EA041327B1 - METHOD FOR PREPARING A FILLER MATERIAL PRODUCT SURFACE-TREATED WITH MONO-SUBSTITUTED SUCINIC ANHYDRIDE(S) AND A MIXTURE OF ALIPHATIC LINEAR OR BRANCHED CARBOXY ACID CONTAINING STEARIC ACID - Google Patents

Description

The invention relates to a method for preparing a filler material product surface-treated with monosubstituted succinic anhydride(s) and a mixture of aliphatic linear or branched carboxylic acids containing stearic acid, to a surface-treated filler material product, to a polymer composition and a thermoplastic polymer product containing a surface-treated product filler material and/or polymer composition.

In practice, filler materials, and in particular filler materials containing calcium carbonates, are often used as particulate fillers in thermoplastic polymer products like fibers, filaments, films, and/or filaments, typically made from polyethylene (PE), polypropylene ( PP), polyurethane (PU), polyvinyl chloride (PVC), polyester (PES) and/or polyamide (PA). However, additives are added to provide the filler material with a coating and to improve the dispersion of said mineral filler material in the polymer matrix of polymer compositions, and possibly also to improve the processability of this polymer composition and/or the properties of ready-to-use products such as fibers, filaments, films, threads, sheets, pipes, profiles, molds for molding, molds for injection molding, molds for blow molding. The elimination of such additives would unacceptably reduce the quality of the resulting fibers, filaments, films, threads, sheets, pipes, profiles, molds, injection molds, blow molds. In addition, it is desirable to provide the filler material with high fluidity to ensure high productivity in the manufacture of the finished product of the processed mineral filler material and in the further processing of this product into ready-to-use products.

Several attempts have been made in the art to improve the usability of mineral filler materials, and in particular calcium carbonate-containing mineral filler materials, for example by treating such mineral filler materials with surface treatment agents. For example, WO 00/20336 relates to ultrafine natural calcium carbonate, which may optionally be treated with one or more fatty acids or one or more salts, or mixtures thereof, and which are used as rheology regulators for polymer compositions.

Similarly, US Pat. No. 4,407,986 relates to precipitated calcium carbonate which is surface treated with a dispersant which may contain higher aliphatic acids and their metal salts to limit the addition of lubricants when mixing this calcium carbonate with crystalline polypropylene and to prevent the formation of calcium carbonate aggregates, which limit the impact strength of polypropylene.

EP 0998522 relates to a surface-treated calcium carbonate filler for breathable films using fatty acids of at least 10 carbon atoms, where the filler before and after the treatment process should contain a little moisture in the range below 0.1 wt.%.

DeArmitt et al., Improved thermoplastic composites by optimized surface treatment of the mineral fillers, Institute for Surface Chemistry, August 2000, describes a wet processing process in which a load of slurry containing a mineral filler material is brought into contact with a dispersant at room temperature for one hour. However, such a wet treatment process has the disadvantage that wetting the dry treatment product and subsequent drying is energy intensive and costly.

In EP 0325114, relating to non-drip anti-corrosion compositions for motor vehicles based on polyvinyl chloride, which have improved rheological and adhesive properties, example 7 describes a mixture of ammonium salt of 12-hydroxystearic acid in combination with a fatty acid (in a mass ratio of 1:1) used for the processing of mineral filler.

WO 03/082966 relates to a cross-linked and/or cross-linked nanofiller composition which, in optional embodiments, may further comprise fillers that may or may not be coated with stearic acid, stearate, silane, siloxane and/or titanate. Such nanofiller compositions are used to increase barrier properties, strength, and heat distortion temperature, making them useful in medical, automotive, electrical, building, and food applications.

US 2002/0102404 describes dispersible calcium carbonate particles coated on their surface with a combination of saturated and unsaturated aliphatic carboxylic acids and their salts together with an organic compound such as a phthalic ester, which are used in adhesive compositions to improve viscosity stability and adhesive properties. In addition, US 2002/0102404 requires a mixture of saturated and unsaturated aliphatic carboxylic acids/salts. The presence of unsaturated aliphatic carboxylic acids/salts increases the risk of undesired in situ double bond side reactions during processing of any material containing unsaturated aliphatic carboxylic acids/salts. In addition, the presence of unsaturated aliphatic carboxylic acids/salts may result in discoloration or

- 1 041327 the appearance of an undesirable odor and obviously unpleasant odors in the material in which they are present.

Claim 11 of the claims of WO 92/02587 shows that a solution of a saponified sodium salt of at least one high molecular weight unsaturated fatty acid or a combination of at least one high molecular weight unsaturated fatty acid and at least one other high molecular weight unsaturated fatty acid can be added to a preheated slurry of precipitated calcium carbonate to ultimately obtain the desired level of fatty acid coating on the calcium carbonate before carrying out further process steps.

Abstract JP 54162746 describes a composition containing predetermined relative amounts of rigid vinyl chloride resin, colloidal calcium carbonate treated with a fatty acid, and barium stearate, used to improve the thermal stability of a vinyl chloride composition.

US Pat. No. 4,520,073 describes mineral filler materials with improved hydrophobic coatings obtained by pressure coating porous minerals using steam as a carrier for the coating material. Said coating material may be selected among other possibilities from long chain aliphatic fatty acids and their salts.

WO 01/32787 describes a particulate alkaline earth metal carbonate material product that comprises on its particles a coating of a hydrophobic material comprising a composition formed from (a) a first component that contains the reaction product of an alkaline earth metal carbonate and at least one given an aliphatic carboxylic acid, and (b) a second component having a carbonate release temperature substantially higher than that of the first component, which contains a compound of formula CH ₃ (CH ₂ )mCOOR.

WO 2008/077156 A2 relates to spunlaid fibers containing at least one polymer resin and at least one filler having an average particle size equal to or less than about 5 microns and/or having a maximum diameter of less than about 15 microns, where at least one filler is present in an amount of less than about 40% by weight, based on the total weight of the spunlaid fibers. The filler coating is described as being at least one organic material selected from fatty acids and their salts and esters, such as stearic acid, stearate, ammonium stearate and calcium stearate.

GB 2336366 A relates to filled thermoplastic compositions and in particular to filled low density polyethylene compositions which are formed into products or articles by means of an extrusion process. In addition, it is described that the hydrophobizing agent is preferably an organic carboxylic acid or a partially or completely neutralized salt thereof, which contains at least one saturated or unsaturated hydrocarbon chain containing from 8 to 28 carbon atoms, if the mineral particulate filler has a surface reaction from neutral to alkaline, for example, calcium carbonate.

EP 2159258 A1 relates to a treated mineral filler product containing: a) at least one mineral filler; b) a treatment layer located on the surface of said mineral filler(s), said treatment layer containing at least one saturated C ₈ -C ₂₄ aliphatic carboxylic acid and at least one salt of a di-and/or trivalent cation and one or more saturated C ₈ -C ₂₄ aliphatic carboxylic acids, characterized in that the mass ratio: all of these salts of aliphatic carboxylic acids: all of these aliphatic carboxylic acids is from 51:49 to 75:25, and the specified treatment layer is present in an amount of at least 2.5 mg /m ² of the specified mineral filler.

EP 1980588A1 relates to a process for producing a treated mineral filler product, which includes the following steps: (a) treating at least one dry mineral filler with at least one group II or group III metal salt of a C ₈ -C ₂₄ aliphatic monocarboxylic acid to obtain an intermediate mineral filler product; then (b) treating the mineral filler intermediate from step (a) with at least one C8- _C24 aliphatic monocarboxylic acid to form a treated mineral filler product.

One surface treatment agent currently selected and of particular utility is monosubstituted succinic anhydride or a mixture of monosubstituted succinic anhydrides.

For example, WO 2014/060286 A1 relates to a process for preparing a filler material product surface-treated with succinic anhydride(s), the process comprising at least the steps of:

a) obtaining at least one filler material containing calcium carbonate having

i) the value of the mass median particle size d ₅₀ in the range from 0.1 to 7 μm, ii) the maximum diameter (d ₉₈ )<15 μm, iii) the specific surface area (BET) from 0.5 to 150 m ² /g, as measured by BET method

- 2 041327 with nitrogen, and iv) a residual total moisture content of from 0.01 to 1 wt.% in relation to the total dry weight of at least one filler material containing calcium carbonate,

b) obtaining at least one monosubstituted succinic anhydride and, optionally, at least one monosubstituted succinic acid in an amount of from 0.1 to 3 wt.% in relation to the total dry weight of at least one filler material containing calcium carbonate, co stage a)

c) contacting the surface of at least one calcium carbonate-containing filler material from step a) while stirring in one or more steps with at least one monosubstituted succinic anhydride and optionally at least one monosubstituted succinic acid from step b), so that a treatment layer containing at least one monosubstituted succinic anhydride and optional at least one monosubstituted succinic acid and/or salt reaction product(s) thereof is formed on the surface of said at least one filler material containing calcium carbonate, from the step a) wherein the temperature before and/or during contacting in step c) is controlled such that the temperature is at least 2° C. above the melting point of at least one monosubstituted succinic anhydride and optionally at least one monosubstituted succinic acid .

WO 2016/023937 A1 relates to a method for producing a breathable film comprising the steps of: a) obtaining a composition containing at least one thermoplastic polymer and a surface-treated filler material product, and b) forming a film from the composition of steps a) and c) stretching the film obtained in step b), in at least one direction, where the product of the surface-treated filler material contains:

A) at least one crushed filler material containing calcium carbonate, having a mass median particle size d ₅₀ in the range from 0.1 to 7 microns, a maximum particle diameter <15 microns, a specific surface area (BET) from 0.5 to 150 m ² /g, as measured using nitrogen and the BET method according to ISO 9277, and a residual total moisture content of <1 wt.% in relation to the total dry weight of at least one crushed filler material containing calcium carbonate, and

B) a treatment layer on the surface of at least one wet ground filler material containing calcium carbonate containing at least one monosubstituted succinic anhydride and/or at least one monosubstituted succinic acid and/or salt product(s) of their reaction, where the product of the surface-treated filler material contains a treatment layer in an amount of from 0.1 to 3 wt.% in relation to the total dry weight of at least one crushed filler material containing calcium carbonate.

However, there is still a need for methods of preparing surface-treated filler materials containing monosubstituted succinic anhydride(s) that allow surface-treated calcium carbonate-containing mineral filler materials to be prepared to improve its flowability and to further improve their dispersion in polymer matrix of the polymer composition, in particular compared to a product that is surface-treated with only mono-substituted succinic anhydride(s). In addition, it is desirable to maintain or improve the mechanical properties of ready-to-use products such as fiber and/or filament and/or film and/or thread and/or sheet and/or pipe and/or profile and/ or a mold and/or an injection mold and/or a blow mold containing such surface treated filler material products.

Accordingly, it is an object of the present invention to provide a process for preparing a surface-treated filler material product that contains monosubstituted succinic anhydride(s). Further, it would be desirable to provide a process for preparing a surface-treated filler material product having improved fluidity, in particular as compared to a product surface-treated with monosubstituted succinic anhydride(s). Another object is to provide a process for preparing a surface-treated filler material product having improved dispersibility in the polymer matrix of the polymer composition, in particular compared to a product surface-treated with monosubstituted succinic anhydride(s). Other purposes can be understood from the following description of the present invention.

The above and other objectives are solved by the subject matter as defined herein in claim 1 of the claims.

Advantageous embodiments of the process for preparing the surface-treated filler material product of the present invention are defined in the respective dependent claims.

According to one aspect of the present invention, a method for preparing a product is provided.

- 3 041327 surface-treated filler material with at least one monosubstituted succinic anhydride and a mixture of saturated aliphatic linear or branched carboxylic acids containing stearic acid, the method includes at least the steps of obtaining at least one filler material containing calcium carbonate, obtaining at least one monosubstituted succinic anhydride, obtaining a mixture of saturated aliphatic linear or branched carboxylic acids, consisting of stearic acid, in an amount of at least 10.0 wt.% relative to the total mass of the mixture, and one or more other saturated aliphatic linear or branched carboxylic acids containing a total number of carbon atoms from C ₁₂ to C ₂₄ , bringing into contact the surface of at least one filler material containing calcium carbonate, from stage a), while stirring in one or more stages in any order at least slightly less with at least one monosubstituted succinic anhydride from step b) and a mixture of saturated aliphatic linear or branched carboxylic acids from step c) such that the treatment layer containing at least one monosubstituted succinic anhydride and/or at least one salt reaction product thereof and a mixture of saturated aliphatic linear or branched carboxylic acids and/or at least one salt reaction product thereof is formed on the surface of said at least one filler material containing calcium carbonate from step a), where the temperature before and/or during step d ) bringing into contact is controlled so that at least one monosubstituted succinic anhydride and a mixture of saturated aliphatic linear or branched carboxylic acids are in a molten or liquid state.

The inventors have surprisingly found that the above method of preparing a surface-treated filler material product results in, compared to a product surface-treated with monosubstituted succinic anhydride(s) only, a surface-treated filler material product having improved flowability and improved dispersion of the surface-treated product. processed filler material in the polymer matrix of the polymer composition. As a result, the method thus also imparts improved mechanical properties to the fiber and/or filament and/or film and/or yarn and/or sheet and/or pipe and/or profile and/or mold, and /or injection mould, and/or blow mould, and corresponding articles containing said product of surface treated filler material. More specifically, the inventors have found that the surface characteristics of the surface-treated filler material product obtained by said process can be improved by adding certain mono-substituted succinic anhydride(s) in combination with a mixture of saturated aliphatic linear or branched carboxylic acids containing stearic acid.

It is to be understood that for the purposes of the present invention, the following terms have the following meanings.

For the purpose of the present invention, the term filler material in the meaning of the present invention refers to substances of mineral origin added to materials such as paper, plastic, rubber, paints and adhesives, and the like, to reduce the consumption of more expensive materials such as binders, or to improve the technical properties of products. Those skilled in the art are well aware of typical filler materials used in their respective fields. In addition, the term calcium carbonate-containing filler material refers to a material that contains at least 80% by weight of calcium carbonate, based on the total dry weight of the calcium carbonate-containing filler material.

The term surface-treated filler material product as used herein refers to a calcium carbonate-containing filler material that is contacted with a surface treatment agent so as to obtain a coating layer on at least a portion of the surface of the calcium carbonate-containing filler material.

The term succinic anhydride, also referred to as dihydro-2,5-furandione, succinic anhydride, or succinyl oxide, has the molecular formula C ₄ H ₄ O ₃ and is succinic acid anhydride.

The term monosubstituted succinic anhydride as used herein refers to succinic anhydride substituted with one substituent.

The term monosubstituted succinic acid as used herein refers to succinic acid substituted with one substituent.

The term dry filler material containing calcium carbonate is understood to be filler material containing less than 0.3 wt.% water relative to the mass of the filler material, % water (equal to the total residual moisture content) is determined according to the coulometric Karl-Fischer measurement method where the fill material is heated to 220° C. and the water content released as vapor and isolated using nitrogen gas flow (at 100 ml/min) is determined in a coulometric Karl-Fischer device.

The term salt reaction products of monosubstituted succinic anhydride(s) as used herein refers to products obtained by contacting a calcium carbonate containing filler material with one or more monosubstituted succinic anhydrides. These salt reaction products are formed from monosubstituted succinic acid, which is formed from the used monosubstituted succinic anhydride and reactive molecules located on the surface of the filler material containing calcium carbonate.

The term salt reaction products of a mixture of aliphatic linear or branched carboxylic acids containing stearic acid as used in the present invention refers to products obtained by contacting a filler material containing calcium carbonate with a mixture of aliphatic linear or branched carboxylic acids containing stearic acid. These salt reaction products are formed from a mixture of aliphatic linear or branched carboxylic acids containing stearic acid and reactive molecules located on the surface of the filler material containing calcium carbonate.

The treatment layer in the spirit of the present invention refers to a layer, preferably a monolayer, of a treatment agent on the surface of a product of a surface-treated filler material. The treatment layer mainly consists of at least one monosubstituted succinic anhydride and/or salt product(s) of its reaction and a mixture of aliphatic linear or branched carboxylic acids containing stearic acid in an amount of at least 10.0 wt.%, with respect to to the total mass of the mixture, and one or more additional saturated aliphatic linear or branched carboxylic acids containing a total number of carbon atoms from C ₁₂ to C ₂₄ and/or salt product (s) of their reaction.

The term generally in the meaning of the present invention refers to a treatment layer which contains compounds other than at least one monosubstituted succinic anhydride and/or salt reaction product(s) thereof and a mixture of aliphatic linear or branched carboxylic acids containing stearic acid in an amount at least 10.0 wt.% in relation to the total mass of the mixture, and one or more additional saturated aliphatic linear or branched carboxylic acids containing a total number of carbon atoms from C ₁₂ to C ₂₄ and / or salt product (s) of them reaction, in an amount of <5 wt.%, preferably <2 wt.%, and most preferably <1 wt.% in relation to the total weight of the treatment layer.

The specific surface area (SSA) of a calcium carbonate-containing fill material as used in the present invention is defined as the surface area of the calcium carbonate-containing fill material divided by its weight. As used herein, specific surface area is measured by nitrogen gas adsorption using the BET isotherm (ISO 9277:2010) and reported in m ² /g.

The particle size of particulate materials, for example, filler material containing calcium carbonate, is described herein by their particle size distribution d _x . The value of d _x is the diameter relative to which x mass particles have a diameter less than d _x . This means, for example, that the d ₂₀ value is the particle size for which 20% by weight of the total particles is smaller than this particle size. Thus the value of d ₅₀ represents the mass median particle size, ie 50 wt.% of all grains are larger, and the remaining 50 wt.% less than this particle size. For the purposes of the present invention, the particle size is indicated as the mass median particle size d ₅₀ unless otherwise indicated. The d ₉₈ value is the particle size for which 98% by weight of all particles are smaller than this particle size. The d ₉₈ value is also referred to as the maximum diameter. Particle sizes are determined using a Sedigraph™5100 or 5120 instrument, Micromeritics Instrument Corporation. The method and tool are known to those skilled in the art and are commonly used to determine particle sizes of fillers and pigments. The measurement is carried out in an aqueous solution of 0.1 wt.% Na ₄ P ₂ O ₇ . The samples are dispersed using a high speed stirrer and ultrasound.

The term molten state as used in the present invention is defined as the state in which the material is completely liquid, in other words, completely molten. Since the melting phenomenon occurs at a constant temperature when energy is applied, a substance is qualified as molten at the time after melting when the temperature begins to rise, as observed in the temperature versus energy input curve obtained by dynamic scanning calorimetry, DSC, (DIN 51005: 198311 ).

The term liquid state of the present invention refers to a material that is liquid at standard ambient temperature and pressure (SATP), which refers to a temperature of 298.15°K (25°C) and to an absolute pressure of exactly 100,000 Pa (1 bar, 14 .5 psi, 0.98692 atm).

When the term comprising is used in the present description and claims, this does not exclude other unspecified elements of great or small functional importance. For the purposes of the present invention, the term consisting of is considered to be the preferred embodiment of the term comprising. If further a certain group is defined as containing at least

- 5 041327 a certain number of embodiments, this is also to be understood as describing a group that preferably consists of only these embodiments.

When the terms including or having are used, these terms are intended to be equivalent to the term containing, as defined above.

When a noun is mentioned in the singular, this includes the plural of that noun, unless specifically stated otherwise.

According to another aspect of the present invention, there is provided a surface treated filler material product comprising:

a) at least one filler material containing calcium carbonate,

b) a treatment layer on the surface of at least one filler material containing calcium carbonate containing at least one monosubstituted succinic anhydride and/or at least one salt reaction product thereof and a mixture of aliphatic linear or branched carboxylic acids, consisting of stearic acid in amount of at least 10.0 wt.%, relative to the total mass of the mixture, and one or more additional saturated aliphatic linear or branched carboxylic acids containing a total number of carbon atoms from C ₁₂ to C ₂₄ , and/or a salt product (products ) their reactions, where the product of the surface-treated filler material contains a treatment layer in an amount of from 0.2 to 6 wt.%, in relation to the total dry weight of at least one filler material containing calcium carbonate.

Preferably, the product of the surface treated filler material is in the form of a powder. It is also preferred that the surface-treated filler material product can be obtained using the method as defined herein.

According to another aspect of the present invention, there is provided a polymer composition comprising at least one thermoplastic polymer resin and from 1 to 95% by weight, based on the total weight of the polymer composition, of a surface treated filler material product. Preferably, at least one thermoplastic polymer resin is at least one thermoplastic polymer, preferably a thermoplastic polymer selected from the group consisting of homopolymers and/or copolymers of polyolefins, polyamides, halogen-containing polymers and/or polyesters. It is also preferred that the polymer composition is a concentrate, preferably the concentrate contains a surface treated filler material product in an amount of 50 to 95 wt.%, preferably 60 to 85 wt.% and more preferably 70 to 80 wt.% with respect to to the total weight of the concentrate.

According to another aspect of the present invention, there is provided a thermoplastic polymer product comprising a surface treated filler material product and/or a polymer composition.

According to one embodiment of the present invention, the filler material containing calcium carbonate from step a) is selected from the group consisting of ground calcium carbonate, preferably marble, limestone, dolomite and/or chalk, precipitated calcium carbonate (PCC), preferably vaterite , calcite and/or aragonite, surface-reacted calcium carbonate (MCC) and mixtures thereof, more preferably the calcium carbonate-containing filler material is ground calcium carbonate.

According to another embodiment of the present invention, at least one calcium carbonate-containing filler material from step a) has a) a mass median particle size value in the range of 0.1 to 7 µm, preferably 0.25 to 5 µm, and most preferably 0.5 to 4 µm, and/or b) maximum diameter (d ₉₈ )<50 µm, preferably <40 µm, more preferably <25 µm, and most preferably <15 µm, and/or c) specific surface area (BET) 0.5 to 150 m ² /g, preferably 0.5 to 50 m ² /g, more preferably 0.5 to 35 m ² /g, and most preferably 0.5 to 10 m ² /g, as measured by the nitrogen BET method, and/or d) a residual total moisture content of 0.01 to 1% by weight, preferably 0.01 to 0.2% by weight, more preferably 0.02 up to 0.2 wt.%, and most preferably from 0.04 to 0.2 wt.%, in relation to the total dry weight of at least one filler material containing calcium carbonate.

According to another embodiment of the present invention, at least one calcium carbonate-containing filler material from step a) is preheated prior to contacting step d), preferably at least one calcium carbonate-containing filler material from step a) preheated at 20 to 200°C, more preferably 40 to 200°C, even more preferably 50 to 150°C, and most preferably 60 to 130°C.

According to one of the embodiments of the present invention, at least one monosubstituted succinic anhydride from step b) consists of succinic anhydride monosubstituted with a group selected from a linear, branched, aliphatic and cyclic group containing a total number of carbon atoms from C ₂ to C ₃₀ , preferably C ₃ to C ₂₅ , and most preferably C ₄ to C ₂₀ in the substituent.

According to another embodiment of the present invention, at least one monosubstituted succinic anhydride from step b) is a) at least one alkyl monosubstituted succinic anhydride, preferably at least one alkyl monosubstituted succinic anhydride, selected from the group consisting of ethyl succinic anhydride, propyl succinic anhydride, бутилянтарный ангидрид, триизобутилянтарный ангидрид, пентилянтарный ангидрид, гексилянтарный ангидрид, гептилянтарный ангидрид, октилянтарный ангидрид, нонилянтарный ангидрид, децилянтарный ангидрид, додецилянтарный ангидрид, гексадеканилянтарный ангидрид, октадеканилянтарный ангидрид и их смеси, и/или b) по меньшей мере один алкенилмонозамещенный янтарный ангидрид, предпочтительноо at least one alkenyl monosubstituted succinic anhydride selected from the group consisting of ethenyl succinic anhydride, propenyl succinic anhydride, butenyl succinic anhydride, triisobutenyl succinic anhydride, pentenyl succinic anhydride, hexenyl succinic anhydride anhydride, heptenylsuccinic anhydride, octenylsuccinic anhydride, nonenylsuccinic anhydride, decenylsuccinic anhydride, dodecenylsuccinic anhydride, hexadecenylsuccinic anhydride, octadecenylsuccinic anhydride and mixtures thereof.

According to another embodiment of the present invention, the mixture of saturated aliphatic linear or branched carboxylic acids from step c) contains stearic acid and one or more additional saturated aliphatic linear or branched carboxylic acids containing a total number of carbon atoms from C ₁₂ to C ₂₂ , preferably from C ₁₂ to C ₂₀ , and most preferably C ₁₄ to C ₂₀ .

According to one embodiment of the present invention, contacting step d) is carried out, wherein at least one monosubstituted succinic anhydride from step b) and a mixture of saturated aliphatic linear or branched carboxylic acids from step c) are added at a weight ratio of [succinic anhydride/mixture carboxylic acids] from 10:1 to 1:10, preferably from 5:1 to 1:5, and most preferably from 4:1 to 1:4, for example, from 4:1 to 1:1.

According to another embodiment of the present invention, at least one monosubstituted succinic anhydride from step b) is added in contacting step d) in a total amount of 0.1 to 3 wt%, preferably 0.2 to 2 wt%, and most preferably from 0.3 to 1.5 wt.% in relation to the total dry weight of at least one filler material containing calcium carbonate from step a); and the mixture of saturated aliphatic linear or branched carboxylic acids from step c) is added in contacting step d) in a total amount of 0.1 to 3% by weight, preferably 0.2 to 2% by weight, and most preferably 0 3 to 1.5 wt.% in relation to the total dry weight of at least one filler material containing calcium carbonate from stage a).

According to another embodiment of the present invention, step d) of bringing into contact is carried out at a temperature of from 20 to 200°C, preferably from 40 to 150°C, and most preferably from 60 to 130°C.

According to one embodiment of the present invention, step d) of bringing into contact is carried out, wherein at least one monosubstituted succinic anhydride from step b) and a mixture of saturated aliphatic linear or branched carboxylic acids from step c) are added simultaneously, or a mixture of saturated aliphatic linear or branched carboxylic acids from step c) are added after at least one monosubstituted succinic anhydride from step b), preferably a mixture of saturated aliphatic linear or branched carboxylic acids from step c) is added after at least one monosubstituted succinic anhydride from step b ).

According to another embodiment of the present invention, at least one monosubstituted succinic anhydride is supplied in step b) in such an amount that the total weight of said at least one monosubstituted succinic anhydride and/or salt product(s) of its reaction on the surface of at least one material filler containing calcium carbonate, less than 5 mg/m ² , for example is from 0.1 to 5 mg/m ² , preferably less than 4.5 mg/m ² , more preferably less than 4.0 mg/m ² , for example is from 0.2 to 4 mg/m ² or from 1 to 4 mg/m ² of at least one filler material containing calcium carbonate obtained in step a) and/or a mixture of saturated aliphatic linear or branched carboxylic acids from step c) is fed to step c) in such an amount that the total weight of the mixture of saturated aliphatic linear or branched carboxylic acids and/or salt product(s) of their reaction on the surface of the product surface of the hard-treated filler material is less than 5 mg/m ² , for example, is from 0.1 to 5 mg/m ² , preferably less than 4.5 mg/m ² , more preferably less than 4.0 mg/m ² , for example is from 0.2 to 4 mg/m ² or 1 to 4 mg/m ² of at least one filler material containing calcium carbonate obtained in step a).

As above, the process of the present invention for preparing a surface-treated filler material product with monosubstituted succinic anhydride(s) and a mixture of aliphatic linear or branched carboxylic acids containing stearic acid,

- 7 041327 includes at least process steps a), b), c) and d). In the following, additional details of the present invention are mentioned, and in particular the preceding steps of the method of the present invention for preparing a surface-treated filler material product.

Characterization of step a): obtaining at least one filler material containing calcium carbonate.

According to step a) of the method of the present invention, at least one filler material is obtained containing calcium carbonate.

The expression at least one filler material containing calcium carbonate means that one or more, for example two or three filler materials containing calcium carbonate can be obtained. According to a preferred embodiment, in step a), only one filler material containing calcium carbonate is obtained.

According to a preferred embodiment of the present invention, the calcium carbonate containing material is selected from the group consisting of ground calcium carbonate (GCC), preferably marble, limestone, dolomite and/or chalk, precipitated calcium carbonate (PCC), preferably vaterite, calcite and/ or aragonite, surface reacted calcium carbonate (MCC) and mixtures thereof, more preferably at least one calcium carbonate containing material is ground calcium carbonate.

GCC is understood to be a naturally occurring form of calcium carbonate mined from sedimentary rocks such as limestone or chalk, or from metamorphic marbles, and processed through processing such as grinding, screening and/or fractionating in wet and/or dry form, for example, using a cyclone or a classifier. In one embodiment of the present invention, the GCC is selected from the group consisting of marble, chalk, dolomite, limestone, and mixtures thereof.

In contrast, PCC-type calcium carbonate includes synthetic calcium carbonate products obtained by carbonizing a calcium hydroxide slurry, commonly referred to in the art as lime slurry or milk of lime, when prepared from fine particles of calcium oxide in water, or by precipitating an ionic salt solution. The PCC may be rhombohedral and/or scalenohedral and/or aragonite; preferred synthetic calcium carbonate or precipitated calcium carbonate includes aragonite, vaterite or calcite mineralogical crystal forms or mixtures thereof.

Surface-reacted calcium carbonate within the meaning of the present invention may refer to natural ground or precipitated calcium carbonate with modification of internal structure or surface-reacted product.

In one preferred embodiment, at least one filler material containing calcium carbonate is marble.

Obviously, the amount of calcium carbonate in at least one of the filler materials containing calcium carbonate is at least 80 wt.%, for example at least 95 wt.%, preferably in the range between 97 and 100 wt.%, more preferably between 98.5 and 99.95 wt.% in relation to the total dry weight of at least one filler material containing calcium carbonate.

The at least one calcium carbonate-containing filler material is preferably in the form of a particulate material and may have a particle size distribution as is commonly used for the material(s) used in the type of product to be produced. It is generally preferred that the at least one calcium carbonate-containing fill material has a mass median particle size in the range of 0.1 to 7 microns. For example, at least one filler material containing calcium carbonate has a mass median particle size d ₅₀ from 0.25 to 5 microns and preferably from 0.5 to 4 microns.

Additionally or alternatively, at least one filler material containing calcium carbonate has a maximum diameter (d ₉₈ )<50 µm. For example, at least one filler material containing calcium carbonate has a maximum diameter (d ₉₈ )<40 microns, preferably <25 microns, and most preferably <15 microns.

It is further preferred that at least one filler material containing calcium carbonate has a BET specific surface area between 0.5 and 150 m ² /g, as measured by the nitrogen BET method. For example, at least one filler material containing calcium carbonate has a specific surface area (BET) from 0.5 to 50 m ² /g, more preferably from 0.5 to 35 m ² /g, and most preferably from 0. 5 to 10 m ² /g, as measured by the BET method with nitrogen.

Thus, it is preferable that at least one filler material containing calcium carbonate has

a) a weight median particle size d ₅₀ in the range of 0.1 to 7 µm, preferably 0.25 µm to 5 µm, and most preferably 0.5 µm to 4 µm, and/or

- 8 041327

b) maximum diameter (d ₉₈ )<50 µm, preferably <40 µm, more preferably <25 µm, and most preferably <15 µm, and/or

c) a specific surface area (BET) from 0.5 to 150 m ² /g, preferably from 0.5 to 50 m ² /g, more preferably from 0.5 to 35 m ² /g, and most preferably from 0, 5 to 10 m ² /g, as measured by the BET method with nitrogen.

For example, at least one filler material containing calcium carbonate has

a) a weight median particle size d ₅₀ in the range of 0.1 to 7 µm, preferably 0.25 to 5 µm, and most preferably 0.5 to 4 µm, or

b) maximum diameter (d ₉₈ )<50 µm, preferably <40 µm, more preferably <25 µm, and most preferably <15 µm, or

c) a specific surface area (BET) from 0.5 to 150 m ² /g, preferably from 0.5 to 50 m ² /g, more preferably from 0.5 to 35 m ² /g, and most preferably from 0, 5 to 10 m ² /g, as measured by the BET method with nitrogen.

Preferably at least one filler material containing calcium carbonate has

a) a weight median particle size d ₅₀ in the range of 0.1 to 7 µm, preferably 0.25 to 5 µm, and most preferably 0.5 to 4 µm, and

b) maximum diameter (d ₉₈ )<50 µm, preferably <40 µm, more preferably <25 µm, and most preferably <15 µm, and

c) a specific surface area (BET) from 0.5 to 150 m ² /g, preferably from 0.5 to 50 m ² /g, more preferably from 0.5 to 35 m ² /g, and most preferably, from 0.5 to 10 m ² /g, as measured by the BET method with nitrogen.

In one of the embodiments of the present invention, at least one filler material containing calcium carbonate is preferably marble, having a mass median particle diameter d ₅₀ value of from 0.1 to 7 μm, preferably from 0.25 to 5 μm, and most preferably 0.5 to 4 µm. In this case, at least one filler material containing calcium carbonate exhibits a BET specific surface area of 0.5 to 150 m ² /g, preferably 0.5 to 50 m ² /g, more preferably 0.5 to 35 m ² /g, and most preferably from 0.5 to 10 m ² /g, as measured by nitrogen BET.

Preferably, the at least one calcium carbonate-containing filler material is a dry ground material, a wet ground and dried material, or a mixture of the materials discussed above. As a rule, the grinding step can be carried out using any conventional grinding device, for example, under such conditions that the grinding mainly occurs as a result of collisions with the secondary body, that is, in one or more devices from a ball mill, a rod mill, a vibrating mill, a roller crusher, centrifugal impact mill, vertical ball mill, attritor mill, needle mill, hammer mill, pulverizer, shredder, lump breaker, knife cutter, or other such equipment known to those skilled in the art.

In the case where at least one calcium carbonate-containing filler material is a wet-ground calcium carbonate-containing filler material, the grinding step may be carried out under such conditions that autogenous grinding takes place and/or by grinding into horizontal ball mill, and/or other such methods known to the person skilled in the art. The wet-processed particulate filler material containing calcium carbonate thus obtained can be washed and dehydrated by well-known methods, for example by flocculation, filtration or forced evaporation before drying. The next drying step may be carried out in one step, such as spray drying, or at least two steps, for example, by applying a first heating step to the calcium carbonate-containing fill material to reduce the bound moisture content to a level that does not exceed about 0.5 wt.% in relation to the total dry weight of at least one filler material containing calcium carbonate. The residual total moisture content of the filler can be measured using a coulometric Karl-Fischer titration method, desorbing the moisture in an oven at 195°C and introducing it continuously into a KF coulometer (coulometric KF Titrator C30, Mettler Toledo, combined with a Mettler DO 0337 oven) using a dry N2 at 100 ml/min for 10 min. The residual total moisture content can be determined using a calibration curve, and a veil of gas flow for 10 minutes without a sample must also be taken into account. The residual total moisture content can be further reduced by applying a second heating stage to at least one filler material containing calcium carbonate. In the case where said drying is carried out in several drying stages, the first stage may be carried out by heating the hot air stream, while the second and other drying stages are preferably carried out

- 9 041327 using indirect heating, in which the atmosphere in a suitable container contains a surface treatment agent. It is also common that at least one calcium carbonate-containing fill material is subjected to an enrichment step (such as a flotation, bleaching or magnetic separation step) to remove impurities.

In one embodiment of the present invention, at least one calcium carbonate-containing fill material comprises dry-ground calcium carbonate-containing fill material. In another preferred embodiment, the at least one calcium carbonate-containing fill material is wet ground in a horizontal ball mill and then dried using a well known spray drying process.

Depending on at least one filler material containing calcium carbonate, this at least one filler material containing calcium carbonate preferably has a residual total moisture content of from 0.01 to 1 wt.%, preferably from 0.01 to 0, 2 wt.%, more preferably from 0.02 to 0.2 wt.%, and most preferably from 0.04 to 0.2 wt.% in relation to the total dry weight of at least one filler material containing calcium carbonate.

For example, in the case where the at least one calcium carbonate-containing filler material is wet-ground and spray-dried marble, the residual total moisture content of the at least one calcium carbonate-containing filler material is preferably from 0.01 up to 0.1 wt.%, more preferably from 0.02 to 0.08 wt.%, and most preferably from 0.04 to 0.07 wt.% in relation to the total dry weight of at least one filler material containing calcium carbonate. If PCC is used as the at least one calcium carbonate-containing fill material, the residual total moisture content of the at least one calcium carbonate-containing fill material is preferably 0.01 to 0.2 mass%, more preferably 0 05 to 0.17 wt.%, and most preferably from 0.05 to 0.15 wt.%, in relation to the total dry weight of at least one filler material containing calcium carbonate.

Characterization of step b): obtaining at least one monosubstituted succinic anhydride.

According to step b) of the process of the present invention, at least one monosubstituted succinic anhydride is obtained.

Obviously, the expression at least one monosubstituted succinic anhydride means that one or more kinds of monosubstituted succinic anhydride can be obtained in the process of the present invention.

Accordingly, it should be noted that at least one monosubstituted succinic anhydride may be one kind of monosubstituted succinic anhydride(s). Alternatively, the at least one monosubstituted succinic anhydride may be a mixture of two or more kinds of monosubstituted succinic anhydrides. For example, at least one monosubstituted succinic anhydride may be a mixture of two or three types of monosubstituted succinic anhydride, for example, two types of monosubstituted succinic anhydride.

In one of the embodiments of the present invention, at least one monosubstituted succinic anhydride is one kind of monosubstituted succinic anhydride.

Obviously, at least one monosubstituted succinic anhydride is a surface treatment agent and consists of succinic anhydride monosubstituted with a group selected from any linear, branched, aliphatic and cyclic group containing a total number of carbon atoms from C ₂ to C ₃₀ in the substituent .

In one embodiment of the present invention, at least one monosubstituted succinic anhydride consists of monosubstituted succinic anhydride with a group selected from a linear, branched, aliphatic and cyclic group containing a total number of carbon atoms from C ₃ to C ₂₅ in the substituent. For example, at least one monosubstituted succinic anhydride consists of succinic anhydride monosubstituted with a group selected from a linear, branched, aliphatic, and cyclic group containing a total of C ₄ to C ₂₀ carbon atoms in the substituent.

In one embodiment of the present invention, at least one monosubstituted succinic anhydride consists of monosubstituted succinic anhydride with one group, which is a linear and aliphatic group containing a total number of carbon atoms from C ₂ to C ₃₀ , preferably from C ₃ to C ₂₅ , and most preferably C ₄ to C ₂₀ in the substituent. In addition or alternatively, at least one monosubstituted succinic anhydride consists of monosubstituted succinic anhydride with one group, which is a branched and aliphatic group containing a total number of carbon atoms from C ₂ to C ₃₀ , preferably from C ₃ to C ₂₅ , and most preferably C ₄ to C ₂₀ in the substituent.

Thus, preferably, at least one monosubstituted succinic anhydride consists of succinic anhydride monosubstituted with one linear or branched alkyl group containing a total number of carbon atoms from C ₂ to

C ₃₀ , preferably C ₃ to C ₂₅ and most preferably C ₄ to C ₂₀ in the substituent.

For example, at least one monosubstituted succinic anhydride consists of succinic anhydride monosubstituted with one group that is a linear alkyl group containing a total number of carbon atoms from C ₂ to C ₃₀ , preferably from C ₃ to C ₂₅ , and most preferably from C ₄ up to C ₂₀ in the substituent. In addition or alternatively, at least one monosubstituted succinic anhydride consists of monosubstituted succinic anhydride with one group, which is a branched alkyl group containing a total number of carbon atoms from C ₂ to C ₃₀ , preferably from C ₃ to C ₂₅ , and most preferably C ₄ to C ₂₀ in the substituent.

The term alkyl as used herein refers to a linear or branched, saturated organic compound composed of carbon and hydrogen. In other words, alkyl monosubstituted succinic anhydrides consist of linear or branched, saturated hydrocarbon chains containing a side group of succinic anhydride.

In one embodiment of the present invention, the at least one monosubstituted succinic anhydride is at least one monosubstituted succinic anhydride with linear or branched alkyl. Например, по меньшей мере один алкилмонозамещенный янтарный ангидрид выбирают из группы, включающей этилянтарный ангидрид, пропилянтарный ангидрид, бутилянтарный ангидрид, триизобутилянтарный ангидрид, пентилянтарный ангидрид, гексилянтарный ангидрид, гептилянтарный ангидрид, октилянтарный ангидрид, нонилянтарный ангидрид, децилянтарный ангидрид, додецилянтарный ангидрид, гексадеканилянтарный ангидрид, octadecanyl succinic anhydride; and mixtures thereof.

Accordingly, it is clear that, for example, the term butylsuccinic anhydride includes linear and branched butylsuccinic anhydride(s). One specific example of linear butyl succinic anhydrides is n-butyl succinic anhydride. Specific examples of branched butyl succinic anhydride(s) are isobutyl succinic anhydride, sec-butyl succinic anhydride and/or t-butyl succinic anhydride.

In addition, it is clear that, for example, the term hexadecanylsuccinic anhydride includes linear and branched hexadecanylsuccinic anhydride(s). One specific example of linear hexadecanylsuccinic anhydride(s) is n-hexadecanylsuccinic anhydride. Конкретные примеры разветвленного гексадеканилянтарного ангидрида (ангидридов) представляют собой 14-метилпентадеканилянтарный ангидрид, 13-метилпентадеканилянтарный ангидрид, 12-метилпентадеканилянтарный ангидрид, 11-метилпентадеканилянтарный ангидрид, 10-метилпентадеканилянтарный ангидрид, 9-метилпентадеканилянтарный ангидрид, 8-метилпентадеканилянтарный ангидрид, 7-метилпентадеканилянтарный ангидрид, 6-метилпентадеканилянтарный ангидрид, 5метилпентадеканилянтарный ангидрид, 4-метилпентадеканилянтарный ангидрид, 3-метилпентадеканилянтарный ангидрид, 2-метилпентадеканилянтарный ангидрид, 1-метилпентадеканилянтарный ангидрид, 13-этилбутадеканилянтарный ангидрид, 12-этилбутадеканилянтарный ангидрид, 11-этилбутадеканилянтарный ангидрид, 10-этилбутадеканилянтарный ангидрид, 9- ethylbutadecanylsuccinic anhydride, 8-ethylbutadecanylsuccinic anhydride, 7-ethylbutadecanylsuccinic anhydride, 6-ethylbutadecanylsuccinic anhydride, 5-ethylbutadecanylsuccinic anhydride, 4-ethylbutadecanylsuccinic anhydride, 3- этилбутадеканилянтарный ангидрид, 2-этилбутадеканилянтарный ангидрид, 1-этилбутадеканилянтарный ангидрид, 2-бутилдодеканилянтарный ангидрид, 1-гексилдеканилянтарный ангидрид, 1гексил-2-деканилянтарный ангидрид, 2-гексилдеканилянтарный ангидрид, 6,12-диметилбутадеканилянтарный ангидрид, 2,2-диэтилдодеканилный ангидрид, 4 ,8,12-trimethyltridecanylsuccinic anhydride, 2,2,4,6,8-pentamethylundecanysuccinic anhydride, 2-ethyl-4-methyl-2-(2-methylpentyl)heptylsuccinic anhydride and/or 2-ethyl-4,6-dimethyl -2-propylnonyl succinic anhydride.

In addition, it is clear that, for example, the term octadecanyl succinic anhydride includes linear and branched octadecanyl succinic anhydride (anhydrides). One specific example of linear octadecanylsuccinic anhydride(s) is n-octadecanylsuccinic anhydride. Конкретные примеры разветвленного гексадеканил-янтарного ангидрида (ангидридов) представляют собой 16-метилгептадеканилянтарный ангидрид, 15-метилгептадеканилянтарный ангидрид, 14метилгептадеканилянтарный ангидрид, 13-метилгептадеканилянтарный ангидрид, 12-метилгептадеканилянтарный ангидрид, 11-метилгептадеканилянтарный ангидрид, 10-метилгептадеканилянтарный ангидрид, 9-метилгептадеканилянтарный ангидрид, 8-метилгептадеканилянтарный ангидрид, 7-метилгептадеканилянтарный ангидрид, 6-метилгептадеканилянтарный ангидрид, 5-метилгептадеканилянтарный ангидрид, 4-метилгептадеканилянтарный ангидрид, 3-метилгептадеканилянтарный ангидрид, 2метилгептадеканилянтарный ангидрид, 1-метилгептадеканилянтарный ангидрид, 14-этилгексадеканилянтарный ангидрид, 13-этилгексадеканилянтарный ангидрид, 12- ethylhexadecanylsuccinic anhydride, 11-ethylhexadecanylsuccinic anhydride, 10-ethylhexadecanylsuccinic anhydride, 9-ethylhexadecanylsuccinic anhydride, 8-ethylhexadecanylsuccinic anhydride, 7-ethylhexadecanylsuccinic anhydride ый ангидрид, 6-этилгексадеканилянтарный ангидрид, 5-этилгексадеканилянтарный ангидрид, 4-этилгекса- 11 041327 деканилянтарный ангидрид, 3-этилгексадеканилянтарный ангидрид, 2-этилгексадеканилянтарный ангидрид, 1-этилгексадеканилянтарный ангидрид, 2-гексилдодеканилянтарный ангидрид, 2-гептилундеканилянтарный ангидрид, изооктадеканилянтарный ангидрид и /or 1-octyl-2-decanylsuccinic anhydride.

In one embodiment of the present invention, the at least one alkyl monosubstituted succinic anhydride is selected from the group consisting of butylsuccinic anhydride, hexylsuccinic anhydride, heptylsuccinic anhydride, octysuccinic anhydride, hexadecanylsuccinic anhydride, octadecanylsuccinic anhydride, and mixtures thereof.

In one embodiment of the present invention, the at least one monosubstituted succinic anhydride is one kind of alkyl monosubstituted succinic anhydride. For example, one alkyl monosubstituted succinic anhydride is butyl succinic anhydride. Alternatively, one alkyl monosubstituted succinic anhydride is hexyl succinic anhydride. Alternatively, one alkyl monosubstituted succinic anhydride is heptylsuccinic anhydride or octysuccinic anhydride. Alternatively, one alkyl monosubstituted succinic anhydride is hexadecanylsuccinic anhydride. For example, one alkyl monosubstituted succinic anhydride is a linear hexadecanylsuccinic anhydride such as nhexadecanylsuccinic anhydride or a branched hexadecanylsuccinic anhydride such as 1hexyl-2-decanylsuccinic anhydride. Alternatively, one alkyl monosubstituted succinic anhydride is octadecanyl succinic anhydride. For example, one alkyl monosubstituted succinic anhydride is a linear octadecanyl succinic anhydride such as n-octadecanyl succinic anhydride or a branched octadecanyl succinic anhydride such as isooctadecanyl succinic anhydride or 1-octyl-2-decanyl succinic anhydride.

In one embodiment of the present invention, the one alkyl monosubstituted succinic anhydride is butyl succinic anhydride, such as n-butyl succinic anhydride.

In one embodiment of the present invention, the at least one monosubstituted succinic anhydride is a mixture of two or more types of alkyl monosubstituted succinic anhydrides. For example, at least one monosubstituted succinic anhydride is a mixture of two or three kinds of alkyl monosubstituted succinic anhydrides.

In one of the embodiments of the present invention, at least one monosubstituted succinic anhydride consists of monosubstituted succinic anhydride with one group representing a linear or branched alkenyl group containing a total number of carbon atoms from C ₂ to C ₃₀ , preferably from C ₃ to C ₂₅ , and most preferably from C ₄ to C ₂₀ in the Deputy.

The term alkenyl as used herein refers to a linear or branched, unsaturated organic compound composed of carbon and hydrogen. Said organic compound additionally contains at least one double bond in the substituent, preferably one double bond. In other words, alkenyl monosubstituted succinic anhydrides consist of linear or branched, unsaturated hydrocarbon chains containing a side group of succinic anhydride. Obviously, the term alkenyl in the meaning of the present invention includes cis and trans isomers.

In one embodiment of the present invention, the at least one monosubstituted succinic anhydride is at least one linear or branched alkenyl monosubstituted succinic anhydride. Например, по меньшей мере один алкенилмонозамещенный янтарный ангидрид выбирают из группы, включающей этенилянтарный ангидрид, пропенилянтарный ангидрид, бутенилянтарный ангидрид, триизобутенилянтарный ангидрид, пентенилянтарный ангидрид, гексенилянтарный ангидрид, гептенилянтарный ангидрид, октенилянтарный ангидрид, ноненилянтарный ангидрид, деценилянтарный ангидрид, додеценилянтарный ангидрид, гексадеценилянтарный ангидрид, octadecenyl succinic anhydride; and mixtures thereof.

Accordingly, it is clear that, for example, the term hexadecenylsuccinic anhydride includes linear and branched hexadecenylsuccinic anhydride(s). Один из конкретных примеров линейного гексадеценилянтарного ангидрида (ангидридов) представляет собой н-гексадеценилянтарный ангидрид, такой как 14-гексадеценилянтарный ангидрид, 13-гексадеценилянтарный ангидрид, 12гексадеценилянтарный ангидрид, 11-гексадеценилянтарный ангидрид, 10-гексадеценилянтарный ангидрид, 9-гексадеценилянтарный ангидрид, 8-гексадеценилянтарный anhydride, 7-hexadecenylsuccinic anhydride, 6-hexadecenylsuccinic anhydride, 5-hexadecenylsuccinic anhydride, 4-hexadecenylsuccinic anhydride, 3-hexadecenylsuccinic anhydride and/or 2-hexadecenylsuccinic anhydride. Specific examples of branched hexadecenylsuccinic anhydride(s) are 14methyl-9-pentadecenylsuccinic anhydride, 14-methyl-2-pentadecenylsuccinic anhydride, 1-hexyl-2decenylsuccinic anhydride, and/or isohexadecenylsuccinic anhydride.

In addition, it is clear that, for example, the term octadecenylsuccinic anhydride includes linear and branched octadecenylsuccinic anhydride (anhydrides). One of the specific examples of the linear octadelyantar anhydride (angidrides) is N-octadesenantary anhydride, such as 16-octade-eyedalic anhydride, 15-octade-eyedalic anhydride, 14-2 041327 Octade-Cosephenic anhydride, 13-octadic anhidride, 12-Octaretherals, 12-October of 12- Angidride, 10-octadelyantary anhydride, 9-octade-core anhydride, 8-octadelyantary anhydride, 7-octade-eyedalic anhydride, 6-octade anhydride, 5-octade anhydride, 4-oxide anhydride, 3-octaneous anhydrodalic anhydrodalic anhydrodalistan. Specific examples of branched octadecenylsuccinic anhydride(s) are 16-methyl-9-heptadecenylsuccinic anhydride, 16methyl-7-heptadecenylsuccinic anhydride, 1-octyl-2-decenylsuccinic anhydride, and/or isooctadecenylsuccinic anhydride.

In one embodiment of the present invention, the at least one alkenyl monosubstituted succinic anhydride is selected from the group consisting of hexenyl succinic anhydride, octenyl succinic anhydride, hexadecenyl succinic anhydride, octadecenyl succinic anhydride, and mixtures thereof.

In one embodiment of the present invention, the at least one monosubstituted succinic anhydride is one alkenyl monosubstituted succinic anhydride. For example, one alkenyl monosubstituted succinic anhydride is hexenyl succinic anhydride. Alternatively, one alkenyl monosubstituted succinic anhydride is octenyl succinic anhydride. Alternatively, one alkenyl monosubstituted succinic anhydride is hexadecenyl succinic anhydride. For example, one alkenyl monosubstituted succinic anhydride is a linear hexadecenyl succinic anhydride such as n-hexadecenyl succinic anhydride or a branched hexadecenyl succinic anhydride such as 1-hexyl-2-decenyl succinic anhydride. Alternatively, one alkenyl monosubstituted succinic anhydride is octadecenyl succinic anhydride. For example, one alkyl monosubstituted succinic anhydride is a linear octadecenylsuccinic anhydride such as n-octadecenylsuccinic anhydride or a branched octadecenylsuccinic anhydride such as isooctadecenylsuccinic anhydride, or 1-octyl-2decenylsuccinic anhydride.

In one embodiment of the present invention, the one alkenyl monosubstituted succinic anhydride is a linear octadecenyl succinic anhydride, such as n-octadecenyl succinic anhydride. In another embodiment of the present invention, the one alkenyl monosubstituted succinic anhydride is a linear octenyl succinic anhydride, such as octenyl succinic anhydride.

If at least one monosubstituted succinic anhydride is one alkenyl monosubstituted succinic anhydride, it is clear that one alkenyl monosubstituted succinic anhydride is present in an amount of >95 wt.%, and preferably >96.5 wt.%, relative to the total mass at least one monosubstituted succinic anhydride obtained in step b).

In one embodiment of the present invention, the at least one monosubstituted succinic anhydride is a mixture of two or more types of alkenyl monosubstituted succinic anhydrides. For example, at least one monosubstituted succinic anhydride is a mixture of two or three kinds of alkenyl monosubstituted succinic anhydrides.

When at least one monosubstituted succinic anhydride is a mixture of two or more kinds of alkenyl monosubstituted succinic anhydride, one alkenyl monosubstituted succinic anhydride is a linear or branched octadecenyl succinic anhydride, while each additional alkenyl monosubstituted succinic anhydride is selected from ethenyl succinic anhydride, propenyl succinic anhydride, butyl succinic anhydride , pentenylsuccinic anhydride, hexenylsuccinic anhydride, heptenylsuccinic anhydride, nonenylsuccinic anhydride, hexadecenylsuccinic anhydride and mixtures thereof. For example, at least one monosubstituted succinic anhydride is a mixture of two or more types of alkenyl monosubstituted succinic anhydride, where one alkenyl monosubstituted succinic anhydride is a linear octadecenyl succinic anhydride, and each additional alkenyl monosubstituted succinic anhydride is selected from ethenyl succinic anhydride, propenyl succinic anhydride, butene anhydride , hexenylsuccinic anhydride, heptenylsuccinic anhydride, nonenylsuccinic anhydride, hexadecenylsuccinic anhydride and mixtures thereof. Альтернативно, по меньшей мере один монозамещенный янтарный ангидрид представляет собой смесь двух или более видов алкенилмонозамещенных янтарных ангидридов, где один алкенилмонозамещенный янтарный ангидрид представляет собой разветвленный октадеценилянтарный ангидрид, а каждый дополнительный алкенилмонозамещенный янтарный ангидрид выбирают из этенилянтарного ангидрида, пропенилянтарного ангидрида, бутенилянтарного ангидрида, пентенилянтарного ангидрида , hexenylsuccinic anhydride, heptenylsuccinic anhydride, nonenylsuccinic anhydride, hexadecenylsuccinic anhydride and mixtures thereof.

For example, at least one monosubstituted succinic anhydride is a mixture of two or more kinds of alkenyl monosubstituted succinic anhydrides containing one or more hexadecenylsuccinic anhydrides, like linear or branched hexadecenylsuccinic anhydride(s), and one or more octadecenylsuccinic anhydrides, like linear or branched octadecenyl anhydride. (anhydrides).

- 13 041327

In one embodiment of the present invention, the at least one monosubstituted succinic anhydride is a mixture of two or more alkenyl monosubstituted succinic anhydrides containing linear hexadecenylsuccinic anhydride(s) and linear octadecenylsuccinic anhydride(s). Alternatively, the at least one monosubstituted succinic anhydride is a mixture of two or more kinds of alkenyl monosubstituted succinic anhydrides containing branched hexadecenylsuccinic anhydride(s) and branched octadecenylsuccinic anhydride(s). For example, one or more hexadecenylsuccinic anhydrides are linear hexadecenylsuccinic anhydride, like hexadecenylsuccinic anhydride, and/or branched hexadecenylsuccinic anhydride, like 1-hexyl-2-decenylsuccinic anhydride. Additionally or alternatively, one or more octadecenylsuccinic anhydrides are linear octadecenylsuccinic anhydride like n-octadecenylsuccinic anhydride and/or branched octadecenylsuccinic anhydride like isooctadecenylsuccinic anhydride and/or 1-octyl-2-decenylsuccinic anhydride.

If at least one monosubstituted succinic anhydride is a mixture of two or more types of alkenyl monosubstituted succinic anhydrides, it is obvious that one alkenyl monosubstituted succinic anhydride is present in an amount of from 20 to 60 wt.%, and preferably from 30 to 50 wt.% in relation to the total weight of at least one monosubstituted succinic anhydride obtained in step b).

For example, if at least one monosubstituted succinic anhydride is a mixture of two or more kinds of alkenyl monosubstituted succinic anhydrides, containing one or more hexadecenylsuccinic anhydrides, like linear or branched hexadecenylsuccinic anhydride(s), and one or more octadecenylsuccinic anhydrides, like linear or branched hexadecenylsuccinic anhydrides anhydride(s), preferably one or more octadecenyl succinic anhydrides are present in an amount of from 20 to 60 wt.%, and preferably from 30 to 50 wt.% in relation to the total weight of at least one monosubstituted succinic anhydride obtained in stage b ).

It is also obvious that at least one monosubstituted succinic anhydride may be a mixture of at least one alkyl monosubstituted succinic anhydride and at least one alkenyl monosubstituted succinic anhydride.

If at least one monosubstituted succinic anhydride is a mixture of at least one alkyl monosubstituted succinic anhydride and at least one alkenyl monosubstituted succinic anhydride, it is clear that the alkyl substituent of at least one alkyl monosubstituted succinic anhydride and the alkenyl substituent of at least one alkenyl monosubstituted succinic anhydride are preferably are the same. For example, at least one monosubstituted succinic anhydride is a mixture of ethyl succinic anhydride and ethenyl succinic anhydride. Alternatively, at least one monosubstituted succinic anhydride is a mixture of propyl succinic anhydride and propenyl succinic anhydride. Alternatively, at least one monosubstituted succinic anhydride is a mixture of butyl succinic anhydride and butyl succinic anhydride. Alternatively, at least one monosubstituted succinic anhydride is a mixture of triisobutyl succinic anhydride and triisobutyl succinic anhydride. Alternatively, at least one monosubstituted succinic anhydride is a mixture of pentylsuccinic anhydride and pentenylsuccinic anhydride. Alternatively, at least one monosubstituted succinic anhydride is a mixture of hexyl succinic anhydride and hexenyl succinic anhydride. Alternatively, at least one monosubstituted succinic anhydride is a mixture of heptylsuccinic anhydride and heptenylsuccinic anhydride. Alternatively, the at least one monosubstituted succinic anhydride is a mixture of octysuccinic anhydride and octenylsuccinic anhydride. Alternatively, the at least one monosubstituted succinic anhydride is a mixture of nonyl succinic anhydride and nonyl succinic anhydride. Alternatively, at least one monosubstituted succinic anhydride is a mixture of decyl succinic anhydride and decenyl succinic anhydride. Alternatively, at least one monosubstituted succinic anhydride is a mixture of dodecyl succinic anhydride and dodecenyl succinic anhydride. Alternatively, the at least one monosubstituted succinic anhydride is a mixture of hexadecanysuccinic anhydride and hexadecenylsuccinic anhydride. For example, at least one monosubstituted succinic anhydride is a mixture of linear hexadecanysuccinic anhydride and linear hexadecenylsuccinic anhydride, or a mixture of branched hexadecanysuccinic anhydride and branched hexadecenylsuccinic anhydride. Alternatively, at least one monosubstituted succinic anhydride is a mixture of octadecanyl succinic anhydride and octadecenyl succinic anhydride. For example, at least one monosubstituted succinic anhydride is a mixture of linear octadecanyl succinic anhydride and linear octadecenyl succinic anhydride, or a mixture of branched octadecanyl succinic anhydride and branched octadecenyl succinic anhydride.

In one embodiment of the present invention, the at least one monosubstituted succinic anhydride is a mixture of nonyl succinic anhydride and nonyl succinic anhydride.

If at least one monosubstituted succinic anhydride is a mixture of at least one alkyl monosubstituted succinic anhydride and at least one alkenyl monosubstituted succinic anhydride, the weight ratio between at least one alkyl monosubstituted succinic anhydride and at least one alkenyl monosubstituted succinic anhydride is between 90 :10 and 10:90 (wt%/wt%). For example, the weight ratio between at least one alkyl monosubstituted succinic anhydride and at least one alkenyl monosubstituted succinic anhydride is between 70:30 and 30:70 (wt%/wt%), or between 60:40 and 40: 60.

Optionally, at least one monosubstituted succinic anhydride is obtained in combination with at least one monosubstituted succinic acid in step b) of the process of the present invention.

Obviously, the expression at least one mono-substituted succinic acid means that in step b) of the method of the present invention, one or more types of mono-substituted succinic acid can be obtained.

Accordingly, it should be noted that at least one monosubstituted succinic acid may be one kind of monosubstituted succinic acid. Alternatively, the at least one monosubstituted succinic acid may be a mixture of two or more types of monosubstituted succinic acid. For example, at least one monosubstituted succinic acid may be a mixture of two or three types of monosubstituted succinic acid, like two types of monosubstituted succinic acid.

In one of the embodiments of the present invention, at least one monosubstituted succinic acid is one type of monosubstituted succinic acid.

Obviously, at least one monosubstituted succinic acid is a surface treatment agent and consists of succinic acid, monosubstituted by a group selected from any linear, branched, aliphatic and cyclic group containing a total number of carbon atoms from C ₂ to C ₃₀ in the substituent .

In one of the embodiments of the present invention, at least one monosubstituted succinic acid consists of succinic acid, a monosubstituted group selected from a linear, branched, aliphatic and cyclic group containing a total number of carbon atoms from C ₃ to C ₂₅ in the substituent. For example, at least one monosubstituted succinic acid consists of succinic acid, monosubstituted by a group selected from a linear, branched, aliphatic and cyclic group containing a total number of carbon atoms from C ₄ to C ₂₀ in the substituent.

If at least one monosubstituted succinic anhydride is obtained using at least one monosubstituted succinic acid in step b) of the process, it is clear that at least one monosubstituted succinic anhydride and at least one monosubstituted succinic acid may contain the same or different substituents.

In one embodiment of the present invention, the succinic acid molecule of at least one monosubstituted succinic acid and the succinic anhydride molecule of at least one monosubstituted succinic anhydride are monosubstituted with the same group selected from any linear, branched, aliphatic, and cyclic group containing a common the number of carbon atoms from C ₂ to C ₃₀ preferably from C ₃ to C ₂₅ and most preferably from C4 to C20 in the substituent.

If at least one monosubstituted succinic anhydride is prepared in combination with at least one monosubstituted succinic acid, at least one monosubstituted succinic acid is present in an amount of <10 mol% relative to the total sum of moles of at least one monosubstituted succinic anhydride and at least one monosubstituted succinic acid. For example, at least one monosubstituted succinic acid is present in an amount of <5 mole, preferably <2.5 mole%, and most preferably <1 mole%, based on the sum of mole% of at least one monosubstituted succinic anhydride and at least one monosubstituted succinic acid.

In one embodiment of the present invention, at least one monosubstituted succinic anhydride and at least one monosubstituted succinic acid are obtained in step b) of the process.

If at least one monosubstituted succinic anhydride is obtained in combination with at least one monosubstituted succinic acid in step b) of the process, at least one monosubstituted succinic anhydride and at least one monosubstituted succinic acid are preferably obtained as a mixture.

To achieve improved flowability of the finished product and its improved dispersibility in

- 15 041327 polymer matrix of the polymer composition, it is obvious that at least one monosubstituted succinic anhydride is obtained in a total amount of from 0.1 to 3 wt.% in relation to the total dry weight of at least one filler material containing calcium carbonate.

For example, at least one monosubstituted succinic anhydride is obtained in an amount of from 0.1 to 2.5 wt.%, preferably in an amount of from 0.2 to 2 wt.%, more preferably in an amount of from 0.3 to 1.5 wt. %, even more preferably in an amount of from 0.3 to 1 wt.%, and most preferably in an amount of from 0.3 to 0.8 wt.% in relation to the total dry weight of at least one filler material containing calcium carbonate.

If at least one monosubstituted succinic anhydride is obtained in combination with at least one monosubstituted succinic acid in step b) of the process, at least one monosubstituted succinic anhydride and optionally at least one monosubstituted succinic acid are preferably obtained in a total amount of 0.1 up to 3 wt.%, preferably from 0.1 to 2.5 wt.%, more preferably from 0.2 to 2 wt.%, even more preferably from 0.3 to 1.5 wt.%, even more preferably from 0.3 to 1 wt.%, and most preferably from 0.3 to 0.8 wt.% in relation to the total dry weight of at least one filler material containing calcium carbonate.

Additionally or alternatively, at least one monosubstituted succinic anhydride and optionally at least one monosubstituted succinic acid of the present invention is preferably prepared in such an amount that the total weight of said at least one monosubstituted succinic anhydride and the optional at least one monosubstituted succinic acid acid on the surface of at least one filler material containing calcium carbonate less than 5 mg/m ² of at least one filler material containing calcium carbonate obtained in step a).

In one embodiment of the present invention, the at least one monosubstituted succinic anhydride and the optional at least one monosubstituted succinic acid of the present invention are preferably obtained in such an amount that the total weight of said at least one monosubstituted succinic anhydride and monosubstituted succinic acid and/or salt product(s) of their reaction on the surface of at least one filler material containing calcium carbonate is less than 4.5 mg/m ² and most preferably less than 4.0 mg/m ² of at least one filler material containing calcium carbonate obtained in step a).

For example, at least one monosubstituted succinic anhydride and optionally at least one monosubstituted succinic acid of the present invention is preferably obtained in such an amount that the total weight of at least one monosubstituted succinic anhydride and optional at least one monosubstituted succinic acid on the surface of the product surface -treated filler material is from 0.1 to 5 mg/m ² , more preferably from 0.2 to 4 mg/m ² , and most preferably from 1 to 4 mg/m ² of at least one filler material containing calcium carbonate obtained in step a).

In addition or alternatively, it should be noted that at least one monosubstituted succinic anhydride from step b) and optional at least one monosubstituted succinic acid of the process of the present invention are obtained in a molten or liquid state, i.e. said at least one monosubstituted succinic anhydride and optionally at least one monosubstituted succinic acid are characterized by a viscosity of less than 500, preferably less than 2500, more preferably less than 1000 mPa-s, and most preferably less than 500 mPa-s at +20°C (±2°C) at measurement using appropriate equipment, for example, Physica MCR 300 Rheometer (Paar Physica), equipped with a TEZ 150 R-C measuring cell and a CC 28.7 measuring system at a shear rate of 5 s ^-1 and at +20°C (±2°C ).

Characterization of step c): preparation of a mixture of aliphatic linear or branched carboxylic acids containing stearic acid.

According to step c) of the method according to the present invention, a mixture of aliphatic linear or branched carboxylic acids is obtained, containing stearic acid in an amount of at least 10.0 wt.%, relative to the total mass of the mixture, and one or more saturated aliphatic linear or branched carboxylic acids containing the total number of carbon atoms from C12 to C24.

The term mixture of aliphatic linear or branched carboxylic acids means that in step c) of the present invention, two or more aliphatic linear or branched carboxylic acids are prepared, provided that one of the two or more aliphatic linear or branched carboxylic acids is stearic acid. Preferably the mixture contains three or more, for example three or four or five aliphatic linear or branched carboxylic acids, provided that one of the three or more aliphatic linear or branched carboxylic acids is stearic acid.

- 16 041327

Specifically, it has been found that surface treatment of a filler material containing calcium carbonate with monosubstituted succinic anhydride(s) and a mixture of aliphatic linear or branched carboxylic acids containing stearic acid is advantageous for improving the flowability of a filler material containing calcium carbonate, compared to a material that surface treated only with monosubstituted succinic anhydride(s), i.e. without a mixture of aliphatic linear or branched carboxylic acids containing stearic acid. An additional advantage is that the dispersion of the resulting product in the polymer matrix in the polymer composition is improved compared to a material that is surface treated with monosubstituted succinic anhydride(s) only, i.e. without a mixture of aliphatic linear or branched carboxylic acids containing stearic acid.

Thus, one of the requirements of the present invention is that in step c) a mixture of aliphatic linear or branched carboxylic acids is obtained. Specifically, a mixture of aliphatic linear or branched carboxylic acids containing stearic acid has been found to be advantageous for the purposes of the present invention.

Thus, one of the specific requirements of the present invention is that the mixture of aliphatic linear or branched carboxylic acids contains stearic acid in an amount of at least 10.0 wt.%, for example from 10.0 to 98.0 wt.%, relative to the total weight of the mixture and that one or more additional saturated aliphatic linear or branched carboxylic acids, contains a total number of carbon atoms from C ₁₂ to C ₂₄ .

In one of the embodiments, the mixture of aliphatic linear or branched carboxylic acids contains stearic acid in an amount of at least 20.0 wt.%, for example from 20.0 to 98.0 wt.%, preferably at least 30.0 wt.% , for example from 30.0 to 98.0 wt.%, more preferably at least 40.0 wt.%, for example from 40.0 to 98.0 wt.%, and most preferably at least 50 wt.%, for example, from 50.0 to 98.0 wt.%, relative to the total weight of the mixture and one or more additional saturated aliphatic linear or branched carboxylic acids, contain a total number of carbon atoms from C ₁₂ to C ₂₄ . Accordingly, the mixture contains one or more additional saturated aliphatic linear or branched carboxylic acids containing a total number of carbon atoms from C ₁₂ to C ₂₄ in an amount equal to or less than 90.0 wt.%, for example from 2.0 to 90.0 wt. .%, preferably equal to or less than 80.0 wt.%, for example from 2.0 to 80.0 wt.%, more preferably equal to or less than 70.0 wt.%, for example from 2.0 to 70.0 wt. %, even more preferably equal to or less than 60.0 wt.%, for example from 2.0 to 60.0 wt.%, and most preferably equal to or less than 50.0 wt.%, for example from 2.0 to 50.0 wt.% relative to the total weight of the mixture.

Obviously, one or more additional saturated aliphatic linear or branched carboxylic acids for the mixture of aliphatic linear or branched carboxylic acids within the meaning of the present invention may be selected from one or more straight chain, branched, saturated, unsaturated and/or alicyclic carboxylic acids. Preferably, the one or more additional saturated aliphatic linear or branched carboxylic acids for the mixture of aliphatic linear or branched carboxylic acids are monocarboxylic acids, i.e. the one or more additional aliphatic linear or branched carboxylic acids are characterized in that one carboxyl group is present. Said carboxyl group is at the end of the carbon skeleton.

Thus, the mixture of saturated aliphatic linear or branched carboxylic acids from step c) contains stearic acid and one or more additional saturated aliphatic linear or branched carboxylic acids containing a total number of carbon atoms from C ₁₂ to C ₂₄ . Preferably, the mixture of saturated aliphatic linear or branched carboxylic acids from step c) contains stearic acid and one or more additional saturated aliphatic linear or branched carboxylic acids containing a total number of carbon atoms from C ₁₂ to C ₂₂ , preferably from C ₁₂ to C ₂₀ , and most preferably C14 to C20.

In one of the embodiments of the present invention, one or more additional saturated aliphatic linear or branched carboxylic acids for a mixture of aliphatic linear or branched carboxylic acids is selected from saturated linear carboxylic acids, that is, so to speak, one or more additional saturated aliphatic linear or branched carboxylic acids for a mixture of aliphatic linear or branched carboxylic acids, preferably selected from the group of carboxylic acids consisting of octanoic acid, nonanoic acid, decanoic acid, undecanoic acid, lauric acid, tridecanoic acid, myristic acid, pentadecanoic acid, palmitic acid, heptadecanoic acid, nonadecanoic acid, arachidonic acid, geneicosanoic acid, behenic acid, tricosanoic acid, lignoceric acid, and mixtures thereof.

In another embodiment of the present invention, one or more additional

- 17 041327 saturated aliphatic linear or branched carboxylic acids for a mixture of aliphatic linear or branched carboxylic acids is selected from the group consisting of octanoic acid, decanoic acid, lauric acid, myristic acid, palmitic acid, arachidic acid and mixtures thereof. Preferably, one or more additional saturated aliphatic linear or branched carboxylic acids for the mixture of aliphatic linear or branched carboxylic acids is selected from the group consisting of myristic acid, palmitic acid, and mixtures thereof.

In one embodiment, the mixture of saturated aliphatic linear or branched carboxylic acids from step c) contains stearic acid and one or more additional saturated aliphatic linear or branched carboxylic acids selected from the group consisting of octanoic acid, decanoic acid, lauric acid, myristic acid, palmitic acid, arachidic acid and mixtures thereof. Preferably the mixture of saturated aliphatic linear or branched carboxylic acids from step c) contains stearic acid and one or more additional saturated aliphatic linear or branched carboxylic acids selected from the group consisting of myristic acid, palmitic acid and mixtures thereof.

If the mixture of saturated aliphatic linear or branched carboxylic acids from step c) contains stearic acid and one or more additional saturated aliphatic linear or branched carboxylic acids selected from the group consisting of myristic acid, palmitic acid and mixtures thereof, it is clear that the mixture contains stearic acid and myristic acid and/or palmitic acid in an amount of at least 60.0 wt.%, preferably at least 70.0 wt.%, more preferably at least 80.0 wt.%, and most preferably at least 90 wt.%, for example from 90.0 to 99.0 wt.%, relative to the total weight of the mixture. Thus, it is possible that the mixture of saturated aliphatic linear or branched carboxylic acids from step c) contains additional saturated aliphatic linear or branched carboxylic acid(s) in small amounts, i.e. each additional saturated aliphatic linear or branched carboxylic acid is present in the mixture. in an amount not exceeding 3.0 wt.%, preferably not exceeding 2.0 wt.%, and most preferably not exceeding 1.0 wt.% relative to the total mass of the mixture.

In order to achieve improved flowability of the finished product and improved dispersion in the polymer matrix of the polymer composition, it is obvious that a mixture of saturated aliphatic linear or branched carboxylic acids from step c) containing stearic acid and one or more saturated aliphatic linear or branched carboxylic acids containing the total number of atoms carbon from C ₁₂ to C ₂₄ are obtained in a total amount of from 0.1 to 3 wt.% in relation to the total dry weight of at least one filler material containing calcium carbonate.

For example, a mixture of saturated aliphatic linear or branched carboxylic acids from step c) containing stearic acid and one or more additional saturated aliphatic linear or branched carboxylic acids containing a total number of carbon atoms from C ₁₂ to C ₂₄ is obtained in an amount of from 0.1 up to 2.5 wt.%, preferably in an amount of from 0.2 to 2 wt.%, more preferably in an amount of from 0.3 to 1.5 wt.%, even more preferably in an amount of from 0.3 to 1 wt. %, and most preferably in an amount of from 0.3 to 0.8 wt.% in relation to the total dry weight of at least one filler material containing calcium carbonate.

Additionally or alternatively, the mixture of saturated aliphatic linear or branched carboxylic acids from step c) is preferably prepared in such an amount that the total weight of said mixture of saturated aliphatic linear or branched carboxylic acids containing stearic acid and one or more additional saturated aliphatic linear or branched carboxylic acids containing a total number of carbon atoms from C ₁₂ to C ₂₄ and / or salt product (s) of their reaction, on the surface of at least one filler material containing calcium carbonate less than 5 mg/m ² , at least one material filler containing calcium carbonate obtained in step a).

In one of the embodiments of the present invention, a mixture of saturated aliphatic linear or branched carboxylic acids from step c) containing stearic acid and one or more additional saturated aliphatic linear or branched carboxylic acids containing a total number of carbon atoms from C ₁₂ to C ₂₄ is preferably obtained in such an amount that the total weight of said mixture of saturated aliphatic linear or branched carboxylic acids and/or salt product(s) of their reaction on the surface of at least one filler material containing calcium carbonate is less than 4.5 mg/m ² , and most preferably less than 4.0 mg/m ² of at least one filler material containing calcium carbonate obtained in step a).

For example, the mixture of saturated aliphatic linear or branched carboxylic acids from step c) is preferably prepared in such an amount that the total weight of the mixture of saturated aliphatic linear or branched carboxylic acids and/or the salt product(s) of their reaction on the product surface is of the treated filler material is from 0.1 to 5 mg/m ² , more preferably from 0.2 to 4 mg/m ² , and most preferably from 1 to 4 mg/m ² of at least one filler material containing calcium carbonate, obtained in step a).

Characterization of step d): contacting at least one filler material containing calcium carbonate with at least one monosubstituted succinic anhydride and a mixture of aliphatic linear or branched carboxylic acids containing stearic acid.

According to step d) of the method of the present invention, the surface of at least one calcium carbonate-containing filler material from step a) is brought into contact, with stirring, in one or more steps, in any order, with at least one monosubstituted succinic anhydride co step b) and a mixture of aliphatic linear or branched carboxylic acids from step c) so that the treatment layer containing at least one monosubstituted succinic anhydride and/or salt reaction product(s) thereof and a mixture of aliphatic linear or branched carboxylic acids and/ or the salt product(s) of their reaction is formed on the surface of said at least one filler material containing calcium carbonate from step a).

Step d) contacting at least one filler material containing calcium carbonate with at least one monosubstituted succinic anhydride and a mixture of aliphatic linear or branched carboxylic acids takes place under stirring conditions. The person skilled in the art will adapt these agitation conditions (such as agitator blade configuration and agitation speed) to suit their process equipment.

In one of the preferred embodiments of the present invention, the method of the present invention may be a continuous method. In this case, it is possible to contact at least one filler material containing calcium carbonate with at least one monosubstituted succinic anhydride and a mixture of aliphatic linear or branched carboxylic acids in a constant flow, so that a constant concentration of at least one monosubstituted succinic anhydride and a mixture of aliphatic linear or branched carboxylic acids during step d).

Alternatively, at least one filler material containing calcium carbonate is brought into contact with at least one monosubstituted succinic anhydride and a mixture of linear or branched aliphatic carboxylic acids in one step, wherein said at least one monosubstituted succinic anhydride and a mixture of linear or branched aliphatic carboxylic acids are preferably added in one portion.

In another embodiment of the present invention, the method of the present invention may be a loading method, that is, at least one filler material containing calcium carbonate is brought into contact with at least one monosubstituted succinic anhydride and a mixture of aliphatic linear or branched carboxylic acids on several stages, where the specified at least one monosubstituted succinic anhydride and a mixture of aliphatic linear or branched carboxylic acids are preferably added in approximately equal portions. Alternatively, it is also possible to add at least one monosubstituted succinic anhydride and a mixture of aliphatic linear or branched carboxylic acids in unequal portions to at least one filler material containing calcium carbonate, i.e. in larger and smaller proportions.

According to one embodiment of the present invention, step d) of bringing into contact is carried out in a batch or continuous manner over a period of time from 0.1 to 1000 seconds. For example, contacting step d) is a continuous process and includes one or more contacting steps, and the total contacting time is from 0.1 to 20 seconds, preferably from 0.5 to 15 seconds, and most preferably from 1 to 10 s.

Obviously, step d) of bringing into contact can be carried out in any order. For example, step d) of bringing into contact is carried out in such a way that at least one monosubstituted succinic anhydride from step b) and a mixture of saturated aliphatic linear or branched carboxylic acids from step c) are added simultaneously to at least one filler material containing calcium carbonate . In this embodiment, at least one monosubstituted succinic anhydride from step b) and a mixture of saturated aliphatic linear or branched carboxylic acids from step c) are preferably added as a mixture to at least one filler material containing calcium carbonate.

Alternatively, the mixture of saturated aliphatic linear or branched carboxylic acids from step c) is added before or after at least one monosubstituted succinic anhydride from step b).

Obviously, an advantageous effect is obtained mainly if the mixture of saturated aliphatic linear or branched carboxylic acids from step c) is added after at least one monosubstituted succinic anhydride from step b).

It is obvious that at least one monosubstituted succinic anhydride and a mixture of saturated aliphatic linear or branched carboxylic acids must have a workable viscosity, that is, at least one monosubstituted succinic anhydride and a mixture of saturated aliphatic linear or branched carboxylic acids must be in molten or in liquid state.

Thus, the temperature before and/or during contacting step d) is required to be controlled such that at least one monosubstituted succinic anhydride and the mixture of aliphatic linear or branched carboxylic acids are in a molten or liquid state.

Typically, contacting step d) is carried out at a treatment temperature of 20 to 200°C, preferably 40 to 150°C, and most preferably 60 to 130°C.

Preferably, at least one monosubstituted succinic anhydride and a mixture of aliphatic linear or branched carboxylic acids are obtained in a liquid state, i.e. at standard ambient temperature and pressure (SATP), which refers to a temperature of 298.15°K (25°C) and an absolute pressure of exactly 100,000 Pa (1 bar, 14.5 psi, 0.98692 atm), it is obvious that step d) of bringing into contact can be carried out at room temperature or at a temperature above room temperature, i.e. from 20 up to 200°C, preferably from 20 to 150°C, and most preferably from 20 to 130°C.

If at least one monosubstituted succinic anhydride and/or a mixture of aliphatic linear or branched carboxylic acids is obtained in the molten state, it is obvious that the temperature before and/or during step d) of bringing into contact is controlled in such a way that the temperature is at least 2 °C above the melting point of at least one monosubstituted succinic anhydride and/or a mixture of aliphatic linear or branched carboxylic acids. For example, the temperature prior to contacting step d) is controlled so that the temperature is at least 2° C. higher than the melting point of at least one monosubstituted succinic anhydride and/or a mixture of aliphatic linear or branched carboxylic acids. Alternatively, the temperature before and during contacting step d) is controlled such that the temperature is at least 2°C above the melting point of at least one monosubstituted succinic anhydride and/or a mixture of aliphatic linear or branched carboxylic acids.

Obviously, the expression melting point of at least one monosubstituted succinic anhydride and/or a mixture of aliphatic linear or branched carboxylic acids refers to the melting point of at least one monosubstituted succinic anhydride or a mixture of aliphatic linear or branched carboxylic acids, or a mixture containing at least at least one monosubstituted succinic anhydride; and a mixture of aliphatic linear or branched carboxylic acids.

In one embodiment of the present invention, the temperature before and/or during step d) of bringing into contact is controlled so that the temperature is at least 5°C, preferably at least 8°C, and most preferably at least 10°C above the melting point of at least one monosubstituted succinic anhydride and/or a mixture of aliphatic linear or branched carboxylic acids. For example, the temperature before and/or during step d) of contacting is controlled such that the temperature is 2-50°C, preferably 5-40°C, more preferably 8-30°C, and most preferably 10 -20°C above the melting point of at least one monosubstituted succinic anhydride and/or a mixture of aliphatic linear or branched carboxylic acids.

In one embodiment of the present invention, contacting at least one filler material containing calcium carbonate with at least one monosubstituted succinic anhydride and a mixture of aliphatic linear or branched carboxylic acids is thus carried out at a processing temperature below 200°C. For example, contacting at least one filler material containing calcium carbonate with at least one monosubstituted succinic anhydride and a mixture of aliphatic linear or branched carboxylic acids is carried out at a processing temperature of from 20 to 200°C, preferably from 40 to 150°C. , and most preferably from 60 to 130°C.

The processing time for contacting at least one filler material containing calcium carbonate with at least one monosubstituted succinic anhydride and a mixture of aliphatic linear or branched carboxylic acids takes a period of 1000 seconds or less, preferably a period of 500 seconds or less, more preferably a period of 250 s or less, and most preferably 0.1 to 1000 s. For example, contacting step d) is carried out for a period of time from 0.1 to 20 seconds, preferably from 0.5 to 15 seconds, and most preferably from 1 to 10 seconds. Typically, the duration of contacting at least one calcium carbonate-containing filler material with at least one monosubstituted succinic anhydride and a mixture of aliphatic linear or branched carboxylic acids is determined by the treatment temperature used during said contacting. For example, when a treatment temperature of about 200° C. is applied, the treatment time may reach, for example, about 0.1 second. If a treatment temperature of about 90° C. is used, the treatment time can be up to, for example, about 1000 seconds.

Obviously, at least one mono-substituted succinic anhydride and a mixture of aliphatic linear or branched carboxylic acids are added in contacting step d) in a total amount of 0.1 to 6 wt.% with respect to the total dry weight of at least one filler material containing calcium carbonate from step a). For example, at least one monosubstituted succinic anhydride and a mixture of aliphatic linear or branched carboxylic acids are added in contacting step d) in an amount of from 0.3 to 4.0 wt.% or from 0.6 to 3.0 wt.% , relative to the total dry weight of at least one filler material containing calcium carbonate from step a).

The ratio of at least one monosubstituted succinic anhydride and a mixture of aliphatic linear or branched carboxylic acids added in contacting step d) can vary over a wide range. Preferably, however, contacting step d) is carried out in such a way that at least one monosubstituted succinic anhydride from step b) and a mixture of saturated aliphatic linear or branched carboxylic acids from step c) are added at a weight ratio of [succinic anhydride/mixture of carboxylic acids ] from 10:1 to 1:10. Preferably, contacting step d) is carried out in such a way that at least one monosubstituted succinic anhydride from step b) and a mixture of saturated aliphatic linear or branched carboxylic acids from step c) are added at a mass ratio of [succinic anhydride/mixture of carboxylic acids] from 5 :1 to 1:5, and most preferably 4:1 to 1:4.

It is clear that advantageous results in terms of flowability as well as dispersion of the surface-treated filler material product in the polymer matrix of the polymer composition are achieved if at least one monosubstituted succinic anhydride from step b) is added in excess compared to the mixture of saturated aliphatic linear or branched carboxylic acids from step c) or if at least one monosubstituted succinic anhydride from step b) and a mixture of saturated aliphatic linear or branched carboxylic acids from step c) are added in equal amounts. Thus, it is preferred that contacting step d) is carried out such that at least one monosubstituted succinic anhydride from step b) and a mixture of saturated aliphatic linear or branched carboxylic acids from step c) are added at a weight ratio of [succinic anhydride /mixture of carboxylic acids] from 4:1 to 1:1.

In one embodiment of the present invention, at least one filler material containing calcium carbonate is preheated, i.e. activated, before contacting step d) is carried out. That is, so to speak, at least one filler material containing calcium carbonate is treated at a temperature of from 20 to 200°C, preferably from 40 to 200°C, more preferably from 50 to 150°C, and most preferably from 60 to 130 °C before carrying out step d) bringing into contact.

The treatment time for preheating at least one filler material containing calcium carbonate takes a period of 30 minutes or less, preferably a period of 20 minutes or less, and more preferably a period of 15 minutes or less.

In one of the embodiments of the present invention, the preheating of at least one filler material containing calcium carbonate is carried out at a temperature that is approximately equal to the temperature used during stage d) bringing into contact.

The term equal temperature in the meaning of the present invention refers to a preheating temperature that is at most 20°C, preferably at most 15°C, more preferably 10°C, and most preferably at most 5°C below or above the temperature. used during step d) bringing into contact.

Thus, it is obvious that the treatment layer formed on the surface of at least one filler material containing calcium carbonate contains at least one monosubstituted succinic anhydride obtained in step b) and/or the salt product(s) of its reaction obtained as the reaction product upon contacting the filler material containing calcium carbonate with at least one monosubstituted succinic anhydride from step b). In such a case, the product treatment layer of the surface-treated filler material preferably further comprises the salt reaction product(s) of at least one monosubstituted succinic anhydride formed on the surface of said at least one calcium carbonate-containing filler material in step c). For example, it is the salt reaction product(s), such as one or more calcium and/or magnesium salts and at least one monosubstituted succinic anhydride.

In addition, the treatment layer formed on the surface of at least one filler material containing calcium carbonate contains a mixture of aliphatic linear or

- 21 041327 branched carboxylic acids containing stearic acid in an amount of at least 10.0 wt.%, relative to the total mass of the mixture, and one or more additional saturated aliphatic linear or branched carboxylic acids containing a total number of carbon atoms from C ₁₂ to C ₂₄ , and the salt product(s) of their reaction obtained by contacting at least one filler material containing calcium carbonate with a mixture of aliphatic linear or branched carboxylic acids from step c). In such a case, the product treatment layer of the surface-treated filler material preferably further comprises the salt reaction product(s) of the mixture of aliphatic linear or branched carboxylic acids formed on the surface of said at least one calcium carbonate-containing filler material in step c). For example, it is the salt reaction product(s), such as one or more calcium and/or magnesium salts and mixtures of aliphatic linear or branched carboxylic acids.

The treatment layer is preferably characterized in that the total weight of at least one monosubstituted succinic anhydride and/or salt product(s) of its reaction, as well as mixtures of aliphatic linear or branched carboxylic acids and/or salt product(s) of their reaction on the surface of the surface of the treated filler material is from 0.2 to 10 mg/m ² , more preferably from 0.4 to 8 mg/m ² and most preferably from 2 to 8 mg/m ² of at least one filler material containing calcium carbonate.

The treatment layer is preferably characterized in that the total weight of at least one monosubstituted succinic anhydride and/or salt product(s) of its reaction, as well as mixtures of aliphatic linear or branched carboxylic acids and/or salt product(s) of their reaction on the surface of the surface of the treated filler material is from 0.1 to 2 wt.% / m ² , more preferably from 0.2 to 1 wt.% / m ² , and most preferably from 0.3 to 0.5 wt.% / m ² , at least one filler material containing calcium carbonate.

In addition, it is obvious that the obtained surface-treated filler material contains a treatment layer in an amount of from 0.2 to 6 wt.%, preferably in an amount of from 0.2 to 5 wt.%, more preferably in an amount of from 0.2 to 4 wt.%, even more preferably in an amount of from 0.2 to 3 wt.%, even more preferably in an amount of from 0.2 to 2 wt.%, and most preferably in an amount of from 0.4 to 1.6 wt.% in relation to the total dry weight of at least one filler material containing calcium carbonate.

Thus, it is obvious that at least one filler material containing the calcium carbonate product obtained in step d) of the process contains, and preferably consists of them, at least one filler material containing calcium carbonate, and a treatment layer containing at least one monosubstituted succinic anhydride and/or salt product(s) of its reaction, as well as a mixture of aliphatic linear or branched carboxylic acids and/or salt product(s) of their reaction. A treatment layer is formed on the surface of said at least one filler material containing calcium carbonate from step a).

Additionally or alternatively, the product treatment layer of the surface-treated filler material contains at least one monosubstituted succinic anhydride and/or salt reaction product(s) thereof in a specific molar ratio. For example, the molar ratio of at least one monosubstituted succinic anhydride to the salt reaction product(s) thereof is 99.9:0.1 to 0.1:99.9, preferably 70:30 to 90:10.

The expression molar ratio of at least one monosubstituted succinic anhydride to the salt product(s) of its reaction as used in the present invention refers to the sum of the molecular weights of at least one monosubstituted succinic anhydride divided by the sum of the molecular weights of the molecules of the monosubstituted succinic anhydride in the salt products his reactions.

Additionally or alternatively, the product treatment layer of the surface-treated filler material contains a mixture of aliphatic linear or branched carboxylic acids and/or salt reaction product(s) thereof in a specific molar ratio. For example, the molar ratio of the mixture of aliphatic linear or branched carboxylic acids to the salt product(s) of their reaction is 99.9:0.1 to 0.1:99.9, preferably 70:30 to 90:10.

The expression molar ratio of a mixture of aliphatic linear or branched carboxylic acids to the salt product(s) of their reaction as used in the present invention refers to the sum of the molecular weights of the mixture of aliphatic linear or branched carboxylic acids divided by the sum of the molecular weights of the mixture of molecules of aliphatic linear or branched carboxylic acids in salt products of their reaction.

In one embodiment, the surface-treated filler material product obtained in step d) is dried. This optional step is preferably carried out to reduce the moisture content of the resulting surface-treated filler material product. Thus, the dried product of the surface-treated filler material obtained in step e) has a moisture content that is lower than the moisture content of the product

- 22 041327 of the surface-treated filler material obtained before the drying step, i.e. after step d).

According to one embodiment of the present invention, the method thus comprises an additional step e) of drying the product of the surface-treated filler material obtained in step d).

For example, the optional drying step e) is carried out at a temperature in the range from 60 to 180°C, preferably from 50 to 150°C, more preferably from 60 to 120°C, and most preferably from 80 to 120°C, at ambient pressure. or under reduced pressure until the moisture content of the resulting surface-treated filler material product is reduced.

In one embodiment, the optional drying step e) is carried out until the moisture content of the resulting surface-treated filler material product is in the range of 0.001 to 20% by weight, preferably 0.005 to 15% by weight, more preferably from 0.01 to 10 wt.%, and most preferably from 0.05 to 5 wt.%, in relation to the total mass of surface-reacted calcium carbonate.

Obviously, the optional drying step e) can be carried out at ambient pressure or under reduced pressure. Preferably, drying is carried out at ambient pressure.

Thus, the optional drying step e) is preferably carried out at a temperature in the range of 60 to 180° C. at ambient pressure. For example, the optional drying step e) is carried out at a temperature in the range of 50 to 150°C, preferably 60 to 120°C, and more preferably 80 to 120°C at ambient pressure.

According to one embodiment, the present invention thus relates to a method for preparing a surface-treated filler material product with monosubstituted succinic anhydride(s) and a mixture of aliphatic linear or branched carboxylic acids containing stearic acid, the method comprising the steps of:

a) obtaining at least one filler material containing calcium carbonate,

b) obtaining at least one monosubstituted succinic anhydride,

c) obtaining a mixture of aliphatic linear or branched carboxylic acids containing stearic acid in an amount of at least 10.0 wt.%, relative to the total mass of the mixture, and one or more additional saturated aliphatic linear or branched carboxylic acids containing a total amount of carbon atoms from C ₁₂ to C ₂₄ ,

d) bringing into contact the surface of at least one calcium carbonate-containing filler material from step a), while stirring in one or more steps in any order, with at least one monosubstituted succinic anhydride from step b) and a mixture of linear or branched aliphatic carboxylic acids from step c) such that a treatment layer comprising at least one monosubstituted succinic anhydride and/or salt reaction product(s) thereof and a mixture of aliphatic linear or branched carboxylic acids and/or salt reaction product(s) thereof is formed on the surface of said at least one filler material containing calcium carbonate from step a),

e) drying the surface-treated filler material product is obtained in step d), where the temperature before and/or during step d) of bringing into contact is controlled in such a way that at least one monosubstituted succinic anhydride and a mixture of aliphatic linear or branched carboxylic acids are in molten or liquid state.

The resulting surface-treated filler material product obtained according to the present invention has excellent flow characteristics as well as dispersion characteristics in the polymer matrix of the polymer composition compared to mineral fillers treated with at least one monosubstituted succinic anhydride only, i.e. without using a mixture aliphatic linear or branched carboxylic acids containing stearic acid in an amount of at least 10.0 wt.% relative to the total mass of the mixture and one or more additional saturated aliphatic linear or branched carboxylic acids containing a total number of carbon atoms from C ₁₂ to From ₂₄ .

Specifically, the resultant surface-treated filler material product has, when measured by the shear cell method on an FT4 Powder Rheometer (ASTM D7891-15) with a pre-normal shear stress of 15 kPa, a yield stress (UYS) that decreases at least by 7%, preferably by 7-30%, more preferably by at least 10%, and most preferably by 10-30%, or a flow factor (FF) that is increased by at least 7%, preferably by 7-30% , more preferably by at least 10%, and most preferably by 10-30%, and/or when measuring powder flow through a method using a programmable stability sequence and variable flow rate sequences on the FT4 Powder Rheometer, a base flow energy (BFE) that is reduced by at least 7%, preferably by 7-30%, more preferably by at least

- 23 041327 at least 10%, and most preferably 10-30%, compared with the same product of surface-treated filler material treated with only at least one mono-substituted succinic anhydride, that is, without using a mixture of aliphatic linear or branched carboxylic acids containing stearic acid, in an amount of at least 10.0 wt.%, relative to the total mass of the mixture, and one or more additional saturated aliphatic linear or branched carboxylic acids containing a total number of carbon atoms from C ₁₂ to C ₂₄ . Apparently, the FT4 Powder Rheometer (Freeman Technology, UK) comes with Powder Rheometer Software (v 5.000.00012) and Freeman Technology Data Analysis Software version 4.0.17.

Considering the very good results obtained, a surface-treated filler material product is obtained containing

a) at least one filler material containing calcium carbonate,

b) a treatment layer on the surface of at least one filler material containing calcium carbonate containing at least one monosubstituted succinic anhydride and / or salt product (s) of its reaction and a mixture of aliphatic linear or branched carboxylic acids containing stearic acid in an amount of at least 10.0 wt.% in relation to the total mass of the mixture and one or more additional saturated aliphatic linear or branched carboxylic acids containing a total number of carbon atoms from C ₁₂ to C ₂₄ and / or salt product (s) of their reaction, where the product of the surface-treated filler material contains a treatment layer in an amount of from 0.2 to 6 wt.%, in relation to the total dry weight of at least one filler material containing calcium carbonate.

Regarding the definition of at least one filler material containing calcium carbonate, at least one monosubstituted succinic anhydride, salt product (s) of its reaction, a mixture of aliphatic linear or branched carboxylic acids containing stearic acid, in an amount of at least 10.0 wt .%, relative to the total mass of the mixture, and one or more additional saturated aliphatic linear or branched carboxylic acids containing a total number of carbon atoms from C ₁₂ to C ₂₄ , the salt product (s) of their reaction, the product of the surface-treated filler material and their preferred embodiments, we will refer to the comments above, where steps a), b), c) and d) of the method are discussed.

Preferably, the surface-treated filler material product is in the form of a powder.

In one of the embodiments of the present invention, the product of the surface-treated filler material can be obtained (or receive) using the method of the present invention.

Thus, a surface-treated filler material product is provided, comprising:

a) at least one filler material containing calcium carbonate,

b) a treatment layer on the surface of at least one filler material containing calcium carbonate containing at least one monosubstituted succinic anhydride and / or salt product (s) of its reaction and a mixture of aliphatic linear or branched carboxylic acids containing stearic acid in an amount of at least 10.0 wt.% in relation to the total mass of the mixture and one or more additional saturated aliphatic linear or branched carboxylic acids containing a total number of carbon atoms from C ₁₂ to C ₂₄ and / or salt product (s) of their reaction, where the surface-treated filler material product contains a treatment layer in an amount of from 0.2 to 6 wt.%, in relation to the total dry weight, at least one filler material containing calcium carbonate, the surface-treated filler material product can be obtained ( or obtain) by means of a method for preparing a surface-treated material product filler with monosubstituted succinic anhydride (anhydrides) and a mixture of aliphatic linear or branched carboxylic acids containing stearic acid, the method includes at least the steps:

a) obtaining at least one filler material containing calcium carbonate,

b) obtaining at least one monosubstituted succinic anhydride,

c) obtaining a mixture of aliphatic linear or branched carboxylic acids containing stearic acid in an amount of at least 10.0 wt.%, relative to the total mass of the mixture, and one or more additional saturated aliphatic linear or branched carboxylic acids containing a total amount of carbon atoms from C ₁₂ to C ₂₄ ,

d) bringing into contact the surface of at least one calcium carbonate-containing filler material from step a) while stirring in one or more steps in any order with at least one monosubstituted succinic anhydride from step b) and a mixture of aliphatic linear or branched carboxylic acids from step c) so that the treatment layer containing at least one monosubstituted succinic anhydride and/or salt product (product

- 24 041327 you) its reaction and a mixture of aliphatic linear or branched carboxylic acids and / or salt product (s) of their reaction, is formed on the surface of the specified at least one filler material containing calcium carbonate, from stage a), where the temperature is up to and /or during step d) bringing into contact is controlled in such a way that at least one monosubstituted succinic anhydride and a mixture of aliphatic linear or branched carboxylic acids are in a molten or liquid state.

The surface-treated filler material product thus obtained is advantageously used in a polymer composition containing at least one polymer resin and from 1 to 95% by weight of the surface-treated filler material product.

In another aspect, the present invention thus relates to a polymer composition comprising at least one polymer resin and from 1 to 95% by weight, based on the total weight of the product polymer composition, of the surface-treated filler material.

Accordingly, the polymer composition contains at least one polymer resin. The polymer resin is the backbone of the composition and provides strength, flexibility, stiffness and wear resistance to the finished fiber and/or filament and/or film and/or yarn and/or sheet and/or pipe and/or profile, and /or molds for molding, and/or molds for injection molding, and/or molds for blow molding.

It is obvious that at least one polymer resin of the present invention is not limited to any particular resin material insofar as the polymer composition is suitable for obtaining fiber and/or filament and/or film and/or thread and/or sheet. , and/or pipes, and/or profiles, and/or molds for molding, and/or molds for injection molding, and/or molds for blow molding.

In one embodiment of the present invention, at least one polymer resin is at least one thermoplastic polymer. Thus, it is preferred that at least one polymer resin is a thermoplastic polymer selected from the group consisting of homopolymers and/or copolymers of polyolefins, polyamides, halogenated polymers and/or polyesters.

Additionally or alternatively, at least one polymer resin is a polyolefin homopolymer and/or copolymer. For example, at least one polymer resin is a polyolefin homopolymer and a copolymer. Alternatively, at least one polymer resin is a polyolefin homopolymer or copolymer.

Obviously, at least one polymer resin is preferably a polyolefin homopolymer.

For example, the polyolefin may be polyethylene and/or polypropylene and/or polybutylene. Accordingly, if the polyolefin is polyethylene, the polyolefin is selected from the group consisting of polyethylene homopolymers and/or copolymers like high density polyethylene (HDPE), medium density polyethylene (MDPE), low density polyethylene (LDPE), very low density polyethylene (VLDPE) , linear low density polyethylene (LLDPE).

For example, the polyolefin is a homopolymer and/or copolymer of polyethylene.

The term polyethylene homopolymer used in the present invention refers to a polyethylene containing a polyethylene which consists essentially, i.e. more than 99.7 wt.%, even more preferably at least 99.8 wt.% with respect to total mass of polyethylene from ethylene units. For example, only ethylene units are detected in a polyethylene homopolymer.

In the case where at least one polymer resin of the polymer composition contains a copolymer of polyethylene, it is obvious that the polyethylene contains units derived from ethylene as the main components. Accordingly, the polyethylene copolymer contains at least 55% by weight of units derived from ethylene, more preferably at least 60% by weight of units derived from ethylene, based on the total weight of polyethylene. For example, the polyethylene copolymer contains 60-99.5% by weight, more preferably 90-99% by weight, of units derived from ethylene, based on the total weight of the polyethylene. The comonomers present in such a polyethylene copolymer are C ₃ -C ₁₀ α-olefins, preferably 1-butene, 1-hexene and 1-octene, the latter being particularly preferred.

Additionally or alternatively, the polyolefin is a homopolymer and/or copolymer of polypropylene.

The expression polypropylene homopolymer, as used in the present invention, refers to a polypropylene that is essentially, i.e., more than 99 wt.%, even more preferably at least 99.5 wt.%, for example, at least 99.8 wt.%, in relation to the total mass of polypropylene, from propylene units. In a preferred embodiment, only propylene units are detected in the polypropylene homopolymer.

In the case where at least one polymer resin of the polymer composition contains a polypropylene copolymer, the polypropylene preferably contains units derived from propylene,

- 25 041327 as main components. The polypropylene copolymer preferably contains, and preferably consists of, units derived from propylene and C ₂ and/or at least one C ₄ -Cu αolefin. In one embodiment of the present invention, the polypropylene copolymer contains, and preferably consists of, units derived from propylene and at least one α-olefin selected from the group consisting of ethylene, 1-butene, 1-pentene, 1-hexene and 1-octene. For example, the polypropylene copolymer contains, and preferably consists of, units derived from propylene and ethylene. In one embodiment of the present invention, the units derived from propylene constitute the majority of the polypropylene, i.e. at least 60% by weight, preferably at least 70% by weight, more preferably at least 80% by weight, even more preferably from 60 to 99 wt.%, even more preferably from 70 to 99 wt.%, and most preferably from 80 to 99 wt.% in relation to the total weight of polypropylene. The number of units derived from C ₂ and/or at least one C ₄ -C ₁₀ aolefin, in the polypropylene copolymer, is in the range from 1 to 40 wt.%, more preferably in the range from 1 to 30 wt.%, and most preferably in the range from 1 to 20 wt.% in relation to the total weight of the polypropylene copolymer.

If the polypropylene copolymer contains only units derived from propylene and ethylene, the amount of ethylene is preferably in the range of 1 to 20 wt.%, preferably in the range of 1 to 15 wt.%, and most preferably in the range of 1 to 10 wt.% , relative to the total weight of the polypropylene copolymer. Accordingly, the amount of propylene is preferably in the range of 80 to 99 wt.%, preferably in the range of 85 to 99 wt.%, and most preferably in the range of 90 to 99 wt.%, based on the total weight of the polypropylene copolymer.

Additionally or alternatively, the polyolefin is a polybutylene homopolymer and/or copolymer.

The expression polybutylene homopolymer, as used in the present invention, refers to a polybutylene which is essentially, i.e. more than 99 wt.%, even more preferably at least 99.5 wt.%, for example, at least 99.8 wt.% in relation to the total mass of polybutylene, from butylene units. In a preferred embodiment, only butylene units are detected in the polybutylene homopolymer.

In the case where at least one polymer resin of the polymer composition contains a polybutylene copolymer, the polybutylene preferably contains units derived from butylene as main components. The polybutylene copolymer preferably contains, and preferably consists of, units derived from butylene and C ₂ and/or C ₃ and/or at least one C ₅ -C ₁₀ α-olefin. In one embodiment of the present invention, the polybutylene copolymer contains, and preferably consists of, units derived from butylene and at least one α-olefin selected from the group consisting of ethylene, 1-propene, 1-pentene, 1-hexene and 1 -octene. For example, the polybutylene copolymer contains, and preferably consists of, units derived from butylene and ethylene. In one embodiment of the present invention, the units derived from butylene make up the bulk of the polybutylene, i.e. at least 60 wt.%, preferably at least 70 wt.%, more preferably at least 80 wt.%, even more preferably from 60 to 99 wt.%, even more preferably from 70 to 99 wt.%, and most preferably from 80 to 99 wt.% in relation to the total mass of polybutylene. The number of units derived from C ₂ and/or C ₃ and/or at least one C ₅ -C ₁₀ α-olefin in the polybutylene copolymer is in the range from 1 to 40 wt.%, more preferably in the range from 1 up to 30 wt.%, and most preferably in the range from 1 to 20 wt.%, relative to the total weight of the polybutylene copolymer.

If at least one polymer resin is a homopolymer and/or copolymer of a halogenated polymer, the at least one polymer resin is preferably selected from polyvinyl chloride (PVC), polyvinylidene chloride (PVDC), polyvinylidene fluoride (PVDF) and polytetrafluoroethylene (PTFE).

If at least one polymer resin is a polyester homopolymer and/or copolymer, the at least one polymer resin is preferably selected from polyethylene terephthalate (PET), polytrimethylene terephthalate (PTT), polybutylene terephthalate (PBT), polyethylene phthalate (PEN), but also from degradable polyesters such as polylactic acid (polylactide, PLA).

In one of the embodiments of the present invention, at least one polymer resin is a homopolymer of polyethylene and/or polypropylene and/or polybutylene. For example, at least one polymer resin is a homopolymer of polyethylene and polypropylene. Alternatively, at least one polymer resin is a polyethylene or polypropylene homopolymer. In one embodiment of the present invention, at least one polymer resin is a polypropylene homopolymer.

The expression at least one polymer resin means that one or more types of polymer resin may be present in the polymer composition of the present invention.

- 26 041327

Accordingly, it is obvious that at least one polymer resin may be a mixture of two or more kinds of polymer resins. For example, if at least one polymer resin is a mixture of two or more polymer resins, one polymer resin is a homopolymer or copolymer of polypropylene, while the second or additional polymer resin is selected from the group consisting of homopolymers and/or copolymers of polyethylene, polybutylene , polyamides, polyesters, halogen-containing polymers and mixtures thereof.

In one embodiment of the present invention, at least one polymer resin is one kind of polymer resin. Preferably, at least one polymer resin is a homopolymer of polyethylene or polypropylene.

In one of the embodiments of the present invention, at least one polymer resin has a melting point Tm above 100°C, more preferably above 150°C, for example above 200°C. For example, the melting temperature of at least one polymer resin is in the range from 100 to 350°C, more preferably in the range from 150 to 325°C, and most preferably in the range from 200 to 300°C.

In addition, it is obvious that at least one polymer resin can be selected from polymer resins having a wide range of melt flow rates. In general, it is preferred that at least one polymer resin has a melt flow rate MFR (190° C.) from 0.1 to 3000 g/10 min, more preferably from 0.2 to 2500 g/10 min. For example, at least one polymer resin has a melt flow rate MFR (190°C) from 0.3 to 2000 g/10 min, or from 0.3 to 1600 g/10 min. In addition or alternatively, at least one polymer resin has a melt flow rate MFR (230°C) from 0.1 to 3000 g/10 min, more preferably from 0.2 to 2500 g/10 min. For example, at least one polymer resin has a melt flow rate MFR (230°C) from 0.3 to 2000 g/10 min, or from 0.3 to 1600 g/10 min.

For example, if at least one polymer resin is a polyolefin that is a polypropylene homopolymer and/or copolymer, it is preferred that the at least one polymer resin has a melt flow rate MFR (190° C., 2.16 kg) of 1 up to 3000 g/10 min, more preferably from 3 to 2500 g/10 min. For example, at least one polymer resin that is a homopolymer and/or copolymer of polypropylene has a melt flow rate MFR (190° C.) of 5 to 2000 g/10 min or 10 to 1600 g/10 min. Preferably, at least one polymer resin, which is a homopolymer and/or copolymer of polypropylene, has a melt flow rate MFR (230°C) from 1 to 3000 g/10 min, more preferably from 3 to 2500 g/10 min. For example, at least one polymer resin that is a homopolymer and/or copolymer of polypropylene has a melt flow rate MFR (230° C.) of 5 to 2000 g/10 min or 10 to 1600 g/10 min.

If at least one polymer resin is a polyolefin, which is a homopolymer and/or copolymer of polyethylene, it is obvious that at least one polymer resin has a rather low melt flow rate. Accordingly, it is preferable that at least one polymer resin, which is a homopolymer and/or copolymer of polyethylene, has a melt flow rate MFR (190°C) from 0.5 to 20 g/10 min, more preferably from 0.7 to 15 g/10 min. For example, at least one polymer resin has an MFR (190° C.) melt flow rate of 0.9 to 10 g/10 min, or 0.9 to 5 g/10 min. In addition or alternatively, at least one polymer resin, which is a homopolymer and/or copolymer of polyethylene, has a melt flow rate MFR (230°C) from 0.1 to 3000 g/10 min, more preferably from 0, 2 to 2500 g/10 min. For example, at least one polymer resin that is a homopolymer and/or copolymer of polyethylene has a melt flow rate MFR (230°C) from 0.3 to 2000 g/10 min or from 0.3 to 1600 g/10 min .

Another major component of the present polymeric composition is the product of a surface treated filler material. Regarding the product definition of surface treated filler material and its preferred embodiments, refer to the comments above when discussing steps a), b), c) and d) of the method.

One of the requirements of the present invention is that the polymer composition contains the product of surface-treated filler material in an amount of from 1 to 95 wt.%, relative to the total weight of the polymer composition.

In one of the embodiments of the present invention, the polymer composition contains the product of surface-treated filler material in an amount of from 5 to 95 wt.%, and preferably from 10 to 85 wt.% in relation to the total weight of the polymer composition. For example, the polymer composition contains the product of surface-treated filler material in an amount of from 15 to 80 wt.% in relation to the total weight of the polymer composition.

In one of the embodiments of the present invention, the polymer composition is a concentrate.

The term concentrate refers to a composition having a product concentration of the surface treated filler material that is higher than the concentration of the polymeric composition used.

- 27 041327 used to obtain a product ready for use, such as fiber and/or filament and/or film and/or thread and/or sheet and/or pipe and/or profile and/or mold for molding and/or injection molding and/or blow molding. That is, so to speak, the concentrate is further diluted in such a way as to obtain a polymer composition that is suitable for obtaining a ready-to-use product, such as a fiber and/or a filament and/or a film and/or a thread and/or a sheet. , and/or pipe, and/or profile, and/or mold for molding, and/or mold for injection molding, and/or mold for blow molding.

For example, the concentrate contains a surface-treated filler material product in an amount of 50 to 95 wt.%, preferably 60 to 85 wt.%, and more preferably 70 to 80 wt.%, based on the total weight of the concentrate.

According to one of the embodiments of the present invention, the concentrate is used to obtain fibers and/or filaments and/or films and/or threads.

In another embodiment of the present invention, the polymer composition used to obtain a ready-to-use product such as fiber and/or filament and/or film and/or thread and/or sheet and/or pipe and/or profile , and/or a mold for molding and/or a mold for injection molding and/or a mold for blow molding, contains the product of surface-treated filler material in an amount of from 1 to 70 wt.%, preferably from 5 to 55 wt.%, and most preferably from 10 to 50 wt.% in relation to the total weight of the polymer composition. For example, the polymer composition used to obtain a ready-to-use product, such as a fiber and/or filament and/or film, contains a surface-treated filler material product in an amount of 15 to 25 wt.% relative to the total weight of the polymer composition.

In another embodiment of the present invention, the polymer composition used to obtain a ready-to-use product such as fiber and/or filament and/or film and/or thread and/or sheet and/or pipe and/or profile , and / or a mold for molding, and / or a mold for injection molding, and / or a mold for blow molding, contains at least one material containing calcium carbonate, in an amount of 1 and 10 wt.% relative to the total mass of the polymer compositions. Obviously, the polymer composition preferably contains this amount when used as a packaging material for an acidic food product like citrus fruits or fruit juice containers and/or bottles.

If the concentrate is used to obtain a fiber and/or a filament and/or a film and/or a thread and/or a sheet and/or a pipe and/or a profile and/or a mold for molding and/or a mold for injection molding and/or blow molding, preferably the concentrate is diluted in such a way as to obtain a polymer composition suitable for obtaining a ready-to-use product such as fiber and/or filament and/or film and/or thread, and/or sheet and/or pipe and/or profile and/or mold and/or injection mold and/or blow mold. That is, so to speak, the concentrate is diluted so that it contains the product of the surface-treated filler material in an amount of from 1 to 70 wt.%, preferably from 5 to 55 wt.%, and most preferably from 10 to 50 wt.%, relative to the total weight of the polymer composition.

According to another embodiment of the present invention, the polymer composition is a fiber and/or a filament and/or a film and/or a thread and/or a sheet and/or a pipe and/or a profile and/or a mould, and /or an injection mold and/or a blow mold. For example, fiber and/or filament and/or film and/or thread and/or sheet and/or pipe and/or profile and/or mold and/or injection mold, and /or the blow mold contains a product of surface-treated filler material in an amount of from 1 to 70 wt.%, preferably from 5 to 55 wt.%, more preferably from 10 to 50 wt.%, and most preferably from 15 to 30 wt. .% with respect to the total weight of the fiber and/or filament and/or film and/or yarn and/or sheet and/or pipe and/or profile and/or mold and/or mold for injection molding, and/or molds for blow molding.

In view of the excellent flow characteristics of the surface treated filler material product, as well as its excellent dispersibility in polymer compositions, the surface treated filler material product of the present invention can advantageously be used in ready-to-use products such as fiber and/or filament, and/ or film and/or thread and/or sheet and/or pipe and/or profile and/or mold and/or injection mold and/or blow mold. With this in mind, the surface-treated filler material product imparts excellent mechanical properties to ready-to-use products such as fiber and/or filament and/or film and/or thread and/or sheet and/or pipe and/or profile and/or mold for molding and/or mold for injection molding and/or mold for blow molding, when the product of surface-treated filler material is obtained in the form of a polymer composition according to the present invention.

Thus, the present invention relates in another aspect to a fiber and/or filament,

- 28 041327 and/or film and/or thread and/or sheet and/or pipe and/or profile and/or mold and/or injection mold and/or blow mold containing a polymer composition as defined above and/or a surface-treated filler material product as defined above.

In addition, the present invention relates in another aspect to a method for producing a fiber and/or a filament and/or a film and/or a thread and/or a sheet and/or a pipe and/or a profile and/or a mold for molding , and/or injection molds and/or blow molds, the method includes at least the steps of:

a) obtaining a polymer composition as defined above, and

b) exposing the polymer composition from step a) to the conditions under which said polymer composition is converted into a fiber and/or a filament and/or a film and/or a thread and/or a sheet and/or a pipe and/or a profile , and/or a mold for molding, and/or a mold for injection molding, and/or a mold for blow molding.

Appropriate process conditions for the production of fiber and/or filament and/or film and/or filament and/or sheet and/or pipe and/or profile and/or mold and/or injection mold , and/or blow molds are commonly known to those skilled in the art, and/or can be ascertained through routine modifications based on ordinary common knowledge.

For example, the polymer composition of the present invention can advantageously be used in a kneading and/or extruding and/or compounding and/or blow molding process to form a fiber and/or filament and/or film and/or filament and/ or sheet and/or pipe and/or profile and/or mold and/or injection mold and/or blow mold, where at least one polymer resin is preferably a thermoplastic polymer selected from the group consisting of homopolymers and/or copolymers of polyolefins, polyamides and/or polyesters.

The term fiber in the meaning of the present invention refers to the linear structure forming textile materials, such as non-woven materials, which typically consist of fibrous webs bonded together, for example, by mechanical means. Accordingly, the term fiber is understood to refer to the final structure.

The term thread in the meaning of the present invention refers to a linear structure forming textile materials, such as nonwoven materials, which typically consist of webs of threads knitted together, for example, by mechanical means. Accordingly, the term thread is understood to refer to the final structure. The thread can be built as mono-, bi- or multi-thread. If bi- or multifilaments are present, the composition of the individual yarn may be substantially the same. That is, so to speak, the compositions of the individual threads contain essentially the same components, that is, at least one polymer resin and surface-treated filler material product, in the same amounts. Alternatively, the composition of the individual threads may vary. That is, so to speak, the individual yarn compositions may contain the same components, i.e., at least one polymer resin and the surface-treated filler material product in different amounts, or the individual yarn compositions may contain different components, i.e., at least one the polymer resin and/or surface-treated filler material products may be different in the same amounts, or the composition of the individual filaments may contain different components, i.e. at least one polymer resin and/or surface-treated filler material product may be different, at different amounts .

The term filament as used in the present invention refers to a structure that differs from fibers in the length of its structure. Accordingly, the term filament is understood to refer to endless fibers. In addition, it is obvious that the filament can be built as a mono-, bi- or multifilament. If a bi- or multifilament is present, the composition of the individual filaments may be substantially the same. That is, so to speak, the compositions of the individual filaments contain essentially the same components, that is, at least one polymer resin and the surface-treated filler material product in the same amounts. Alternatively, the composition of the individual filaments may be different. That is, so to speak, the individual filament compositions may contain the same components, i.e., at least one polymer resin and the surface-treated filler material product, in different amounts, or the individual filament compositions may contain different components, i.e., at least one the polymer resin and/or surface treated filler material product may be different at the same amounts, or the composition of the individual filaments may contain different components, i.e. at least one polymer resin and/or surface treated filler material product may be different at different amounts .

The cross section of the filaments and/or fibers and/or filaments can take on a wide variety of shapes. Preferably, the cross-sectional shape of the filaments and/or fibers and/or filaments

- 29 041327 was round, oval or n-gonal, where n>3, for example, n is 3. For example, the cross-sectional shape of the filaments and/or fibers and/or threads is round or trilobal, for example, round.

Additionally or alternatively, the cross-sectional shape of the filaments and/or fibers and/or filaments is hollow.

Obviously, filaments and/or fibers and/or threads can be obtained using all technologies known in the field used to obtain such filaments and/or fibers and/or threads. For example, the filaments and/or fibers and/or yarns of the present invention can be produced by the well-known meltblown process, spunbond process, or staple fiber process.

The term film as used in the present invention refers to a structure that differs from filaments and/or fibers in its spatial structure. Accordingly, the term film is understood to refer to a sheet.

It is obvious that films can be obtained using all technologies known in this field, used to obtain such films. For example, the films of the present invention can be made using well-known techniques used to make stretched/oriented films, and preferably extrusion coating films, blown films, technical blown films, monotapes, cast films, and the like.

In view of the very good results obtained with respect to product flowability of surface treated filler material treated with monosubstituted succinic anhydride(s) and a mixture of aliphatic linear or branched carboxylic acids containing stearic acid as defined above, another aspect of the present invention is directed to the use of at least one monosubstituted succinic anhydride and / or salt product (s) of its reaction in combination with a mixture of aliphatic linear or branched carboxylic acids containing stearic acid in an amount of at least 10.0 wt.%, relative to the total mass of the mixture, and one or several additional saturated aliphatic linear or branched carboxylic acids containing a total number of carbon atoms from C ₁₂ to C ₂₄ and/or salt reaction product(s) thereof, to improve the fluidity of the surface-treated filler material product.

Clearly, an improvement is achieved if, when measuring the powder flow using the shear cell method on an FT4 Powder Rheometer (ASTM D7891-15) with a pre-normal shear stress of 15 kPa, the onset stress (UYS) is reduced by at least 7%, preferably by 7-30%, more preferably at least 10%, and most preferably 1030%, or the flow factor (FF) is increased by at least 7%, preferably 7-30%, more preferably at least 10% , and most preferably by 10-30%, and/or when measuring the powder flowability by means of a method using a programmable stability sequence and sequences of variable rates on the FT4 Powder Rheometer, the base flow energy (BFE) is reduced by at least 7%, preferably by 7- 30%, more preferably at least 10%, and most preferably 10-30%, compared to the same surface-treated filler material product a solvent treated with only one at least monosubstituted succinic anhydride. In this application, unless otherwise stated, FT4 Powder Rheometer (Freeman Technology, UK) is provided with Powder Rheometer software (v 5.000.00012) and Freeman Technology Data Analysis Software version 4.0.17.

Obviously, the expression same surface-treated filler material product treated with at least one monosubstituted succinic anhydride refers to a surface-treated filler material product that has been treated with a similar amount (±0.2 wt%) of at least , only one monosubstituted succinic anhydride instead of the sum of the amounts of at least one monosubstituted succinic anhydride and a mixture of aliphatic linear or branched carboxylic acids containing stearic acid of the present invention.

The surface-treated filler material product treated with monosubstituted succinic anhydride(s) and a mixture of aliphatic linear or branched carboxylic acids containing stearic acid as defined above also shows improved dispersion in the polymer matrix of the polymer composition. Thus, another aspect of the present invention relates to the use of at least one monosubstituted succinic anhydride and/or salt reaction product(s) thereof in combination with a mixture of aliphatic linear or branched carboxylic acids containing stearic acid in an amount of at least 10.0 wt.% in relation to the total mass of the mixture, and one or more additional saturated aliphatic linear or branched carboxylic acids containing a total number of carbon atoms from C ₁₂ to C ₂₄ and / or salt product (s) of their reaction, to improve the dispersion of carbonate calcium in the polymer matrix of the polymer composition.

Obviously, an improvement is achieved if, when measuring the flowability of the powder using the method

- 30 041327 shear cell on an FT4 Powder Rheometer (ASTM D7891-15) with a pre-normal shear stress of 15 kPa, the yield strength (UYS) is reduced by at least 7%, preferably by 7-30%, more preferably by at least 10 %, and most preferably by 1030%, or the flow factor (FF) is increased by at least 7%, preferably by 7-30%, more preferably by at least 10%, and most preferably by 10-30%, and/ or when measuring the flowability of a powder by a method using a programmable stability sequence and variable rate sequences on the FT4 Powder Rheometer, the basic flow energy (BFE) is reduced by at least 7%, preferably by 7-30%, more preferably by at least 10% , and most preferably by 10-30% compared to the same surface-treated filler material product treated with at least one monosubstituted succinic anhydride going.

Obviously, the expression same surface-treated filler material product treated with at least one monosubstituted succinic anhydride refers to a surface-treated filler material product that has been treated with a similar amount (±0.2 wt%) of at least one monosubstituted succinic anhydride instead of the sum of the amounts of at least one monosubstituted succinic anhydride and a mixture of aliphatic linear or branched carboxylic acids containing stearic acid of the present invention.

Another aspect of the present invention is directed to an article containing a polymer composition as defined above and/or to a surface treated filler material product as defined above and/or to a fiber and/or to a filament and/or to a film, and /or on a thread, and/or on a sheet, and/or on a pipe, and/or on a profile, and/or on a mold for molding, and/or on a mold for injection molding, and/or on a mold for blow molding, as defined above. The product is preferably selected from the group consisting of hygiene products, medical and sanitary products, filter products, geotextile products, agronomic and horticultural products, clothing, footwear and luggage products, household and industrial products, packaging products, construction products, and the like.

Preferably, the hygiene products are selected from the group consisting of absorbent hygiene products such as baby diapers or diapers, feminine hygiene products, adult incontinence products, depilatory strips, dressings and wound dressings, disposable bath towels and face towels, disposable flip flops and shoes, top sheets or covers, consumer face masks, diaper cuffs, take-up/distribution layers, insulation layers, backing sheets, stretch eyelets, receiving areas, sprinkle layers, and attachment systems; and wipes such as wet wipes, skin care wipes, baby wipes, facial wipes, cleaning wipes, hand and body wipes, wet toilet paper, personal care wipes, feminine hygiene wipes, antibacterial wipes, and medicated wipes. napkins.

Preferably the medical and sanitary products are selected from the group consisting of medical products that can be sterilized, medical packaging, caps like disposable surgical caps, protective clothing, surgical gowns, surgical masks and face masks, surgical gowns, surgical covers, surgical drapes, wraps. , bags, sponges, dressings, wipes, linens, contamination control gowns, examination gowns, lab coats, isolation gowns, transdermal drug delivery devices, diapers, absorbent pads, treatment packs, thermal packs, colostomy pads, fixation bands, incubation mattresses, sterilized wraps (CSR wraps), wound care items, cold/hot compresses, patch-like drug delivery systems.

Preferably the filter products are selected from the group consisting of gasoline filters, oil filters, air filters, water filters, coffee filters, tea bags, pharmaceutical industry filters, mineral processing filters, fluid cartridges and bag filters, vacuum bags, membranes. for allergens and laminates with non-woven layers.

Preferably the geotextile products are selected from the group consisting of soil and pavement stabilizers, foundation stabilizers, erosion control, canal structures, drainage systems, geomembrane protection, thermal insulation, agronomic mulching, water barriers for ponds and canals, infiltration barrier sand for drainage pipes and insulating coatings for land.

Preferably, the agronomic and horticultural products are selected from the group consisting of crop covers, plant protection, seed covers, weed control fabrics, greenhouse shading, root control bags, biodegradable plant pots, capillary mats and landscape fabric.

Preferably, clothing, footwear, and luggage products are selected from the group consisting of linings like outerwear fronts, collars, trims, waistbands, lapels, and the like, disposable undergarments, shoe components like lace hole reinforcements, sports shoe reinforcements. and sandals and insoles, and the like, bag components, binding agents, tags for joining parts and (for laundry).

Preferably the packaging products are selected from the group consisting of handle bags, waste bags, transparent foil, sanitary films, agronomic foil, paper-like foil, bottles, (thermoformable) foil, extrusion-coated paper and paperboard, boxboard, paperboard, paper bags , bags, corrugated cardboard boxes, flexible tubes, for example for creams, for example for dermal creams and cosmetics, bags, for example for household waste, and containers, oriented and biaxially oriented films, pallets, and the like.

Preferably, household and industrial products are selected from the group consisting of abrasives, linens like mattress spring covers, spacer sheets, spring cases, topsheets, quilted liners, duvet covers, pillowcases, and the like, curtains/curtains, carpets/pads. for carpets like rugs, carpet tiles, bath mats, and the like, cover material and release material, detergent packs, fabric softener sheets, flooring, furniture/upholstery like upholstery, cushion lining, dust cover , spring covers, tear tapes, and the like, mops, table linens, tea and coffee bags, vacuum cleaner bags, wall covering, wipes like household wipes, floor cloths, cleaning wipes, pet wipes, and the like, automotive structures, cable sheathing, civil structures, filtration packaging, protective clothing, primary and secondary carpet backings, composites, sailing laminates, tablecloth laminates, cut yarn mats, machine embroidery backing/stabilizer, packaging when porosity is required, insulation similar to fiberglass wadding, pillows, cushions, padding similar to padding furniture, padding in quilts or duvets, household and medical face masks, postal envelopes, tarpaulins, awning and transportation material (lumber, steel), disposable clothing like shoe covers and coveralls, and windscreens.

Preferably construction products are selected from the group consisting of windscreen, asphalt pavement, road and railroad tracks, golf and tennis courts, wall covering underlays, acoustic wall coverings, roofing materials and self leveling screed under tiles, soil and road base stabilizers, foundation stabilizers, erosion control, canal structures, drainage systems, geomembrane protection, frost protection, agronomic mulching, water barriers for ponds and channels, and sand infiltration barriers for drainage pipes.

Preferably the product is a packaging product, more preferably a product selected from the group consisting of handle bags, waste bags, transparent foils, sanitary films, agronomic foils, paper-like foils, bottles, (thermoformable) foils, extrusion-coated paper and board, boxboard, paperboard, paper bags, bags, corrugated cardboard boxes, flexible tubes, e.g. for creams, e.g. for dermal creams and cosmetics, bags, e.g. for household waste, and containers, oriented and biaxially oriented films, pallets, etc.

Brief description of the figures

Fig. 1 and 2 refer to the flowability of the powder - stability and variable consumption of powders 1-4.

The following examples may further illustrate the present invention, but are not intended to limit the invention to the illustrated embodiments. The examples below show the improved product flow of the surface treated filler material and its improved dispersion in the polymer matrix of the polymer composition.

Examples

A. Methods of measurement.

The following measurement methods are used to evaluate the parameters given in the examples and claims.

Particle size distribution (wt. % particle diameter <X) and mass median diameter (d ₅₀ ) of the particulate material

As used herein and as generally defined in the art, the d ₅₀ value is determined based on measurements made using a Sedigraph™ 5100, Micromeritics Instrument Corporation, and is defined as the size for which 50% (median point) of the particle mass corresponds to particles , having a diameter equal to the specified value.

The method and instrument are known to those skilled in the art and are commonly used to determine the grain sizes of fillers and pigments. The measurement is carried out in an aqueous solution of 0.1 wt.% Na ₄ P ₂ O ₇ . The samples are dispersed using a high speed stirrer and ultrasound.

Specific surface area of the material according to BET.

Herein, the specific surface area (in m ² /g) of the mineral filler is determined using the BET method (using nitrogen as adsorbed gas), which is well known to those skilled in the art (ISO 9277:1995). The total surface area (in m ² ) of the mineral filler is then obtained by multiplying the specific surface area by the mass (in g) of the mineral filler prior to processing.

The number of surface treatment layers.

The amount of treatment layer of the calcium carbonate-containing filler material is calculated theoretically from the BET values of the untreated calcium carbonate-containing filler material and from the amount of monosubstituted succinic anhydride and a mixture of aliphatic linear or branched carboxylic acids containing stearic acid that is used for surface treatment. It is believed that 100% mono-substituted succinic anhydride and a mixture of aliphatic linear or branched carboxylic acids containing stearic acid added to the calcium carbonate-containing filler material are present in the surface treatment layer on the surface of the calcium carbonate-containing filler material.

Water capture.

The water entrapment propensity of a material, as mentioned herein, is defined in mg moisture/g after exposure to an atmosphere of 10% and 85% relative humidity, respectively, for 2.5 hours at +23°C (±2°C ). For this purpose, the sample is first exposed to an atmosphere of 10% relative humidity for 2.5 hours, then the atmosphere is changed to an atmosphere of 85% relative humidity, at which the sample is kept for another 2.5 hours. Weight increase for a relative humidity of 10 and 85% is then used to calculate moisture uptake in mg moisture/g sample.

Powder flow - a method using a programmable stability sequence and variable rate sequences.

Basic Flow Energy (BFE), Stability Index (SI), Specific Energy (SE), Flow Index (FRI) and Conditioned Bulk Density (CBD) are measured on an FT4 Powder Rheometer (Freeman Technology, UK) equipped with Powder Rheometer software (v 5.000 .00012) and Freeman Technology Data Analysis Software version 4.0.17 using a programmable stability sequence and variable rate sequence method.

This method consists in filling a cylindrical container (glass container 25 mmx25 ml).

The first step of the test method is to obtain a uniform, conditioned state of the powder in order to make it possible to carry out measurements with high reproducibility. The conditioning cycle involves the dynamic separation of the powder into thin layers by means of a bottom-up examination impeller followed by an upward rotating return that lifts the powder above the blade and drops it. This process helps eliminate the impact of varying sampling techniques and powder storage times.

After the initial conditioning step, the volume of the powder is adjusted to the size of the container with excess powder removed (separation), and the weight is recorded after the separation step. This is followed by 8 repetitive conditioning and measurement cycles with a 23.5 mm blade. For each examination cycle, the blade passes through the powder layer from top to bottom, rotating (counterclockwise, blade tip speed 100 mm/s, helical angle=5°/target height 5 mm) and up. For the conditioning step, the blade is introduced into the powder bed from top to bottom (blade edge speed 40 mm/s, helical angle 5°, target height 5 mm) and up. After these 8 passes, 3 more cycles (conditioning+examination) are carried out at different flow rates, i.e. at the impeller edge speed of 70 mm/s (pass 9), 40 mm/s (pass 10) and finally 10 mm/s ( passage 11). The energy and the torque are recorded and this makes it possible to calculate various flow parameters defined as follows.

Base flow energy (BFE, mJ): power cycle 7 (down).

Stability indicator: (energy passage 7) / (energy cycle 1).

Specific energy (SE, mJ/g): (energy cycle up 6+energy cycle up 7)/(2xdivided mass).

Flow Rate (FRI): (energy pass 11)/(energy pass 8).

Conditioned bulk density (CBD, g/ml): (divided mass)/(divided volume).

Powder flow - shear cell method.

Shear cell performance is measured using an FT4 Powder Rheometer (Freeman Technology, UK) according to ASTM D7891-15 using a cylindrical vial (glass vial 50 mm x 85 ml or 25 mm x 10 ml), a 48 mm or 24 mm shear cell and pre-normal shear stress. 15 kPa.

The measurement is carried out using the following stepwise procedure.

Initial powder conditioning.

The first step of the testing method is to obtain a uniform, conditioned state of the powder in order to enable measurements with high reproducibility. The conditioning cycle includes the dynamic separation of the powder into thin layers using

- 33 041327 movement of the research impeller from bottom to top followed by an upward rotation that lifts the powder and pours it over the blade. This process helps eliminate the impact of varying sampling techniques and powder storage times.

Initial compaction.

The conditioned column of powder is compacted using a ventilated compacting piston (allowing entrapped air to escape) with a force equal to that of the pre-normal shear stress.

critical consolidation.

The points on the yield curve represent the shear stress values corresponding to the initial yield at each level of normal stress. To achieve initial fluidity, the specimen must be over-consolidated with respect to the normal shear stress applied. This is realized by reaching a critical level of consolidation at steady flow and then decreasing the normal shear stress. Thus, shear research is a two-stage method, consisting of:

1. Pre-shift.

The purpose of pre-shear is to achieve critical consolidation at a given level of pre-normal shear stress. During this process, shearing is continued until a stationary flow rate is reached, at which point the pre-shearing application is terminated.

2. Shift research.

The normal stress is reduced so that the sample now becomes over-consolidated with respect to the now applied normal stress. Then the shear is resumed and the initial yield point is measured.

For each preliminary normal shear stress, five measurements are made at five normal stresses defined by the standard (9; 8; 7; 6 and 5 kPa). The shear stress measurement is also carried out at the pre-normal shear stress level, i.e. at 15 kPa.

The five measurements taken constitute the yield points for each level of pre-normal shear stress. Yield points are plotted as a function of normal stress, from which Mohr circles can be added to extrapolate data for different flows.

Extrapolated data includes:

cohesion, (C, kPa) - shear stress, where the line of best fit crosses the y-axis, i.e. normal stress=0;

yield stress, (UYS, kPa) - the larger of the 2 values at which the smaller Mohr circle intersects the x-axis, (also known as σc);

the largest principal stress, (MPS, kPa) is the larger of the two values at which the larger Mohr circle intersects the x-axis (also known as σ1);

angle of internal friction (AIF, °) - the angle formed by the line of best fit with the horizontal axis;

flow factor (FF): corresponds to MPS/UYS;

bulk density (BD, g/ml): conditioned bulk density after initial compaction.

extrusion modeling.

An extrusion simulation is developed to evaluate the dispersion of the miner in the polymer composition. The study is carried out on a commercially available Collin Pressure Filter Test Teach-Line FT-E20T-IS.

The test method is carried out for each of the respective polymer compositions, while the melt pump is not used, the speed of the extruder screw is maintained at 100 rpm, and the melt temperature is from 225 to 230°C (temperature setting of the extruder: 190°C210°C230 °C; temperature setting of the extruder head: 230°C-230°C).

Each of the respective polymer compositions (900 g of effective powder A or B per 2500 g of the finished sample obtained by diluting the polymer composition in LLDPE ExxonMobil LL 1001 VX) is measured using a 40 µm filter (GKD Gebr. Kufferath AG, Duren, Germany, Artikelnummer 12102170055).

The results are expressed as a bar and can be calculated by subtracting the final melt temperature (determined after 5 minutes of pure polymer material purge) from the initial pressure of the pure polymer material (LLDPE ExxonMobil LL 1001 VX).

Ash content.

Ash content testing is carried out by burning 5-30 g of the respective polymer composition at 570° C. for 120 minutes.

- 34 041327

B) materials.

Filler materials containing calcium carbonate.

Filler material containing calcium carbonate, 1 (powder 1; comparative).

0.7 kg of wet ground and spray dried marble from Carrara, Italy (d ₅₀ = 1.6 µm, BET specific surface area = 4.1 m ² /g) are placed in a high speed mixer (Somakon MPLB Mixer, Somakon Verfahrenstechnik , Germany) and conditioned by stirring for 10 min (1000 rpm, 120°C). After this time, 0.6 parts by weight per 100 parts by weight of CaCO ₃ monosubstituted succinic anhydride 1 was added to the mixture. Stirring and heating were then continued for another 15 minutes (120° C., 1000 rpm). After this time, the mixtures are allowed to cool and the powder is collected (powder 1).

Filler material containing calcium carbonate, 2 (powder 2; according to the present invention).

0.7 kg of wet ground and spray dried marble from Carrara, Italy (d50=1.6 µm, BET specific surface area=4.1 m ² /g) are placed in a high speed mixer (Somakon MPLB Mixer, Somakon Verfahrenstechnik , Germany) and conditioned by stirring for 10 min (1000 rpm, 120°C). After this time, 0.5 wt.h. per 100 wt.h. CaCO ₃ monosubstituted succinic anhydride 1 and 0.2 wt.h. per 100 wt.h. CaCO ₃ carboxylic acids from mixture 2. Stirring and heating are then continued for another 15 min (120° C., 1000 rpm). After this time, the mixtures are allowed to cool and the powder is collected (powder 2).

Filler material containing calcium carbonate, 3 (powder 3; according to the present invention).

0.7 kg of wet ground and spray dried marble from Carrara, Italy (d50=1.6 µm, BET specific surface area=4.1 m ² /g) are placed in a high speed mixer (Somakon MPLB Mixer, Somakon Verfahrenstechnik, Germany and conditioned by stirring for 10 min (1000 rpm, 120° C.) At the end of this time, 0.4 parts by weight per 100 parts by weight of CaCO ₃ monosubstituted succinic anhydride 1 and 0 are simultaneously added to the mixture 4 parts by weight per 100 parts by weight CaCO ₃ carboxylic acids from mixture 2. Stirring and heating are then continued for a further 15 minutes (120° C., 1000 rpm). and the powder is collected (powder 3).

Filler material containing calcium carbonate, 4 (powder 4; according to the present invention).

0.7 kg of wet ground and spray dried marble from Carrara, Italy (d50=1.6 µm, BET specific surface area=4.1 m ² /g) are placed in a high speed mixer (Somakon MPLB Mixer, Somakon Verfahrenstechnik, Germany) and conditioned by stirring for 10 min (1000 rpm, 120°C). After this time, 0.4 wt.h. is added to the mixture. per 100 wt.h. CaCO ₃ monosubstituted succinic anhydride 1. Then stirring and heating continued for another 15 min (120°C, 1000 rpm). Then, 0.2 wt.h. is added to the mixture. per 100 wt.h. CaCO ₃ carboxylic acids from mixture 2, and then stirring and heating continued for another 15 min (120°C, 1000 rpm). After this time, the mixtures are allowed to cool and the powder is collected (powder 4).

Monosubstituted succinic anhydride.

Monosubstituted succinic anhydride (ASA) 1.

Alkenyl monosubstituted succinic anhydride (2,5-furandione, dihydro-, mono-C ₁₅ - ₂₀ alkenyl derivative, CAS No. 68784-12-3) is a mixture of mainly branched octadecenyl succinic anhydrides (CAS #28777-98-2) and in mainly branched hexadecenyl succinic anhydrides (CAS #32072-96-1). More than 80% of the mixture are branched octadecenyl succinic anhydrides. The purity of the mixture >95 wt.%. The residual content of olefins is below 3 wt.%.

A mixture of carboxylic acids 2.

The mixture of carboxylic acids 2 is a 1:1 mixture of stearic acid and palmitic acid.

Powder A (of the present invention): dry ground limestone from Nocera Umbria (d ₅₀ =3.2, maximum diameter=12 µm; BET specific surface area=3.0 m ² /g) treated with 0.35 wt .% monosubstituted succinic anhydride 1 and 0.15 wt.% mixture of carboxylic acids 2.

Powder B (known from the literature): dry ground limestone from Nocera Umbria (d50=3.2, maximum diameter=12 µm; BET specific surface area=3.0 m ² /g) treated with 0.45 wt. % monosubstituted succinic anhydride 1.

Results of analyzes and studies

Example 1 Water Entrainment Results.

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Table 1. Water Pickup Values for Powders 1-4

Powder Water uptake (mg/g) Powder 1: comparative 0.5 Powder 2: according to the present invention 0.4 Powder 3: according to the present invention 0.45 Powder 4: according to the present invention 0.2

Example 2 Powder Flow: Stability and Variable Rate. Fluidity of powders 1-4 was measured on the FT4 Powder Rheometer, Freeman Technology, using a programmable stability sequence and variable flow sequences method in a 25 mm x 25 ml measuring cell. Improved powder flows are achieved for powders 2-4 compared to reference powder 1, as can be seen from the lower base flow energy obtained for these powders (Figure 1 and Table 2)

Table 2. Powder Flow - Stability and Variable Rate (Powders 1-4), Basic Flow Energy (BFE), Stability Index (SI), Flow Index (FRI), Specific Energy (SE), Conditioned Bulk Density (CBD)

Powder BFE, mJ SI FRI SE, mJ/g CBD, g/ml Powder 1 158.13 1.07 1.81 7.89 0.69 Powder 2 122.42 1, Yu 1.96 6.95 0.70 Powder 3 99.49 1, Yu 2.10 6.17 0.71 Powder 4 142.47 1.06 1.78 7.19 0.70

Improved powder flow is achieved for powders 2-4 compared to reference powder 1, as can be seen from the lower base flow energy obtained for these powders (Fig. 1 and Table 2)

Example 3. Obtaining a polymer composition (concentrate) and the result of research (sol content and extrusion simulation).

Concentrates (MW) are prepared following the protocol described below.

Polymer compositions containing 25 wt.% Dowlex 5056G (LLPDE, MFI=1 g/10 min) and 75 wt.% powder A or B, respectively, (concentrate A or B) are prepared on a laboratory scale using a Buss mixer (PR46, Buss AG, Switzerland, L/d 10) at 10 kg/h, and processed with the following equipment settings:

Screw temperature: 100°C.

Extruder temperature (2 zones): 190°C-170°C.

Extraction temperature (1 zone): 170°C.

Screw speed: 200 rpm.

Dosing of polymer: 100% in the main tray.

Powder dosage: 73% to the main tray, 27% to the side feeder.

The mixtures obtained are granulated in a spring-loaded granulator, model SLC (Gala, USA) in a water bath having an initial temperature between 20 and 25°C. The composition and content of the filler obtained Concentrates are given in table. 3 below. The exact filler content is determined from the ash content. In addition, an extrusion simulation study is carried out to determine the dispersion quality of the filler material product in the polymer matrix of the compounded materials.

The results shown in table. 3 confirm that concentrates A and B are obtained with good quality. In addition, an extrusion simulation study showed that the surface treated filler material product of the present invention, i.e., concentrate A, shows improved dispersion quality in the compounded polymer matrix, compared to the filler material product known from the literature, i.e., concentrate B.

Table 3. Compositions and properties of the prepared concentrates

MBA (based on powder A) MV V (based on powder B) Powder quantity 74.3 74 (% mass) Amount of LLPDE (% mass) 25.7 26 Pressure increase during extrusion simulation study at 40 µm (bar) pore size 12.4 13.4

The pressure increase when extruding 900 g of powder A on a 40 µm sieve is lower than for powder B, thus showing advantageous properties, improved powder dispersion

Claims (12)

And in a compounded polymer matrix Example 4 Powder Flow: Shear Cell. Powder flow for powders 1-4 was measured on an FT4 Powder Rheometer, Freeman Technology, using a shear cell method (15 kPa), in a 25 mm x 10 ml measuring cell. Achieve improved powder flow and lower cohesion for powders 2 and 4 compared to reference powder 1 as can be seen from the lower cohesion values, lower yield stress (UYS) and higher yield factor (FF) obtained for these powders (Fig. 2 and Table 4) Table 4. Powder Flow - Shear Cell (Powders 1-4), Cohesion, Yield Stress (UYS), Major Principal Stress (MPS) and Flow Factor (FF) Powder Cohesion, kPa UYS, kPa MPS, kPa FF Powder 1 3.25 10.85 24.56 2.26 Powder 2 2.64 8.68 23.37 2.69 Powder 4 2.71 8.66 22.97 2.65 CLAIM 1. A process for preparing a filler material product surface-treated with at least one monosubstituted succinic anhydride and a mixture of saturated aliphatic linear or branched carboxylic acids containing stearic acid, comprising at least the steps of: a) obtaining at least one filler material containing calcium carbonate, b) obtaining at least one monosubstituted succinic anhydride, c) obtaining a mixture of saturated aliphatic linear or branched carboxylic acids, consisting of stearic acid in an amount of at least 10.0 wt.% in relation to the total mass of the mixture and one or more additional saturated aliphatic linear or branched carboxylic acids containing the total number of atoms carbon from C ₁₂ to C ₂₄ , d) bringing into contact the surface of at least one calcium carbonate-containing filler material from step a), while stirring in one or more steps in any order, with at least one monosubstituted succinic anhydride from step b) and a mixture of saturated aliphatic linear or branched carboxylic acids from step c) so that the treatment layer containing this at least one monosubstituted succinic anhydride and/or at least one salt reaction product thereof and a mixture of saturated aliphatic linear or branched carboxylic acids and/or at least one the salt product of their reaction is formed on the surface of said at least one filler material containing calcium carbonate from step a), where the temperature before and/or during contacting step d) is controlled in such a way that this at least one monosubstituted succinic anhydride and a mixture of saturated aliphatic linear or branched carbons oic acids are in a molten or liquid state. 2. Method according to claim 1, wherein the calcium carbonate-containing filler material from step a) is selected from the group consisting of ground calcium carbonate, preferably marble, limestone, dolomite and/or chalk, precipitated calcium carbonate (PCC), preferably vaterite , calcite and/or aragonite, surface-reacted calcium carbonate (MCC) and mixtures thereof, more preferably the filler material containing calcium carbonate is ground calcium carbonate. 3. The method according to claim 1 or 2, where at least one filler material containing calcium carbonate from step a) has a) a value of the mass median size d ₅₀ of particles in the range from 0.1 to 7 µm, preferably from 0.25 to 5 µm, and most preferably from 0.5 to 4 µm, and/or b) maximum diameter (d ₉₈ )<50 µm, preferably <40 µm, more preferably <25 µm, and most preferably <15 µm, and/or c) a specific surface area (BET) from 0.5 to 150 m ² /g, preferably from 0.5 to 50 m ² /g, more preferably from 0.5 to 35 m ² /g, and most preferably from 0, 5 to 10 m ² /g, as measured by the BET method with nitrogen, and/or d) a residual total moisture content of 0.01 to 1% by weight, preferably 0.01 to 0.2% by weight, more preferably 0.02 to 0.2% by weight and most preferably 0.04 up to 0.2 wt.% in relation to the total dry weight of at least one filler material containing calcium carbonate. 4. The method according to any one of claims 1 to 3, where at least one filler material containing calcium carbonate from step a) is preheated before step d) is carried out. - 37 041327 contact, preferably at least one filler material containing calcium carbonate, from stage a) is preheated at a temperature of from 20 to 200°C, more preferably from 40 to 200°C, even more preferably from 50 to 150°C, and most preferably from 60 to 130°C. 5. The method according to any one of claims 1 to 4, wherein at least one monosubstituted succinic anhydride from step b) consists of succinic anhydride monosubstituted with a group selected from a linear, branched, aliphatic and cyclic group containing a total number of carbon atoms from C ₂ to C ₃₀ , preferably C ₃ to C ₂₅ and most preferably C ₄ to C ₂₀ in the substituent. 6. The method according to any one of claims 1 to 5, wherein at least one monosubstituted succinic anhydride from step b) is a) at least one alkyl monosubstituted succinic anhydride, preferably at least one alkyl monosubstituted succinic anhydride, selected from the group consisting of ethyl succinic anhydride, propyl succinic anhydride, butyl succinic anhydride, triisobutyl succinic anhydride, pentyl succinic anhydride, hexyl succinic anhydride, heptyl succinic anhydride, octysuccinic anhydride, no , decyl succinic anhydride, dodecyl succinic anhydride, hexadecanyl succinic anhydride, octadecanyl succinic anhydride and mixtures thereof, and/or b) по меньшей мере один алкенилмонозамещенный янтарный ангидрид, предпочтительно по меньшей мере один алкенилмонозамещенный янтарный ангидрид, выбранный из группы, включающей этенилянтарный ангидрид, пропенилянтарный ангидрид, бутенилянтарный ангидрид, триизобутенилянтарный ангидрид, пентенилянтарный ангидрид, гексенилянтарный ангидрид, гептенилянтарный ангидрид, октенилянтарный ангидрид, ноненилянтарный ангидрид , decenylsuccinic anhydride, dodecenylsuccinic anhydride, hexadecenylsuccinic anhydride, octadecenylsuccinic anhydride and mixtures thereof. 7. The method according to any one of claims 1 to 6, wherein the mixture of saturated aliphatic linear or branched carboxylic acids from step c) contains stearic acid and one or more additional saturated aliphatic linear or branched carboxylic acids containing a total number of carbon atoms from C ₁₂ to C ₂₂ , preferably C ₁₂ to C ₂₂ , more preferably C ₁₂ to C ₂₀ , and most preferably C ₁₄ to C ₂₀ . 8. The method according to any one of claims 1 to 7, wherein step d) of bringing into contact is carried out in such a way that at least one monosubstituted succinic anhydride from step b) and a mixture of saturated aliphatic linear or branched carboxylic acids from step c) are added at weight ratio succinic anhydride/carboxylic acid mixture from 10:1 to 1:10, preferably from 5:1 to 1:5, and most preferably from 4:1 to 1:4, for example from 4:1 to 1:1. 9. Process according to any one of claims 1 to 8, wherein at least one monosubstituted succinic anhydride from step b) is added in contacting step d) in a total amount of from 0.1 to 3% by weight, preferably from 0.2 up to 2 wt.%, and most preferably from 0.3 to 1.5 wt.% in relation to the total dry weight of at least one filler material containing calcium carbonate from stage a); and the mixture of saturated aliphatic linear or branched carboxylic acids from step c) is added in contacting step d) in a total amount of 0.1 to 3% by weight, preferably 0.2 to 2% by weight, and most preferably 0 ,3 to 1.5 wt.% in relation to the total dry weight of at least one filler material containing calcium carbonate from stage a). 10. The method according to any one of claims 1 to 9, wherein step d) of bringing into contact is carried out at a temperature of from 20 to 200°C, preferably from 40 to 150°C, and most preferably from 60 to 130°C. 11. The method according to any one of claims 1 to 10, wherein step d) of bringing into contact is carried out in such a way that at least one monosubstituted succinic anhydride from step b) and a mixture of saturated aliphatic linear or branched carboxylic acids from step c) are added simultaneously or so that the mixture of saturated aliphatic linear or branched carboxylic acids from step c) is added after at least one monosubstituted succinic anhydride from step b), preferably so that the mixture of saturated aliphatic linear or branched carboxylic acids from step c) is added after at least one monosubstituted succinic anhydride from step b). 12. The method according to any one of claims 1 to 11, where at least one monosubstituted succinic anhydride is obtained in step b) in such an amount that the total weight of said at least one monosubstituted succinic anhydride and/or at least one salt product of their reactions on the surface of at least one filler material containing calcium carbonate, less than 5 mg/m ² , for example from 0.1 to 5 mg/m ² , preferably less than 4.5 mg/m ² , more preferably less than 4.0 mg /m ² , for example from 0.2 to 4 mg/m ² or from 1 to 4 mg/m ² of at least one filler material containing calcium carbonate obtained in step a), and/or a mixture of saturated aliphatic linear or branched carboxylic acids from step c) are obtained in step c) in such an amount that the total weight of the mixture of saturated aliphatic linear or branched carboxylic acids and/or at least one salt product of their reaction on the product surface of the surface-treated material fills ate is less than 5 mg/m ² , for example is from 0.1 to 5 mg/m ² , preferably less than 4.5 mg/m ² , more preferably less than 4.0 mg/m ² , for example is from 0.2 to 4 mg/m ² or 1 to 4 mg/m ² of at least one filler material containing calcium carbonate -