CN109384648A - A kind of new method recycling octyl alconyl raffinate - Google Patents
A kind of new method recycling octyl alconyl raffinate Download PDFInfo
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- CN109384648A CN109384648A CN201710685424.XA CN201710685424A CN109384648A CN 109384648 A CN109384648 A CN 109384648A CN 201710685424 A CN201710685424 A CN 201710685424A CN 109384648 A CN109384648 A CN 109384648A
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- China
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- distillation column
- column
- butanol
- octanol
- rectifying column
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
- B01D3/146—Multiple effect distillation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
- C07C45/81—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C45/82—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention provides a kind of new methods for recycling octyl alconyl raffinate, and steps are as follows: first rectifying column (i.e. butyraldehyde tower) mainly separates butyraldehyde with butanol and dehydration.The product that Second distillation column tower top distillates is butanol, guarantees that the purity (mass fraction, similarly hereinafter) of butanol is greater than 98%；Third distillation column tower top distillates the C5-C7 component such as whole butyl butyrates；The product that 4th the top of the distillation column distillates is octanol and octenal, guarantees that the purity of octanol is greater than 98%.
Description
Technical field
Present invention is mainly applied to octyl alconyl manufacturing enterprises, and in particular to a kind of recycling octyl alconyl raffinate new method.
Background technique
In the device of China's oxo synthesis production octyl alconyl, due to process requirement, about several tons is discharged per hour and contains
There is the waste liquid of butyraldehyde, butanol, octanol and polymer etc., be commonly called as octyl alconyl raffinate, originally these waste liquids are burnt as boiler oil
Fall, but contains phosphide in waste liquid, it is harmful to boiler plant, it cannot utilize, if waste liquid is exhausted, it will cause serious rings
Border pollution, state's laws regulation also do not allow.Main component is water, n-butanol, isobutanol, butyraldehyde, isobutyl in butanol and octanol waste liquid
The substances such as aldehyde, octenal (EPA), octanol, and a small amount of light component, 2- ethyl hexanal (EHA), triphenyl phosphorus, triphenyl phosphorus oxygen.It is useless
N-butanol, isobutanol, octanol total amount are higher in liquid, if will cause the huge waste of resource directly as fuel.Octyl alconyl raffinate
Present in the impurity compositions such as water, light component, C5-C7 component, butyl butyrate tremendous influence is caused to recovery system.It seriously affects
Purity, coloration and the rate of recovery of recovery system product.Meanwhile containing a large amount of useful substances in octyl alconyl raffinate, if energy
It is carried out purification & isolation, separates the material of the high added values such as butyraldehyde, butanol, octanol, such as butyraldehyde, butanol, octanol, Ke Yibian
Waste be changed into values, creates considerable economic benefit, and a kind of recycling octyl alconyl raffinate production new technique just solves the problems, such as this.
Summary of the invention
To solve the above problems, process route is reasonable, energy consumption the present invention provides a kind of recycling octyl alconyl raffinate new method
Low, product purity is high.Operating flexibility is big, adapts to the variation requirement of butanol and octanol waste liquid flow and composition completely.Process is simple, can
It leans on, does not influence the operation and properties of product of butyl octanol unit.The organic matter rate of recovery is high, and economic benefit is obvious, and the investment payback time is short.
System automation degree is high, convenient operating maintenance, and operating cost is low.The main composition of my company's butanol and octanol waste liquid includes: just different
Butyraldehyde: 3-5%wt, positive isobutanol: 15-30%wt, octenal: 5-10%wt, octanol 15-25%wt, heavy constituent 15-30%
wt。
A kind of new method recycling octyl alconyl raffinate, which is characterized in that butanol and octanol waste liquid is subjected to product fractionation, fractionation is single
Member includes first rectifying column, Second distillation column, third distillation column, the 4th rectifying column, and raw material is through first rectifying column by butanol and fourth
Aldehyde separation, and moisture is removed, first rectifying column tower reactor component enters Second distillation column and fractionates out butanol, Second distillation column tower reactor group
Divide into third distillation column and fractionate out C5-C7, third distillation column tower reactor component enters the 4th rectifying column and fractionates out octanol and octene
Aldehyde；The heavy constituent that 4th rectifier bottoms come out enters cracking still cracking, which is intermittent catalytic pyrolysis, used to urge
Agent is cobalt series catalyst, and cracking temperature is 150-300 DEG C, and the light component cracked enters first rectifying column, separates again
Butanol, octanol and octenal therein.
Preferably, the purity for the butanol that Second distillation column fractionates out is greater than 98%.
What third distillation column was isolated is the component of the C5-C7 such as butyl butyrate, and the C5-C7's isolated is directly entered waste liquid
Tank.
Preferably, the purity of the 4th rectifying column fractionates out octanol and octenal is greater than 98%.
Preferably, the butanol and octanol waste liquid contains: positive isobutylaldehyde: 3-5wt%, positive isobutanol: 15-30wt%, octene
Aldehyde: 5-10wt%, octanol 15-25wt%, heavy constituent 15-30wt%.
The present invention also provides it is a kind of recycle octyl alconyl raffinate production system, including first rectifying column, Second distillation column,
Third distillation column, the 4th rectifying column, the first rectifying column, Second distillation column, third distillation column, the 4th rectifying column successively phase
Even, the 4th rectifying tower bottom discharge port is connected with the material inlet of cracking still, the gaseous phase outlet of cracking still and first rectifying column
Feed inlet is connected.
Beneficial effects of the present invention:
A, first rectifying column separates and recovers butyraldehyde；My Products composition butyraldehyde, isobutyraldehyde content are higher, this process route energy
It is directly separated out butyraldehyde, it can be directly for sale.
[heavy constituent that b, the 4th rectifier bottoms come out enters cracking still cracking；Content is up to 30% in heavy constituent, can be with
System is traveled further into, useful component is isolated, separation system is gone successively to and carries out further recycling separation, recycling is wherein
Useful component achievees the purpose that sufficiently to extract wherein butyraldehyde and octenal, octanol.
C, octanol and octenal do not have to separation at the top of the 4th rectifying column, and the purity isolated is higher, reaches 98%, mixture
Both it can be directly entered the hydrogenation system of butyl octanol unit, can also have been sold directly as product, flexibility ratio is higher.
Detailed description of the invention
The flow sheet of Fig. 1 recycling octyl alconyl raffinate
Specific embodiment
Embodiment 1
Butanol and octanol waste liquid raw material is heated to 60 DEG C and enters first rectifying column by middle part, and the heat of material evaporation is mentioned by tower reactor reboiler
For.Entrainment reagent toluene is added from first block of column plate, flow 2Kg/h, and temperature of charge is 40 DEG C.First rectifying column overhead extraction object
For material after decanter is layered, supernatant liquid is recycled back into first rectifying column.Tower top temperature is controlled at 70 DEG C, by circulating liquid stream
Amount control.Bottom temperature is controlled at 120 DEG C, by tower reactor heating quantity of steam control.
First rectifying column tower top pressure is 0.02Mpa~-0.06Mpa, and tower top temperature is 60~110 DEG C, and bottom temperature is
100 DEG C~180 DEG C
First rectifying column tower bottoms is sent into feed inlet in the middle part of Second distillation column, Second distillation column tower top pressure through kettle liquid extraction pump 1
For -0.06Mpa~-0.2Mpa, tower top temperature is 50~120 DEG C, and bottom temperature is 110~180 DEG C
Second distillation column tower bottoms is sent into feed inlet in the middle part of third distillation column, third distillation column tower top pressure through kettle liquid extraction pump 2
For -0.02Mpa~-0.1Mpa, tower top temperature is 50~130 DEG C, and bottom temperature is 110~-180 DEG C
Third distillation column tower bottoms is sent into feed inlet in the middle part of the 4th rectifying column, the 4th rectifying tower pressure on top surface through kettle liquid extraction pump 3
For -0.08Mpa~-0.1Mpa, tower top temperature is 120~160 DEG C, and bottom temperature is 100~180 DEG C
Butanol purity > 99%, the rate of recovery > 90% are obtained from Second distillation column tower top；The octanol purity that 4th rectifying tower top obtains >
99%, the rate of recovery > 95%.
The heavy constituent come out from the 4th rectifier bottoms enters cracking still cracking, and cracking temperature is returned at 150-300 degrees Celsius
Yield >=60%, the light component cracked enter raffinate separation and recovery system, separate butanol, octanol and octene therein again
Aldehyde.
Embodiment 2
Butanol and octanol waste liquid raw material is heated to 90 DEG C and enters first rectifying column by middle part, and the heat of material evaporation is mentioned by tower reactor reboiler
For.Entrainment reagent benzene is added from first block of column plate, flow 2Kg/h, and temperature of charge is 40 DEG C.First rectifying column overhead extraction material
After decanter is layered, supernatant liquid is recycled back into first rectifying column.Tower top temperature is controlled at 100 DEG C, by circulating liquid stream
Amount control.Bottom temperature is controlled at 150 DEG C, by tower reactor heating quantity of steam control.Tower top pressure is -0.08MPa.
First rectifying column tower bottoms is sent into feed inlet in the middle part of Second distillation column through kettle liquid extraction pump 1, and tower top temperature control exists
90 DEG C, at 150 DEG C, tower top pressure is -0.08MPa for bottom temperature control.
Second distillation column tower bottoms is sent into feed inlet in the middle part of third distillation column through kettle liquid extraction pump 2, and tower top temperature control exists
100 DEG C, at 150 DEG C, tower top pressure is -0.09MPa for bottom temperature control.
Third distillation column tower bottoms is sent into feed inlet in the middle part of the 4th rectifying column through kettle liquid extraction pump 3, and tower top temperature control exists
140 DEG C, at 170 DEG C, tower top pressure is -0.09MPa for bottom temperature control.
Butanol purity > 99%, the rate of recovery > 90% are obtained from Second distillation column tower top；The octanol that 4th rectifying tower top obtains
Purity > 99%, the rate of recovery > 95%.
The heavy constituent come out from the 4th rectifier bottoms enters cracking still cracking, and cracking temperature is returned at 150-300 degrees Celsius
Yield >=62%, the light component cracked enter raffinate separation and recovery system, separate butanol, octanol and octene therein again
Aldehyde.
Embodiment 3
Butanol and octanol waste liquid raw material is heated to 100 DEG C and enters first rectifying column by middle part, and the heat of material evaporation is by tower reactor reboiler
It provides.Entrainment reagent benzene is added from first block of column plate, flow 0.5Kg/h, and temperature of charge is 40 DEG C.First rectifying column overhead extraction
For material after decanter is layered, supernatant liquid is recycled back into first rectifying column.Tower top temperature is controlled at 50 DEG C, by circulating liquid
Flow control.Bottom temperature is controlled at 130 DEG C, by tower reactor heating quantity of steam control.Tower top pressure is -0.01MPa.
First rectifying column tower bottoms is sent into feed inlet in the middle part of Second distillation column through kettle liquid extraction pump 1, and tower top temperature control exists
60 DEG C, at 120 DEG C, tower top pressure is -0.01MPa for bottom temperature control.
Second distillation column tower bottoms is sent into feed inlet in the middle part of third distillation column through kettle liquid extraction pump 2, and tower top temperature control exists
70 DEG C, at 130 DEG C, tower top pressure is -0.02MPa for bottom temperature control.
Third distillation column tower bottoms is sent into feed inlet in the middle part of the 4th rectifying column through kettle liquid extraction pump 3, and tower top temperature control exists
110 DEG C, at 140 DEG C, tower top pressure is -0.04MPa for bottom temperature control.
Butanol purity > 99%, the rate of recovery > 95% are obtained from Second distillation column tower top；The octanol that 4th rectifying tower top obtains
Purity > 99%, the rate of recovery > 96%
The heavy constituent come out from the 4th rectifier bottoms enters cracking still cracking, and cracking temperature is at 150-300 degrees Celsius, the rate of recovery
>=61%, the light component cracked enters raffinate separation and recovery system, separates butanol, octanol and octenal therein again.
Although above-mentioned in conjunction with specific embodiments of the present invention have been described, not to the scope of the present invention
Limitation, those skilled in the art should understand that, based on the technical solutions of the present invention, those skilled in the art do not need
Make the creative labor the various modifications or changes that can be made still within protection scope of the present invention.
Claims (6)
1. a kind of new method for recycling octyl alconyl raffinate, which is characterized in that butanol and octanol waste liquid is carried out product fractionation, separation and recovery
Unit includes first rectifying column, Second distillation column, third distillation column, the 4th rectifying column, raw material through first rectifying column by butanol with
Butyraldehyde separation, and moisture is removed, first rectifying column tower reactor component enters Second distillation column and fractionates out butanol, Second distillation column tower reactor
Component enters third distillation column and fractionates out C5-C7, third divide tower bottom of rectifying tower component enter the 4th rectifying column fractionate out octanol and
Octenal；The heavy constituent come out from the 4th rectifier bottoms enters cracking still cracking, and cracking temperature is cracked at 150-300 DEG C
To light component enter first rectifying column, separate butanol, octanol and octenal therein again.
2. the method as described in claim 1, which is characterized in that the purity for the butanol that Second distillation column fractionates out is greater than 98%.
3. the method as described in claim 1, which is characterized in that the purity for the octanol that the 4th rectifying column fractionates out is greater than 98%.
4. the method as described in claim 1, which is characterized in that the butanol and octanol waste liquid contains: positive isobutylaldehyde: 3-5wt%, just
Isobutanol: 15-30wt%, octenal: 5-10wt%, octanol 15-25wt%, heavy constituent 15-30wt%.
5. the method as described in claim 1, which is characterized in that the cracking reaction is intermittent catalytic pyrolysis, using cobalt system
Catalyst, cracking temperature are 150-300 DEG C.
6. it is a kind of recycle octyl alconyl raffinate separation and recovery system, including first rectifying column, Second distillation column, third distillation column,
4th rectifying column, which is characterized in that the first rectifying column, Second distillation column, third distillation column, the 4th rectifying column successively phase
Even, the 4th rectifying tower bottom discharge port is connected with the material inlet of cracking still, the gaseous phase outlet of cracking still and first rectifying column
Feed inlet is connected.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710685424.XA CN109384648A (en) | 2017-08-11 | 2017-08-11 | A kind of new method recycling octyl alconyl raffinate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710685424.XA CN109384648A (en) | 2017-08-11 | 2017-08-11 | A kind of new method recycling octyl alconyl raffinate |
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| Publication Number | Publication Date |
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| CN109384648A true CN109384648A (en) | 2019-02-26 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201710685424.XA Pending CN109384648A (en) | 2017-08-11 | 2017-08-11 | A kind of new method recycling octyl alconyl raffinate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111393261A (en) * | 2020-04-20 | 2020-07-10 | 聊城鲁西多元醇新材料科技有限公司 | System and method for recycling butanol and octanol residual liquid |
-
2017
- 2017-08-11 CN CN201710685424.XA patent/CN109384648A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111393261A (en) * | 2020-04-20 | 2020-07-10 | 聊城鲁西多元醇新材料科技有限公司 | System and method for recycling butanol and octanol residual liquid |
| CN111393261B (en) * | 2020-04-20 | 2023-08-01 | 聊城鲁西多元醇新材料科技有限公司 | System and method for recycling residual liquid of butyl alcohol and octyl alcohol |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20190226 |
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| WD01 | Invention patent application deemed withdrawn after publication |