CN107162877A - The device of cyclohexanol is reclaimed from cyclohexanol rectifying column kettle liquid - Google Patents

The device of cyclohexanol is reclaimed from cyclohexanol rectifying column kettle liquid Download PDF

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Publication number
CN107162877A
CN107162877A CN201710532885.3A CN201710532885A CN107162877A CN 107162877 A CN107162877 A CN 107162877A CN 201710532885 A CN201710532885 A CN 201710532885A CN 107162877 A CN107162877 A CN 107162877A
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CN
China
Prior art keywords
storage tank
cyclohexanol
rectifying column
complete condenser
pump
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
CN201710532885.3A
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Chinese (zh)
Inventor
李涛
杨涛
任保增
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Zhengzhou University
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Zhengzhou University
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Filing date
Publication date
Application filed by Zhengzhou University filed Critical Zhengzhou University
Priority to CN201710532885.3A priority Critical patent/CN107162877A/en
Publication of CN107162877A publication Critical patent/CN107162877A/en
Priority to CN201721194088.0U priority patent/CN207276528U/en
Withdrawn legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
    • C07C29/80Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
    • C07C29/86Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by liquid-liquid treatment

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses the device that cyclohexanol is reclaimed in a kind of rectifying column kettle liquid from cyclohexanol, belong to field of chemical equipment.The device includes rectifying column, storage tank and cooler, it is characterised in that rectifying column uses double tower, is connected in series by pump and storage tank A;Connected at the top of first rectifying column by pipeline at the top of complete condenser A, complete condenser A connection storage tank B, Second distillation column by pipeline connection complete condenser B, complete condenser B connections storage tank C, storage tank C by valve while being connected in parallel storage tank B and storage tank D;Complete condenser B is connected in parallel complete condenser A and vavuum pump simultaneously;Second distillation column bottom connects extractant delivery pump and discharging pump, discharging pump connection storage tank E respectively.The arrangement increases the rate of recovery of cyclohexanol and the purity of recovery cyclohexanol, extractant used is water, economic and environmental protection.

Description

The device of cyclohexanol is reclaimed from cyclohexanol rectifying column kettle liquid
Technical field
The present invention relates to the device that cyclohexanol is reclaimed in a kind of rectifying column kettle liquid from cyclohexanol, belong to chemical technology field.
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.Prior art is obtained by rectifying The cyclohexanol of part high-purity, part cyclohexanol and heavy constituent constitute kettle liquid.Cyclohexanol content is up to 68% in kettle liquid, so having Necessity is reclaimed to cyclohexanol, not only contributes to twice laid, and reduce environmental pollution.
The content of the invention
For the purpose of fully reclaiming the cyclohexanol in cyclohexanol rectifying column kettle liquid, the present invention proposes a kind of recovery cyclohexanol Device.
The purpose of the present invention is achieved through the following technical solutions:Cyclohexanol is reclaimed in the rectifying column kettle liquid from cyclohexanol Device, including rectifying column, storage tank and cooler, it is characterised in that rectifying column uses double tower, pass through pump and storage tank A series connection connects Connect;Connected at the top of first rectifying column by pipeline and pass through pipeline at the top of complete condenser A, complete condenser A connection storage tank B, Second distillation column Complete condenser B is connected, complete condenser B connections storage tank C, storage tank C are connected in parallel storage tank B and storage tank D simultaneously by valve;Complete condenser B is same When be connected in parallel complete condenser A and vavuum pump;Second distillation column bottom connects extractant delivery pump and discharging pump respectively, and discharging pump connects Meet storage tank E.
Each rectifying column inner top is provided with cooler.Bottom connects dehvery pump.
Innovative point of the present invention:First rectifying column tower top cooler plays a part of backflow heavy constituent purification light component, light group Divide and storage tank B is flowed into by complete condenser A.Kettle liquid is pumped into storage tank A, because two tower reaction time are different with temperature, and the storage tank plays cooling And cushioning effect, the kettle liquid in the storage tank is pumped into Second distillation column, while being pumped into 25% extractant, stirs 1h, rectifying.Tower top Cooler makes the azeotropic mixture of heavy constituent and water flow back, and the azeotropic mixture of light component and water is purified, and storage tank is flowed into by complete condenser B C, is stood in the storage tank, and extraction agent flows into storage tank D, and upper strata light component flows into storage tank B by gravity, and kettle liquid is pumped into storage Tank E.
Rectifying column is using ceramic raschig rings as filler in described device.
First rectifying column cooler and Second distillation column cooler are water-cooled in described device.
Extractant is deionized water in described device.
Advantage of the present invention:The device is simple to operate, input cost is low, can more fully reclaim cyclohexanol rectifying column kettle liquid In cyclohexanol, the rate of recovery is up to 83 more than %;Extractant used is water, economic and environmental protection.
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- cooler B, 6- Second distillation column, 7- complete condensers B, 8- storage tank C, 9- storage tank D, 10- vavuum pump, 11- storage tanks E, 12- extraction Take agent delivery pump, 13- discharging pumps, 14- delivery pumps C, 15- storage tank A, 16- delivery pump B, 17- delivery pump A.
Specific embodiment
For the present invention is better described, it is described in detail with reference to accompanying drawing.
Embodiment 1
The device of cyclohexanol, including rectifying column, storage tank and cooler are reclaimed in such as Fig. 1, the rectifying column kettle liquid from cyclohexanol, its It is characterised by, rectifying column uses double tower, is sequentially connected in series by pump (16), storage tank A (15) and pump (14);First rectifying column (1) top is connected by pipeline passes through pipe at the top of complete condenser A (3), complete condenser A (3) connection storage tank B (4), Second distillation column (6) Road connection complete condenser B (7), complete condenser B (7) connection storage tank C (8), storage tank C (8) are connected in parallel storage tank B (4) simultaneously by valve With storage tank D (9);Complete condenser B (7) is while be connected in parallel complete condenser A (3) and vavuum pump (10);Second rectifying (6) tower bottom is distinguished Connect extractant delivery pump(12)And discharging pump(13), discharging pump(13)Connect storage tank E(11).
First rectifying column(1)Inner top is provided with cooler(2), bottom connection dehvery pump(17).Second distillation column(6)It is interior Top is provided with cooler(5), bottom connection dehvery pump(14).
Application examples 1
Cyclohexanol rectifying tower reactor liquid pump is entered into first rectifying column(1), negative pressure 0.1MPa, tower reactor is gradually heated to 100 DEG C, now tower Push up as 60 DEG C, cooler(2)Control backflow, improves light component purity.Light component flows into storage tank B by complete condenser A (3) liquefaction (4), kettle liquid is pumped into storage tank A (15) and is down to normal temperature, is pumped into Second distillation column (6), while passing through extractant delivery pump(12)To Two rectifying columns (6) are pumped into the extractant of above-mentioned kettle liquid 25%, and stir 1h.Tower reactor is gradually heated to 60 DEG C, and now tower top is 44 DEG C, tower top cooler control backflow, raising distillates compositional purity.Light component flows into storage tank C (8) by complete condenser B (7) liquefaction, A point liquid is stood, lower floor's water is put into storage tank D (9), and upper strata light component flows into storage tank B (4) by gravity.
Rectifying column is using ceramic raschig rings as filler in described device.
The control of first rectifying column cooler is 80 DEG C in described device, and the control of Second distillation column cooler is 50 DEG C.
Extractant is deionized water in described device.
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, can realize that the cyclohexanol in cyclohexanol rectifying column kettle liquid is reclaimed well.Cyclohexanol overall recovery is up to 83% and returns The purity of cyclohexanol is received up to 97%.

Claims (2)

1. the device of recovery cyclohexanol from cyclohexanol rectifying column kettle liquid, including rectifying column, storage tank and cooler, its feature exist In rectifying column 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, entirely Complete condenser B is connected by pipeline at the top of condenser A connection storage tank B, Second distillation column, complete condenser B connections storage tank C, storage tank C pass through valve Door is connected in parallel storage tank B and storage tank D simultaneously;Complete condenser B is connected in parallel complete condenser A and vavuum pump simultaneously;Second distillation column bottom Extractant delivery pump and discharging pump, discharging pump connection storage tank E are connected respectively;
Each rectifying column inner top is provided with cooler;Bottom connects dehvery pump.
2. the device of cyclohexanol is reclaimed from cyclohexanol rectifying column kettle liquid as claimed in claim 1, it is characterised in that rectifying column Make filler with ceramic raschig rings.
CN201710532885.3A 2017-07-03 2017-07-03 The device of cyclohexanol is reclaimed from cyclohexanol rectifying column kettle liquid Withdrawn CN107162877A (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
CN201710532885.3A CN107162877A (en) 2017-07-03 2017-07-03 The device of cyclohexanol is reclaimed from cyclohexanol rectifying column kettle liquid
CN201721194088.0U CN207276528U (en) 2017-07-03 2017-09-18 The device of cyclohexanol is recycled from cyclohexanol rectifying column kettle liquid

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710532885.3A CN107162877A (en) 2017-07-03 2017-07-03 The device of cyclohexanol is reclaimed from cyclohexanol rectifying column kettle liquid

Publications (1)

Publication Number Publication Date
CN107162877A true CN107162877A (en) 2017-09-15

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CN201710532885.3A Withdrawn CN107162877A (en) 2017-07-03 2017-07-03 The device of cyclohexanol is reclaimed from cyclohexanol rectifying column kettle liquid
CN201721194088.0U Expired - Fee Related CN207276528U (en) 2017-07-03 2017-09-18 The device of cyclohexanol is recycled from cyclohexanol rectifying column kettle liquid

Family Applications After (1)

Application Number Title Priority Date Filing Date
CN201721194088.0U Expired - Fee Related CN207276528U (en) 2017-07-03 2017-09-18 The device of cyclohexanol is recycled from cyclohexanol rectifying column kettle liquid

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Also Published As

Publication number Publication date
CN207276528U (en) 2018-04-27

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Application publication date: 20170915