# US 11,441,037 B2 · Process for preparing a surface treated filler material product with mono-substituted succinic anhydride(s) and a mixture of aliphatic linear or branched carboxylic acids comprising stearic acid

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- Number: US 11,441,037 B2
- Document ID: US11441037B2
- Status: Granted
- Kind: B2
- Application number: 16/620,550
- Filed: 2018-06-12
- Published: 2020-05-21
- Granted: 2022-09-13
- Earliest claimed: 2017-06-14
- Assignees: Onya International AG
- Applicants: Omya International AG
- Inventors: Francesco Pullega; Pierre Blanchard; Tazio Fornera; Matthias Welker
- Web page: https://patentgrep.com/patent/US11441037B2

## CPC

- C09C 1/021: {Calcium carbonates}
- C08K 3/26: Carbonates; Bicarbonates
- C08K 9/00: Use of pretreated ingredients
- C08K 9/04: Ingredients treated with organic substances {(treated with macromolecular compounds C08K9/08)}
- C01P 2004/61: Micrometer sized, i.e. from 1-100 micrometer
- C01P 2004/62: Submicrometer sized, i.e. from 0.1-1 micrometer
- C01P 2006/12: Surface area
- C01P 2006/82: water content
- C08K 2003/265: {Calcium, strontium or barium carbonate}
- C08K 2201/005: Additives being defined by their particle size in general
- C08K 2201/006: Additives being defined by their surface area
- C09C: TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES (treatment of materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone C04B14/00, C04B18/00, C04B20/00); PREPARATION OF CARBON BLACK {; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS}
- C08K: Use of inorganic or non-macromolecular organic substances as compounding ingredients (paints, inks, varnishes, dyes, polishes, adhesives C09)
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS

## Abstract

The present invention relates to a process for preparing a surface treated filler material product with mono-substituted succinic anhydride(s) and a mixture of aliphatic linear or branched carboxylic acids comprising stearic acid, a surface treated filler material product, a polymer composition, a 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 molds and/or blow mold comprising the surface treated filler material product and/or the polymer composition, an article comprising the surface treated filler material product and/or the polymer composition and/or the 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 as well as the use of at least one mono-substituted succinic anhydride and/or salty reaction product(s) thereof in combination with a mixture of aliphatic linear or branched carboxylic acids comprising stearic acid and/or salty reaction product(s) thereof, for improving the flowability of a surface treated filler material product and for improving the dispersion of the calcium carbonate in the polymer matrix of a polymer composition.

## Claims

### Claim 1

A surface treated filler material product comprising
a) at least one calcium carbonate-containing filler material,
b) a treatment layer on the surface of the at least one calcium carbonate-containing filler material comprising at least one mono-substituted succinic anhydride and/or salty reaction product(s) thereof and a mixture of aliphatic linear or branched carboxylic acids comprising stearic acid in an amount of at least 10.0 wt. %, based on the total weight of the mixture, and one or more further saturated aliphatic linear or branched carboxylic acid(s) having a total amount of carbon atoms from C8 to C24, and/or salty reaction product(s) thereof,
wherein the surface treated filler material product comprises the treatment layer in an amount of from 0.2 to 6 wt. %, based on the total dry weight of the at least one calcium carbonate-containing filler material, wherein the surface treated filler material product is in form of a powder.

### Claim 2 (depends on 1)

The surface treated filler material product according to claim 1, wherein the calcium carbonate-containing filler material is selected from the group consisting of ground calcium carbonate, marble, limestone, dolomite, chalk, precipitated calcium carbonate (PCC), vaterite, calcite, aragonite, surface-reacted calcium carbonate (MCC) and mixtures thereof.

### Claim 3 (depends on 1)

A polymer composition comprising at least one polymeric resin and from 1 to 95 wt.-%, based on the total weight of the polymer composition, of the surface treated filler material product according to claim 1.

### Claim 4 (depends on 3)

The polymer composition according to claim 3, wherein the at least one polymeric resin is at least one thermoplastic polymer.

### Claim 5 (depends on 3)

The polymer composition according to claim 3, wherein the polymer composition is a masterbatch.

### Claim 6 (depends on 1)

A 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 molds and/or blow mold comprising the surface treated filler product according to claim 1 or a polymer composition comprising at least one polymeric resin and from 1 to 95 wt. %, based on the total weight of the polymer composition, of the surface treated filler material product according to claim 1.

### Claim 7 (depends on 1)

An article comprising the surface treated filler material product according to claim 1 or a polymer composition comprising at least one polymeric resin and from 1 to 95 wt. %, based on the total weight of the polymer composition, of the surface treated filler material product according to claim 1,
wherein the article is selected from the group consisting of hygiene products, medical and healthcare products, filter products, geotextile products, agriculture and horticulture products, clothing, footwear and baggage products, household and industrial products, packaging products, and construction products.

### Claim 8 (depends on 7)

The article according to claim 7 being a packaging product selected from the group consisting of carrier bags, waste bags, transparent foils, hygiene films, agriculture foils, paper like foils, bottles, thermoform foils, extrusion coated papers and boards, boxboards, paperboard cartons, paper bags, sacks, corrugated boxes, flexible tubes, bags, oriented and bi-oriented films, and trays.

### Claim 9 (depends on 6)

An article comprising the 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 molds and/or blow mold according to claim 6, wherein the article is selected from the group consisting of hygiene products, medical and healthcare products, filter products, geotextile products, agriculture and horticulture products, clothing, footwear and baggage products, household and industrial products, packaging products, and construction products.

### Claim 10 (depends on 1)

The surface treated filler material product according to claim 1, wherein the at least one calcium carbonate-containing filler material has
a) a weight median particle size d50 value in the range from 0.1 μm to 7 μm and/or
b) a top cut (d98) of ≤50 μm and/or
c) a specific surface area (BET) of from 0.5 to 150 m2/g and/or
d) a residual total moisture content of from 0.01 wt.-% to 1 wt.-%, based on the total dry weight of the at least one calcium carbonate-containing filler material.

### Claim 11 (depends on 3)

The polymer composition according to claim 3, wherein the polymer composition is a masterbatch and the masterbatch comprises the surface treated filler material product in an amount of from 50 to 95 wt.-%.

### Claim 12 (depends on 1)

The surface treated filler material product according to claim 1, wherein the at least one calcium carbonate-containing filler material has
a) a weight median particle size d50 value in the range from 0.5 μm to 4 μm and/or
b) a top cut (d98) of ≤15 μm and/or
c) a specific surface area (BET) of from 0.5 to 10 m2/g and/or
d) a residual total moisture content of from 0.04 wt.-% to 0.2 wt.-%, based on the total dry weight of the at least one calcium carbonate-containing filler material.

### Claim 13 (depends on 1)

The surface treated filler material product according to claim 1, wherein the at least one mono-substituted succinic anhydride consists of succinic anhydride mono-substituted with a group selected from a linear, branched, aliphatic and cyclic group having a total amount of carbon atoms from C2 to C30 in the substituent.

### Claim 14 (depends on 1)

The surface treated filler material product according to claim 1, wherein the at least one mono-substituted succinic anhydride is
a) at least one alkyl mono-substituted succinic anhydride, ethylsuccinic anhydride, propylsuccinic anhydride, butylsuccinic anhydride, triisobutyl succinic anhydride, pentylsuccinic anhydride, hexylsuccinic anhydride, heptylsuccinic anhydride, octylsuccinic anhydride, nonylsuccinic anhydride, decyl succinic anhydride, dodecyl succinic anhydride, hexadecanyl succinic anhydride, octadecanyl succinic anhydride, and mixtures thereof, and/or
b) at least one alkenyl mono-substituted succinic anhydride, ethenylsuccinic anhydride, propenylsuccinic anhydride, butenylsuccinic anhydride, triisobutenyl succinic anhydride, pentenylsuccinic anhydride, hexenylsuccinic anhydride, heptenylsuccinic anhydride, octenylsuccinic anhydride, nonenylsuccinic anhydride, decenyl succinic anhydride, dodecenyl succinic anhydride, hexadecenyl succinic anhydride, octadecenyl succinic anhydride, and mixtures thereof.

### Claim 15 (depends on 1)

The surface treated filler material product according to claim 1, wherein the mixture of saturated aliphatic linear or branched carboxylic acids comprises stearic acid and one or more further saturated aliphatic linear or branched carboxylic acid(s) having a total amount of carbon atoms from C8 to C22.

### Claim 16 (depends on 1)

A process for preparing a surface treated filler material product of claim 1, the process comprising the steps of:
a) providing at least one calcium carbonate-containing filler material,
b) providing at least one mono-substituted succinic anhydride,
c) providing a mixture of aliphatic linear or branched carboxylic acids comprising stearic acid in an amount of at least 10.0 wt. %, based on the total weight of the mixture, and one or more further saturated aliphatic linear or branched carboxylic acid(s) having a total amount of carbon atoms from C8 to C24,
d) contacting the surface of the at least one calcium carbonate-containing filler material of step a), under mixing, in one or more steps, in any order, with the at least one mono-substituted succinic anhydride of step b) and the mixture of aliphatic linear or branched carboxylic acids of step c) such that a treatment layer comprising the at least one mono-substituted succinic anhydride and/or salty reaction product(s) thereof and the mixture of aliphatic linear or branched carboxylic acids and/or salty reaction product(s) thereof is formed on the surface of said at least one calcium carbonate-containing filler material of step a),
wherein the temperature before and/or during contacting step d) is adjusted such that the at least one mono-substituted succinic anhydride and the mixture of aliphatic linear or branched carboxylic acids is in a molten or liquid state, wherein the surface treated filler material product is in form of a powder.

### Claim 17 (depends on 16)

The process according to claim 16, wherein the at least one calcium carbonate-containing filler material of step a) is preheated before contacting step d) is carried out.

### Claim 18 (depends on 16)

The process according to claim 16, wherein contacting step d) is carried out in that the at least one mono-substituted succinic anhydride of step b) and the mixture of saturated aliphatic linear or branched carboxylic acids of step c) are added in a weight ratio [succinic anhydride/mixture of carboxylic acids] of from 10:1 to 1:10.

### Claim 19 (depends on 16)

The process according to claim 16, wherein the at least one mono-substituted succinic anhydride of step b) is added in contacting step d) in a total amount of from 0.1 to 3 wt.-%, based on the total dry weight of the at least one calcium carbonate-containing filler material of step a); and the mixture of saturated aliphatic linear or branched carboxylic acids of step c) is added in contacting step d) in a total amount of from 0.1 to 3 wt.-%, based on the total dry weight of the at least one calcium carbonate-containing filler material of step a).

### Claim 20 (depends on 16)

The process according to claim 16, wherein contacting step d) is carried out at a temperature of from 20 to 200° C.

### Claim 21 (depends on 16)

The process according to claim 16, wherein contacting step d) is carried out in that the at least one mono-substituted succinic anhydride of step b) and the mixture of saturated aliphatic linear or branched carboxylic acids of step c) are added simultaneously or in that the mixture of saturated aliphatic linear or branched carboxylic acids of step c) is added after the at least one mono-substituted succinic anhydride of step b).

### Claim 22 (depends on 16)

The process according to claim 16, wherein the at least one calcium carbonate-containing filler material has
a) a weight median particle size d50 value in the range from 0.1 μm to 7 μm and/or
b) a top cut (d98) of ≤50 μm and/or
c) a specific surface area (BET) of from 0.5 to 150 m2/g and/or
d) a residual total moisture content of from 0.01 wt.-% to 1 wt.-%, based on the total dry weight of the at least one calcium carbonate-containing filler material.

### Claim 23 (depends on 16)

The process according to claim 16, wherein the at least one mono-substituted succinic anhydride consists of succinic anhydride mono-substituted with a group selected from a linear, branched, aliphatic and cyclic group having a total amount of carbon atoms from C2 to C30 in the substituent.
