CN100412051C - Heat pump rectifying prodn. process and plant for n-butyl acetate - Google Patents
Heat pump rectifying prodn. process and plant for n-butyl acetate Download PDFInfo
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- CN100412051C CN100412051C CNB2006100339355A CN200610033935A CN100412051C CN 100412051 C CN100412051 C CN 100412051C CN B2006100339355 A CNB2006100339355 A CN B2006100339355A CN 200610033935 A CN200610033935 A CN 200610033935A CN 100412051 C CN100412051 C CN 100412051C
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Abstract
The present invention discloses a method for producing butyl acetate by heat pump distillation, which comprises the following steps: esterifying raw materials in an esterification tank and an esterification tower; then, rectifying the raw materials in a rectifying tower to obtain the butyl acetate. The method is characterized in that the method also comprises the step: compressing mixed gas from the top of the esterification tower and mixed gas from the top of the rectifying tower as a heat source to exchange heat with the raw materials, the esterification tank and reboilers at tower bottoms. A device used by the method comprises the esterification tower, the esterification reboiler, the esterification tank, the rectifying tower, the rectifying reboiler, a cooling device, a phase separator and a modulation valve, wherein the esterification tank is connected with the esterification reboiler and the esterification tower; the rectifying tower is connected with the rectifying reboiler. The device is characterized in that the device also comprises two sets of heat pumps. The method can save heating steam and cooling water in the production of the butyl acetate, so the energy efficiency in the process is greatly enhanced, and the energy consumption for rectifying the butyl acetate is reduced by 56.9%. The method is suitable for the production field of the butyl acetate.
Description
Technical field
The present invention relates to a kind of production method of N-BUTYL ACETATE, particularly a kind of heat pump distillation production method of N-BUTYL ACETATE.
The invention still further relates to the device that a kind of aforesaid method uses.
Background technology
N-BUTYL ACETATE is a kind of good organic solvent, is widely used in industries such as coating, spices, process hides, pharmacy.In recent years, replace aliphatic ketone and aromatic solvents such as benzene, toluene and dimethylbenzene such as methylethylketone and methyl iso-butyl ketone (MIBK) gradually along with acetates, the demand of N-BUTYL ACETATE increases substantially both at home and abroad.
The method for preparing N-BUTYL ACETATE mainly contains neodymium sesquioxide catalysis synthesis process, DH type catalyst synthesis method and adopts sulfuric acid catalyst esterification process etc.At present, what domestic industry production N-BUTYL ACETATE generally adopted is traditional sulfuric acid catalysis esterification process, and this method is because of unit processes such as main employing reactive distillations, and energy consumption, material consumption are higher relatively.In Chemical Manufacture, rectifying is the bigger unit process of energy consumption normally, and its power consumption accounts for 40% of total energy consumption.Therefore, improving servant's efficient of rectifying, reduce the process energy consumption, is that N-BUTYL ACETATE is produced energy-conservation important channel.
Heat pump distillation has been widely used in the various chemical processs as a kind of power-saving technology that can effectively improve rectified heat efficient.As in the separation and alcohol production of systems such as Trimethylmethane/normal butane, propane/propylene, ethane/ethylene, exist the example that successfully uses heat pump techniques in a large number, use is the result show, the heat pump distillation technology can greatly reduce the production process energy consumption, obtains remarkable economic efficiency.
Summary of the invention
The present invention has overcome the deficiencies in the prior art, and a kind of heat pump distillation production method of N-BUTYL ACETATE is provided, and this method is simple in structure, and is energy-efficient, safe and reliable.
The device that another object of the present invention is to provide a kind of aforesaid method to use.
The heat pump distillation production method of N-BUTYL ACETATE of the present invention, comprise that raw acetic acid, butyl ester are through esterifying kettle, esterification column esterification after, rectifying makes through rectifying tower, it is characterized in that also comprising:
With the compressed overheated gas that becomes of the gas mixture of esterification column cat head as thermal source and raw material and esterifying kettle heat exchange, gas mixture dependence after the heat exchange self pressure returns the high position at cat head place, phase-splitting obtains thick ester and water after cooling off, the thick ester of part, water are back to esterification column, and all the other thick esters enter rectifying tower; With
The compressed overheated gas that becomes of the gas mixture of rectifying tower cat head as thermal source and bottom reboiler heat exchange, is obtained phlegma and is back to rectifying tower through further cooling off the rear section after the heat exchange, rest part is delivered to feed end as raw material.
Described gas mixture from the esterification column cat head is the N-BUTYL ACETATE that contains 60～64% weight, the butanols of 8～12% weight and the water of 26～30% weight, pressure is the mixed gas of 91～93 ℃ of 0.103MPa, temperature, described mixed gas after compression, its pressure is 0.309MPa, and temperature is 154 ℃.
Described gas mixture from the rectifying tower cat head is the N-BUTYL ACETATE that contains 39% weight, the butanols of 49% weight and the water of 12% weight, pressure is the mixed gas of 114 ℃ of 0.103Mpa, temperature, described mixed gas after compression, its pressure is 0.515Mpa, temperature is 180 ℃.
A kind of device of realizing the heat pump distillation production method use of N-BUTYL ACETATE disclosed by the invention, comprise esterification column, the esterification reboiler, esterifying kettle, rectifying tower, the rectifying reboiler, water cooler, phase splitter, variable valve, two cover heat pumps, wherein: esterification reboiler one end is a feed end, the other end is connected with the esterifying kettle feed end by pipeline, the discharge end of esterifying kettle is connected with the esterification column feed end by pipeline, the bottom of esterification column is connected by the feed end of pipeline with the esterification reboiler, the top of esterification column is connected with an end of phase splitter by pipeline, the other end of phase splitter is by pipe connection rectifying tower feed end, the rectifying tower bottom by pipeline respectively with the entrance end of rectifying reboiler, pan tank connects, the exit end of rectifying reboiler is connected with the rectifying tower bottom by pipeline, the top of rectifying tower is connected with an end of phase splitter by pipeline, the other end of phase splitter is by the feed end of pipe connection esterification reboiler, one end of one cover heat pump links to each other with the esterification column tower top outlet by pipeline, the other end is connected with the gas inlet end of esterifying kettle and the gas inlet end of esterification reboiler respectively by two variable valve, the gas outlet end of the gas outlet end of esterifying kettle and esterification reboiler is connected with water cooler one end by pipeline, the other end of water cooler connects phase splitter, one end of another set of heat pump links to each other with the rectifying tower tower top outlet by pipeline, the other end is connected with the gas inlet end of rectifying reboiler, the gas outlet end of rectifying reboiler is connected with water cooler one end by pipeline, and the other end of water cooler connects phase splitter.
The present invention is on the basis of conventional rectification N-BUTYL ACETATE production equipment, set up two cover compression heat pumps, save overhead condenser, equipment such as compressor, esterification column, rectifying tower, bottom reboiler, reactor are combined the circulation technology flow process of formation, by consuming a spot of electric energy, condenser heat-obtaining from the lower temperature position is used for the heat supply of reboiler and reactor, reaches energy saving purposes.
The present invention compared with prior art has following advantage:
(1) the present invention compares technology and the operating parameters that does not change former esterification column and rectifying tower with old process, but the present invention is by heating up cat head gas phase azeotrope through the heat pump compression, after heat release condensation at the bottom of the tower, utilize self pressure to return the cat head phase splitter, by the low warm upgrading utilization of cat head, can save heating steam and water coolant, greatly improve the energy consumption efficiency of process.
(2) method of the present invention need not change the process operation parameter of former esterification column, rectifying tower, is suitable for the reducing energy consumption of existing conventional N-BUTYL ACETATE production equipment.
(3) remarkable in economical benefits of the present invention, can reduce the production process energy consumption significantly, compare with the common process flow process, heat pump distillation new technological flow energy consumption descends 56.9%, the facility investment expense increases by 14.5%, by producing 2.5 ten thousand tons of N-BUTYL ACETATE production equipments per year, can save 3,540,000 yuan of process costs every year.
Description of drawings
Fig. 1 is an apparatus structure synoptic diagram of the present invention.
Embodiment
As shown in Figure 1, one end of esterification reboiler 1 is a feed end, the other end is connected with esterifying kettle 2 feed ends by pipeline, the discharge end of esterifying kettle 2 is connected with esterification column 3 feed ends by pipeline, the bottom of esterification column 3 is connected by the feed end of pipeline with esterification reboiler 1, the top of esterification column 3 is connected with an end of phase splitter 6 by pipeline, the other end of phase splitter 6 is by pipe connection rectifying tower 7 feed ends, one end of heat pump 4 links to each other with esterification column 3 tower top outlets by pipeline, the other end is by two variable valve 12,13 are connected with the gas inlet end of esterifying kettle 2 and the gas inlet end of esterification reboiler 1 respectively, the gas outlet end of the gas outlet end of esterifying kettle 2 and esterification reboiler 1 is connected with water cooler 5 one ends by pipeline, the other end of water cooler 5 connects phase splitter 6, rectifying tower 7 bottoms by pipeline respectively with the entrance end of rectifying reboiler 8, pan tank connects, the exit end of rectifying reboiler 8 is connected with rectifying tower 7 bottoms by pipeline, the top of rectifying tower 7 is connected with an end of phase splitter 11 by pipeline, the other end of phase splitter 11 is by the feed end of pipe connection esterification reboiler 8, one end of heat pump 9 links to each other with rectifying tower 7 tower top outlets by pipeline, the other end is connected with the gas inlet end of rectifying reboiler 8, the gas outlet end of rectifying reboiler 8 is connected with water cooler 10 1 ends by pipeline, and the other end of water cooler 10 connects phase splitter 11 and constitutes.
Gas mixture from the rectifying tower cat head is made up of the N-BUTYL ACETATE of 39% weight, the butanols of 49% weight and the water of 12% weight, and pressure is 114 ℃ of 0.103Mpa, temperature, described mixed gas after compression, its pressure is 0.515Mpa, temperature is 180 ℃.
Compare with common process, 1 ton of N-BUTYL ACETATE of every production can the energy efficient expense 141.6 yuan, and concrete energy consumption of saving is as shown in table 1.
Table 1
Wherein: steam is with 110 yuan/t, and electricity is with 0.6 yuan/kWh, and water calculates with 0.8 yuan/t.
Gas mixture from the rectifying tower cat head is made up of the N-BUTYL ACETATE of 39% weight, the butanols of 49% weight and the water of 12% weight, and pressure is 114 ℃ of 0.103Mpa, temperature, described mixed gas after compression, its pressure is 0.515Mpa, temperature is 180 ℃.
Compare and increase by two to overlap heat pumps with common process, saved steam boiler system, cooling water recirculation system and two overhead condensers simultaneously.Because as working medium, the bottom reboiler overall heat transfer coefficient is low than water vapor with the azeotrope mixed gas, so the heat interchanging area of tower bottom reboiler will suitably increase, and perhaps adopts the enhancement of heat transfer technology.Facility investment of the present invention improves benefit such as table 2.
Table 2
N-BUTYL ACETATE device for 1,100 ten thousand yuan of gross investments, 2.5 ten thousand tons of annual outputs, heat pump technology is compared with common process, facility investment increases about 1,590,000 yuan, account for 14.5% of equipment gross investment, but the heat pump distillation flow process can be saved about 3,540,000 yuan of device process cost such as energy consumption every year, and the simple payback period that heat pump flowsheet is transformed is usually less than 1 year.
Claims (4)
1. the heat pump distillation production method of a N-BUTYL ACETATE, comprise that raw material is through esterifying kettle, esterification column esterification after, rectifying makes through rectifying tower, it is characterized in that also comprising:
With the compressed overheated gas that becomes of the gas mixture of esterification column cat head as thermal source and raw material and esterifying kettle heat exchange, gas mixture dependence after the heat exchange self pressure returns the high position at cat head place, phase-splitting obtains thick ester and water after cooling off, the thick ester of part, water are back to esterification column, and all the other thick esters enter rectifying tower; With
The compressed overheated gas that becomes of the gas mixture of rectifying tower cat head as thermal source and tower bottom reboiler heat exchange, is obtained phlegma and is back to rectifying tower through further cooling off the rear section after the heat exchange, rest part is delivered to feed end as raw material.
2. method according to claim 1, it is characterized in that described gas mixture from the esterification column cat head is made up of the N-BUTYL ACETATE of 60～64% weight, the butanols of 8～12% weight and the water of 26～30% weight, its pressure is 91～93 ℃ of 0.103MPa, temperature, described mixed gas after compression, its pressure is 0.309MPa, and temperature is 154 ℃.
3. method according to claim 1, it is characterized in that described gas mixture from the rectifying tower cat head is made up of the N-BUTYL ACETATE of 39% weight, the butanols of 49% weight and the water of 12% weight, pressure is 114 ℃ of 0.103Mpa, temperature, described mixed gas after compression, its pressure is 0.515Mpa, and temperature is 180 ℃.
4. device of realizing the described method of one of claim 1～3, comprise esterification column, the esterification reboiler, esterifying kettle, rectifying tower, the rectifying reboiler, water cooler, phase splitter, variable valve, esterification reboiler one end is a feed end, the other end is connected with the esterifying kettle feed end by pipeline, the discharge end of esterifying kettle is connected with the esterification column feed end by pipeline, the bottom of esterification column is connected by the feed end of pipeline with the esterification reboiler, the top of esterification column is connected with an end of phase splitter by pipeline, the other end of phase splitter is by pipe connection rectifying tower feed end, the rectifying tower bottom by pipeline respectively with the entrance end of rectifying reboiler, pan tank connects, the exit end of rectifying reboiler is connected with the rectifying tower bottom by pipeline, the top of rectifying tower is connected with an end of phase splitter by pipeline, the other end of phase splitter is by the feed end of pipe connection esterification reboiler, it is characterized in that also comprising two cover heat pumps, wherein:
One end of one cover heat pump links to each other with the esterification column tower top outlet by pipeline, the other end is connected with the gas inlet end of esterifying kettle and the gas inlet end of esterification reboiler respectively by two variable valve, the gas outlet end of the gas outlet end of esterifying kettle and esterification reboiler is connected with water cooler one end by pipeline, the other end of water cooler connect phase splitter and
One end of another set of heat pump links to each other with the rectifying tower tower top outlet by pipeline, and the other end is connected with the gas inlet end of rectifying reboiler, and the gas outlet end of rectifying reboiler is connected with water cooler one end by pipeline, and the other end of water cooler connects phase splitter.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100339355A CN100412051C (en) | 2006-02-28 | 2006-02-28 | Heat pump rectifying prodn. process and plant for n-butyl acetate |
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| CNB2006100339355A CN100412051C (en) | 2006-02-28 | 2006-02-28 | Heat pump rectifying prodn. process and plant for n-butyl acetate |
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| CN1834082A CN1834082A (en) | 2006-09-20 |
| CN100412051C true CN100412051C (en) | 2008-08-20 |
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| CNB2006100339355A Expired - Fee Related CN100412051C (en) | 2006-02-28 | 2006-02-28 | Heat pump rectifying prodn. process and plant for n-butyl acetate |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102350076B (en) * | 2011-08-03 | 2013-09-04 | 江门谦信化工发展有限公司 | Energy saving reforming system of rectifying tower in production of ethyl acetate |
| CN103239876B (en) * | 2012-02-07 | 2015-04-29 | 中国石油天然气股份有限公司 | Method for avoiding operation and control of reboiler in unstable transition boiling zone |
| CN104086363B (en) * | 2014-07-14 | 2015-12-30 | 河北工业大学 | The energy-saving reclaiming process of N-BUTYL ACETATE and butanols in waste acid water |
| CN104130101B (en) * | 2014-07-29 | 2016-01-20 | 河北工业大学 | Azeotropic distillation and conventional distillation combine the technique reclaiming butanols and N-BUTYL ACETATE |
| CN113521780B (en) * | 2021-09-02 | 2022-08-23 | 东营益盛化工有限公司 | Esterification tower for producing butyl acetate |
| CN114751822B (en) * | 2022-03-16 | 2024-04-09 | 浙江建业化工股份有限公司 | Device for producing n-propyl acetate by thermal coupling and production method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1299807A (en) * | 2000-12-22 | 2001-06-20 | 天津大学 | Single rectifying tower equipment and process of producing high-purity ethyl acetate |
| CN1326923A (en) * | 2000-06-02 | 2001-12-19 | 唐山市冀东溶剂厂 | Method for continuously producing butyl acetate |
| JP2002316967A (en) * | 2001-02-16 | 2002-10-31 | Daicel Chem Ind Ltd | High purity butyl acetate and method for producing the same |
| CN1417182A (en) * | 2002-12-10 | 2003-05-14 | 西安交通大学 | Heat pump azeotropic rectification process and equipment for fuel ethanol |
| US6605738B1 (en) * | 1996-05-29 | 2003-08-12 | Union Carbide Chemicals & Plastics Technology Corporation | Processes for refining butyl acrylate |
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2006
- 2006-02-28 CN CNB2006100339355A patent/CN100412051C/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6605738B1 (en) * | 1996-05-29 | 2003-08-12 | Union Carbide Chemicals & Plastics Technology Corporation | Processes for refining butyl acrylate |
| CN1326923A (en) * | 2000-06-02 | 2001-12-19 | 唐山市冀东溶剂厂 | Method for continuously producing butyl acetate |
| CN1299807A (en) * | 2000-12-22 | 2001-06-20 | 天津大学 | Single rectifying tower equipment and process of producing high-purity ethyl acetate |
| JP2002316967A (en) * | 2001-02-16 | 2002-10-31 | Daicel Chem Ind Ltd | High purity butyl acetate and method for producing the same |
| CN1417182A (en) * | 2002-12-10 | 2003-05-14 | 西安交通大学 | Heat pump azeotropic rectification process and equipment for fuel ethanol |
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Assignee: Jiangmen Handsome Chemical Development Co., Ltd. Assignor: South China University of Technology Contract fulfillment period: 2008.10.8 to 2013.10.7 contract change Contract record no.: 2009440000422 Denomination of invention: Heat pump rectifying prodn. process and plant for n-butyl acetate Granted publication date: 20080820 License type: Exclusive license Record date: 2009.5.27 |
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Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2008.10.8 TO 2013.10.7; CHANGE OF CONTRACT Name of requester: JIANGMEN QIANXIN CHEMICAL DEVELOPMENT CO., LTD. Effective date: 20090527 |
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Granted publication date: 20080820 Termination date: 20140228 |