IP Library Granted Patent US 10,544,074
Granted Patent B2
US 10,544,074 · App. 15/503,186 · Granted Jan 28, 2020

Low-viscosity solutions of alkaline-earth metal alkoxides in aprotic solvents, method for the production of same and use for the production of Ziegler-Natta catalysts

Inventors: Ulrich Wietelmann (Friedrichsdorf, DE); Ute Emmel (Frankfurt am Main, DE); Armin Stoll (Hirschberg an der Bergstraße, DE); Florian Kiefer (Goslar, DE)
Assignee: Albemarle Germany GmbH
C07C31/30C07C29/70
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Quick Facts
Patent No.
US 10,544,074
App. No.
15/503,186
Granted
Jan 28, 2020
Kind
B2
Abstract

One or more concentrated low-viscosity solutions of alkaline earth alkoxide compounds M(OCH 2 R 6 ) 2-a-b (OR 7 ) a [O(CHR 8 ) n OR 9 ] b in mixture with a metal alkyl compound M(R 10 R 11 ) in an aprotic solvent and related methods are disclosed herein.

Claims (19)

1. A solution of alkaline earth alkoxide compounds M(OCH 2 R 6 ) 2-a-b (OR 7 ) a [O(CHR) n OR 9 ] b in mixture with an alkaline earth metal alkyl compound M(R 10 R 11 ) with an alkaline earth metal concentration in the range of 0.2 to 1.8 mmol/g in an aprotic solvent, wherein

M is an alkaline earth metal selected from the group consisting of Mg, Ca, Ba, and Sr;

OCH 2 R 6 is an alkoxide radical consisting of at least 3 and at most 40 carbon atoms with a branch in position 2 relative to the O function;

R 7 is an alkyl radical with 2-15 carbon atoms, which is either linear or has a branch in ≥position 3 relative to the O function;

R 8 is an alkyl radical with 1 to 6 carbon atoms, which is either linear or has a branch at ≥position 3 (relative to the O function;

R 9 is an alkyl radical with 2 to 15 carbon atoms, which is either linear or has a branch;

R 10 and R 11 are any alkyl radicals with 1 to 15 carbon atoms;

n is an integer from 1 to 4;

a+b≤2 wherein a and b each have a value of 0 to 2; and

the solution has a molar ratio of M(OCH 2 R 6 ) 2-a-b (OR 7 ) a [O(CHR 8 ) n OR 9 ] b to M(R 10 R 11 ) that is in the range of from 99.5:0.5 to 60:40.

2. The solution according to claim 1 , characterized in that the alkaline earth metal concentration is in the range of 0.4 to 1.6 mmol/g.

3. The solution according to claim 1 , characterized in that the solution, at the alkaline earth metal concentration of ≥1 mmol/g to ≤1.6 mmol/g, has a viscosity, measured at room temperature, of ≤300 cP.

4. The solution according to claim 1 , characterized in that the molar ratio of M(OCH 2 R) 2-a-b (OR 7 ) n [O(CHR 8 ) n OR 9 ] b to M(R 10 R 11 ) is in the range of from 99:1 to 70:30.

5. The solution according to claim 1 , characterized in that it contains from 0.1 to 30 mol % M(R 10 R 11 ), determined by direct titration with sec-butanol and biquinoline as the indicator and based on the total alkaline earth metal M in solution and the solution non-pyrophoric according to one selected from the group consisting of United Nations test N.2, United Nations test N.3, and both United Nations test N.2 and United Nations test N.3.

6. The solution according to claim 1 , characterized in that the alkaline earth metal concentration is in the range of 0.7 to 1.4 mmol/g.

7. The solution according to claim 1 , characterized in that the solution, at the alkaline earth metal concentration of >1 mmol/g to <1.6 mmol/g, has a viscosity, measured at room temperature, of <100 cP.

8. The solution according to claim 1 , characterized in that the molar ratio of M(OCH 2 R 6 ) 2-a-b (OR 7 ) a [O(CHR 8 ) n OR 9 ] b to M(R 10 R 11 ) is in the range of from 95:5 to 80:20.

9. A method for synthesis of alkaline earth alkoxide compounds M(OCH 2 R 6 ) 2-a-b (OR 7 ) a [O(CHR 8 ) n OR 9 ] b in mixture with a metal alkyl compound M(R 10 R 11 ) according to claim 1 , the method comprising:

mixing a solution of the metal alkyl compound M(R 10 R 11 ) in an aprotic solvent with one or more alcohols selected from the group of HOCH 2 R 6 , HOR 7 , HO(CHR 8 ) n OR 9 , and any mixture thereof, wherein half of the molar ratio of the total number of moles of all alcohols to the metal alkyl compound is from 99.5:0.5 to 60:40.

Assignments (4)
CORRECTIVE ASSIGNMENT TO CORRECT THE TYPOGRAPHICAL ERROR IN THE SPELLING OF ONE OF THE INVENTORS ARMIN STOLL PREVIOUSLY RECORDED ON REEL 044888 FRAME 0904. ASSIGNOR(S) HEREBY CONFIRMS THE ASSIGNMENT. Recorded Mar 3, 2020
From: WIETELMANN, ULRICH; EMMEL, UTE; STOLL, ARMIN; KIEFER, FLORIAN
To: ROCKWOOD LITHIUM GMBH
Reel/Frame 052104/0924 →
CHANGE OF NAME Recorded Mar 6, 2018
From: ROCKWOOD LITHIUM GMBH
To: ALBEMARLE GERMANY GMBH
Reel/Frame 045502/0922 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Dec 18, 2017
From: WIETELMANN, ULRICH; EMMEL, UTE; STOLL, AMIN; KIEFER, FLORIAN
To: ROCKWOOD LITHIUM GMBH
Reel/Frame 044888/0904 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 22, 2017
From: WIETELMANN, ULRICH; EMMEL, UTE; STOLL, AMIN; KIEFER, FLORIAN
To: ROCKWOOD LITHIUM GMBH
Reel/Frame 044794/0873 →
Priority Claims (3)
DE 10 2014 215 919 · Aug 12, 2014 · national
DE 10 2014 216 067 · Aug 13, 2014 · national
DE 10 2014 224 139 · Nov 26, 2014 · national
Continuity (1)
Related Publication 20170247305A1 · Aug 31, 2017