CN1008731B - The acetic ester new process of production - Google Patents
The acetic ester new process of productionInfo
- Publication number
- CN1008731B CN1008731B CN 86104220 CN86104220A CN1008731B CN 1008731 B CN1008731 B CN 1008731B CN 86104220 CN86104220 CN 86104220 CN 86104220 A CN86104220 A CN 86104220A CN 1008731 B CN1008731 B CN 1008731B
- Authority
- CN
- China
- Prior art keywords
- ethanol
- ethyl hexanoate
- esterification
- dehydrated alcohol
- production
- 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
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Novel process and equipment thereof that ethyl hexanoate is produced, its main points are: determined new proportion scale; Select for use dehydrated alcohol to make dewatering agent, esterification equipment, rectifying device are united two into one, change electrically heated atmospheric distillation ethyl hexanoate into the steam heating rectification under vacuum.Compare with equipment with ethyl hexanoate production technique of the prior art.Have that raw material consumption is low, power consumption is few, with short production cycle, characteristics such as facility investment is few, good product quality.Be applicable to the production of the ethyl hexanoate that perfume industry, organic synthesis, foodstuffs industry etc. are adopted.
Description
The present invention relates to the new process of production of ethyl hexanoate.
According to the retrieval, before the present invention makes, do not find the document relevant especially as yet with the present invention." the Japanese aboveground spices of world's fine chemistry industry handbook (nineteen eighty-two version) introduction is made the method that companies such as institute, Gaoyang chemistry, three Rong Huaxue, Feng Yu spices produce the caproic acid acetate: " in the presence of sulfuric acid; dehydrated alcohol is heated with n-caproic acid, distillation promptly.Refining with distillation method ".But dehydrated alcohol only is used to the esterification of preparing burden in this method for making, is not as dewatering agent.
In addition, produce ethyl hexanoate both at home and abroad, continue to use traditional production technique mostly, be about to caproic acid (content 95%), ethanol (content 92.4%), sulfuric acid by a certain percentage (three's weight ratio is 1: 0.5: 0.2 usually) prepare burden, put into the esterification of esterification pot internal heating, cooling then adds in the sig water and nonesterified caproic acid again.Add in the alkali and after Sodium n-caproate solution, reclaim Diluted Alcohol and a small amount of thick ester after, pump into concentrating pan after concentrated, with pumping in the acidifying pot, add sulfuric acid and carry out acidifying, gained reclaims caproic acid and is used further to batching, reply and use, Diluted Alcohol also is used for replying and uses after concentrating.The thick ester in upper strata sucks in the oil bath rectifying pot (tower) after washing, surplus the electrically heated rectifying 30 hour, the ethyl hexanoate finished product.
The shortcoming of above-mentioned traditional technology is: raw material consumption is big, the production cost height; Complex process, the production cycle is long; Productive rate is low; The discharging of waste liquid amount is big; The power consumption height; The equipment complexity is huge; Only major equipment just needs esterification pot, concentrating pan, acidifying pot, rectifying pot (tower) etc.
The objective of the invention is in order to provide a kind of productive rate height, the reliable ethyl hexanoate new process of production of good economy performance and stable operation.
The objective of the invention is to realize:, and put into esterification rectifying pot (tower) according to new proportioning preparation raw material by following technical process; Steam heating, the backflow esterification; Splash into the esterification of dewatering of anhydrous ethyl ester; Normal pressure recovery ethanol, cooling, light buck are washed; The steam heating rectification under vacuum makes the ethyl hexanoate finished product.
Finishing the used major equipment of above-mentioned novel process is an esterification rectifying pot (tower).
Main points of the present invention are: determined new proportion scale; Select for use dehydrated alcohol as dewatering agent; Use the steam heating rectification under vacuum.
Fig. 1 shows to adopt new technology and produces the apparatus sketch of ethyl hexanoate.
The equipment of producing ethyl hexanoate of adopting new technology comprises: reactor (1), reaction tower (2), condenser (3), liquid storage device (4), double-tube heat exchanger (5), look tube (6), a spinner-type flowmeter (7), (8), (9) and other utility appliance, as thermometer (T), tensimeter (P) etc.
(10) are ethyl hexanoate finished product discharge port among the figure; (11) be light ethanol (ethyl hexanoate chieftain) discharge port; (12) be the dehydrated alcohol opening for feed; (13) be the reactor opening for feed.
Obviously, equipment involved in the present invention, than adopt traditional technology produce ethyl hexanoate simplified equipment many, not only with esterification, rectifying two complete equipments have been combined in together, and saved concentrate, equipment such as acidifying.
Following with reference to accompanying drawing, and, the present invention is carried out detailed description in conjunction with the embodiment that the inventor did:
1. it is raw material that the present invention for preparing burden adopts caproic acid (content 95%) and ethanol (content 92.4%), selects for use sulfuric acid or h type resin to make catalyzer.When making catalyzer with sulfuric acid, the weight ratio between caproic acid, ethanol, the sulfuric acid three was advisable with 1: 0.8～1.2: 0.008, as making catalyzer with h type resin, then selected 1: 0.8～1.2: 0.04 weight ratio.
2. the total reflux esterification will drop into 1000 liter reactors (1) by the raw material (containing catalyzer) of said ratio preparation, feed steam in the chuck of reactor (1), with raw material reflux esterification 2.5 hours, generate the thick ester of ethyl hexanoate.In the total reflux esterification process, vapor pressure, quantity of reflux (by spinner-type flowmeter (7) control) should be controlled at 3.92～4.9N/cm respectively
2With 150～165 liters/hour.After the total reflux esterification finished, feed acidity should be 10～12% in the pot.
3. dehydrated alcohol dehydration esterification after the total reflux esterification process finishes, splashes into reactor (1) bottom with dehydrated alcohol in order to improve the caproic acid transformation efficiency as much as possible, the esterification of dewatering, and open bleeder valve, steam light ethanol.The dehydrated alcohol dripping quantity is by spinner-type flowmeter (8) control, so that the light ethanol amount of steaming and the dehydrated alcohol amount of splashing into keep in a basic balance for well.This process is 11.8～17.3N/cm at vapor pressure
3, reaction tower (2) head temperature is 78.5～79.2 ℃, the liquid temperature is to carry out under 87～88 ℃ the condition in the pot.Through 6～7 hours, steam light alcohol concn and reach 95～96 ℃, feed acidity is reduced to (as adopting the h type resin esterification, then acidity is below 0.8%) below 1.8% in the pot, and the dehydration esterification finishes.
4. after normal pressure recovery ethanol dehydration esterification finished, the beginning normal pressure reclaimed ethanol (as adopting resin catalysis, then need cool off, after branch removes resin, carry out normal pressure again and reclaim ethanol).The ethanol that reaction tower steams, through condenser (3), liquid storage device (4), double-tube heat exchanger (5), look the tube (6), light ethanol (ethyl hexanoate chieftain) discharge port (11), be recycled in the container.In this stage, reactor (1) the jacket steam pressure that raises gradually is until 24.5N/cm
2; Reduce quantity of reflux gradually,, finally reduce to 0 from 130 liters of/hour beginnings; 78.4～78.2 ℃ of tower top temperatures, feed temperature rises to 128～130 ℃ in pot, steams amount of alcohol seldom the time, and normal pressure reclaims ethanol to be finished.
5. after washing the end of ester normal pressure recovery ethanol, feed liquid in the pot is cooled to 60 ℃, adding concentration is 0.35% sodium hydroxide solution, agitator treating.After treating layering, abandon lower floor's alkali waste water, with two times clear water washings, after washing finished, feed acidity should be below 0.2% again.
6. after the ester end is washed in the steam heating rectification under vacuum, feed steam in the chuck, and open vacuum pump simultaneously, under reduced pressure, go out moisture content to the greatest extent earlier, go out the ethyl hexanoate chieftain again, go out the ethyl hexanoate finished product at last.
Vacuum tightness should be controlled at 9.07 * 10 at (going out moisture content, the chieftain) reaction tower in early stage (2) top of this process
4Vapor pressure is 11.8N/cm in the Pa, chuck
2, when going out moisture content, quantity of reflux be controlled at 85～90 liters/time, and closing volume valve, go out to the greatest extent moisture content after, begin the ethyl hexanoate chieftain, quantity of reflux be 50～55 liters/time, when tower top temperature rises to 90 ℃, vacuum tightness reaches 9.33 * 10
4Pa, when fluid was more and stable, fragrance was commented in sampling.Pure as fragrance, promptly change out finished product over to.
Go out finished product in earlier stage, quantity of reflux is controlled at 150～160 liters/hour, goes out output and is controlled at 140～150 liters/hour, 90～95 ℃ of tower top temperatures, vacuum tightness 9.33 * 10
4Pa; The later stage quantity of reflux is reduced to 50～30 liters/hour gradually, goes out output and is controlled at 50～30 liters/hour, 95～95.8 ℃ of tower top temperatures, vacuum tightness 9.53 * 10
4Pa.
When the finished product liquid outlet quantity is reduced to 25 liters/hour, take a sample at any time and comment fragrance.Fragrance promptly finishes finished product as changing slightly.
Of the present invention Yu ethyl hexanoate production technology of the prior art is compared, it is low (for example to have consumption of raw materials, the caproic acid unit consumption standard of existing special class national enterprises is 0.950 ton/ton, and caproic acid unit consumption of the present invention only is 0.8648 ton/ton, the actual yield of caproic acid reaches 97.05%), power consumption low (power consumption reduces by 90% than traditional old technology), it is with short production cycle that (the old technology of tradition is 55 hours, and the present invention only is 22 hours), output big (output improves 3.7 times than traditional old technology), good product quality (reaching U.S. FCC III standard), the characteristics such as equipment investment is few are applicable to perfume industry, the You machine is synthetic, the production of the ethyl hexanoate that food industry etc. adopt.
Claims (2)
1, a kind of novel process of producing ethyl hexanoate, comprise batching, the backflow esterification, the dehydration esterification, normal pressure reclaims ethanol, flow processs such as rectifying, it is characterized in that: the rational proportion of having determined raw material and catalyzer, raw material is caproic acid (content 95%) and ethanol (content 92.4%), catalyzer is sulfuric acid or h type resin, caproic acid, ethanol, prepared (caproic acid between the sulfuric acid three by weight in 1: 0.8～1.2: 0.008, ethanol, Hydrogen is set between the sour three by weight preparation in 1: 0.8～1.2: 0.04, select for use dehydrated alcohol (content 99.1～99.6%) as dewatering agent, use the steam heating rectification under vacuum.
2, novel process according to claim 1 is characterized in that dehydrated alcohol is after the total reflux esterification process finishes, adding reactor (1), steaming light ethanol simultaneously, it is in a basic balance that dehydrated alcohol add-on and the light ethanol amount of steaming keep.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 86104220 CN1008731B (en) | 1986-06-18 | 1986-06-18 | The acetic ester new process of production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 86104220 CN1008731B (en) | 1986-06-18 | 1986-06-18 | The acetic ester new process of production |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN86104220A CN86104220A (en) | 1987-12-30 |
| CN1008731B true CN1008731B (en) | 1990-07-11 |
Family
ID=4802391
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 86104220 Expired CN1008731B (en) | 1986-06-18 | 1986-06-18 | The acetic ester new process of production |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1008731B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101723828B (en) * | 2008-10-27 | 2013-06-19 | 谷长安 | Method for preparing ethyl caproate by continuous esterification |
| CN102974114B (en) * | 2012-12-18 | 2014-10-29 | 上海试四化学品有限公司 | Dichloroethane distillation device and distillation process |
-
1986
- 1986-06-18 CN CN 86104220 patent/CN1008731B/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| CN86104220A (en) | 1987-12-30 |
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