CN103058439A - Processing method of mother liquor generated in production of glyphosate by alkyl ester method - Google Patents

Abstract

The invention relates to a processing method of waste liquor produced in a production process of a chemical herbicide, and particularly relates to a processing method of mother liquor generated in production of glyphosate by an alkyl ester method. The method comprises the following steps of: a: preparing the mother liquor generated by producing glyphosate by the alkyl ester method, and adding hydrochloric acid or sulfuric acid in the mother liquor to adjust PH value to 0.1-1.5; b: adding FeCl3 in the adjusted waste liquor, wherein the addition of FeCl3 is 1-5% of the quality of the mother liquor of glyphosate, raising a temperature and stirring to produce flocculating settling, filtering and separating out flocculate; and controlling the raised temperature at 60-80 DEG C; and c: raising the temperature of filtrate and concentrating, cooling, filtering and separating out NaCl, and mixing residual liquid with the next batch of wastewater and processing or adding in a hydrolysis deacidification section of glyphosate to replace industrial water. The processing method is simple in technology step and low in implementation cost and has no secondary pollution; no phosphorus-containing wastewater during processing process is discharged, and the processing effect is improved.

Description

Alkyl esterification method is produced the treatment process of the mother liquor of glyphosate

Technical field

The present invention relates to the treatment process of the waste liquid that produces in a kind of chemical herbicide production process, specifically a kind of alkyl esterification method is produced the treatment process of the mother liquor of glyphosate.

Background technology

The glyphosate chemical herbicide is the product of domestic and international Pesticidal products tonnage maximum.Glyphosate output accounts for whole agricultural chemicals output more than 1/3rd.The glyphosate synthesis method mainly contains two sweet phosphorus oxidation methods and take glycine, dimethylphosphite as main raw material synthesis of alkyl ester method production technique, because the alkyl esterification method production technique has starting material and is easy to get, the high characteristics of element utilization ratio, enterprise adopts by most domestic.Existing alkyl esterification method is produced glyphosate and is accounted for domestic glyphosate ultimate production more than 70%.Yearly capacity is about more than 700,000 tons.

The alkyl esterification method glyphosate technicals is produced, and one ton of former medicine of every production produces 4.5 tons of mother liquors approximately.Glyphosate mother solution is a kind of high density saliferous, phosphorus-containing wastewater, and this waste water is yellow liquid, and density is 1160kg/m3, PH=9 ~ 11, about COD=50000mg/L, total phosphine 22g/L, wherein glyphosate 23g/L, phosphorous acid 47g/L, glycine 2%, sodium chloride content is about 15%.The harmless treatment of glyphosate mother solution is glyphosate industry Sustainable development key subjects.Present existing treatment process exists the problems such as processing cost height, secondary pollution be serious mostly.

Summary of the invention

Technical problem to be solved by this invention is that the treatment process of the mother liquor of the alkyl esterification method production glyphosate that a kind of processing step is simple, implementation cost is low, treatment effect is good is provided.

The treatment process that alkyl esterification method of the present invention is produced the mother liquor of glyphosate is:

A. the mother liquor of getting alkyl esterification method production glyphosate and producing adds hydrochloric acid or sulphur acid for adjusting pH value to 0.1-1.5 in mother liquor;

B. add FeCI3 in the waste liquid after adjustment, add-on is the 1-5% of glyphosate mother solution quality, and the stirring that heats up produces flocculating settling, filters to isolate throw out; The intensification temperature is controlled at 60-80 ℃;

C. filtrate is concentrated through heating up, and isolates NaCI through cold filtration again, and raffinate is incorporated lower batch waste water into and processed or add glyphosate hydrolysis depickling workshop section and substitute process water.

The described throw out that filters to isolate burns through incinerator and generates composite phosphate, can be used as industrial raw material.

Processing step of the present invention is simple, implementation cost is low, and treating processes is discharged without phosphorus-containing wastewater, and non-secondary pollution has improved treatment effect.

Embodiment

Embodiment one

Take by weighing 200 gram glyphosate mother solutions (pH value=9.5), add the hydrochloric acid of 22 grams, pH value is adjusted to 1, adds 6 gram FeCl3, stirs and is warmed up to 80 degree.Be incubated 30 minutes, filtered while hot gets filter cake 38g, and filtrate continuation is warmed up to 100 degree underpressure distillation, and phlegma reaches 120ml, cooling filtering separation raffinate and NaCl.Get NaCI29.6g through check NaCI content〉more than 96%, raffinate 38g preserves also and the next batch waste liquid is together processed.Filter cake burns and obtains glue sodium phosphate 1 gram.

Embodiment two

The raffinate 38g that embodiment one is obtained adds glyphosate mother solution 200g again, and the waste liquid that mixes is processed according to the method identical with embodiment one.Acquired results and embodiment one are basic identical.

Embodiment three

Get methyl alcohol 175ml, triethylamine 57ml, Paraformaldehyde 96 263g, glycine 31.3g, dimethylphosphite 54.5g, carry out the glyphosate synthesis reaction, add 130mi hydrochloric acid and carry out the glyphosate hydrolysis reaction, dealcoholysis slowly heats up, depickling, temperature rises to 120 ℃ of hydrolysis reaction and finishes, add suitable quantity of water and embodiment one gained raffinate, add after being cooled to 70 ℃ glyphosate reclaim triethylamine after alkaline mother liquor regulate ph value 0.7-1.0, continue cooling down crystallization filtration, get glyphosate wet-milling 94.06g, get former powder 72.35 g of glyphosate after the drying, glyphosate content 95.5%, glyphosate technicals yield are more than 77 %.

Claims (2)

1. an alkyl esterification method is produced the treatment process of the mother liquor of glyphosate, it is characterized in that: may further comprise the steps,

A. the mother liquor of getting alkyl esterification method production glyphosate and producing adds hydrochloric acid or sulphur acid for adjusting pH value to 0.1-1.5 in mother liquor;

B. add FeCI3 in the waste liquid after adjustment, add-on is the 1-5% of glyphosate mother solution quality, and the stirring that heats up produces flocculating settling, filters to isolate throw out; The intensification temperature is controlled at 60-80 ℃;

C. filtrate is concentrated through heating up, and isolates NaCI through cold filtration again, and raffinate is incorporated lower batch waste water into and processed or add glyphosate hydrolysis depickling workshop section and substitute process water.

2. alkyl esterification method according to claim 1 is produced the treatment process of the mother liquor of glyphosate, it is characterized in that: the described throw out that filters to isolate burns through incinerator and generates composite phosphate.