# US 10,501,561 B2 · High pressure free radical polymerization process with flexible control of molecular weight distribution

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- Number: US 10,501,561 B2
- Document ID: US10501561B2
- Status: Granted
- Kind: B2
- Application number: 15/738,064
- Filed: 2016-06-24
- Published: 2018-06-07
- Granted: 2019-12-10
- Earliest claimed: 2015-06-25
- Assignees: Dow Global Technologies LLC
- Applicants: Dow Global Technologies LLC
- Inventors: Otto J. Berbee; Cornelis J F Hosman; Sergio E. Goncalves; Stefan Hinrichs
- Web page: https://patentgrep.com/patent/US10501561B2

## CPC

- C08F 2/34: Polymerisation in gaseous state
- A46B 11/06: connected to supply pipe {or to other external supply means (A46B11/0003 and A46B11/0006 take precedence)}
- B01J 3/02: Feed or outlet devices therefor
- B01J 3/042: {in the form of a tube}
- B01J 3/046: {Pressure-balanced vessels}
- B01J 12/00: Chemical processes in general for reacting gaseous media with gaseous media; Apparatus specially adapted therefor (B01J3/08, B01J8/00, B01J19/08 take precedence)
- B05C 17/00503: {Details of the outlet element (B05C17/00523 takes precedence; nozzles for deformable tubular containers B65D35/38)}
- B05C 17/00569: {with a pump in the hand tool}
- B05C 17/00573: {the reservoir or container being pneumatically or hydraulically pressurized (B05C17/0054, B05C17/015 take precedence)}
- C08F 2/00: Processes of polymerisation
- C08F 2/01: characterised by special features of the polymerisation apparatus used
- C08F 6/001: {Removal of residual monomers by physical means}
- C08F 10/02: Ethene
- C08F 210/02: Ethene
- B01J 2203/06: High pressure synthesis
- Y02P 20/582: Recycling of unreacted starting or intermediate materials
- C08F: MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- A46B: BRUSHES (handles not integral with brushware B25G)
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B05C: APPARATUS FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL (spraying apparatus, atomising apparatus, nozzles B05B; plant for applying liquids or other fluent materials to objects by electrostatic spraying B05B5/08)
- Y02P: CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS

## Abstract

Ethylene-based polymer, LDPE, is made in a high pressure polymerization process to comprising at least the step of polymerizing a reaction mixture comprising ethylene, using a reactor configuration comprising (A) at least two reaction zones, a first reaction zone (reaction zone 1) and an i reaction zone (reaction zone i where i>2), (B) at least two ethylene feed streams, each feed stream comprising a percentage of the total make-up ethylene fed to the polymerization process, in which a first ethylene feed stream is sent to reaction zone 1 and a second ethylene feed stream is sent to reaction zone i, and (C) a control system to control the percentage of the total make-up ethylene in the ethylene feed stream sent to reaction zone 1 and the percentage of the total make-up ethylene in the ethylene feed stream sent to reaction zone i.

## Claims

### Claim 1

A high pressure polymerization process to form an ethylene-based polymer, the process comprising at least the following step:
polymerizing a reaction mixture comprising ethylene, using a reactor configuration comprising (A) at least two reaction zones, a first reaction zone (reaction zone 1) and an i reaction zone (reaction zone i where i≥2), (B) at least two ethylene feed streams, each feed stream comprising a percentage of the total make-up ethylene fed to the polymerization process, in which a first ethylene feed stream is sent to reaction zone 1 and a second ethylene feed stream is sent to reaction zone i, and (C) a control system to control the percentage of the total make-up ethylene in the ethylene feed stream sent to reaction zone 1 and the percentage of the total make-up ethylene in the ethylene feed stream sent to reaction zone i,
wherein the reactor configuration further comprises at least one analyzer for detecting a component of a stream of the reactor configuration or determining a property of the ethylene-based polymer produced by the high pressure polymerization process,
wherein the analyzer and a valve of the control system are connected through a feedback loop.

### Claim 2 (depends on 1)

The process of claim 1, wherein the control system comprises a valve on a line through which an ethylene feed stream is delivered to a reaction zone.

### Claim 3 (depends on 2)

The process of claim 2, wherein the valve is a three-port valve.

### Claim 4 (depends on 1)

The process of claim 1, wherein the analyzer is at least one of a gas chromatograph or an infrared spectrometer.

### Claim 5 (depends on 1)

The process of claim 1, wherein the measured property of the ethylene-based polymer is at least one of a rheological property or an optical property.

### Claim 6 (depends on 5)

The process of claim 5, wherein the rheological property is at least one of melt strength and melt elasticity.

### Claim 7 (depends on 1)

The process of claim 1, wherein the percentage of make-up ethylene in each of the first and second ethylene feed streams is from 1 to 99%.

### Claim 8 (depends on 1)

The process of claim 1, wherein each of the first and second ethylene feed streams further comprises a percentage of the total of at least one CTA make-up system fed to the high pressure polymerization process.

### Claim 9 (depends on 1)

The process of claim 1, wherein Z1 is a ratio of moles of CTA to moles of ethylene in reaction zone 1 and Zi is a ratio of moles of CTA to moles of ethylene in reaction zone i, Z1 and Zi reported in units of parts per million (ppm).

### Claim 10 (depends on 9)

The process of claim 9, wherein a ratio Z1/Zi is controlled to be from 0.2 to 2.0.