CN108675929A - A kind of production technology of ethyl acetate - Google Patents
A kind of production technology of ethyl acetate Download PDFInfo
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- CN108675929A CN108675929A CN201810242954.1A CN201810242954A CN108675929A CN 108675929 A CN108675929 A CN 108675929A CN 201810242954 A CN201810242954 A CN 201810242954A CN 108675929 A CN108675929 A CN 108675929A
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- ethyl acetate
- acetic acid
- esterification reaction
- reaction tower
- tower
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- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 title claims abstract description 111
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 22
- 238000005516 engineering process Methods 0.000 title claims abstract description 18
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 147
- 238000005886 esterification reaction Methods 0.000 claims abstract description 65
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 55
- 238000006243 chemical reaction Methods 0.000 claims abstract description 34
- 235000019441 ethanol Nutrition 0.000 claims abstract description 27
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 25
- 150000002148 esters Chemical class 0.000 claims abstract description 23
- 239000002994 raw material Substances 0.000 claims abstract description 21
- 230000032050 esterification Effects 0.000 claims abstract description 20
- OTGFEQJKSRFOED-UHFFFAOYSA-N [P].[V].[Mo] Chemical compound [P].[V].[Mo] OTGFEQJKSRFOED-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 12
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 12
- 239000011964 heteropoly acid Substances 0.000 claims abstract description 11
- 230000008676 import Effects 0.000 claims description 27
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 8
- 238000010992 reflux Methods 0.000 claims description 5
- 239000000654 additive Substances 0.000 claims description 2
- 230000000996 additive effect Effects 0.000 claims description 2
- 238000007781 pre-processing Methods 0.000 claims description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims 1
- 229910052799 carbon Inorganic materials 0.000 claims 1
- 239000004408 titanium dioxide Substances 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 14
- 238000000034 method Methods 0.000 description 7
- 239000002253 acid Substances 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 125000004494 ethyl ester group Chemical group 0.000 description 3
- 238000004128 high performance liquid chromatography Methods 0.000 description 3
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 239000000052 vinegar Substances 0.000 description 2
- 235000021419 vinegar Nutrition 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- 102000007698 Alcohol dehydrogenase Human genes 0.000 description 1
- 108010021809 Alcohol dehydrogenase Proteins 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- -1 Pharmaceutical field Substances 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000000976 ink Substances 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000000269 nucleophilic effect Effects 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/186—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J27/195—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with vanadium, niobium or tantalum
- B01J27/198—Vanadium
- B01J27/199—Vanadium with chromium, molybdenum, tungsten or polonium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/20—Carbon compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/19—Catalysts containing parts with different compositions
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
The invention belongs to ester type compound production technical fields, specifically disclose a kind of production technology of ethyl acetate.The production industry of ethyl acetate of the present invention includes the following steps：(1) pretreatment of raw material：Acetic acid and ethyl alcohol are added in pretreated tube, handled using phosphorus molybdenum vanadium heteropolyacid and carbon dioxide；(2) esterification：Obtained pretreatment object is imported in esterification reaction tower and is reacted；(3) prepared by finished product：Product obtained by the reaction is condensed, is dehydrated, it is refined after can be obtained finished product.The production technology of ethyl acetate of the present invention is first pre-processed before by acetic acid and ethyl alcohol input esterification reaction tower, effectively shortens raw material in the residence time of esterification reaction tower, and improve the conversion ratio of acetic acid and the yield of ethyl acetate.
Description
【Technical field】
The present invention relates to ester type compound production technical fields, and in particular to a kind of production technology of ethyl acetate.
【Background technology】
Ethyl acetate is a kind of critically important organic solvent and chemical industry base stock, China be mainly used in paint of coating,
Pharmaceutical field, paint adhesive, ink, cellulose, artificial essence's drug and organic acid production in, market demand is year by year
Increase.Currently, the synthetic method of ethyl acetate mainly has acetic acid esterified method, acetaldehyde condensation method, alcohol dehydrogenase method and acetic acid with ethylene
Four kinds of addition process.
Wherein, acetic acid esterified method is most common production method.Acetic acid esterified method is to use the concentrated sulfuric acid for catalyst, will be former
It is esterified in material acetic acid and ethyl alcohol mixing input esterifying kettle, then reaction product is with ethyl acetate, alcohol and water ternary azeotrope
Form steamed from esterification tower top, after be dehydrated and be refining to obtain ethyl acetate, and the boiling point taken out of together in esterifying kettle compared with
The materials such as high acetic acid flow back into esterifying kettle that the reaction was continued from esterification column bottom.
Since esterification is reversible reaction, above method is long there are the reaction time, acetic acid conversion is not high, acetic acid second
The problems such as yield of ester is not high.
Raw material is pre-processed using granular ion exchange resin although Chinese patent CN106478415A is disclosed
Scheme, but it is to improve heat utilization rate to reduce energy consumption that it, which carries out pretreatment of raw material,.
【Invention content】
The goal of the invention of the present invention is：In view of the above problems, a kind of production technology of ethyl acetate is provided.This
The production technology of invention ethyl acetate is first pre-processed before by acetic acid and ethyl alcohol input esterification reaction tower, is effectively shortened
Residence time of the raw material in esterification reaction tower, and improve the conversion ratio of acetic acid and the yield of ethyl acetate.
To achieve the goals above, the technical solution adopted by the present invention is as follows：
A kind of production technology of ethyl acetate, includes the following steps：
(1) pretreatment of raw material：By acetic acid and ethyl alcohol 1-1.5 in molar ratio：After 1 mixing, import miscellaneous more added with phosphorus molybdenum vanadium
In the pretreated tube of acid, it is filled in carbon dioxide gas to pretreated tube when the pretreated tube is evacuated to -1~-2MPa
Pressure is 5-7MPa, keeps 30min, obtains pretreatment object；And preceding 25min controlling reaction temperatures are 60-65 DEG C, rear 5min controls are anti-
It is 100-110 DEG C to answer temperature；
(2) esterification：Above-mentioned pretreatment object is imported from the middle epimere of esterification reaction tower in esterification reaction tower, from esterification
The hypomere of reaction tower imports ethyl alcohol and the molar ratio of acetic acid and ethyl alcohol is made to reach 1 successively:2-2.5, and the concentrated sulfuric acid is added, Yu Chang
Pressure after stopping 40-50min in esterification reaction tower at 95-100 DEG C, reacts the ethyl acetate of generation and what water, ethyl alcohol were formed is total to
Boiling object is steamed from the tower top of esterification reaction tower, is reacted remaining acetic acid and is flowed back into esterification reaction tower from the bottom of tower of esterification reaction tower
The reaction was continued；
(3) prepared by finished product：The azeotropic mixture distilled from tower top obtains thick ester after condensing, being dehydrated successively, wherein one
Partly thick ester flows back into band water in the esterification reaction tower, and the thick ester of a part, which enters after treating column refines, obtains finished product acetic acid second
Ester.
Further, in step (1), the additive amount of the phosphorus molybdenum vanadium heteropolyacid is the 2-3% of the acetic acid quality.
Further, in step (1), the purity of the carbon dioxide is 99.5% or more.
Further, in step (2), the ethyl alcohol, which divides 3 times, to be imported in the esterification reaction tower, and first time import volume is
The 3/5 of total amount is imported, for the second time and the import volume of third time is import total amount 1/5.
Further, in step (2), the addition of the concentrated sulfuric acid is the 0.5-0.8% of the quality of acetic acid.
Further, in step (2), the reflux ratio of the esterification reaction tower is 1.5-2.
In conclusion by adopting the above-described technical solution, the beneficial effects of the invention are as follows：
(1) raw material of the invention by after the excessive ratio mixing of acetic acid by pre-processing so that raw material pretreated tube
Reactiveness is carried out by abundant activation, reaction has been further speeded up when entering esterification reaction tower by pretreated raw material, and divide
The ethyl alcohol of Duan Luxu supplements has not only effectively facilitated the conversion of acetic acid, is swift in response, and esterification is promoted to be carried out to forward direction, and
Avoiding disposable addition causes insufficient contact, reaction in the raw material short time slowly, to be converted so as to cause raw material incomplete existing
As occur, effectively improve the conversion ratio of raw material and reaction time be short, esterification into enter equilibrium stage before just
Start to steam product, the selectivity of ethyl acetate is strong, to improve the yield of product.
(2) there is synergistic effect in the phosphorus molybdenum vanadium heteropolyacid and carbon dioxide that pretreatment of raw material of the present invention uses, first, preceding
25min, the pressure for the 5-7MPa that carbon dioxide generates so that phosphorus molybdenum vanadium heteropolyacid, which generates to be crushed, forms micro- of loose cellular
Grain, has sufficiently promoted the mixing of raw material and phosphorus molybdenum vanadium heteropolyacid and the interior diffusion of raw material, and then it is miscellaneous more to effectively improve phosphorus molybdenum vanadium
The catalytic activity and Catalysis Rate of acid, make raw material proceed by reaction rapidly, secondly, rear 5min, in 100-110 DEG C of high temperature
Under, carbon dioxide reacted with the water that esterification generates generate carbonic acid it is ionizable go out a large amount of hydrogen ion, the hydrogen ion of generation
The acid intensity of reaction system can be effectively improved with a small amount of sulfuric acid added in esterification reaction tower, it is miscellaneous to promote phosphorus molybdenum vanadium
The attack of polyacid nucleophilic group promotes raw material dehydration and generates ethyl acetate, meanwhile, extra carbon dioxide can be further combined with
The water of generation reduces the water content of reaction system, is carried out to further promote the positive of esterification, ethyl acetate
High selectivity reduces side reaction, product yield high.
(3) present invention is using phosphorus molybdenum vanadium heteropolyacid as major catalyst, using carbon dioxide and sulfuric acid as catalyst promoter, three
Synergistic effect is generated, the selectivity of esterification rate, original conversion ratio and ethyl acetate is improved, to effectively improve acetic acid second
The yield of ester, also, greatly reduce conventional method and use the strong acid such as sulfuric acid, hydrochloric acid to be generated to equipment as catalyst completely
Extent of corrosion improves the service life of equipment.
【Specific implementation mode】
Below in conjunction with specific embodiment, the present invention is further illustrated.
Embodiment 1
A kind of production technology of ethyl acetate, includes the following steps：
(1) pretreatment of raw material：By acetic acid and ethyl alcohol in molar ratio 1：After 1 mixing, it is the acetic acid to import added with quality
Being filled with purity in the pretreated tube of the phosphorus molybdenum vanadium heteropolyacid of quality 2%, when the pretreated tube is evacuated to -1MPa is
99.5% or more carbon dioxide gas to pretreatment overpressure is 5MPa, keeps 30min, obtains pretreatment object；And preceding 25min
Controlling reaction temperature is 60 DEG C, and rear 5min controlling reaction temperatures are 100 DEG C；
(2) esterification：Above-mentioned pretreatment object is imported from the middle epimere of esterification reaction tower in esterification reaction tower, from esterification
3 importing ethyl alcohol of the hypomere of reaction tower point make the molar ratio of acetic acid and ethyl alcohol reach 1:2, and first time import volume is to import always
The 3/5 of amount, for the second time and the import volume of third time is import total amount 1/5；And it is the quality of acetic acid 0.5% that quality, which is added,
The concentrated sulfuric acid, under normal pressure, 95 DEG C, reflux ratio 1.5 in esterification reaction tower stop 40min after, react generation ethyl acetate and
The azeotropic mixture that water, ethyl alcohol are formed is steamed from the tower top of esterification reaction tower, is reacted remaining acetic acid and is returned from the bottom of tower of esterification reaction tower
Flow in esterification reaction tower that the reaction was continued；
(3) prepared by finished product：The azeotropic mixture distilled from tower top obtains thick ester after condensing, being dehydrated successively, wherein one
Partly thick ester flows back into band water in the esterification reaction tower, and the thick ester of a part, which enters after treating column refines, obtains finished product acetic acid second
Ester.
It takes 3mL acetic acid product ethyl esters to be analyzed with high performance liquid chromatography, obtains following result：Acetic acid conversion is
91.7%, ethyl acetate yield is 83.4%.
Embodiment 2
A kind of production technology of ethyl acetate, includes the following steps：
(1) pretreatment of raw material：By acetic acid and ethyl alcohol in molar ratio 1.3：After 1 mixing, it is the vinegar to import added with quality
In the pretreated tube of the phosphorus molybdenum vanadium heteropolyacid of sour quality 2.5%, purity is filled with when the pretreated tube is evacuated to -1.5MPa
It is 6MPa for 99.5% or more carbon dioxide gas to pretreatment overpressure, keeps 30min, obtain pretreatment object；And it is preceding
25min controlling reaction temperatures are 62 DEG C, and rear 5min controlling reaction temperatures are 105 DEG C；
(2) esterification：Above-mentioned pretreatment object is imported from the middle epimere of esterification reaction tower in esterification reaction tower, from esterification
3 importing ethyl alcohol of the hypomere of reaction tower point make the molar ratio of acetic acid and ethyl alcohol reach 1:2.3, and first time import volume is to import
The 3/5 of total amount, for the second time and the import volume of third time is import total amount 1/5；And it is the quality of acetic acid 0.6% that quality, which is added,
The concentrated sulfuric acid, under normal pressure, 98 DEG C, reflux ratio 1.8 in esterification reaction tower stop 45min after, react the ethyl acetate of generation
The azeotropic mixture formed with water, ethyl alcohol is steamed from the tower top of esterification reaction tower, reacts bottom of tower of the remaining acetic acid from esterification reaction tower
Flow back into esterification reaction tower that the reaction was continued；
(3) prepared by finished product：The azeotropic mixture distilled from tower top obtains thick ester after condensing, being dehydrated successively, wherein one
Partly thick ester flows back into band water in the esterification reaction tower, and the thick ester of a part, which enters after treating column refines, obtains finished product acetic acid second
Ester.
It takes 3mL acetic acid product ethyl esters to be analyzed with high performance liquid chromatography, obtains following result：Acetic acid conversion is
92.3%, ethyl acetate yield is 83.8%.
Embodiment 3
A kind of production technology of ethyl acetate, includes the following steps：
(1) pretreatment of raw material：By acetic acid and ethyl alcohol in molar ratio 1.5：After 1 mixing, it is the vinegar to import added with quality
Being filled with purity in the pretreated tube of the phosphorus molybdenum vanadium heteropolyacid of sour quality 3%, when the pretreated tube is evacuated to -2MPa is
99.5% or more carbon dioxide gas to pretreatment overpressure is 7MPa, keeps 30min, obtains pretreatment object；And preceding 25min
Controlling reaction temperature is 65 DEG C, and rear 5min controlling reaction temperatures are 110 DEG C；
(2) esterification：Above-mentioned pretreatment object is imported from the middle epimere of esterification reaction tower in esterification reaction tower, from esterification
3 importing ethyl alcohol of the hypomere of reaction tower point make the molar ratio of acetic acid and ethyl alcohol reach 1:2.5, and first time import volume is to import
The 3/5 of total amount, for the second time and the import volume of third time is import total amount 1/5；And it is the quality of acetic acid 0.8% that quality, which is added,
The concentrated sulfuric acid, under normal pressure, 100 DEG C, reflux ratio 2 in esterification reaction tower stop 50min after, react generation ethyl acetate and
The azeotropic mixture that water, ethyl alcohol are formed is steamed from the tower top of esterification reaction tower, is reacted remaining acetic acid and is returned from the bottom of tower of esterification reaction tower
Flow in esterification reaction tower that the reaction was continued；
(3) prepared by finished product：The azeotropic mixture distilled from tower top obtains thick ester after condensing, being dehydrated successively, wherein one
Partly thick ester flows back into band water in the esterification reaction tower, and the thick ester of a part, which enters after treating column refines, obtains finished product acetic acid second
Ester.
It takes 3mL acetic acid product ethyl esters to be analyzed with high performance liquid chromatography, obtains following result：Acetic acid conversion is
90.9%, ethyl acetate yield is 82.7%.
Above description is the detailed description for the present invention preferably possible embodiments, but embodiment is not limited to this hair
Bright patent claim, it is all the present invention suggested by technical spirit under completed same changes or modifications change, should all belong to
In the covered the scope of the claims of the present invention.
Claims (6)
1. a kind of production technology of ethyl acetate, which is characterized in that include the following steps：
(1) pretreatment of raw material：By acetic acid and ethyl alcohol 1-1.5 in molar ratio：After 1 mixing, import added with phosphorus molybdenum vanadium heteropolyacid
In pretreated tube, carbon dioxide gas is filled with when the pretreated tube is evacuated to -1~-2MPa to pre-processing overpressure
For 5-7MPa, 30min is kept, pretreatment object is obtained；And preceding 25min controlling reaction temperatures are 60-65 DEG C, rear 5min controls reaction temperature
Degree is 100-110 DEG C；
(2) esterification：Above-mentioned pretreatment object is imported from the middle epimere of esterification reaction tower in esterification reaction tower, from esterification
The hypomere of tower imports ethyl alcohol and the molar ratio of acetic acid and ethyl alcohol is made to reach 1 successively:2-2.5, and the concentrated sulfuric acid is added, in normal pressure, 95-
At 100 DEG C in esterification reaction tower stop 40-50min after, react generation ethyl acetate and water, ethyl alcohol formed azeotropic mixture from
The tower top of esterification reaction tower steams, and reacts remaining acetic acid and is flowed back into esterification reaction tower from the bottom of tower of esterification reaction tower and is continued instead
It answers；
(3) prepared by finished product：The azeotropic mixture distilled from tower top obtains thick ester, a portion after condensing, being dehydrated successively
Thick ester flows back into band water in the esterification reaction tower, and the thick ester of a part, which enters after treating column refines, obtains finished product ethyl acetate.
2. a kind of production technology of ethyl acetate according to claim 1, which is characterized in that in step (1), the phosphorus molybdenum vanadium
The additive amount of heteropoly acid is the 2-3% of the acetic acid quality.
3. a kind of production technology of ethyl acetate according to claim 1, which is characterized in that in step (1), the titanium dioxide
The purity of carbon is 99.5% or more.
4. a kind of production technology of ethyl acetate according to claim 1, which is characterized in that in step (2), the ethyl alcohol point
It imports in the esterification reaction tower for 3 times, and first time import volume is import total amount 3/5, the import volume of second and third time
To import the 1/5 of total amount.
5. a kind of production technology of ethyl acetate according to claim 1, which is characterized in that in step (2), the concentrated sulfuric acid
Addition be the quality of acetic acid 0.5-0.8%.
6. a kind of production technology of ethyl acetate according to claim 1, which is characterized in that in step (2), the esterification is anti-
It is 1.5-2 to answer the reflux ratio of tower.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810242954.1A CN108675929A (en) | 2018-03-23 | 2018-03-23 | A kind of production technology of ethyl acetate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810242954.1A CN108675929A (en) | 2018-03-23 | 2018-03-23 | A kind of production technology of ethyl acetate |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1325840A (en) * | 2001-04-20 | 2001-12-12 | 清华大学 | Process for preparing ethyl acetate |
| CN1580031A (en) * | 2004-05-21 | 2005-02-16 | 河北科技大学 | Method for producing acetic ether |
| CN1660765A (en) * | 2004-12-13 | 2005-08-31 | 上海吴泾化工有限公司 | New technique of esterifying reaction for producing ethyl acetate |
| CN106478415A (en) * | 2016-08-17 | 2017-03-08 | 泰兴金江化学工业有限公司 | A kind of ethyl acetate energy-saving processing technique |
-
2018
- 2018-03-23 CN CN201810242954.1A patent/CN108675929A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1325840A (en) * | 2001-04-20 | 2001-12-12 | 清华大学 | Process for preparing ethyl acetate |
| CN1580031A (en) * | 2004-05-21 | 2005-02-16 | 河北科技大学 | Method for producing acetic ether |
| CN1660765A (en) * | 2004-12-13 | 2005-08-31 | 上海吴泾化工有限公司 | New technique of esterifying reaction for producing ethyl acetate |
| CN106478415A (en) * | 2016-08-17 | 2017-03-08 | 泰兴金江化学工业有限公司 | A kind of ethyl acetate energy-saving processing technique |
Non-Patent Citations (1)
| Title |
|---|
| 胡拖平等: "高压CO2存在下的乙醇/乙酸酯化反应", 《石油化工》 * |
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Application publication date: 20181019 |