US2751280A - Process for effecting double conversion between two solutions of ionogenic substances by using ion exchangers - Google Patents

Process for effecting double conversion between two solutions of ionogenic substances by using ion exchangers Download PDF

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Publication number
US2751280A
US2751280A US331473A US33147353A US2751280A US 2751280 A US2751280 A US 2751280A US 331473 A US331473 A US 331473A US 33147353 A US33147353 A US 33147353A US 2751280 A US2751280 A US 2751280A
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columns
group
column
solution
loaded
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US331473A
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English (en)
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Hasselder Willem
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Stamicarbon BV
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Stamicarbon BV
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J49/00—Regeneration or reactivation of ion-exchangers; Apparatus therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J47/00—Ion-exchange processes in general; Apparatus therefor
    • B01J47/02—Column or bed processes
    • B01J47/026—Column or bed processes using columns or beds of different ion exchange materials in series

Definitions

  • the present invention relates to a process of converting substanceswhich are ionized in solution (i. e., bases, acids, salts) with the help of ion exchangers. and, more particularly, the invention pertains to a method of loading and regenerating, the ion exchanger used in this conversion process.
  • the necessary alternating loading and regeneration of the ion exchanger is effected by periodically disconnecting the first column of one set and;'after washing the column to remove the solution leftin the-free spaces'between the particles of ion exchanger, connectingsame: to the discharge side ofthe other set of columns.
  • the operatingcon ditions selected are such that, asra result of therloading,a virtually pure BrAz solution isobtained, the regeneration operation with a BiAi. solution produces a BaAr solution containing-a .considerable amount of BiAr. Likewise, if the regeneration-iscarried out insucha way as to result in the formation of. avirtuallypure B2A1- solution, the loading operation produces a solution which contains, in addition tothe desired BrAz, an appreciable amount: of B2A2.
  • Objects g, Y Accordingly, the principal object of the presentinvenztion: is-the provision of anovel improvement in effecting doubleconversion between solutions of ionogenic substances. 1
  • A- more specific 'object-of'theinvention is the provision of new procedures forloading and regenerating columns filled withflion eucharvgerfor the purpose of efiectin'g doubleconversions, said procedures being. free of the dis? advantages-noted above.
  • the objects outlined above are realized according to the present invention by a process involving the steps of providing a first group of columns connected together in series to be loaded and a second group of columns connected together in series to be regenerated, passing the loading solution through the first group of columns to load the ion exchanger therein, and withdrawing from the last column of this first group of columns a solution containing the product formed by the loading operation and the ionogenic substance of the loading solution, removing the product formed .by the loading operation from the withdrawn solution, returning the resulting liquor to an intermediate column in the group of columns being loaded, feeding the other solution of ionogenic substance through the second group of columns to be regenerated and withdrawing a substantially pure solution of the product formed in this regenerating operation from the last column in this second group of columns, disconnecting the first column in the group of columns being regenerated when said column is partially regenerated and connecting same as the last column in the group of columns being loaded, disconnecting the first column in the group of columns being loaded and connecting same as the last column
  • the success of the invention resides, at least to a substantial extent, in two features: (a) regenerating the columns only partially, rather than completely, as is customary, while obtaining a substantially pure solution of the product BZAI resulting from regeneration, i. e., substantially completely converting the regenerating agent to give a solution in which the molar ratio of and (b) in the loading phase, removing the desired conversion product B1A2 from the solution withdrawn from the last column in the group being loaded, as by cooling and crystallizing, and returning the resulting mother liquor to an intermediate column, e. g., the fourth column in a group of six columns.
  • an intermediate column e. g., the fourth column in a group of six columns.
  • the group of columns being loaded is itself divided into two groups, and the loading operation is effected by passing a solution of a loading agent (BzAz) successively through a first group of these columns and thereafter the solution discharged from the last column of this first group is passed through a second group of columns to be loaded.
  • the solution discharged from the last column in this second group which is rich in B1A2 and relatively poor in BzAz, is freed of most, or at least a substantial part, of the BiAz dissolved therein, in any conventional manner, e. g., by cooling and crystallizing the solution in auxiliary apparatus.
  • the remaining mother liquor which now contains more BzAz than BlA2, is continuouslyconcentrated by evaporation and subsequently is returned to the first column of the second group undergoing loading.
  • the loading operation is stopped and the first column of the first group, which has been completely loaded in the meantime, is disconnected and cut out of the circuit, the first column of the second group is made the last of the first group and a new column, which has just been regenerated and Washed, is introduced at the end of the second group. Thereafter the loading operation is repeated.
  • Figure l is a flow diagram of the loading operation
  • Figure 2 is a flow diagram of the regeneration of the columns containing the ion exchanger.
  • C1, C2 Cm represent a first group of a limited number (m) of columns arranged in series
  • D1, D2 Dn represent a second group of a limited number (n) of columns arranged in series
  • Cr and Ev represent, respectively, a crystallizer and evaporator arranged after the last column of the second group.
  • E1, E2 Ep represent a series of a limited number (p) of columns to be regenerated.
  • a BzAa solution is supplied to column Ci; successively the solution traverses the columns C and D, the ion exchanger in the columns taking up the B2 ion while releasing B1 ions.
  • the invention may be applied for double conversions brought about both with cation and anion. exchangers, and for the purpose of eiiecting double conversion of all substances to which double conversion by ion exchanger is applicable.
  • the following example illustrates-.further the nature of the invention and the manner in which it may becarried into efiect- Example A double conversion was'ett'ected between a Ca(NO3-)-2 solution and aKCl solution. resulting in the production of KNO: crystals and a CaClz solution.
  • the cation exchanger used in this example was the normal commercial product Dowex 50 (-a sulfonated styrene). This ion exchanger has the property of more readily exchanging Ca ions than vice versa.
  • the KCl solution functions as the BIAI solution (regenerating agent)
  • the CaNOs solution as the BzAa solution (loading agent)- i
  • the loading operation was carried out in six columns arranged in series and dividedinto two groups of three columns each. For the regenerating operation a number of three columns arranged inseries was utilized.
  • Each column contained 100 liters of Dowex 50; the capacity of each column amounted to 218 grams equivalents of CaO, and the free space between the grains of cation exchanger amounted to 40 liters per column.
  • Per regeneration period 100 kg. of a 25% KCl solution was supplied to the first of the series of columns to be regenerated, while a total amount of 62 kg. of CaClz solution with a CaClz content of 15.6% and a KCl content of 0.2% was discharged from the last column after a first draw-oft of about 30 kg. of water, which had been left behind in the free spaces between the grains of Dowex 50 as a result of the washings between each regeneration and loading of the column.
  • the first column of the series of columns undergoing regeneration was 80% regenerated into the K ion loaded state.
  • 48 kg. of a 25% KCl solution was left behind. This KCl solution was regained by washing, after which the column was added to the end of the set of columns to be loaded.
  • 58 kg. of a 60% Ca(NO3)2 loading solution was left behind',lisonie heingreg'ained by washing before the column wasregenerated.
  • the present invention provides a new and highly ad'- vantageous process for carryingv out double conversion between twdionogenic'solutions, e. g'.,. the double conversiori between KCl' .and Ca(NO's)z to give KNO: and C3Cl2.
  • the process of theinvention otters the advantagesfof discharge 'fro'mion'exchangercontaining'columns of a substantially pure solution ofa compound containingtheaion removed from the indexchanger during regenerationf
  • the invention' provides,;duriiig the loading. operation, substa n-, tially pure crystals of a second'compouiidina way which eliminates. the necessity ,of attempting. separation from mother liquors which. cannot. be completely broken down into theirconstituents.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Treatment Of Water By Ion Exchange (AREA)
  • Treatment Of Liquids With Adsorbents In General (AREA)
US331473A 1952-01-19 1953-01-15 Process for effecting double conversion between two solutions of ionogenic substances by using ion exchangers Expired - Lifetime US2751280A (en)

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NL313763X 1952-01-19

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US (1) US2751280A (de)
BE (1) BE516816A (de)
CH (1) CH313763A (de)
DE (1) DE958019C (de)
FR (1) FR1069599A (de)
GB (1) GB725660A (de)
NL (1) NL79196C (de)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1064080B (de) * 1958-06-14 1959-08-27 Basf Ag Verfahren zur Herstellung von ballastfreien Kaliumammoniumsalpeter-Duengemitteln
US3059777A (en) * 1956-10-05 1962-10-23 Michigan Chem Corp Apparatus for the separation of metallic ions by the use of an ion exchange resin
US3096153A (en) * 1960-10-17 1963-07-02 Standard Magnesium Corp Inc Ion exchange process for producing potassium sulfate and sulfuric acid
US3448043A (en) * 1964-02-10 1969-06-03 Dynamit Nobel Ag Ion exchange process
WO2004018404A1 (en) * 2002-08-21 2004-03-04 Kemira Oyj Process for manufacture of carboxylic acid salts

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1283192B (de) * 1965-01-15 1968-11-21 Braunschweigische Maschb Ansta Vorrichtung zur Reinigung von Zuckersaft oder anderen Loesungen
DE2800516A1 (de) * 1978-01-03 1979-07-12 Permutit Gmbh Verfahren und vorrichtung zum behandeln von wasser, wie trink- und/oder gebrauchswasser

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1859738A (en) * 1929-09-28 1932-05-24 Firm Odda Smelteverk As Process of manufacturing fertilizers
GB415660A (en) * 1933-03-17 1934-08-30 Ig Farbenindustrie Ag Improvements in the manufacture and production of alkali metal nitrate from calcium nitrate and alkali metal chloride
US2344617A (en) * 1933-06-22 1944-03-21 Norsk Hydro Elektrisk Process for the production of salts by base-exchanging substances

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE624141C (de) * 1931-06-03 1936-01-14 Luxemburgeoise Mutosel Sa Verfahren zur Gewinnung von Salzen
DE628139C (de) * 1933-06-02 1936-04-01 Luxemburgeoise Mutosel Sa Verfahren zur Herstellung und Reinigung von Salzen mittels Basenaustauscher
DE650086C (de) * 1933-06-22 1937-09-14 Norsk Hydro Elek Sk Kvaelstofa Verfahren zur Herstellung von Salzen, insbesondere von Natriumnitrat, unter Anwendung von basenaustauschenden Stoffen

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1859738A (en) * 1929-09-28 1932-05-24 Firm Odda Smelteverk As Process of manufacturing fertilizers
GB415660A (en) * 1933-03-17 1934-08-30 Ig Farbenindustrie Ag Improvements in the manufacture and production of alkali metal nitrate from calcium nitrate and alkali metal chloride
US2344617A (en) * 1933-06-22 1944-03-21 Norsk Hydro Elektrisk Process for the production of salts by base-exchanging substances

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3059777A (en) * 1956-10-05 1962-10-23 Michigan Chem Corp Apparatus for the separation of metallic ions by the use of an ion exchange resin
DE1064080B (de) * 1958-06-14 1959-08-27 Basf Ag Verfahren zur Herstellung von ballastfreien Kaliumammoniumsalpeter-Duengemitteln
US3096153A (en) * 1960-10-17 1963-07-02 Standard Magnesium Corp Inc Ion exchange process for producing potassium sulfate and sulfuric acid
US3448043A (en) * 1964-02-10 1969-06-03 Dynamit Nobel Ag Ion exchange process
WO2004018404A1 (en) * 2002-08-21 2004-03-04 Kemira Oyj Process for manufacture of carboxylic acid salts

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Publication number Publication date
GB725660A (en) 1955-03-09
DE958019C (de) 1957-02-14
CH313763A (de) 1956-05-15
NL79196C (de)
FR1069599A (fr) 1954-07-09
BE516816A (de)

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