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Synthesis and purification method of high-purity N-isobutoxy methacrylamide (IBMA)

A technology of isobutoxymethacrylamide and purification method is applied in the separation/purification of carboxylic acid amide, chemical instruments and methods, preparation of carboxylic acid amide, etc. and other problems, to achieve the effect of reducing self-aggregation behavior, convenient operation and high reactivity

Pending Publication Date: 2022-04-08
ZHEJIANG XINYONG BIOCHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The technical problem to be solved by the present invention is to provide a method for synthesizing and purifying high-purity N-isobutoxymethacrylamide IBMA, so as to solve the complex process, low efficiency and many impurities of the prepared product in the conventional synthesis method currently on the market. , the problem of low purity

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  • Synthesis and purification method of high-purity N-isobutoxy methacrylamide (IBMA)
  • Synthesis and purification method of high-purity N-isobutoxy methacrylamide (IBMA)
  • Synthesis and purification method of high-purity N-isobutoxy methacrylamide (IBMA)

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Embodiment 1

[0029] Embodiment 1: This embodiment provides a synthesis and purification method of high-purity grade N-isobutoxymethacrylamide IBMA, comprising the following steps:

[0030] S1: Add 350ml of absolute ethanol to a 500ml round bottom flask, add 11g (0.1mol) of tetramethylammonium chloride, 5.2g (0.13mol) of sodium hydroxide, heat and reflux for 4 hours, cool to room temperature, and centrifuge to separate the precipitate , take 200ml of supernatant. Add about 200g of calcined and activated aluminum oxide (α-Al 2 o 3 ), ensure that the aluminum oxide is completely immersed in the solution, and stand at room temperature for 24 hours. The mesoporous alumina was filtered out, and nitrogen was purged at room temperature for 24 hours to dryness to obtain a supported quaternary ammonium base catalyst, which was stored in a vacuum desiccator for future use. The obtained catalyst was recorded as Cat Me 4 NOH / AO.

[0031] S2: In a 500ml round bottom flask, add 120g Cat Me 4 NOH / AO,...

Embodiment 2

[0035] S1: Add 350ml of absolute ethanol to a 500ml round bottom flask, add 15g (0.1mol) of tetrabutylammonium bromide, 11.2g (0.2mol) of potassium hydroxide, heat and reflux for 4 hours, cool to room temperature, and centrifuge to separate the precipitate , take 200ml of supernatant. Add about 200 g of calcined and activated aluminum oxide (α-Al2O3) to the supernatant to ensure that the aluminum oxide is completely immersed in the solution, and stand at room temperature for 24 hours. Mesoporous alumina was filtered out, and room temperature was purged with nitrogen for 24 hours to dryness to obtain a supported quaternary ammonium base catalyst, which was stored in a vacuum desiccator for future use. The obtained catalyst was designated as Cat Bu4NOH / AO.

[0036] S2: In a 500ml round bottom flask, add 150g Cat Bu4NOH / AO, add 170g deionized water, add 4.4g (0.04mol) of hydroquinone, 574g (8mol) of acrylamide and 600g (8.1mol) of isobutanol to the system mol), the temperature o...

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Abstract

The invention provides a method for synthesizing and purifying high-purity N-isobutoxy methacrylamide (IBMA), which comprises the following steps: S1, preparing a supported quaternary ammonium base catalyst, S2, preparing N-isobutoxy methacrylamide, and finally, S3, preparing N-isobutoxy methacrylamide. The N-isobutoxy methacrylamide prepared by the synthesis and purification method disclosed by the invention is high in chemical purity, less in moisture and less in residual amounts of isobutanol and formaldehyde, and the method disclosed by the invention is simple in steps and high in preparation efficiency and has relatively high commercial and popularization values.

Description

technical field [0001] The invention relates to the field of chemical product preparation and purification methods, in particular to a synthesis and purification method of high-purity N-isobutoxymethacrylamide IBMA. Background technique [0002] N-isobutoxymethacrylamide (IBMA) is a new type of crosslinking monomer. Compared with the current printing adhesive crosslinking monomer methylolacrylamide (NMA), IBMA has three advantages: (1). The printing adhesive made of IBMA has good water and heat resistance of the coating film, and the printing film Flexible, changing people's opinion that "pigment printing feels hard and only suitable for small pieces of printing"; (2). Low curing energy consumption (120 ° C / 5 minutes), compared with adhesives made of NMA, energy saving 20-25% ; (3). Isobutanol gas is released during film formation, which is harmless to the environment, while NMA emulsion releases formaldehyde, an irritating gas, when solidified into film. In addition, N-...

Claims

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Application Information

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IPC IPC(8): C07C233/20C07C231/08C07C231/24B01J31/02
Inventor 张虎寅肖杰王恒吴乐先吴恒山庄贤军
Owner ZHEJIANG XINYONG BIOCHEM
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