Polycarbonate Polyol Synthesis with Distillate Feedback Control

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Solution Overview

Problem

Existing methods for producing polycarbonate polyol result in unstable molecular weight and hydroxyl value fluctuations due to discrepancies between actual and theoretical stoichiometric amounts of carbonate, necessitating time-consuming post-processing corrections.

Innovation Solution

A semi-continuous synthesis method involving continuous feeding of carbonate with real-time monitoring and adjustment of carbonate mass percentage in the reaction system to maintain stability, ensuring |Z1-Z2| × 100% / Z2 ≤ 0.1%, thereby stabilizing the hydroxyl value and reducing the need for post-processing corrections.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Productivity

If continuous feeding of carbonate is used to promote reaction speed, then reaction efficiency is improved, but the amount of carbonate actually participating in reaction deviates from stoichiometric amount, causing hydroxyl value fluctuations

Engineering Contradiction:
Improvereaction speedVSAvoidhydroxyl value
Core Design Contradiction:
ProductivityVSManufacturing precision

Solution Approach 1:

The patent implements a feedback control system where the composition of distillate is monitored in real-time during continuous carbonate feeding. Based on the measured carbonate content in distillate, the system dynamically adjusts the feeding rate to maintain the correct stoichiometric ratio, ensuring both high reaction speed and precise hydroxyl value control.

Inventive Principle:
Principle #23Feedback

Solution Approach 2:

The patent changes the control parameter from fixed stoichiometric feeding to dynamic feeding based on distillate composition. By monitoring the carbonate content in distillate and adjusting the feeding rate accordingly, the system maintains optimal reaction conditions throughout the process, resolving the contradiction between speed and precision.

Inventive Principle:
Principle #35Parameter changes

2Temperature

If pressure is increased to raise reaction temperature, then reaction efficiency is improved, but the difference between actual and theoretical carbonate amount increases, affecting product quality

Engineering Contradiction:
Improvereaction temperatureVSAvoidhydroxyl value
Core Design Contradiction:
TemperatureVSManufacturing precision

Solution Approach 1:

The patent uses feedback control to monitor distillate composition and adjust carbonate feeding rate in response to temperature and pressure changes. This ensures that even when temperature is increased for efficiency, the stoichiometric balance is maintained through real-time corrections.

Inventive Principle:
Principle #23Feedback

Solution Approach 2:

The patent transitions from static stoichiometric feeding to dynamic feeding that adapts to changing reaction conditions. The feeding rate is continuously adjusted based on real-time monitoring of distillate composition, allowing the system to maintain precision despite temperature variations.

Inventive Principle:
Principle #15Dynamics

3Reliability

If pressure is reduced to distill off by-products, then reaction thoroughness is improved, but the amount of carbonate actually participating in reaction deviates from theoretical amount, requiring post-processing corrections

Engineering Contradiction:
Improvereaction thoroughnessVSAvoidhydroxyl value
Core Design Contradiction:
ReliabilityVSManufacturing precision

Solution Approach 1:

The patent implements feedback control that monitors distillate composition during reduced-pressure distillation. By measuring the carbonate content in the distillate stream, the system adjusts the feeding rate to compensate for carbonate loss, maintaining the correct stoichiometric ratio even during thorough by-product removal.

Inventive Principle:
Principle #23Feedback

Solution Approach 2:

The patent performs preliminary adjustment of feeding rate based on expected carbonate loss during distillation. By proactively compensating for the deviation before it affects the final product, the system maintains hydroxyl value precision throughout the reaction and distillation process.

Inventive Principle:
Principle #10Preliminary action

4Device complexity

If batch process with one-time feeding is used, then process simplicity is maintained, but molecular weight and hydroxyl value fluctuate significantly, decreasing production feasibility

Engineering Contradiction:
Improveprocess complexityVSAvoidmolecular weight
Core Design Contradiction:
Device complexityVSManufacturing precision

Solution Approach 1:

The patent replaces batch feeding with continuous feeding of carbonate throughout the reaction. This continuous supply maintains stable reaction conditions and consistent stoichiometric ratios, eliminating the significant fluctuations in molecular weight and hydroxyl value that occur with one-time feeding.

Inventive Principle:
Principle #20Continuity of useful action

Solution Approach 2:

The patent transitions from static batch feeding to dynamic continuous feeding with real-time adjustments. The feeding rate is continuously monitored and adjusted based on distillate composition, maintaining stable reaction conditions and precise product properties throughout the process.

Inventive Principle:
Principle #15Dynamics

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

Stable production of polycarbonate polyol with consistent hydroxyl values is achieved, eliminating the need for post-treatment and enhancing labor productivity by maintaining reaction stability and efficiency.

Implementation Method 1

an azeotrope of by-products and the carbonate is distilled

Methodology Applied
Scientific EffectAzeotrope formation:

Implementation Method 2

an azeotrope of by-products and the carbonate is distilled

Methodology Applied
Scientific EffectDistillation: Distillation

Implementation Method 3

samples are taken to monitor mass percentage of the carbonate in the distillates

Methodology Applied
Scientific EffectRectification: Distillation

Data Source

PatentEP3730535B1Polycarbonate polyol, synthesis method therefor and application thereof
Publication Date: 2025.10.01 WANHUA CHEM GRP CO LTD
  • EP3730535B1 patent drawing
  • EP3730535B1 patent drawing

AI summary

Provided in the present invention are a polycarbonate polyol, a synthesis method therefor and an application thereof, the synthesis method comprising the following steps: carrying out a transesterification reaction between raw material A containing a polyol or a mixture of a polyol and a lactone and a carbonate so as to generate the polycarbonate polyol, performing one-time feeding of raw material A, loading a stoichiometrically pre-determined total carbonate feed amount of carbonate into the reaction system by using a manner of continuous feeding, and distilling an azeotrope of a by-product and carbonate during the reaction; sampling and monitoring the mass percentage of carbonate in fractions when completing the process of loading the stoichiometrically pre-determined total carbonate feed amount of carbonate, controlling the stability of the carbonate content in the collected fractions and/or adding more or less carbonate according to changes in the carbonate content in the fraction. The method provided in the present invention may quickly and stably produced a product that satisfies requirements for hydroxyl value, and post-treatment is simple.