Title of Invention

A METHOD FOR THE SYNTHESIS OF POLYMER BEADS AND SUBSEQUENT CONVERSION INTO ION-EXCHANGE RESINS WITH NARROW PARTICLE SIZE DISTRIBUTION

Abstract

In the method for the synthesis of ion-exchange resins with narrow particle size distribution the use of the capillaries is done for the generation of monomer jets. Also, under this method the agitators are used for the controlled break up of the jets to form the monomer droplets and the reaction kettle is used as a reaction vessel for monomer droplet formation, stabilization, polymerization and hardening. This method is able to improve the particle size distribution from >1.5 to <1.5. Very importantly this method is able to produce ion exchange resins of uniform particle distribution in a single kettle vessel.

Full Text

FORM-2 THE PATENTS ACT, 1970 (39 of 1970) AND THE PATENTS RULES, 2003 COMPLETE SPECIFICATION (See Section 10; Rule 13) 1. TITLE OF THE INVENTION: "A method for the synthesis of polymer beads and subsequent conversion into ion-exchange resins with narrow particle size distribution" 2. APPLICANT: (a) NAME: ION EXCHAGE (INDIA) LIMITED. (b) NATIONALITY: AN INDIAN COMPANY INCORPORATE UNDER THE COMPANIES ACT, 1956. (c) ADDRESS: TIECICON HOUSE, DR. E. MOSES ROAD, MAHALAXMI, MUMBAI-400 011, MAHARASHTRA, INDIA. The following specification describes the nature of the invention and the manner in which it is to be performed:- METHOD FOR THE SYNTHESIS OF ION-EXCHANGE RESINS WITH NARROW PARTICLE SIZE DISTRIBUTION 3, PREAMBLE TO THE DESCRIPTION Field of Invention The present invention relates to a method for the synthesis of polymer beads and subsequent conversion into ion-exchange resins with narrow particle size distribution. Background of the Invention & the Related Art Ion exchange resin has been manufactured by a batch process using a kettle reactor for monomer droplet formation. The droplets are formed due to the cutting of the bulk monomer in an aqueous phase. The monomer droplets thus formed are stabilized in the aqueous phase with the help of suitable stabilizers. They are kept in the solution without an agglomeration with the help of the mechanical agitation. Such a type of monomer droplet formation and stabilization leads to a wide distribution of the droplet size. Subsequent polymerization of the same yields the required polymers. If, the monomers based on the styrene and the cross linked with divinyl benzene then, the polymer beads need to be functionalized. The functionalization of such polymer using sulfuric acid and oleum leads to the formation of cation exchange resin with the active functional group of sulphonate ion. On the other hand, when the polymers are first functionalized with chloromethy group the subsequent amination leads to anion exchange resins. The use of acrylic monomers like acrylamide, acrylic acid, metacyrylic acid, esters of acrylic acid or methacrylic acid leads to the formation of weak acid cation exchange resins. The cross linking agent used are either divinyl benzene or EGDMA. The acrylic based anion exchangers can be achieved by either functionalization of these acrylates or the use of functionalized monomers. The ion exchange cesins obtained by such conventional methods have a wide particle distribution. The particle distribution is normally called uniformity coefficient. The uniformity coefficient of ion exchange resin above 1.5 is normally obtained by the conventional methods. If the ion exchange resin having a uniformity coefficient less than 12, lias got few advantageous in terms of its performance in the water treatment application viz., reduction in rinse volume, reduction in channeling and improved OBR. The uniformity coefficient less than 1.2 do not have much advantage further. To exploit the above advantageous, the narrow distribution of ion exchange resins are being popularly used for the demineralization of water. Such application normally requires # uniformity coefficient less than or equal to 1.2. To the best of our knowledge and experience, there isn't much of a difference in the operation and the regeneration parameters of the ion exchange resin when, their uniformity coefficient is less than 1.2. Therefore, it is our aim to produce ion exchange resins of narrow distribution by a novel methodology. The method of production of polymer beads of narrow distribution was described in many patents: US 3204934, US 3226092, US 3922255, US 4192920, US 4333969, US 4419245, US 4427794, US 4424318, US 4444961, US 4487898, US 4521352, US 4623706, US 4666673, US 4680320, US 4870143, US 5061741, US 5231115, US 5276113, US 5380496, US 5540927, US 6251314 Bl, US 6277932 Bl, US 6365683 B2, US 6464886 B2, US 6610798 Bl, US 7053129 Bl. All the patents disclose that, the controlled formation of monomer droplets is an important step towards the preparation of uniformly sized ion exchange resins. Most of the patents use vibratory excitation of monomer droplets through the nozzle holes for the formation of monomer droplets. The various types of stabilizations of the monomer droplets formed were also disclosed in these patents. In all the patents, the uniform size droplets obtained are passed through large eolumns till they stabilized in the aqueous phase. Rohm and Hass filed a patent in 1986 (US 4,579,718) on the formation of uniform droplets by controlled coalescence methodology. Some of the patents claim the novelty on the composition of aqueous phase required for the stabilization in a column. The apparatus for the production of uniformly size polymer beads was disclosed in US 4,666,673. Mitshubushi (US 5,061,741) claims primarily on the types of nozzles used for the jet breaking technology. Bayer, Germany focuses on the stabilization of the droplets using micro-encapsulation methodology. All the patents on the present topic disclose the vibratory excitation methodology for the formation of uniform droplets. Accordingly, the monomer is passed through a vibrating nozzle. The vibratory motion breaks the monomer jet coming out the nozzle. As the vibration is uniform, the monomer jet break up is also uniform. The uniform jet break up of the monomer leads to the formation of uniform droplets. The uniform droplets thus obtained are then allowed to pass through a column containing aqueous phase. The droplets get stabilized in this column are then allowed to polymerize in a second reactor. Such a type of approach requires a large column size for bulk production of the beads. The coordination between the droplet formation and the transportation of the beads through the column for stabilization is one of the critical phenomena, which require a precise control of the aqueous phase flow rate with respect to the monomer droplet stabilization to avoid the coalescence of the same. 4. DESCRIPTION OF THE INVENTION The present invention aims to produce ion exchange resins with narrow size distribution. This is achieved by purging the monomer through a fine capillary. This process leads to the formation of a fine get and the jet break up is achieved with the help of a suitable agitator. Accordingly, the monomer mixture is passed through the capillaries and the droplets are formed by the break up of the monomer get generated out of the needles with the help of a suitable agitation conditions. The monomer droplets thus formed are then stabilized in the reaction vessel. This process is the extension of the simple conventional process of manufacturing ion exchange resins, where the monofner is added to the aqueous phase as a slug dose. The monomer droplets are then created using suitable agitation conditions. But in the present invention, the monomer passes through the capillary gets converted into the monomer droplets v^ith uniform cutting through agitators are further stabilized in the reaction kettle on\y. Upon the stabilization, the coalescence is prevented with the use of suitable agitation conditions. The stabilized monomer droplets are then polymerized in the same kettle. Further hardening and functionalization can be achieved in the same vessel or in a different vessel. The use of the second monomer mixture post hardening or before polymerization can also be achieved through this methodology. The basic and main features of the invention under consideration are the use of capillaries for the generation of monomer jets, use of agitators for the controlled break up of the jets to form the monomer droplets. Unlike earlier methodology, one can produce ion exchange resins of uniform particle distribution in a single kettle vessel. The major the improvements in the current invention under consideration over the earlier methods includes the use of capillaries instead of the precise nozzles, controlled agitation conditions for jet breaks up instead of the vibratory excitation methodology claimed by other inventions, The use of lengthy columns, for the stabilization of monomer droplets, is avoided; instead the reaction kettle is used as a reaction vessel for monomer droplet formation, stabilization, polymerization and hardening. The particle size distribution is improved from >1.5 to The invention under consideration can be better understood with the help of the flow diagram attached herewith. 5. We claim: 1. A method for the synthesis of ion-exchange resins with narrow particle size distribution. 2. A method for the synthesis of ion-exchange resins with narrow particle size distribution as claimed in claim 1, using the capillaries for the generation of monomer jets. 3. A method for the synthesis of ion-exchange resins with narrow particle size distribution as claimed in claims 1 & 2, using the agitators for the controlled break up of the jets to form the monomer droplets. 4. A method for the synthesis of ion-exchange resins with narrow particle size distribution as claimed in claims 1, 2 & 3, using the reaction kettle as a reaction vessel for monomer droplet formation, stabilization, polymerization and /or hardening. 5. A method for the synthesis of ion-exchange resins with narrow particle size distribution as claimed in claims 1, 2, 3 & 4, being able to improve the particle size distribution from >1.5 to 6. A method for the synthesis of ion-exchange resins with narrow particle size distribution as claimed in claims 1, 2, 3, 4 & 5 being able to produce ion exchange resins of narrow particle distribution in a single kettle vessel.

Documents:

1228-mum-2009-abstract.doc

1228-mum-2009-abstract.pdf

1228-MUM-2009-CLAIMS(AMENDED)-(16-7-2012).pdf

1228-mum-2009-claims.doc

1228-mum-2009-claims.pdf

1228-MUM-2009-CORRESPONDENCE(9-7-2013).pdf

1228-MUM-2009-CORRESPONDENCE(IPO)-(1-10-2009).pdf

1228-mum-2009-description(complete).doc

1228-mum-2009-description(complete).pdf

1228-mum-2009-drawing.pdf

1228-MUM-2009-FORM 1(12-5-2009).pdf

1228-mum-2009-form 1.pdf

1228-MUM-2009-FORM 18(19-05-2010).pdf

1228-mum-2009-form 2(title page).pdf

1228-mum-2009-form 2.doc

1228-mum-2009-form 2.pdf

1228-MUM-2009-FORM 26(9-7-2013).pdf

1228-mum-2009-form 3.pdf

1228-MUM-2009-REPLY TO EXAMINATION REPORT(16-7-2012).pdf

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