CN1151112C - Process for purifying 2-octanol and 2-octanone from organic mixture - Google Patents
Process for purifying 2-octanol and 2-octanone from organic mixtureInfo
- Publication number
- CN1151112C CN1151112C CNB00120744XA CN00120744A CN1151112C CN 1151112 C CN1151112 C CN 1151112C CN B00120744X A CNB00120744X A CN B00120744XA CN 00120744 A CN00120744 A CN 00120744A CN 1151112 C CN1151112 C CN 1151112C
- Authority
- CN
- China
- Prior art keywords
- methyln
- water
- sec
- hexyl ketone
- octyl alcohol
- 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.)
- Expired - Lifetime
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a method for purifying 2-octanol and 2-octanone from an organic mixture, which comprises the following steps that in a rectification tower, water or vapor is added to an organic mixture containing 2-octanol and 2-octanone, and a new mixture is heated to be boiling; then, water, 2-octanone and other light components are distilled from the top of the tower, distilled liquid is condensed and settled so that the distilled liquid is divided into a water phase and an organic phase, and an organic phase and kettle liquid at the top of the tower are collected. In the present invention, 2-octanol and 2-octanone, which have similar boiling points, are effectively separated, and the purity of 2-octanol and 2-octanone is more than 99 wt%.
Description
The present invention relates to the method for purification sec-n-octyl alcohol and methyln-hexyl ketone from organic mixture.
Sec-n-octyl alcohol is the colourless inflammable oily liquids that aromatic odour is arranged, the raw material that is used for nitric acid oxidation legal system caproic acid in a large number, also can be used for the raw material of the synthetic di-sec-octyl phthalate of phthalic anhydride esterification process, can be used for synthon oiliness improver, farm chemical emulgent and flotation agent etc. in addition.Methyln-hexyl ketone also is the raw material of nitric acid oxidation system caproic acid.Sec-n-octyl alcohol as industrial chemicals is the mixture that contains sec-n-octyl alcohol, methyln-hexyl ketone, amylalcohol, hexanol, enanthol, octane, 2-methyl octene, 6-octene-2-ketone, wherein sec-n-octyl alcohol content is about 90 ± 1%, methyln-hexyl ketone content is about 9 ± 1%, and the content of all the other light constituents is about 1 ± 0.5%.Because sec-n-octyl alcohol, methyln-hexyl ketone mainly prepare the raw material of caproic acid as nitric acid oxidation, purity is not had too high requirement, according to product standard, it is qualified that the purity of sec-n-octyl alcohol 〉=82% is.But the atrophy gradually of sour in recent years market, in order to develop premium quality product, the purification of methyln-hexyl ketone, sec-n-octyl alcohol becomes urgent problem.
The boiling point of sec-n-octyl alcohol and methyln-hexyl ketone is very approaching, differs about 5 ℃, therefore adopts traditional rectificating method to be difficult to its separation, purification.
Add the water distillation technique and application is all arranged in a plurality of fields.US 4985131 discloses a kind of method of handling the dregs of fat, it be with the moisture dregs of fat be heated to more than the boiling point of water, below the cracking temperature of hydrocarbons, moisture in the dregs of fat forms steam like this, can remove the light hydrocarbon material, and remaining material is recovered as burnt shape residue.
US 3979465 discloses the method for preparing low carbon fat alcohol, it is that C2-C4 alkene and sulfuric acid reaction are formed ester, the above-mentioned product of while thin up, distill out the C2-C4 Fatty Alcohol(C12-C14 and C12-C18) with water vapor from cat head then, and with the sulfuric acid evaporation and concentrating, after steam reclaims, be recycled to the front reactions steps and reuse.
Prior art thinks, for being easy to decompose when distilling with the immiscible material of water again, for reducing its boiling point, can adopt wet distillation, but in general, and wet distillation can not improve the dissolve each other separating effect of system of the approaching binary of boiling point.
The purpose of this invention is to provide the method for two kinds of purification sec-n-octyl alcohol and methyln-hexyl ketones from organic mixture, these two kinds method technology is simple, refining effect good.
First method (interrupter method) comprising:
In rectifying tower, with weight ratio is 0.01-2: 1 water is heated to boiling with the organic mixture that contains sec-n-octyl alcohol and methyln-hexyl ketone as still liquid, from cat head with 0.1-10: 1 reflux ratio distillates water, methyln-hexyl ketone and all the other light constituents, distillate is divided into water and organic phase through condensation, after leaving standstill, collect organic phase, when sec-n-octyl alcohol concentration reaches requirement in the still liquid, stop rectifying, collect still liquid.
Specifically, first method of the present invention is in conventional plate distillation column or stuffing rectification column, with weight ratio is 0.01-1: 1, preferred 0.05-1.5: 1 water is heated to boiling with the organic mixture that contains sec-n-octyl alcohol and methyln-hexyl ketone as still liquid, water, methyln-hexyl ketone and other light constituent are stripped to cat head, in reflux ratio is 0.1-10: 1, preferred 1-4: 1 condition bottom discharge, feed liquid leaves standstill after the overhead condenser condensation, water and organic phase layering, can return after the water preheating at the bottom of the still, organic phase is the cut that is rich in methyln-hexyl ketone, collects organic phase.When sec-n-octyl alcohol concentration reaches requirement in the still liquid, stop rectifying, collect still liquid.
If obtain highly purified methyln-hexyl ketone, after can earlier a small amount of light constituent being extracted, regather overhead fraction.
Second method (continuous processing) comprising:
The organic mixture that will contain sec-n-octyl alcohol and methyln-hexyl ketone is fed in the rectifying tower by feed points, at the bottom of tower, add water vapor, the weight ratio of water vapour and organic mixture is 0.05-4: 1, after the boiling of still liquid, from cat head with 0.3-15: 1 reflux ratio distillates water, methyln-hexyl ketone and all the other light constituents, distillate is divided into water and organic phase through condensation, after leaving standstill, and collects cat head organic phase and still liquid.
Specifically, second method of the present invention is in conventional plate distillation column or stuffing rectification column, the organic mixture that will contain sec-n-octyl alcohol and methyln-hexyl ketone is entered by the feed points of rectifying tower, at the bottom of tower, feed water vapor, the weight ratio of water vapour and organic mixture is 0.05-4: 1, preferred 0.1-2: 1, with the extremely boiling of still liquid direct heating, water, methyln-hexyl ketone and other light constituent vapour are put to cat head, are 0.3-15 in reflux ratio: 1, preferred 1-6: 1 condition bottom discharge, feed liquid leaves standstill after the overhead condenser condensation, water and organic phase layering, and water returns the water vapour boiler, organic phase is the cut that is rich in methyln-hexyl ketone, collects cat head organic phase and still liquid.
The feed points of said rectifying tower is meant sec-n-octyl alcohol and methyln-hexyl ketone concentration and the feeding liquid concentration consistent location in tower, and this position those of ordinary skills can be by calculating.
The temperature of said water vapor can be more than or equal to 100 ℃, and for the ease of operation and saving energy consumption, vapor temperature should not be too high, preferably is no more than 200 ℃.
The water yield that is added in the inventive method (steam vapour amount) should determine that as adding the water yield very little, then the effect of Ti Chuning is undesirable, does not reach required purity according to the content of methyln-hexyl ketone in the organic mixture; The water yield is too many, and then energy consumption increases, and production cost is risen.
Pressure suitable in the inventive method is between the 0.1-1.0MPa, for the ease of operation, and preferred 0.1-0.3MPa.
In the separating of methyln-hexyl ketone and sec-n-octyl alcohol, as not adding water, the weight ratio of methyln-hexyl ketone and sec-n-octyl alcohol is about 1: 1 in the overhead distillate, thereby is difficult to obtain purer methyln-hexyl ketone, and also purification has lost the sec-n-octyl alcohol in this mixture because of being difficult to further simultaneously.The present invention is by adding entry or water vapour in organic mixture, significantly improved the separation efficiency of methyln-hexyl ketone and sec-n-octyl alcohol, after particularly a small amount of light constituent being extracted, the weight ratio of methyln-hexyl ketone and sec-n-octyl alcohol can reach 99: 1 in the overhead distillate, and the content of methyln-hexyl ketone in the cat head organic phase can reach 99wt%.
In addition, the inventive method can play organism and stir and dissemination by add entry or water vapour when distilling, and reduces gelationus and produces.The inventive method also has characteristics such as technology is simple, pollution-free, cost is low, safe and reliable simultaneously.
Further specify the present invention below by embodiment, but the present invention is not limited to this.
Embodiment 1
Adopt the conventional rectification device, at column length 150cm, 3mm * 1mm stainless steel ring the filler of packing in the separator column of diameter 2.5cm, in still (there-necked flask), add 89 gram organic mixture (sec-n-octyl alcohols 90 ± 1%, methyln-hexyl ketone 9 ± 1%, hexanol, octane, 2-methyl octene etc. 1 ± 0.5%) and water, water and organic weight ratio 0.08: 1.Adorn a sampling valve in the still, still liquid continues to be warming up to about 180 ℃ after about 100 ℃ of boilings, when tower top temperature reaches about 98 ℃, with 2.5: 1 reflux ratio discharging, treat that light constituent is extracted after, regather the cut that is rich in methyln-hexyl ketone, remove a small amount of tailings.Overhead distillate is divided into water and organic phase after condenser condenses, monitor the content of sec-n-octyl alcohol in the still liquid at any time with sampling valve, stops rectifying when reaching 98.5wt%, treats to put to leaving standstill a jar layering after the still liquid cooling but, and upper organic phase is sec-n-octyl alcohol.Cat head is rich in that the weight ratio of methyln-hexyl ketone and sec-n-octyl alcohol is 99: 1 (methyln-hexyl ketone content is 99wt%) in the organic phase of methyln-hexyl ketone, and aqueous phase methyln-hexyl ketone content is 0.Production concentration detects with the gas chromatograph FID of capillary column OV-1.
Embodiment 2
The device that adopts is identical with example 1 with the Intake Quantity of organic mixture, water and organic liquor weight ratio 1: 1, and still liquid maintains this temperature after about 100 ℃ of boilings, and when tower top temperature reached about 98 ℃, with 4: 1 reflux ratio discharging, all the other were operated with example 1.Stop rectifying when sec-n-octyl alcohol content reaches 99.5wt% at the bottom of the still, cat head is rich in that the weight ratio of methyln-hexyl ketone and sec-n-octyl alcohol is 99: 1 in the organic phase of methyln-hexyl ketone.
Embodiment 3
Adopt the conventional rectification device, at column length 300cm, in the separator column of diameter 4.4cm, the 3mm that packs into * 3mm stainless steel ring filler, organic mixture is entered by the middle part of separator column, water vapor is entered in the tower by the bottom, and the weight ratio of water vapour and organic mixture is 0.8: 1, and steam temperature is slightly larger than 100 ℃, reflux ratio discharging with 2: 1, temperature is about 98 ℃ during the cat head discharging, and overhead distillate is divided into water and organic phase after condenser condenses, and water returns the water vapour boiler.Cat head is rich in that the weight ratio of methyln-hexyl ketone and sec-n-octyl alcohol is 98: 2 in the organic phase of methyln-hexyl ketone, and sec-n-octyl alcohol content is 99.3wt% at the bottom of the still.
Comparative example
Adopt the operation of example 1, different is not add entry, and temperature is about 170 ℃ during the cat head discharging, and after the condensation layering, the weight ratio of methyln-hexyl ketone and sec-n-octyl alcohol is 1.01: 1 in the cat head organic phase, and sec-n-octyl alcohol content is 95wt% at the bottom of the still.
Claims (7)
1. the method for purification sec-n-octyl alcohol and methyln-hexyl ketone from the mixture that contains sec-n-octyl alcohol and methyln-hexyl ketone, comprise: in rectifying tower, with weight ratio is 0.01-2: 1 water is heated to boiling with the mixture that contains sec-n-octyl alcohol and methyln-hexyl ketone as still liquid, from cat head with 0.1-10: 1 reflux ratio distillates water, methyln-hexyl ketone and all the other light constituents, distillate is divided into water and organic phase through condensation, after leaving standstill, collect organic phase, when sec-n-octyl alcohol concentration reaches requirement in the still liquid, stop rectifying, collect still liquid.
2. according to the said method of purification of claim 1, it is characterized in that water is 0.05-1.5 with the weight ratio that contains the mixture of sec-n-octyl alcohol and methyln-hexyl ketone: 1.
3. according to the said method of purification of claim 1, it is characterized in that reflux ratio is 1-4: 1.
4. the method for purification sec-n-octyl alcohol and methyln-hexyl ketone from the mixture that contains sec-n-octyl alcohol and methyln-hexyl ketone, comprise: the mixture that will contain sec-n-octyl alcohol and methyln-hexyl ketone is fed in the rectifying tower by feed points, at the bottom of tower, add water vapor, the weight ratio of water vapour and mixture is 0.05-4: 1, after the boiling of still liquid, from cat head with 0.3-15: 1 reflux ratio distillates water, methyln-hexyl ketone and all the other light constituents, and distillate is divided into water and organic phase through condensation, after leaving standstill, and collects cat head organic phase and still liquid.
5. according to the said method of purification of claim 4, it is characterized in that steam temperature is no more than 200 ℃.
6. according to the said method of purification of claim 4, it is characterized in that reflux ratio is 1-6: 1.
7. according to the said method of purification of claim 4, it is characterized in that the weight ratio of water vapour and mixture is 0.1-2: 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB00120744XA CN1151112C (en) | 2000-07-13 | 2000-07-13 | Process for purifying 2-octanol and 2-octanone from organic mixture |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB00120744XA CN1151112C (en) | 2000-07-13 | 2000-07-13 | Process for purifying 2-octanol and 2-octanone from organic mixture |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1334263A CN1334263A (en) | 2002-02-06 |
| CN1151112C true CN1151112C (en) | 2004-05-26 |
Family
ID=4588371
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB00120744XA Expired - Lifetime CN1151112C (en) | 2000-07-13 | 2000-07-13 | Process for purifying 2-octanol and 2-octanone from organic mixture |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1151112C (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR3029913B1 (en) * | 2014-12-16 | 2018-07-06 | Arkema France | 2-OCTANONE CUTTING PROCESS |
| CN109438186B (en) * | 2018-11-16 | 2021-08-17 | 安阳市景晟科技有限公司 | Industrial production method of high-purity sec-octanol |
-
2000
- 2000-07-13 CN CNB00120744XA patent/CN1151112C/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| CN1334263A (en) | 2002-02-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| TWI421121B (en) | Low-energy extractive distillation process for dehydration of aqueous ethanol | |
| US4366032A (en) | Process for producing dehydrated alcohols for use as component of a motor fuel composition | |
| US5811606A (en) | Process and equipment for treatment of waste plastics | |
| CN102675265B (en) | Method of refining furfural through six-tower continuous rectification | |
| KR20120039017A (en) | Recovery of butanol from a mixture of butanol, water and an organic extractant | |
| JP7168037B2 (en) | Method and apparatus for producing organic carboxylic acid aqueous solution | |
| JP2013511550A (en) | Recovery of butanol from a mixture of butanol, water, and organic extractant | |
| CA2314402C (en) | Process of recovering methyl ethyl ketone from an aqueous mixture of methyl ethyl ketone and ethanol | |
| CN203923057U (en) | Improved Butanol Recycling device | |
| KR100513187B1 (en) | Water Separation Process | |
| CN101074211A (en) | Process for treating high-purity pyridine solution | |
| CN1721380A (en) | Process for extracting 1-methylnaphthalene and 2-methylnaphthalene from tar | |
| CN1094482C (en) | Azeotropic distillation process | |
| CN1331070A (en) | Process for separating methylisobutanone synthesized from acetone | |
| CN1956928A (en) | Removal of propylene glycol and propylene glycol ethers from aqueous streams | |
| CN1151112C (en) | Process for purifying 2-octanol and 2-octanone from organic mixture | |
| FR2683523A1 (en) | PROCESS FOR SEPARATING ETHYL TERTIOBUTYL ETHER AND ETHANOL | |
| CN108358754B (en) | Process method and system for separating ethanol, ethyl acetate and water mixture | |
| CN1062294C (en) | Deacidifying process for petroleum cut fraction with amino-alcohol | |
| CN1306450A (en) | Process for treatment of waste water | |
| JP6916936B2 (en) | Methods and equipment for processing tall oil | |
| US4623432A (en) | Removal of brominated organics from acetic acid obtained by oxidation of liquid butane in presence of Co-Br or Co-Mn-Br system catalysis | |
| CN1304343C (en) | Method and device for separating 1,2,3-trimethylbenzene | |
| BR112021022064B1 (en) | METHOD FOR RECOVERING ONE OR MORE CHEMICALS | |
| CN109679679A (en) | A kind of heavy aromatics industrial process |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C06 | Publication | ||
| PB01 | Publication | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CX01 | Expiry of patent term | ||
| CX01 | Expiry of patent term |
Granted publication date: 20040526 |