Method for synthesizing m-phenetidine

Method for synthesizing m-phenetidine

  • CN 106,336,361 A
  • Filed: 08/24/2016
  • Published: 01/18/2017
  • Est. Priority Date: 08/24/2016
  • Status: Active Application
First Claim
Patent Images

1. a kind of method of synthesis m-phenetidine is it is characterised in that comprise the steps:

  • Step s1, m-aminophenol, alkali, solvent is put in reactor, is then simultaneously introduced catalyst and alkylating reagent, plusMaterial finishes, closed reactor, under stirring at room temperature 0.5-1.5h;

    Then heat to 40 DEG C -80 DEG C reaction 2-8h, reaction terminatesAfterwards, gained reactant liquor filters after being cooled to room temperature, obtains filtrate;

    Wherein, alkali and m-aminophenol mol ratio are 1;

    0.8-1.2, urgeAgent is 0.04-0.08;

    1 with the mass ratio of m-aminophenol, and alkylating reagent is 1.0- with the mol ratio of m-aminophenol1.6;

    1;

    Step s2, the filtrate decompression distillation of step s1 gained obtains m-phenetidine;

    Wherein, described catalyst is Ti-Si composite oxide, is prepared via a method which;

    step s1, and following weight portion is formerMaterial is mixed and made into silicon solution;

    silicon source, 20-30 part;

    Surfactant, 5-15 part;

    Deionized water, 60-80 part;

    Step s2, will be asThe mixed raw material of lower weight portion becomes titanium solution;

    titanium source, 20-30 part;

    Deionized water, 60-80 part;

    Step s3, titanium solution is delayedSlowly it is added in silicon solution, 50-70 DEG C of stirring 1-2 hour obtains titanium silicon mixed solution;

    Step s4, adds to above-mentioned titanium silicon mixed solutionPlus copper sulfate and nano barium sulfate;

    Add copper sulfate 4-6 part and nano barium sulfate in the titanium silicon mixed solution of every 100 weight portions6-8 part;

    Step s5, step s4 resulting solution is spray-dried, spray dryer nozzle temperature between 200-240 DEG C,Outlet temperature is between 90-110 DEG C;

    Step s6, by step s5 products therefrom in 550-650 DEG C of roasting 1-3 hour, obtains final product describedTi-Si composite oxide;

    In Ti-Si composite oxide, the molar ratio of ti and si element is 2-4;

    1.

View all claims
    ×
    ×

    Thank you for your feedback

    ×
    ×