Carbamic Acid Derivative Solid Powder Preparation via High Pressure

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Solution Overview

Problem

Existing methods for preparing solid carbamic acid derivatives from liquid amines using carbon dioxide result in gel-type compounds rather than solid powder forms, making it difficult to separate and handle these compounds effectively, and often require solvents and additional processing steps that can lead to environmental pollution.

Innovation Solution

A method involving a reaction between an amine derivative and carbon dioxide at specific temperature and pressure ranges, without the use of solvents, to produce a stable solid powder form of carbamic acid derivatives, which can then be reduced back to the amine derivative and carbon dioxide, minimizing impurities and by-products.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Reliability

If a reaction is made between a liquid amine and carbon dioxide under atmospheric pressure for a long time, then carbamic acid derivatives are formed, but the reaction requires long time and produces gel-type compounds that are difficult to separate

Engineering Contradiction:
Improveformation of carbamic acid derivativesVSAvoidreaction time
Core Design Contradiction:
ReliabilityVSLoss of time

Solution Approach 1:

The patent applies parameter changes by conducting the reaction under high pressure (1-100 atm) instead of atmospheric pressure, and at controlled temperatures (-30°C to 500°C). This dramatically accelerates the reaction rate and enables the formation of solid powder products rather than gel-type compounds, resolving both the time consumption and product form issues.

Inventive Principle:
Principle #35Parameter changes

2Reliability

If conventional methods are used to prepare solid carbamic acid derivatives, then the derivatives can be formed, but gel-type compounds are produced instead of solid powder forms making separation difficult

Engineering Contradiction:
Improveformation of carbamic acid derivativesVSAvoidseparation and handling of products
Core Design Contradiction:
ReliabilityVSEase of manufacture

Solution Approach 1:

By changing the physical state parameters (pressure and temperature), the patent transforms the product from gel-type compound to solid powder form. The high pressure condition promotes the formation of crystalline solid powder that can be easily separated and handled, directly resolving the manufacturing ease issue.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent utilizes phase transition by controlling the reaction conditions to produce solid powder directly from the liquid amine and gaseous carbon dioxide. The high pressure and controlled temperature facilitate the transition to solid powder form, which has superior separation and handling properties compared to gel-type compounds.

Inventive Principle:
Principle #36Phase transitions

3Ease of manufacture

If solvents are used in the reaction process, then the reaction can proceed, but additional processing steps are required to remove solvents causing environmental pollution

Engineering Contradiction:
Improvereaction processabilityVSAvoidenvironmental pollution from solvent removal
Core Design Contradiction:
Ease of manufactureVSObject-generated harmful factors

Solution Approach 1:

The patent extracts and eliminates the solvent from the reaction system entirely. By conducting the reaction under high pressure between liquid amine and gaseous carbon dioxide without any solvent, the method produces solid powder that can be directly separated by filtration or decantation, completely avoiding the environmental pollution associated with solvent removal processes.

Inventive Principle:
Principle #2Taking out (Extraction)

Solution Approach 2:

The reactants themselves (liquid amine and gaseous carbon dioxide) serve as the reaction medium, eliminating the need for external solvents. The high pressure condition enables the gaseous carbon dioxide to dissolve in the liquid amine and react directly, with the solid powder product forming directly in the reaction mixture for easy separation.

Inventive Principle:
Principle #25Self-service

4Reliability

If strong acids are used to prepare amine salts, then solid salts are formed with good solubility, but neutralization processes are required removing strong acids causing environmental pollution

Engineering Contradiction:
Improvesolubility and stability of amine derivativesVSAvoidenvironmental pollution from neutralization process
Core Design Contradiction:
ReliabilityVSObject-generated harmful factors

Solution Approach 1:

The patent converts the traditionally harmful strong acids into a beneficial eco-friendly reagent. By using carbon dioxide (a naturally occurring gas) instead of strong acids like HCl or H2SO4, the method forms carbamic acid derivatives that do not require neutralization. The carbon dioxide reacts with the amine to form stable solid salts directly, eliminating the need for harmful neutralization processes and associated environmental pollution.

Inventive Principle:
Principle #22Blessing in disguise (Convert harm into benefit)

Applied Scientific Principles

This section explains which scientific principles are used to turn an abstract innovation direction into a practical engineering solution.

Function Achieved in This Case

This method allows for the production of pure solid powder carbamic acid derivatives that are stable, odorless, non-oxidizable, and easy to handle, with high purity and reactivity, reducing toxicity and environmental impact while eliminating the need for solvents and additional processing steps.

Implementation Method 1

reacting an amine derivative with carbon dioxide at a temperature in a range of from about −30° C. to about 500° C. and at a pressure in a range of from about 0.3 MPa to about 100 MPa

Methodology Applied
Scientific EffectChemical reaction: Chemical Bonding

Implementation Method 2

dissolving the solid powder of the carbamic acid derivative prepared by the preparation method of the present disclosure in a solvent; refluxing the carbamic acid derivative in the solvent at a temperature in a range of from about 30° C. to about 100° C.

Methodology Applied
Scientific EffectHeating: Heating

Implementation Method 3

evaporating the solvent

Methodology Applied
Scientific EffectEvaporation: Evaporation

Data Source

PatentUS9126903B2Preparation method for solid powder of a carbamic acid derivative
Publication Date: 2015.09.08 SOGANG UNIV RES FOUND
  • US9126903B2 patent drawing
  • US9126903B2 patent drawing
  • US9126903B2 patent drawing

AI summary

The present application relates to a preparation method for solid powder of a carbamic acid derivative, which includes reacting an amine derivative with carbon dioxide at a temperature in a range of from about −30° C. to about 500° C. and at a pressure in a range of from about 0.3 MPa to about 100 MPa. In addition, the present disclosure relates to a reduction method for solid powder of a carbamic acid derivative to an amine derivative and carbon dioxide, which includes dissolving solid powder of the carbamic acid derivative prepared in a solvent; refluxing the carbamic acid derivative at a temperature in a range of from about 30° C. to about 100° C.; and evaporating the solvent.