DL-p-hydroxyphenylglycine asymmetric conversion and resolution waste liquid treatment method
A technology for the treatment of p-hydroxyphenylglycine and waste liquid, applied in chemical instruments and methods, organic chemistry, ammonium sulfate, etc., can solve the problems of poor quality of split products and complex components of mother liquor, so as to save costs and realize waste The effect of comprehensive utilization and reduction of solid waste
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Embodiment 1
[0038] Example 1 Step 1: Recovery of D-p-hydroxyphenylglycine-(+)-phenylethanesulfonic acid double salt
[0039] The split filtrate is adjusted to pH=1~2 with sulfuric acid, and the acidified split filtrate is mixed with n-butanol at a flow rate of 10:1 (the flow rate of the normal acidified split filtrate is 6.2m 3 / h, the flow rate can be adjusted according to the production needs of the workshop), after mixing and extraction, it enters the stratification tank for stratification, the lower aqueous phase is transferred to step 3 for processing, and the upper organic phase is pumped into the resolving agent recovery tank after turnover.
[0040] When the organic phase in the resolving agent recovery kettle reaches 5000L, add 500kg of water, start stirring, put in 200kg of D-hydroxyphenylglycine, add 65kg of sulfuric acid dropwise, and stir for 3 to 5 hours after the dropwise addition is complete. Blow the material to the centrifuge for centrifugation, wash the filter cake with 2...
Embodiment 2
[0041] Embodiment 2 step 2: reclaim embodiment 1 organic solvent
[0042] The filtrate in Example 1 was transferred to a layered tank for standing and stratified, the water phase was transferred to step 3 for processing, and the organic phase was transferred to single-effect concentration, the concentration temperature was 50-65°C, and the vacuum degree was 0.05-0.1MPa. After efficient concentration, the raffinate is transferred to the slag steaming kettle for further concentration. After the concentration of the slag steaming kettle is completed, the residue is transferred to the incineration workshop for incineration. The n-butanol recovered by concentration is transferred to the next stage step 1 for extraction, and the GC purity of recovered n-butanol is 98.7%.
Embodiment 3
[0043] Example 3 Step 3: Recover the second part of D-p-hydroxyphenylglycine-(+)-phenylethanesulfonic acid double salt
[0044] Combine the liquid-separated water phase in Example 1 and the liquid-separated water phase in Example 3, start to concentrate under reduced pressure, the concentration temperature is 55-75° C., and the vacuum degree is 0.05-0.1 MPa. After the temperature and concentration vacuum are stable, control the feed amount of the water phase for continuous discharge and concentration, and the concentration density is greater than 1.1g / m 3 When the concentration is stopped, the COD of the condensed water produced by the concentration meets the discharge requirements, and the COD value is 145mg / L, and it is transferred to the biochemical pool for treatment. Transfer the concentrated solution to the double salt recovery kettle for cooling and crystallization. The crystallization temperature is 20-30°C, centrifuge, wash the solid with water, and then dry it by cen...
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