CN110395747A - The method of Hydrolysis kinetics sylvite from cefixime side chain production waste water - Google Patents
The method of Hydrolysis kinetics sylvite from cefixime side chain production waste water Download PDFInfo
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- CN110395747A CN110395747A CN201910516140.7A CN201910516140A CN110395747A CN 110395747 A CN110395747 A CN 110395747A CN 201910516140 A CN201910516140 A CN 201910516140A CN 110395747 A CN110395747 A CN 110395747A
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- waste water
- sylvite
- side chain
- chain production
- production waste
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/14—Purification
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/048—Purification of waste water by evaporation
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
- F23G—CREMATION FURNACES; CONSUMING WASTE PRODUCTS BY COMBUSTION
- F23G7/00—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals
- F23G7/04—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste liquors, e.g. sulfite liquors
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/343—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the pharmaceutical industry, e.g. containing antibiotics
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- Hydrology & Water Resources (AREA)
- Life Sciences & Earth Sciences (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Water Supply & Treatment (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Processing Of Solid Wastes (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The present invention relates to technical field of waste water processing, and in particular to a method of the Hydrolysis kinetics sylvite from cefixime side chain production waste water.Cefixime side chain production waste water, is first concentrated, adjusts its calorific value and pH value by the method for Hydrolysis kinetics sylvite in the slave cefixime side chain production waste water；High-temp liquid is burned into furnace temperature control at 600-1200 DEG C again, pretreated waste water is sprayed into high-temp liquid incinerator and carries out pyrolytic, the gas of generation empties after high temperature denitration, desulfurization, absorption, washing process, burns residue and is recycled in furnace bottom；Residue will finally be burned to be dissolved in water, filter, be concentrated, crystallize, obtain sylvite.Method of the invention extracts the sylvite in waste water simultaneously during wastewater treatment, and entire process equipment input cost is low, and cost for wastewater treatment is low, and the sylvite rate of recovery is high, recycles the purity is high of sylvite.
Description
Technical field
The present invention relates to technical field of waste water processing, and in particular to a kind of to extract from cefixime side chain production waste water
The method for refining sylvite.
Background technique
Cefixime side chain (MICA ACID) is a kind of important medicine intermediate, needs successively to pass through in the preparation
The reaction such as oximate, hydrocarbonylation, chloro acidolysis, cyclization, wherein alkylation reaction and cyclization reaction need to be added sylvite as reactant, instead
Contain a large amount of potassium ion and organic matter in the waste water that should be generated after the completion, wherein water-soluble content of organics is higher.It is this
The processing difficulty of brine waste is larger, and the treatment effect of traditional biological processing method is affected by salinity, high concentration inorganic salts
The cell membrane and endobacillary enzyme of bad microorganism can be crushed by increasing environment seepage, so that the physiological activity of microorganism is destroyed,
Toxic action is generated to biological wastewater treatment, treatment effect is made to be greatly lowered and be unable to reach national emission standard.
Studying more high-salt wastewater materilization freatment method at present mainly has: evaporation, coagulating sedimentation, electrolysis method and UF membrane
Technology.Evaporation in waste water salinity and organic pollutant have removal effect, although by using natural conditions evaporate it is dense
Contracting high slat-containing wastewater to reduce the method economically feasible of pollutant emission volume, but has local natural conditions and waste water quality
It is certain to require.Coagulation Method cannot be removed effectively the dissolubility salt in high-salt wastewater, but it is same to effectively remove colloid COD therein
When reduce turbidity of wastewater, be commonly used for high-salt wastewater pretreating process.The principle of Treatment of Wastewater by Electrolysis is mainly by outer power-up
The effect of stream generates a series of physical-chemical reaction, is reduced the poisonous and harmful substance in waste water, and give up Organic substance in water
Anodizing reduction reaction occurs on yin-yang the two poles of the earth for matter, generates substance not soluble in water, by precipitating (or air bearing) or directly
Redox is innocuous gas removing, to reduce COD.Membrane separation waste water be using film ultrafiltration, reverse osmosis waited
Function is filtered, the inorganic salts in waste water are concentrated, to extract inorganic salts.
A kind of processing of Tebuconazole pesticide wastewater is disclosed in patent CN2018100535423 and potassium sulfate salt resource is returned
Receiving method, by ketenes, condensation production workshop section's waste water using stripping-light electrolysis-Fenton oxidation-neutralization precipitation processing, by epoxy
Production workshop section's waste water handle and recycles potassium sulfate using resin adsorption, and finally by two ways, treated is discharged and is combined into life
Change processing.Although this method has recycled potassium sulfate salt resource, but desorption and regeneration processing is also carried out after resin adsorption used, makes
Desorption liquid will carry out rectifying, and distillation residual liquid will carry out burning disposal, and entire treatment process is more complicated, equipment input cost
It is high.
A kind of method of high sylvite waste water of silicated method recycling treatment is disclosed in patent CN2017101456693,
High sylvite waste water is added plastics, rubber, agricultural crop straw and silica, carried out at 1250-1500 DEG C after heat preservation melting
It burns, that burns generation is rich in HCl, NOX、SOXIt is discharged into atmosphere after the purified processing of flue gas of equal noxious materials, is burned remaining
Fuse salt pours to arrive potassium silicate.This method treatment temperature is excessively high, needs to be added the substances such as plastics, rubber, increases
Pernicious gas content in combustion tail gas, it is also necessary to silica be added, processing cost is higher, and burns the solid generated simultaneously
It is not separated with potassium silicate, obtained potassium silicate purity is lower.
Summary of the invention
In view of the deficiencies of the prior art, the object of the present invention is to provide one kind mentions from cefixime side chain production waste water
The method for taking purification sylvite extracts the sylvite in waste water, entire process equipment investment to waste water simultaneously in the process of processing
At low cost, cost for wastewater treatment is low, and the sylvite rate of recovery is high, recycles the purity is high of sylvite.
The method of the Hydrolysis kinetics sylvite of the present invention from cefixime side chain production waste water, steps are as follows:
(1) it pre-processes: cefixime side chain production waste water being concentrated, adjustment heat value substance and pH tune is then added
Substance is saved, its calorific value 100-1000cal/g, pH value 7-9 are made；
(2) it burns: high-temp liquid being burned into furnace temperature control at 600-1200 DEG C, pretreated waste water is sprayed into high temperature
Liquid incinerator carries out pyrolytic, and the gas of generation empties after high temperature denitration, desulfurization, absorption, washing process, burns surplus
Excess is recycled in furnace bottom；
(3) it separates sylvite: residue will be burned and be dissolved in water, filter, be concentrated, crystallize, obtain inorganic potassium salt.
The main component that cefixime side chain produces waste water is sylvite and intermediate product, by-product.
Adjustment heat value substance in step (1) is the water solubility that calorific value is higher than 1000cal/g lower than 100cal/g or calorific value
Substance, preferably low heat value waste water, high heating value waste water, pure water, methanol or ethyl alcohol.
PH Auto-regulator in step (1) is waste hydrochloric acid, useless potassium hydroxide or useless potassium oxide.
It is 15-20% that potassium ion mass content in waste water is concentrated into step (1).Method for concentration uses conventional method, can
Using single-action concentration, double effect concentration, Multi-effect concentration or MVR concentration.
Carrying out pretreated main function to waste water is the carbonate and bicarbonate radical removed in waste water, is made finally obtained
Sylvite purity is higher；And the water content in waste water is reduced by concentration, reduce the energy consumption of subsequent burning disposal.
Step (2) high temperature liquid incinerator is provided using the electrically heated method of internal combustion of natural gas and furnace wall to burner hearth
Heat, the burning of waste water, which is decomposed, also provides heat to burner hearth.It can be by adjusting natural gas dosage, adjusting electric heating electric current, tune
The method control high-temp liquid of whole waste water calorific value burns furnace temperature.The waste heat of high-temp liquid incinerator can provide for other workshop sections
Heat realizes the comprehensive utilization of heat.
It does not need to be passed through oxygen or air in burning process, waste water be sprayed into high-temperature space with Sprayable, waste water wink
Between high temperature, organic matter decomposes, the solids such as remaining inorganic salts, and realizes gas solid separation by cyclone separator and bag filter.
In burning process, the COD value of residue is burned by detection to determine whether the organic matter in waste water decomposes completely.
Detection method are as follows: 10g burning residue is dissolved into 100ml water, tests its COD value；It is said if COD value is less than 200mg/L
Bright organic matter decomposes completely, and process conditions can be kept constant；If COD value is greater than 200mg/L, need to process conditions in range
It is inside adjusted, decomposes organic matter complete.
The mass ratio that residue and water are burned in step (3) is 1:3-5.
Active carbon is added in the course of dissolution of step (3), active carbon additional amount is to burn residue and water gross mass
0.1-1.0%, preferably 0.1-0.5%.
Inorganic potassium salt is the mixture of potassium chloride and potassium carbonate in step (3), and potassium carbonate mass content is less than 3%.
When producing cefixime side chain, tert-butyl acetoacetate and acetic acid, sodium nitrite are first passed through into oximation reaction
Oxime compounds are generated, then oxime compounds and methyl chloroacetate cyclization are generated into hydrocarbonylation product, cyclised products are after alkylation reaction, again
Cefixime side chain is obtained by cyclization.When carrying out hydrogenation and cyclization reaction, need to be added potassium carbonate or bicarbonate
Potassium obtains corresponding product chlorinated potassium as reactant, wherein excessive potassium carbonate, saleratus and product chlorinated potassium pass through
After the operations such as extraction washing, become the higher waste water of potassium salts content.Sylvite in waste water is mainly potassium chloride, is also contained on a small quantity
Potassium carbonate, saleratus.
In actual production, cefixime side chain production technology and subsequent treatment process can change, such as extract
Washing times difference etc. causes the ingredient of waste water and property to change.Different batches cefixime side chain produces waste water
Potassium ion mass content is relatively stable, maintains between 6-10%, but its calorific value and pH value fluctuation are very big.Under normal circumstances,
The calorific value that cefixime side chain produces waste water is lower than 100cal/g, and pH value is weakly acidic between 5-7；Production technology not
When stablizing, calorific value the case where will appear higher than 1000cal/g of cefixime side chain production waste water, pH value also will appear and be higher than
9 the case where.
Cefixime side chain production waste water is pre-processed before burning, its pH value and calorific value is made to reach defined model
In enclosing, the energy consumption of burning process can reduce, reduce the corrosion to high-temp liquid incinerator, not only reduce processing cost, but also prolong
Duration of service is grown.
The work that method of the invention has been applied to the processing of cefixime side chain production waste water and purification sylvite extracts
In skill, entire processing method is easy to operate, and cost for wastewater treatment is reduced to 1000-1500 yuan/ton, and treatment effeciency is in 1-3m3/ h,
And the inorganic potassium salt in waste water has been recycled simultaneously, after treatment, obtained potassium chloride purity reaches 97% or more, sylvite recycling
Rate reaches 98% or more, has preferable economic benefit.
Compared with prior art, the invention has the following beneficial effects:
(1) after cefixime side chain is produced Wastewater Pretreatment by the present invention, it is injected directly into high-temp liquid incinerator, makes to give up
Organic matter in water decomposes at high temperature, obtains sylvite by gas solid separation, entire process equipment input cost is low, wastewater treatment
High-efficient, cost for wastewater treatment is 1000-1500 yuan/ton；
(2) present invention is extracting the sylvite in waste water to waste water simultaneously in the process of processing, is removed by pretreatment
Carbonate and bicarbonate radical in waste water, and the sylvite burned in residue is extracted by dissolution, filtering, concentration, crystallization, make most
The potassium chloride salt impurity obtained eventually is few, and purity reaches 97% or more, and the sylvite rate of recovery reaches 98% or more.
Specific embodiment
The present invention will be further described with reference to embodiments, but protection scope of the present invention is not limited only to this.
Embodiment 1
10t cefixime side chain production waste water is handled, and extracts potassium chloride, detects the potassium ion quality of waste water
Content is 7.8%, calorific value 82cal/g, pH value 6.5, the method is as follows:
(1) pre-process: using Conventional concentration method by cefixime side chain production waste water be concentrated, be concentrated into potassium from
Protonatomic mass content is 18%, and then addition high heating value waste water (calorific value > 1000cal/g) to its calorific value reaches 500 ± 50cal/g,
Adding useless potassium hydroxide to its pH value is 8 ± 0.5；
(2) it burns: high-temp liquid being burned into furnace temperature control at 900 DEG C, pretreated waste water is sprayed into high-temp liquid
Incinerator is burned, and carries out gas solid separation by cyclone separator and bag filter, and the gas of generation is de- by high temperature
It is emptied after nitre, desulfurization, absorption, washing process, burns residue and recycled in furnace bottom；
(3) it separates sylvite: residue, water and active carbon 1:4:0.01 in mass ratio will be burned and carry out mixed dissolution, then
It is successively filtered, is concentrated, crystallizes, obtain sylvite, be weighed as 1460kg.
Obtained sylvite is analyzed, wherein potassium chloride mass content is 98.2%, and potassium carbonate mass content is
1.8%.
The processing cost of waste water is about 1240 yuan/ton.
Embodiment 2
5t cefixime side chain production waste water is handled, and extracts potassium chloride, detects the potassium ion quality of waste water
Content is 9.6%, calorific value 1130cal/g, pH value 12.2, the method is as follows:
(1) pre-process: using Conventional concentration method by cefixime side chain production waste water be concentrated, be concentrated into potassium from
Protonatomic mass content is 20%, and then addition low heat value waste water (calorific value < 100cal/g) to its calorific value reaches 900 ± 100cal/g,
Adding waste hydrochloric acid to its pH value is 8 ± 0.5；
(2) it burns: high-temp liquid being burned into furnace temperature control at 600 DEG C, pretreated waste water is sprayed into high-temp liquid
Incinerator is burned, and carries out gas solid separation by cyclone separator and bag filter, and the gas of generation is de- by high temperature
It is emptied after nitre, desulfurization, absorption, washing process, burns residue and recycled in furnace bottom；
(3) it separates sylvite: residue, water and active carbon 1:5:0.06 in mass ratio will be burned and carry out mixed dissolution, then
It is successively filtered, is concentrated, crystallizes, obtain sylvite, be weighed as 906kg.
Obtained sylvite is analyzed, wherein potassium chloride mass content is 98.5%, and potassium carbonate mass content is
1.5%.
The processing cost of waste water is about 1000 yuan/ton.
Embodiment 3
10t cefixime side chain production waste water is handled, and extracts potassium chloride, detects the potassium ion quality of waste water
Content is 6.2%, calorific value 95cal/g, pH value 5.3, the method is as follows:
(1) pre-process: using Conventional concentration method by cefixime side chain production waste water be concentrated, be concentrated into potassium from
Protonatomic mass content is 15%, and methanol to its calorific value is then added and reaches 200 ± 50cal/g, adds useless potassium oxide and useless hydrogen-oxygen
Changing potassium to its pH value is 8 ± 0.5；
(2) it burns: high-temp liquid being burned into furnace temperature control at 1200 DEG C, pretreated waste water is sprayed into high-temp liquid
Incinerator is burned, and carries out gas solid separation by cyclone separator and bag filter, and the gas of generation is de- by high temperature
It is emptied after nitre, desulfurization, absorption, washing process, burns residue and recycled in furnace bottom；
(3) it separates sylvite: residue, water and active carbon 1:5:0.025 in mass ratio will be burned and carry out mixed dissolution, then
It is successively filtered, is concentrated, crystallizes, obtain sylvite, be weighed as 1164kg.
Obtained sylvite is analyzed, wherein potassium chloride mass content is 97.7%, and potassium carbonate mass content is
2.3%.
The average treatment cost of waste water is about 1450 yuan/ton.
Claims (7)
1. a kind of method of the Hydrolysis kinetics sylvite from cefixime side chain production waste water, it is characterised in that: steps are as follows:
(1) it pre-processes: cefixime side chain production waste water being concentrated, adjustment heat value substance and pH instrumentality is then added
Matter makes its calorific value 100-1000cal/g, pH value 7-9；
(2) it burns: high-temp liquid being burned into furnace temperature control at 600-1200 DEG C, pretreated waste water is sprayed into high-temp liquid
Incinerator carries out pyrolytic, and the gas of generation empties after high temperature denitration, desulfurization, absorption, washing process, burns residue
It is recycled in furnace bottom；
(3) it separates sylvite: residue will be burned and be dissolved in water, filter, be concentrated, crystallize, obtain inorganic potassium salt.
2. the method for the Hydrolysis kinetics sylvite according to claim 1 from cefixime side chain production waste water, feature
Be: the adjustment heat value substance in step (1) is the water-soluble object that calorific value is higher than 1000cal/g lower than 100cal/g or calorific value
Matter.
3. the method for the Hydrolysis kinetics sylvite according to claim 1 from cefixime side chain production waste water, feature
Be: the pH Auto-regulator in step (1) is waste hydrochloric acid, useless potassium hydroxide or useless potassium oxide.
4. the method for the Hydrolysis kinetics sylvite according to claim 1 from cefixime side chain production waste water, feature
Be: it is 15-20% that potassium ion mass content in waste water is concentrated into step (1).
5. the method for the Hydrolysis kinetics sylvite according to claim 1 from cefixime side chain production waste water, feature
Be: the mass ratio that residue and water are burned in step (3) is 1:3-5.
6. the method for the Hydrolysis kinetics sylvite according to claim 1 from cefixime side chain production waste water, feature
It is: active carbon is added in the course of dissolution of step (3), active carbon additional amount is to burn the 0.1- of residue and water gross mass
1.0%.
7. the method for the Hydrolysis kinetics sylvite according to claim 1 from cefixime side chain production waste water, feature
Be: inorganic potassium salt is the mixture of potassium chloride and potassium carbonate in step (3), and potassium carbonate mass content is less than 3%.
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| CN201910516140.7A CN110395747A (en) | 2019-06-14 | 2019-06-14 | The method of Hydrolysis kinetics sylvite from cefixime side chain production waste water |
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| CN201910516140.7A CN110395747A (en) | 2019-06-14 | 2019-06-14 | The method of Hydrolysis kinetics sylvite from cefixime side chain production waste water |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111484365A (en) * | 2020-03-12 | 2020-08-04 | 山东清博生态材料综合利用有限公司 | Organic potash fertilizer prepared from waste potassium salt and preparation method thereof |
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2019
- 2019-06-14 CN CN201910516140.7A patent/CN110395747A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111484365A (en) * | 2020-03-12 | 2020-08-04 | 山东清博生态材料综合利用有限公司 | Organic potash fertilizer prepared from waste potassium salt and preparation method thereof |
| CN111484365B (en) * | 2020-03-12 | 2022-05-27 | 山东清博生态材料综合利用有限公司 | Organic potash fertilizer prepared from waste potassium salt and preparation method thereof |
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