The method of purification polysulfide silanes coupling agent by-product salt solution
Technical field
The present invention relates to a kind of method purifying polysulfide silanes coupling agent by-product salt solution, belong to chemical technology field.
Background technology
In the aqueous phase production technique of polysulfide silanes coupling agent, having side product chlorinated sodium to generate, is the form output with salt solution.Because organic chemical reactions can not 100% to react completely and the generation of some side reactions, some unreacteds completely sulfonium ion remain in by-product salt solution, these sulfonium ions can be converted into toxic and harmful hydrogen sulfide once touch sour environment, to environment, and likely personnel are damaged, and be unfavorable for that the further purification of side product chlorinated sodium transforms.
The domestic relevant report not to this by-product brine treatment, does not have a kind for the treatment of process of maturation of the waste water for this kind of character at present.
Summary of the invention
Goal of the invention: for solving the problems of the technologies described above, the object of this invention is to provide a kind of method purifying polysulfide silanes coupling agent by-product salt solution, solves the purification process of environmental issue and side product chlorinated sodium.
Technical scheme: for achieving the above object, the present invention adopts following technical proposals:
Purify a method for polysulfide silanes coupling agent by-product salt solution, comprise the steps:
A, sulfur oxide ion: the by-product salt solution of polysulfide silanes coupling agent is put in reaction unit, under whipped state, drips hydrogen peroxide solution, the sulfonium ion in by-product salt solution is all converted into sulfate radical;
B, hot method are except nitre: by the brine filter removal of impurities after above-mentioned process, gained clear liquid carries out multiple-effect evaporation, obtains byproduct sodium-chlor and sodium sulfate.
Wherein, the detection method whether sulfonium ion in by-product salt solution is all converted into sulfate radical is Lead acetate paper detection method or cupric chloride variable color method.
Beneficial effect: the present invention alkalescence, the polysulfide silanes coupling agent by-product salt solution that has sulfonium ion purified as product sodium-chlor except nitre operation by oxidation, hot method, efficiently solves the process of polysulfide silanes coupling agent by-product salt solution.Sulfonium ion can be converted into sulfate radical by the inventive method completely, and is separated with sodium-chlor by vitriol product by the method for hot method except nitre, obtains the sodium-chlor of higher degree.Solve the environmental issue of polysulfide silanes coupling agent by-product salt solution and the purification process of by-product salt sodium-chlor.
Embodiment
Below in conjunction with specific embodiment, the present invention is further described.
Purify a method for polysulfide silanes coupling agent by-product salt solution, comprise the steps:
A, sulfur oxide ion: the by-product salt solution of polysulfide silanes coupling agent is put in reaction unit, under whipped state, drips hydrogen peroxide solution, the sulfonium ion in by-product salt solution is all converted into sulfate radical;
B, hot method are except nitre: by the brine filter removal of impurities after above-mentioned process, gained clear liquid carries out multiple-effect evaporation, obtains byproduct sodium-chlor and sodium sulfate.
Wherein, the detection method whether sulfonium ion in by-product salt solution is all converted into sulfate radical is Lead acetate paper detection method or cupric chloride variable color method.
Embodiment:
The by-product salt solution of two (propyl-triethoxysilicane) polysulfide of 3m3 is dropped in 5000L stirring tank, the hydrogen peroxide 30Kg that massfraction is 27.5% is dripped under whipped state, temperature of reaction system is kept to be less than 90 DEG C in dropping process, dropping terminates rear stirring 15min to reacting completely, and stops stirring.From reaction system, get about 50ml sample pours in Erlenmeyer flask, 1 dropper Cupric Chloride Solution is dripped in sample with 5mL Dispette, rock, produce precipitation, drip hydrochloric acid again to record the pH < 4 of sample with wide pH value test paper, if precipitation is not dissolved, illustrate that reaction not exclusively, continue to drip hydrogen peroxide until sulfonium ion is fully oxidized; If being deposited in of producing drips (the pH < 4 of sample) precipitation after hydrochloric acid and disappear, show that sulfonium ion is fully oxidized, reaction is reached home.Salt solution after above-mentioned process is crossed pressure filter, removing impurity solid.Clear liquid is pumped into hot method except nitre multi-effect evaporation system, controlling an effect vaporization temperature is 90 DEG C ~ 100 DEG C, two effect vaporization temperatures control at 60 DEG C ~ 65 DEG C, entering whizzer mother liquor temperature controls at 45 DEG C ~ 50 DEG C, whizzer solid is out product sodium-chlor, when after circulation for some time, mother liquor sampling survey sodium sulphate content reaches about 61g/L, mother liquor is entered preheater preheats to proceed to and analyse nitre tank, enter after making the content of sodium sulfate be down to 53g/L flash distillation lower the temperature further concentrated after, enter the evaporation of sodium-chlor salt cellar again, run so continuously, distill out byproduct sodium-chlor and sodium sulfate respectively.
The by-product salt of polysulfide silanes coupling agent Aqueous phase production technique produces as an aqueous solution, and remaining unreacted sulfonium ion completely in this aqueous solution, if deal with sulfonium ion improperly may be converted into poisonous and hazardous hydrogen sulfide, causes environmental pollution and accident.Sulfonium ion can be converted into sulfate radical by the inventive method completely, and is separated with sodium-chlor by vitriol product by the method for hot method except nitre, thus obtains the by-product salt solid sodium chloride of higher degree.Solve the environmental issue of polysulfide silanes coupling agent by-product salt solution and the purification process of by-product salt sodium-chlor.