CN1468835A - Ester exchange process of methyl acetate to prepare fatty alcohol acetate - Google Patents
Ester exchange process of methyl acetate to prepare fatty alcohol acetate Download PDFInfo
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Abstract
Fatty alcohol and methyl acetate are made to produce ester exchange reaction in the presence of catalyst at reaction temperature 50-120 deg.c. The steam material in the reactant system after being methyl ester eliminated is returned to the reaction system, and after reaction for 2-6 hr, the reactant material is rectified and separated to produce the fatty alcohol acetate product. During the process of eliminating methyl alcohol from steam material, the steam material is either treated through condensation and extraction with saturated water solution of NaCl, or treated through extraction with water as extractant and rectification. The present invention solves the technological problem that methyl acetate with relatively low boiling point could not produce ester exchange reaction with other fatty alcohol to produce corresponding fatty alcohol acetate.
Description
Technical field
The invention belongs to a kind of is raw material with ritalin and Fatty Alcohol(C12-C14 and C12-C18), prepares the method for corresponding amyl acetate fatty alcohol in the presence of catalyzer by transesterification reaction.
Background technology
At present, the suitability for industrialized production polyvinyl alcohol generally is to make Vinyl Acetate Copolymer earlier, and alcoholysis in alkaline aqueous solution makes polyvinyl alcohol with Vinyl Acetate Copolymer and methyl alcohol then.In this process, will produce a large amount of by-product methyl acetates.The ritalin of this by-product exists with the form of mixtures of ritalin, methyl alcohol, water and small amount of impurities, wherein the content of ritalin is about 60～85%, the content of methyl alcohol is about 15～40%, the content of water is about 0.5%～10%, the content of impurity is about 0.1～5%, because by-product ritalin purity is not high, contains more methyl alcohol, so direct using value is little.Therefore, industrial many ritalin mixtures with this by-product are hydrolyzed and reclaim acetic acid and methyl alcohol is applied mechanically.But, in the prior art by-product methyl acetate hydrolysis reclaim operational path long, relate to that appliance arrangement is many, complicated operation, energy consumption greatly, production cost is higher.Particularly produce the industrialization of acetic acid along with carbonylating process, making that the production cost of acetic acid is low greatly reduces, and the method that still adopts the hydrolysis recovery set to use to the ritalin of by-product just seems very uneconomical.
Theoretically, ester compound can make by direct esterification reaction or transesterify (comprise ester and alcohol, ester and the exchange of acid or the exchange of ester and the ester) reaction of alcohol with acid, and ritalin can make corresponding amyl acetate fatty alcohol by transesterification reaction with Fatty Alcohol(C12-C14 and C12-C18).Many amyl acetate fatty alcohols all have higher using value, can be used in the perfume industry as N-BUTYL ACETATE, and also can be used as solvent and be used for industry such as plastics, coating, nitrocotton, imitation leather, or as extraction agent, band aqua etc.; Propyl acetate can be used as the retentivity quick dry agent, is used for printing-ink or is used for nitrocellulose, chlorinated rubber and resol etc. as solvent; Amyl acetate-n can be used as solvent, is used for coating, spices, makeup, wood binder, or is used for imitation leather, weaving processing, film and gunpowder manufacture view; Isobutyl acetate except that as nitrocotton and the solvent of paint, be commonly used for fruit flavors or as the aromatics modifier of rose.But, ritalin and Fatty Alcohol(C12-C14 and C12-C18) carry out transesterification reaction and prepare corresponding amyl acetate fatty alcohol and will face such problem: the boiling point (54 ℃) of the azeotrope that ritalin or it and methyl alcohol form is usually less than the boiling point of other materials in the transesterification reaction system (reactant or reaction product), therefore, in the transesterify process, the evaporation because of ritalin in the reaction system makes that transesterification reaction is difficult to carry out.So, can't make ritalin and other Fatty Alcohol(C12-C14 and C12-C18) generation transesterification reactions prepare corresponding amyl acetate fatty alcohol with conventional method.
Summary of the invention
It is raw material with ritalin and Fatty Alcohol(C12-C14 and C12-C18) that technical problem to be solved by this invention provides a kind of, prepares the method for corresponding amyl acetate fatty alcohol by transesterification reaction.Particularly being prepared the mixture that is rich in ritalin of by-product in the polyvinyl alcohol process by Vinyl Acetate Copolymer and methyl alcohol alcoholysis, and Fatty Alcohol(C12-C14 and C12-C18) is raw material, prepares corresponding amyl acetate fatty alcohol by transesterification reaction.It will for the ritalin of this by-product seek a kind of benefit higher utilize method.
Below be the technical scheme that the present invention solves the problems of the technologies described above:
A kind of is raw material with ritalin and Fatty Alcohol(C12-C14 and C12-C18), the method for preparing corresponding amyl acetate fatty alcohol, Fatty Alcohol(C12-C14 and C12-C18) and ritalin are carried out transesterification reaction in the presence of catalyzer, temperature of reaction is 50～120 ℃, the vapor feed of reaction system Returning reacting system after methyl alcohol is removed in separation reacts 2～6 hours afterreaction materials and gets product amyl acetate fatty alcohol through rectifying separation.
Above-mentioned Fatty Alcohol(C12-C14 and C12-C18) can be in ethanol, propyl alcohol, Virahol, butanols, isopropylcarbinol, amylalcohol, primary isoamyl alcohol, hexanol, isohexyl alcohol, enanthol, iso-heptanol, octanol or the isooctyl alcohol a kind of.
Above-mentioned catalyzer can be sulfuric acid, phosphoric acid, tosic acid, storng-acid cation exchange resin, macropore strong acid cation exchange resin, sal enixum, sodium pyrosulfate, HZSM-5 molecular sieve, h-mordenite, zinc acetate, sodium methylate or sodium ethylate, and catalyst consumption is 0.1%～8% of a reaction mass total mass.Wherein, catalyzer is preferably sulfuric acid, tosic acid or sal enixum.
Feeding intake of transesterification reaction raw material is can ritalin excessive, and at this moment, Fatty Alcohol(C12-C14 and C12-C18) and ritalin feed intake with following mol ratio and carry out transesterification reaction:
Fatty Alcohol(C12-C14 and C12-C18): ritalin=1: 1.1～1: 3.5, and the contriver more recommends:
Fatty Alcohol(C12-C14 and C12-C18): ritalin=1: 1.5～1: 1.9;
Feeding intake also of transesterification reaction raw material is can Fatty Alcohol(C12-C14 and C12-C18) excessive, and at this moment, Fatty Alcohol(C12-C14 and C12-C18) and ritalin feed intake with following mol ratio and carry out transesterification reaction:
Fatty Alcohol(C12-C14 and C12-C18): ritalin=1.1: 1～3.0: 1, and the contriver more recommends:
Fatty Alcohol(C12-C14 and C12-C18): ritalin=1.5: 1～1.9: 1.
The vapor feed of above-mentioned reaction system separate remove methyl alcohol method can for: after the vapor feed condensation be 5～20% CuSO with water, dimethyl formamide, concentration expressed in percentage by weight
4The aqueous solution, concentration expressed in percentage by weight are that 10～30% the NaCl aqueous solution or the saturated NaCl aqueous solution are that extraction agent carries out extracting and separating, extraction temperature is 10～40 ℃, the consumption of extraction agent is that the weight ratio of extraction agent and raw material ritalin amount is 1: 1～2: 1, solvent phase is rich in methyl alcohol, wherein the contriver more to recommend with the saturated NaCl aqueous solution be that extraction agent carries out extracting and separating;
The vapor feed of above-mentioned reaction system separate remove methyl alcohol method also can for: vapor feed is that extraction agent carries out extracting rectifying with water, the tower top temperature of extractive distillation column is 50～70 ℃, tower still temperature is 80～100 ℃, the input material volume ratio of material and water is 1: 1～3: 1, reflux ratio is 0.2～0.75, and working pressure is normal pressure～0.4MPa, and stage number is 25～36, tower still material is rich in methyl alcohol, returns the transesterification reaction system after being rich in the cat head material condensation of ritalin.
The used ritalin raw material of above-mentioned transesterification reaction can be by Vinyl Acetate Copolymer and methyl alcohol alcoholysis prepare produce in the polyvinyl alcohol process, after the methyl alcohol initial gross separation mixture that is rich in ritalin of institute's by-product, wherein the content of ritalin is 60～85%.
In above technical scheme, the vapor feed of reaction system separated to remove behind the methyl alcohol Returning reacting system be unusual critical step, this has reduced the methanol concentration of one of reaction product on the one hand, simultaneously reactant ritalin concentration is maintained enough levels, this has just improved the forward impellent of transesterification reaction, thereby reaction can be carried out smoothly.It only is that the contriver recommends that above-mentioned two kinds of vapor feed with reaction system are separated the method for removing methyl alcohol, this can not be interpreted as limitation of the invention, other any suitable known method also can be applied in the technical scheme provided by the invention, as technology of adopting membrane sepn or the like.
Compared with prior art, positive effect of the present invention is to provide a kind of and is easy to be raw material with ritalin and Fatty Alcohol(C12-C14 and C12-C18), to prepare the method for corresponding amyl acetate fatty alcohol by transesterification reaction industrialized.It has solved the boiling point that is lower than other materials in the transesterification reaction system because of the ritalin boiling point, and conventional method can't make ritalin and other Fatty Alcohol(C12-C14 and C12-C18) generation transesterification reactions prepare the technical problem of corresponding amyl acetate fatty alcohol to apply.Particularly the present invention for prepare by Vinyl Acetate Copolymer and methyl alcohol alcoholysis produce in the polyvinyl alcohol process, after the methyl alcohol initial gross separation ritalin of institute's by-product sought a kind of benefit higher utilize method.
Embodiment
To come below that the invention will be further described by some specific embodiments, in an embodiment, the yield of the transformation efficiency of ritalin, amyl acetate fatty alcohol is defined as:
[embodiment 1～10]
With purity is that Fatty Alcohol(C12-C14 and C12-C18) more than 95% and purity are the ritalin more than 95%, adds one by required feed ratio and has in the enamel reactor of condenser, and add the catalyzer of aequum.Reactant is heated to suitable temperature while stirring carries out transesterification reaction under normal pressure.Evaporation material in the reaction system enters an extract return method device after condenser condenses.Add extraction agent in the extract return method device in advance, the consumption of extraction agent is that the weight ratio of extraction agent and raw material ritalin amount is 1: 1～2: 1.Phlegma is with after extraction agent fully contacts, and the methyl alcohol in the phlegma is extracted separation, is enriched in the extraction agent; The ritalin that is not extracted in the phlegma is back to the transesterification reaction system.The content of each component in the material chromatographically detection reaction product is answered in negate after the suitable reaction times of process, calculates reaction result.Reaction end afterreaction product separates purification and obtains corresponding amyl acetate fatty alcohol product.
Fatty Alcohol(C12-C14 and C12-C18) raw material, catalyzer and the consumption thereof that each embodiment transesterification reaction is concrete, concrete reaction conditions see Table 1 and table 2, and the used concrete extraction agent of extraction separation process, the extraction process condition of reaction system evaporation material see Table 3, and reaction result sees Table 5.[embodiment 11～15]
The raw material ritalin is for being prepared the mixture that is rich in ritalin of by-product in the polyvinyl alcohol process by Vinyl Acetate Copolymer and methyl alcohol alcoholysis, wherein the content of ritalin is 60～85%, and all the other are with [embodiment 1～10].
Fatty Alcohol(C12-C14 and C12-C18) raw material, catalyzer and the consumption thereof that each embodiment transesterification reaction is concrete, concrete reaction conditions see Table 1 and table 2, and the used concrete extraction agent of extraction separation process, the extraction process condition of reaction system evaporation material see Table 3, and reaction result sees Table 5.[embodiment 16～18]
Evaporation material in the reaction system is introduced extractive distillation column from the middle and lower part of an extractive distillation column, and it is reverse from top to bottom descending from the middle and upper part of extractive distillation column to make extraction agent with water.Reflux ratio is 0.2～0.75, and stage number is 2 5～36.Methyl alcohol is rich in the discharging of tower still; The cat head discharging is that content is not less than 95% ritalin, returns transesterification reaction system all the other same [embodiment 1～10].
Fatty Alcohol(C12-C14 and C12-C18) raw material, catalyzer and the consumption thereof that each embodiment transesterification reaction is concrete, concrete reaction conditions see Table 1 and table 2, and the concrete processing condition of reaction system evaporation material extracting rectifying process see Table 4, and reaction result sees Table 5.[embodiment 19～21]
The raw material ritalin is for being prepared the mixture that is rich in ritalin of by-product in the polyvinyl alcohol process by Vinyl Acetate Copolymer and methyl alcohol alcoholysis, wherein the content of ritalin is 60～85%, and all the other are with [embodiment 16～18].
Fatty Alcohol(C12-C14 and C12-C18) raw material, catalyzer and the consumption thereof that each embodiment transesterification reaction is concrete, concrete reaction conditions see Table 1 and table 2, and the concrete processing condition of extracting rectifying process of reaction system evaporation material see Table 4, and reaction result sees Table 5.Table 1.
Annotate: feed ratio is a Fatty Alcohol(C12-C14 and C12-C18): ritalin (mol ratio).Table 2.
| Fatty Alcohol(C12-C14 and C12-C18) is former | Feed ratio | Catalyzer | |
| Embodiment 1 | Butanols | ???3∶2 | Sal enixum |
| Embodiment 2 | Butanols | ???3∶2 | Sulfuric acid |
| Embodiment 3 | Butanols | ???4∶2 | Sal enixum |
| Embodiment 4 | Butanols | ???3∶2 | Sal enixum |
| Embodiment 5 | Butanols | ???3∶2 | Sulfuric acid |
| Embodiment 6 | Butanols | ???5∶2 | ????HZSM-5 |
| Embodiment 7 | Butanols | ???3∶2 | Tosic acid |
| Embodiment 8 | Butanols | ???3∶2 | H-mordenite |
| Embodiment 9 | Butanols | ???3∶2 | Zeo-karb |
| Embodiment 10 | Butanols | ???2∶3 | Sal enixum |
| Embodiment 11 | Butanols | ???3∶2 | Sal enixum |
| Embodiment 12 | Primary isoamyl alcohol | ???3∶2 | ????HZSM-5 |
| Embodiment 13 | Hexanol | ???3∶2 | Sulfuric acid |
| Embodiment 14 | Isooctyl alcohol | ???3∶2 | Sal enixum |
| Embodiment 15 | Ethanol | ???6∶2 | Zinc acetate |
| Embodiment 16 | Butanols | ???3∶2 | Sal enixum |
| Embodiment 17 | Primary isoamyl alcohol | ???3∶2 | Sulfuric acid |
| Embodiment 18 | Butanols | ???3∶2 | Tosic acid |
| Embodiment 19 | Butanols | ???3∶2 | Sal enixum |
| Embodiment 20 | Butanols | ???4∶2 | ????HZSM-5 |
| Embodiment 21 | Butanols | ???3∶2 | H-mordenite |
| Catalyst levels (%) | Temperature of reaction (℃) | Reaction times (hr) | |
| Embodiment 1 | ????1.2 | ????50～90 | ??????5 |
| Embodiment 2 | ????0.8 | ????50～90 | ??????4 |
| Embodiment 3 | ????1.2 | ????50～90 | ??????5 |
| Embodiment 4 | ????1.2 | ????50～90 | ??????5 |
| Embodiment 5 | ????0.8 | ????50～90 | ??????4 |
| Embodiment 6 | ????2.0 | ????50～85 | ??????6 |
| Embodiment 7 | ????0.9 | ????50～90 | ??????5 |
| Embodiment 8 | ????2.0 | ????50～83 | ??????6 |
| Embodiment 9 | ????2.0 | ????50～80 | ??????6 |
| Embodiment 10 | ????1.2 | ????50～90 | ??????5 |
| Embodiment 11 | ????1.2 | ????50～90 | ??????5 |
| Embodiment 12 | ????2.0 | ????50～85 | ??????6 |
| Embodiment 13 | ????0.8 | ????50～95 | ??????5 |
| Embodiment 14 | ????1.2 | ????50～95 | ??????5 |
| Embodiment 15 | ????1.0 | ????50～80 | ??????5 |
| Embodiment 16 | ????1.2 | ????50～100 | ??????3 |
| Embodiment 17 | ????0.8 | ????50～100 | ??????4 |
| Embodiment 18 | ????0.9 | ????50～100 | ??????4 |
| Embodiment 19 | ????1.2 | ????50～100 | ??????3 |
| Embodiment 20 | ????2.0 | ????50～95 | ??????6 |
| Embodiment 21 | ????2.0 | ????50～95 | ??????6 |
Annotate: catalyst levels is the weight percentage in the reaction mass total mass.Table 3.
| Extraction agent | The extraction agent consumption | Extraction temperature (℃) | |
| Embodiment 1 | Water | ????1.3∶1 | ????20 |
| Embodiment 2 | ??DMF | ????1.1∶1 | ????20 |
| Embodiment 3 | ??15％NaCl | ????1.3∶1 | ????18 |
| Embodiment 4 | Saturated NaCl | ????1.3∶1 | ????20 |
| Embodiment 5 | ??10％CuSO4 | ????1.1∶1 | ????40 |
| Embodiment 6 | Saturated NaCl | ????1.3∶1 | ????20 |
| Embodiment 7 | Saturated NaCl | ????1.4∶1 | ????18 |
| Embodiment 8 | Saturated NaCl | ????2∶1 | ????10 |
| Embodiment 9 | Saturated NaCl | ????1.5∶1 | ????18 |
| Embodiment 10 | Saturated NaCl | ????1.3∶1 | ????20 |
| Embodiment 11 | Saturated NaCl | ????1.3∶1 | ????18 |
| Embodiment 12 | Saturated NaCl | ????1.6∶1 | ????20 |
| Embodiment 13 | Saturated NaCl | ????1.3∶1 | ????18 |
| Embodiment 14 | Saturated NaCl | ????1.5∶1 | ????20 |
| Embodiment 15 | Saturated NaCl | ????1.6∶1 | ????18 |
Annotate: the extraction agent consumption is the weight ratio of extraction agent and raw material ritalin amount.Table 4.
Annotate: charge ratio is the volume ratio that is extracted the material and the water of rectifying.Table 5.
| Charge ratio | Tower top temperature (℃) | Column bottom temperature (℃) | Working pressure (MPa) | |
| Embodiment 16 | ??2∶1 | ???61 | ??????88 | ????0.15 |
| Embodiment 17 | ??2.5∶1 | ???63 | ??????87 | ????0.10 |
| Embodiment 18 | ??3∶1 | ???65 | ??????85 | ????0.10 |
| Embodiment 19 | ??1.5∶1 | ???59 | ??????90 | ????0.20 |
| Embodiment 20 | ??1.3∶1 | ???58 | ??????95 | ????0.25 |
| Embodiment 21 | ??2∶1 | ???61 | ??????88 | ????0.4 |
| Ritalin transformation efficiency (%) | Amyl acetate fatty alcohol yield (%) | |
| Embodiment 1 | ???????63.5 | ???????52.1 |
| Embodiment 2 | ???????64.0 | ???????51.3 |
| Embodiment 3 | ???????66.1 | ???????58.3 |
| Embodiment 4 | ???????68.3 | ???????60.2 |
| Embodiment 5 | ???????62.6 | ???????50.7 |
| Embodiment 6 | ???????53.8 | ???????45.7 |
| Embodiment 7 | ???????60.2 | ???????49.5 |
| Embodiment 8 | ???????50.1 | ???????43.3 |
| Embodiment 9 | ???????45.4 | ???????33.6 |
| Embodiment 10 | ???????42.8 | ???????37.4 |
| Embodiment 11 | ???????67.9 | ???????60.3 |
| Embodiment 12 | ???????60.5 | ???????48.2 |
| Embodiment 13 | ???????62.1 | ???????53.9 |
| Embodiment 14 | ???????61.4 | ???????52.7 |
| Embodiment 15 | ???????52.7 | ???????42.8 |
| Embodiment 16 | ???????91.3 | ???????83.1 |
| Embodiment 17 | ???????88.1 | ???????75.3 |
| Embodiment 18 | ???????86.8 | ???????78.5 |
| Embodiment 19 | ???????91.0 | ???????82.9 |
| Embodiment 20 | ???????78.5 | ???????70.1 |
| Embodiment 21 | ???????75.1 | ???????68.7 |
Claims (12)
1, a kind of is raw material with ritalin and Fatty Alcohol(C12-C14 and C12-C18), the method for preparing corresponding amyl acetate fatty alcohol by transesterification reaction, Fatty Alcohol(C12-C14 and C12-C18) and ritalin are carried out transesterification reaction in the presence of catalyzer, temperature of reaction is 50～120 ℃, the vapor feed of reaction system is separated except that Returning reacting system behind the methyl ester removal, reacts 2～6 hours afterreaction materials and gets product amyl acetate fatty alcohol through rectifying separation.
2, the method for preparing the amyl acetate fatty alcohol according to claim 1 is characterized in that described Fatty Alcohol(C12-C14 and C12-C18) is a kind of in ethanol, propyl alcohol, Virahol, butanols, isopropylcarbinol, amylalcohol, primary isoamyl alcohol, hexanol, isohexyl alcohol, enanthol, iso-heptanol, octanol or the isooctyl alcohol.
3, the method for preparing the amyl acetate fatty alcohol according to claim 1, it is characterized in that described catalyzer for being sulfuric acid, phosphoric acid, tosic acid, storng-acid cation exchange resin, macropore strong acid cation exchange resin, sal enixum, sodium pyrosulfate, HZSM-5 molecular sieve, h-mordenite, zinc acetate, sodium methylate or sodium ethylate, catalyst consumption is 0.1%～8% of a reaction mass total mass.
4, the method for preparing the amyl acetate fatty alcohol according to claim 3 is characterized in that described catalyzer is sulfuric acid, tosic acid or sal enixum.
5, the method for preparing the amyl acetate fatty alcohol according to claim 1, it is characterized in that described Fatty Alcohol(C12-C14 and C12-C18) and ritalin feed intake with following mol ratio carries out transesterification reaction:
Fatty Alcohol(C12-C14 and C12-C18): ritalin=1: 1.1～1: 3.5.
6, the method for preparing the amyl acetate fatty alcohol according to claim 5, it is characterized in that described Fatty Alcohol(C12-C14 and C12-C18) and ritalin feed intake with following mol ratio carries out transesterification reaction:
Fatty Alcohol(C12-C14 and C12-C18): ritalin=1: 1.5～1: 1.9.
7, the method for preparing the amyl acetate fatty alcohol according to claim 1, it is characterized in that described Fatty Alcohol(C12-C14 and C12-C18) and ritalin feed intake with following mol ratio carries out transesterification reaction:
Fatty Alcohol(C12-C14 and C12-C18): ritalin=1.1: 1～3.0: 1.
8, the method for preparing the amyl acetate fatty alcohol according to claim 7, it is characterized in that described Fatty Alcohol(C12-C14 and C12-C18) and ritalin feed intake with following mol ratio carries out transesterification reaction:
Fatty Alcohol(C12-C14 and C12-C18): ritalin=1.5: 1～1.9: 1.
9, the method for preparing the amyl acetate fatty alcohol according to claim 1, the method that the vapor feed that it is characterized in that described reaction system separate to be removed methyl ester removal is: after the vapor feed condensation be 5～20% CuSO with water, dimethyl formamide, concentration expressed in percentage by weight
4The aqueous solution, concentration expressed in percentage by weight are that 10～30% the NaCl aqueous solution or the saturated NaCl aqueous solution are that extraction agent carries out extracting and separating, extraction temperature is 10～40 ℃, the consumption of extraction agent is that the weight ratio of extraction agent and raw material ritalin amount is 1: 1～2: 1, and solvent phase is rich in methyl alcohol.
10, the method for preparing the amyl acetate fatty alcohol according to claim 9 is characterized in that after the described vapor feed condensation with the saturated NaCl aqueous solution being that extraction agent carries out extracting and separating.
11, the method for preparing the amyl acetate fatty alcohol according to claim 1, the vapor feed that it is characterized in that described reaction system is separated the method remove methyl alcohol and is: vapor feed is that extraction agent carries out extracting rectifying with water, the tower top temperature of extractive distillation column is 50～70 ℃, tower still temperature is 80～100 ℃, the input material volume ratio of material and water is 1: 1～3: 1, reflux ratio is 0.2～0.75, working pressure is normal pressure～0.4MPa, stage number is 25～36, tower still material is rich in methyl alcohol, returns the transesterification reaction system after being rich in the cat head material condensation of ritalin.
12, according to claim 1,2,3,4,5,6,7,8,9, the 10 or 11 described methods that prepare the amyl acetate fatty alcohol, it is characterized in that described ritalin raw material for prepared the mixture that is rich in ritalin of by-product in the polyvinyl alcohol process by Vinyl Acetate Copolymer and methyl alcohol alcoholysis, wherein the content of ritalin is 60～85%.
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| CN1304358C (en) * | 2005-04-22 | 2007-03-14 | 清华大学 | Method for preparing high pure methyl acetate through adsorption of liquid phase |
| CN101759561A (en) * | 2009-12-31 | 2010-06-30 | 浙江理工大学 | Preparation method of aryl a-keto esters |
| CN104710306A (en) * | 2015-01-12 | 2015-06-17 | 吉林化工学院 | Method for preparing acetate through ester interchange-adsorption ethanol removal combined technology |
| CN104945251A (en) * | 2015-07-08 | 2015-09-30 | 常州大学 | Method for preparing isopropyl acetate through rectification |
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2002
- 2002-07-15 CN CN 02136050 patent/CN1242980C/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1304358C (en) * | 2005-04-22 | 2007-03-14 | 清华大学 | Method for preparing high pure methyl acetate through adsorption of liquid phase |
| CN101759561A (en) * | 2009-12-31 | 2010-06-30 | 浙江理工大学 | Preparation method of aryl a-keto esters |
| CN104710306A (en) * | 2015-01-12 | 2015-06-17 | 吉林化工学院 | Method for preparing acetate through ester interchange-adsorption ethanol removal combined technology |
| CN104945251A (en) * | 2015-07-08 | 2015-09-30 | 常州大学 | Method for preparing isopropyl acetate through rectification |
| CN105017019A (en) * | 2015-07-08 | 2015-11-04 | 常州大学 | Energy-saving method for preparing isopropyl acetate |
| CN107759473A (en) * | 2017-10-23 | 2018-03-06 | 江苏馨瑞香料有限公司 | A kind of green synthesis method of allyl cyclohexyl propionate |
| CN110743372A (en) * | 2019-11-27 | 2020-02-04 | 南京九思高科技有限公司 | Device and process for preparing methanol and butyl acetate |
| CN116351470A (en) * | 2023-03-03 | 2023-06-30 | 沈阳化工大学 | Preparation method of heterogeneous catalyst for transesterification reaction |
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