IP Library Granted Patent US 9,403,923
Granted Patent B2
US 9,403,923 · App. 12/516,152 · Granted Aug 2, 2016

Process for preparing synthetic polyethylene waxes having a high crystallinity and low viscosity

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 9,403,923
App. No.
12/516,152
Granted
Aug 2, 2016
Kind
B2
Abstract

A process for preparing a polyethylene wax by polymerization of ethylene in the presence of a Ziegler-Natta catalyst system composed of titanium tetrachloride and dialkylaluminium halide, wherein the polymerization temperature is in the range from 170 to 200° C., the polymerization is carried out essentially in the absence of solvents and the Al/Ti molar ratio is less than 1.6, gives a wax having the following property profile: dropping point of from 115 to 125° C.; penetration number of not more than 1 mm·10 −1 ; viscosity at 150° C. of less than 60 mPas; density of from 0.945 to 0.960 g/cm 3 at 23° C.; molar mass of less than 1500 g/mol and crystallinity of more than 70%.

Claims (71)

1. A process for preparing a polyethylene wax, the wax having a penetration number in accordance with DIN 51579 of not more than 1 mm·10 −1 , by polymerizing of ethylene in the presence of a Ziegler-Natta catalyst system composed of titanium tetrachloride and a dialkylaluminium halide, wherein

the polymerization temperature is in the range from 170 to 200° C.,

the polymerization is carried out essentially in the absence of solvents,

the dialkylaluminium halide is added to the process at a rate of 1.4 kg/hour,

and the Al/Ti molar ratio is less than 1.6.

2. The process according to claim 1 , wherein the polymerization temperature is in the range from 175 to 195° C.

3. The process according to claim 1 , wherein the Al/Ti molar ratio is less than 1.5.

4. A polyethylene wax prepared according to the process of claim 1 that has the following properties:

dropping point in accordance with DIN 51801 in the range from 115 to 125° C.;

penetration number in accordance with DIN 51579 of not more than 1 mm·10 −1 ;

viscosity in accordance with DIN 52007/1 at 150° C. of less than 60 mPas;

density of from 0.945 to 0.960 g/cm 3 at 23° C.;

molar mass in accordance with ASTM D 6474-99 of less than 1500 g/mol;

crystallinity in accordance with ISO 11357-3 of more than 70% and

a polydispersity of between 3.4 and 4.2.

5. The polyethylene wax according to claim 4 having a viscosity in accordance with DIN 52007/1 at 150° C. of less than 50 mPas.

6. The polyethylene wax according to claim 4 , wherein the density is from 0.950 to 0.960 g/cm 3 at 23° C.

7. The polyethylene wax according to claim 4 , wherein the molar mass is less than 1400 g/mol.

8. An additive used for printing inks, surface coating compositions, powder coatings or hot melts, the additive comprising a polyethylene wax that has the following properties:

dropping point in accordance with DIN 51801 in the range from 115 to 125° C.;

penetration number in accordance with DIN 51579 of not more than 1 mm·10 −1 ;

viscosity in accordance with DIN 52007/1 at 150° C. of less than 60 mPas;

density of from 0.945 to 0.960 g/cm 3 at 23° C.;

molar mass in accordance with ASTM D 6474-99 of less than 1500 g/mol;

crystallinity in accordance with ISO 11357-3 of more than 70% and

a polydispersity of between 3.4 and 4.2.

9. A nucleating agent for expandable polystyrene, a lubricant in PVC and a starting material for producing wax oxidate, all of which comprise a polyethylene wax that has the following properties:

dropping point in accordance with DIN 51801 in the range from 115 to 125° C.;

penetration number in accordance with DIN 51579 of not more than 1 mm·10 −1 ;

viscosity in accordance with DIN 52007/1 at 150° C. of less than 60 mPas;

density of from 0.945 to 0.960 g/cm 3 at 23° C.;

molar mass in accordance with ASTM D 6474-99 of less than 1500 g/mol;

crystallinity in accordance with ISO 11357-3 of more than 70% and

a polydispersity of between 3.4 and 4.2.

10. The process of claim 1 , wherein the dialkylaluminium halide is diethylaluminium bromide.

11. The process of claim 1 , wherein the dialkylaluminium halide is diethylaluminium chloride.

12. The polyethylene wax according to claim 4 , having a viscosity in accordance with DIN 52007/1 at 150° C. of less than 45 mPas.

13. The polyethylene wax according to claim 4 having a throughput micronization of 160 kg/h.

14. A printing ink containing a polyethylene wax that has the following properties:

dropping point in accordance with DIN 51801 in the range from 115 to 125° C.;

penetration number in accordance with DIN 51579 of not more than 1 mm·10 −1 ;

viscosity in accordance with DIN 52007/1 at 150° C. of less than 60 mPas;

density of from 0.945 to 0.960 g/cm 3 at 23° C.;

molar mass in accordance with ASTM D 6474-99 of less than 1500 g/mol;

crystallinity in accordance with ISO 11357-3 of more than 70% and

a polydispersity of between 3.4 and 4.2.

15. The printing ink of claim 14 , comprising 1% by weight of the polyethylene wax according to claim 4 , and wherein the printing ink has an abrasion protection of 1200 strokes as determined using a Prüfbau Quartant abrasion tester.

16. A surface coating composition containing a polyethylene wax that has the following properties:

dropping point in accordance with DIN 51801 in the range from 115 to 125° C.;

penetration number in accordance with DIN 51579 of not more than 1 mm·10 −1 ;

viscosity in accordance with DIN 52007/1 at 150° C. of less than 60 mPas;

density of from 0.945 to 0.960 g/cm 3 at 23° C.;

molar mass in accordance with ASTM D 6474-99 of less than 1500 g/mol;

crystallinity in accordance with ISO 11357-3 of more than 70% and

a polydispersity of between 3.4 and 4.2.

17. A powder coating containing a polyethylene wax that has the following properties:

dropping point in accordance with DIN 51801 in the range from 115 to 125° C.;

penetration number in accordance with DIN 51579 of not more than 1 mm·10 −1 ;

viscosity in accordance with DIN 52007/1 at 150° C. of less than 60 mPas;

density of from 0.945 to 0.960 g/cm 3 at 23° C.;

molar mass in accordance with ASTM D 6474-99 of less than 1500 g/mol;

crystallinity in accordance with ISO 11357-3 of more than 70% and

a polydispersity of between 3.4 and 4.2.

18. A hot melt containing a polyethylene wax that has the following properties:

dropping point in accordance with DIN 51801 in the range from 115 to 125° C.;

penetration number in accordance with DIN 51579 of not more than 1 mm·10 −1 ;

viscosity in accordance with DIN 52007/1 at 150° C. of less than 60 mPas;

density of from 0.945 to 0.960 g/cm 3 at 23° C.;

molar mass in accordance with ASTM D 6474-99 of less than 1500 g/mol;

crystallinity in accordance with ISO 11357-3 of more than 70% and

a polydispersity of between 3.4 and 4.2.

Assignments (3)
SECURITY INTEREST Recorded Jan 12, 2026
From: SOLSTICE ADVANCED MATERIALS US, INC.
To: JPMORGAN CHASE BANK, N.A., AS ADMINISTRATIVE AGENT
Reel/Frame 074569/0260 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Mar 30, 2012
From: EVONIK DEGUSSA GMBH
To: HONEYWELL INTERNATIONAL INC.
Reel/Frame 027962/0681 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 2, 2009
From: SCHRENK, VOLKER; SPITZER, UDO; ZAGEFKA, HANS-DIETER
To: EVONIK DEGUSSA GMBH
Reel/Frame 022762/0914 →