Treatment, recovery and utilization method for waste liquid from dinitolmide production
A technique for treating dinitramine and its treatment method, which is applied in the fields of chemical instruments and methods, preparation of carboxylic acid amides, preparation of organic compounds, etc., which can solve the problems of difficult treatment, high treatment cost, complex chemical composition, etc., and achieve good quality , high conversion rate, cost-saving effect
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Embodiment 1
[0026] A kind of treatment method of dinitramine production waste liquid, comprises the following steps:
[0027] (1) Separating the ammoniated waste liquid produced in the synthesis reaction of dinitramide, recovering and storing the separated organic phase (from the solvent toluene used in the acyl chloride reaction), and entering the separated aqueous phase into the next step for processing;
[0028] (2) Slowly add the waste acid solution produced during the water washing process of the nitration product into the obtained water phase, while stirring, continue to add the waste acid solution until the pH<1, and the precipitate no longer precipitates (when the pH value of the mixed solution reaches neutral , continue to add the waste acid solution dropwise, precipitation begins to precipitate, and continue to drop until pH<1, a large amount of precipitation precipitates);
[0029] (3) Separating and collecting the precipitate, washing with water and drying to obtain light yell...
Embodiment 2
[0039] A kind of recycling method of dinitramine production waste liquid, comprises the following steps:
[0040] (a) Add 6 times the weight of methanol to the solid A obtained in Example 1, continue to stir and raise the temperature to 62°C, keep stirring for 1 hour, then cool down to room temperature, perform suction filtration, and dry the obtained filter residue to obtain light yellow Powdered solid B, see figure 2 , its melting point is 203-208°C after testing;
[0041] (b) Mix 25 parts by weight of toluene with 20 parts by weight of the solid B, keep stirring and raise the temperature to 62°C, then add 0.5 parts by weight of DMF (N,N-dimethylformamide) and 15 parts by weight of thionyl chloride After stirring for 1 hour, the temperature was slowly raised to 90°C, and after reflux for 1 hour, the temperature was lowered to room temperature to obtain liquid X;
[0042] (c) Mix 30 parts by weight of ammonia water (25%) with 30 parts by weight of water, continue to stir a...
Embodiment 3
[0046] A kind of treatment method of dinitramine production waste liquid, comprises the following steps:
[0047] (1) Separating the ammoniated waste liquid produced in the synthesis reaction of dinitramide, recovering and storing the separated organic phase (from the solvent toluene used in the acyl chloride reaction), and entering the separated aqueous phase into the next step for processing;
[0048] (2) Slowly add the waste acid solution produced during the water washing process of the nitration product into the obtained water phase, while stirring, continue to add the waste acid solution until the pH<1, and the precipitate no longer precipitates (when the pH value of the mixed solution reaches neutral , continue to add the waste acid solution dropwise, precipitation begins to precipitate, and continue to drop until pH<1, a large amount of precipitation precipitates);
[0049] (3) The precipitate was separated and collected, washed with water and dried to obtain light yell...
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