CN103254067A - Esterification production method of isopropyl acetate - Google Patents
Esterification production method of isopropyl acetate Download PDFInfo
- Publication number
- CN103254067A CN103254067A CN2013101545557A CN201310154555A CN103254067A CN 103254067 A CN103254067 A CN 103254067A CN 2013101545557 A CN2013101545557 A CN 2013101545557A CN 201310154555 A CN201310154555 A CN 201310154555A CN 103254067 A CN103254067 A CN 103254067A
- Authority
- CN
- China
- Prior art keywords
- tower
- esterification
- waste water
- column
- reaction
- 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.)
- Pending
Links
Images
Abstract
The invention discloses an esterification production method of isopropyl acetate, which can improve the yield and reduce the energy consumption in a production process. The esterification production method is a new technology which increases the temperature of esterification reaction, accelerates reaction, improves the yield and reduces the energy consumption by use of a pressurizing method. The method disclosed by the invention controls the pressure in an esterification tower and a rectifying tower through the flow of common nitrogen so as to increase the reaction rate and achieve the aims of improving yield and reducing energy consumption. Through continuous processes of reaction rectification, isopropyl acetate refining, wastewater recovery and the like, high-purity isopropyl acetate is conveniently and efficiently prepared. The esterification production method disclosed by the invention overcomes the shortcomings of lower reaction rate, lower yield and higher energy consumption due to normal-pressure reaction of a traditional method during production of isopropyl acetate.
Description
Technical field
The present invention relates to a kind of esterification production method of Iso Butyl Acetate, relate in particular to a kind of flow size of utilizing ordinary nitrogen and control the esterification production method that pressure in esterification column and the rectifying tower makes reaction rate accelerates, the esterification production method of this Iso Butyl Acetate can reach the raising productive rate, cut down the consumption of energy, reduce production cost greatly.
Background technology
Iso Butyl Acetate mainly reclaims manufacturing processedes such as dewatering agent, medicine, pesticide industry, high-grade printing ink, imitation leather, plastics, film, caking agent as paint solvent, acetic acid.Because the esterification of acetic acid and methyl alcohol is subjected to Equilibrium limit, the water that reaction generates can suppress the carrying out of esterification, influences the productive rate of esterification, and temperature of reaction also can influence the speed of reaction, has increased production cost.
The Iso Butyl Acetate content of being badly in need of is that the highly purified Iso Butyl Acetate more than 99% is to produce by the complicated technologies such as esterification extracting rectifying of acetic acid and Virahol at present, usually adopt synthesis under normal pressure, but adopt normal pressure band outlet capacity limited, speed of reaction is also slow, and production cost compares higher.The technology of production acetates is comparative maturity all, is difficult under the normal pressure cut down the consumption of energy and material consumption again.
Summary of the invention
Technical problem to be solved by this invention is the defective that overcomes prior art, and a kind of esterification production method of the Iso Butyl Acetate of can productivity gain, cutting down the consumption of energy is provided.When this esterification production method was intended to overcome the produced in conventional processes Iso Butyl Acetate, because synthesis under normal pressure, speed of reaction was slower, and productive rate is lower, the deficiency that energy consumption is higher.Esterification production method of the present invention improves the transformation efficiency of Iso Butyl Acetate, and output increases, and energy consumption reduces, and has also reduced production cost and reduced follow-up intractability when having solved traditional deficiency.
The technical solution adopted for the present invention to solve the technical problems is: a kind of esterification production method of Iso Butyl Acetate, and this esterification production method may further comprise the steps:
(1) reactive distillation: acetic acid and Virahol are entered the esterification column reaction by the esterification reboiler, and nitrogen enters from the cat head of esterification column, and the pressure of esterification reaction tower is 0.13-0.14MPa, and temperature of reaction is 106-110 ℃; The thick ester that esterification column reaction generates and water enter phase splitter from the cat head of esterification column and carry out layering, and layering goes out organic phase and water, and a part of organic phase reflux is to esterification column, and remaining organic phase enters treating tower, and water enters the waste water reclamation tower;
(2) Iso Butyl Acetate is refining: it is refining that the thick ester that comes out from the esterification column cat head enters treating tower, and nitrogen enters from the cat head for the treatment of tower, and the pressure for the treatment of tower is 0.16-0.17MPa, and temperature of reaction is 115-116 ℃; Product comes out to enter the product jar at the bottom of the tower for the treatment of tower, moisture and other impurity enter the waste water reclamation tower from the cat head for the treatment of tower;
(3) waste water reclamation: the waste water that esterification column and treating tower come out enters the waste water reclamation tower and carries out wastewater treatment; Entering esterification column again after Virahol and Iso Butyl Acetate are handled the back and raw material is mixed through the waste water reclamation tower recycles.
Esterification production method of the present invention is to control pressure in esterification column and the rectifying tower by the flow size of ordinary nitrogen, make reaction rate accelerates, azeotropic point raises, the band outlet capacity strengthens, thick ester quantity of reflux reduces, productive rate improves, and energy consumption reduces, and conveniently makes highly purified Iso Butyl Acetate efficiently.When this esterification production method had overcome the produced in conventional processes Iso Butyl Acetate, because synthesis under normal pressure, speed of reaction was slower, and productive rate is lower, the deficiency that energy consumption is higher.The pressure-controlling of esterification column of the present invention is at 0.13-0.14MPa, and temperature of reaction is all controlled at 106-110 ℃, and the pressure-controlling of rectifying tower is at 0.16-0.17kPa, temperature control is at 115-118 ℃, reduced by 15% with energy consumption under the condition, productive rate has improved 8%, greatly reduces production cost.
Further be designed to: in step (1), acetic acid and Virahol are delivered to the esterification reboiler by former material conveying pump, by entering the esterifying kettle reaction after the heating of esterification reboiler, enter the esterification column compressive reaction again; The thick ester that comes out from the esterification column cat head and water enter phase splitter after by the condensation of esterification column overhead condenser, and organic phase flows in the esterification column by the blowback of esterification column trim the top of column.
Further be designed to: in step (2), thick ester enter treating tower reduce pressure refining after, product comes out to heat through the treating tower reboiler at the bottom of the tower for the treatment of tower, enter the product jar by the product discharging pump again, the moisture that the treating tower reaction is produced, Virahol and Iso Butyl Acetate come out by the condensation for the treatment of tower overhead condenser from the cat head for the treatment of tower, enter the treating tower cat head after the condensation and be subjected to flow container, part Virahol and Iso Butyl Acetate flow in the treating tower by the blowback for the treatment of tower trim the top of column, and remaining Virahol and Iso Butyl Acetate enter the usefulness that an ester jar is made an ester.
Further be designed to: in step (3), waste water enters waste water column overhead accumulator after the cat head of waste water reclamation tower enters waste water column overhead condenser condenses, by waste water column overhead reflux pump a part of Virahol and Iso Butyl Acetate are delivered to the usefulness that an ester jar is made an ester then, remaining Virahol and Iso Butyl Acetate are back to the waste water reclamation tower; The waste water that comes out from the waste water reclamation tower bottom enters waste water tower reboiler heating back and delivers to purification tank for liquid waste esterification of the present invention by the waste water transferpump and carry out high-pressure tower, and the pressure in esterification column and the rectifying tower is to control by the flow size of ordinary nitrogen.
In sum, the esterification production method of Iso Butyl Acetate of the present invention is compared with the conventional production methods of prior art, has the following advantages and the high-lighting effect:
1. this esterification production method is that flow size by ordinary nitrogen guarantees pressure in esterification column and the rectifying tower and the pressure in the dehydration tower, accelerates speed of reaction, increases productive rate, cuts down the consumption of energy;
2. increase the pressure of esterification column, rising esterification column temperature, output improves 8%, and energy consumption obviously reduces by 5%;
3. increase the pressure of rectifying tower, compare same treatment amount energy consumption with normal pressure and reduce by 10%;
The technology of 4. producing method is easy, conveniently makes highly purified Iso Butyl Acetate efficiently, has reduced production cost greatly.
Description of drawings
Fig. 1 is the process flow diagram of the esterification production method of a kind of Iso Butyl Acetate of the present invention.
Wherein: P
1-former material conveying pump; R
1-reaction kettle of the esterification; E
1-esterification reboiler; T
1-esterification column; P
2-esterification column trim the top of column pump; E
2-esterification column overhead condenser; V
1-phase splitter; T
2-treating tower; P
3-product discharging pump; E
3-treating tower reboiler; P
4-treating tower trim the top of column pump; E
4-treating tower overhead condenser; V
2-treating tower cat head is subjected to flow container; T
2-waste water reclamation tower; P
5-waste water transferpump; E
5-waste water tower reboiler; P
6-waste water column overhead reflux pump; E
6-waste water column overhead condenser; V
3-waste water column overhead is subjected to flow container; V
4-ester jar.
Embodiment
Embodiment 1
The embodiment of the invention 1 described doing below in conjunction with the present invention of embodiment describes in further detail.
As shown in Figure 1, a kind of esterification production method of Iso Butyl Acetate, this esterification production method may further comprise the steps:
(1) reactive distillation: with acetic acid and Virahol in molar ratio 1:1.2 enter the esterification column reaction by the esterification reboiler, deliver to the esterification reboiler by former material conveying pump, by entering the esterifying kettle reaction after the heating of esterification reboiler, enter the esterification column compressive reaction again; Ordinary nitrogen enters from the cat head of esterification column, and the pressure of esterification reaction tower is 0.13-0.14MPa, and temperature of reaction is 106-110 ℃; The thick ester that comes out from the esterification column cat head and water enter phase splitter after by the condensation of esterification column overhead condenser, layering goes out organic phase and water, part organic phase flows to by the blowback of esterification column trim the top of column and is back to esterification column in the esterification column, remaining organic phase enters treating tower, and water enters the waste water reclamation tower.
(2) Iso Butyl Acetate is refining: the thick ester that comes out from the esterification column cat head enters treating tower and reduces pressure refiningly, and ordinary nitrogen enters from the cat head for the treatment of tower, and the pressure for the treatment of tower is 0.16-0.17MPa, and temperature of reaction is 115-116 ℃; Product comes out to heat through the treating tower reboiler at the bottom of the tower for the treatment of tower, enter the product jar by the product discharging pump again, moisture, Virahol and the Iso Butyl Acetate that the treating tower reaction is produced comes out by the condensation for the treatment of tower overhead condenser from the cat head for the treatment of tower, enter the treating tower cat head after the condensation and be subjected to flow container, part Virahol and Iso Butyl Acetate flow in the treating tower by the blowback for the treatment of tower trim the top of column, and remaining Virahol and Iso Butyl Acetate enter the usefulness that an ester jar is made an ester.
(3) waste water reclamation: waste water enters waste water column overhead accumulator after the cat head of waste water reclamation tower enters waste water column overhead condenser condenses, by waste water column overhead reflux pump a part of Virahol and Iso Butyl Acetate are delivered to the usefulness that an ester jar is made an ester then, an ester with enter esterification column again after raw material mixes and recycle; Remaining Virahol and Iso Butyl Acetate are back to the waste water reclamation tower; The waste water that comes out from the waste water reclamation tower bottom enters waste water tower reboiler heating back and delivers to purification tank for liquid waste by the waste water transferpump.
The esterification production method of present embodiment carries out in high-pressure tower, and the pressure in esterification column and the rectifying tower is to control by the flow size of ordinary nitrogen.
The above only is preferred embodiment of the present invention, is not technology contents of the present invention is done any pro forma restriction.Every foundation technical spirit of the present invention all still belongs in the scope of technical scheme of the present invention any simple modification, equivalent variations and modification that above embodiment does.
Claims (4)
1. the esterification production method of an Iso Butyl Acetate, it is characterized in that: this esterification production method may further comprise the steps:
(1) reactive distillation: acetic acid and Virahol are entered the esterification column reaction by the esterification reboiler, and nitrogen enters from the cat head of esterification column, and the pressure of esterification reaction tower is 0.13-0.14MPa, and temperature of reaction is 106-110 ℃; The thick ester that esterification column reaction generates and water enter phase splitter from the cat head of esterification column and carry out layering, and layering goes out organic phase and water, and a part of organic phase reflux is to esterification column, and remaining organic phase enters treating tower, and water enters the waste water reclamation tower;
(2) Iso Butyl Acetate is refining: it is refining that the thick ester that comes out from the esterification column cat head enters treating tower, and nitrogen enters from the cat head for the treatment of tower, and the pressure for the treatment of tower is 0.16-0.17MPa, and temperature of reaction is 115-116 ℃; Product comes out to enter the product jar at the bottom of the tower for the treatment of tower, moisture and other impurity enter the waste water reclamation tower from the cat head for the treatment of tower;
(3) waste water reclamation: the waste water that esterification column and treating tower come out enters the waste water reclamation tower and carries out wastewater treatment; Entering esterification column again after Virahol and Iso Butyl Acetate are handled the back and raw material is mixed through the waste water reclamation tower recycles.
2. according to the esterification production method of the described a kind of Iso Butyl Acetate of claim 1, it is characterized in that: in step (1), acetic acid and Virahol are delivered to the esterification reboiler by former material conveying pump, by entering the esterifying kettle reaction after the heating of esterification reboiler, enter the esterification column compressive reaction again; The thick ester that comes out from the esterification column cat head and water enter phase splitter after by the condensation of esterification column overhead condenser, and organic phase flows in the esterification column by the blowback of esterification column trim the top of column.
3. according to the esterification production method of the described a kind of Iso Butyl Acetate of claim 2, it is characterized in that: in step (2), thick ester enter treating tower reduce pressure refining after, product comes out to heat through the treating tower reboiler at the bottom of the tower for the treatment of tower, enter the product jar by the product discharging pump again, the moisture that the treating tower reaction is produced, Virahol and Iso Butyl Acetate come out by the condensation for the treatment of tower overhead condenser from the cat head for the treatment of tower, enter the treating tower cat head after the condensation and be subjected to flow container, part Virahol and Iso Butyl Acetate flow in the treating tower by the blowback for the treatment of tower trim the top of column, and remaining Virahol and Iso Butyl Acetate enter the usefulness that an ester jar is made an ester.
4. according to the esterification production method of any described a kind of Iso Butyl Acetate of claim 1-3, it is characterized in that: in step (3), waste water enters waste water column overhead accumulator after the cat head of waste water reclamation tower enters waste water column overhead condenser condenses, by waste water column overhead reflux pump a part of Virahol and Iso Butyl Acetate are delivered to the usefulness that an ester jar is made an ester then, remaining Virahol and Iso Butyl Acetate are back to the waste water reclamation tower; The waste water that comes out from the waste water reclamation tower bottom enters waste water tower reboiler heating back and delivers to purification tank for liquid waste by the waste water transferpump.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013101545557A CN103254067A (en) | 2013-04-28 | 2013-04-28 | Esterification production method of isopropyl acetate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013101545557A CN103254067A (en) | 2013-04-28 | 2013-04-28 | Esterification production method of isopropyl acetate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103254067A true CN103254067A (en) | 2013-08-21 |
Family
ID=48958341
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2013101545557A Pending CN103254067A (en) | 2013-04-28 | 2013-04-28 | Esterification production method of isopropyl acetate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103254067A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104557538A (en) * | 2014-12-04 | 2015-04-29 | 江门谦信化工发展有限公司 | Industrial production method for producing butyl acrylate by in-column reaction rectification |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1458917A (en) * | 2000-09-16 | 2003-11-26 | 人造丝化学欧洲有限公司 | Coupled production of two esters |
| CN101367724A (en) * | 2008-09-18 | 2009-02-18 | 中国石油大学(华东) | Method and apparatus for synthesis of isopropyl acetate |
| CN101735045A (en) * | 2009-12-18 | 2010-06-16 | 中山大学 | Method for producing ethyl acetate by using entrainer |
| CN101830799A (en) * | 2010-05-25 | 2010-09-15 | 张超 | Single-tower rectifying method for synthetizing ethyl acetate by esterification method |
| CN102001936A (en) * | 2009-09-01 | 2011-04-06 | 北京石油化工学院 | Continuous production method of propyl acetate |
| CN102690197A (en) * | 2012-05-29 | 2012-09-26 | 江门谦信化工发展有限公司 | Method for preparing acetic acid mixed butyl ester by continuous reaction and rectification |
| CN102753515A (en) * | 2010-02-04 | 2012-10-24 | 罗狄亚聚酰胺特殊品有限公司 | Method for preparing a carboxylic acid ester |
-
2013
- 2013-04-28 CN CN2013101545557A patent/CN103254067A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1458917A (en) * | 2000-09-16 | 2003-11-26 | 人造丝化学欧洲有限公司 | Coupled production of two esters |
| CN101367724A (en) * | 2008-09-18 | 2009-02-18 | 中国石油大学(华东) | Method and apparatus for synthesis of isopropyl acetate |
| CN102001936A (en) * | 2009-09-01 | 2011-04-06 | 北京石油化工学院 | Continuous production method of propyl acetate |
| CN101735045A (en) * | 2009-12-18 | 2010-06-16 | 中山大学 | Method for producing ethyl acetate by using entrainer |
| CN102753515A (en) * | 2010-02-04 | 2012-10-24 | 罗狄亚聚酰胺特殊品有限公司 | Method for preparing a carboxylic acid ester |
| CN101830799A (en) * | 2010-05-25 | 2010-09-15 | 张超 | Single-tower rectifying method for synthetizing ethyl acetate by esterification method |
| CN102690197A (en) * | 2012-05-29 | 2012-09-26 | 江门谦信化工发展有限公司 | Method for preparing acetic acid mixed butyl ester by continuous reaction and rectification |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104557538A (en) * | 2014-12-04 | 2015-04-29 | 江门谦信化工发展有限公司 | Industrial production method for producing butyl acrylate by in-column reaction rectification |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101830799B (en) | Single-tower rectifying method for synthetizing ethyl acetate by esterification method | |
| CN103951544B (en) | Method for separating ethyl acetate and ethanol azeotrope by differential pressure rectification | |
| CN104513159A (en) | Butyl acetate energy saving production method | |
| CN102451573B (en) | Acetic acid dehydrating tower rectifying method | |
| CN102557932B (en) | Method for producing isobutyl acetate | |
| CN106883121A (en) | The method that methyl formate hydrolysis prepares anhydrous formic acid | |
| CN102134191A (en) | Process method for producing ethyl acetate by catalytic rectification | |
| CN104557524A (en) | Production method of ethyl acetate | |
| CN203602526U (en) | Reactive distillation device for producing ethanol from methyl acetate by adding hydrogen | |
| CN103254067A (en) | Esterification production method of isopropyl acetate | |
| CN103772185B (en) | Device and method for removing moisture and heteroacids in acetic acid | |
| CN203639370U (en) | Continuous rectification system for m-toluic acid | |
| CN204897793U (en) | DOTP plasticizer esterification reaction device | |
| CN105111052A (en) | Method for purifying acetone from waste residue and waste water produced in ketene dimmer production process | |
| CN101596371B (en) | Device for purifying formic acid solution with interval azeotropic distillation and method thereof | |
| CN104649862A (en) | Method and equipment for producing ethanol product by taking ethyl acetate as raw material | |
| CN103588618A (en) | Reactive distillation method and device for producing ethanol from methyl acetate by adding hydrogen | |
| CN103373919A (en) | Method and equipment for separating and recycling alcoholysis waste liquid in polyvinyl alcohol production | |
| CN103254071A (en) | Butyl acrylate esterification and production technology | |
| CN106083586B (en) | Technological method for synthesizing ethyl formate by using formic acid and ethanol and purifying product | |
| CN102850374A (en) | Method for preparing jolkinolide B | |
| CN104803828A (en) | Device and method for improving 1,4-butanediol yield | |
| CN102126943B (en) | Recycling and separating process of heavy component residual liquid in carbonylation production process of acetic acid | |
| CN202131247U (en) | Device for purifying sec-butyl acetate from acetic acid mixture | |
| CN205170709U (en) | A device for improving 1, 4 - butanediol yield |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20130821 |