US2771418A - Process of converting substances ionized in solution, with the help of ion exchangers - Google Patents

Process of converting substances ionized in solution, with the help of ion exchangers Download PDF

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Publication number
US2771418A
US2771418A US314832A US31483252A US2771418A US 2771418 A US2771418 A US 2771418A US 314832 A US314832 A US 314832A US 31483252 A US31483252 A US 31483252A US 2771418 A US2771418 A US 2771418A
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ion
column
solution
columns
group
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US314832A
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English (en)
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Johannes A Zeegers
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Stamicarbon BV
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Stamicarbon BV
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J47/00Ion-exchange processes in general; Apparatus therefor
    • B01J47/02Column or bed processes
    • B01J47/026Column or bed processes using columns or beds of different ion exchange materials in series
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J49/00Regeneration or reactivation of ion-exchangers; Apparatus therefor

Definitions

  • the present invention relates to a process of converting substances which 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 regenerating the ion exchanger used in this conversion process.
  • the first phase of the process the so called loading of the I.E., may be represented by the equation:
  • the I.E. which is now charged with B2 ions, is subsequently Washed with. water and thereafter regenerated by passing a solution of the salt- B1A1 over it.
  • the second phase of the conversion process may be represented by the equation:
  • this transition zone is constant and the dimensions of the columns are always chosen so that the whole transition zone lies within one column or a few columns.
  • solution of which as such is obtainable in large amounts For instance, the previously proposed preparation of NaNO;; by converting a Ca(NO3)2 solution with sea water with the help of an I.E. can be effected economically without recovering the regenerating agent NaCl.
  • the solution obtained in the regeneration is nothing but sea water which has become poor in NaCl and has some CaCl2 dissolved therein.
  • Such a solution contains no valuable components and may, therefore, be directly pumped into the sea without objection.
  • the principal object of the present invention is the provision of a novel method for the regeneration of ionexchangers, or columns filled with such ion-exchangers, which method is free from the disadvantages noted above in connection with prior regeneration techniques.
  • the present invention provides the improvements in a process for regenerating an ion-ex- 4 changer by passing a solution of a regenerating agent successively through a series of columns containing the ion-exchanger loaded with the ion to be replaced and withdrawing regenerated ion-exchanger from the first of the series and a solution of spent substantially completely converted regenerating agent from the last of the series, comprising the steps of dividing the series of columns into two groups and passing an excess of regenerating agent through the first group, removing excess regenerating agent from the solution discharged from the first group of columns, thereafter, passing said solution through the second group of columns, collecting the substantially completely converted regenerating solution from the last column of the second group, cutting out the first column of the first group and making the first column of the second. group the last of the first group, introducing a new column filled with untreated ion-exchanger loaded with the ion to be replaced at the end of the second group and, thereafter, repeating said operation.
  • the regenerating method according to the invention is not only applicable to the preparation of KNO: by double conversion of KCl and Ca(NO3)2 solutions with the help of an ion-exchanger, but in principle, the process may be used advantageously for many double conversions between ionog'enic substances, in which a series of successive loadings and regenerations of the ion-exchanger, according to the above-mentioned Equations (2) and (3) are employed, namely:
  • Figure 1 is a flow diagram of the regeneration
  • Figure 2 is a flow diagram of the loading 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
  • Ev and Cr represents, respectively, an evaporator and crystallizer arranged between the two groups of columns to be regenerated.
  • E1, E2 Ep represent a series of a limited'number (p) of columns to be loaded.
  • the completely regenerated column C1 at the side where the'regenerating agent is supplied, is put out of the circuit at the end of a certain lapse of time, i. e., the regeneration period.
  • the series of columns is recom'pleted by adding a new column containing ion exchanger which is completely unregenerated, the feed and discharge of the two groups ofcolumns at. the same time being subjected to an alteration such, that the first column of group D is moved over to group C and becomes Cm, Anew regeneration period isthen begun whereby one more column, the first of the first stage, is completely regenerated.
  • column C2 is put'out of the circuit and the other columns" are again rearranged with the addition ofjstill another new column in the manner denoted above.
  • the success of the invention is due, at least to a large extent,, to the splitting up of the regeneration into three stages and the corresponding change effected in the composition of the solution traversing the groups of columns 6 and D'during one regeneration period by virtue of the removal, as by crystallization, of excess regenerating agentin the second stage 'ofthe regeneration.
  • B2Aa precipitates and an equivalent amount of BIAI is dissolved.
  • This newly-formed amount of BiAi should then be removed by crystallization together with the excess of B1A1.
  • the amount of B2 ions to be removed cannot be determined exactly and must be ascertained experimentally in those cases where it isiound that, after removing B1A1 in the secondstage of the regeneration process, thesolution discharged from the last column is not practically free from BlAl. In practice, however, it. has been foundthat it generally suffices to remove only a relatively small quantity of B2 ions.
  • the loading of the regenerated columns may be carried out in the conventional way shown in Figure 2, i. e., by
  • the completely loaded column E1 at the side where the loading agent is supplied',;is put out of the circuit at the end of a certain lapse of time, i. e., at the end of the loading. period.
  • the series of columns' is recompleted' by adding anew column containing ion-exchanger which is fully regenerated, i. e., one to be loaded, and a new loading period begun, in which just the first column is completely loaded.
  • the regeneration of the columns loaded with Ca ions was carried out in such a manner that for each regeneration period six columns were traversed by the regenerating liquid, the columns being arranged in two groups of three columns each.
  • a 37% KCl solution was fed to the first column of the first group at 90 C.
  • a total of 198 kg. of solution was fed to the first column.
  • From the third column of the first group a total amount of 196 kg. of solution was discharged, first 52 kg. present in the free space and after that 144 kg., the mean composition of which was as follows:
  • a new regeneration period was started in which the column that had been totally regenerated in the preceding period was first put out of the circuit and a new column to be regenerated thereafter added.
  • the solution was evaporated to such a degree that at 25 C. 48.8 kg. of MgSO4 were crystallized out and separated from the remaining mother lye (17.2 kg.) by centrifuging.
  • the mother lye, having the composition 25% MgCl2 5% MgSO4 70% H2O was supplied to the first column of the second group of columns together with 40 litres of liquid discharged from the free space in the last column of the first group.
  • the present invention provides a new and highly advantageous process for the regeneration of columns filled with ion-exchangers, particularly those used in carrying out double conversion between two salt solutions, e. g., the double conversion between KCl and Ca(NOs)2 to give KNOs and CaClz.
  • the regeneration process of the present invention possesses the advantage of enabling complete ion-exchange regeneration using a limited and constant number of columns containing the ion-exchanger to be regenerated, while avoiding the disadvantages involved if an everwidening transition zone moving within the columns is allowed to build up.
  • the present process possesses the additional advantage of permitting discharge from the regenerating columns of a single solution containing a compound of the ion removed from the ion-exchanger which is substantially free of the regenerating agent.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Treatment Of Liquids With Adsorbents In General (AREA)
  • Treatment Of Water By Ion Exchange (AREA)
US314832A 1951-10-24 1952-10-15 Process of converting substances ionized in solution, with the help of ion exchangers Expired - Lifetime US2771418A (en)

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NL314631X 1951-10-24

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US (1) US2771418A (el)
BE (1) BE515065A (el)
CH (1) CH314631A (el)
DE (1) DE933446C (el)
NL (1) NL76322C (el)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3004824A (en) * 1957-03-18 1961-10-17 Colgate Palmolive Co Copper phosphate salts
US3457032A (en) * 1964-06-22 1969-07-22 Alusuisse Process for purifying solutions containing aluminates
US3714143A (en) * 1971-04-13 1973-01-30 Us Army Continuous process for manufacture of nitrocellulose
US4707347A (en) * 1985-04-17 1987-11-17 Kali Und Salz Process for the production of potassium sulfate from potassium chloride by means of ion exchangers
AU577460B2 (en) * 1985-04-17 1988-09-22 Kali Und Salz A.G. Method for manufacture of potassium sulphate from potassium chloride with ion exchangers

Families Citing this family (1)

* 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

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1978447A (en) * 1931-06-02 1934-10-30 Austerweil Geza Process for the preparation, separation, and purification of salts, salt solutions, and other solutions
US2252065A (en) * 1939-09-11 1941-08-12 Culligan Zeolite Co Method and apparatus for treating water softeners
US2397575A (en) * 1938-08-09 1946-04-02 Permutit Co Method for recovering copper value from dilute solutions of copper salts
US2458115A (en) * 1947-08-02 1949-01-04 Dorr Co Control of ion exchange systems
US2564820A (en) * 1939-10-18 1951-08-21 Octrooien Mij Activit Nv Mixed bed sugar purification
US2599558A (en) * 1947-09-25 1952-06-10 Ionics Method of regenerating anion exchange materials and composition therefor
US2689229A (en) * 1951-12-04 1954-09-14 Standard Oil Dev Co Regeneration of ion-exchange materials

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1978447A (en) * 1931-06-02 1934-10-30 Austerweil Geza Process for the preparation, separation, and purification of salts, salt solutions, and other solutions
US2397575A (en) * 1938-08-09 1946-04-02 Permutit Co Method for recovering copper value from dilute solutions of copper salts
US2252065A (en) * 1939-09-11 1941-08-12 Culligan Zeolite Co Method and apparatus for treating water softeners
US2564820A (en) * 1939-10-18 1951-08-21 Octrooien Mij Activit Nv Mixed bed sugar purification
US2458115A (en) * 1947-08-02 1949-01-04 Dorr Co Control of ion exchange systems
US2599558A (en) * 1947-09-25 1952-06-10 Ionics Method of regenerating anion exchange materials and composition therefor
US2689229A (en) * 1951-12-04 1954-09-14 Standard Oil Dev Co Regeneration of ion-exchange materials

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3004824A (en) * 1957-03-18 1961-10-17 Colgate Palmolive Co Copper phosphate salts
US3457032A (en) * 1964-06-22 1969-07-22 Alusuisse Process for purifying solutions containing aluminates
US3714143A (en) * 1971-04-13 1973-01-30 Us Army Continuous process for manufacture of nitrocellulose
US4707347A (en) * 1985-04-17 1987-11-17 Kali Und Salz Process for the production of potassium sulfate from potassium chloride by means of ion exchangers
AU577460B2 (en) * 1985-04-17 1988-09-22 Kali Und Salz A.G. Method for manufacture of potassium sulphate from potassium chloride with ion exchangers

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NL76322C (el)
CH314631A (de) 1956-06-30
DE933446C (de) 1955-09-29
BE515065A (el)

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