CN101746910B - PMIDA wastewater treatment method - Google Patents

Abstract

The invention discloses a PMIDA wastewater treatment method, wherein PMIDA wastewater washing, drying, press filtration, catalyst pretreatment, wet acetylene reaction and treatment of carbide slurry produced after the reaction are comprised. The method treats and sends the PMIDA wastewater produced in the condensation section reaction in a glyphosate production process to an acetylene section of a resin production line, takes the wastewater as wet acetylene production water, and simultaneously, adjusts an acetylene generation process, thereby realizing the recycling of water resource and the zero emission of the PMIDA wastewater, reducing the environment protection pressure, and meeting the national policies of energy saving and emission reduction.

Description

A kind of treatment process of N-(phosphonomethyl) iminodiacetic acid wastewater

Technical field

The present invention relates to a kind of processing method of industrial waste water, specifically is a kind of treatment process of N-(phosphonomethyl) iminodiacetic acid wastewater.

Background technology

Glyphosate 62 IPA Salt belongs to efficiently, the steriland herbicide of low toxicity, low residue, broad weed-killing spectrum, has become the output maximum, sales volume is maximum and fastest-rising pesticide species at present.The Glyphosate 62 IPA Salt synthetic route is more, and wherein diethylolamine-iminodiethanoic acid IDA method is because starting material and energy consumption is low, the present dominate of transformation efficiency advantages of higher.The synthetic Glyphosate IPA salt of IDA method is to be starting raw material preparation N-(the acyl group methyl of seeing) iminodiethanoic acid (being called for short two sweet seeing) earlier with diethylolamine, formaldehyde, phosphorus trichloride, reoxidizes and processes Glyphosate IPA salt.Can give off high density pH=0.6-1.0 strongly-acid N-(phosphonomethyl) iminodiacetic acid wastewater in Glyphosate IPA salt condensation workshop section rotary process; Contain high concentration organic phosphorus compound, 2-4% formaldehyde, organic amine, the saturated inorganic salt sodium-chlor of 18--22% etc. in the waste water, above-claimed cpd is biostats.N-(phosphonomethyl) iminodiacetic acid wastewater has characteristics such as quantity discharged is big, Pollutant levels are high, toxicity is big, saltiness is high, the difficult degradation compounds content high, difficulty of governance is big; The at present domestic green technology that generally adopts is difficult to administer this waste water, and therefore two sweet phosphorus waste water treatments are one of difficult problems of puzzlement imido oxalic acid explained hereafter Glyphosate IPA salt enterprise.

Summary of the invention

The invention provides a kind of treatment process of N-(phosphonomethyl) iminodiacetic acid wastewater; N-(phosphonomethyl) iminodiacetic acid wastewater in condensation workshop section reacted in the glyphosate production process is sent to production of resins line acetylene workshop section after treatment,, simultaneously acetylene generation technology is adjusted as wet method acetylene generation water; Realized the recycle of water resources; Accomplish the zero release of N-(phosphonomethyl) iminodiacetic acid wastewater, alleviated environmental protection pressure, met the national policy of energy-saving and emission-reduction.

Technical scheme of the present invention is:

A kind of treatment process of N-(phosphonomethyl) iminodiacetic acid wastewater; Diethylolamine-iminodiacetic acid (salt) acid system is produced Glyphosate IPA salt technology and is comprised dehydrogenation, condensation, three operations of redox; Diethylolamine generates two sweet phosphorus through dehydrogenation, acidifying, condensation, neutralization reaction; Wherein neutralization reaction is produced has two sweet phosphorus waste water, it is characterized in that:

(1), described N-(phosphonomethyl) iminodiacetic acid wastewater is put into whizzer through washing, drying, press filtration; Filtrating gets into the mother liquor settling bowl; Wherein add flocculation agent and remove impurity contained in the N-(phosphonomethyl) iminodiacetic acid wastewater, then with the supernatant in the mother liquor settling bowl through the mother liquor pump delivery in settling tank;

(2), be equipped with in the carbide-feed generator of calcium carbide, the calcium carbide reaction that in water, is hydrolyzed, the acetylene gas that reaction produces is overflowed from the producer top; When the carbide-feed generator temperature rises to 75-85 ℃; Open the flow spill valve of carbide-feed generator, make that water overflows in the carbide-feed generator, and in carbide-feed generator, add settling tank supernatant or water; Control the temperature of carbide-feed generator with amount of water, make temperature remain on 85-95 ℃;

(3), contain responseless calcium carbide in the dense slag slurry that produces of hydrolysis reaction, discharge by the bottom of carbide-feed generator; The shoddye slurry on dense slag slurry upper strata is discharged from the upflow tube at carbide-feed generator middle part, and shoddye is starched after the plate-and-frame filter press press filtration, and backwater gets in the settling tank, in settling tank, adds flocculation agent again to remove the solids in the said backwater; Supernatant composition in the said settling tank is a water, sends constantly in the carbide-feed generator as the reaction water.

The treatment process of described N-(phosphonomethyl) iminodiacetic acid wastewater is characterized in that: described flocculation agent is selected alum, polymerization aluminum chloride, Tai-Ace S 150 or ZX-I for use.

The invention has the beneficial effects as follows:

1. realize the resource circulation utilization, reduced production costs, reduced the environmental protection treatment expense, improved economic benefit.Production of resins line acetylene workshop section consumes 140 tons on calcium carbide every day, and calcium carbide hydrolysis per ton needs 4.55m ³Water, water consumption 637m altogether ³/ d, wherein about 420m ³Water is by reuse in rare carbide slag of producer discharge, and make up water is provided by the glyphosate production line.Condensation workshop section rotary process will produce N-(phosphonomethyl) iminodiacetic acid wastewater 210m every day in the glyphosate production process of 10000 tons of scales ³, can satisfy the water demand of acetylene workshop section, 2.4 * 210 * 330=166320 unit can save production cost every year.The at present domestic existing industrialization technology that can be used for handling N-(phosphonomethyl) iminodiacetic acid wastewater (partially disposed is removed COD), cost is at 32 yuan of/ton waste water.Can practice thrift every year and be used to handle waste water expenses of environmental protection 32 * 210 * 330=2217600 unit.

2. make enterprise production system wastewater zero discharge, alleviate environmental protection pressure.The N-(phosphonomethyl) iminodiacetic acid wastewater quantity discharged is big, toxicity is big, concentration is high, saltiness is high, the difficult degradation compounds content is high, causes that difficulty of governance is big, expense is high.The present invention with wastewater treatment after all recyclings not only economize on resources, and reduce the environmental protection treatment expense, solved the not tractable difficult problem of enterprise's N-(phosphonomethyl) iminodiacetic acid wastewater.

Description of drawings

Fig. 1 is a process flow sheet of the present invention.

Embodiment

The treatment process of N-(phosphonomethyl) iminodiacetic acid wastewater:

(1), with in the glyphosate production process in condensation workshop section and the N-(phosphonomethyl) iminodiacetic acid wastewater of still 1 internal reaction production put into whizzer 2 through washing, drying, press filtration; Get into the mother liquor settling bowl; Wherein add catalyzer and carry out pre-treatment, then with the supernatant in the mother liquor settling bowl 3 in mother liquor pump 4 is transported to settling tank 12;

(2), the hopper 5 that will fill calcium carbide puts into first hopper 6, behind nitrogen replacement, puts into two hoppers 7 through valve again; By hertz oscilltor calcium carbide is transported in the producer 8 then; Open the inlet valve of producer 8 then, the supernatant in the settling tank 12 is pumped in the producer, the calcium carbide reaction that in water, is hydrolyzed; The acetylene gas that reaction produces is overflowed from producer 8 tops, gets into next operation through mud separator 9;

(3), when producer 8 temperature rise to 75-85 ℃, open the flow spill valve and the priming valve door of producer 8, with the temperature that amount of water comes control generator, make temperature remain on 95-95 ℃;

(4), the dense slag slurry of hydrolysis reaction generation is discharged by the bottom of producer 8; The carbide slag slurries that hydrolysis reaction produces; Discharge from upflow tube 10; After plate-and-frame filter press 11 press filtrations, backwater gets into settling tank 12, carries out neutralization reaction with the N-(phosphonomethyl) iminodiacetic acid wastewater supernatant through catalyst pretreatment in the settling tank 12;

The supernatant that is pumped in the reactions step 2 in the settling tank 12 in the producer 8 is the supernatant that obtains through adding settling agent in the solution after the neutralization reaction by in settling tank 12.

Catalyzer is selected flocculation agent and alkaline matter for use.

Is settling agent selected for use?

Claims (1)

1. the treatment process of a N-(phosphonomethyl) iminodiacetic acid wastewater; Diethylolamine-iminodiacetic acid (salt) acid system is produced Glyphosate IPA salt technology and is comprised dehydrogenation, condensation, three operations of redox; Diethylolamine generates two sweet phosphorus through dehydrogenation, acidifying, condensation, neutralization reaction; Wherein neutralization reaction is produced has two sweet phosphorus waste water, it is characterized in that:

(1), described N-(phosphonomethyl) iminodiacetic acid wastewater is put into whizzer through washing, drying, press filtration; Filtrating gets into the mother liquor settling bowl; Wherein add flocculation agent and remove impurity contained in the N-(phosphonomethyl) iminodiacetic acid wastewater, then with the supernatant in the mother liquor settling bowl through the mother liquor pump delivery in settling tank;

(2), be equipped with in the carbide-feed generator of calcium carbide, the calcium carbide reaction that in water, is hydrolyzed, the acetylene gas that reaction produces is overflowed from the producer top; When the carbide-feed generator temperature rises to 75-85 ℃; Open the flow spill valve of carbide-feed generator, make that water overflows in the carbide-feed generator, and in carbide-feed generator, add settling tank supernatant or water; Control the temperature of carbide-feed generator with amount of water, make temperature remain on 85-95 ℃;

(3), contain responseless calcium carbide in the dense slag slurry that produces of hydrolysis reaction, discharge by the bottom of carbide-feed generator; The shoddye slurry on dense slag slurry upper strata is discharged from the upflow tube at carbide-feed generator middle part, and shoddye is starched after the plate-and-frame filter press press filtration, and backwater gets in the settling tank, in settling tank, adds flocculation agent again to remove the solids in the said backwater; Supernatant composition in the said settling tank is a water, sends constantly in the carbide-feed generator as the reaction water.

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