CN1325467C - Technological process of synthesizing dimethyl acetylamide with methyl acetate and dimethylamine - Google Patents
Technological process of synthesizing dimethyl acetylamide with methyl acetate and dimethylamine Download PDFInfo
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- CN1325467C CN1325467C CNB2004100405358A CN200410040535A CN1325467C CN 1325467 C CN1325467 C CN 1325467C CN B2004100405358 A CNB2004100405358 A CN B2004100405358A CN 200410040535 A CN200410040535 A CN 200410040535A CN 1325467 C CN1325467 C CN 1325467C
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- methyl acetate
- dimethylamine
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- dimethylacetamide
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Abstract
The present invention discloses a technological method for synthesizing dimethyl acetylamide by methyl acetate and dimethylamine. Dimethyl acetamide is prepared from methyl acetate and dimethylamine which serve as raw materials at the certain temperature and pressure, and the molar ratio of the methyl acetate to the dimethylamine is from 1: 0.8 to 1:2. Methanol serves as a reaction auxiliary agent. A synthesized reaction catalyst at least contains one of the following substances: molybdenum trioxide (a) and sodium metavanadate (b). The technological process has the advantage that the corrosion of acetic acid on devices is reduced; the reaction temperature is reduced; the conversion rate and the selectivity of positive reaction are enhanced; the catalyst productivity is high; the reaction time is shortened; the stability is good; the product is easy to separate; and the catalyst can be circularly and repetitively utilized.
Description
The invention belongs to organic synthesis technology, especially the N,N-DIMETHYLACETAMIDE synthesis technical field.
[technical background of invention]
N,N-DIMETHYLACETAMIDE is a colourless transparent liquid, and low toxicity is arranged, and can dissolve multiple mineral compound, can be miscible with water, alcohol, ether, ester and aromatic substance.Under the condition of anhydrous, acid or alkali, good stability is arranged.Be the good polar solvent of synthesis of natural resin, be used for the synthetic of polyimide, polysulfonamides and other macromolecular compounds, also be used for the film forming and the spinning of synthetic resins, the crystallization and purification of synthetic drugs, aromatic dicarboxylic acid (as terephthalic acid).Also can in some organic reaction, make catalyzer.Compare with homologous dimethyl formamide, its thermostability, stability to hydrolysis height, corrodibility and toxicity are little.Synthesization of dimethyl ethanamide technology acetate is to the seriously corroded of equipment at present, and transformation efficiency and selectivity are lower.
In view of the above shortcoming of prior art, the objective of the invention is to study the new process that a kind of methyl acetate and dimethylamine liquid phase reaction make N,N-DIMETHYLACETAMIDE, make it to overcome the above shortcoming of prior art.
Purpose of the present invention makes and realizes by following method.
[summary of the invention]
Methyl acetate and dimethylamine liquid phase reaction make the N,N-DIMETHYLACETAMIDE processing method, are raw material system N,N-DIMETHYLACETAMIDE with methyl acetate and dimethylamine, it is characterized in that, make reaction promoter with methyl alcohol; And contain a kind of of following material in the synthetic catalysts at least: a) molybdic oxide; B) inclined to one side sodium vanadate.
After adopting method as above, technological process reduced acetate to transformation efficiency and the selectivity that the burn into of device has reduced temperature of reaction, positive reaction improve, the catalyst production height, the reaction times shortens, good stability, the recycling that can circulate of product separate easily, catalyzer.Product N,N-DIMETHYLACETAMIDE purity can reach more than 99.5%, and the methyl acetate transformation efficiency can reach 100%, and the N,N-DIMETHYLACETAMIDE selectivity is higher than 96%.Reaction product removes excessive dimethylamine and methyl alcohol, rectifying obtain product (purity is greater than 99.5%) N,N-DIMETHYLACETAMIDE through distillation, and the recovery per pass of product can reach more than 92%.
Be reflected at and carry out in the autoclave, reactor is furnished with off-set facility such as conventional agitator and electric heater unit.Methyl acetate and dimethylamine mol ratio are joined in the reactor at methyl acetate, methyl alcohol and the catalyzer of 1: 0.8～2 proportionings (optimum mole ratio is 1: 1～1.5), after adding dimethylamine, reactor begins heating, adopt that dimethylamine is excessive, system boosts voluntarily or make to reach and need pressure condition, 120～190 ℃ of synthesis reaction temperatures with nitrogen pressure; Building-up reactions pressure 0.8～2.5Mpa.Auxiliary agent methyl alcohol, its consumption mol ratio is a methyl acetate: methyl alcohol is mole 1: 0.3～0.5.
Use special-purpose catalyst as at least a in molybdic oxide and the inclined to one side sodium vanadate in the described processing method of this patent, the mass ratio of catalyzer is a methyl acetate: catalyzer is 1: 0.0 1～0.10.The catalyst consumption optimum quality ratio is a methyl acetate: catalyzer is 1: 0.02～0.05.
[concrete implementation method]
Reaction is all carried out in autoclave in following examples, and reactor has stirring and electric heater unit.Add earlier quantitative raw acetic acid methyl esters and methyl alcohol, catalyzer, add quantitative dimethylamine post-heating gradually and heat up, reach timing sampling behind the reaction conditions, with the variation of gas chromatographic detection reactant.
Embodiment 1:
Molybdic oxide is made catalyzer: molybdic oxide 6g, methyl acetate 336g, methyl alcohol 65g, dimethylamine 250g, reaction is natural pressure 2.0Mpa, 172 ℃ of temperature of reaction, and pressure rises to 2.25Mpa, stirring reaction 4 hours, the transformation efficiency 100% of methyl acetate, the selectivity of N,N-DIMETHYLACETAMIDE 〉=99%.
Embodiment 2:
Sodium vanadate is made catalyzer partially: inclined to one side sodium vanadate 6g, methyl acetate 336g, methyl alcohol 65g, dimethylamine 250g, 170 ℃ of temperature of reaction are reacted and are natural pressure 2.0Mpa, stirring reaction 3.5 hours, the transformation efficiency 100% of methyl acetate, the selectivity 96.84% of N,N-DIMETHYLACETAMIDE.
Embodiment 3:
Molybdic oxide and inclined to one side sodium vanadate composite catalyst: molybdic oxide 3g, inclined to one side sodium vanadate 3g, methyl acetate 336g, methyl alcohol 65g, dimethylamine 250g, 170 ℃ of temperature of reaction, reaction is natural pressure 2.0Mpa, stirring reaction 4 hours, the transformation efficiency 100% of methyl acetate, the selectivity of N,N-DIMETHYLACETAMIDE 〉=98%.
Embodiment 4:
Reaction product contains dimethylamine 8.58%, methyl alcohol 31.74%, N,N-DIMETHYLACETAMIDE 59.34%, the rectifying in the glass tower of φ 40mm of the material of acetate 0.28% (weight percent), glass spring packed height 1500mm, cat head extraction mouth under the overhead condenser, the 500mm place is provided with side line extraction mouth on the tower, the heating of tower still electricity consumption heating jacket, 500mm place charging under the tower, operate continuously.Elder generation's atmospheric distillation, dimethylamine that the cat head extraction is excessive and the methyl-formiate that does not react completely on a small quantity, extraction methyl alcohol in the tower.Through rectification under vacuum, cat head extraction small amount of methanol obtains N,N-DIMETHYLACETAMIDE purity greater than 99.5% in the tower again, and the recovery per pass of product is more than 92%.
Claims (4)
1, methyl acetate and dimethylamine liquid phase reaction make the N,N-DIMETHYLACETAMIDE processing method, are that raw material is made N,N-DIMETHYLACETAMIDE under certain temperature and pressure with methyl acetate and dimethylamine, and methyl acetate and dimethylamine mol ratio are 1: 0.8～2; Methyl alcohol is made reaction promoter, and its consumption mol ratio methyl acetate: methyl alcohol is 1: 0.3～0.5; At least contain a kind of of following material in the synthetic catalysts: a) molybdic oxide; B) inclined to one side sodium vanadate; 120～190 ℃ of synthesis reaction temperatures, the quality of catalyzer are than methyl acetate: catalyzer is 1: 0.01～0.10; Building-up reactions pressure 0.8～2.5Mpa.
2, make the N,N-DIMETHYLACETAMIDE processing method according to claim 1 described methyl acetate and dimethylamine liquid phase reaction, the mol ratio of methyl acetate and dimethylamine is 1: 1～1.5.
3, make the N,N-DIMETHYLACETAMIDE processing method according to claim 1 described methyl acetate and dimethylamine liquid phase reaction, the catalyst consumption quality is than methyl acetate: catalyzer is 1: 0.02～0.05.
4, make the N,N-DIMETHYLACETAMIDE processing method according to claim 1 described methyl acetate and dimethylamine liquid phase reaction, reaction product removes excessive dimethylamine, methyl acetate and part methyl alcohol Returning reacting system and recycles through slightly heating up in a steamer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100405358A CN1325467C (en) | 2004-08-26 | 2004-08-26 | Technological process of synthesizing dimethyl acetylamide with methyl acetate and dimethylamine |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100405358A CN1325467C (en) | 2004-08-26 | 2004-08-26 | Technological process of synthesizing dimethyl acetylamide with methyl acetate and dimethylamine |
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| CN1740144A CN1740144A (en) | 2006-03-01 |
| CN1325467C true CN1325467C (en) | 2007-07-11 |
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| CNB2004100405358A Expired - Fee Related CN1325467C (en) | 2004-08-26 | 2004-08-26 | Technological process of synthesizing dimethyl acetylamide with methyl acetate and dimethylamine |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102807500B (en) * | 2012-08-13 | 2014-04-23 | 西南化工研究设计院有限公司 | Method for liquid-phase preparation of N, N-dimethylacetamide |
| CN113856607B (en) * | 2021-10-21 | 2023-03-28 | 聊城鲁西甲胺化工有限公司 | DMAC (dimethyl acetamide) reaction device for thermal condensation of dimethylamine and acetic acid and application method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4258200A (en) * | 1980-03-11 | 1981-03-24 | Air Products And Chemicals, Inc. | Production of carboxylic acid amides and carbamates using cobalt catalysts |
| CN1298382A (en) * | 1998-04-20 | 2001-06-06 | 三菱丽阳株式会社 | Process for producing dimethylacetamide |
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- 2004-08-26 CN CNB2004100405358A patent/CN1325467C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4258200A (en) * | 1980-03-11 | 1981-03-24 | Air Products And Chemicals, Inc. | Production of carboxylic acid amides and carbamates using cobalt catalysts |
| CN1298382A (en) * | 1998-04-20 | 2001-06-06 | 三菱丽阳株式会社 | Process for producing dimethylacetamide |
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