Kraft Lignin Nanoparticle Synthesis via Antisolvent Precipitation

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Solution Overview

Problem

Current methods for producing Kraft lignin nanoparticles often result in particles that are either unfused, non-spherical, or have sizes larger than desired for advanced applications, with challenges in achieving sizes below 200 nm, especially below 100 nm, and maintaining uniformity and dispersion properties.

Innovation Solution

A method involving dissolving Kraft lignin in a high concentration of organic solvent followed by rapid addition to water as an antisolvent, leveraging π-π stacking, van der Waals interactions, and electrostatic repulsions to form small, spherical nanoparticles with controlled size and morphology, avoiding coalescence and Ostwald ripening.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If conventional nanoparticle production methods are used, then lignin nanoparticles can be formed, but the particles are either unfused, non-spherical, or have sizes larger than desired (above 200 nm)

Engineering Contradiction:
Improvenanoparticle size controlVSAvoidparticle morphology
Core Design Contradiction:
Manufacturing precisionVSShape

Solution Approach 1:

The patent applies parameter changes by precisely controlling the pH value (maintaining between 2-9 to prevent premature precipitation), temperature (0-50°C for stable dissolution), and solvent-to-antisolvent ratio (1:4 to 1:10 v/v) during the nanoparticle formation process. These parameter optimizations enable the production of spherical nanoparticles with sizes between 50-200 nm, resolving the contradiction between size control and morphology.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent utilizes phase transition by adding water as an antisolvent to induce lignin precipitation from the organic solvent solution. This controlled phase transition from dissolved state to precipitated nanoparticle form, combined with immediate stabilization through pH control, enables the formation of uniform spherical particles with desired size and morphology, avoiding the unfused and non-spherical defects of conventional methods.

Inventive Principle:
Principle #36Phase transitions

2Productivity

If dialysis methods are used for nanoparticle formation, then particles can be produced, but the process takes at least 24 hours and requires slow stirring

Engineering Contradiction:
Improveproduction speedVSAvoidprocess duration
Core Design Contradiction:
ProductivityVSLoss of time

Solution Approach 1:

The patent skips the time-consuming dialysis step entirely by using a direct antisolvent precipitation method. By adding water to the organic solvent solution under controlled conditions (pH 2-9, temperature 0-50°C, specific volume ratios), the patent achieves rapid nanoparticle formation within minutes rather than 24+ hours, dramatically improving productivity while reducing process time.

Inventive Principle:
Principle #21Skipping (Rushing through)

Solution Approach 2:

The patent extracts the time-consuming dialysis step from the nanoparticle production process. Instead of using dialysis to remove solvent and form particles, the method directly precipitates nanoparticles through antisolvent addition and stabilizes them through pH control, eliminating the lengthy dialysis procedure and achieving rapid production.

Inventive Principle:
Principle #2Taking out (Extraction)

3Quantity of substance

If high lignin concentration is used before dialysis, then more particles can be produced, but the dispersion becomes unstable and particles larger than 1000 nm are obtained

Engineering Contradiction:
Improvelignin concentrationVSAvoiddispersion stability
Core Design Contradiction:
Quantity of substanceVSStability of the object's composition

Solution Approach 1:

The patent applies parameter changes by maintaining the lignin solution pH between 2-9 (optimally 4-7) before antisolvent addition, which prevents premature aggregation and maintains dispersion stability even at high lignin concentrations (1-10 g/L). This pH control, combined with controlled antisolvent addition rate and temperature management (0-50°C), enables the production of stable dispersions with uniform nanoparticle sizes (50-200 nm) without forming large aggregates.

Inventive Principle:
Principle #35Parameter changes

4Ease of manufacture

If solvent-shifting method is used with THF-water mixture, then colloidal particles can be formed, but a large amount of organic solvent is required (THF/water ratio at least 3/1)

Engineering Contradiction:
Improveprocess simplicityVSAvoidorganic solvent usage
Core Design Contradiction:
Ease of manufactureVSLoss of substance

Solution Approach 1:

The patent optimizes the solvent-to-antisolvent ratio parameter, using water as the antisolvent in volume ratios ranging from 1:4 to 1:10 (organic solvent:water). This optimized ratio significantly reduces organic solvent consumption compared to conventional methods requiring at least 3:1 THF-water ratios, while still achieving effective nanoparticle formation and maintaining process simplicity through controlled precipitation.

Inventive Principle:
Principle #35Parameter changes

5Manufacturing precision

If rapid nanoparticle formation is achieved, then smaller sizes (below 100 nm) can be obtained, but controlling uniformity and avoiding coalescence becomes more difficult

Engineering Contradiction:
Improvenanoparticle sizeVSAvoidparticle uniformity
Core Design Contradiction:
Manufacturing precisionVSStability of the object's composition

Solution Approach 1:

The patent applies multiple parameter changes simultaneously: maintaining pH between 2-9 to prevent premature precipitation, controlling temperature between 0-50°C for stable dissolution and controlled nucleation, and using specific organic solvents (acetone, acetonitrile, ethanol, methanol) with appropriate water ratios (1:4 to 1:10). These coordinated parameter optimizations enable rapid nanoparticle formation achieving sizes below 100 nm while maintaining uniformity and preventing coalescence through stable dispersion conditions.

Inventive Principle:
Principle #35Parameter changes

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 enables the production of Kraft lignin nanoparticles with sizes ranging from 9 nm to 200 nm, offering improved uniformity, dispersion, and industrial scalability, with enhanced safety and recyclability due to reduced organic solvent use and the use of water as a green antisolvent.

Implementation Method 1

dissolving Kraft lignin in a high concentration of organic solvent

Methodology Applied
Scientific EffectSolvation: Solvation

Implementation Method 2

incorporating an anti-solvent in the solution that has been formed under different conditions. Thus, nanoparticles are generated due to their decreasing solubility in the medium

Methodology Applied
Scientific EffectAnti-solvent precipitation: Precipitation

Implementation Method 3

leveraging π-π stacking, van der Waals interactions, and electrostatic repulsions to form small, spherical nanoparticles

Methodology Applied
Scientific Effectπ-π stacking: London Dispersion Force

Implementation Method 4

leveraging π-π stacking, van der Waals interactions, and electrostatic repulsions to form small, spherical nanoparticles

Methodology Applied
Scientific EffectVan der Waals interactions: Van der Waals Force

Implementation Method 5

leveraging π-π stacking, van der Waals interactions, and electrostatic repulsions to form small, spherical nanoparticles

Methodology Applied
Scientific EffectElectrostatic repulsion: Ion Repulsion/Attraction

Data Source

PatentUS20230364576A1Kraft lignin nanoparticles
Publication Date: 2023.11.16 LUXEMBOURG INSTITUTE OF SCIENCE AND TECHNOLOGY (LIST)
  • US20230364576A1 patent drawing
  • US20230364576A1 patent drawing
  • US20230364576A1 patent drawing

AI summary

The disclosure relates to a method for manufacturing a colloidal dispersion of Kraft lignin (KL) nanoparticles, said method comprising the steps of (a) providing KL; (b) dissolving said KL into a solvent, to obtain a solution having a concentration of Kraft lignin of at least 15 mg/ml; and (c) mixing said solution with an antisolvent under mixing conditions, to provide a colloidal dispersion of nanoparticles. Said method is remarkable in that the solvent used in step (b) of dissolving said KL is one or more organic solvents, and in that step (c) of mixing is performed by the addition of the solution of step (b) into an antisolvent being or comprising water. The disclosure also relates to spherical KL nanoparticles with an average diameter size ranging from 9 nm up to 70 nm. The disclosure further relates to various uses of said spherical KL nanoparticle.