Method for evaluating reinforcement effect and efficiency of filler on natural rubber based on particle size of bound rubber particle formed by the filler and natural rubber latex

Patent metadata

Field	Value
Publication number	US-12436144-B2
Application number	US-202519028108-A
Country	US
Kind code	B2
Filing date	Jan 17, 2025
Priority date	Feb 6, 2024
Publication date	Oct 7, 2025
Grant date	Oct 7, 2025

Abstract

A method for evaluating reinforcement effect and efficiency of a filler on natural rubber based on particle size of bound rubber particles formed by the filler and natural rubber particle in a natural rubber latex, in which the natural rubber latex and the filler are mixed and diluted to obtain a to-be-detected emulsion, and an average particle size of bound rubber particles is measured using an instrument; a ratio of the average particle size to an average particle size of natural rubber particles in a pure rubber latex emulsion with the same concentration is calculated; the reinforcement effect of the filler on the natural rubber is evaluated based on the ratio; a function expression is established to derive a stress at definite elongation of various filler-modified natural rubber vulcanizates; and according to the function expression, the reinforcement efficiency of the filler on the natural rubber is evaluated.

First claim

What is claimed is:

1. A method for screening a filler with a reinforcement effect on natural rubber based on a particle size of bound natural rubber particles formed by the filler and a natural rubber particle in a natural rubber latex, comprising:
(S1) mixing the natural rubber latex respectively with a plurality of to-be-tested fillers in a weight ratio of 100:5-0.1 to produce a plurality of mixtures, wherein the bound natural rubber particles are formed by an interaction between the natural rubber particle in the natural rubber latex and each of the plurality of to-be-tested fillers; and diluting the plurality of mixtures to obtain a plurality of first emulsions, respectively;
(S2) measuring an average particle size of the bound natural rubber particles in each of the plurality of first emulsions by using a particle size measurement instrument; measuring an average particle size of natural rubber particles in a second emulsion, wherein the second emulsion is a pure natural rubber latex emulsion, and the second emulsion is the same as the first emulsion in terms of a concentration of the natural rubber particles; and calculating a particle size ratio x according to x=d/d 1 , wherein d represents the average particle size of the bound natural rubber particles in each of the plurality of first emulsions, and d 1 represents the average particle size of the natural rubber particles in the second emulsion;
(S3) evaluating a reinforcement effect of the plurality of to-be-tested fillers on natural rubber based on the particle size ratio, wherein when the particle size ratio x is equal to or larger than 1.14, the reinforcement effect of a corresponding to-be-tested filler on the natural rubber is determined to be strong; when the particle size ratio x ranges from 1 to 1.07, the reinforcement effect of the corresponding to-be-tested filler on the natural rubber is determined to be weak; and when the particle size ratio x is larger than 1.07 and less than 1.14, the reinforcement effect of the corresponding to-be-tested filler on the natural rubber is determined to be medium; and
screening a filler with the particle size ratio x equal to or larger than 1.14 from the plurality of to-be-tested fillers for compounding with the natural rubber latex to prepare a rubber composite.

2. The method of claim 1 , wherein in step (S1), the plurality of mixtures are diluted such that a concentration of the bound natural rubber particles in each of the plurality of first emulsions is within a detection range of the particle size measurement instrument.

3. The method of claim 1 , wherein in step (S1) and step (S2), the plurality of first emulsions and the second emulsion are each in a stable state without emulsion breaking.

4. A method for screening a filler with a reinforcement effect on natural rubber based on a particle size of bound natural rubber particles formed by the filler and a natural rubber particle in a natural rubber latex, comprising:
(SI) mixing the natural rubber latex respectively with a plurality of to-be-tested fillers in a weight ratio of 100:5-0.1 to produce a plurality of mixtures, wherein bound natural rubber particles are formed by an interaction between the natural rubber particle in the natural rubber latex and each of the plurality of to-be-tested fillers, diluting the plurality of mixtures to obtain a plurality of first emulsions, respectively;
(SII) measuring an average particle size of the bound natural rubber particles in each of the plurality of first emulsions by using a particle size measurement instrument; measuring an average particle size of natural rubber particles in a second emulsion, wherein the second emulsion is a pure natural rubber latex emulsion without the filler, and the second emulsion is the same as the first emulsion in terms of a concentration of the natural rubber particles in the natural rubber latex; calculating a particle size ratio x according to x=d/d 1 , wherein d represents the average particle size of the bound natural rubber particles in each of the plurality of first emulsions, and d 1 represents the average particle size of the natural rubber particles in the second emulsion;
(SIII) evaluating a reinforcement effect of the plurality of to-be-tested fillers on natural rubber based on the particle size ratio, wherein when the particle size ratio x is equal to or larger than 1.14, the reinforcement effect of a corresponding to-be-tested filler on the natural rubber is determined to be strong; when the particle size ratio x ranges from 1 to 1.07, the reinforcement effect of the corresponding to-be-tested filler on the natural rubber is determined to be weak; and when the particle size ratio x is larger than 1.07 and less than 1.14, the reinforcement effect of the corresponding to-be-tested filler on the natural rubber is determined to be medium; and
screening a filler with the particle size ratio x equal to or larger than 1.14 from the plurality of to-be-tested fillers;
(SIV) preparing at least two modified fillers from the screened filler respectively through at least two different modification techniques used for calculating constants; measuring an average particle size x of bound natural rubber particles formed by the natural rubber particles in the natural rubber latex and one of the at least two modified fillers used for calculating constants according to steps (SI)-(SII), respectively; preparing at least two natural rubber vulcanizates respectively filled with one of the at least two modified fillers used for calculating constants; measuring a value y of stress at definite elongation of one of the at least two natural rubber vulcanizates filled with one of the at least two modified fillers used for calculating constants;
plugging one of the at least two obtained y values and the corresponding one of the at least two particle size ratio x values into the following formula to calculate constants a and b, so as to obtain a function expression for evaluating the reinforcement efficiency of the screened filler on the natural rubber:

y
=

a
+
bx

;

(SV) measuring an average particle size of bound natural rubber particles formed by the natural rubber particles in the natural rubber latex and each of a plurality of to-be-tested modified fillers from the screened filler respectively obtained through a plurality of to-be-tested modification technologies according to steps (SI)-(SII), and then obtaining a particle size ratio x t ;
substituting the particle size ratio x t into the function expression obtained in step (SIV) to calculate a corresponding value y t of stress at definite elongation of each of a plurality of natural rubber vulcanizates respectively filled with the plurality of to-be-tested modified fillers;
measuring a value y′ of stress at definite elongation of a filler-free natural rubber vulcanizate; and
calculating the reinforcement efficiency R according to the following formula:

R
=

[

(

y
t

-

y
′

Assignees

• Univ North China
• Shanxi Zhongbei New Material Tech Co Ltd

Inventors

• Liu Yaqing
• Tao Rongyao
• Wang Wenqi
• Zhao Guizhe

Classifications

• G01N15/02

  Investigating particle size or size distribution (by measuring osmotic pressure G01N7/10; investigating sedimentation of particle suspensions G01N15/04; investigating individual particles G01N15/10) · CPC title

• G01N2015/0277

  Average size only · CPC title

• G01N2015/0053

  in liquids, e.g. trouble · CPC title

• G01N33/445 Primary

  Rubber · CPC title