CN109796494B - A method of recycling L-fosfomycin dextrorotation phenyl ethylamine salt industrial Phosphorus From Wastewater resource and organic matter - Google Patents
A method of recycling L-fosfomycin dextrorotation phenyl ethylamine salt industrial Phosphorus From Wastewater resource and organic matter Download PDFInfo
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- CN109796494B CN109796494B CN201910268560.8A CN201910268560A CN109796494B CN 109796494 B CN109796494 B CN 109796494B CN 201910268560 A CN201910268560 A CN 201910268560A CN 109796494 B CN109796494 B CN 109796494B
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- 238000000034 method Methods 0.000 title claims abstract description 22
- 150000007925 phenylethylamine derivatives Chemical class 0.000 title claims abstract description 20
- 229960000308 fosfomycin Drugs 0.000 title claims abstract description 19
- 238000004064 recycling Methods 0.000 title claims abstract description 13
- 239000002351 wastewater Substances 0.000 title claims abstract description 12
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 11
- 239000011574 phosphorus Substances 0.000 title claims abstract description 8
- 229910052698 phosphorus Inorganic materials 0.000 title claims abstract description 8
- 239000005416 organic matter Substances 0.000 title claims abstract description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 27
- YMDXZJFXQJVXBF-STHAYSLISA-N fosfomycin Chemical compound C[C@@H]1O[C@@H]1P(O)(O)=O YMDXZJFXQJVXBF-STHAYSLISA-N 0.000 claims abstract description 15
- 238000001914 filtration Methods 0.000 claims abstract description 11
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000011575 calcium Substances 0.000 claims abstract description 9
- 239000010842 industrial wastewater Substances 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims description 18
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- 239000000725 suspension Substances 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- YMZJBJPWTXJQMR-MUWMCQJSSA-L calcium;[(2s,3r)-3-methyloxiran-2-yl]-dioxido-oxo-$l^{5}-phosphane Chemical compound [Ca+2].C[C@H]1O[C@H]1P([O-])([O-])=O YMZJBJPWTXJQMR-MUWMCQJSSA-L 0.000 claims description 9
- 239000012074 organic phase Substances 0.000 claims description 8
- 239000012071 phase Substances 0.000 claims description 8
- 230000002378 acidificating effect Effects 0.000 claims description 6
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- 238000006460 hydrolysis reaction Methods 0.000 claims description 6
- 230000003647 oxidation Effects 0.000 claims description 6
- 238000007254 oxidation reaction Methods 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 6
- HHVPUBYDASYGFG-UHFFFAOYSA-N CC1=CC=CC=C1.C(C)NC1=CC=CC=C1 Chemical group CC1=CC=CC=C1.C(C)NC1=CC=CC=C1 HHVPUBYDASYGFG-UHFFFAOYSA-N 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical group [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims description 4
- 159000000007 calcium salts Chemical class 0.000 claims description 4
- 230000000694 effects Effects 0.000 claims description 4
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- 229940078494 nickel acetate Drugs 0.000 claims description 4
- 239000003054 catalyst Substances 0.000 claims description 3
- 230000006835 compression Effects 0.000 claims description 3
- 238000007906 compression Methods 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 claims description 3
- 238000001556 precipitation Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 238000006555 catalytic reaction Methods 0.000 claims description 2
- 239000003153 chemical reaction reagent Substances 0.000 claims description 2
- XMOKRCSXICGIDD-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O XMOKRCSXICGIDD-UHFFFAOYSA-N 0.000 claims 1
- 238000009938 salting Methods 0.000 claims 1
- 239000000243 solution Substances 0.000 abstract description 25
- BHHGXPLMPWCGHP-UHFFFAOYSA-N Phenethylamine Chemical compound NCCC1=CC=CC=C1 BHHGXPLMPWCGHP-UHFFFAOYSA-N 0.000 abstract description 7
- 229910017053 inorganic salt Inorganic materials 0.000 abstract description 7
- 239000012266 salt solution Substances 0.000 abstract description 7
- 230000001681 protective effect Effects 0.000 abstract description 3
- 230000003287 optical effect Effects 0.000 abstract description 2
- 238000010525 oxidative degradation reaction Methods 0.000 abstract description 2
- 229910000391 tricalcium phosphate Inorganic materials 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 7
- 238000011084 recovery Methods 0.000 description 7
- 229910001220 stainless steel Inorganic materials 0.000 description 6
- 239000010935 stainless steel Substances 0.000 description 6
- 239000002699 waste material Substances 0.000 description 6
- 150000003839 salts Chemical class 0.000 description 5
- 238000004065 wastewater treatment Methods 0.000 description 5
- 241000894006 Bacteria Species 0.000 description 4
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- 238000004519 manufacturing process Methods 0.000 description 4
- 239000003960 organic solvent Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 239000001506 calcium phosphate Substances 0.000 description 3
- 229910000389 calcium phosphate Inorganic materials 0.000 description 3
- 235000011010 calcium phosphates Nutrition 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 230000000844 anti-bacterial effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- -1 fosfomycin phenylethylamines Chemical class 0.000 description 2
- 239000010985 leather Substances 0.000 description 2
- 239000012452 mother liquor Substances 0.000 description 2
- GNMQOUGYKPVJRR-UHFFFAOYSA-N nickel(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ni+3].[Ni+3] GNMQOUGYKPVJRR-UHFFFAOYSA-N 0.000 description 2
- 238000012797 qualification Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 206010067484 Adverse reaction Diseases 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 108090000204 Dipeptidase 1 Proteins 0.000 description 1
- 241000194033 Enterococcus Species 0.000 description 1
- RJQXTJLFIWVMTO-TYNCELHUSA-N Methicillin Chemical compound COC1=CC=CC(OC)=C1C(=O)N[C@@H]1C(=O)N2[C@@H](C(O)=O)C(C)(C)S[C@@H]21 RJQXTJLFIWVMTO-TYNCELHUSA-N 0.000 description 1
- 241000607142 Salmonella Species 0.000 description 1
- 239000005708 Sodium hypochlorite Substances 0.000 description 1
- 241000191967 Staphylococcus aureus Species 0.000 description 1
- 108010059993 Vancomycin Proteins 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 230000006838 adverse reaction Effects 0.000 description 1
- 229940126575 aminoglycoside Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 102000006635 beta-lactamase Human genes 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 229940041011 carbapenems Drugs 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000012531 culture fluid Substances 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- DZPRNEDIQAHKCV-UHFFFAOYSA-N ethanamine N-ethylaniline Chemical compound CCN.CCNC1=CC=CC=C1 DZPRNEDIQAHKCV-UHFFFAOYSA-N 0.000 description 1
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- 229960003165 vancomycin Drugs 0.000 description 1
- MYPYJXKWCTUITO-UHFFFAOYSA-N vancomycin Natural products O1C(C(=C2)Cl)=CC=C2C(O)C(C(NC(C2=CC(O)=CC(O)=C2C=2C(O)=CC=C3C=2)C(O)=O)=O)NC(=O)C3NC(=O)C2NC(=O)C(CC(N)=O)NC(=O)C(NC(=O)C(CC(C)C)NC)C(O)C(C=C3Cl)=CC=C3OC3=CC2=CC1=C3OC1OC(CO)C(O)C(O)C1OC1CC(C)(N)C(O)C(C)O1 MYPYJXKWCTUITO-UHFFFAOYSA-N 0.000 description 1
- MYPYJXKWCTUITO-LYRMYLQWSA-O vancomycin(1+) Chemical compound O([C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC1=C2C=C3C=C1OC1=CC=C(C=C1Cl)[C@@H](O)[C@H](C(N[C@@H](CC(N)=O)C(=O)N[C@H]3C(=O)N[C@H]1C(=O)N[C@H](C(N[C@@H](C3=CC(O)=CC(O)=C3C=3C(O)=CC=C1C=3)C([O-])=O)=O)[C@H](O)C1=CC=C(C(=C1)Cl)O2)=O)NC(=O)[C@@H](CC(C)C)[NH2+]C)[C@H]1C[C@](C)([NH3+])[C@H](O)[C@H](C)O1 MYPYJXKWCTUITO-LYRMYLQWSA-O 0.000 description 1
- 150000003952 β-lactams Chemical class 0.000 description 1
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- Removal Of Specific Substances (AREA)
Abstract
The invention discloses a kind of methods for recycling L-fosfomycin dextrorotation phenyl ethylamine salt industrial Phosphorus From Wastewater resource and organic matter, by the way that saturation Ca (OH) is added into industrial wastewater2Two kinds of main optical isomers are hydrolyzed to fosfomycin calcium and phenyl ethylamine, extract phenyl ethylamine using toluene and recycle by solution, and filtering gained fosfomycin calcium is using NaClO oxidative degradation at Ca3(PO4)2It recycles, treated, and waste water is inorganic salt solution.This method is environmentally protective, safe and simple, can effectively recycle phosphor resource and organic matter in L-fosfomycin dextrorotation phenyl ethylamine salt industrial waste water.
Description
Technical field
The present invention relates to a kind of sides for recycling L-fosfomycin dextrorotation phenyl ethylamine salt industrial Phosphorus From Wastewater resource and organic matter
Method belongs to sewage treatment and resource technology field.
Background technique
Phosphonomycin starts after 1969 are found from unwrapping wire bacteria culture fluid in EU market list marketing for 1973,
So far have more than 40 years usage histories.Modern study studies have shown that phosphonomycin is to a variety of Gram-positives (G+) bacterium and leather
Lan Shi feminine gender (G-) bacterium bag includes part drug-fast bacteria, and the leather such as methicillin-resistant staphylococcus aureus, wide spectrum beta-lactamase is blue
Salmonella, Vancomycin-resistant Enterococcus etc. all remain higher antibacterial activity.Because of its mechanism of action uniqueness, with beta-lactam
The combination of the antibiotic such as class, fluoroquinolones, aminoglycoside and Carbapenems has synergistic effect, while also having adverse reaction
Less, the advantages that tolerance is good, cheap, concern of the phosphonomycin series of products increasingly by market.
The various phosphonomycin salt of listing have been achieved with fully synthetic production, and L-fosfomycin dextrorotation phenyl ethylamine salt is as important
Intermediate, synthesis and the resolution process for the intermediate are directed in many patents, the especially product was synthesizing
Cheng Zhong is generated with racemate form.Due to the left-handed benzene of optical isomer dextrorotation phosphonomycin of L-fosfomycin dextrorotation phenyl ethylamine
Ethylamine salt does not have antibacterial activity, and China pharmacy worker is groping always the method for making full use of the product, such as CN
The patents such as 101928301B and CN 103113408B are converted by the configuration to active substance, improve the acquisition of active constituent
Rate.Separation means mainly carry out fractionation preparation using the deliquescent difference of compound of two kinds of configurations.With recrystallization number
Increase, various impurity enricheds cause to discard in mother liquor, and there are the fosfomycin phenylethylamines of two kinds of configurations in remaining waste liquid
Salt and organic solvent, the cost further split completely is excessively high, without commercial value, is not suitable for industrialized production.
For the waste mother liquor generated in production process, wherein the L-fosfomycin dextrorotation containing the active effect in part
Phenyl ethylamine salt and organic solvent, direct emission can cause environmental pollution, while waste of resources is caused.Traditional recycling and place
Reason method can recycle fractions, and the utilization rate of resource has further improved space.Common oxidation degradation method
Raw material H2O2Solvent usage is big, and condition of storage is stringent, degradable during storage, and there are biggish security risks.This product city
Gradually expanding for field demand needs us to develop a kind of environmentally protective, safe and simple, high financial profit phosphorus for industrial wastewater
Resource and organic compounds recovery method.
The present invention uses calcium hydroxide and sodium hypochlorite stepwise degradation, makes phosphonomycin Precipitation in the form of calcium salt, and
Oxidative degradation is at Phos in a manner of relatively mild, while the phenyl ethylamine for recycling organic solvent layer recycles, and realizes resource
Sustainable use, while reducing and using a large amount of H2O2Existing security risk is aoxidized, the waste of large-scale industrial production is suitble to
Environmental protection treatment.
Summary of the invention
The purpose of the present invention is to provide a kind of recycling L-fosfomycin dextrorotation phenyl ethylamine salt industrial Phosphorus From Wastewater resource and
The method of organic matter.The technology can be for phosphor resource and organic in the waste that production L-fosfomycin dextrorotation phenyl ethylamine salt generates
The sustainable of object recycles, and reduces environmental pollution, and improves the overall economic efficiency of product.
In order to achieve the above object, the present invention the following steps are included:
(1) hydrolysis: under the conditions of 30-45 DEG C of temperature, to filtered L-fosfomycin dextrorotation phenyl ethylamine salt industrial
Saturation Ca (OH) is slowly added in waste water2Solution adjusts pH value to 8-9.Make the left side in industrial wastewater by electric stirring effect
Revolve phosphonomycin dextrorotation phenyl ethylamine salt, the left-handed phenyl ethylamine salt of dextrorotation phosphonomycin and Ca (OH)2It sufficiently reacts, slowly adds in whipping process
Enter toluene, sufficiently reaction is to without more Precipitations.
(2) be separated by filtration: under the conditions of 20-40 DEG C of temperature, the suspension that step 1 is obtained is filtered, and obtains being precipitated as phosphorus
Mycin calcium salt.It is layered after filtered solution left standstill, separates water phase and organic phase, organic phase is phenyl ethylamine toluene solution, water phase
For inorganic salt solution.
(3) catalysis oxidation: the phosphonomycin calcium salt that step 2 is obtained is water-dispersible, under the conditions of 20-40 DEG C of temperature, to mixed
The NaClO solution for containing a small amount of catalyst is added in suspension, is generated after keeping fosfomycin calcium fully oxidized by electric stirring effect
Ca3(PO4)2Precipitating adjusts PH weakly acidic pH, is separated by filtration precipitated product.
Wherein, the reagent for adjusting pH value is hydrochloric acid and sodium hydroxide, and solution concentration is 0.5mol/L.
Electric stirring revolving speed described in step (1) is 40-60rpm, reaction time 2-3h.Toluene solvant additional amount is suitable
In the 20-30% of processing waste water total amount, the solvent or fresh solvent that can be recycled with recycling phenyl ethylamine.
Plate compression or centrifugal rejection filter can be selected in filter type described in step (2).
The water for dispersing phosphonomycin calcium salt described in step (3) is pure water, and water consumption is the 8-10 of handled calcium salt weight in wet base
Times.Nickel acetate, nickel sesquioxide or iron oxide and its compound can be selected in catalyst.The NaClO solution concentration of addition is 1-
1.5mol/L, additional amount 2-5L/L.Electric stirring revolving speed is 40-60rpm, reaction time 3-5h.Filter type can be selected
Plate compression or centrifugal rejection filter.
The beneficial effects of the present invention are:
1, improvement is optimized to the Industrial Wastewater Treatment prevention of L-fosfomycin dextrorotation phenyl ethylamine salt in the present invention, with biography
System technology is compared, the technology recycling phenyl ethylamine solution can synthesis L-fosfomycin dextrorotation phenyl ethylamine salt in repetitive cycling benefit
With degradation gained calcium phosphate can be used as the raw material of replenish the calcium drug or food, or use as controlled availability fertilizer, take full advantage of work
Phosphor resource and organic matter in industry waste water improve the product economy added value of waste.
2, organic solvent used in the present invention can be recycled, the waste water of generation, mainly based on harmless inorganic salt solution, into
One step handles qualified discharge, and cost is relatively low, and treatment process is more environmentally protective.
3, with tradition H2O2Oxidizing process is compared, and the extent of reaction of oxidation process is easier to control, and safety is higher.
Combined with specific embodiments below, the present invention is furture elucidated, it should be appreciated that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In the following examples, the experimental methods for specific conditions are not specified, usually according to conventional strip
Condition proposed by part or manufacturer.
Specific embodiment
According to following embodiments, the present invention may be better understood.However, content described in embodiment is merely to illustrate
The present invention, without the present invention described in detail in claims should will not be limited.
Embodiment 1:
(1) the hydrolysis stage: L-fosfomycin dextrorotation phenyl ethylamine salt industrial waste water 10L is taken, plate and frame filter press mistake is used
It after filter, is placed in 50L stainless steel cauldron, adjusting temperature of reaction kettle is 35 DEG C.Adjusting electric stirring paddle revolving speed is 45rpm, to
Saturation Ca (OH) is slowly added in reaction kettle2Solution, adjusts pH value to 8.2, at this time solution total amount about 18L.4L is slowly added to return
Toluene solution after receipts, is persistently stirred to react 3h.
(2) be separated by filtration the stage: stirring suspension is cooled to room temperature 22 DEG C, will be obtained after hydrolysis using centrifugal drying filter
Suspension filtering, rejection filter machine revolving speed 2500rpm obtain 0.66kg phosphonomycin calcium salt.Filtered solution is placed in stainless steel reaction
1.5h is stood in kettle, after solution layering, obtains 15.8L water phase and 3.8L organic phase respectively, organic phase is that phenyl ethylamine toluene is molten
Synthetic reaction use is done in liquid, recycling, and water phase is inorganic salt solution, after adjusting pH value weakly acidic pH with 0.5mol/L hydrochloric acid, according to nothing
It is discharged after machine salt wastewater treatment is qualified.The phosphonomycin rate of recovery 72.3%, the phenyl ethylamine rate of recovery 73.1%.
(3) catalytic oxidation stage: the phosphonomycin calcium salt 0.5kg for taking previous step to be obtained by filtration adds the pure water dispersion of 4L, is placed in
In 50L stainless steel cauldron, adjusting temperature of reaction kettle is 35 DEG C.Adjusting electric stirring paddle revolving speed is 50rpm, is added into suspension
Enter 50g nickel acetate, the NaClO solution of 1mol/L is slowly added into reaction kettle, 2h is added NaClO solution 15L, continues to stir
2h, adjusts PH weakly acidic pH using the NaOH solution of 0.5mol/L, is filtered the suspension obtained after reaction using centrifugal drying filter,
Rejection filter machine revolving speed 2500rpm, obtains 0.193kg calcium phosphate.Filtrate is inorganic salt solution, after inorganic salts wastewater treatment qualification
Discharge.The P elements rate of recovery 72.5%.
Embodiment 2:
(1) the hydrolysis stage: L-fosfomycin dextrorotation phenyl ethylamine salt industrial waste water 10L is taken, plate and frame filter press mistake is used
It after filter, is placed in 50L stainless steel cauldron, adjusting temperature of reaction kettle is 40 DEG C.Adjusting electric stirring paddle revolving speed is 50rpm, to
Saturation Ca (OH) is slowly added in reaction kettle2Solution, adjusts pH value to 8.6, at this time solution total amount about 20L.5L is slowly added to return
Toluene solution after receipts, is persistently stirred to react 3h.
(2) be separated by filtration the stage: stirring suspension is cooled to room temperature 25 DEG C, will be obtained after hydrolysis using centrifugal drying filter
Suspension filtering, rejection filter machine revolving speed 3000rpm obtain 0.85kg phosphonomycin calcium salt.Filtered solution is placed in stainless steel reaction
1h is stood in kettle, after solution layering, obtains 17.7L water phase and 4.7L organic phase respectively, organic phase is phenyl ethylamine toluene solution,
Synthetic reaction use is done in recycling, and water phase is inorganic salt solution, after adjusting pH value weakly acidic pH with 0.5mol/L hydrochloric acid, according to inorganic salts
It is discharged after wastewater treatment is qualified.The phosphonomycin rate of recovery 92.8%, the phenyl ethylamine rate of recovery 93.7%.
(3) catalytic oxidation stage: the phosphonomycin calcium salt 0.5kg for taking previous step to be obtained by filtration adds the pure water dispersion of 5L, is placed in
In 50L stainless steel cauldron, adjusting temperature of reaction kettle is 30 DEG C.Adjusting electric stirring paddle revolving speed is 55rpm, is added into suspension
Enter 50g nickel acetate, the NaClO solution of 1mol/L is slowly added into reaction kettle, 2h is added NaClO solution 22L, continues to stir
2h, adjusts PH weakly acidic pH using the NaOH solution of 0.5mol/L, is filtered the suspension obtained after reaction using centrifugal drying filter,
Rejection filter machine revolving speed 3000rpm, obtains 0.251kg calcium phosphate.Filtrate is inorganic salt solution, after inorganic salts wastewater treatment qualification
Discharge.The P elements rate of recovery 94.4%.
Claims (5)
1. a kind of method for recycling L-fosfomycin dextrorotation phenyl ethylamine salt industrial Phosphorus From Wastewater resource and organic matter, feature exist
In, comprising the following steps:
Hydrolysis: under the conditions of 30-45 DEG C of temperature, delay into filtered L-fosfomycin dextrorotation phenyl ethylamine salt industrial waste water
It is slow that saturation Ca (OH) is added2Solution is adjustedpH value is to 8-9；Make the L-fosfomycin in industrial wastewater by electric stirring effect
The left-handed phenyl ethylamine salt of dextrorotation phenyl ethylamine salt, dextrorotation phosphonomycin and Ca (OH)2It sufficiently reacts, is slowly added to toluene in whipping process,
Sufficiently reaction is to without more Precipitations；
Be separated by filtration: under the conditions of 20-40 DEG C of temperature, the suspension that step (1) is obtained is filtered, and obtains being precipitated as fosfomycin calcium
Salt；It is layered after filtered solution left standstill, separates water phase and organic phase, organic phase is phenyl ethylamine toluene solution, and water phase is inorganic
Salting liquid；
Catalysis oxidation: the phosphonomycin calcium salt that step (2) is obtained is water-dispersible, under the conditions of 20-40 DEG C of temperature, into suspension
The NaClO solution containing proper amount of acetic acid nickel is added, generates Ca after keeping fosfomycin calcium fully oxidized by electric stirring effect3
(PO4)2Precipitating is adjustedpH weakly acidic pH, is separated by filtration precipitated product.
2. the method according to claim 1, wherein for adjustingpThe reagent of H value is that hydrochloric acid or sodium hydroxide are molten
The concentration of liquid, hydrochloric acid or sodium hydroxide solution is 0.5mol/L.
3. the method according to claim 1, wherein electric stirring revolving speed is 40-60rpm, reaction in step (1)
Time is 2-3h；Toluene solvant additional amount is equivalent to the 20-30% of processing waste water total amount, with the recycling phenyl ethylamine toluene solution
Obtained toluene or fresh toluene.
4. the method according to claim 1, wherein filter type is plate compression or centrifugal drying in step (2)
Filter.
5. the method according to claim 1, wherein step (3) in dispersion phosphonomycin calcium salt water be pure water,
Water consumption is 8-10 times of handled calcium salt weight in wet base；Catalyst is nickel acetate, and the concentration of NaClO is 1- in NaClO solution
1.5mol/L, additional amount 2-5L/L；Electric stirring revolving speed is 40-60rpm, reaction time 3-5h；Filter type is sheet frame
Filters pressing or centrifugal rejection filter.
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| CN201910268560.8A CN109796494B (en) | 2019-04-03 | 2019-04-03 | A method of recycling L-fosfomycin dextrorotation phenyl ethylamine salt industrial Phosphorus From Wastewater resource and organic matter |
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| CN201910268560.8A CN109796494B (en) | 2019-04-03 | 2019-04-03 | A method of recycling L-fosfomycin dextrorotation phenyl ethylamine salt industrial Phosphorus From Wastewater resource and organic matter |
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| CN109796494B true CN109796494B (en) | 2019-09-13 |
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Effective date of registration: 20231023 Address after: Rooms 1503 and 1504, 15th floor, Building F, Life Science Park, No. 22 Tiansheng Road, Jiangbei New District, Nanjing, Jiangsu Province, 210000 Patentee after: Nanjing Dao'er Medical Research Institute Co.,Ltd. Address before: No. 21 Huashen Avenue, Yuhuatai District, Nanjing City, Jiangsu Province, 210000 (first floor of Dexun Technology Company) Patentee before: NANJING DARRA PHARMACEUTICAL TECHNOLOGY Co.,Ltd. |