CN108383687A - A kind of purification rectifying column and method of purification for 3- methyl-3-butene-1-alcohols - Google Patents
A kind of purification rectifying column and method of purification for 3- methyl-3-butene-1-alcohols Download PDFInfo
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- CN108383687A CN108383687A CN201810176513.6A CN201810176513A CN108383687A CN 108383687 A CN108383687 A CN 108383687A CN 201810176513 A CN201810176513 A CN 201810176513A CN 108383687 A CN108383687 A CN 108383687A
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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
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- 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
- C07C29/84—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation by extractive distillation
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of purification rectifying columns and method of purification being used for 3 methyl, 3 butylene, 1 alcohol, including rectifying column tower, the middle part of rectifying column tower has material inlet, in rectifying column tower solvent inlet is equipped with close to the position of tower top, solvent heater is connected with by pipeline on solvent inlet, the bottom of tower of rectifying column tower is equipped with bottom of tower pipeline, kettle liquid pump is connected on the pipeline of bottom of tower, the bottom of rectifying column tower is equipped with gas phase import, it is also associated with bottom of tower heater on the bottom of tower pipeline of rectifying column tower, one end of bottom of tower heater is connect with bottom of tower pipeline, the other end of bottom of tower heater is connect with gas phase import.The purifying column of the present invention using the above scheme is simple in structure；Above-mentioned method of purification is conducive to inhibit the autohemagglutination of 3 methyl, 3 butylene, 1 alcohol, is conducive to the decomposition penalty that long-term production reduces solvent；The intersolubility for being conducive to enhance separation system and solvent, improves the separative efficiency operated step by step, the yield of 3 methyl, 3 butylene, 1 alcohol is up to 99.99%.
Description
Technical field
The present invention relates to a kind of method of purification and device more particularly to a kind of purifications for 3- methyl-3-butene-1-alcohols
Rectifying column and method of purification.
Background technology
3- methyl-3-butene-1-alcohols are a kind of water reducer midbodies, can further be synthesized by hysomer again different
Pentenol（3-M2BOL）.In hysomer, part 3- first is also had in addition to mainly obtaining prenol
Base -3- butene-1-ols are converted into isoamyl alcohol.In order to obtain higher prenol yield, needed in production by 3- methyl -3- fourths
Alkene -1- alcohol is detached with isoamyl alcohol.Since the boiling point of 3- methyl-3-butene-1-alcohols and isoamyl alcohol is sufficiently close to, conventional point
It is all extremely difficult to ideal separating effect from means, exploitation is needed to efficiently separate method.
Detaching the conventional method of alkane and alkene mixture can use extraction fractional distillation, generally use ethylene glycol, dimethyl sub-
The intensive polar solvents such as sulfone, DMAC N,N' dimethyl acetamide are extractant.Such solvent and unsaturated bond interaction force are stronger, are dividing
From when be easier to be combined into rectifying column bottom with alkene and obtain high-purity alkane from tower top, in butadiene, isoprene
Deng separation field have been widely used.Since alkene enters rectifying column bottom with solvent, the temperature of bottom of tower is again often higher,
The problems such as yield declines, equipment blocks is be easy to cause for the unsaturated hydrocarbons of easy autohemagglutination, when using nitrogenous or sulfur-bearing molten
There is also the unfavorable factors such as solvent pyrolytic when agent.
Invention content
The technical problem to be solved by the present invention is in view of the deficiencies of the prior art, provide for 3- methyl-3-butene-1-alcohols
Purification rectifying column and method of purification, the purifying column it is simple in structure；The method of purification is conducive to inhibit 3- methyl -3- butene-1s -
The autohemagglutination of alcohol is conducive to the decomposition penalty that long-term production reduces solvent；The intersolubility for being conducive to enhance separation system and solvent, carries
The separative efficiency that height operates step by step.
The present invention uses following technical scheme：A kind of purification rectifying column for 3- methyl-3-butene-1-alcohols, including essence
Evaporating tower tower body, the middle part of rectifying column tower has a material inlet, and solvent inlet is equipped with close to the position of tower top in rectifying column tower,
Solvent heater is connected with by pipeline on solvent inlet, the bottom of tower of rectifying column tower is equipped with bottom of tower pipeline, connects on the pipeline of bottom of tower
It is connected to kettle liquid pump, the bottom of rectifying column tower is equipped with gas phase import, and being also associated with bottom of tower on the bottom of tower pipeline of rectifying column tower adds
One end of hot device, bottom of tower heater is connect with bottom of tower pipeline, and the other end of bottom of tower heater is connect with gas phase import, rectifying tower
There is phegma import, the top of tower of rectifying column tower to be sequentially connected with overhead condenser, return tank by pipeline at the top of body
And reflux pump, the liquid outlet of reflux pump are connected separately with products pot and phegma import by pipeline；Solvent inlet is 24 pieces of reasons
By plate, material inlet is 55 pieces of theoretical plates.
A method of 3- methyl-3-butene-1-alcohols are purified using above-mentioned purification rectifying column, are included the following steps：
A, rectifying column operates at reduced pressure conditions, by the raw material of 3- methyl-3-butene-1-alcohols and isoamyl alcohol and higher boiling fat alkane
Hydrocarbon solvent is added in extractive distillation column by material inlet and solvent inlet simultaneously respectively；
B, bottom liquid is gasified partially liq by bottom of tower heater, and obtained gas returns to tower from the gas phase import of bottom of tower
It is interior；
The gas of tower top is sent after overhead condenser is all condensed into liquid to return tank of top of the tower, then is pressed centainly by reflux pump
Partially liq is sent into from the phegma import of tower top in tower by reflux ratio；
Extra liquid is overhead product in return tank, and overhead product is high-purity 3- methyl-3-butene-1-alcohols, tower top production
Product are discharged out of tank to be sent to products pot, and remaining liquid is bottom product after the heating of bottom of tower, and bottom product is isoamyl alcohol and solvent
Mixture, bottom product through kettle liquid pump discharge after carry out later separation again.
It is further improved：
Higher boiling fat alkane is n-dodecane in step a, and fatty alcohol is n-octyl alcohol or n-nonyl alcohol, higher boiling fat alkane solvent
Feeding temperature be 110 DEG C.
It is further improved：
The feeding temperature of the raw material of the method and isoamyl alcohol of the methyl-3-butene-1-alcohol containing 3- is 30 DEG C in step a.
It is further improved：
Rectifying column operating pressure is -0.095-0.07MPa in step a.
It is further improved：
It is 3 that flow and the flow-rate ratio of raw material, which is added, in fat alkane solvent in step a:2.
It is further improved：
Reflux ratio is 15 in step b:1.
The purifying column of the present invention using the above scheme is simple in structure；Above-mentioned method of purification is conducive to inhibit 3- methyl -3- fourths
The autohemagglutination of alkene -1- alcohol is conducive to the decomposition penalty that long-term production reduces solvent；Be conducive to enhance dissolving each other for separation system and solvent
Property, the separative efficiency operated step by step is improved, the yield of 3- methyl-3-butene-1-alcohols is up to 99.99%.
Description of the drawings
Fig. 1 is the schematic diagram that rectifying column is purified in the present invention.
In figure, 1- solvents；2- solvent heaters；3- solvent inlets；4- raw materials；5- material inlets；6- overhead condensers；7-
Return tank；8- reflux pumps；9- phegma imports；10- overhead products；11- products pots；The bottoms of tower 12- heater；13- gas phase imports；
14- kettle liquids pump；15- bottom products；16- rectifying column towers.
Specific implementation mode
Embodiment, as shown in Figure 1, a kind of purification rectifying column for 3- methyl-3-butene-1-alcohols, including rectifying tower
Body 16, the middle part of rectifying column tower 16 have a material inlet 5, and solvent inlet is equipped with close to the position of tower top in rectifying column tower 16
3, solvent heater 2 is connected with by pipeline on solvent inlet 3, the bottom of tower of rectifying column tower 16 is equipped with bottom of tower pipeline, bottom of tower pipe
It is connected with kettle liquid pump 14 on road, the bottom of rectifying column tower 16 is equipped with gas phase import 13, on the bottom of tower pipeline of rectifying column tower 16
Be also associated with bottom of tower heater 12, one end of bottom of tower heater 12 is connect with bottom of tower pipeline, the other end of bottom of tower heater 12 with
Gas phase import 13 connects, and there is phegma import 9, the top of tower of rectifying column tower 16 to pass through pipeline at the top of rectifying column tower 16
It is sequentially connected with overhead condenser 6, return tank 7 and reflux pump 8, the liquid outlet of reflux pump 8 is connected separately with product by pipeline
Tank 11 and phegma import 9.
Solvent inlet 3 is 24 pieces of theoretical plates, and material inlet 5 is 55 pieces of theoretical plates.
When work, high boiling fat alkane or the fat alkane solvent 1 containing fatty alcohol are heated by solvent heater 2
It is added from solvent inlet 3 after to certain temperature, the raw material 4 containing 3- methyl-3-butene-1-alcohols and isoamyl alcohol is at a certain temperature
It is added from material inlet 5；Bottom liquid is gasified partially liq by bottom of tower heater 12, gas phase of the obtained gas from bottom of tower
Import 13 returns in tower；The gas of tower top is sent after overhead condenser 6 is all condensed into liquid to return tank of top of the tower 7, then is passed through
Partially liq is sent into from the phegma import 9 of tower top in tower by reflux pump 8 by certain reflux ratio, extra liquid in return tank 7
Body is overhead product 10（High-purity 3- methyl-3-butene-1-alcohols）Discharge is sent to products pot 11 out of tank, is remained after the heating of bottom of tower
Remaining liquid is bottom product 15（The mixture of isoamyl alcohol and solvent）Later separation is carried out again after 14 discharge of kettle liquid pump.
A method of 3- methyl-3-butene-1-alcohols are purified using above-mentioned purification rectifying column, are included the following steps：
1, rectifying column operates at reduced pressure conditions, by the raw material 4 of 3- methyl-3-butene-1-alcohols and isoamyl alcohol and higher boiling fat
Alkane solvent 1 is added in extractive distillation column by material inlet 5 and solvent inlet 3 simultaneously respectively.
2, bottom liquid is gasified partially liq by bottom of tower heater 12, gas phase import 13 of the obtained gas from bottom of tower
It returns in tower；
The gas of tower top is sent after overhead condenser 6 is all condensed into liquid to return tank of top of the tower 7, then presses one by reflux pump 8
Partially liq is sent into from the phegma import 9 of tower top in tower by fixed reflux ratio；
Extra liquid is overhead product 10 in return tank 7, and overhead product 10 is high-purity 3- methyl-3-butene-1-alcohols, tower
Top product 10 is discharged out of tank to be sent to products pot 11, and remaining liquid is bottom product 15 after the heating of bottom of tower, and bottom product 15 is
The mixture of isoamyl alcohol and solvent, bottom product 15 carry out later separation again after 14 discharge of kettle liquid pump.
Higher boiling fat alkane is n-dodecane in step 1, and fatty alcohol is n-octyl alcohol or n-nonyl alcohol, higher boiling fat alkane
The feeding temperature of solvent 1 is 110 DEG C.
The feeding temperature of the raw material 4 of methyl-3-butene-1-alcohol containing 3- and isoamyl alcohol is 30 DEG C in step 1；
Rectifying column operating pressure is -0.095 ~ -0.07MPa in step 1.
It is 3 that flow and the flow-rate ratio of raw material 4, which is added, in fat alkane solvent 1 in step 1:2.
Reflux ratio is 15 in step 2:1.
Claims (7)
1. a kind of purification rectifying column for 3- methyl-3-butene-1-alcohols, it is characterised in that：Including rectifying column tower（16）, essence
Evaporate tower tower body（16）Middle part have material inlet（5）, rectifying column tower（16）It is upper to be equipped with solvent inlet close to the position of tower top
（3）, solvent inlet（3）It is upper that solvent heater is connected with by pipeline（2）, rectifying column tower（16）Bottom of tower equipped with bottom of tower manage
Road is connected with kettle liquid pump on the pipeline of bottom of tower（14）, rectifying column tower（16）Bottom be equipped with gas phase import（13）, rectifying column tower
（16）Bottom of tower pipeline on be also associated with bottom of tower heater（12）, bottom of tower heater（12）One end connect with bottom of tower pipeline, tower
Bottom heater（12）The other end and gas phase import（13）Connection, rectifying column tower（16）Top have phegma import（9）,
Rectifying column tower（16）Top of tower overhead condenser has been sequentially connected with by pipeline（6）, return tank（7）And reflux pump（8）, return
Stream pump（8）Liquid outlet products pot is connected separately with by pipeline（11）And phegma import（9）；Solvent inlet（3）It is 24 pieces
Theoretical plate, material inlet（5）For 55 pieces of theoretical plates.
2. a kind of method purifying 3- methyl-3-butene-1-alcohols using above-mentioned purification rectifying column, it is characterised in that：Including as follows
Step：
A, rectifying column operates at reduced pressure conditions, by the raw material of 3- methyl-3-butene-1-alcohols and isoamyl alcohol（4）With higher boiling fat
Fat alkane solvent（1）Pass through material inlet respectively（5）And solvent inlet（3）It is added in extractive distillation column simultaneously；
B, bottom liquid passes through bottom of tower heater（12）Partially liq is gasified, gas phase import of the obtained gas from bottom of tower（13）
It returns in tower；
The gas of tower top is through overhead condenser（6）It is sent to return tank of top of the tower after being all condensed into liquid（7）, then pass through reflux pump
（8）By certain reflux ratio by partially liq from the phegma import of tower top（9）It is sent into tower；
Return tank（7）Interior extra liquid is overhead product（10）, overhead product（10）For high-purity 3- methyl -3- butylene -
1- alcohol, overhead product（10）It is discharged and is sent to products pot out of tank（11）, remaining liquid is bottom product after the heating of bottom of tower（15）,
Bottom product（15）For the mixture of isoamyl alcohol and solvent, bottom product（15）It is pumped through kettle liquid（14）Subsequently divided again after discharge
From.
3. the method for purification 3- methyl-3-butene-1-alcohols according to claim 2, it is characterised in that：
Higher boiling fat alkane is n-dodecane in step a, and fatty alcohol is n-octyl alcohol or n-nonyl alcohol, higher boiling fat alkane solvent
（1）Feeding temperature be 110 DEG C.
4. the method for purification 3- methyl-3-butene-1-alcohols according to claim 2, it is characterised in that：Contain 3- in step a
The method of methyl-3-butene-1-alcohol and the raw material of isoamyl alcohol（4）Feeding temperature be 30 DEG C.
5. the method for purification 3- methyl-3-butene-1-alcohols according to claim 2, it is characterised in that：
Rectifying column operating pressure is -0.095-0.07MPa in step a.
6. the method for purification 3- methyl-3-butene-1-alcohols according to claim 2, it is characterised in that：
Fat alkane solvent in step a（1）Flow and raw material is added（4）Flow-rate ratio be 3:2.
7. the method for purification 3- methyl-3-butene-1-alcohols according to claim 2, it is characterised in that：
Reflux ratio is 15 in step b:1.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810176513.6A CN108383687A (en) | 2018-03-03 | 2018-03-03 | A kind of purification rectifying column and method of purification for 3- methyl-3-butene-1-alcohols |
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|---|---|---|---|
| CN201810176513.6A CN108383687A (en) | 2018-03-03 | 2018-03-03 | A kind of purification rectifying column and method of purification for 3- methyl-3-butene-1-alcohols |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111377798A (en) * | 2018-12-31 | 2020-07-07 | 江苏苏博特新材料股份有限公司 | Purification equipment and process of 3-methyl-3-buten-1-ol |
-
2018
- 2018-03-03 CN CN201810176513.6A patent/CN108383687A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111377798A (en) * | 2018-12-31 | 2020-07-07 | 江苏苏博特新材料股份有限公司 | Purification equipment and process of 3-methyl-3-buten-1-ol |
| CN111377798B (en) * | 2018-12-31 | 2022-12-02 | 江苏苏博特新材料股份有限公司 | Purification equipment and process of 3-methyl-3-butene-1-ol |
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Application publication date: 20180810 |