Process for Preparing a Triazine-Based Precursor, the Precursor Prepared Thereby, a Method for Producing a Micro-Particulate Complex Using the Precursor, and the Micro-Particulate Complex Produced Thereby

Abstract

A process for preparing a triazine-based precursor for producing a micro-particulate complex containing a far infrared-emissive silica particle comprises steps of: a) subjecting 2-4-6-trichloro-1,3,5-triazine and a first nucleophilic compound to a displacement reaction in the presence of a first solvent at a first temperature range to form an intermediate; and b) subjecting the intermediate and a second nucleophilic compound to a further displacement reaction in the presence of a second solvent at a second temperature range higher than the first temperature range.

What is claimed is: 
     
         1 . A process for preparing a triazine-based precursor for producing a micro-particulate complex containing a far infrared-emissive silica particle, the process comprising steps of:
 a) subjecting 2-4-6-trichloro-1,3,5-triazine and a first nucleophilic compound represented by a formula of H—X(R 1 ) n  to a displacement reaction in the presence of a first solvent at a first temperature range to form an intermediate represented by Formula (1)   
       
         
           
           
               
               
           
         
       
       wherein
 each X is a nucleophilic atom independently selected from the group consisting of N, O, and S, 
 each R 1  is independently selected from the group consisting of H, C 1 -C 22  linear alkyl, and C 1 -C 22  branched alkyl and is unsubstituted with amino, and 
 each n is independently 1 or 2, 
 with the proviso that
 X is O or S and R 1  is not H when n is 1, and 
 X is N and at least one R 1  is not H when n is 2; and 
 
 b) subjecting the intermediate represented by Formula (1) and a second nucleophilic compound represented by a formula of H—NH-R 2 —Si(OR 3 ) 3  to a further displacement reaction in the presence of a second solvent at a second temperature range higher than the first temperature range to form the triazine-based precursor represented by Formula (a), 
 
       
         
           
           
               
               
           
         
         wherein
 R 2  represents C 2 -C 4  alkylene, and 
 each R 3  independently represents C 1 -C 2  alkyl. 
 
       
     
     
         2 . The process according to  claim 1 , wherein in step a), the first temperature range is up to 40° C. 
     
     
         3 . The process according to  claim 1 , wherein in step b), the second temperature range is from 35° C. to 70° C. 
     
     
         4 . The process according to  claim 2 , wherein step a) includes sub-steps of:
 a1) subjecting 2-4-6-trichloro-1,3,5-triazine and the first nucleophilic compound to a first stage of the displacement reaction in the presence of the first solvent at a lower temperature ranging from 0° C. to 25° C. to form a pre-intermediate represented by Formula (i):   
       
         
           
           
               
               
           
         
       
       and
 a2) subjecting the pre-intermediate represented by Formula (i) and the first nucleophilic compound to a second stage of the displacement reaction in the presence of the first solvent at an upper temperature which is higher than the lower temperature in sub-step a1) and which is from 15° C. to 40° C. to form the intermediate represented by Formula (1). 
 
     
     
         5 . The process according to  claim 4 , wherein the first nucleophilic compound used in sub-step a1) is different from that used in sub-step a2), and the first solvent used in sub-step a1) is different from that used in sub-step a2). 
     
     
         6 . A triazine-based precursor prepared by the process according to  claim 1 . 
     
     
         7 . A method for producing a micro-particulate complex containing a far infrared-emissive silica particle, comprising a step of subjecting the triazine-based precursor according to  claim 6  and tetra-alkyl orthosilicate to hydrolysis and polycondensation. 
     
     
         8 . The method according to  claim 7 , wherein the tetra-alkyl orthosilicate is tetraethyl orthosilicate. 
     
     
         9 . A micro-particulate complex containing a far infrared-emissive silica particle produced by the method according to  claim 7 .