CN109650627A - A kind of organic liquid waste resource utilization method containing ammonium sulfate - Google Patents
A kind of organic liquid waste resource utilization method containing ammonium sulfate Download PDFInfo
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- CN109650627A CN109650627A CN201910006764.4A CN201910006764A CN109650627A CN 109650627 A CN109650627 A CN 109650627A CN 201910006764 A CN201910006764 A CN 201910006764A CN 109650627 A CN109650627 A CN 109650627A
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- organic liquid
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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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/78—Compounds containing aluminium and two or more other elements, with the exception of oxygen and hydrogen
-
- 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
-
- 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
-
- 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
- C02F2001/007—Processes including a sedimentation step
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- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Inorganic Chemistry (AREA)
- Geology (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Hydrology & Water Resources (AREA)
- Water Supply & Treatment (AREA)
- Heat Treatment Of Water, Waste Water Or Sewage (AREA)
- Removal Of Specific Substances (AREA)
Abstract
The organic liquid waste resource utilization method containing ammonium sulfate that the present invention provides a kind of, comprising the following steps: step 1: to organic liquid waste add with the equimolar aluminum sulfate of sulphur ammonium content and auxiliary agent in organic liquid waste, and heat；Step 2: cooling to organic liquid waste；Step 3: being separated by solid-liquid separation, the alum solid separated is through drying, packing and selling；Step 4: being evaporated concentration to solution, evaporation condensate simultaneously send biochemical device to carry out sewage treatment；Cooling and standings are carried out step 5: concentrate is discharged into tank or slot, stand the bottom liquid and crystalline deposit of formation, bottom liquid are entered into third step, concentrate enters the 6th step；Step 6: the concentrate of removal precipitating and bottom liquid, which is discharged into product storage tank, obtains furnace fuel oil, method of the invention, which is carried out, after qualified by furnace fuel standard detection obtains liquid fuel, it realizes comprehensive utilization of resources, is particularly suitable for the sulphur ammonium liquid waste processing being concentrated after benzene extraction in caprolactam production process.
Description
Technical field
The invention belongs to Chemical Manufacture and environment protection field, in particular to a kind of organic liquid waste recycling benefit containing ammonium sulfate
Use method.
Background technique
In caprolactam and Acrylonitrile Production, high concentrated organic wastewater largely containing sulphur ammonium can be generated.
In the production process of caprolactam, caprolactam and oleum mixed liquor generate caprolactam water after ammonium hydroxide neutralizes
Solution and ammonium sulfate solution obtain most of caprolactam through Gravity Separation, and the caprolactam in ammonium sulfate solution is extracted using benzene
After fetching receipts, then recycling benzene is stripped, the ammonium sulfate solution of purification is then subjected to condensing crystallizing.Containing a small amount of sulphur ammonium and by-product
Caprolactam water solution is extracted with benzene, removes most of sulphur ammonium and by-product, forms raffinate, and extract liquor carries out vapour
It mentions, the heavy component that lighter component can send sewage-treatment plant to handle, but separate after recycling benzene is containing sulphur ammonium, water
And the mixed liquor of by-product, complex in composition, concentration is high, and routinely sewage treatment process is difficult to handle, and processing cost is high, generally
This strand of waste liquid is mixed into introducing incinerator with other waste materials and does burning disposal.
Unreacted ammonia generallys use the method removal that pickling generates ammonium salt in Acrylonitrile Production, and practical raw
Unreacted ammonia is generally removed using sulfuric acid during producing and generates sulphur ammonium, the sulphur ammonium of generation is largely used as chemical fertilizer.In material point
Containing high polymer, high-boiling components and a small amount of byproduct of reaction in sulphur ammonium raffinate from process, such solution C OD is greater than 15000mg/
L, total cyanogen are greater than 10mg/L, and the sulphur ammonium of recycling contains environmentally harmful organic matter and can not be used as fertilizer application.
The worker of many chemical industry and environment protection field attempted to carry out above-mentioned waste water innoxious or comprehensive utilization, such as: right
Such waste liquid is evaporated concentration, and solvent, which is added, is precipitated sulphur ammonium, and ammonium sulfate crystals, the liquid phase after separation are obtained after being separated by solid-liquid separation
By being distilled to recover solvent and going to remove water, the organic matter crystallization containing caprolactam is obtained after cooling.To containing 5-25% sulphur ammonium,
The acrylonitrile amine wastewater of sulphuric acid progress wet oxidation processing of ten thousand mg/L of COD6.5-18, total cyanogen content 300-1500mg/L, wet oxidation
230-320 °C of reaction temperature, reaction pressure 5-12MPa, reaction time 10-150 minutes.
Due to containing a large amount of sulphur ammonium in waste liquid, makes total sulfur content 2-8% in liquid, cause burning process to generate a large amount of
Sulfur dioxide, that is, increase the operation cost of desulphurization denitration, and serious equipment is caused to corrode.Sulphur ammonium is decomposed in the high temperature process
Heat is absorbed, needs to consume a large amount of supplemental heat source, causes the energy consumption of incinerator high.Sulphur ammonium and acyl in oneself are realized using solvent method
The higher cost of amine recycling, and due to material viscosity increase after concentration, even if the mobility that solvent increases material is added, but sulphur
Tiny particle suspension be will form after ammonium dehydration in material, sulphur ammonium difficult to realize and organic materials are completely separated.Using wet
Formula oxidation processes amine wastewater of sulphuric acid, investment is big, and operation cost is high, and cannot achieve the resource utilization of sulphur ammonium.
For the waste liquid containing sulphur ammonium and high-enriched organics, the present inventor proposes a kind of new method of resource.
Summary of the invention
1, technical problem to be solved:
The existing organic liquid waste containing sulphur ammonium is difficult to handle, and processing cost is high, generally mixes this strand of waste liquid with other waste materials
It introduces incinerator and does burning disposal, cannot achieve the resource utilization of sulphur ammonium.
2, technical solution:
A kind of organic liquid waste resource utilization method containing sulphur ammonium, comprising the following steps: step 1: to organic liquid waste add with
0.1% -8% auxiliary agent of the equimolar aluminum sulfate of sulphur ammonium content and waste liquid volume in organic liquid waste, and heating dissolves aluminum sulfate；
Step 2: it is cooling to organic liquid waste, so that organic liquid waste is generated alum crystalline deposit；Step 3: being separated by solid-liquid separation, separate
Alum solid out is after drying, by standard GB25592-2010 detection qualification, packing and selling；Step 4: to removing
The solution of solid crystal precipitating is evaporated concentration, and evaporation condensate simultaneously send biochemical device to carry out sewage treatment；Step 5: by dense
Contracting liquid, which is discharged into tank or slot, carries out cooling and standings, stands the bottom liquid and crystalline deposit of formation, concentrate floats on above the liquid of bottom, the bottom of by
Liquid enters third step, and concentrate enters the 6th step；It is obtained step 6: the concentrate of removal precipitating and bottom liquid is discharged into product storage tank
To furnace fuel oil, to be sold by the qualified laggard marketing of oily (GB25989-2010) standard detection of furnace fuel.
If containing acrylonitrile in organic wastewater, the processing method of the 6th step are as follows: handled using incinerator special.
Contain ammonium sulfate in organic liquid waste, the mass percentage content of ammonium sulfate is 2% -35%, and content of organics is
5% -63%, remaining is water, in the first step, is first tested and analyzed to ammonium sulphate content, to adding equimolar sulphur in solution
Sour aluminium, the aluminum sulfate added are anhydrous slufuric acid aluminium or the aluminum sulfate containing the crystallization water, and the aluminum sulfate added is powdered
Or block or solution shape.
The aluminum sulfate added is powdered or block or solution shape.
In the first step, the auxiliary agent added is normal propyl alcohol, propilolic alcohol, ethylene glycol, acetylacetone,2,4-pentanedione, n-butanol, isobutanol, three second
The one or more of acid glyceride, n-amyl alcohol.Add 0.1% -8% that ratio is waste liquid volume.
The method, the alum obtained in the third step can also heat resolve, produce the aluminium oxide of high-purity
Sale, the ammonia and SO3 for decomposing generation are absorbed with ammonium hydroxide is cooling, form ammonium sulfate solution, produce sulphur ammonium.
The alum obtained in the third step can also be heated to 800 °C or more decomposition generate aluminum oxides, ammonia,
SO3, aluminum oxide are sold as high added value ceramic raw material, ammonia and the SO3 cooling absorption production sulphur ammonium of ammonium hydroxide.
The alum pure water not high to unqualified or credit rating heating in the third step is re-dissolved, is cooled down, tying
Brilliant, separation, drying are to obtain the product for complying with standard GB25592-2010.
In the third step, the separation of solid and liquid uses one or more of methods of filtering, filters pressing, sedimentation, centrifuge separation
It is used in combination.
In step 6, the furnace fuel oil and other fuel oil mixed sellings use, or are delivered to CWS system
Multifuel combustion utilizes together with coal.
3, the utility model has the advantages that
The processing cost of such waste liquid can be greatly lowered using method for organic wastewater resources regeneration containing sulphur ammonium provided by the invention,
Sulphur ammonium and organic matter are all realized into resource utilization, generate the economic benefit of aobvious tool；Evaporation condensed water uses biochemical method
Processing, processing cost are low.
After going out alum by products standards GB25592-2010 detection qualification using ammonium sulfate production, it can make extensively
Used in fields such as water process, papermaking, printing and dyeing, ceramics.The sulphur ammonium waste liquid removing sulphur ammonium of caprolactam and the organic matter calorific value of water can
Up to 5000kCaL/kg or more, after furnace heavy oil standard detection qualification, it can the fuel as oil burning boiler uses, can also
To be used directly as the auxiliary agent of water-coal-slurry.After acrylonitrile amine wastewater of sulphuric acid realizes sulphur ammonium resource utilization, the highly concentrated of sulphur ammonium is removed
Degree organic wastewater directly burns after being concentrated by evaporation, and evaporation condensate carries out biochemical treatment.
Specific embodiment
A kind of organic liquid waste resource utilization method containing ammonium sulfate, comprising the following steps: step 1: to organic liquid waste
0.1% -8% auxiliary agent with the equimolar aluminum sulfate of sulphur ammonium content and waste liquid volume in organic liquid waste is added, and heating makes aluminum sulfate
Dissolution；Step 2: it is cooling to organic liquid waste, so that organic liquid waste is generated alum crystalline deposit；Step 3: carrying out solid-liquid point
From the alum solid separated is after drying, by standard GB25592-2010 detection qualification, packing and selling；Step 4:
Concentration is evaporated to the solution of removing solid crystal precipitating, evaporation condensate simultaneously send biochemical device to carry out sewage treatment；5th
Step: concentrate is discharged into tank or slot and carries out cooling and standings, stands the bottom liquid and crystalline deposit of formation, concentrate floats on the liquid of bottom
Side, enters third step for bottom liquid, concentrate enters the 6th step；Step 6: removal precipitating and the concentrate of bottom liquid are discharged into production
Product storage tank obtains furnace fuel oil, to sell by the qualified laggard marketing of oily (GB25989-2010) standard detection of furnace fuel.
For acrylonitrile amine wastewater of sulphuric acid processing technical solution due in organic matter contain cyanogen substance, it is dense in step 6
Contracting liquid cannot be used as conventional fuel, but incinerator special is used to handle.
The alum obtained in the third step can also be heated to 800 °C or more decomposition generate aluminum oxides, ammonia,
SO3, aluminum oxide are sold as ceramic raw material, ammonia and the SO3 cooling absorption production sulphur ammonium of ammonium hydroxide.
Below by embodiment, the present invention is described in detail.
Embodiment 1
Certain contains 1 liter of high concentrated organic waste liquid of ammonium sulfate, ten thousand mg/litre of COD:68, and 3.12 ten thousand mg/litre of ammonia nitrogen is added 20
Milliliter ethylene glycol and aluminum sulfate 381g, heating make solution temperature to 80 °C or more, stir, until aluminum sulfate dissolves, stir, use ice
Bath is cooled to 0 °C, static 12 hours, filters, dry, obtains the alum white precipitate 945g containing the crystallization water.
Embodiment 2
Certain contains 5 liters of high concentrated organic waste liquid of ammonium sulfate, ten thousand mg/litre of COD:54, and 1.96 ten thousand mg/litre of ammonia nitrogen is added 100
Milliliter ethylene glycol and aluminum sulfate 1197g, heating makes solution temperature to 80 °C or more, stirs, until aluminum sulfate dissolves, stirs, certainly
30 °C so are cooled to, is cooled with an ice bath to 0 °C, static 12 hours, sedimentation filtration was dry, obtained the alum containing the crystallization water
White precipitate 2790g is evaporated concentration, crystallisation by cooling, filtering, precipitated crystal, drying to the solution for filtering off precipitating, then obtains
White 300g.Solution is concentrated into 1.5 liters, calorific value 5300kcal/kg, total sulfur is less than 1%.
Embodiment 3
1 cubic metre of concentrate of the benzene extraction containing ammonium sulfate of certain caprolactam production enterprise, ten thousand mg/litre of COD:33.1, ammonia
40 liters of auxiliary agents and aluminum sulfate 347kg are added in 2.84 ten thousand mg/litre of nitrogen, and heating makes solution temperature at 80 to 95 °C, stir, until
Aluminum sulfate dissolution, stirring are cooled to 0 °C with ice water, static 12 hours, filtering, to the solution for filtering off precipitating be evaporated concentration,
Crystallisation by cooling, centrifuge separation, is obtained the alum white precipitate 860kg containing the crystallization water.By surplus solution be concentrated by evaporation to
350 liters, the calorific value 5100kcal/kg of solution detection, total sulfur content is less than 1%.To alum with pure water reheat dissolution,
Cooling, crystallization, centrifuge separation, drying, obtain the product for meeting GB25592-2010.
In three above embodiment, the alum obtained can also be heated to 800 °C or more decomposition and generate three oxidations
Two aluminium, ammonia, SO3, aluminum oxide are sold as high added value ceramic raw material, and ammonia and SO3 are produced with cooling absorb of ammonium hydroxide
Sulphur ammonium.Method provided by the invention is not only able to processing organic wastewater, and can be by handling and producing aluminum sulfate
Ammonium is sold, or even is able to produce out the ceramics of high added value and is sold, and makes to spend into present treatment organic wastewater originally, is led to
It crosses simple technique to generate, generates huge income.It is also beneficial to the protection of environment simultaneously.
Although the present invention has been described by way of example and in terms of the preferred embodiments, they be not it is for the purpose of limiting the invention, it is any ripe
This those skilled in the art is practised, without departing from the spirit and scope of the invention, can make various changes or retouch from working as, therefore guarantor of the invention
Shield range should be subject to what claims hereof protection scope was defined.
Claims (10)
1. a kind of organic liquid waste resource utilization method containing ammonium sulfate, comprising the following steps: step 1: throwing organic liquid waste
Add 0.1% -8% auxiliary agent with the equimolar aluminum sulfate of sulphur ammonium content and waste liquid volume in organic liquid waste, and heating keeps aluminum sulfate molten
Solution；Step 2: it is cooling to organic liquid waste, so that organic liquid waste is generated alum crystalline deposit；Step 3: be separated by solid-liquid separation,
The alum solid separated is after drying, by standard GB25592-2010 detection qualification, packing and selling；Step 4: right
The solution of removing solid crystal precipitating is evaporated concentration, and evaporation condensate simultaneously send biochemical device to carry out sewage treatment；Step 5:
Concentrate is discharged into tank or slot and carries out cooling and standings, stands the bottom liquid and crystalline deposit of formation, concentrate floats on above the liquid of bottom,
Bottom liquid is entered into third step, concentrate enters the 6th step；Step 6: the concentrate of removal precipitating and bottom liquid is discharged into product storage
Tank obtains furnace fuel oil, to sell by the qualified laggard marketing of oily (GB25989-2010) standard detection of furnace fuel.
2. the method as described in claim 1, it is characterised in that: if containing acrylonitrile in organic wastewater, the 6th step are as follows: use
Processing method be incinerator special processing.
3. the method as described in claim 1, it is characterised in that: contain ammonium sulfate, the quality hundred of ammonium sulfate in organic liquid waste
Dividing than content is 2% -35%, and content of organics is 5% -63%, remaining is water, in the first step, is first carried out to ammonium sulphate content
It tests and analyzes, to adding equimolar aluminum sulfate in solution, the aluminum sulfate added is anhydrous slufuric acid aluminium or containing the crystallization water
Aluminum sulfate, the aluminum sulfate added are powdered or block or solution shape.
4. the method as described in claim 1-3 any claim, it is characterised in that: the aluminum sulfate added is powdered
Or block or solution shape.
5. the method as described in claim 1-3 any claim, it is characterised in that: in the first step, the auxiliary agent added is positive
The one or more of propyl alcohol, propilolic alcohol, ethylene glycol, acetylacetone,2,4-pentanedione, n-butanol, isobutanol, glyceryl triacetate, n-amyl alcohol are thrown
Adding ratio is 0.1%-the 8% of waste liquid volume.
6. the method as described in claim 1-3 any claim, it is characterised in that: the method obtains in the third step
Alum can also heat resolve, produce the aluminium oxide sale of high-purity, ammonia and the SO3 ammonium hydroxide for decomposing generation is cold
But it absorbs, forms ammonium sulfate solution, produce sulphur ammonium.
7. the method as described in claim 1-3 any claim, it is characterised in that: the alum obtained in the third step
It can also be heated to 800 °C or more decomposition and generate aluminum oxide, ammonia, SO3, aluminum oxide is former as high added value ceramics
Material sale, ammonia and SO3 absorb production sulphur ammonium with ammonium hydroxide is cooling.
8. the method as described in claim 1-3 any claim, not high to unqualified or credit rating in the third step
The heating of alum pure water is re-dissolved, is cooled down, crystallizing, separating, drying to obtain the production for complying with standard GB25592-2010
Product.
9. the method as described in claim 1-3 any claim, in the third step, the separation of solid and liquid is using filtering, pressure
One or more of methods of filter, sedimentation, centrifuge separation are used in combination.
10. the method as described in claim 1-3 any claim, it is characterised in that: in step 6, the furnace fuel
Oily and other fuel oil mixed sellings use, or are delivered to CWS system multifuel combustion together with coal and utilize.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201910006764.4A CN109650627A (en) | 2019-01-04 | 2019-01-04 | A kind of organic liquid waste resource utilization method containing ammonium sulfate |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910006764.4A CN109650627A (en) | 2019-01-04 | 2019-01-04 | A kind of organic liquid waste resource utilization method containing ammonium sulfate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110330035A (en) * | 2019-08-13 | 2019-10-15 | 青岛哈工资源环境技术有限公司 | System for recycling ammonium sulfate and organic matter in evaporation concentrated solution of acrylonitrile dilute ammonium sulfate solution and using method thereof |
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| CN108439430A (en) * | 2018-05-10 | 2018-08-24 | 扬州康龙环保工程有限公司 | The method that ammonium thiocyanate and ammonium sulfate are extracted in oven gas ammonia process of desulfurization waste liquid |
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| CN1590300A (en) * | 2003-12-15 | 2005-03-09 | 镇江市农业科学研究所 | Method of manufacturing industrial ammonium aluminium sulfate using waste liquid in production of fosetyl-aluminium bacteriocide |
| CN102381723A (en) * | 2011-07-25 | 2012-03-21 | 北京世纪地和科技有限公司 | Method for extracting aluminium oxide from pulverized fuel ash |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110330035A (en) * | 2019-08-13 | 2019-10-15 | 青岛哈工资源环境技术有限公司 | System for recycling ammonium sulfate and organic matter in evaporation concentrated solution of acrylonitrile dilute ammonium sulfate solution and using method thereof |
| CN110330035B (en) * | 2019-08-13 | 2022-05-13 | 青岛哈工资源环境技术有限公司 | System for recycling ammonium sulfate and organic matter in evaporation concentrated solution of acrylonitrile dilute ammonium sulfate solution and using method thereof |
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Application publication date: 20190419 |