CN100554192C - Waste water treatment process in a kind of pmida98 preparation process - Google Patents
Waste water treatment process in a kind of pmida98 preparation process Download PDFInfo
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Abstract
The present invention relates to waste water treatment process in a kind of pmida98 preparation process, this method mainly is in the pmida98 preparation process, remove by filter filtrate behind the pmida98 crystal through pretreatment system, after the water inlet that reaches ultrafiltration apparatus requires, again according to the molecular structure of the components such as pmida98 of needs separating and concentrating in the mother liquor, molecular mass, particle size and electric charge, from big to small, select suitable ultra-filtration membrane, nanofiltration membrane is separated step by step with reverse osmosis membrane, and to carrying dense effective constituent pmida98, carrying pmida98 mother liquor after dense can mix through oxidation with the pmida98 solid and make glyphosate, isolated sodium chloride solution does not have other impurity substantially after film is handled, can be used as salt solution and be used for purposes such as chlorine industry or obtain solid sodium chloride through concentrating water.The invention has the beneficial effects as follows: this method has been handled the waste water that produces in the pmida98 preparation process very effectively, has reclaimed the pmida98 and the sodium-chlor of high value, and resource obtains recycling.
Description
Technical field
The present invention relates to a kind of waste water treatment process, mainly is waste water treatment process in a kind of pmida98 preparation process.
Background technology
N-(phosphonomethyl) oxalic acid (abbreviation pmida98) is the intermediate that the IDA legal system is equipped with glyphosate, and the formula of branch is
The existing technology of preparation glyphosate intermediate pmida98 mainly contains two: first diethanolamine method, produce Iminodiacetic acid sodium salt salt by the catalytic dehydrogenation in sodium hydroxide solution of diethanolamine, catalyzer, add then and under acidic conditions, react the production pmida98 with phosphorous acid, formaldehyde after hydrochloric acid returns acid, pmida98 is separated out in repeated hydrogenation sodium oxide PH=0.5～1.5 that neutralize, obtain the solid pmida98 after separating mother liquor, mother liquor is as wastewater treatment.It two is that iminodiacetonitrile is produced Iminodiacetic acid sodium salt salt through the sodium hydroxide alkaline hydrolysis, add then and under acidic conditions, react the production pmida98 with phosphorous acid, formaldehyde after hydrochloric acid returns acid, pmida98 is separated out in repeated hydrogenation sodium oxide PH=0.5～1.5 that neutralize, obtain the solid pmida98 after separating mother liquor, mother liquor is as wastewater treatment.Below which bar technology no matter all produces a large amount of acid waste water inevitably, contains 1.5%～3% pmida98 and 15%～20% sodium-chlor in this waste water, handles comparatively difficulty.
For above-mentioned waste water, many people have done the research of recycling.The patent of invention that application number is 01807900.8, publication number is CN1422275A is mentioned the method that the sodium-chlor in this waste water is reclaimed, but the pmida98 of high value does not obtain recycling.Application number for 200510060020.9, publication number provides the novel process of wastewater treatment in a kind of glyphosate synthetic intermediate pmida98 preparation process for the patent of invention of CN1837105A, this technology is to add bicarbonate of ammonia in waste water, fully reaction obtains sodium bicarbonate and ammonium chloride, this method also only is to have reclaimed sodium-chlor wherein, but also needs to add raw material.
Summary of the invention
Purpose of the present invention is just in order to overcome the deficiency of above-mentioned technology; and the pmida98 and the sodium-chlor that provide waste water treatment process in a kind of pmida98 preparation process, this technology can reclaim high value in the waste water, the residual solution after reclaiming can be used as the process water reuse; save resource greatly, protected environment.
The present invention solves the technical scheme that its technical problem adopts: waste water treatment process in a kind of pmida98 preparation process, and this technology mainly may further comprise the steps:
1), the pmida98 mother liquor is regulated PH=2～7 with sodium hydroxide or ammoniacal liquor, one or more devices that adopt pressure filter, bag type filtering machine, microfroc filter are removed wherein solids component with above-mentioned pmida98 mother liquor, remove viscous liquid in the mother liquor with the more medium filter that contains gac again, be that the micropore filtering film of 1～50 μ m is directly removed the micron particle in the mother liquor with the aperture then, above-mentioned pmida98 mother liquor is divided into two strands after ultra-filtration membrane separates, dense side solution returns raw liquid box, and light side enters secondary film system;
2), the pmida98 mother liquor solution that enters secondary film system is divided into two strands, the solution that dense side is rich in pmida98 returns the front end import, treat in the solution that pmida98 massfraction concentration reaches 5-12% when above, concentrated solution is squeezed into reservoir No. 1, light side solution enters three grades of film systems;
3), the light liquid of pmida98 that enters three grades of film systems is divided into two strands, dense side solution returns the import of secondary film system, the solution that light side is rich in sodium-chlor is collected in reservoir No. 2;
4), the concentrated solution in No. 1 reservoir mixes the glyphosate through oxidation system with pmida98 solid, deionized water; Solution in No. 2 reservoirs obtains solid sodium chloride as production or thickening that crude brine is used for chlor-alkali after film is handled, the water of deviating from is used for the FEOL water.
Contained salt comprises but not only comprises sodium-chlor in the pmida98 mother liquor of the present invention, and contained salt can be hydrochlorides such as sodium-chlor, ammonia chloride, sulfate of ammoniac, nitric acid ammonia, vitriol, and one or more in the nitrate, salts contg is more than 3%.
The deionized water that can in mother liquor or concentrated solution, add 1～4 times of volume in the membrane concentration sepn process of the present invention.
The combination of one or several that two, three grades of film systems of the present invention are nanofiltration and reverse osmosis membrane, working pressure is between 1-6MPa; Two, three grades of film systems also can adopt the rolling polyamide composite film, and its molecular weight cut-off is 50～500.
Nanofiltration membrane material of the present invention is polymeric amide, aromatic polyamides, polysulfones or polysulfones/aromatic polyamides composite membrane: described reverse osmosis membrane material is polymeric amide or aromatic polyamides.
Oxidation of the present invention can be hydrogen peroxide oxidation method, dioxygen oxidation method or air oxidation process.Described hydrogen peroxide oxidation method, be that the pmida98 concentrated solution is mixed with solid pmida98, deionized water, make catalyzer with sodium wolframate, hydrogen peroxide as oxidant, ferrous sulfate is made reductive agent, in carry out oxidizing reaction and reduction reaction under the normal pressure in reactor, with its synthesizing glyphosate, the mole proportioning of pmida98, pmida98 concentrated solution, hydrogen peroxide, ferrous sulfate is 1: 0.04～0.15: 1.20～2.0: 0.005～0.05.The mole proportion optimization of pmida98, pmida98 concentrated solution, hydrogen peroxide, ferrous sulfate is 1: 0.04～0.10: 1.35～1.65: 0.009～0.02.Described dioxygen oxidation method is that the pmida98 concentrated solution is mixed with solid pmida98, deionized water, and as catalyzer, oxygen makes glyphosate as oxygenant in carry out oxidizing reaction under 0.6Mpa～1.0Mpa in reactor with gac or palladium charcoal.
Thickening of the present invention, be that the solution in No. 2 reservoirs is divided into two strands earlier after nanofiltration membrane or reverse osmosis membrane separation, light side is collected in and is used for process water in the storage tank, dense side obtains sodium-chlor after evaporating economic benefits and social benefits thickener continuous concentration, the steam that steams is collected in after water cooling and is used for process water in the storage tank.
The invention has the beneficial effects as follows: the present invention all reclaims valuable ingredients pmida98 and sodium-chlor in the pmida98 mother liquor, and particularly pmida98 is made glyphosate after reclaiming, and value is further enhanced.After adopting art breading of the present invention, the production of pmida98 has reached wastewater zero discharge, and the effective constituent in the waste water obtains utilizing, and is a kind of typical waste water reclaiming processing scheme.
Embodiment
The present invention is further detailed explanation below in conjunction with drawings and Examples.
Embodiment 1:
The 10000kg mother liquor that produces in the preparation pmida98 process is joined in the reactor, regulate PH=2.0 with sodium hydroxide, the pmida98 mother liquor that regulates PH pumps in the raw liquid box after pressure filter or bag type filtering machine or microfroc filter press filtration, pmida98 mother liquor in the raw liquid box is squeezed into the more medium filter that contains gac with the pump of lift 20m with stock liquid and is removed viscous liquid in the mother liquor, via hole diameter is that the micropore filtering film of 50 μ m is directly removed the micron particle in the mother liquor again, after separating, ultra-filtration membrane is divided into two strands again, dense side liquid turns back to raw liquid box, and light side liquid enters secondary film system after the high-pressure pump pressurization.The pmida98 mother liquor solution that enters secondary film system is divided into two strands behind the secondary membrane sepn, the solution that dense side is rich in pmida98 returns the front end import, treat that pmida98 massfraction concentration reaches at 5% o'clock in the solution, concentrated solution is squeezed into reservoir No. 1,4000kg altogether, light side solution enter three grades of film systems after the high-pressure pump pressurization of 100m.The light liquid of pmida98 that enters three grades of film systems is divided into two strands behind three grades of membrane sepn, dense side solution returns the import of secondary nanofiltration membrane system, and the solution that light side is rich in sodium-chlor is collected in reservoir No. 2, altogether 6000kg.
Liquid 800kg in No. 1 reservoir is joined in the glassed steel reaction vessels, start and stir, add the 500kg deionized water successively, contain the pmida98 massfraction and be 90% solid 1110kg, sodium wolframate 3kg, mix, be warmed up to 60 ℃, 61 ± 2 ℃ of control reaction temperature, slowly add massfraction and be 28% hydrogen peroxide 720kg, finish insulation 0.5 hour, cool to 25 ℃ again and slowly add copperas solution 100kg, finish crystallisation by cooling, filter, it is 95% glyphosate products 610kg that the crystal oven dry obtains massfraction, the glyphosate massfraction is 3.8% filtrate 2500kg, make 10% gyphosate solution 940kg through concentrating, in the pmida98 that drops into, the glyphosate yield is 90.48%.
6000kg liquid in No. 2 reservoirs is obtained solution and the 1000kg water that 5000kg is rich in sodium-chlor behind membrane sepn.The crude brine that the solution that 5000kg is rich in sodium-chlor is directly used in chlor-alkali uses.
Embodiment 2:
Liquid 1000kg in No. 1 reservoir among the embodiment 1 is joined in the autoclave, open stirring, add 1500kg deionized water, 300kg massfraction more successively and be 90% pmida98,10kg activated-carbon catalyst, be warmed up to 60 ℃, aerating oxygen, 62 ± 2 ℃ of reaction temperature of control, reaction pressure 0.6Mpa reaction 2 hours, remove by filter catalyzer, the filtrate crystallisation by cooling, obtain massfraction after the oven dry of crystal that filtration obtains and be 96% glyphosate 190kg, filtrate 2600kg makes 10% gyphosate solution 200kg through concentrating.Yield in the pmida98 solid glyphosate that drops into is 99.75%.
Embodiment 3:
The 10000kg mother liquor that produces in the preparation pmida98 process is joined in the reactor, regulate PH=7.0 with sodium hydroxide, after press filtration, pump into raw liquid box, the more medium filter that contains gac squeezed into stock liquid by pump with lift 32m, to be that the millipore filtration membrane filtration of 20 μ m is laggard go into ultrafiltration to via hole diameter again, dense side liquid turns back to raw liquid box, and light side liquid enters secondary film system after the high-pressure pump pressurization.The pmida98 mother liquor solution that enters secondary film system is divided into two strands behind membrane sepn, the solution that dense side is rich in pmida98 returns the front end import, treat that pmida98 massfraction concentration reaches at 20% o'clock in the solution, concentrated solution is squeezed into reservoir No. 1,1000kg altogether, light side solution enter three grades of film systems after the high-pressure pump pressurization of 150m.The light liquid of pmida98 that enters three grades of film systems is divided into two strands behind membrane sepn, dense side solution returns the import of secondary film system, and the solution that light side is rich in sodium-chlor is collected in reservoir No. 2, altogether 9000kg.
Liquid 500kg in No. 1 reservoir is joined in the glassed steel reaction vessels, start and stir, add the 800kg deionized water successively, contain the pmida98 massfraction and be 90% solid 1110kg, sodium wolframate 3kg, mix, be warmed up to 70 ℃, 70 ± 2 ℃ of control reaction temperature, slowly add massfraction and be 28% hydrogen peroxide 880kg, finish insulation 2 hours, cool to 25 ℃ again and slowly add copperas solution 120kg, finish crystallisation by cooling, filter, it is 95% glyphosate products 640kg that the crystal oven dry obtains massfraction, the glyphosate massfraction is 3.8% filtrate 2480kg, make 10% gyphosate solution 930kg through concentrating, in the pmida98 that drops into, the glyphosate yield is 94.17%.
9000kg liquid in No. 2 reservoirs is obtained solution and the 4000kg water that 5000kg is rich in sodium-chlor after reverse osmosis membrane separation.The solution that 5000kg is rich in sodium-chlor obtains 1600kg sodium-chlor after stainless steel economic benefits and social benefits thickener concentrates, sell as the raw material of chlor-alkali the oven dry back.
Embodiment 4:
The 10000kg mother liquor that produces in the preparation pmida98 process is joined in the reactor, regulate PH=4.0 with sodium hydroxide, after press filtration, pump into raw liquid box, the more medium filter that contains gac squeezed into stock liquid by pump with lift 50M, to be that the millipore filtration membrane filtration of 1 μ m is laggard go into ultrafiltration to via hole diameter again, dense side liquid turns back to raw liquid box, and light side liquid enters secondary film system after the high-pressure pump pressurization.The pmida98 mother liquor solution that enters secondary film system is divided into two strands behind nanofiltration membrane separation, the solution that dense side is rich in pmida98 returns the front end import, treat that pmida98 massfraction concentration reaches at 12% o'clock in the solution, concentrated solution is squeezed into reservoir No. 1,1600kg altogether, light side solution enter three grades of film systems after the high-pressure pump pressurization of 300m.The light liquid of pmida98 that enters three grades of film systems is divided into two strands after reverse osmosis membrane separation, dense side solution returns the import of secondary nanofiltration membrane system, and the solution that light side is rich in sodium-chlor is collected in reservoir No. 2, altogether 8400kg.
Liquid 600kg in No. 1 reservoir is joined in the glassed steel reaction vessels, start and stir, add the 700kg deionized water successively, contain the pmida98 massfraction and be 90% solid 1110kg, sodium wolframate 3kg, mix, be warmed up to 80 ℃, 78 ± 2 ℃ of control reaction temperature, slowly add massfraction and be 28% hydrogen peroxide 800kg, finish insulation 1 hour, cool to 25 ℃ again and slowly add copperas solution 110kg, finish crystallisation by cooling, filter, it is 95.2% glyphosate products 620kg that the crystal oven dry obtains massfraction, the glyphosate massfraction is 3.8% filtrate 2450kg, make 10% gyphosate solution 925kg through concentrating, in the pmida98 that drops into, the glyphosate yield is 91.72%.
8400kg liquid in No. 2 reservoirs is obtained solution and the 3400kg water that 5000kg is rich in sodium-chlor after reverse osmosis membrane separation.The solution that 5000kg is rich in sodium-chlor obtains 1600kg sodium-chlor after stainless steel economic benefits and social benefits thickener concentrates, sell as the raw material of chlor-alkali the oven dry back.
Embodiment 5:
Liquid 200kg in No. 1 reservoir among the embodiment 3 is joined in the autoclave, open stirring, add 2300kg deionized water, 300kg massfraction more successively and be 90% pmida98,10kg activated-carbon catalyst, be warmed up to 95 ℃, aerating oxygen, 93 ± 2 ℃ of reaction temperature of control, reaction pressure 0.9Mpa reaction 1 hour, remove by filter catalyzer, the filtrate crystallisation by cooling, obtain massfraction after the oven dry of crystal that filtration obtains and be 96.5% glyphosate 185kg, filtrate 2600kg makes 10% gyphosate solution 198kg through concentrating.Yield in the pmida98 solid glyphosate that drops into is 98.67%.
Embodiment 6:
Liquid 500kg in No. 1 reservoir among the embodiment 4 is joined in the autoclave, open stirring, add 2000kg deionized water, 300kg massfraction more successively and be 90% pmida98,10kg palladium carbon catalyst, be warmed up to 70 ℃, aerating oxygen, 70 ± 2 ℃ of reaction temperature of control, reaction pressure 0.8Mpa reaction 8 hours, remove by filter catalyzer, the filtrate crystallisation by cooling, obtain massfraction after the oven dry of crystal that filtration obtains and be 97% glyphosate 186kg, filtrate 2570kg makes 10% gyphosate solution 190kg through concentrating.Yield in the pmida98 solid glyphosate that drops into is 99.21%.
Claims (9)
1, waste water treatment process in a kind of pmida98 preparation process, it is characterized in that: this technology mainly may further comprise the steps:
1), the pmida98 mother liquor is regulated pH=2～7 with sodium hydroxide or ammoniacal liquor, above-mentioned pmida98 mother liquor is removed wherein solids component, remove viscous liquid in the pmida98 mother liquor with the more medium filter that contains gac again, be that the micropore filtering film of 1～50 μ m is directly removed the micron particle in the pmida98 mother liquor with the aperture then, above-mentioned pmida98 mother liquor is divided into two strands after ultra-filtration membrane separates, dense side solution returns raw liquid box, and light side enters secondary film system;
2), the pmida98 mother liquor solution that enters secondary film system is divided into two strands, the solution that dense side is rich in pmida98 returns the front end import, treat in the solution that pmida98 massfraction concentration reaches 5-12% when above, concentrated solution is squeezed into reservoir No. 1, light side solution enters three grades of film systems;
3), the light liquid of pmida98 that enters three grades of film systems is divided into two strands, dense side solution returns the import of secondary film system, the solution that light side is rich in sodium-chlor is collected in reservoir No. 2;
4), the concentrated solution in No. 1 reservoir mixes through oxidation with pmida98 solid and deionized water and makes glyphosate; Solution in No. 2 reservoirs obtains solid sodium chloride as production or thickening that crude brine is used for chlor-alkali after film is handled, the water of deviating from is used for the FEOL water.
2, waste water treatment process in the pmida98 preparation process according to claim 1 is characterized in that: the combination of one or several that described two, three grades of film systems are nanofiltration and reverse osmosis membrane, working pressure is between 1-6MPa.
3. waste water treatment process in the pmida98 preparation process according to claim 2, it is characterized in that: described nanofiltration membrane material is polymeric amide, aromatic polyamides, polysulfones or polysulfones/aromatic polyamides composite membrane, and described reverse osmosis membrane material is polymeric amide or aromatic polyamides.
4. waste water treatment process in the pmida98 preparation process according to claim 1 is characterized in that: described two, three grades of film systems, adopt the rolling polyamide composite film, and its molecular weight cut-off is 50～500.
5. waste water treatment process in the pmida98 preparation process according to claim 1 is characterized in that: described oxidation is hydrogen peroxide oxidation method, dioxygen oxidation method or air oxidation process.
6. waste water treatment process in the pmida98 preparation process according to claim 5, it is characterized in that: described hydrogen peroxide oxidation method, be that the pmida98 concentrated solution is mixed with solid pmida98 and deionized water, make catalyzer with sodium wolframate, hydrogen peroxide as oxidant, ferrous sulfate is made reductive agent, in in reactor, carrying out oxidizing reaction and reduction reaction under the normal pressure, with its synthesizing glyphosate, the mole proportioning of pmida98, pmida98 concentrated solution, hydrogen peroxide, ferrous sulfate is 1: 0.04～0.15: 1.20～2.0: 0.005～0.05.
7, waste water treatment process in the pmida98 preparation process according to claim 6, it is characterized in that: described hydrogen peroxide oxidation method, the mole proportioning of pmida98, pmida98 concentrated solution, hydrogen peroxide, ferrous sulfate is 1: 0.04～0.10: 1.35～1.65: 0.009～0.02.
8, waste water treatment process in the pmida98 preparation process according to claim 5, it is characterized in that: described dioxygen oxidation method, be that the pmida98 concentrated solution is mixed with solid pmida98 and deionized water, with gac or palladium charcoal as catalyzer, oxygen makes glyphosate as oxygenant in carry out oxidizing reaction under 0.6Mpa～1.0Mpa in reactor.
9, waste water treatment process in the pmida98 preparation process according to claim 1, it is characterized in that: described thickening, be that the solution in No. 2 reservoirs is divided into two strands earlier after nanofiltration membrane or reverse osmosis membrane separation, light side is collected in and is used for process water in the storage tank, dense side obtains sodium-chlor after evaporating economic benefits and social benefits thickener continuous concentration, the steam that steams is collected in after water cooling and is used for process water in the storage tank.
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Denomination of invention: A wastewater treatment process in the preparation of glyphosate Effective date of registration: 20220630 Granted publication date: 20091028 Pledgee: Hangzhou Qingchun sub branch of Guangfa Bank Co.,Ltd. Pledgor: HANGZHOU TIAN CHUANG ENVIRONMENTAL TECHNOLOGY Co.,Ltd. Registration number: Y2022330001189 |
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Date of cancellation: 20230629 Granted publication date: 20091028 Pledgee: Hangzhou Qingchun sub branch of Guangfa Bank Co.,Ltd. Pledgor: HANGZHOU TIAN CHUANG ENVIRONMENTAL TECHNOLOGY Co.,Ltd.|Zhejiang Yimo New Material Technology Co.,Ltd. Registration number: Y2022330001189 |