Reactive Distillation Column for Halosilane Esterification

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Solution Overview

Problem

Existing single-column esterification processes for halosilanes with alcohols suffer from reduced conversion yield and selectivity, particularly when using vaporous alcohol, and require optimization of feed locations and amounts to improve reaction efficiency.

Innovation Solution

The process involves feeding halosilane and alcohol in liquid form into a single reactive distillation column, with the halosilane supplied at the top and a significant portion of the alcohol at the top and a smaller portion at the bottom, allowing reaction temperatures to be below the alcohol's boiling point initially, then rising to its boiling point, facilitating high selectivity and conversion by removing hydrogen chloride at the top and the esterification product at the bottom.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Device complexity

If a single column is used for esterification of halosilanes with alcohols, then equipment complexity and cost are reduced, but conversion yield and selectivity deteriorate

Engineering Contradiction:
Improveequipment complexityVSAvoidconversion yield
Core Design Contradiction:
Device complexityVSProductivity

Solution Approach 1:

The single column is divided into multiple feeding zones with different temperature conditions. The column includes a lower feeding zone with temperature below the alcohol boiling point and an upper feeding zone with temperature at or above the boiling point, allowing segmented reaction conditions within one column to achieve both high conversion and simplified equipment

Inventive Principle:
Principle #1Segmentation

Solution Approach 2:

Different regions of the column are assigned different thermal conditions and feeding locations. The lower section operates below boiling point for initial reaction, while the upper section operates at boiling point for complete conversion and product removal, creating local quality variations that optimize both yield and equipment simplicity

Inventive Principle:
Principle #3Local quality

2Speed

If vaporous alcohol is used in the column, then reaction speed increases, but conversion yield and selectivity deteriorate

Engineering Contradiction:
Improvereaction speedVSAvoidconversion yield
Core Design Contradiction:
SpeedVSProductivity

Solution Approach 1:

The patent dynamically adjusts the physical state of alcohol based on location within the column. Liquid alcohol is fed in the lower zone for controlled reaction, while vaporization occurs progressively as the mixture rises to the upper zone, creating a dynamic transition from liquid-phase to vapor-phase reaction that maintains both speed and yield

Inventive Principle:
Principle #15Dynamics

Solution Approach 2:

The reaction is initiated in the lower feeding zone with liquid alcohol at controlled temperature before the mixture reaches the upper zone. This preliminary reaction stage ensures high selectivity, followed by complete conversion in the upper zone, achieving both speed and yield through staged action

Inventive Principle:
Principle #10Preliminary action

3Productivity

If two-column technology is used for esterification, then conversion completeness is improved, but equipment complexity and energy consumption increase

Engineering Contradiction:
Improveconversion completenessVSAvoidequipment complexity
Core Design Contradiction:
ProductivityVSDevice complexity

Solution Approach 1:

The patent merges the functions of two separate columns into a single integrated column. The column simultaneously performs initial esterification in the lower zone and complete conversion in the upper zone, eliminating the need for separate reactor and finishing column while achieving the same conversion completeness

Inventive Principle:
Principle #5Merging (Combining)

Solution Approach 2:

The single column is designed to perform multiple functions that traditionally required two columns. It handles both the initial reaction stage and the complete conversion stage, as well as product separation, making the single column a multi-functional unit that reduces overall equipment complexity

Inventive Principle:
Principle #6Universality (Multi-functionality)

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 achieves high conversion levels and selectivity with reduced equipment costs, improved energy efficiency, and lower maintenance, eliminating the need for cooling and reheating steps, while minimizing residue formation.

Implementation Method 1

the temperatures inside the column (1) between line (7) and line (8) is below the boiling temperature of the alcohol of the formula II

Methodology Applied
Scientific EffectTemperature gradient: Temperature Gradient

Implementation Method 2

removing the hydrogen chloride formed in the reaction via the top of the column (1)

Methodology Applied
Scientific EffectDistillation: Distillation

Implementation Method 3

circulation evaporator (3), which heats the bottom product in the column (1)

Methodology Applied
Scientific EffectEvaporation: Evaporation

Data Source

PatentEP2956462B1Method for the esterification of silicon halogen compounds in a column, and suitable device therefor
Publication Date: 2018.03.07 EVONIK OPERATIONS GMBH
  • EP2956462B1 patent drawingFigure 1
  • EP2956462B1 patent drawingFigure 2

AI summary

The invention relates to a method for the continuous esterification of halogen silanes of the formula (I) with alcohols of the formula (II) to obtain silane esters of the formula (III) in a single column (1): R1 aSIHalb (I), R2-(OH) (II), R1 aSi-(OR2)b (III). The method is characterized by the steps: i) feeding the halogen silane (I) in liquid form into the upper third of the column (1) [line (6)]; ii) feeding a major portion of the alcohol (II) in liquid form into the upper third of the column (1) [line (7)]; iii) feeding the remaining alcohol (II) in liquid form into the lower third of the column [by way of line (8)]. The hydrogen chloride formed during the reaction is discharged via the head of the column, the esterification product is discharged from the bottom of the column. The invention further relates to a column (1) for the continuous esterification of halogen silanes having the following characteristics: lines (6), (7), and (8) as described above, and furthermore, a rotating evaporator (3) in the lower third of the column, and a line (8) for discharging the hydrogen halide via the head of the column, and a line (10) for discharging the esterification product from the bottom of the column.