Process of controlled chemical reaction of a solid filler material surface and additives to produce a surface treated filler material product

Abstract

The present invention relates to a process for preparing a surface treated filler material product with succinic anhydride(s), a surface treated filler material product, a polymer composition, a fiber and/or filament and/or film and/or thread 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 as well as the use of a mono-substituted succinic anhydride for decreasing the hydrophilicity of a calcium carbonate-containing filler material surface and the use of a surface-treated filler material product for initiating the crosslinking reaction in epoxide resins.

1 . A process for preparing a surface treated filler material product with succinic anhydride(s), the process comprising at least the steps of:
 a) providing at least one calcium carbonate-containing filler material having
 i) a weight median particle size d 50  value in the range from 0.1 μm to 7 μm, 
 ii) a top cut (d 98 ) of≦15 μm, 
   iii) a specific surface area (BET) of from 0.5 to 150 m 2 /g as measured by the BET nitrogen method, and
 iv) 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, 
   b) providing at least one mono-substituted succinic anhydride and optionally at least one mono-substituted succinic acid in an 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),   c) contacting the surface of the at least one calcium carbonate-containing filler material of step a) under mixing, in one or more steps, with the at least one mono-substituted succinic anhydride and the optional at least one mono-substituted succinic acid of step b) such that a treatment layer comprising the at least one mono-substituted succinic anhydride and the optional at least one mono-substituted succinic acid 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 c) is adjusted such that the temperature is at least 2° C. above the melting point of the at least one mono-substituted succinic anhydride and the optional at least one mono-substituted succinic acid. 
     
     
         2 . The process according to  claim 1 , wherein the at least one calcium carbonate-containing filler material of step a) is selected from among ground calcium carbonate (GCC), precipitated calcium carbonate (PCC), modified calcium carbonate (MCC) and mixtures thereof. 
     
     
         3 . The process according to  claim 1 , wherein the at least one calcium carbonate-containing filler material of step a) comprises at least one ground calcium carbonate (GCC) selected from the group comprising marble, chalk, dolomite, limestone and mixtures thereof and/or at least one precipitated calcium carbonate (PCC) selected from the group comprising one or more of the aragonitic, vateritic and calcitic mineralogical crystal forms and/or at least one modified calcium carbonate (MCC). 
     
     
         4 . The process according to  claim 1 , wherein the at least one calcium carbonate-containing filler material of step a) has a weight median particle size d 50  from 0.25 μm to 5 μm and preferably from 0.7 μm to 4 μm. 
     
     
         5 . The process according to  claim 1 , wherein the at least one calcium carbonate-containing filler material of step a) has a top cut (d 98 )≦12.5 μm, preferably≦10 μm and most preferably≦7.5 μm. 
     
     
         6 . The process according to  claim 1 , wherein the at least one calcium carbonate-containing filler material of step a) has a specific surface area (BET) of from 0.5 to 50 m 2 /g, more preferably of from 0.5 to 35 m 2 /g and most preferably of from 0.5 to 15 m 2 /g as measured by the BET nitrogen method. 
     
     
         7 . The process according to  claim 1 , wherein the at least one calcium carbonate-containing filler material of step a) has a residual total moisture content of from 0.01 to 0.2 wt.-%, preferably from 0.02 to 0.15 wt.-% and most preferably from 0.04 to 0.15 wt.-%, based on the total dry weight of the at least one calcium carbonate-containing filler material. 
     
     
         8 . The process according to  claim 1 , wherein the at least one calcium carbonate-containing filler material of step a) is preheated before contacting step c) is carried out, preferably the at least one calcium carbonate-containing filler material of step a) is preheated at a temperature of from 50 to 200° C., more preferably of from 80 to 200° C., even more preferably of from 90 to 150° C. and most preferably of from 100 to 130° C. 
     
     
         9 . The process according to  claim 1 , wherein the at least one mono-substituted succinic anhydride and the optional at least one mono-substituted succinic acid of step b) are provided in a total amount of from 0.1 to 2.5 wt.-%, preferably in an amount of from 0.1 to 2 wt.-%, more preferably in an amount of from 0.1 to 1.5 wt.-%, even more preferably in an amount of from 0.1 to 1 wt.-% and most preferably in an amount of from 0.2 to 0.8 wt.-% based on the total dry weight of the at least one calcium carbonate-containing filler material. 
     
     
         10 . The process according to  claim 1 , wherein the at least one mono-substituted succinic anhydride of step b) 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, preferably from C3 to C25 and most preferably from C4 to C20 in the substituent. 
     
     
         11 . The process according to  claim 1 , wherein the at least one mono-substituted succinic anhydride of step b) is at least one alkyl mono-substituted succinic anhydride, preferably at least one alkyl mono-substituted succinic anhydride selected from the group comprising 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. 
     
     
         12 . The process according to  claim 1 , wherein the at least one mono-substituted succinic anhydride of step b) is at least one alkenyl mono-substituted succinic anhydride, preferably at least one alkenyl mono-substituted succinic anhydride selected from the group comprising 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. 
     
     
         13 . The process according to  claim 1 , wherein the at least one mono-substituted succinic anhydride and the optional at least one mono-substituted succinic acid of step b) are added in contacting step c) in a total amount of from 0.1 to 2 wt.-%, preferably of from 0.2 to 1.5 wt.-% and most preferably of from 0.3 to 1 wt.-%, based on the total dry weight of the at least one calcium carbonate-containing filler material of step a). 
     
     
         14 . The process according to  claim 1 , wherein the at least one mono-substituted succinic acid of step b) is present in an amount of≦10 mol.-%, based on the molar sum of the at least one mono-substituted succinic anhydride and the at least one mono-substituted succinic acid. 
     
     
         15 . The process according to  claim 1 , wherein contacting step c) is carried out at a temperature of from 30 to 200° C., preferably of from 80 to 150° C. and most preferably of from 110 to 130° C. 
     
     
         16 . The process according to  claim 1 , wherein contacting step c) is carried out in a batch or continuous process, preferably for a period of time from 0.1 to 1000 seconds. 
     
     
         17 . The process according to  claim 16 , wherein the contacting step c) is a continuous process and comprises one or several contacting steps and the total contacting time is from 0.1 to 20 s, preferably from 0.5 to 15 s and most preferably from 1 to 10 s. 
     
     
         18 . The process according to  claim 1 , wherein the salty reaction product(s) of the mono-substituted succinic acid and/or the at least one mono-substituted succinic anhydride formed on the surface of said at least one calcium carbonate-containing filler material in step c) are one or more calcium salts and/or one or more magnesium salts thereof. 
     
     
         19 . The process according to  claim 1 , wherein the process further comprises step d) of contacting the at least one calcium carbonate-containing filler material of step a), in one or more steps, with at least one organic material such as polysiloxanes. 
     
     
         20 . The process according to  claim 19 , wherein contacting step d) is carried out during and/or after contacting step c), preferably after contacting step c). 
     
     
         21 . The process according to  claim 19 , wherein contacting step d) is carried out at a temperature of from 40 to 200° C., preferably of from 50 to 150° C. and most preferably of from 60 to 120° C. 
     
     
         22 . The process according to  claim 19 , wherein the at least one organic material is added in contacting step d) in an amount of from 100 to 1000 ppm, preferably from 200 to 800 ppm and most preferably from 300 to 700 ppm, based on the total dry weight of the at least one calcium carbonate-containing filler material of step a). 
     
     
         23 . The process according to  claim 1 , wherein the obtained surface treated filler material product has a water pick-up of from 0.1 to 0.8 mg/g, preferably of from 0.2 to 0.7 mg/g and most preferably of from 0.2 to 0.6 mg/g at a temperature of 23° C. (±2° C.). 
     
     
         24 . The process according to  claim 1 , wherein the obtained surface treated filler material product has a volatile onset temperature of ≧250° C., preferably of≧260° C. and most preferably of≧270° C. 
     
     
         25 . The process according to  claim 1 , wherein the obtained surface treated filler material product has a hydrophilicity of below 8:2 volumetric ratio of water:ethanol measured at +23° C. (±2° C.) with the sedimentation method. 
     
     
         26 . Surface treated filler material product comprising
 a) at least one calcium carbonate-containing filler material, as defined in  claim 1 , having
 i) a weight median particle size d 50  value in the range from 0.1 μm to 7 μm, 
 ii) a top cut (d 98 )≦15 μm, 
 iii) a specific surface area (BET) of from 0.5 to 150 m 2 /g as measured by the BET nitrogen method, and 
 iv) a residual total moisture content of≦1 wt.-%, based on the total dry weight of the at least one calcium carbonate-containing filler material, and 
   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 at least one mono-substituted succinic acid and/or salty reaction product(s) thereof,   
       wherein the surface treated filler material product comprises the treatment layer in an amount of from 0.1 to 3 wt.-%, based on the total dry weight of the at least one calcium carbonate-containing filler material. 
     
     
         27 . Surface treated filler material product according to  claim 26 , wherein the molar ratio of the at least one mono-substituted succinic anhydride and the optional at least one mono-substituted succinic acid to the salty reaction product(s) thereof is from 99.9:0.1 to 0.1:99.9, preferably from 70:30 to 90:10. 
     
     
         28 . Surface treated filler material product according to  claim 26 , wherein the salty reaction product(s) of the mono-substituted succinic acid and/or the at least one mono-substituted succinic anhydride are one or more calcium and/or magnesium salts thereof. 
     
     
         29 . Surface treated filler material product according to  claim 26 , wherein the treatment layer further comprises at least one organic material such as polysiloxanes. 
     
     
         30 . Surface treated filler material product according to  claim 26 , wherein the surface treated filler material product comprises the treatment layer in an amount of from 0.1 to 2.5 wt.-%, preferably in an amount of from 0.1 to 2 wt.-%, more preferably in an amount of from 0.1 to 1.5 wt.-%, even more preferably in an amount of from 0.1 to 1 wt.-% and most preferably in an amount of from 0.2 to 0.8 wt.-% based on the total dry weight of the at least one calcium carbonate-containing filler material. 
     
     
         31 . A polymer composition comprising at least one polymeric resin and from 1 to 85 wt.-%, based on the total weight of the polymer composition, of a surface treated filler material product as defined in  claim 26 . 
     
     
         32 . The polymer composition according to  claim 31 , wherein the at least one polymeric resin is at least one thermoplastic polymer, preferably a thermoplastic polymer selected from the group comprising homopolymers and/or copolymers of polyolefins, polyamides, halogen-containing polymers and/or polyesters. 
     
     
         33 . The polymer composition according to  claim 31 , wherein the polymer composition is a masterbatch, preferably the masterbatch comprises the surface treated filler material product in an amount of from 50 to 85 wt.-%, preferably from 60 to 85 wt.-% and more preferably from 70 to 80 wt.-%, based on the total weight of the masterbatch. 
     
     
         34 . A fiber and/or filament and/or film and/or thread comprising a surface treated filler material product according to  claim 26  and/or a polymer composition comprising the surface treated filler material product. 
     
     
         35 . Article comprising a surface treated filler material product according to  claim 26  and/or a polymer composition comprising the surface treated filler material product and/or a fiber and/or filament and/or film and/or thread comprising the surface treated filler material product, wherein the article is selected from the group comprising 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, construction products and the like. 
     
     
         36 . Use of a mono-substituted succinic anhydride, as defined in  claim 1 , for decreasing the hydrophilicity of a calcium carbonate-containing filler material surface. 
     
     
         37 . Use of a surface-treated filler material product, as defined in  claim 26 , for initiating the crosslinking reaction in epoxide resins.