Silica masterbatch made with emulsion and solution rubber

• US 10,344,146 B2
• Filed: 07/20/2017
• Issued: 07/09/2019
• Est. Priority Date: 03/07/2014
• Status: Active Grant

• Current Assignee: Industrias Negromex S.A. de C.V. (Grupo Kuo, S.A.B. De C.V.)
• Original Assignee: Industrias Negromex S.A. de C.V. (Grupo Kuo, S.A.B. De C.V.)
• Inventors: Hardiman, Christopher J., Fu, Xuan, Scribner, Robert J., Maldonado Valenzuela, Julian
• Primary Examiner(s): Huhn, Richard A
• Application Number:
  US15/655,615
• Publication Number:
  US 20170313857A1
• Time in Patent Office: 719 Days
• Field of Search: None
• CPC Class Codes: B01D 3/38 Steam distillation
• CPC Class Codes: C08F 2/44 Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
• CPC Class Codes: C08F 6/10 Removal of volatile materials, e.g. solvents C08F6/001, C08F6/003, C08F6/005, C08F6/006, C08F6/008, C08F6/02, C08F6/04 take precedence
• CPC Class Codes: C08J 2321/02 Latex
• CPC Class Codes: C08J 3/16 by coagulating dispersions C08J3/122 takes precedence
• CPC Class Codes: C08J 3/22 using masterbatch techniques
• CPC Class Codes: C08K 9/00 Use of pretreated ingredients
• CPC Class Codes: C08K 9/04 Ingredients treated with organic substances treated with macromolecular compounds C08K9/08
• CPC Class Codes: C08K 9/06 with silicon-containing compounds
• CPC Class Codes: C08L 21/00 Compositions of unspecified rubbers
• CPC Class Codes: C08L 21/02 Latex
• CPC Class Codes: C08L 2310/00 Masterbatches
• CPC Class Codes: C08L 2314/00 Polymer mixtures characterised by way of preparation

Abstract

The present invention provides a process for making a silica masterbatch that contains hydrophobated silica, solution-made rubber and emulsion-made rubber. Hydrophobated silica is mixed into a latex emulsion. Solution-rubber crumb in an aqueous suspension is mixed into the latex emulsion, which is coagulated, and a crumb is recovered, further homogenized, dried and baled to yield the silica masterbatch. A well-dispersed mixture of hydrophobated silica and emulsion-made rubber is added into a steam distillation step of a solution-rubber process from which a silica masterbatch is recovered. The emulsion-made rubber can be omitted to make a silica masterbatch of solution rubber and silica without emulsion rubber. The silica masterbatch has physical properties similar to those found in a comparable dry-mixed composition, but the silica masterbatch can be incorporated more easily and less expensively into tires and other rubber products than the dry-mixed composition.

Claims

1. A process for making a masterbatch of silica and solution-made rubber, comprising the steps of:

making a hydrophobated silica slurry by;

mixing silica into water in a vessel;

preparing an aqueous solution of silane; and

adding the aqueous solution of silane to the vessel to make the hydrophobated silica slurry;

adding a dispersant, a coagulant and water to a reactor, thereby forming an aqueous dispersant-coagulant mixture;

adding a mixture of solution-made rubber and organic solvent to the reactor;

adding the hydrophobated silica slurry to the reactor;

adding a process oil to the reactor to make a reactor mixture;

steam distilling the reactor mixture; and

recovering a masterbatch of silica and solution-made rubber.

2. The process of claim 1, further comprising heating the aqueous dispersant-coagulant mixture to at least 70°

C.

3. The process of claim 1, further comprising preheating the mixture of solution-made rubber and organic solvent to at least 30°

C.

4. The process of claim 1, wherein the amount of each of the dispersant and the coagulant in the aqueous dispersant-coagulant mixture is between about 50 and about 500 ppm.

5. The process of claim 1, wherein the solids level in the mixture of solution-made rubber and organic solvent is between 10 and 25 wt %.

6. The process of claim 1, further comprising adding a base to the vessel after the silica and the aqueous solution of silane are added to the vessel.

7. The process of claim 1, wherein the oil content in the masterbatch is at least 20 phr.

8. The process of claim 7, wherein extender oil is not added to the process.

9. The process of claim 1, wherein the reactor mixture contains at least about 20 phr of silica.

10. The process of claim 1, wherein the masterbatch contains less than 5 wt % extender oil, wherein the oil content in the masterbatch is at least 25 phr, and wherein the reactor mixture contains at least 30 phr of silica.

11. The process of claim 1, wherein the coagulant is calcium chloride.

12. The process of claim 1, wherein the hydrophobated silica slurry is made by (i) dissolving a trimethoxy silane coupling agent in a mixture of alcohol, a weak acid and water to provide a trimethoxy silane coupling agent solution that contains at least 75% water by weight, and (ii) mixing the trimethoxy silane coupling agent solution with silica and adding a base to increase the pH to form the hydrophobated silica, wherein the trimethoxy silane coupling agent bonds to the silica and provides a site for bonding to rubber.

13. The process of claim 1, further comprising dewatering, homogenizing, drying and baling the masterbatch.