IP Library Granted Patent US 9,758,646
Granted Patent B2
US 9,758,646 · App. 14/355,241 · Granted Sep 12, 2017

NdBR wet masterbatch

View Patent ↗
Loading inventors, assignments & file history…
Monitor This Case
Get email alerts when status or documents change.
Order Certified Copies
Most orders are placed with the USPTO same day — all within 24 business hours.
Order via The Patent Place →
Pre-filled with this patent's details
Quick Facts
Patent No.
US 9,758,646
App. No.
14/355,241
Granted
Sep 12, 2017
Kind
B2
Abstract

The invention relates to an NdBR wet masterbatch comprising —neodymium-catalyzed polybutadienes having a high proportion of cis-1,4 units of >95% and a low proportion of 1,2-vinyl content of <1%, with narrow polydispersity of less than 3, with a Mooney viscosity (ML 1+4 100° C.) between 30 and 90 MU, with a high linearity index (ratio of solution viscosity to Mooney viscosity) of 3 to 10 m Pas/MU and with a Mooney relaxation after 30 seconds of 2 to 12%, the latter being prepared by means of solution polymerization, —at least one carbon black, the carbon black having an iodine absorption number (ION) between 85 and 210 mg/g, measured to ASTM D1510-1304, and an oil absorption number (OAN) between 75 and 150 ml/100 g, measured to ASTM D2414, and —an oil.

Claims (15)

1. A process for producing a wet neodymium-catalysed polybutadiene masterbatch, the process comprising:

a) suspending a carbon black having:

an iodine absorption number (ION) of 95-210 mg/g, measured to ASTM D1510-1304, and an oil absorption number (OAN) of 80 and 140 ml/100 g, measured to ASTM D2414 in water, hexane or a water/hexane mixture to form a liquid suspension comprising 10 to 30 wt % carbon black;

b) mixing a neodymium-catalysed polybutadiene, prepared by a solution polymerization, and having >95% of cis-1,4 units, <1% of 1,2-vinyl content, a narrow polydispersity of less than 3, a Mooney viscosity (ML 1+4 100° C.) between 30 and 90 MU, a high linearity index (ratio of solution viscosity to Mooney viscosity) of 3 to 10 mPas/MU, and a Mooney relaxation after 30 seconds of 2 to 12% with:

the liquid suspension of carbon black,

a hydrogenated naphthenic oil having less than 10 ppm of polycyclic aromatics, less than 1 ppm of alpha-benzopyrene, measured by the Grimmer test, a glass transition temperature (Tg) between −80° C. and −40° C., and a level of extractables, extracted with DMSO by the IP 346 method, of less than 3% by weight, and

a stabilizer,

thereby forming a resultant solution; and

c) removing suspension liquid from the resultant solution by a stripping process to provide a wet neodymium-catalysed polybutadiene masterbatch comprising 100 phr of the neodymium-catalysed polybutadienes, 50 to 70 phr of the carbon black, 3 to 10 phr of the oil, and 0.2 to 2 phr of the stabilizer.

2. The process according to claim 1 , wherein the oil is added prior to, during, or after the mixing of the liquid suspension of carbon black with the polybutadiene.

3. The process according to claim 1 , wherein the polybutadiene, the liquid suspension of the carbon black, the oil, and the stabilizer are mixed in any sequence.

4. The process according to claim 2 , wherein the polybutadiene is mixed with the liquid suspension of the carbon black until homogeneity, and prior to mixing with the oil and the stabilizer.

5. The process according to claim 4 , wherein the neodymium-catalysed polybutadiene is prepared by solution polymerization in a polymerization solvent, and after polymerization is dissolved in the polymerization solvent, and the neodymium-catalysed polybutadiene dissolved in the polymerization solvent is mixed with the liquid suspension of the carbon black.

6. The process according to claim 5 , wherein:

the carbon black has an iodine absorption number 100 to 160 mg/g, and an oil absorption number of 85 to 120 ml/g.

Assignments (2)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Aug 19, 2016
From: LANXESS DEUTSCHLAND GMBH
To: ARLANXEO DEUTSCHLAND GMBH
Reel/Frame 039753/0760 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 27, 2015
From: KLOPPENBURG, HEIKE; LUCASSEN, ALEX; HARDY, DAVID; GROSS, THOMAS; DOUGLAS, JUDY ELIZABETH
To: LANXESS DEUTSCHLAND GMBH
Reel/Frame 035497/0382 →