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Publication Detail
Crystal Product Engineering in the Seeded Cooling Crystallization of Adipic Acid from Aqueous Solution
  • Publication Type:
    Journal article
  • Publication Sub Type:
    Article
  • Authors:
    Narducci O, Jones AG, Kougoulos E
  • Publisher:
    AMER CHEMICAL SOC
  • Publication date:
    09/2011
  • Pagination:
    974, 980
  • Journal:
    Organic process research and development
  • Volume:
    15
  • Issue:
    5
  • Status:
    Published
  • Print ISSN:
    1083-6160
  • Language:
    EN
  • Addresses:
    Jones, AG
    UCL
    Dept Chem Engn
    London
    WC1E 7JE
    England
Abstract
The effects of seed preparation method and operating conditions during the batch cooling crystallization of adipic acid in aqueous solution are reported. Seeds were prepared by cooling crystallization with and without ultrasound and by-grinding commercial crystals. The effects of cooling rate, initial concentration, seeding load, and supersaturation at the point of seeding on the crystal size distribution and crystal habit of the final product were studied to characterize the conditions for the achievement of a growth-dominated operation. A seed loading at 10% of the total mass of dissolved material ensured a near unimodal distribution of product crystal particles for any type of seed source investigated. Higher values of initial concentration/temperature led to larger particles; however the nucleation rates increased as well, requiring slower cooling rates to maintain the growth predominantly within the metastable zone. A slow cooling (0.1 K/min) applied exclusively during the first 10 degrees C subcooling, followed by a higher rate (0.5 K/min) provided large product crystal particles with reduced secondary nucleation, shortening the operation times. Seeding with round crystals obtained from a continuously insonated crystallization resulted in a product of more regular crystal habit with increased thickness than seeding with conventionally ground material.
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