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In-situ recycling technology of alkylamine

An alkylamine, in-situ technology, applied in the field of in-situ recycling of amines, can solve the problems of increased difficulty in disposal of process wastewater, waste of amine compounds, disadvantage, etc.

Active Publication Date: 2019-04-26
SHANDONG JIURI CHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

From the point of view of atom economy, this undoubtedly causes a great waste of amine compounds, which is not conducive to reducing production costs
The quaternary ammonium salts generated during the preparation process will enter the process wastewater, greatly increasing the ammonia nitrogen value of the wastewater, making it more difficult to dispose of the process wastewater

Method used

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  • In-situ recycling technology of alkylamine
  • In-situ recycling technology of alkylamine
  • In-situ recycling technology of alkylamine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Example 1: Substitution reaction of dimethylamine gas, using a solid basic compound as an acid-binding agent.

[0042] Experimental steps: Take a 2000mL reaction bottle and add 1000mL organic solvent;

[0043] Put in α-haloketone and start stirring;

[0044] Put in the basic compound solid;

[0045] Dimethylamine gas is introduced, and the temperature is kept at 40-45°C for 2 hours, and the organic phase is taken into liquid chromatography to detect the remaining α-haloketone of the raw material and the content of the product α-(N,N-dimethyl)aminoketone;

[0046] The response data is as follows:

[0047]

[0048] From the above experimental data, it can be seen that since basic compounds such as potassium carbonate, sodium carbonate, sodium hydroxide, and potassium hydroxide are basically insoluble in organic solvents, solid-liquid two-phase contact basically cannot play the role of binding halogen anions. Dimethylamine gas is under the condition of 40-45°C, a lar...

Embodiment 2

[0049] Example 2: Substitution reaction of dimethylamine gas, using a basic compound solution as an acid-binding agent.

[0050] Experimental steps: Take a 3000mL reaction bottle and add 1000mL organic solvent;

[0051] Put in α-haloketone and start stirring;

[0052] Put into the prepared alkaline compound solution;

[0053] Dimethylamine gas is introduced, and the temperature is kept at 40-45°C for 2 hours, and the organic phase is taken into liquid chromatography to detect the remaining α-haloketone of the raw material and the content of the product α-(N,N-dimethyl)aminoketone;

[0054] The response data is as follows:

[0055]

[0056] From the above experimental data, it can be seen that after adding the aqueous solution of the alkali compound, the alkali compound is completely dissolved, and the liquid-liquid two-phase contact can promote the combination of the alkali compound and the halogen anion. At the same time, the introduction of water can also bind dimethyl...

Embodiment 3

[0057] Example 3: A 40% aqueous solution of dimethylamine is used for substitution reaction, and a basic compound solution is used as an acid-binding agent.

[0058] Experimental steps: Take a 3000mL reaction bottle and add 1000mL organic solvent;

[0059] Put in α-haloketone and start stirring;

[0060] Put into the prepared alkaline compound solution;

[0061] Add 40% dimethylamine aqueous solution, keep it warm at 40-45°C for 2 hours, take the organic phase and enter it into liquid chromatography to detect the remaining α-haloketone of the raw material and the content of the product α-(N,N-dimethyl)aminoketone;

[0062] The response data is as follows:

[0063]

[0064]

[0065]It can be seen from the above experimental data that when 40% dimethylamine aqueous solution is used for the reaction, due to the reduction of gas dissolution and escape process, dimethylamine can react rapidly when it contacts with materials, and the utilization rate of dimethylamine is obvi...

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Abstract

The invention relates to an in-situ recycling technology of amine during alpha-aminoketone production, in particular to a technology by which a certain amount of alkali compounds or other low-cost acid binding agents are added to bind with substituted halogen anions while amine compounds react with alpha-haloketone. By adopting the in-situ recycling technology, the using amount of amine compoundssuch as dimethylamine and the like can be greatly reduced and the atom economy is improved.

Description

technical field [0001] The invention relates to an in-situ recovery and utilization technology of amines in the production process of α-amino ketones. Background technique [0002] Photoinitiator 369 is a high-efficiency UV curing initiator for UV polymerization of unsaturated prepolymerization systems. 369 is especially suitable for colored UV curing systems, photoresists and printing plates. Its structural formula is as follows: [0003] [0004] CAS NO: 119313-12-1 [0005] Molecular weight: 366.5 [0006] Appearance: yellow powder [0007] Melting point: 110-114°C [0008] Absorption peak: 233nm, 324nm (in methanol solution) [0009] Solubility: 20°C (g / 100g solution) [0010] acetone Butyl acetate HDDA toluene Photoinitiator 1173 17 11 10 27 25 [0011] Photoinitiator 369 has been tested and can be used alone or mixed with appropriate initiators (such as: Photoinitiator 184, 651, etc.) for UV-curable inks and va...

Claims

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Application Information

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IPC IPC(8): C07C225/06C07C221/00C07D295/135
CPCC07C221/00C07D295/135C07C225/06
Inventor 程兵兵陈波崔金素石智铭吕振波罗想刘金熹
Owner SHANDONG JIURI CHEM TECH CO LTD
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