CN102807500A - Method for liquid-phase preparation of N, N-dimethylacetamide - Google Patents
Method for liquid-phase preparation of N, N-dimethylacetamide Download PDFInfo
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- CN102807500A CN102807500A CN2012102860592A CN201210286059A CN102807500A CN 102807500 A CN102807500 A CN 102807500A CN 2012102860592 A CN2012102860592 A CN 2012102860592A CN 201210286059 A CN201210286059 A CN 201210286059A CN 102807500 A CN102807500 A CN 102807500A
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Abstract
The invention discloses a method for liquid-phase preparation of N, N-dimethylacetamide. The method includes adding methyl acetate, dimethylamine, carbinol and catalyst into a reactor for reaction at a certain temperature and pressure; subjecting liquid-phase mixture reacted to removing the dimethylamine, the methyl acetate, carbinol and water by crude distillation and then depressurizing and rectifying in a rectifying tower, and obtaining N, N-dimethylacetamide with purity higher than 99.9% by rectifying. By the aid of the method, defects of serious corrosion of acetic acid to equipment, high cost of raw materials, low transformation rate and selectivity and the like in the prior synthetizing art are overcome, and the method has excellent industrial application prospect.
Description
Technical field
The invention belongs to organic synthesis technology, particularly the DMAC N,N synthesis technical field.
Background technology
DMAC N,N is a kind of colourless transparent liquid, and low toxicity is arranged, and can dissolve multiple mineral compound, can be miscible with water, alcohol, ether, ester and aromatics.Under the condition of anhydrous, acid or alkali, has good stability.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 (like terephthalic acid).Also can in some organic reaction, make catalyzer.Compare with homologous N, its thermostability, stability to hydrolysis height, corrodibility and toxicity are little.Traditional synthetic DMAC N,N technology mainly comprises: DMAC N,N is produced in (1) acetonitrile and methyl alcohol reaction; (2) the synthetic DMAC N,N of Trimethylamine 99 and CO carbonylation reaction; (3) the synthetic DMAC N,N of ketene and n n dimetylaniline; (4) N-methylacetamide and methyl alcohol, the synthetic DMAC N,N of pyridine etc.More than exist in several kinds of compound method processes acetate to shortcomings such as corrosion on Equipment are comparatively serious, toxicity is big, raw materials cost is high and transformation efficiency and selectivity be lower.
Summary of the invention
In view of existing N; The above shortcoming of N-N,N-DIMETHYLACETAMIDE synthesis technology; The object of the present invention is to provide a kind of methyl acetate and n n dimetylaniline liquid phase reaction to make N; The new process of N-N,N-DIMETHYLACETAMIDE makes it to overcome acetate that existing synthetic technology exists to shortcomings such as corrosion on Equipment are comparatively serious, toxicity is big, raw materials cost is high and transformation efficiency and selectivity be lower.
In order to realize the foregoing invention purpose, the present invention adopts following technical proposals:
A kind of method of liquid phase production DMAC N,N may further comprise the steps:
A) a certain amount of methyl acetate, n n dimetylaniline, methyl alcohol and catalyzer are joined in the reaction kettle, the water cut of wherein said methyl acetate is less than or equal to 1.5%, and n n dimetylaniline purity is more than or equal to 99.5%, and the mass ratio of methyl alcohol and methyl acetate is 0.5:1 ~ 5:1; Said catalyzer is one or both a mixture of molybdic oxide and sodium metavanadate;
B) reacted liquid phase mixture carries out rectification under vacuum through slightly heating up in a steamer after removing n n dimetylaniline, methyl acetate, first alcohol and water again in rectifying tower; Obtain purity greater than 99.9% N through rectifying; The N-N,N-DIMETHYLACETAMIDE returns reaction kettle and recycles through slightly heating up in a steamer the excessive n n dimetylaniline, methyl acetate and the part methyl alcohol that remove;
C) in rectifying; Return a certain amount of N continuously from the tower still; The mixed solution of N-N,N-DIMETHYLACETAMIDE, acetate and catalyzer is realized recycling of catalyzer to reaction kettle, the quality of returning the mixed solution of reaction kettle be in the tower still mixed solution total amount 10% ~ 30%.
In the above-mentioned method for preparing DMAC N,N, the mass ratio of catalyzer and methyl acetate is 0.01:1 ~ 0.5:1 in the step a), is preferably 0.02:1 ~ 0.25:1;
In the above-mentioned method for preparing DMAC N,N, the temperature of reaction of step a) is 60 ℃ ~ 170 ℃, is preferably 100 ℃ ~ 160 ℃;
In the above-mentioned method for preparing DMAC N,N, the reaction pressure of step a) is 0.3 MPa ~ 2.0MPa, is preferably 0.8 MPa ~ 1.8MPa;
In the above-mentioned method for preparing DMAC N,N, the weight ratio of methyl alcohol and methyl acetate is preferably 1:1 ~ 3:1 in the step a);
In the above-mentioned method for preparing DMAC N,N, step c) also is included in adds a certain amount of catalyzer as replenishing in the mixed solution that returns reaction kettle;
In the above-mentioned method for preparing DMAC N,N, catalyzer is one or both mixtures of molybdic oxide and sodium metavanadate;
In the above-mentioned method for preparing DMAC N,N, the catalyzer of adding in the step c) and the mass ratio of methyl acetate are 0.001:1 ~ 0.005:1, preferred 0.002:1 ~ 0.004:1;
In the above-mentioned method for preparing DMAC N,N, the quality of the mixed solution that returns in the step c) is the 15%-25% of mixed solution total amount in the tower still.
In the above-mentioned method for preparing DMAC N,N, n n dimetylaniline is excessive with respect to another reactant methyl acetate in the step a); The excessive 10%-20% of mole number of preferred n n dimetylaniline, raw acetic acid methyl esters water cut refers to the shared mass percent of moisture in the aqueous methyl acetate; The purity of n n dimetylaniline is meant the mass percent that pure n n dimetylaniline is shared;
Methyl acetate and n n dimetylaniline liquid phase reaction make the DMAC N,N process method, mainly may further comprise the steps:
(1) proportionally a certain amount of methyl acetate, n n dimetylaniline, methyl alcohol and catalyzer are joined in the reaction kettle, be reflected at and carry out in the autoclave, reaction kettle is furnished with off-set facility such as conventional whisking appliance and heating unit; In employing molybdic oxide and the inclined to one side sodium vanadate one or both are as catalysts, and the catalyzer that adds for the first time and the mass ratio of methyl acetate are 0.01:1 ~ 0.5:1;
(2) after the adding of reaction mass and catalyzer finishes in the step (1); Reaction kettle begins heating then; Adopt the excessive 10%-20% of n n dimetylaniline (mol ratio), system boosts voluntarily or make to reach in the reaction kettle with the mode of nitrogen pressure and need pressure condition; Synthesis reaction temperature is 60-170 ℃, and building-up reactions pressure is 0.3 MPa-2.0MPa; The mass ratio of auxiliary agent methyl alcohol and methyl acetate is 0.5:1 ~ 5:1;
(3) the reaction solution material after reaction is accomplished in the step (2) slightly heats up in a steamer in rectifying tower, adopts the glass spring filler, cat head extraction mouth under the overhead condenser, and tower is provided with side line extraction mouth, the heating of tower still electricity consumption heating jacket, charging in the tower, operate continuously; Slightly heat up in a steamer earlier n n dimetylaniline and the methyl-formiate that does not react completely on a small quantity, extraction methyl alcohol in the tower that the cat head extraction is excessive; Through vacuumizing rectification under vacuum, cat head extraction small amount of methanol and water, tower still obtain the thick product of the higher DMAC N,N of purity again;
(4) rectifying Tata still returns a certain amount of mixed solution that comprises DMAC N,N and catalyzer and acetate continuously to reaction kettle in the step (3), the quality of returning the mixed solution of reaction kettle be in the tower still mixed solution total amount 10% ~ 30%.
(5) in step (4), return in the mixture and to add a certain amount of catalyzer as replenishing, the catalyzer of adding and the mass ratio of methyl acetate are: 0.001:1 ~ 0.005:1.
Compare with existing DMAC N,N synthesis technology, the present invention has the advantage of being described below:
(1) among the present invention in the reaction process raw material methyl acetate allow the existence of a large amount of methyl alcohol, the requirement to the raw acetic acid methyl esters lower, methyl acetate need not to carry out purification process and promptly can be used for reaction process;
(2) adopt as above method after, a large amount of existence of methyl alcohol reduce the methyl acetate hydrolysis reaction conversion ratio, more important be can the check hydrolysis reaction generation, the generation of acetate is seldom in the reaction process.Because acetate and DMAC N,N can form azeotrope, a large amount of existence of acetate can cause the effect of rectifying to reduce greatly, cause energy consumption too high, and the existence of acetate simultaneously causes equipment corrosion serious, poor product quality.Adopt method of the present invention can synthesize high-quality DMAC N,N, product DMAC N,N purity can reach more than 99.8%, and the recovery per pass of product can reach more than 92%;
(3) technological process among the present invention has reduced the amination reaction temperature, temperature of reaction under 60 ℃-170 ℃ condition, the transformation efficiency of methyl acetate and N; The selectivity of N-N,N-DIMETHYLACETAMIDE is higher; The methyl acetate transformation efficiency can reach 100%, and the DMAC N,N selectivity is higher than 96%;
(4) catalyzer is higher relatively with respect to traditional sodium methylate and other basic catalyst productive rates among the present invention, and has shortened the reaction times, and catalyst stability is good, the product separate easily, and catalyzer can the cycle repeats utilization;
(5) N of the present invention; In the process of N-N,N-DIMETHYLACETAMIDE rectifying; Return a certain amount of N from the tower still; N-N,N-DIMETHYLACETAMIDE, acetate and mixture of catalysts are to reaction kettle, and catalyzer and acetate are dissolved state with a kind of form of acetate, and this dissolved state makes that catalyzer disperses more evenly, catalytic effect is more obvious.
(6) realized the operate continuously of reaction and rectifying separation process; Particularly reduced the catalyst recovery process that original catalyzer cools off, separates out, filters, dries and calcining etc. is complicated; Thereby reduced catalyzer loss, reduced the energy consumption of reaction and rectifying separation process, the throughput that has finally reduced production cost of products and increased device.
Embodiment
Below in conjunction with embodiment the present invention is made further detailed description.But should this be interpreted as that the scope of the above-mentioned theme of the present invention only limits to following embodiment, allly all belong to scope of the present invention based on the technology that content of the present invention realized.
Reaction is all carried out in autoclave in following examples, and reaction kettle has stirring and electric heater unit.Add earlier quantitative raw acetic acid methyl esters and methyl alcohol, catalyzer, add quantitative n n dimetylaniline post-heating intensification gradually, reach timing sampling behind the reaction conditions, with the variation of gas chromatographic detection reactant.
Embodiment 1:
Reaction adds materials and is primary catalyst molybdic oxide 12g, methyl acetate 336g (water cut≤1.5%), methyl alcohol 336g; N n dimetylaniline 240g (purity>=99.5%), reaction kettle natural pressure 1.2MPa, 150 ℃ of temperature of reaction; Pressure rises to 1.5MPa, stirring reaction 4 hours, the transformation efficiency 100% of methyl acetate; The selectivity of DMAC N,N>=99.2%.
Reaction product contains n n dimetylaniline 3.64%, methyl alcohol 62.92%, N; N-N,N-DIMETHYLACETAMIDE 33.20%, the material of acetate 0.24% (weight percent) slightly heats up in a steamer and distillation operation glass spring packed height 1500mm in the rectifying tower respectively in the rectifying tower of the identical Φ 40mm of two structures; 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.Take out normal pressure earlier and slightly heat up in a steamer, n n dimetylaniline and the methyl-formiate that does not react completely on a small quantity that the cat head extraction is excessive, extraction methyl alcohol in the tower is back to respectively and proceeds reaction in the reaction kettle.Crude distillation column liquid gets into rectifying tower and carries out rectification under vacuum, and gauge pressure is-0.085Mpa cat head extraction small amount of methanol; The DMAC N,N mixed solution of continuous discharge 20% is added molybdenum trioxide catalyst 0.8g at the bottom of the rectifying tower still; After pump boosts, get into reaction kettle together and proceed reaction; Obtain DMAC N,N purity in the tower greater than 99.8%, the recovery per pass 92.5% of product.
Embodiment 2:
Reaction adds materials and is the inclined to one side sodium vanadate 12g of primary catalyst, methyl acetate 336g (water cut≤1.5%), methyl alcohol 600g; N n dimetylaniline 250g (purity>=99.5%), 165 ℃ of temperature of reaction are reacted and are natural pressure 1.6MPa; Stirring reaction 3.5 hours; The transformation efficiency 100% of methyl acetate, the selectivity 96.80% of DMAC N,N.
Reaction product contains n n dimetylaniline 2.6%, methyl alcohol 73.49%, N; N-N,N-DIMETHYLACETAMIDE 23.74%, the material of acetate 0.17% (weight percent) slightly heats up in a steamer and distillation operation glass spring packed height 1500mm in the rectifying tower respectively in the rectifying tower of the identical Φ 40mm of two structures; 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.Take out normal pressure earlier and slightly heat up in a steamer, n n dimetylaniline and the methyl-formiate that does not react completely on a small quantity that the cat head extraction is excessive, extraction methyl alcohol in the tower is back to respectively and proceeds reaction in the reaction kettle.Crude distillation column liquid gets into rectifying tower and carries out rectification under vacuum, and gauge pressure is-0.085Mpa cat head extraction small amount of methanol; The DMAC N,N mixed solution of continuous discharge 20% is added inclined to one side sodium vanadate catalyzer 1.2g at the bottom of the rectifying tower still; After pump boosts, get into reaction kettle together and proceed reaction; Obtain DMAC N,N purity in the tower greater than 99.9%, the recovery per pass 92% of product.
Embodiment 3:
Reaction adds materials and is molybdic oxide 6g, sodium vanadate 6g partially, methyl acetate 336g (water cut≤1.5%); Methyl alcohol 800g, n n dimetylaniline 220g (purity>=99.5%), 160 ℃ of temperature of reaction; Reaction is natural pressure 1.5MPa, stirring reaction 4 hours, the transformation efficiency 100% of methyl acetate; The selectivity of DMAC N,N>=98%.
Reaction product contains n n dimetylaniline 2.14%, methyl alcohol 78.20%, N; N-N,N-DIMETHYLACETAMIDE 19.53%, the material of acetate 0.13% (weight percent) slightly heats up in a steamer and distillation operation glass spring packed height 1500mm in the rectifying tower respectively in the rectifying tower of the identical Φ 40mm of two structures; 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 normal pressure slightly heats up in a steamer, n n dimetylaniline and the methyl-formiate that does not react completely on a small quantity that the cat head extraction is excessive, and extraction methyl alcohol in the tower is back to respectively and proceeds reaction in the reaction kettle.Crude distillation column liquid gets into rectifying tower and carries out rectification under vacuum, and gauge pressure is-0.085MPa cat head extraction small amount of methanol; The DMAC N,N mixed solution of continuous discharge 20% at the bottom of the rectifying tower still is added molybdic oxide and inclined to one side each 0.3g of sodium vanadate catalyzer; After pump boosts, get into reaction kettle together and proceed reaction; Obtain DMAC N,N purity in the tower greater than 99.9%, the recovery per pass 92% of product.
Claims (10)
1. the method for a liquid phase production DMAC N,N is characterized in that may further comprise the steps:
A) a certain amount of methyl acetate, n n dimetylaniline, methyl alcohol and catalyzer are joined in the reaction kettle; The water cut of wherein said methyl acetate is less than or equal to 1.5%; N n dimetylaniline purity is more than or equal to 99.5%, and the mass ratio of methyl alcohol and methyl acetate is 0.5: 1～5: 1; Said catalyzer is one or both a mixture of molybdic oxide and sodium metavanadate;
B) reacted liquid phase mixture carries out rectification under vacuum through slightly heating up in a steamer after removing n n dimetylaniline, methyl acetate, first alcohol and water again in rectifying tower; Obtain purity greater than 99.9% N through rectifying; The N-N,N-DIMETHYLACETAMIDE returns reaction kettle and recycles through slightly heating up in a steamer the excessive n n dimetylaniline, methyl acetate and the part methyl alcohol that remove;
C) in rectifying; Return a certain amount of N continuously from the tower still; The mixed solution of N-N,N-DIMETHYLACETAMIDE, a spot of acetate (side reaction generation) and catalyzer is to reaction kettle; Realize recycling of catalyzer, the quality of returning the mixed solution of reaction kettle be in the tower still mixed solution total amount 10%～30%.
2. a kind of according to claim 1 liquid phase production N; The method of N-N,N-DIMETHYLACETAMIDE; It is characterized in that step c) also is included in the mixed solution that returns reaction kettle adds a certain amount of catalyzer as replenishing, and said catalyzer is one or both a mixture of molybdic oxide and sodium metavanadate.
3. like the said a kind of liquid phase production N of claim 2; The method of N-N,N-DIMETHYLACETAMIDE; It is characterized in that the mass ratio of catalyzer and methyl acetate is 0.01: 1～0.5: 1 in the step a), the catalyzer of adding in the step c) and the mass ratio of methyl acetate are 0.001: 1～0.005: 1.
4. like the method for the said a kind of liquid phase production DMAC N,N of arbitrary claim among the claim 1-3, it is characterized in that temperature of reaction is 60 ℃～170 ℃ in the step a), reaction pressure is 0.3 MPa～2.0MPa.
5. the method for a kind of liquid phase production DMAC N,N as claimed in claim 4, the weight ratio that it is characterized in that methyl alcohol and methyl acetate is 1: 1～3: 1.
6. the method for a kind of liquid phase production DMAC N,N as claimed in claim 4 is characterized in that temperature of reaction is 100 ℃～160 ℃ in the step a).
7. the method for a kind of liquid phase production DMAC N,N as claimed in claim 4 is characterized in that reaction pressure is 0.8 MPa～1.8MPa in the step a).
8. the method for a kind of liquid phase production DMAC N,N as claimed in claim 4 is characterized in that the catalyzer of step a) adding and the mass ratio of methyl acetate are 0.02: 1～0.25: 1.
9. the method for a kind of liquid phase production DMAC N,N as claimed in claim 4 is characterized in that the catalyzer of step c) adding and the mass ratio of methyl acetate are 0.002: 1～0.004: 1.
10. the method for a kind of liquid phase production DMAC N,N as claimed in claim 4, the quality of the mixed solution that returns in the step c) are the 15%-25% of mixed solution total amount in the tower still.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104981453A (en) * | 2012-12-19 | 2015-10-14 | 巴斯夫欧洲公司 | Continuous method for separating salts in the production of dimethylacetamide |
| CN107011198A (en) * | 2017-03-30 | 2017-08-04 | 南通沃兰化工有限公司 | One kind synthesis N, the technique of N dimethyl acetamides |
| CN110156621A (en) * | 2019-05-08 | 2019-08-23 | 重庆建峰工业集团有限公司 | The method of liquid-liquid Homogeneous synthesis DMAC N,N' dimethyl acetamide is carried out in micro passage reaction |
| CN111253277A (en) * | 2020-03-31 | 2020-06-09 | 迈奇化学股份有限公司 | Production method of N, N-diethyl acetamide |
| CN112521301A (en) * | 2020-12-21 | 2021-03-19 | 安徽金禾实业股份有限公司 | Synthesis device and synthesis method of DMAC (dimethylacetamide) |
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| CN1807401A (en) * | 2005-12-29 | 2006-07-26 | 西南化工研究设计院 | Process for synthesizing dimethylacetamide by ethyl acetate and dimethylamine |
| CN1884255A (en) * | 2005-06-20 | 2006-12-27 | 上海经纬化工有限公司 | Process for producing N,N-dimethyl acetamide |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104981453A (en) * | 2012-12-19 | 2015-10-14 | 巴斯夫欧洲公司 | Continuous method for separating salts in the production of dimethylacetamide |
| CN107011198A (en) * | 2017-03-30 | 2017-08-04 | 南通沃兰化工有限公司 | One kind synthesis N, the technique of N dimethyl acetamides |
| CN107011198B (en) * | 2017-03-30 | 2019-03-05 | 南通沃兰化工有限公司 | A kind of technique synthesizing n,N-dimethylacetamide |
| CN110156621A (en) * | 2019-05-08 | 2019-08-23 | 重庆建峰工业集团有限公司 | The method of liquid-liquid Homogeneous synthesis DMAC N,N' dimethyl acetamide is carried out in micro passage reaction |
| CN111253277A (en) * | 2020-03-31 | 2020-06-09 | 迈奇化学股份有限公司 | Production method of N, N-diethyl acetamide |
| CN112521301A (en) * | 2020-12-21 | 2021-03-19 | 安徽金禾实业股份有限公司 | Synthesis device and synthesis method of DMAC (dimethylacetamide) |
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