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Synthesis method of N-vinylformamide

A technology of vinylformamide and hydroxyethylformamide, which is applied in the field of synthesis of N-vinylformamide, can solve the problems of large amount of acid-base wastewater, cumbersome reaction steps, serious side reactions, etc., and achieve simple separation and purification, The effect of simple reaction steps and low synthesis cost

Inactive Publication Date: 2019-06-21
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The highly toxic substance HCN is produced in the above method a; the formamide to be removed in c is close to the boiling point of the product NVF, and it is not easy to separate; the b scheme is patented by Mitsubishi Corporation, which is the main method for producing NVF at present, but there is acid-base wastewater in this method A large amount, complicated reaction steps, low yield, etc.
In short, in the current production technology, the synthesis of NVF has many reaction steps, serious side reactions, difficult separation, and high synthesis cost.

Method used

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  • Synthesis method of N-vinylformamide
  • Synthesis method of N-vinylformamide
  • Synthesis method of N-vinylformamide

Examples

Experimental program
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Effect test

Embodiment 1

[0050] (1) Distilled acetaldehyde

[0051] Take 100ml of acetaldehyde in a round bottom flask, add a few drops of concentrated sulfuric acid, and distill at 60°C for 3 hours.

[0052] (2) Synthetic N-a hydroxyethyl formamide

[0053] Take 26.4g (0.6mol) of distilled acetaldehyde and put it into a constant pressure funnel, take 22.5g (0.5mol) of formamide and put it into a four-necked flask, add a reflux condenser, a thermometer, and a constant pressure Funnel, and add 0.6g catalyst anhydrous potassium carbonate, react 70min at 45 ℃, obtain N-a hydroxyethyl formamide, and carry out infrared analysis to it, the result is as follows Figure 8 shown.

[0054] (3) Synthetic reactant intermediate

[0055] 20 g of N-a ethyl formamide obtained in step (2) was reacted with 85.5 g of alkenyl succinic anhydride (R=16) in a four-necked flask at 70° C. for 2.0 h.

[0056] (4) Use a high temperature cracking furnace to crack the reaction intermediate

[0057] Put the obtained polymer i...

Embodiment 2

[0060] The 250ml four-necked flask is equipped with stirrer, reflux condenser, thermometer and constant pressure funnel, adds 22.5g formamide (0.5mol) and 0.6g anhydrous potassium carbonate in the four-necked flask, adds 26.4g (0.6 mol) in the constant pressure funnel mol) distilled acetaldehyde (purity>95%), the temperature was maintained at 45°C and the acetaldehyde was slowly added dropwise for 70min. After rising to room temperature, 52.5 g (0.25 mol) of octenyl succinic anhydride was added, and the temperature was raised to 70° C. for 3.0 h. Put the obtained reactant intermediate into a magnetic cup and put it into a tube furnace. Adjust the temperature of the tube furnace to 150°C and react for 2.0 hours. When the temperature of the tube furnace cools down to room temperature, collect the resulting Liquid, the obtained product was put into a rotary evaporator and evaporated at 120°C, and the obtained liquid was N-vinylformamide. The NVF yield of the product is 58.6%, an...

Embodiment 3

[0062] The 250ml four-necked flask is equipped with stirrer, reflux condenser, thermometer and constant pressure funnel, adds 22.5g formamide (0.5mol) and 0.6g anhydrous potassium carbonate in the four-necked flask, adds 26.4g (0.6 mol) in the constant pressure funnel mol) distilled acetaldehyde (purity>95%), the temperature was maintained at 45°C and the acetaldehyde was added dropwise for 70min. Then 85.5 g (0.25 mol) of alkenyl succinic anhydride with R=16 was added, and the temperature was raised to 70° C. for 3.0 h. Put the obtained reactant intermediate into a magnetic cup and put it into a tube furnace. Adjust the temperature of the tube furnace to 150°C and react for 2.0 hours. When the temperature of the tube furnace cools down to room temperature, collect the resulting Liquid, the obtained product is added to a thin film evaporator and rotated at 120°C, and the obtained liquid is N-vinylformamide. The NVF yield of the product is 63.0%, and the purity is 94.1%.

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Abstract

The invention discloses a synthesis method of N-vinylformamide. The synthesis method comprises the following steps: taking alkenyl succinic anhydride, acetaldehyde and formamide as raw materials and synthesizing an intermediate under the action of a basic catalyst; carrying out cracking reaction on the synthesized intermediate under the condition of 45 to 150 DEG C to obtain the N-vinylformamide.The synthesis method disclosed by the invention has the advantages of high yield, mild reaction conditions, easily-obtained raw materials, simple separation and the like; in addition, the synthesis method is lower in synthesis cost and good in industrial application prospect.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a synthesis method of N-vinylformamide. Background technique [0002] N-vinylformamide (NVF) is a non-toxic water-soluble monomer (its structural formula is figure 1 shown), are isomers of acrylamide (AAM), which is a solid, while NVF is a liquid under normal conditions, and the two isomers differ in their copolymerization reactivity, i.e., NVF is more reactive. The molecular weight M of NVF is 71 g / mol (N-vinylamine equivalent 43 g / mol). The boiling point is higher at 80°C under a pressure of 80mbar. NVF is a clear, colorless liquid that can be stored for several months under proper conditions without decomposing. [0003] NVF as a vinyl monomer (Q value 0.29, e value -0.52) can usually be polymerized in the presence of free radical initiators, using azo initiators, PNVF can be generated by solution polymerization; in other organic Precipitation polymer...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C221/00C07C223/02
Inventor 王松林杨旭旭王飞宋宗徍
Owner QINGDAO UNIV OF SCI & TECH
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