Industrial process for continuous production of zeolite A

• US 4,314,979 A
• Filed: 12/19/1979
• Issued: 02/09/1982
• Est. Priority Date: 07/29/1977
• Status: Expired due to Term

• Current Assignee: Pcuk Produits Chimiques Ugine Kuhlmann
• Original Assignee: Pcuk Produits Chimiques Ugine Kuhlmann
• Inventors: Deabriges, Jean
• Primary Examiner(s): Meros, Edward J.
• Application Number:
  US06/105,273
• Time in Patent Office: 783 Days
• Field of Search: 423/328-330, 253/455 Z
• US Class Current: 423/700
• CPC Class Codes: C01B 33/2823 from aqueous solutions of an alkali metal aluminate and an alkali metal silicate excluding any other source of alumina or silica
• CPC Class Codes: Y10S 423/24 LTA, e.g. A, alpha, ZK-4, ZK-21, ZK-22

Abstract

A process for continuous preparation of zeolite A of constant and homogeneous quality, consisting of instantly and continously mixing a sodium silicate solution and a sodium aluminate solution in the correct proportions and at an elevated temperature followed by transfer of the resulting slurry to a crystallization reactor. The product is recovered from the crystallization reactor washed and dried.

Claims

1. A process for the continuous preparation of zeolite A, suitable for use in detergents to soften calcium containing waters, having a constant homogeneity and quality wherein at least about 90 percent of the product has a granulometry within a range of 4 microns and a median diameter between about 1 and about 10 microns is characterized by:

(a) instantaneously and continuously mixing at an elevated temperature in a reaction zone subjected to strong suction;

(i) a sodium silicate solution prepared from silica and NaOH which contains a minimal excess of NaOH and a SiO₂ /Na₂ O molar ratio ≧

2.8 to 1; and

containing about 45 to 105 g/l of NaOH and about 120 to 350 g/l of SiO₂ ;

(ii) a sodium aluminate solution made from alumina and NaOH having an excess of NaOH solution, and containing about 80 to 110 g/l of NaOH and about 50 to 65 g/l of Al₂ O₃ ;

(b) precipitating the zeolite while continuously stirring the resulting solution at an elevated temperature and while restricting the volume of the reaction zone to insure that there is a local excess of dissolved alumina in relation to dissolved silica in the solution;

by;

(i) introducing the sodium silicate and sodium aluminate solutions into the suction zone created by a rapidly rotating turbine; and

(ii) adjacently surrounding the turbine with plates constructed and arranged to restrict the volume in which the above silicate and aluminate solutions are initially mixed;

(c) continuously removing the precipitated zeolite A and resulting liquor to a crystallization zone;

(d) continuously stirring the resultant precipitate and liquor in the crystallization zone at an elevated temperature until the desired crystallization is obtained;

(e) maintaining the concentration of the liquor in the crystallization zone between about 2 to 10 g/l of Al₂ O₃ ;

(f) removing the most dense or larger particles in suspension at the bottom of the crystallization zone; and

(g) recovering the zeolite A containing at least about 90 percent of the particles within a range of about 4 microns and having a median diameter between about 1 and 10 microns and an ion exchange capacity greater than 85 mg. Ca⁺⁺ /g of dry product.

2. The process according to claim 1 wherein the separately prepared sodium aluminate solution is in the form of a sodium aluminate liquor taken from an alumina production plant and the liquor from the stirring mixture is returned for use in an alumina production plant.

3. The process according to claim 1 comprising a recycling of the mother liquor which is characterized by continuously:

(a) concentrating the mother liquor sufficient to permit a replenished aluminate solution having substantially the same volume as the prior aluminate solution;

(b) replenishing the NaOH in the mother liquor in an amount sufficient to compensate for the NaOH consumed during the prior crystallization of zeolite A;

(c) charging the mother liquor with alumina in an amount sufficient to compensate for the alumina consumed during the prior crystallization of zeolite A; and

(d) mixing the charged mother liquor with the sodium silicate solution as recited in claim 11.

4. The process according to claim 1 or 3 wherein the sodium aluminate solution is saturated with alumina at atmospheric pressure.

5. The process of claim 1 wherein the sodium aluminate solution has a molar ratio for Al₂ O₃ /Na₂ O between 0.35 and 0.65.

6. The process of claim 1 wherein the sodium aluminate solution has a molor ratio for Al₂ O₃ /Na₂ O between 0.41 and 0.57.