped into first rectifying column recycling, and upper strata is by weight
Power flows into dicyclohexyl ether storage tank D（10）, dicyclohexyl ether is obtained, is merged with storage tank G components, kettle liquid is pumped into Second distillation column kettle
Liquid storage tank E (14).
Present invention temperature required in the process of running is low, so reducing energy consumption, water is cheap and easy to get as extractant, right
Environment non-hazardous, and can largely reclaim cyclohexanol and dicyclohexyl ether in cyclohexanol rectifying column kettle liquid.
Claims (2)
1. the method for dicyclohexyl ether is reclaimed from cyclohexanol rectifying column kettle liquid, it is characterised in that use cyclohexanol retracting device,
The device includes rectifying column, storage tank and cooler, it is characterised in that rectifying column uses double tower, is connected by pump and storage tank A series connection
Connect；Complete condenser A, complete condenser A connections storage tank B, storage tank B connection storage tank G are connected by pipeline at the top of first rectifying column；Second rectifying
Top of tower connects complete condenser B by pipeline, and complete condenser B connections storage tank C, storage tank C are connected in parallel storage tank G, storage simultaneously by valve
Tank D and storage tank F, storage tank F connect first rectifying column and Second distillation column by parallel connection of pumps；Complete condenser B is connected in parallel complete solidifying simultaneously
Device A and vavuum pump；Second distillation column bottom connects discharging pump, discharging pump connection storage tank E respectively；
Each rectifying column inner top is provided with cooler, bottom connection dehvery pump；
Rectifying column is using ceramic raschig rings as filler in described device, and extractant is deionized water in described device；
Cyclohexanol rectifying tower reactor liquid pump is entered into first rectifying column, while being pumped into the deionized water of kettle liquid weight 35%, stirred, tower reactor
60-70 DEG C is gradually heated to, now tower top is 40-50 DEG C, cooler control backflow, light component is liquefied by complete condenser A and flowed into
First rectifying column distillates liquid storage tank B, stands a point liquid, and lower floor's water flows into extractant storage tank F by gravity, and upper strata light component flows into first
Rectifying column distillate upper strata storage tank G；
Kettle liquid is pumped into intermediate storage tank A, because two tower reaction time are different with temperature, and the storage tank plays cooling and cushioning effect；Then
Kettle liquid in the storage tank is pumped into Second distillation column, while being pumped into the deionized water of kettle liquid weight 45%, stirred, tower reactor gradually adds
Heat is to 80-90 DEG C, and now tower top is 50-60 DEG C, cooler control backflow, and Second distillation column distillate is flowed into by complete condenser B
Storage tank C, is stood in the storage tank, and separation water flows into extractant storage tank F, and extractant is pumped into first rectifying column recycling,
Upper strata flows into dicyclohexyl ether storage tank D by gravity, merges with storage tank G components, kettle liquid is pumped into Second distillation column kettle liquid storage tank E.
2. the method for dicyclohexyl ether is reclaimed from cyclohexanol rectifying column kettle liquid as claimed in claim 1, it is characterised in that the
One rectifying column tower top chiller water is cooled down, and temperature control is in 50 DEG C, the cooling of Second distillation column tower top chiller water, temperature control
System is at 60 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710532096.XA CN107235831A (en) | 2017-07-03 | 2017-07-03 | The method that dicyclohexyl ether is reclaimed from cyclohexanol rectifying column kettle liquid |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710532096.XA CN107235831A (en) | 2017-07-03 | 2017-07-03 | The method that dicyclohexyl ether is reclaimed from cyclohexanol rectifying column kettle liquid |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108299139A (en) * | 2018-01-30 | 2018-07-20 | 岳阳昌德化工实业有限公司 | The preparation method of cyclohexene |
| CN108707065A (en) * | 2018-08-10 | 2018-10-26 | 平顶山市神马万里化工股份有限公司 | The method and its device of dicyclohexyl ether are extracted from cyclohexanol distillation residual liquid |
| CN109251134A (en) * | 2018-10-26 | 2019-01-22 | 河南省化工研究所有限责任公司 | A kind of refining methd of the dicyclohexyl ether recycled in cyclohexanol distillation residual liquid |
| CN114920624A (en) * | 2022-05-27 | 2022-08-19 | 辽宁石油化工大学 | Separation and purification method and system for cyclohexanol and butyl cyclohexyl ether |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN204111623U (en) * | 2014-08-06 | 2015-01-21 | 东营市海科新源化工有限责任公司 | A kind of process unit of purifying for by product diisopropyl ether in Virahol production |
| CN104817429A (en) * | 2015-04-10 | 2015-08-05 | 平顶山市神马万里化工股份有限公司 | Method for recovering cyclohexanol from bottom material fluid of cyclohexanol rectifying tower |
-
2017
- 2017-07-03 CN CN201710532096.XA patent/CN107235831A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN204111623U (en) * | 2014-08-06 | 2015-01-21 | 东营市海科新源化工有限责任公司 | A kind of process unit of purifying for by product diisopropyl ether in Virahol production |
| CN104817429A (en) * | 2015-04-10 | 2015-08-05 | 平顶山市神马万里化工股份有限公司 | Method for recovering cyclohexanol from bottom material fluid of cyclohexanol rectifying tower |
Non-Patent Citations (1)
| Title |
|---|
| HOU WEIFENG 等: "Modeling, Simulation and Optimization of a Whole Industrial Catalytic Naphtha Reforming Process on Aspen Plus Platform", 《CHINESE JOURNAL OF CHEMICAL ENGINEERING》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108299139A (en) * | 2018-01-30 | 2018-07-20 | 岳阳昌德化工实业有限公司 | The preparation method of cyclohexene |
| CN108299139B (en) * | 2018-01-30 | 2020-10-20 | 岳阳昌德环境科技有限公司 | Preparation method of cyclohexene |
| CN108707065A (en) * | 2018-08-10 | 2018-10-26 | 平顶山市神马万里化工股份有限公司 | The method and its device of dicyclohexyl ether are extracted from cyclohexanol distillation residual liquid |
| CN108707065B (en) * | 2018-08-10 | 2021-10-08 | 平顶山市神马万里化工股份有限公司 | Method and device for extracting dicyclohexyl ether from cyclohexanol rectification residual liquid |
| CN109251134A (en) * | 2018-10-26 | 2019-01-22 | 河南省化工研究所有限责任公司 | A kind of refining methd of the dicyclohexyl ether recycled in cyclohexanol distillation residual liquid |
| CN109251134B (en) * | 2018-10-26 | 2021-04-23 | 河南省化工研究所有限责任公司 | Refining method of dicyclohexyl ether recovered from cyclohexanol distillation residual liquid |
| CN114920624A (en) * | 2022-05-27 | 2022-08-19 | 辽宁石油化工大学 | Separation and purification method and system for cyclohexanol and butyl cyclohexyl ether |
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