Process and apparatus for forced circulation evaporative crystallization with large deposit inventory

Patent metadata

Field	Value
Publication number	US-9776104-B2
Application number	US-201214364601-A
Country	US
Kind code	B2
Filing date	Dec 14, 2012
Priority date	Dec 22, 2011
Publication date	Oct 3, 2017
Grant date	Oct 3, 2017

Abstract

Disclosed are processes and apparatuses for producing a crystalline product. The processes and apparatuses may extend the operational time of an evaporative crystallizer by providing an internal volume or large deposit inventory for fouling deposits to reside without impacting the unit operation.

First claim

What is claimed is:

1. An apparatus comprising:
an evaporative crystallizer, wherein the evaporative crystallizer includes a deposit accumulation volume located at the bottom of the evaporative crystallizer;
a recirculation system including:
a first inlet for supplying a first flow of a feedstock comprising a solvent and a solute to the evaporative crystallizer to produce a slurry;
an outlet for supplying the slurry from the evaporative crystallizer to the recirculation system;
a heat exchanger; and
a recirculation pump;

a second inlet for supplying a portion of the slurry to the evaporative crystallizer; and
means for extracting the portion of the slurry from the recirculation system and introducing it into the evaporative crystallizer through the second inlet,
wherein the evaporative crystallizer has a substantially vertical sidewall;
wherein the outlet is located above the deposit accumulation volume;
wherein the first inlet enters the evaporative crystallizer at a position offset from the lowest point of the evaporative crystallizer and comprises a particle exit positioned above the outlet; and
wherein the second inlet is located above the deposit accumulation volume and oriented at an angle of less than 85 degrees from the substantially vertical sidewall.

2. The apparatus of claim 1 , wherein the second inlet is of a diameter sufficient to permit a flow of between about 0.1 percent and about 20 percent of the flow permitted by the first inlet.

3. The apparatus of claim 1 , wherein the evaporative crystallizer includes a cone portion allowing the formation of a liquid-vapor interface.

4. The apparatus of claim 1 , further comprising a recovery system for recovering a crystalline product from a second portion of the slurry.

5. The apparatus of claim 1 , wherein the deposit accumulation volume has a volume of between about 2 percent and about 50 percent of the volume of the evaporative crystallizer.

6. A process comprising:
providing a feedstock comprising a solvent and a solute to a recirculation system including a first inlet; an outlet; a heat exchanger; and a recirculation pump;
heating the feedstock with the heat exchanger to provide a heated feedstock;
supplying the heated feedstock to an evaporative crystallizer through the first inlet to produce a slurry, wherein the evaporative crystallizer includes a deposit accumulation volume, wherein the evaporative crystallizer has a substantially vertical sidewall, wherein the outlet is located above the deposit accumulation volume, and wherein the first inlet enters the evaporative crystallizer at a position offset from the lowest point of the evaporative crystallizer and comprises a particle exit positioned above the outlet;
returning the slurry to the recirculation system through the outlet;
extracting a portion of the slurry from the recirculation loop; and
supplying a first portion of the extracted slurry to the evaporative crystallizer through a second inlet, wherein the second inlet is located above the deposit accumulation volume and oriented at an angle of less than 85 degrees from the substantially vertical sidewall.

7. The process claim 6 , further comprising accumulating fouling deposits in the deposit accumulation volume.

8. The process of claim 6 , wherein the first portion of the extracted slurry is introduced into the crystallizer at a direction sufficient to sweep crystalline product away from the deposit accumulation volume.

9. The process of claim 6 , further comprising supplying a second portion of the extracted slurry to a cooling crystallizer for cooling the second portion of the extracted slurry.

10. The process of claim 9 , further comprising recovering crystalline product.

11. A process comprising:
providing a feedstock comprising a solvent and a solute to a recirculation system including a first inlet; an outlet; a heat exchanger; and a recirculation pump;
heating the feedstock with the heat exchanger to provide a heated feedstock;
supplying the heated feedstock to evaporative crystallizer through the first inlet to produce a slurry, wherein the evaporative crystallizer includes a deposit accumulation volume, and wherein fouling deposits accumulate in the deposit accumulation volume, wherein the evaporative crystallizer has a substantially vertical sidewall, wherein the outlet is located above the deposit accumulation volume, and wherein the first inlet enters the evaporative crystallizer at a position offset from the lowest point of the evaporative crystallizer and comprises a particle exit positioned above the outlet;
returning the slurry to the recirculation system through the outlet;
extracting a portion of the slurry from the recirculation loop;
supplying a first portion of the extracted slurry to the evaporative crystallizer through a second inlet, wherein the second inlet is located above the deposit accumulation volume and oriented at an angle of less than 85 degrees from the substantially vertical sidewall, and wherein the first portion of the extracted slurry sweeps crystalline product away from the deposit accumulation volume; and

recovering crystalline product in a recovery system.

Assignees

• Dow Global Technologies Llc

Inventors

• Frank Timothy C
• Moore J W
• Larsen Paul A
• Patil Pramod D
• Whittingslow Robert M
• Gillis Paul A

Classifications

• B01D9/00 Primary

  Crystallisation (crystallisation directly from the vapour phase B01D7/02; making single crystals C30B {; crystallisation as part of the Bayer process also classified in C01F7/14}) · CPC title

• B01D9/0031 Primary

  by heating (B01D9/0022, B01D9/0027 take precedence) · CPC title

• B01D1/24

  to obtain dry solids · CPC title

• B01D1/007

  the liquid feed being split up in at least two streams before entering the evaporator · CPC title