CN1060089A - C 6～24Semicontinuous esterification reaction of organic acid operating method of lipid acid and optimization - Google Patents
C 6～24Semicontinuous esterification reaction of organic acid operating method of lipid acid and optimization Download PDFInfo
- Publication number
- CN1060089A CN1060089A CN 91109949 CN91109949A CN1060089A CN 1060089 A CN1060089 A CN 1060089A CN 91109949 CN91109949 CN 91109949 CN 91109949 A CN91109949 A CN 91109949A CN 1060089 A CN1060089 A CN 1060089A
- Authority
- CN
- China
- Prior art keywords
- acid
- methyl alcohol
- optimization
- reaction
- alcohol
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Abstract
The present invention relates to a kind of realization C
6～24The operation mode and the optimization of saturated and unsaturated fatty acids esterification, semicontinuous esterification is the disposable charging that has replaced interrupter method with the methyl alcohol continuously feeding, and the employing methyl-hydrogen-sulfate monomethyl-sulfate is a catalyzer, in operating process, determined the differential responses stage, adopt the optimum relations of different methanol feed rate, the present invention compares with intermittent process, has methyl alcohol and energy expenditure is low, the characteristics that throughput is high.
Description
The invention belongs to the improvement of methyl esterification of fatty acid operating method and the optimization of operational condition.
C
6～24The esterification reaction of organic acid of saturated and unsaturated fatty acids generally is to carry out under the effect of catalyzer, and its reaction formula is:
Realize this reaction process in industrial production, traditional method is to adopt operating method intermittently, is about to lipid acid and methyl alcohol.In the disposable by a certain percentage input reactor of catalyzer, under certain temperature and pressure, in the reaction times through about 4-5 hour, reaction finishes.This intermittent process is because methyl alcohol is to drop into once, and esterification reaction process is finished in a long time, methyl alcohol has occupied the effective volume of reactor, its consumption is higher, energy consumption is also high simultaneously, for this reason, the operation mode of seeking a kind of new methyl esterification of fatty acid then becomes one of research topic that people attract attention.
The object of the present invention is to provide a kind of operation mode and optimization of new methyl esterification of fatty acid, reduce the consumption of methyl alcohol and energy in the esterification process.
Technical essential of the present invention is: the one, and serialization adds methyl alcohol; The 2nd, with methyl-hydrogen-sulfate monomethyl-sulfate (CH
3OSO
3H) be catalyzer; The 3rd, determined the optimum feeding rate of different step of reaction methyl alcohol.
Accompanying drawing is the process flow diagram that the present invention adopts.Wherein 1 is that methyl alcohol metering cylinder 2 is pump, and 3 is reactor, and 4 is agitator, and 5 is condenser, and 6 is the phlegma basin.
Specific implementation process of the present invention: first with in the disposable input reactor 3 of aliphatic acid, rotating mixer 4 and heat temperature raising, when the temperature of acid reaches 115 ℃～140 ℃ in reactor, begin to squeeze into continuously methyl alcohol in the reactor with pump 2, and adding methyl-hydrogen-sulfate monomethyl-sulfate catalyst, reaction namely begins, then make reactor keep working condition to be: temperature at 115 ℃～140 ℃ for well, pressure at 0～0.2MPa for well, and by condenser unreacted methyl alcohol and the water that reaction generates are shifted out reactor, when the conversion ratio of acid reaches setting, stop to add methyl alcohol, whole course of reaction need be carried out about 1.5～2.0 hours, the conversion ratio of last acid can reach more than 99%, in order further effectively to reduce the consumption of methyl alcohol in the course of reaction, in the different stages of reaction, adopt different methanol feed rate, this is very important, to this, the present invention emphasizes: when aliphatic acid (oleic acid) feed intake as 1Kmol the time, begin to 30 minute stage in reaction, the feed rate of methyl alcohol keeps alcohol, the acid mol ratio is 2.0～2.5Kmol/h for well, reaction carry out 30 minutes with after-stage in, methanol feed rate keeps alcohol, sour mol ratio at 1.2～1.8Kmol/h for well.
The present invention compares with batch process, has greatly shortened the reaction time, saves energy and can reach 10～12 times, has reduced the consumption of methyl alcohol, when the conversion ratio of acid reaches 98%, and alcohol, sour mol ratio can reach 1.50: 1～1.70: 1. Simultaneously can improve production capacity and reach 9 times.
Table 1 the present invention is with interrupter method data contrast table
| Operating method | Fat | Methyl alcohol | Reaction | Acid value | Alkyd | Fat |
| Acid throwing amount kg | Charging capacity kg | Time h | Mol ratio | Acid transformation efficiency % | ||
| Periodical operation | 630 | 540 | 5.0 | 2.19 | 7.07 | 78.87 |
| Semicontinuous Optimizing operation | 800 | 195.1 | 1.25 | 1.24 | 2.05 | 99.36 |
Embodiment 1:
Raw material: cotton oil pin lipid acid, its mole is formed:
Palmitinic acid: 35.6%; Oleic acid: 22.9%; Linolic acid: 41.5%; 120 ℃～140 ℃ scope reactions, adopt constant continuous methanol feeding operating method, data are as follows:
Reaction times (min) transformation efficiency acid-alcohol ratio
60??0.9185??1.73
25??0.9820??2.16
90??0.9865??2.60
105??0.9923??3.02
120??0.9952??3.46
Embodiment 2:
Raw material: cotton oil acid: acid value: 195.1, iodine value: 51.7, moisture content: 2.1%; Methanol concentration: 98%.
Adopt different methanol feed rate operating method continuously, data are as follows:
Reaction times (min) transformation efficiency mol ratio acid value
45??0.980??1.14??3.84
60??0.990??1.50??1.90
25??0.994??1.94??1.24
90??0.997??2.11??0.599
Claims (1)
1, a kind of C that is implemented on
6～24The operation mode and the optimization of the semicontinuous esterification of lipid acid is characterized in that:
1., the temperature of acid in reactor begins to add methyl alcohol when reaching 115～140 ℃, the transformation efficiency that is added to acid in the reactor continuously reaches till the prescribed value;
2., after beginning to add methyl alcohol, add the methyl-hydrogen-sulfate monomethyl-sulfate catalyzer immediately;
3., when the charging capacity of lipid acid is 1Kmol, begin to 30 minute stage in reaction, the feeding rate of methyl alcohol keeps alcohol, the acid mol ratio at 2.0～2.5Kmol/h for well, reaction carry out 30 minutes with latter stage in, methanol feed rate keep alcohol, sour mol ratio at 1.2～1.8Kmol/h for well.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 91109949 CN1025958C (en) | 1991-10-25 | 1991-10-25 | Operation type and optimization for C6-24 fatty acid semi-continous carbomethoxy reaction |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 91109949 CN1025958C (en) | 1991-10-25 | 1991-10-25 | Operation type and optimization for C6-24 fatty acid semi-continous carbomethoxy reaction |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1060089A true CN1060089A (en) | 1992-04-08 |
| CN1025958C CN1025958C (en) | 1994-09-21 |
Family
ID=4910073
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 91109949 Expired - Fee Related CN1025958C (en) | 1991-10-25 | 1991-10-25 | Operation type and optimization for C6-24 fatty acid semi-continous carbomethoxy reaction |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1025958C (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5585506A (en) * | 1994-07-22 | 1996-12-17 | Lonza Inc. | One phase production of polyglycerol esters |
| CN110218574A (en) * | 2019-06-03 | 2019-09-10 | 北京凯瑞英科技有限公司 | By the method for methyl-hydrogen-sulfate monomethyl-sulfate catalysis for preparing biodiesel oil |
-
1991
- 1991-10-25 CN CN 91109949 patent/CN1025958C/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5585506A (en) * | 1994-07-22 | 1996-12-17 | Lonza Inc. | One phase production of polyglycerol esters |
| CN110218574A (en) * | 2019-06-03 | 2019-09-10 | 北京凯瑞英科技有限公司 | By the method for methyl-hydrogen-sulfate monomethyl-sulfate catalysis for preparing biodiesel oil |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1025958C (en) | 1994-09-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107935846B (en) | Device and method for continuously producing environment-friendly plasticizer | |
| CN1041410C (en) | High yield process for the production of methacylic acid esters | |
| CN106977582B (en) | A kind of method of Hydrolysis kinetics phytosterol in deodorization distillate | |
| CN106800976A (en) | A kind of method that glycerine round-robin method continous way prepares biodiesel | |
| CN103045664A (en) | Method for producing biodiesel, sterol and vitamin E from deodorized distillate | |
| CN1060089A (en) | C 6～24Semicontinuous esterification reaction of organic acid operating method of lipid acid and optimization | |
| CN202116468U (en) | Device for producing methyl acetoacetate continuously | |
| CN101671624A (en) | Reaction unit for sludge acclimation and polyhydroxyalkanoates synthesis by sludge and synthetic method thereof | |
| CN111662168A (en) | Method for preparing terephthalaldehyde by catalytic oxidation of terephthalyl alcohol with polyoxometallate | |
| CN102259008B (en) | Solid acid catalyst for esterification reaction and preparation method thereof | |
| CN101293205A (en) | Magnetic solid base catalyst for biological diesel oil production and method for producing the same | |
| CN102796620B (en) | Fixed bed-based continuous catalytic esterification production method | |
| CN1171839C (en) | Production method of alpha, omega bielement alcohol | |
| CN206188686U (en) | Device of butyraldehyde oxidation preparation butyric acid | |
| CN201144226Y (en) | Equipment for processing biodiesel | |
| CN101074391A (en) | Method and catalyst for producing biological diesel oil by high-acid value grease | |
| CN102718632B (en) | Method for preparing terpin hydrate by virtue of continuous hydration | |
| CN103801349B (en) | A kind of vpo catalyst and the application in dehydrating glycerin preparing propone aldehyde thereof | |
| CN108947786B (en) | Method for preparing acrolein by glycerol dehydration | |
| CN111115853A (en) | Safe composite carbon source and production process thereof | |
| CN1907950A (en) | Method of preparing diethylaminoethanol caproate | |
| CN1903829A (en) | Dewater technology of isooctyl nitrate | |
| CN104194945A (en) | Method for preparing biodiesel by screw extruder | |
| CN2813611Y (en) | Alpha, beta unsaturated primary alcohol continuous production apparatus | |
| CN110773237B (en) | Alkyl pyrrole-phosphotungstate catalyst and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C06 | Publication | ||
| PB01 | Publication | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |