US4160812A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Multi-stage crystallization of sodium carbonate
Assignee: E A DEVELOPMENT Inc
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Filing: 1977-09-20
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Granted: 1979-07-10
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Expires: 1997-09-20
Abstract
Abstract Sodium carbonate is crystallized in multi-stage evaporative crystallizers from a pregnant liquor process solution typically obtained by dissolving calcined crude trona in water, separating insoluble impurities, and removing the majority of organic matter with activated carbon. After separation from the sodium carbonate crystals, a portion of the mother liquor usually is recycled to the crystallizers, and the remainder is purged to prevent buildup of impurities. Product quality is improved, and the amount of purged mother liquor is reduced by feeding the pregnant liquor predominantly to the initial stage crystallizers, directing the majority of the recycled mother liquor to a final stage crystallizer, recovering sodium carbonate crystals from slurries from at least the initial stages, and withdrawing purge liquor only from the slurry from the final stage crystallizer. Automatic compensation for variations in feed rates is obtained by introducing fresh feed into one end of a common crystallizer feed pipe adjacent to the first stage and directing recycled mother liquor to the other end of the feed pipe adjacent to the final stage. Preferably the stages are arranged in order of decreasing temperature so that the purge liquor is taken from the lowest temperature stage.
Inventors
- 👤 Edward H. Conroy
- 👤 Arthur Gloster
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-04 09:59
CPC Classifications
B; B01; B01D; B01D1/00; B01D1/26; B01D9/00; B01D9/0018; B01D9/0031; B01D9/0036; B01D9/0059
Claims Analysis
Total Claims: 19
Claim 1
Independent Claim
156 words
A process for preparing sodium carbonate crystals comprising: feeding a substantially saturated sodium carbonate process solution to a multiple-effect evaporative crystallizer having at least three stages including a highest temperature first stage and a lowest temperature final stage, the process solution being directed in parallel to at least the first two stages and with the majority of the process solution being fed to at least one stage ahead of the final stage; drawing a slurry of sodium carbonate crystals in mother liquor from at least one stage of the crystallizer ahead of the final stage; separating the sodium carbonate crystals in the drawn slurry from the mother liquor; recycling the mother liquor to the crystallizer, the mother liquor being directed in parallel to at least the final two stages and with the majority of the recycled mother liquor being delivered to the final stage; and withdrawing purge liquor only from the final stage of the crystallizer.
Claim 2
Dependent Claim
156 words
A process for preparing sodium carbonate crystals comprising: feeding a substantially saturated sodium carbonate process solution to a multiple-effect evaporative crystallizer having at least three stages including a highest temperature first stage and a lowest temperature final stage, the process solution being directed in parallel to at least the first two stages and with the majority of the process solution being fed to at least one stage ahead of the final stage; drawing a slurry of sodium carbonate crystals in mother liquor from at least one stage of the crystallizer ahead of the final stage; separating the sodium carbonate crystals in the drawn slurry from the mother liquor; recycling the mother liquor to the crystallizer, the mother liquor being directed in parallel to at least the final two stages and with the majority of the recycled mother liquor being delivered to the final stage; and withdrawing purge liquor only from the final stage of the crystallizer.
Claim 3
Dependent Claim
46 words
A process according to claim 1 wherein the step of drawing a slurry of sodium carbonate crystals in mother liquor from at least one stage of the crystallizer ahead of the final stage comprises drawing the slurry from at least the first stage of the crystallizer.
Claim 4
Dependent Claim
43 words
A process according to claim 1 wherein the step of drawing a slurry of sodium carbonate crystals in mother liquor from at least one stage of the crystallizer comprises drawing the slurry from all stages of the crystallizer ahead of the final stage.
Claim 5
Dependent Claim
42 words
A process according to claim 3 comprising combining the slurries drawn from each stage of the crystallizer ahead of the final stage with a slurry of carbonate crystals drawn from the final stage prior to separating the crystals from the mother liquor.
Claim 6
Dependent Claim
49 words
A process according to claim 1 wherein the step of withdrawing purge liquor comprises drawing a purge stream slurry of sodium carbonate crystals from the final stage of the crystallizer; removing the crystals from the purge stream drawn from the final stage; and purging the remaining substantially crystal-free liquor.
Claim 7
Dependent Claim
37 words
A process according to claim 5 comprising adding the sodium carbonate crystals removed from the purge stream slurry from the final stage to the slurry drawn from the at least one stage ahead of the final stage.
Claim 8
Dependent Claim
60 words
A process according to claim 1 wherein the step of feeding the sodium carbonate process solution to the crystallizer comprises directing the process solution into a single feed pipe that extends alongside the separate stages of the multiple-effect crystallizer and has successive branch pipes extending to each stage, the process solution entering the feed pipe adjacent to the first stage.
Claim 9
Dependent Claim
63 words
A process according to claim 1 wherein the step of recycling the mother liquor to the crystallizer comprises directing the recycled mother liquor into a single recycle pipe that extends alongside the separate stages of the multiple-effect crystallizer and has successive branch pipes extending to each stage of the crystallizer, the recycled mother liquor entering the feed pipe adjacent to the final stage.
Claim 10
Dependent Claim
167 words
A process for preparing sodium carbonate crystals comprising: feeding a substantially saturated sodium carbonate process solution into one end of a common feed pipe extending alongside a multiple-effect evaporator crystallizer having at least three stages including a first stage and a final stage arranged in order of decreasing temperature, said one end of the common feed pipe being adjacent to the first stage and another end of the feed pipe being adjacent to the final stage, and the feed pipe having branch lines spaced between the one end and the other end and connected to the respective stages of the crystallizer; drawing a slurry of sodium carbonate crystals in mother liquor from at least each stage of the crystallizer ahead of the final stage; combining the drawn slurries; separating the sodium carbonate crystals in the combined slurries from the mother liquor; recycling the mother liquor into the other end of the common feed pipe; and withdrawing a purge stream only from the final stage of the crystallizer.
Claim 11
Dependent Claim
167 words
A process for preparing sodium carbonate crystals comprising: feeding a substantially saturated sodium carbonate process solution into one end of a common feed pipe extending alongside a multiple-effect evaporator crystallizer having at least three stages including a first stage and a final stage arranged in order of decreasing temperature, said one end of the common feed pipe being adjacent to the first stage and another end of the feed pipe being adjacent to the final stage, and the feed pipe having branch lines spaced between the one end and the other end and connected to the respective stages of the crystallizer; drawing a slurry of sodium carbonate crystals in mother liquor from at least each stage of the crystallizer ahead of the final stage; combining the drawn slurries; separating the sodium carbonate crystals in the combined slurries from the mother liquor; recycling the mother liquor into the other end of the common feed pipe; and withdrawing a purge stream only from the final stage of the crystallizer.
Claim 12
Dependent Claim
50 words
A process according to claim 9 comprising drawing a slurry of sodium carbonate crystals from the final stage and combining the slurry drawn from the final stage with the slurries drawn from each stage ahead of the final stage prior to separating the sodium carbonate crystals from the mother liquor.
Claim 13
Dependent Claim
226 words
A process for preparing sodium carbonate crystals comprising: feeding a substantially saturated sodium carbonate process solution into one end of a common feed pipe extending alongside a multiple-effect evaporator crystallizer having at least a first stage and a final stage arranged in order of decreasing temperature, said one end of the common feed pipe being adjacent to the first stage and another end of the feed pipe being adjacent to the final stage, and the feed pipe having branch lines spaced between the one end and the other end and connected to the respective stages of the crystallizer; drawing a slurry of sodium carbonate crystals in mother liquor from at least each stage of the crystallizer ahead of the final stage; combining the drawn slurries; separating the sodium carbonate crystals in the combined slurries from the mother liquor; recycling the mother liquor into the other end of the common feed pipe; and withdrawing a purge stream only from the final stage of the crystallizer, wherein the purge stream contains sodium carbonate crystals in a mother liquor having a higher concentration of impurities than in the preceding stages; separating the sodium carbonate crystals from the impure mother liquor in the purge stream; adding the crystals separated from the purge stream to the crystals drawn from the other stages of the crystallizer; and purging the impure mother liquor.
Claim 14
Dependent Claim
226 words
A process for preparing sodium carbonate crystals comprising: feeding a substantially saturated sodium carbonate process solution into one end of a common feed pipe extending alongside a multiple-effect evaporator crystallizer having at least a first stage and a final stage arranged in order of decreasing temperature, said one end of the common feed pipe being adjacent to the first stage and another end of the feed pipe being adjacent to the final stage, and the feed pipe having branch lines spaced between the one end and the other end and connected to the respective stages of the crystallizer; drawing a slurry of sodium carbonate crystals in mother liquor from at least each stage of the crystallizer ahead of the final stage; combining the drawn slurries; separating the sodium carbonate crystals in the combined slurries from the mother liquor; recycling the mother liquor into the other end of the common feed pipe; and withdrawing a purge stream only from the final stage of the crystallizer, wherein the purge stream contains sodium carbonate crystals in a mother liquor having a higher concentration of impurities than in the preceding stages; separating the sodium carbonate crystals from the impure mother liquor in the purge stream; adding the crystals separated from the purge stream to the crystals drawn from the other stages of the crystallizer; and purging the impure mother liquor.
Claim 15
Dependent Claim
255 words
A process for preparing sodium carbonate crystals comprising: feeding a substantially saturated sodium carbonate process solution into one end of a common feed pipe extending alongside a triple-effect evaporator crystallizer having first, second, and final stages arranged in order of decreasing temperature, said one end of the common feed pipe being adjacent to the first stage and another end of the feed pipe being adjacent to the final stage, and the feed pipe having branch lines spaced between the one end and the other end and connected to the respective stages of the crystallizer, so that a majority of the sodium carbonate process solution is fed to the first and second stages; drawing a slurry stream of sodium carbonate crystals in mother liquor from each stage of the crystallizer; combining the drawn slurry streams; separating the sodium carbonate crystals in the combined slurry from the mother liquor; recycling the mother liquor into the other end of the common feed pipe, so that the majority of recycled mother liquor is directed into the final stage of the crystallizer; withdrawing a purge stream only from the final stage of the crystallizer, the purge stream containing sodium carbonate crystals in a mother liquor having a higher concentration of impurities than in the first and second stages; separating the sodium carbonate crystals from the impure mother liquor in the purge stream, adding the crystals separated from the purge stream to the drawn slurry stream prior to crystal separation from the combined slurry; and purging the separated impure mother liquor.
Claim 16
Dependent Claim
255 words
A process for preparing sodium carbonate crystals comprising: feeding a substantially saturated sodium carbonate process solution into one end of a common feed pipe extending alongside a triple-effect evaporator crystallizer having first, second, and final stages arranged in order of decreasing temperature, said one end of the common feed pipe being adjacent to the first stage and another end of the feed pipe being adjacent to the final stage, and the feed pipe having branch lines spaced between the one end and the other end and connected to the respective stages of the crystallizer, so that a majority of the sodium carbonate process solution is fed to the first and second stages; drawing a slurry stream of sodium carbonate crystals in mother liquor from each stage of the crystallizer; combining the drawn slurry streams; separating the sodium carbonate crystals in the combined slurry from the mother liquor; recycling the mother liquor into the other end of the common feed pipe, so that the majority of recycled mother liquor is directed into the final stage of the crystallizer; withdrawing a purge stream only from the final stage of the crystallizer, the purge stream containing sodium carbonate crystals in a mother liquor having a higher concentration of impurities than in the first and second stages; separating the sodium carbonate crystals from the impure mother liquor in the purge stream, adding the crystals separated from the purge stream to the drawn slurry stream prior to crystal separation from the combined slurry; and purging the separated impure mother liquor.
Claim 17
Dependent Claim
180 words
A process for preparing sodium carbonate crystals comprising: feeding a substantially saturated sodium carbonate process solution into one end of a two-ended common feed pipe extending alongside a multiple-effect evaporator crystallizer having at least three stages including a first stage and a final stage, said one end of the common feed pipe being adjacent to one of the stages of the crystallizer, and the other end of the feed pipe being adjacent to another stage of the crystallizer, and the feed pipe having branch lines equal to the number of stages spaced between the one end and the other end and each branch line being connected to a different one of the stages of the crystallizer; drawing a slurry of sodium carbonate crystals in mother liquor from each stage of the crystallizer; combining the drawn slurries; separating the sodium carbonate crystals in the combined slurries from the mother liquor; recycling the mother liquor into the other end of the common feed pipe; and withdrawing a purge stream from only one stage of the crystallizer having the highest concentration of impurities.
Claim 18
Dependent Claim
180 words
A process for preparing sodium carbonate crystals comprising: feeding a substantially saturated sodium carbonate process solution into one end of a two-ended common feed pipe extending alongside a multiple-effect evaporator crystallizer having at least three stages including a first stage and a final stage, said one end of the common feed pipe being adjacent to one of the stages of the crystallizer, and the other end of the feed pipe being adjacent to another stage of the crystallizer, and the feed pipe having branch lines equal to the number of stages spaced between the one end and the other end and each branch line being connected to a different one of the stages of the crystallizer; drawing a slurry of sodium carbonate crystals in mother liquor from each stage of the crystallizer; combining the drawn slurries; separating the sodium carbonate crystals in the combined slurries from the mother liquor; recycling the mother liquor into the other end of the common feed pipe; and withdrawing a purge stream from only one stage of the crystallizer having the highest concentration of impurities.
Claim 19
Dependent Claim
50 words
A process according to claim 11 comprising drawing a slurry of sodium carbonate crystals from the final stage and combining a slurry drawn from the final stage with the slurries drawn from each stage ahead of the final stage prior to separating the sodium carbonate crystals from the mother liquor.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1982-07-09 | 1983-01-08 | 1983-07-10 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1986-07-09 | 1987-01-08 | 1987-07-10 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1990-07-09 | 1991-01-08 | 1991-07-10 | $7700.00 | Window Closed / Lapsed |