Polycarbonate Polyol Synthesis via Reflux Condenser

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Solution Overview

Problem

Conventional methods for producing polycarbonate polyol face challenges in achieving efficient production with good hue and high transparency, as they struggle with significant volatilization of dihydroxy compounds during transesterification reactions, leading to reduced raw material consumption rates and difficulties in controlling terminal group concentrations.

Innovation Solution

A method involving a polycondensation reaction of a dihydroxy compound with a carbonic acid diester using a catalyst, where the reaction is performed in a reactor with an internal volume of 20 L or more, equipped with a reflux condenser and a heating device, maintaining a temperature difference of at least 5°C between the heat medium and the reaction solution, and limiting the total monomer distillate to 15 wt% or less based on raw material monomers.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Productivity

If transesterification reaction is performed at high temperature under reduced pressure to distill out byproduct monohydroxy compound, then productivity is improved, but significant volatilization of dihydroxy compound occurs causing reduced raw material consumption rate

Engineering Contradiction:
Improvereaction rateVSAvoidraw material consumption rate
Core Design Contradiction:
ProductivityVSLoss of substance

Solution Approach 1:

A reflux condenser is introduced as an intermediary device between the reactor and the distillation system. The condenser condenses the volatilized dihydroxy compound vapor and returns it to the reaction system, preventing material loss while maintaining the high-temperature, reduced-pressure conditions necessary for high productivity.

Inventive Principle:
Principle #24Intermediary (Mediator)

Solution Approach 2:

The invention recovers the dihydroxy compound that would otherwise be lost through volatilization. The reflux condenser captures the vaporized monomer and returns it to the reaction mixture, effectively recovering the substance that would be discarded, thus improving raw material consumption rate while maintaining high reaction temperature and pressure conditions.

Inventive Principle:
Principle #34Discarding and recovering

2Productivity

If high temperature transesterification is performed to improve productivity, then reaction speed increases, but control of terminal group concentration becomes difficult

Engineering Contradiction:
Improvereaction speedVSAvoidterminal group concentration control
Core Design Contradiction:
ProductivityVSManufacturing precision

Solution Approach 1:

The reflux condenser provides a feedback mechanism by continuously monitoring and returning volatilized dihydroxy compound to the reaction system. This automatic feedback loop maintains the dihydroxy compound concentration within the reaction mixture, enabling precise control of terminal group concentration even at high reaction temperatures that improve productivity.

Inventive Principle:
Principle #23Feedback

3Adaptability or versatility

If multiple dihydroxy compounds are used to achieve desired composition, then product functionality is improved, but molar ratio changes during polymerization making quality control difficult

Engineering Contradiction:
Improveproduct compositionVSAvoidmolar ratio control
Core Design Contradiction:
Adaptability or versatilityVSManufacturing precision

Solution Approach 1:

The reflux condenser acts as an intermediary that stabilizes the composition of the reaction mixture by preventing selective loss of volatile dihydroxy compounds. This allows multiple dihydroxy compounds with different volatilities to be used together while maintaining their intended molar ratios throughout the polymerization process, enabling both product versatility and manufacturing precision.

Inventive Principle:
Principle #24Intermediary (Mediator)

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 approach efficiently produces a polycarbonate polyol with low coloration, suitable for durable applications like paints and adhesives, improving raw material consumption rates and maintaining desired molecular weights and compositions.

Implementation Method 1

performing a polycondensation reaction... in a reactor having an internal volume of 20 L or more and being equipped with a reflux condenser

Methodology Applied
Scientific EffectCondensation: Condensation

Implementation Method 2

heating device for heating the reactor by using a heat medium, the difference between the temperature of the heat medium and the temperature of the reaction solution in the reactor is at least 5°C or more

Methodology Applied
Scientific EffectHeat transfer: Conduction (thermal)

Implementation Method 3

performing a polycondensation reaction of a dihydroxy compound with a carbonic acid diester through a transesterification reaction therebetween

Methodology Applied
Scientific EffectPolycondensation:

Data Source

PatentEP2716679B1Method for producing polycarbonate polyols, polyurethane using said polycarbonate polyols
Publication Date: 2020.01.22 MITSUBISHI CHEM CORP
  • EP2716679B1 patent drawing
  • EP2716679B1 patent drawing
  • EP2716679B1 patent drawing

AI summary

A method for producing a polycarbonate polyol having a specific structure and specific physical properties, comprising performing a polycondensation reaction of a dihydroxy compound with a carbonic acid diester through a transesterification reaction therebetween in the presence of a catalyst, wherein at least one reactor is a reactor having an internal volume of 20 L or more and being equipped with a reflux condenser and a heating device for heating the reactor by using a heat medium, the difference between the temperature of the heat medium and the temperature of the reaction solution in the reactor is at least 5°C or more, and the total amount of monomers distilled out in all reaction steps is 15 wt% or less based on the gross weight of raw material monomers.