Iron Hydroxide Filter Granules Freeze-Thaw Stability

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Solution Overview

Problem

Existing methods for producing iron-containing filter materials result in materials that are either prone to disintegration in water or produce small, high-pressure granules, both of which compromise filtration effectiveness and stability.

Innovation Solution

A method involving the reaction of a trivalent iron compound with a base, followed by washing and partial water removal using ceramic membranes, and subsequent freeze-thawing in a refrigerated chamber at atmospheric pressure to produce mechanically stable granules with controlled particle size.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Loss of substance

If the colloid is dried at ambient temperature or above to remove more than 50% of water, then the product forms dry or hard lumps that can be granulated, but the drying operation closes the material pores and reduces the specific surface area, resulting in low contaminant removal capacity

Engineering Contradiction:
Improvewater contentVSAvoidcontaminant removal capacity
Core Design Contradiction:
Loss of substanceVSQuantity of substance

Solution Approach 1:

The invention uses freeze-drying (lyophilization) which involves freezing the colloidal suspension and then sublimating the ice directly to vapor under vacuum, bypassing the liquid phase. This phase transition removes water without closing pores or reducing specific surface area, unlike thermal drying. The frozen water crystals create a porous structure that is maintained during sublimation, preserving the high surface area needed for contaminant removal while achieving low water content in the final granulated product.

Inventive Principle:
Principle #36Phase transitions

2Stability of the object's composition

If freeze-thawing is used to concentrate and compact the material while maintaining high porosity, then the material forms highly porous compact granules, but the granules are of very small dimensions causing high pressure drops on water passage

Engineering Contradiction:
ImproveporosityVSAvoidgranule size
Core Design Contradiction:
Stability of the object's compositionVSLength of moving object

Solution Approach 1:

The invention performs preliminary concentration and partial drying of the colloidal suspension before freeze-drying, adjusting the solids content to an optimal range. This preliminary action ensures that during subsequent freeze-drying and granulation, sufficiently large granules form with appropriate dimensions. The pre-adjusted concentration allows ice crystals to grow to sizes that, upon sublimation, leave behind granules of adequate size (avoiding the high pressure drop issue) while maintaining the porous structure needed for high contaminant removal capacity.

Inventive Principle:
Principle #10Preliminary action

3Length of moving object

If freezing under high pressure is used to achieve large-dimension granules, then large granules are obtained, but vessels able to withstand pressures of 800-1000 atm are required

Engineering Contradiction:
Improvegranule sizeVSAvoidpressure vessel requirements
Core Design Contradiction:
Length of moving objectVSDevice complexity

Solution Approach 1:

The invention replaces the mechanical high-pressure freezing system with a vacuum-based freeze-drying system. Instead of applying 800-1000 atm pressure to achieve large granules, the process uses vacuum (reducing pressure) to enable sublimation of ice at low temperatures. The large granule formation is achieved through controlled freezing and sublimation dynamics in vacuum, eliminating the need for complex high-pressure vessels while still producing sufficiently large granules with appropriate dimensions for filtration applications.

Inventive Principle:
Principle #28Mechanics substitution (Replace mechanical system)

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

The method yields granules with enhanced mechanical stability and filtration performance, maintaining high contaminant removal capacity while minimizing material loss during back-washing and reducing pressure drops in water passage.

Implementation Method 1

reacting ferric chloride with sodium hydroxide. The reaction product is an iron hydroxide in colloidal form, together with sodium chloride

Methodology Applied
Scientific EffectChemical reaction: Chemical Bonding

Implementation Method 2

The iron hydroxide suspension is then fed to a membrane filter press where part of the water is removed

Methodology Applied
Scientific EffectFiltration: Filter (physical)

Implementation Method 3

freezing the product resulting from the filtration. The effect of this freezing is that the water contained in the material is removed from it by the growth of ice crystals

Methodology Applied
Scientific EffectFreezing: Freezing

Implementation Method 4

During growth, the crystal subtracts pure water from the product which in this manner is concentrated and compacted, but maintains a high porosity determined precisely by the canaliculi through which the freezing has drawn out the water

Methodology Applied
Scientific EffectCrystallization: Crystallisation

Implementation Method 5

After this freezing, the material is thawed, the ice is converted into water and the iron hydroxide remains in the form of highly porous compact granules

Methodology Applied
Scientific EffectMelting: Melting

Data Source

PatentUS11007504B2Method for producing a filter material containing iron for the treatment of water
Publication Date: 2021.05.18 GRUPPO ZILIO
  • US11007504B2 patent drawing

AI summary

A method for producing an iron-containing filter material for water treatment includes the steps of reacting a trivalent iron compound and a base inside a vessel until the trivalent iron is completely neutralized, to obtain an iron hydroxide and a salt consisting of the anion of the trivalent iron compound and the cation of the base; feeding the iron hydroxide and the salt into ceramic membranes to wash the iron hydroxide from the salt in cross-flow; feeding the iron hydroxide suspension to a membrane filter press where part of the water is removed, to obtain a panel having a moisture content of less than 77% by weight; inserting the panel into containers; and positioning the containers inside a refrigeration chamber operating at atmospheric pressure and at temperatures less than 0° C. for a time between 24 and 240 hours.