Unlock instant, AI-driven research and patent intelligence for your innovation.

A kind of preparation method of trihydroxymethylaminomethane

An aminomethane and hydroxymethyl technology, which is applied in the field of preparation of trihydroxymethylaminomethane, can solve the problems of high reduction and hydrogenation reaction pressure, unsuitable for industrial production, and high condensation reaction temperature, and achieves reduction of by-products and impurities. content, the effect of complete condensation reaction

Active Publication Date: 2022-04-15
SHE COUNTY JINDONG ECONOMIC & TRADE CO LTD
View PDF5 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Chinese patent CN200610037713.0 discloses that nitromethane and excess paraformaldehyde are used as main raw materials to undergo condensation reaction at a certain temperature to form tris(hydroxymethyl)nitromethane; And catalyst, through hydrogenation reduction reaction, crystallization, and recrystallization to produce trishydroxymethylaminomethane, the condensation temperature is 40-55 °C, the reduction temperature is 40-55 °C, the pressure is 2-3 MPa, the catalyst is nickel The catalyst, the solvent is methanol, and the molar ratio of nitromethane to paraformaldehyde is 1:3-4, the product yield is low, the condensation reaction temperature is high, and the reduction hydrogenation reaction pressure is high, so it is not suitable for industrial production

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • A kind of preparation method of trihydroxymethylaminomethane
  • A kind of preparation method of trihydroxymethylaminomethane
  • A kind of preparation method of trihydroxymethylaminomethane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Embodiment 1; The preparation of three (hydroxymethyl) aminomethane

[0033] Step A: Preparation of tris(hydroxymethyl)nitromethane: add 153g of methanol to the reaction kettle, start stirring, add 149.6g of paraformaldehyde (polymerization degree 7-8), 0.51g of potassium hydroxide, triethylamine 0.11g, dissolved and stirred for 30 minutes until the solution was colorless and transparent; 85g of nitromethane was added dropwise in 1.2 hours, the temperature of the dropwise addition of nitromethane was controlled at 30°C-40°C, and the reaction temperature was controlled at 30°C-40°C after the dropwise addition was completed. °C, react for 5 hours, add oxalic acid to adjust the pH to 8.5.

[0034] Step B: Preparation of crude tris(hydroxymethyl)aminomethane: Pour the reaction solution in step (1) into a hydrogenation kettle, add 750g of methanol, 10.2g of catalyst Raney nickel, control the temperature at 30°C-40°C, and the pressure 1.3Mpa, hydrogenation for 2.5 hours; aft...

Embodiment 2

[0036] Embodiment 2; The preparation of three (hydroxymethyl) aminomethane

[0037] Step A: Preparation of tris(hydroxymethyl)nitromethane: add 157g of methanol to the reaction kettle, start stirring, add 149.6g of paraformaldehyde (polymerization degree 7-8), 0.46g of potassium hydroxide, triethylamine 0.10g, dissolved and stirred for 30 minutes until the solution was colorless and transparent; 85g of nitromethane was added dropwise in 1.5 hours, the temperature of the dropwise addition of nitromethane was controlled at 30°C-40°C, and the reaction temperature was controlled at 30°C-40°C after the dropwise addition was completed. °C, react for 5.5 hours, add oxalic acid to adjust the pH to 8.5.

[0038] Step B: Preparation of crude tris(hydroxymethyl)aminomethane: Pour the reaction solution in step (1) into a hydrogenation kettle, add 750g of methanol, 11.05g of catalyst Raney nickel, control the temperature at 30°C-40°C, and the pressure 1.2Mpa, hydrogenation for 2.7 hours; ...

Embodiment 3

[0040] Embodiment 3; The preparation of three (hydroxymethyl) aminomethane

[0041]Step A: Preparation of tris(hydroxymethyl)nitromethane: add 153g of methanol to the reaction kettle, start stirring, add 149.6g of paraformaldehyde (polymerization degree 7-8), 0.51g of potassium hydroxide, triethylamine 0.11g, dissolved and stirred for 30 minutes until the solution was colorless and transparent; 85g of nitromethane was added dropwise in 1.2 hours, the temperature of the dropwise addition of nitromethane was controlled at 30°C-40°C, and the reaction temperature was controlled at 30°C-40°C after the dropwise addition was completed. °C, react for 5 hours, add oxalic acid to adjust the pH to 8.5.

[0042] Step B: Preparation of crude tris(hydroxymethyl)aminomethane: Pour the reaction solution in step (1) into a hydrogenation kettle, add 710g of methanol and 8.5g of catalyst Raney nickel, control the temperature at 30°C-40°C, and the pressure 1.2Mpa, hydrogenation for 3 hours; afte...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
degree of polymerizationaaaaaaaaaa
degree of polymerizationaaaaaaaaaa
Login to View More

Abstract

The invention provides a method for preparing tris(hydroxymethyl)aminomethane, comprising the following steps: step A: paraformaldehyde and nitromethane generate tris(hydroxymethyl)nitromethane under alkaline conditions; step B : Tris(hydroxymethyl)nitromethane is hydrogenated and reduced to generate tris(hydroxymethyl)aminomethane crude product; Step C: refining to obtain tris(hydroxymethyl)aminomethane, the tris(hydroxymethyl)aminomethane obtained in the present invention The molar yield is above 85%, and the product content reaches 99.95%.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis and relates to a preparation method of trishydroxymethylaminomethane. Background technique [0002] Tris(hydroxymethyl)aminomethane is an important biochemical, chemical and pharmaceutical intermediate with the molecular formula (CH 2 Oh) 3 CNH 2 , whose structural formula is shown in Formula 1, is widely used in acute metabolic and respiratory acidemia, and is an alkaline buffer, which has a good buffering effect on metabolic acidosis and enzyme activity reactions, and can also be used as an acid titration These two applications have higher requirements on the content of standard substances used in the law, generally 99.9%-100.1%. [0003] [0004] Formula 1 [0005] The preparation of tris(hydroxymethyl)aminomethane generally uses nitromethane and formaldehyde as raw materials. After condensation, cooling and crystallization, etc., tris(hydroxymethyl)nitromethane is obtained, an...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C07C213/02C07C213/10C07C215/10C07C201/12C07C205/15
CPCC07C213/02C07C213/10C07C201/12C07C205/15C07C215/10
Inventor 刘俊成刘晓张迪樊靖华詹石玉刘东东南彦冬
Owner SHE COUNTY JINDONG ECONOMIC & TRADE CO LTD