CN112707558A - Method for recycling wastewater - Google Patents
Method for recycling wastewater Download PDFInfo
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- CN112707558A CN112707558A CN201911019045.2A CN201911019045A CN112707558A CN 112707558 A CN112707558 A CN 112707558A CN 201911019045 A CN201911019045 A CN 201911019045A CN 112707558 A CN112707558 A CN 112707558A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B7/00—Fertilisers based essentially on alkali or ammonium orthophosphates
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- 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
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
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- 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
- C02F1/06—Flash evaporation
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- 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
- C02F1/38—Treatment of water, waste water, or sewage by centrifugal separation
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- 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
- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/105—Phosphorus compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A40/00—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
- Y02A40/10—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in agriculture
- Y02A40/20—Fertilizers of biological origin, e.g. guano or fertilizers made from animal corpses
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- Hydrology & Water Resources (AREA)
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Abstract
The invention discloses a method for recycling wastewater, wherein the wastewater comprises organic amine, phosphorus and aluminum; the method comprises the following steps: (1) adding an alkaline compound to the wastewater to obtain a mixture; (2) separating the mixture, and recovering the organic amine to obtain slurry without the organic amine; (3) adding a modifier into the slurry, and then carrying out solid-liquid separation to obtain a solid and a liquid; (4) and preparing the solid to obtain the phosphate fertilizer. According to the technical scheme, the alkaline compound is added into the phosphorus-aluminum molecular sieve production wastewater, so that decomposition and separation of an organic-inorganic mixed system are achieved, organic amine is recovered from a light component, a modifier is added after solid-liquid separation of a heavy component, and finally, a phosphate fertilizer is obtained after drying treatment, so that resource utilization of beneficial components in the wastewater is realized.
Description
Technical Field
The invention relates to a method for recycling wastewater, in particular to a method for recycling wastewater generated in the production process of a phosphorus-aluminum molecular sieve in the fields of coal chemical industry, natural gas chemical industry and petrochemical industry.
Background
Molecular sieves have been widely used in the fields of petrochemical industry, chemical fiber, and the like due to their excellent adsorption properties and catalytic effects. The phosphorus-aluminum molecular sieve can present physicochemical properties from medium-strong acid to strong acid, and can be used for catalytic reactions of various hydrocarbons, such as catalytic reforming, catalytic cracking, hydrofining, hydroisomerization, dehydrocyclization, aromatic hydrocarbon disproportionation, methanol conversion and the like. SAPO-34 is one of the industrialized important varieties of similar aluminophosphate molecular sieves, and has been successfully applied to the industrial production of preparing olefin (MTO) by converting methanol. As another example, APO-11 molecular sieves are useful in the isomerization of alkanes and alkenes.
However, organic amine/ammonium is often used as a directing agent in the synthesis process of the molecular sieve, so that a large amount of waste water, waste gas and waste residues containing various inorganic salts containing organic amine/ammonium are inevitably generated in the preparation process of the molecular sieve, if the organic amine/ammonium is not properly treated, the environment is seriously polluted, the human health is harmed, and the problem of solving the three wastes in the production process of the molecular sieve is an unavoidable problem. The phosphorus-aluminum molecular sieve crystallization wastewater mainly contains components such as water, a phosphorus source, organic amine, an aluminum source, a silicon source and the like, and part of organic amine can be recycled by rectification, but most of organic amine and inorganic anions are combined into a salt form and are difficult to recycle.
In the CN101759246A patent, a study is made on the treatment of wastewater containing organic solvent, a molecular sieve is used to adsorb the organic solvent in the wastewater, then the same kind of organic solvent steam is introduced into the molecular sieve, so that the organic solvent adsorbed in the molecular sieve is changed into organic solvent steam, and the organic solvent is recovered after condensation. Compared with the traditional rectification, the method has the advantages of low energy consumption and the like, but the method has low processing capacity and cannot process a system containing phosphorus, aluminum, silicon and solid.
The CN1205987A patent is studied for recovering suspended matter in catalyst production wastewater, and it adopts microporous filtration technology, and does not add any auxiliary agent into the recovered solid material, including the processes of wastewater collection, filtration, discharge, and backwashing, but the operation process is complex, not easy to control, and is intermittent operation, and is not suitable for continuous wastewater treatment device.
The patent CN201510593981.X is to perform acid separation gel breaking on the wastewater, then add a compound containing iron and/or a compound containing calcium into the wastewater after the acid separation gel breaking to generate a precipitate, perform filtration treatment to obtain a filtrate, adjust the pH value of the filtrate to 9-13, perform secondary filtration treatment to obtain a second filtrate, extract triethylamine in the second filtrate by using an extracting agent to obtain an extract phase and a raffinate; and recovering triethylamine in the extracted phase by distillation. According to the technical scheme, triethylamine in the triethylamine-containing wastewater can be effectively removed, and the triethylamine and the wastewater are recycled, but the operation steps are complex.
The patent CN201410169450.3 relates to a method for recovering triethylamine from water, which mainly uses hydrochloric acid to adjust the pH value of a triethylamine aqueous solution system to 1, then uses cyclohexane to extract triethylamine in water, uses sodium hydroxide to adjust the pH value of an extraction phase to be more than 12, and carries out distillation to obtain high-purity triethylamine, and recovers an extractant cyclohexane. The patent is applicable to the recovery of a triethylamine aqueous solution with the concentration of 5-50%, but the operation is complicated, and a system containing phosphorus, aluminum, silicon and solid cannot be processed.
The prior art relates to a method for recycling molecular sieve crystallization liquid and treating or recovering amine-containing wastewater, but the resource utilization of phosphate in the phosphorus-aluminum molecular sieve crystallization wastewater is not related, and the problems of low recovery rate of organic amine, environmental pollution and the like exist.
Disclosure of Invention
The invention aims to solve the technical problems that phosphorus element and/or silicon and/or aluminum element and organic amine are contained in the production wastewater of the phosphorus-aluminum molecular sieve, the treatment is difficult, the resource recovery rate is low and the environment is polluted, and provides a novel method for recycling the wastewater.
In order to solve the technical problem, the invention provides a method for recycling wastewater, wherein the wastewater comprises organic amine, phosphorus and aluminum; the method comprises the following steps:
(1) adding an alkaline compound to the wastewater to obtain a mixture;
(2) separating the mixture, and recovering the organic amine to obtain slurry without the organic amine;
(3) adding a modifier into the slurry, and then carrying out solid-liquid separation to obtain a solid and a liquid;
(4) and preparing the solid to obtain the phosphate fertilizer.
According to some embodiments of the invention, the wastewater is wastewater produced during the production of aluminophosphate molecular sieves; preferably, the wastewater is crystallized wastewater generated in the process of producing SAPO, APO or MeAPO.
According to a preferred embodiment of the present invention, the composition of the wastewater is, based on the total weight of the wastewater taken as 100%: 75-95% of water, 3.1-20% of organic amine, 1-5% of phosphorus and 0.5-3% of aluminum; the organic amine is preferably triethylamine and tetraalkylammonium hydroxide.
According to a preferred embodiment of the invention, the composition of the waste water is: 75-95% of water, 3-15% of triethylamine, 0.1-5% of tetraalkylammonium hydroxide, 1-5% of phosphorus and 0.5-3% of aluminum. The tetraalkylammonium hydroxide is preferably tetrapropylammonium hydroxide and tetraethylammonium hydroxide.
According to some embodiments of the invention, the basic compound comprises at least one of a hydroxide, an oxide and a carbonate of sodium, potassium, calcium, magnesium.
According to a preferred embodiment of the present invention, in the step (1), the ratio of the monovalent cation in the basic compound to the molar amount of phosphate in the wastewater is (1 to 4): 1, preferably (1.5-2): 1.
according to some embodiments of the invention, the step (2) comprises:
carrying out flash evaporation treatment on the mixture to obtain light component and heavy component slurry containing organic amine and water;
and (4) further separating and treating the light component, and recovering the organic amine in the light component.
According to a preferred embodiment of the invention, the flash evaporation treatment is carried out at a temperature of 50 to 100 ℃ and at a pressure of 10 to 101 KPa.
According to some embodiments of the invention, the step (3) comprises: and adding a modifier into the slurry to obtain a solid-liquid mixture, and then carrying out solid-liquid separation to obtain a solid and a liquid. The solid-liquid separation can be carried out by any means known to those skilled in the art, and preferably by means of pressure filtration, suction filtration, centrifugal separation and the like.
According to a preferred embodiment of the invention, the modifier comprises at least one of chlorides and sulphates of calcium, magnesium, iron.
According to a preferred embodiment of the present invention, in the step (3), the molar ratio of the divalent cation in the modifier to the phosphate radical in the wastewater is (0.1-1): 1.
the modifier is added to control the content of organic matters in the final material, improve the solid slag treatment process (adjust the viscosity of the solid slag to ensure that the solid slag is suitable for material transmission in a continuous operation process, improve the treatment efficiency), reduce the treatment cost (the price cost of the modifier is far lower than that of an alkaline compound), and simultaneously be an effective index of a resource product calcium magnesium phosphate fertilizer.
According to a preferred embodiment of the present invention, the solid is dried in the step (4) to prepare a phosphate fertilizer; the drying temperature is preferably 90 to 400 ℃.
By adopting the technical scheme of the invention, the alkaline compound is added into the phosphorus-aluminum molecular sieve production wastewater to decompose and separate an organic-inorganic mixed system, organic amine is recovered from light components, a modifier is added after solid-liquid separation of heavy components, and finally, the phosphate fertilizer is obtained after drying treatment, so that the resource utilization of beneficial components in the wastewater is realized. The scheme improves the recovery rate of beneficial resources in the wastewater, greatly reduces the pollution to the environment, obtains good technical effect, has simple operation of the treatment process, is easy to control, and is suitable for industrial application.
Drawings
FIG. 1 is a schematic view of a method for resource utilization of wastewater according to an embodiment of the invention.
Detailed Description
The present invention will be further illustrated by the following examples, but is not limited to these examples.
The wastewater treated in the examples had the following composition:
TABLE 1 Main composition of wastewater (unit: wt%)
[ example 1 ]
Adding 1000g g of wastewater stock solution I, 2g of calcium oxide, 2g of magnesium oxide and 40g of sodium hydroxide into a flask, stirring, performing flash evaporation at the flash evaporation temperature of 50 ℃ and the pressure of 20KPa, collecting 300g of flash evaporation condensate, and stopping. The condensate is rectified to recover 85.3g of triethylamine, the concentration is 89%, and the recovery rate of the triethylamine is 78.4%. 10g of calcium chloride is added into the residual slurry in the flask, then solid-liquid separation is carried out, the solid is dried at 300 ℃ to prepare the phosphate fertilizer, the available phosphorus content in the phosphate fertilizer is 25.3 percent, the water-soluble phosphorus content is 17.3 percent (calculated by phosphorus pentoxide), and the phosphorus recovery rate is 79.4 percent.
[ examples 2 to 5 ]
The wastewater was treated according to the respective procedures in example 1 except for changing the kind of the stock solution, the composition and amount of the basic compound to be added, the composition and amount of the modifier, and the treatment conditions, the process conditions are summarized in Table 2, and the results of resource utilization of the product are shown in Table 3.
[ COMPARATIVE EXAMPLES 1 to 2 ]
The wastewater was treated according to the respective procedures in example 1 except that the kind of the stock solution, the composition and amount of the basic compound to be added, and the modifier were not added, the process conditions are summarized in Table 2, and the results of the resource utilization products are shown in Table 3.
TABLE 2 summary of different wastewater treatment process conditions
In Table 2, m (B: P) represents the ratio of the monovalent cation in the basic compound to the molar amount of phosphate radical in the wastewater; the molar ratio of divalent cations in the M (M: P) modifier to phosphate in the wastewater.
TABLE 3 results of resource utilization of products under different treatment conditions
Any numerical value mentioned in this specification, if there is only a two unit interval between any lowest value and any highest value, includes all values from the lowest value to the highest value incremented by one unit at a time. For example, if it is stated that the amount of a component, or a value of a process variable such as temperature, pressure, time, etc., is 50 to 90, it is meant in this specification that values of 51 to 89, 52 to 88 … …, and 69 to 71, and 70 to 71, etc., are specifically enumerated. For non-integer values, units of 0.1, 0.01, 0.001, or 0.0001 may be considered as appropriate. These are only some specifically named examples. In a similar manner, all possible combinations of numerical values between the lowest value and the highest value enumerated are to be considered to be disclosed in this application.
It should be noted that the above-mentioned embodiments are only for explaining the present invention, and do not constitute any limitation to the present invention. The present invention has been described with reference to exemplary embodiments, but the words which have been used herein are words of description and illustration, rather than words of limitation. The invention can be modified, as prescribed, within the scope of the claims and without departing from the scope and spirit of the invention. Although the invention has been described herein with reference to particular means, materials and embodiments, the invention is not intended to be limited to the particulars disclosed herein, but rather extends to all other methods and applications having the same functionality.
Claims (10)
1. A method for recycling wastewater, wherein the wastewater comprises organic amine, phosphorus and aluminum; the method comprises the following steps:
(1) adding an alkaline compound to the wastewater to obtain a mixture;
(2) separating the mixture, and recovering the organic amine to obtain slurry without the organic amine;
(3) adding a modifier into the slurry, and then carrying out solid-liquid separation to obtain a solid and a liquid;
(4) and preparing the solid to obtain the phosphate fertilizer.
2. The method of claim 1, wherein the wastewater is wastewater generated in a process for producing aluminophosphate molecular sieves; preferably, the wastewater is crystallized wastewater generated in the process of producing SAPO, APO or MeAPO.
3. The method according to claim 1 or 2, characterized in that the composition of the wastewater is, based on 100% by total weight of the wastewater: 75-95% of water, 3.1-20% of organic amine, 1-5% of phosphorus and 0.5-3% of aluminum; preferably, the composition of the wastewater is: 75-95% of water, 3-15% of triethylamine, 0.1-5% of tetraalkylammonium hydroxide, 1-5% of phosphorus and 0.5-3% of aluminum.
4. The method of any one of claims 1-3, wherein the basic compound comprises at least one of a hydroxide, an oxide, and a carbonate of sodium, potassium, calcium, magnesium.
5. The method according to any one of claims 1 to 4, wherein in the step (1), the ratio of the monovalent cation in the basic compound to the molar amount of phosphate in the wastewater is (1 to 4): 1.
6. the method according to any one of claims 1-4, wherein the step (2) comprises:
carrying out flash evaporation treatment on the mixture to obtain light component and heavy component slurry containing organic amine and water;
and (4) further separating and treating the light component, and recovering the organic amine in the light component.
7. The process according to any one of claims 1 to 6, wherein the flash evaporation treatment is carried out at a temperature of 50 to 100 ℃ and a pressure of 10 to 101 KPa.
8. The method of any one of claims 1-7, wherein the modifier comprises at least one of chlorides and sulfates of calcium, magnesium, iron.
9. The method according to any one of claims 1 to 8, wherein in the step (3), the molar ratio of the divalent cation in the modifier to the phosphate in the wastewater is (0.1 to 1): 1.
10. the method according to any one of claims 1 to 9, wherein the solid is dried in the step (4) to prepare a phosphate fertilizer; the drying temperature is preferably 90 to 400 ℃.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112678788A (en) * | 2019-10-18 | 2021-04-20 | 中国石油化工股份有限公司 | Process for preparing dibasic salts of hydrogen phosphate |
| CN114477653A (en) * | 2022-02-24 | 2022-05-13 | 陕西煤业化工技术研究院有限责任公司 | Method and system for treating wastewater in molecular sieve production process |
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| CN104230077A (en) * | 2013-06-17 | 2014-12-24 | 中国石油化工股份有限公司 | Method for treating organic amine wastewater containing phosphorus, aluminum and silicon |
| CN105130822A (en) * | 2015-09-21 | 2015-12-09 | 四川乐创科技有限公司 | Method for recovering triethylamine, removing phosphorus pollutants and recovering phosphorus resources in glyphosate mother liquor |
| CN105130082A (en) * | 2015-09-17 | 2015-12-09 | 博天环境集团股份有限公司 | Method for treating triethylamine-contained wastewater |
| CN105198147A (en) * | 2015-09-15 | 2015-12-30 | 博天环境集团股份有限公司 | Treatment method for organic amine waste water generated by producing molecular sieve and carrier catalyst thereof |
| CN112694142A (en) * | 2019-10-22 | 2021-04-23 | 中国石油化工股份有限公司 | Modifier for treating wastewater and application thereof |
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2019
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Patent Citations (5)
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| CN104230077A (en) * | 2013-06-17 | 2014-12-24 | 中国石油化工股份有限公司 | Method for treating organic amine wastewater containing phosphorus, aluminum and silicon |
| CN105198147A (en) * | 2015-09-15 | 2015-12-30 | 博天环境集团股份有限公司 | Treatment method for organic amine waste water generated by producing molecular sieve and carrier catalyst thereof |
| CN105130082A (en) * | 2015-09-17 | 2015-12-09 | 博天环境集团股份有限公司 | Method for treating triethylamine-contained wastewater |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112678788A (en) * | 2019-10-18 | 2021-04-20 | 中国石油化工股份有限公司 | Process for preparing dibasic salts of hydrogen phosphate |
| CN112678788B (en) * | 2019-10-18 | 2022-10-11 | 中国石油化工股份有限公司 | Process for preparing dibasic salts of hydrogen phosphate |
| CN114477653A (en) * | 2022-02-24 | 2022-05-13 | 陕西煤业化工技术研究院有限责任公司 | Method and system for treating wastewater in molecular sieve production process |
| CN114477653B (en) * | 2022-02-24 | 2023-06-02 | 陕西煤业化工技术研究院有限责任公司 | Method and system for treating wastewater in molecular sieve production process |
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