# US 5,710,326 A · Catalyst regeneration process

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- Number: US 5,710,326 A
- Document ID: US5710326A
- Status: Granted
- Kind: A
- Application number: 07/695,165
- Filed: 1991-05-03
- Granted: 1998-01-20
- Earliest claimed: 1991-05-03
- Assignees: Exxon Chemical Patents Inc.
- Inventors: Carl R. Beck
- Web page: https://patentgrep.com/patent/US5710326A

## CPC

- C07C 51/14: on a carbon-to-carbon unsaturated bond in organic compounds
- B01J 27/32: of catalysts comprising compounds of halogens
- Y02P 20/584: Recycling of catalysts
- C07C: ACYCLIC OR CARBOCYCLIC COMPOUNDS
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- Y02P: CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS

## Abstract

A process for controlling the regeneration of boron trifluoride catalyst complexes in the production of carboxylic acids and other products using boron trifluoride hydrates as a catalyst. Catalyst strength is determined by measuring the electrical conductivity of the catalyst recovered from hydrolysis. If the conductivity is greater than a predetermined value, the hydrolysis water rate is reduced and if the conductivity is leas than a predetermined value, the hydrolysis water rate is increased. Conductivity is determined by a toroidal conductivity sensor and a control valve responsive to operation of the conductivity sensor serves to increase or decrease the flow rate accordingly.

## Claims

### Claim 1

In a continuous process for the production of aliphatic carboxylic acids by the reaction of an olefin and carbon monoxide in the presence of a catalyst comprising a BF.sub.3 hydrate composition and the regeneration of said catalyst by control of the water content of said regenerated catalyst exiting hydrolysis, a method of determining catalyst strength as a function of the water content in the catalyst comprising the steps of:
(a) introducing water for hydrolysis of the reaction product of the olefin and carbon monoxide and for catalyst strength control;
(b) withdrawing the BF.sub.3 hydrate composition catalyst resulting from hydrolysis;
(c) measuring the electrical conductivity of the catalyst complex exiting hydrolysis;
(d) continuously comparing the electrical conductivity measured in step with a predetermined value thereof;
(e) increasing the rate of introduction of water per step (a) in the event the electrical conductivity measured in step (c) is less than the predetermined value; and
(f) decreasing the rate of introduction of water per step (a) in the event the electrical conductivity measured in step (c) is greater than the predetermined value.

### Claim 2 (depends on 1)

A process as set forth in claim 1 wherein said BF.sub.3 hydrate composition comprises H.sub.3 PO.sub.4 as a co-Catalyst in a molar ratio with the BF.sub.3 of up to one to one.

### Claim 3 (depends on 1)

A process as set forth in claim 1 wherein said BF.sub.3 hydrate composition comprises H.sub.2 SO.sub.4 as a co-catalyst in a molar ratio with the BF.sub.3 of up to one to one.

### Claim 4 (depends on 1)

A process as set forth in claim 1 including the step of:
(g) reintroducing the BF.sub.3 hydrate composition catalyst obtained in step (c) for reaction with the olefin and carbon monoxide.

### Claim 5 (depends on 1)

A process as set forth in claim 1 wherein step (b) is performed by a toroidal conductivity sensor.

### Claim 6

A process for the introduction of aliphatic carboxylic acid comprising the steps of:
(i) reacting an olefin and carbon monoxide in the presence of a catalyst comprising a BF.sub.3 hydrate composition;
(j) introducing water to thereby perform hydrolysis of the reaction product resulting from step (i);
(k) recycling the BF.sub.3 hydrate composition catalyst resulting from step (j), reintroducing it for reaction with the olefin and carbon monoxide;
(l) measuring the electrical conductivity of the hydrate composition catalyst following step (j);
(m) continuously comparing the electrical conductivity measured in step with predetermined value thereof;
(n) increasing the introduction of water per step (j) in the event the electrical conductivity measured in step (l) is less than the predetermined value; and
(o) decreasing the introduction of water per step (j) in the event the electrical conductivity measured in step (l) is greater than the predetermined value.