Classifications

• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
  • C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
  • C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
  • C08L23/16—Ethylene-propylene or ethylene-propylene-diene copolymers
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
  • C08H6/00—Macromolecular compounds derived from lignin, e.g. tannins, humic acids
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
  • C08L97/00—Compositions of lignin-containing materials
  • C08L97/005—Lignin

Definitions

• the present invention relates to a novel use of a pure and non-degraded natural polyphenol biopolymer represented by a particular lignin - hereinafter lignin - for mechanical reinforcement in polymeric structures of elastomeric type.
• the present invention also relates to an elastomer prepared by implementing the use according to the invention.
• novel use according to the present invention resides in the implementation of a particular lignin derived from a vegetable raw material, in particular wheat straw, and which is composed of linear oligomers of low molecular weight which behave like the homologous oligomers and phenolic polymers.
• Biolignine TM or “Lignin CIMV”
• CIMV Process a process - hereinafter "CIMV Process” - perfectly controlled and described in particular in the patent document EP-B1 -1.180.171.
• Biolignine TM The notion of purity and the native character of "Biolignine TM” can be summarized in particular by the following points: residual polysaccharide levels, mineral matter content, average molecular mass and distribution, rate of reactive functions (in particular hydroxyls), all these characteristics being obtained without special treatment.
• this lignin has confirmed the potential of this lignin as an excellent substitute for carbon black for mechanical reinforcement in elastomeric polymeric structures.
• the structure of the lignin described in this document is not defined, its physicochemical properties, for example in terms of specific surface area, and its functionality are fundamentally different from those of the prepared lignin and non-degraded lignin. the use according to the invention.
• EP-A1-2,223,928 relate to the use of so-called “functionalized” lignin, all of which refer to chemically modified lignin in rubber-based compositions.
• this document indicates an attempt to reduce the diameter of the particles to obtain a specific surface of between 3 and 5 m 2 / g.
• this modification has not been satisfactory from the point of view of the results obtained and, on the other hand, it is still in attempts to use chemically modified lignins.
• column 3, line 17 and following reference is made to a method of heating and chemical modification of lignin in order to obtain the lignin powder having a specific surface area of at least 20 m 2 / g.
• US-A-3,984,362 relates to chemically modified lignin and especially to Examples 1 and 2 (see especially the added products for the preparation of lignin powder).
• a lignin preparation by washing and re-precipitation at acidic pH before use in a mixture with the rubber, ie a preparation before use.
• the lignin according to the use according to the invention differs in that it is not chemically modified and that its functional groups are "available".
• the subject of the present invention is a use, for the mechanical reinforcement of elastomer-type polymers, of a lignin which is not chemically modified to the available functional groups which has a specific surface area of between 0.5 m 2 / g and 5 m 2 / g, and preferably between 1 m2 / g and 2.5 m2 / g.
• said lignin has a low molecular weight and whose Mw is between 700 g / mol and 2000 g / mol;
• said lignin has a polydispersity index equal to about
• said lignin comprises available functional groups chosen from the group consisting of aliphatic hydroxyls, phenolic hydroxyls and carboxylic acids;
• the aliphatic hydroxyls are present at a rate of 1.5 mmol / g at 3.0 mmol / g, preferably at a rate of 2.3 mmol / g;
• the phenolic hydroxyls are present in a proportion of 1.1 mmol / g to 2.0 mmol / g, preferably at a content of not less than 1.1 mmol / g;
• the carboxylic acids are present in a proportion of 0.5 mmol / g at 1.5 mmol / g, preferably at a content equal to approximately 1.0 mmol / g;
• said lignin has a weight average particle diameter of between 5 microns and 100 microns, and preferably between 10 microns and 15 microns.
• the invention also relates to an elastomer.
• the invention also provides an elastomer incorporating a lignin used in a use according to the teachings of the invention.
• the elastomer does not comprise carbon black.
• FIG. 1 is a graph illustrating the distribution / particle size distribution of the particles of a "standard” Biolignine TM 500 microns;
• Fig. 2 is a graph illustrating the particle size distribution / particle size distribution of a finely ground 15 micron Biolignine TM;
• FIGS. 3 to 6 are microscopic views by Scanning Electron Microscopy of various mixtures according to the invention and / or reference products. DETAILED DESCRIPTION OF THE INVENTION
• a lignin powder was prepared as follows from a Biolignine TM obtained according to the CIMV Method: From a wheat straw Biolignine TM, a "fine” grinding was carried out using a ball mill and planetary mill, which has the following characteristics:
• FIG. 1 The particle size distribution is illustrated in FIG. 1 of the drawings appended to the present description.
• FIG. 2 also shows the particle size distribution of a "standard" Biolignine TM particle which has the following characteristics:
• Particle size distribution 40% of the particles have a weight average particle diameter of between 350 microns and 1000 microns and 90% of the particles have a weighted average particle diameter of between 45 microns and 1000 microns.
• the lignin powder was incorporated directly into a rubber by a roller mixer system.
• the specific surface area has been measured according to the method known as "laser diffraction” confirmed by nitrogen adsorption (so-called “BET” method).
• the molecular weight was determined according to the SEC method ("Size Exclusion Chromatography") Eluent THF, Detection "Refractometer", three columns in series 100, 500, 1000 Angstroms, in SDVB (Styrene Divinyl Benzene) at 30 ° C. This conventional method has been described in all publications “Biolignine TM” or “Lignine CIMV”.

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• Chemical & Material Sciences (AREA)
• Polymers & Plastics (AREA)
• Health & Medical Sciences (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Medicinal Chemistry (AREA)
• Organic Chemistry (AREA)
• Materials Engineering (AREA)
• Engineering & Computer Science (AREA)
• Life Sciences & Earth Sciences (AREA)
• Biochemistry (AREA)
• Compositions Of Macromolecular Compounds (AREA)
• Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
• Paints Or Removers (AREA)
• Reinforced Plastic Materials (AREA)
• Pigments, Carbon Blacks, Or Wood Stains (AREA)

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• 2012
  • 2012-07-17 FR FR1256889A patent/FR2993568B1/fr not_active Expired - Fee Related
• 2013
  • 2013-07-16 EP EP13739651.1A patent/EP2875065B1/fr active Active
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