# US 2018/0022870 A1 · Method and device for producing polyamides, with optimized flow management

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- Number: US 2018/0022870 A1
- Document ID: US20180022870A1
- Status: Published application
- Kind: A1
- Application number: 15/547,950
- Filed: 2016-02-02
- Published: 2018-01-25
- Earliest claimed: 2015-02-04
- Assignees: Uhde Inventa-Fischer GmbH; thyssenkrupp AG
- Applicants: Uhde Inventa-Fischer GmbH; thyssenkrupp AG
- Inventors: Bernd KÖNIGSMANN
- Web page: https://patentgrep.com/patent/US20180022870A1

## CPC

- C08G 69/16: Preparatory processes
- B01D 11/0253: {Fluidised bed of solid materials}
- B01D 11/0284: {Multistage extraction}
- B01J 2/02: by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops
- B01J 19/06: Solidifying liquids (making microcapsules B01J13/02)
- B29B 9/065: {under-water, e.g. underwater pelletizers}
- C08G 69/46: Post-polymerisation treatment
- C08G 69/48: Polymers modified by chemical after-treatment
- B01D 2011/002: {Counter-current extraction}
- B29B 9/12: characterised by structure or composition
- C08G: MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- B01D: SEPARATION (separating solids from solids by wet methods B03B, B03D; by pneumatic jigs or tables B03B; by other dry methods B07; magnetic or electrostatic separation of solid materials from solid materials or fluids, separation by high-voltage electric fields B03C; centrifuges, vortex apparatus B04; presses per se for squeezing-out liquid from liquid-containing material B30B9/02; treatment of water C02F, e.g. softening by ion-exchange C02F1/42; {arrangements of air intake cleaners in gas turbine plants F02C7/05} ; arrangements or mounting of filters in air-conditioning, air-humidification or ventilation F24F13/28)
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B29B: PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS

## Abstract

A process for producing polyamides makes flow guidance within the process more efficient. In some respects, the process is based on the polymerization of lactam to a polyamide-containing polymer melt, the subsequent granulation of the polymer melt to polyamide granules using granulation liquid, and the subsequent extraction of monomeric and oligomeric constituents from the PA granules in an extraction column. In some examples, a temperature of the granulation liquid before being fed into an extraction liquid stream is lower than a temperature of the extraction liquid stream before the granulation liquid is fed into the extraction liquid stream. The invention relates also to a device for carrying out processes such as this one.

## Claims

### Claim at position 1

-15. (canceled)

### Claim 16

A process for producing polyamides with optimized flow guidance, the process comprising:
polymerizing lactam to a polyamide-containing polymer melt;
granulating the polyamide-containing polymer melt to PA granules using granulation liquid;
extracting monomeric and oligomeric constituents from the PA granules in an extraction column, wherein the PA granules are guided countercurrently to an extraction liquid stream; and
feeding at least a portion of the granulation liquid into the extraction liquid stream at at least one infeed point of the extraction column to adjust a temperature and a lactam concentration of the extraction liquid stream, wherein the at least one infeed point comprises ten infeed points at most, wherein if the at least one infeed point comprises more than one infeed point the infeed points are disposed at different heights of the extraction column.

### Claim 17 (depends on 16)

The process of claim 16 wherein a temperature of the granulation liquid before being fed into the extraction liquid stream is lower than the temperature of the extraction liquid stream before the granulation liquid is fed in.

### Claim 18 (depends on 17)

The process of claim 17 wherein the temperature of the granulation liquid before being fed into the extraction liquid stream is from 10° C. to 50° C.

### Claim 19 (depends on 17)

The process of claim 17 wherein the temperature of the granulation liquid before being fed into the extraction liquid stream is from 15° C. to 40° C.

### Claim 20 (depends on 16)

The process of claim 16 wherein a content of lactam and oligomeric constituents in the granulation liquid before the granulation liquid is fed into the extraction liquid stream is lower than a content of at least one of lactam or oligomeric constituents in the extraction liquid stream before the granulation liquid is fed in, wherein the content of the at least one of the lactam or oligomeric constituents in the granulation liquid before the granulation liquid is fed into the extraction liquid stream is from 0.1% by weight to 5.0% by weight.

### Claim 21 (depends on 16)

The process of claim 16 wherein the at least one infeed point of the extraction column comprises between one and four infeed points.

### Claim 22 (depends on 16)

The process of claim 16 further comprising measuring and adjusting an amount of granulation liquid fed into the extraction liquid stream.

### Claim 23 (depends on 16)

The process of claim 16 wherein the granulation liquid contains at least one of lactam or oligomeric constituents, the process further comprising:
providing the granulation liquid by way of a granulation liquid circuit;
feeding demineralized water into the granulation liquid circuit;
measuring a content of the at least one of lactam or oligomeric constituents in the granulation liquid; and
adjusting an amount of the demineralized water fed into the granulation liquid circuit based on the measured content of the at least one of lactam or oligomeric constituents in the granulation liquid so as to keep the content of the at least one of lactam or oligomeric constituents in the granulation liquid within a range.

### Claim 24 (depends on 16)

The process of claim 16 further comprising pre-extracting in a pre-extraction column after the granulating and before the extracting, wherein after the extracting the extraction liquid stream is discharged from the extraction column and fed to the pre-extraction column and guided countercurrently to the PA granules.

### Claim 25 (depends on 16)

The process of claim 16 further comprising discharging the extraction liquid stream from the extraction column after the extraction.

### Claim 26 (depends on 25)

The process of claim 25 wherein no additional granulation liquid from another source is fed to a collecting tank for evaporation.

### Claim 27

A device for producing polyamides with optimized flow guidance, the device comprising:
a polymerization system;
a granulation system; and
an extraction column that comprises an inlet suitable for PA granules disposed at a top of the extraction column, an outlet suitable for the PA granules disposed at a bottom of the extraction column, an inlet suitable for an extraction liquid disposed at the bottom of the extraction column, an outlet suitable for the extraction liquid disposed at the top of the extraction column, and at least one infeed point suitable for a granulation liquid, wherein the at least one infeed point comprises ten infeed points at most, wherein if the at least one infeed point comprises more than one infeed point the infeed points are disposed at different heights of the extraction column,
wherein the granulation system and the at least one infeed point are connected via a line through which a portion of the granulation liquid used in the granulation system is transferable to the at least one infeed point.

### Claim 28 (depends on 27)

The device of claim 27 further comprising a collecting tank for evaporation, wherein the collecting tank is connected to the extraction column such that an extraction liquid stream discharged from the extraction column is fed to the collecting tank for evaporation, wherein the collecting tank is not connected to the granulation system such that the granulation liquid can be fed directly to the collecting tank for evaporation.

### Claim 29 (depends on 27)

The device of claim 27 wherein the granulation system is connected to a granulation liquid circuit that comprises a granulation liquid tank.

### Claim 30 (depends on 29)

The device of claim 29 wherein the granulation liquid tank includes an overflow valve.

### Claim 31 (depends on 27)

The device of claim 27 wherein the at least one infeed point comprises between one infeed point and four infeed points for the granulation liquid.

### Claim 32 (depends on 27)

The device of claim 27 further comprising a pre-extraction vessel.