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A kind of preparation method of trihydroxyalkylaminomethane

A technology of trihydroxyalkylaminomethane and trihydroxyalkylamino, which is applied in the field of compound preparation, can solve problems such as high installation and maintenance costs, unstable production process, susceptibility to disease, etc., to reduce the discharge of three wastes, overcome safety hazards and Unstable factors, the effect of simple production

Active Publication Date: 2020-10-16
SUZHOU YACOO SCI CO LTD
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Problems solved by technology

The method of the metal reducing agent used: such as iron powder, sodium amalgam, tin dichloride, etc., the amount of such reducing agent is large, the production process is unstable, the particle size of the reducing agent, the distribution state in the system, the heating process, etc. Many factors will affect product quality and generate more solid waste
The electrolytic reduction method adopted: through the electrolytic reduction process, the nitro group is reduced, the electrodes are easily polluted during the process, and there are many instabilities in the amplification process, which is not easy to scale up production, and it is not easy to carry out in organic chemical factories.
The hydrogenation reduction method adopted: Although the hydrogenation reduction can reduce the solid waste using metal reducing agents, and the process control is relatively easy, the hydrogenation process is a dangerous chemical process, and there are also major safety hazards, and the installation and maintenance of the whole set of equipment high cost, large investment

Method used

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  • A kind of preparation method of trihydroxyalkylaminomethane
  • A kind of preparation method of trihydroxyalkylaminomethane
  • A kind of preparation method of trihydroxyalkylaminomethane

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preparation example Construction

[0028] A method for preparing trihydroxyalkylaminomethane, using di(hydroxyalkyl)oxirane as a substrate, and using a catalyst to catalyze the substrate and ammonia for ammonolysis reaction, to obtain trihydroxyalkylaminomethane; the preparation method The reaction scheme is as shown in chemical formula I:

[0029]

[0030] Wherein m is 1-5, n is 1-5, m+n≤8; the catalyst includes silicon dioxide.

[0031] As a preferred embodiment, the mass ratio of ammonia to substrate is (16-30):100; the mass ratio of catalyst to substrate is (1-10):100.

[0032] The specific method is as follows:

[0033] 1. Prepare reagents:

[0034] 1) Ammonia (NH 3 ) solution: prepared with water, methanol or ethanol as a solvent;

[0035] 2) Solvent: water, methanol or ethanol;

[0036] 3) Catalyst: including silicon dioxide or 1-4wt% iron element or titanium element, and silicon dioxide;

[0037] Its preparation method is:

[0038] After drying 100-200 mesh silicon dioxide at 200°C for 6 hours...

Embodiment 1

[0044] 1. Prepare reagents:

[0045] 1) Ammonia solution: 9wt% 27g is pre-prepared with methanol as a solvent;

[0046] 2) Solvent: methanol 13g;

[0047] 3) Catalyst: the main components are silicon dioxide, 1.97wt% iron element, and the catalyst consumption is 0.35g; the preparation method of the catalyst is the same as the specific embodiment.

[0048] 4) Bis(hydroxymethyl)oxirane solution: pre-prepared with methanol as a solvent, 50wt%, 20g.

[0049] 2. Mixing step: Stir and mix the ammonia solution, solvent and catalyst at a rotation speed of 200rpm to obtain a mixed solution, and the temperature of the mixed solution is 30°C;

[0050] 3. Reaction steps: Add bis(hydroxymethyl)oxirane solution dropwise to the mixed solution for about 10 minutes, and the temperature when adding bis(hydroxymethyl)oxirane solution is ≤35°C; after the addition is completed , reacting at a temperature of 30° C. for 16 hours;

[0051] 4. Filtration step: filter the product obtained by comple...

Embodiment 2

[0054] 1. Prepare reagents:

[0055] 1) Ammonia solution: pre-prepared 9wt% 20g with methanol as a solvent;

[0056] 2) Solvent: methanol 20g;

[0057] 3) Catalyst: the main components are silicon dioxide, 3.08wt% iron element, and the catalyst consumption is 0.5g; the preparation method of the catalyst is the same as the specific embodiment.

[0058] 4) Bis(hydroxyethyl)oxirane solution: preformed with methanol as a solvent, 50wt%, 20g.

[0059] 2. Mixing step: Stir and mix the ammonia solution, solvent and catalyst at a rotation speed of 200rpm to obtain a mixed solution, and the temperature of the mixed solution is 30°C;

[0060] 3. Reaction steps: Add di(hydroxyethyl)oxirane solution dropwise to the mixture for about 10 minutes, and the temperature when adding di(hydroxyalkyl)oxirane solution is ≤35°C; after the addition is complete , reacting at a temperature of 30°C for 16 hours;

[0061]4. Filtration step: filter the product obtained by completing the reaction to ta...

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Abstract

The invention discloses a preparation method of trihydroxyalkyl aminomethane. The preparation method comprises the steps of adopting di(hydroxyalkyl) ethylene oxide as a substrate, using a catalyst for catalyzing the substrate and carrying out ammonolysis reaction on the substrate and ammonia to obtain the trihydroxyalkyl aminomethane. A reaction route of the preparation method is as shown in a chemical formula I, and comprises the steps of mixing: preparing the ammonia into an ammonia solution, and then stirring and mixing the ammonia solution, a solvent and the catalyst to obtain a mixed liquor; reacting: adding a di(hydroxyalkyl) ethylene oxide solution into the mixed liquor, wherein the temperature is smaller than or equal to 35 DEG C when the di(hydroxyalkyl) ethylene oxide solution is added; after finishing adding, reacting at the temperature of 20 to 80 DEG C; filtering: filtering a product obtained through reaction, taking out a filter residue, and obtaining the trihydroxyalkylaminomethane through recrystallization. During a production process, the emission of three wastes is greatly reduced, potential safety hazards and unstabilizing factors existed in a conventional process are overcome, and the compound can be safely, simply and conveniently produced.

Description

technical field [0001] The invention relates to a preparation method of trihydroxyalkylaminomethane, which belongs to the technical field of compound preparation. Background technique [0002] Trihydroxyalkylaminomethane products are widely used chemical raw materials. Applied in the fields of biochemistry and medicine: the solution system can provide a wide range of pH adjustment. Applied in the field of pharmaceutical raw materials, it can be used not only as a molecular building block, but also as a compound base for active acidic drug molecules; at the same time, it can be used as a specific enzyme inhibitor in molecular biology. Applied in the field of materials: directly added to the coating to improve the affinity of the coating to the adhesion surface, and also has the performance of regulating air humidity; at the same time, in recent years, this type of product has also begun to be widely used in electronic materials. At the same time, it does not reduce the tran...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C213/04C07C215/10
CPCC07C213/04C07C215/10
Inventor 袁永坤
Owner SUZHOU YACOO SCI CO LTD
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