CN106431506A - Nitrogen fertilizer containing amide nitrogen and nitrate nitrogen and method for treating concentrated nitric acid contained wastewater - Google Patents

Nitrogen fertilizer containing amide nitrogen and nitrate nitrogen and method for treating concentrated nitric acid contained wastewater Download PDF

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Publication number
CN106431506A
CN106431506A CN201610822079.5A CN201610822079A CN106431506A CN 106431506 A CN106431506 A CN 106431506A CN 201610822079 A CN201610822079 A CN 201610822079A CN 106431506 A CN106431506 A CN 106431506A
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solution
nitric acid
concentrated nitric
waste water
nitrogen
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CN106431506B (en
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刘晓鹏
王吉财
闫峰
马强
杨文芳
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Guangfeng Jin Yuan (beijing) Technology Co Ltd
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Guangfeng Jin Yuan (beijing) Technology Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05CNITROGENOUS FERTILISERS
    • C05C5/00Fertilisers containing other nitrates
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05CNITROGENOUS FERTILISERS
    • C05C11/00Other nitrogenous fertilisers
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/16Nitrogen compounds, e.g. ammonia

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Fertilizers (AREA)
  • Processing Of Solid Wastes (AREA)
  • Removal Of Specific Substances (AREA)

Abstract

The invention relates to the field of wastewater treatment and particularly provides nitrogen fertilizer containing amide nitrogen and nitrate nitrogen and a method for treating concentrated nitric acid contained wastewater. The method comprises the following steps: firstly, preparing a carbonyl-containing alkaline substance solution; then, adding the concentrated nitric acid contained wastewater to the solution during stirring, performing solid-liquid separation after thorough reaction to obtain the nitrogen fertilizer containing amide nitrogen and nitrate nitrogen. The method has the advantages of being efficient, reliable, simple in technological process, convenient to operate and low in cost; the reaction only takes 0.5 to 2 hours, the nitrogen conversion rate is high, the mass percentage of the residual nitrogen in the concentrated nitric acid contained wastewater after treatment is only 0.01%-0.1%, and the converted nitrogen fertilizer can be directly used as crop fertilizer. Accordingly, the method has the advantages of protecting the environment, creating useful resources and realizing good economic benefits.

Description

The nitrogenous fertilizer of a kind of amide containing state nitrogen and nitrate nitrogen and process method containing concentrated nitric acid waste water
Technical field
The present invention relates to sewage treatment area, the nitrogenous fertilizer in particular to a kind of amide containing state nitrogen and nitrate nitrogen and place The method containing concentrated nitric acid waste water for the reason.
Background technology
At present, chip factory produces in chip processes, can produce a kind of concentrated nitric acid waste water, concentration of nitric acid (quality hundred in waste water Divide ratio) up to 95%, the waste water containing concentrated nitric acid is processed with the technique of alkaline matter neutralization after having been used up diluting, and processes Need in journey to consume a large amount of clear water and alkaline matter, the production cost that process product is carried out with polish is too high, and causing cannot be right It is comprehensively utilized, and after draining into water body, causes water body serious eutrophication, easily causes secondary pollution to water body;Therefore Said method has that purification of waste water difficulty is big, technological process length, production cost are high, easily cause secondary pollution problems.
In view of this, the special proposition present invention.
Content of the invention
The first object of the present invention is to provide a kind of method processing containing concentrated nitric acid waste water, the method have efficiently, can Lean on, advantage that technological process is simple, easy and simple to handle and with low cost.
The second object of the present invention is to provide the nitrogenous fertilizer of a kind of amide containing state nitrogen and nitrate nitrogen, and this nitrogenous fertilizer adopts above-mentioned side Method prepares, and prepares the efficiency high of nitrogenous fertilizer, environmental friendliness, saving water resource using said method.
In order to realize the above-mentioned purpose of the present invention, spy employs the following technical solutions:
The invention provides a kind of method processing containing concentrated nitric acid waste water, comprise the following steps:
Prepare the solution of the alkaline matter containing carbonyl first, then, under conditions of stirring, concentrated nitric acid waste water will be contained and add To in solution, after question response is complete, solid-liquid separation, obtain the nitrogenous fertilizer of amide containing state nitrogen and nitrate nitrogen.
In the present invention, anti-with the alcoholysis of nitrate anion nitrogen oxygen single key structure using the carbonyl structure in the alkaline matter containing carbonyl Should, make above-mentioned solution and nitrate anion react the nitrogenous fertilizer of generation amide containing state nitrogen and nitrate nitrogen, thus reach making in waste water nitric acid no The beneficial effect of evilization;Additionally, the present invention also can be processed so as to innoxious to the hydrochloric acid in waste water.The method has height Effect, reliability, technological process advantage simple, easy and simple to handle and with low cost, reaction only needs 0.5-2 hour, and conversion rate of nitrogen is high, warp In waste water containing concentrated nitric acid after process, the mass percent of contained remaining nitrogen is only 0.01-0.1%.
Further, the solvent of the solution of the described alkaline matter containing carbonyl is water, or, the solution after solid-liquid separation and clear Wash the water after nitrogenous fertilizer.
Solution after from solid-liquid separation and the water after cleaning nitrogenous fertilizer can be realized following as solvent in subsequent technique Ring uses, and can reduce the addition of fresh water, realize integrated artistic and do not produce new pollutant, do not cause secondary pollution to environment, Realize comprehensive utilization of resources, the target of saving water resource simultaneously.
Preferably, in the solution of the described alkaline matter containing carbonyl, the described alkaline matter containing carbonyl and described solvent Volume ratio be 1-2:1;In the present invention, above-mentioned volume ratio is typical but non-limiting to be 1:1、1.1:1、1.2:1、1.3:1、 1.4:1、1.5:1、1.6:1、1.7:1、1.8:1、1.9:1 or 2:1.
Preferably, described waste water containing concentrated nitric acid and the volume ratio of the solution of the described alkaline matter containing carbonyl are 1-2:1;This In invention, above-mentioned volume ratio is typical but non-limiting to be 1:1、1.1:1、1.2:1、1.3:1、1.4:1、1.5:1、1.6:1、 1.7:1、1.8:1、1.9:1 or 2:1.
In said method, by control the described alkaline matter containing carbonyl and described solvent volume ratio and described containing dense nitre The volume ratio of the solution of sour waste water and the described alkaline matter containing carbonyl to optimize chemical reaction, make concentrated nitric acid successful conversion be containing Amidonitrogen and the nitrogenous fertilizer of nitrate nitrogen.
Further, the described method processing containing concentrated nitric acid waste water, comprises the following steps:
S1, the aqueous solution of the alkaline matter containing carbonyl for the preparation are as solution A;
S2, stirring under conditions of, concentrated nitric acid waste water will be contained and be added in solution A, after question response is complete, solid-liquid separation, Obtain the nitrogenous fertilizer of amide containing state nitrogen and nitrate nitrogen;
S3, preparation B solution:Described B solution is by the water after nitrogenous fertilizer in the alkaline matter containing carbonyl, cleaning S2 and S2 solid-liquid Solution composition after separating;
S4, stirring under conditions of, concentrated nitric acid waste water will be contained and be added in B solution, after question response is complete, solid-liquid separation, Obtain the nitrogenous fertilizer of amide containing state nitrogen and nitrate nitrogen.
In said method, the solvent of solution A is water, the solvent of B solution be nitrogenous fertilizer in cleaning S2 after water and S2 solid-liquid divide From after solution it is clear that decreasing the consumption of fresh water in subsequent treatment process, saving water resource.
Further, methods described is further comprising the steps of:S5, preparation C solution:Described C solution is by the alkalescence containing carbonyl Water after nitrogenous fertilizer in material, cleaning S4 and the solution composition after S4 solid-liquid separation;
S6, stirring under conditions of, concentrated nitric acid waste water will be contained and be added in C solution, after question response is complete, solid-liquid separation, Obtain the nitrogenous fertilizer of amide containing state nitrogen and nitrate nitrogen.
Further, the described alkaline matter containing carbonyl is amide, or the mixture of carboxylic acid and amide.Amide is in weak base Property, with concentrated nitric acid, alcoholysis reaction can occur, generate the nitrogenous fertilizer of amidonitrogen and nitrate nitrogen;Hydroxyl in carboxylic acid is by the amine of amide Base replaces generation amide substance, and newly-generated amide substance occurs alcoholysis reaction with concentrated nitric acid, generates amidonitrogen and nitre The nitrogenous fertilizer of state nitrogen.
Further, described carboxylic acid be formic acid, acetic acid, propanoic acid and butanoic acid any one or at least two mixture;
Described amide be Methanamide, propionic acid amide. and phosphoamide any one or at least two mixture.
Formic acid also known as formic acid, are simplest carboxylic acids, colourless irritant abnormal smells from the patient, formic acid can with water, ethanol, ether and Glycerol is arbitrarily miscible, and most polar organic solvent is miscible.Acetic acid is also glacial acetic acid, can be dissolved in water, ethanol, ether, four The organic solvent such as chlorination carbon and glycerol.Propanoic acid (propanoic acid), also known as propionic acid, water-miscible, be dissolved in ethanol, third Ketone and ether.Butanoic acid is also known as butyric acid, soluble in water, and being soluble in ethanol, propylene glycol, ether, most of volatile oil and major part has Machine solvent.Methanamide is a kind of compound, colourless transparent liquid, slightly ammonia taste, can with water, methanol, ethanol, acetic acid, acetone, two Oxygen six ring, ethylene glycol, phenol and lower member ester are miscible.Propionic acid amide. is white plates crystal, is dissolved in water, ethanol, ether and chloroform.Carbon Amide is also called carbamide, is colourless or white needles or bar-shaped crystalline solid, is dissolved in water, formaldehyde, liquid ammonia and alcohol.
Further, the mixing speed of described stirring is 10-200r/min.In the present invention, above-mentioned mixing speed typical case but Nonrestrictive for 10r/min, 20r/min, 30r/min, 40r/min, 50r/min, 60r/min, 70r/min, 80r/min, 90r/min、100r/min、110r/min、120r/min、130r/min、140r/min、150r/min、160r/min、170r/ Min, 180r/min, 190r/min or 200r/min.
It should be noted that should ensure that reaction temperature in course of reaction in the range of 30-50 DEG C.
Further, described waste water containing concentrated nitric acid is concentrated nitric acid copper-containing wastewater.
Further, the described method processing containing concentrated nitric acid waste water, comprises the following steps:
S1, prepare the aqueous solution of alkaline matter containing carbonyl as solution A, wherein, the described alkaline matter containing carbonyl with The volume ratio of water is 1-2:1;
Concentrated nitric acid waste water will be contained while S2, stirring solution A to be added in solution A, after question response is complete, solid-liquid separation, Obtain the nitrogenous fertilizer of amide containing state nitrogen and nitrate nitrogen, wherein, described waste water containing concentrated nitric acid is 1-2 with the volume ratio of described solution A:1;
S3, preparation B solution:Described B solution is by the water after nitrogenous fertilizer in the alkaline matter containing carbonyl, cleaning S2 and S2 solid-liquid Solution composition after separating, wherein, cleans the water after nitrogenous fertilizer in S2 and the volume sum of solution after S2 solid-liquid separation and institute The ratio stating the volume of alkaline matter containing carbonyl is 1:1-2;
Concentrated nitric acid waste water will be contained while S4, stirring B solution to be added in B solution, after question response is complete, solid-liquid separation, Obtain the nitrogenous fertilizer of amide containing state nitrogen and nitrate nitrogen, wherein, described waste water containing concentrated nitric acid is 1-2 with the volume ratio of described B solution:1;
S5, preparation C solution:Described C solution is by the water after nitrogenous fertilizer in the alkaline matter containing carbonyl, cleaning S4 and S4 solid-liquid Solution composition after separating, wherein, cleans the water after nitrogenous fertilizer in S4 and the volume sum of solution after S4 solid-liquid separation and institute The ratio stating the volume of alkaline matter containing carbonyl is 1:1-2;
Concentrated nitric acid waste water will be contained while S6, stirring C solution to be added in C solution, after question response is complete, solid-liquid separation, Obtain the nitrogenous fertilizer of amide containing state nitrogen and nitrate nitrogen, wherein, described waste water containing concentrated nitric acid is 1-2 with the volume ratio of described C solution:1;
The mixing speed of described stirring is 10-200r/min;Described waste water containing concentrated nitric acid is concentrated nitric acid copper-containing wastewater.
Above-mentioned process contains the method carbonyl structure of concentrated nitric acid waste water and the alcoholysis reaction of nitrate anion nitrogen oxygen single key structure, makes State solution and react, with nitrate anion, the nitrogenous fertilizer generating amide containing state nitrogen and nitrate nitrogen, thus reach making innoxious the having of nitric acid in waste water Beneficial effect;Adopt reverse piecewise processing technique simultaneously, recycle the water after cleaning nitrogenous fertilizer and the solution after solid-liquid separation is made For the solvent of B solution and C solution, it is not only able to reduce secondary pollution moreover it is possible to reduce the consumption of fresh water, has saved water resource, Both decrease sewage quantity, alleviated sewage disposal difficulty, decrease cost again;When above-mentioned waste water containing concentrated nitric acid is concentrated nitric acid cupric Moreover it is possible to copper ion in orienting enriching waste water during waste water, it is that the technique of later collection metallic copper creates favorable conditions.
It should be noted that above-mentioned solid-liquid separation adopts centrifugal separation, the nitrogenous fertilizer of amide containing state nitrogen and nitrate nitrogen is solid Body is separated, packaging and storage.
Present invention also offers the nitrogenous fertilizer of a kind of amide containing state nitrogen and nitrate nitrogen, this nitrogenous fertilizer is to be prepared by said method , the efficiency high of nitrogenous fertilizer, environmental friendliness, saving water resource are prepared using said method.
Compared with prior art, beneficial effects of the present invention are:
The method that a kind of process that the present invention provides contains concentrated nitric acid waste water has that efficient, reliability, technological process be simple, operation Advantage easy and with low cost, reaction only needs 0.5-2 hour, and conversion rate of nitrogen is high, institute in waste water containing concentrated nitric acid after treatment Mass percent containing remaining nitrogen is only 0.01-0.1%, and the nitrogenous fertilizer being transformed therefore can be gone up directly as the fertilizer of crops Method of stating also creates beneficial resource while protecting environment, good in economic efficiency.
In addition, by controlling the volume ratio of the described alkaline matter containing carbonyl and described solvent and described waste water containing concentrated nitric acid To optimize chemical reaction with the volume ratio of the solution of the described alkaline matter containing carbonyl, to make concentrated nitric acid successful conversion be amide containing state Nitrogen and the nitrogenous fertilizer of nitrate nitrogen;Solution after from solid-liquid separation and the water after cleaning nitrogenous fertilizer can be in subsequent techniques as solvent Middle realization recycles, and can reduce the addition of fresh water, realize integrated artistic and do not produce new pollutant, do not cause two to environment Secondary pollution, realizes comprehensive utilization of resources, the target of saving water resource simultaneously;The reverse piecewise processing technique that the present invention adopts, follows Ring is used the water after cleaning nitrogenous fertilizer and the solution after solid-liquid separation as the solvent of B solution and C solution, is not only able to reduce two Secondary pollution, moreover it is possible to reduce the consumption of fresh water, has been saved water resource, has both been decreased sewage quantity, alleviated sewage disposal difficulty, and Decrease cost;Copper ion when above-mentioned waste water containing concentrated nitric acid is concentrated nitric acid copper-containing wastewater moreover it is possible in orienting enriching waste water, be The technique of later collection metallic copper creates favorable conditions.
Amide containing state nitrogen and the nitrogenous fertilizer of nitrate nitrogen that the present invention provides, this nitrogenous fertilizer is prepared using said method, adopts Said method prepares the efficiency high of nitrogenous fertilizer, environmental friendliness, saving water resource.
Specific embodiment
Below in conjunction with embodiment, embodiment of the present invention is described in detail, but those skilled in the art will Understand, the following example is merely to illustrate the present invention, and be not construed as limiting the scope of the present invention.Unreceipted concrete in embodiment Condition person, the condition according to normal condition or manufacturer's suggestion is carried out.
The invention provides a kind of method processing containing concentrated nitric acid waste water, comprise the following steps:
Prepare the solution of the alkaline matter containing carbonyl first, then, under conditions of stirring, concentrated nitric acid waste water will be contained and add To in solution, after question response is complete, solid-liquid separation, obtain the nitrogenous fertilizer of amide containing state nitrogen and nitrate nitrogen.
With reference to embodiment and specific embodiment, the present invention is further detailed explanation.
Embodiment 1
A kind of method processing containing concentrated nitric acid waste water, comprises the following steps:
S1, the aqueous solution of preparation Methanamide;
S2, stirring under conditions of, waste water containing concentrated nitric acid is added in the aqueous solution of Methanamide, after question response is complete, Solid-liquid separation, obtains the nitrogenous fertilizer of amide containing state nitrogen and nitrate nitrogen.
Embodiment 2
A kind of method processing containing concentrated nitric acid waste water, comprises the following steps:
The aqueous solution of the mixture of S1, preparation Methanamide and propanoic acid;
S2, stirring under conditions of, in the aqueous solution of mixture waste water containing concentrated nitric acid being added to Methanamide and propanoic acid, After question response is complete, solid-liquid separation, obtain the nitrogenous fertilizer of amide containing state nitrogen and nitrate nitrogen;
Wherein, the ratio of the volume of the volume sum of the mixture of Methanamide and propanoic acid and water is 1.5:1;
The mixing speed of above-mentioned stirring is 30r/min;Above-mentioned waste water containing concentrated nitric acid is 1 with the volume ratio of above-mentioned solution A:1.
Embodiment 3
A kind of method processing containing concentrated nitric acid waste water, comprises the following steps:
S1, the aqueous solution of the mixture of preparation Methanamide, propionic acid amide. and acetic acid;
S2, stirring under conditions of, waste water containing concentrated nitric acid is added to the water of the mixture of Methanamide, propionic acid amide. and acetic acid In solution, after question response is complete, solid-liquid separation, obtain the nitrogenous fertilizer of amide containing state nitrogen and nitrate nitrogen;
Wherein, the ratio of the volume of the volume sum of the mixture of above-mentioned Methanamide, propionic acid amide. and acetic acid and water is 2:1;
The mixing speed of above-mentioned stirring is 90r/min;Above-mentioned waste water containing concentrated nitric acid is 1.2 with the volume ratio of above-mentioned solution A: 1;Above-mentioned waste water containing concentrated nitric acid is concentrated nitric acid copper-containing wastewater.
Embodiment 4
A kind of method processing containing concentrated nitric acid waste water, comprises the following steps:
S1, the aqueous solution of the mixture of preparation Methanamide, formic acid and propanoic acid are as solution A;
S2, stirring under conditions of, concentrated nitric acid waste water will be contained and be added in solution A, after question response is complete, solid-liquid separation, Obtain the nitrogenous fertilizer of amide containing state nitrogen and nitrate nitrogen;
S3, preparation B solution:Described B solution is by the water after nitrogenous fertilizer in the mixture of Methanamide, formic acid and propanoic acid, cleaning S2 And the solution composition after S2 solid-liquid separation;
S4, stirring under conditions of, concentrated nitric acid waste water will be contained and be added in B solution, after question response is complete, solid-liquid separation, Obtain the nitrogenous fertilizer of amide containing state nitrogen and nitrate nitrogen;
Wherein, the ratio of the volume of the volume sum of the mixture of Methanamide, formic acid and propanoic acid and water is 2:1;Above-mentioned contain Concentrated nitric acid waste water is 1.2 with the volume ratio of above-mentioned solution A:1;
Water after the volume sum of the mixture of Methanamide, formic acid and propanoic acid and nitrogenous fertilizer in above-mentioned cleaning S2 and S2 solid-liquid divide From after solution volume sum ratio be 1.5:1;Above-mentioned waste water containing concentrated nitric acid is 1.8 with the volume ratio of above-mentioned B solution:1;
The mixing speed of above-mentioned stirring is 120r/min;Above-mentioned waste water containing concentrated nitric acid is concentrated nitric acid copper-containing wastewater.
Embodiment 5
A kind of method processing containing concentrated nitric acid waste water, comprises the following steps:
, as solution A, wherein, phosphoamide is 1.3 with the volume ratio of water for S1, the aqueous solution of preparation phosphoamide:1;
Concentrated nitric acid waste water will be contained while S2, stirring solution A to be added in solution A, after question response is complete, solid-liquid separation, Obtain the nitrogenous fertilizer of amide containing state nitrogen and nitrate nitrogen, wherein, above-mentioned waste water containing concentrated nitric acid is 1 with the volume ratio of above-mentioned solution A:1;
S3, preparation B solution:Described B solution is by molten after the water after nitrogenous fertilizer in phosphoamide, cleaning S2 and S2 solid-liquid separation Liquid forms, and wherein, cleans the volume of the water after nitrogenous fertilizer in S2 and the volume sum of solution after S2 solid-liquid separation and phosphoamide Ratio be 1:1.4;
Concentrated nitric acid waste water will be contained while S4, stirring B solution to be added in B solution, after question response is complete, solid-liquid separation, Obtain the nitrogenous fertilizer of amide containing state nitrogen and nitrate nitrogen, wherein, above-mentioned waste water containing concentrated nitric acid is 1.4 with the volume ratio of above-mentioned B solution:1;
S5, preparation C solution:Described C solution is by molten after the water after nitrogenous fertilizer in phosphoamide, cleaning S4 and S4 solid-liquid separation Liquid forms, and wherein, cleans the volume of the water after nitrogenous fertilizer in S4 and the volume sum of solution after S4 solid-liquid separation and phosphoamide Ratio be 1:1.7;
Concentrated nitric acid waste water will be contained while S6, stirring C solution to be added in C solution, after question response is complete, solid-liquid separation, Obtain the nitrogenous fertilizer of amide containing state nitrogen and nitrate nitrogen, wherein, above-mentioned waste water containing concentrated nitric acid is 1.7 with the volume ratio of above-mentioned C solution:1;
The mixing speed of above-mentioned stirring is 150r/min;Above-mentioned waste water containing concentrated nitric acid is concentrated nitric acid copper-containing wastewater.
Embodiment 6
A kind of method processing containing concentrated nitric acid waste water, comprises the following steps:
S1, the aqueous solution of the mixture of preparation propionic acid amide., phosphoamide and butanoic acid are as solution A, wherein, propionic acid amide., phosphinylidyne The mixture of amine and butanoic acid and the volume ratio of water are 1.3:1;
Concentrated nitric acid waste water will be contained while S2, stirring solution A to be added in solution A, after question response is complete, solid-liquid separation, Obtain the nitrogenous fertilizer of amide containing state nitrogen and nitrate nitrogen, wherein, above-mentioned waste water containing concentrated nitric acid is 1.5 with the volume ratio of above-mentioned solution A:1;
S3, preparation B solution:Described B solution is by the mixture of propionic acid amide., phosphoamide and butanoic acid, cleaning S2 after nitrogenous fertilizer Solution composition after water and S2 solid-liquid separation, wherein, the water after nitrogenous fertilizer and the solution after S2 solid-liquid separation in cleaning S2 The ratio of the volume of the mixture of volume sum and described propionic acid amide., phosphoamide and butanoic acid is 1:1.6;
Concentrated nitric acid waste water will be contained while S4, stirring B solution to be added in B solution, after question response is complete, solid-liquid separation, Obtain the nitrogenous fertilizer of amide containing state nitrogen and nitrate nitrogen, wherein, above-mentioned waste water containing concentrated nitric acid is 1.6 with the volume ratio of above-mentioned B solution:1;
S5, preparation C solution:Described C solution is by the mixture of propionic acid amide., phosphoamide and butanoic acid, cleaning S4 after nitrogenous fertilizer Solution composition after water and S4 solid-liquid separation, wherein, the water after nitrogenous fertilizer and the solution after S4 solid-liquid separation in cleaning S4 The ratio of the volume of the mixture of volume sum and propionic acid amide., phosphoamide and butanoic acid is 1:1.5;
Concentrated nitric acid waste water will be contained while S6, stirring C solution to be added in C solution, after question response is complete, solid-liquid separation, Obtain the nitrogenous fertilizer of amide containing state nitrogen and nitrate nitrogen, wherein, described waste water containing concentrated nitric acid is 1.5 with the volume ratio of described C solution:1;
The mixing speed of above-mentioned stirring is 170r/min;Above-mentioned waste water containing concentrated nitric acid is concentrated nitric acid copper-containing wastewater.
Comparative example 1
A kind of method processing containing concentrated nitric acid waste water, comprises the following steps:
The aqueous solution of the mixture of S1, preparation Methanamide and propanoic acid;
S2, stirring under conditions of, in the aqueous solution of mixture waste water containing concentrated nitric acid being added to Methanamide and propanoic acid, After question response is complete, solid-liquid separation, obtain the nitrogenous fertilizer of amide containing state nitrogen and nitrate nitrogen;
Wherein, the ratio of the volume of the volume of the mixture of Methanamide and propanoic acid and water is 0.2:1;
The mixing speed of above-mentioned stirring is 5r/min;Above-mentioned waste water containing concentrated nitric acid is 3 with the volume ratio of above-mentioned solution A:1.
Comparative example 2
A kind of method processing containing concentrated nitric acid waste water, comprises the following steps:
S1, the aqueous solution of the mixture of preparation Methanamide, propionic acid amide. and acetic acid;
S2, stirring under conditions of, waste water containing concentrated nitric acid is added to the water of the mixture of Methanamide, propionic acid amide. and acetic acid In solution, after question response is complete, solid-liquid separation, obtain the nitrogenous fertilizer of amide containing state nitrogen and nitrate nitrogen;
Wherein, the ratio of the volume of the volume of the mixture of Methanamide, propionic acid amide. and acetic acid and water is 2.2:1;
The mixing speed of above-mentioned stirring is 5r/min;Above-mentioned waste water containing concentrated nitric acid is 0.8 with the volume ratio of above-mentioned solution A: 1;Above-mentioned waste water containing concentrated nitric acid is concentrated nitric acid copper-containing wastewater.
Comparative example 3
A kind of method processing containing concentrated nitric acid waste water, comprises the following steps:
S1, the aqueous solution of the mixture of preparation Methanamide, formic acid and propanoic acid are as solution A;
S2, stirring under conditions of, concentrated nitric acid waste water will be contained and be added in solution A, after question response is complete, solid-liquid separation, Obtain the nitrogenous fertilizer of amide containing state nitrogen and nitrate nitrogen;
S3, preparation B solution:Described B solution is by the water after nitrogenous fertilizer in the mixture of Methanamide, formic acid and propanoic acid, cleaning S2 And the solution composition after S2 solid-liquid separation;
S4, stirring under conditions of, concentrated nitric acid waste water will be contained and be added in B solution, after question response is complete, solid-liquid separation, Obtain the nitrogenous fertilizer of amide containing state nitrogen and nitrate nitrogen;
Wherein, the ratio of the volume of the volume of the mixture of Methanamide, formic acid and propanoic acid and water is 3:1;Above-mentioned containing dense nitre Sour waste water is 3 with the volume ratio of above-mentioned solution A:1;
Water after nitrogenous fertilizer in the volume of the mixture of Methanamide, formic acid and propanoic acid and above-mentioned cleaning S2 and S2 solid-liquid separation The ratio of the volume of solution afterwards is 0.2:1;Above-mentioned waste water containing concentrated nitric acid is 0.2 with the volume ratio of above-mentioned B solution:1;
The mixing speed of above-mentioned stirring is 220r/min;Above-mentioned waste water containing concentrated nitric acid is concentrated nitric acid copper-containing wastewater.
Comparative example 4
A kind of method processing containing concentrated nitric acid waste water, comprises the following steps:
, as solution A, wherein, phosphoamide is 2.5 with the volume ratio of water for S1, the aqueous solution of preparation phosphoamide:1;
Concentrated nitric acid waste water will be contained while S2, stirring solution A to be added in solution A, after question response is complete, solid-liquid separation, Obtain the nitrogenous fertilizer of amide containing state nitrogen and nitrate nitrogen, wherein, above-mentioned waste water containing concentrated nitric acid is 2.5 with the volume ratio of above-mentioned solution A:1;
S3, preparation B solution:Described B solution is by molten after the water after nitrogenous fertilizer in phosphoamide, cleaning S2 and S2 solid-liquid separation Liquid forms, and wherein, cleans the volume of the water after nitrogenous fertilizer in S2 and the volume sum of solution after S2 solid-liquid separation and phosphoamide Ratio be 1:0.4;
Concentrated nitric acid waste water will be contained while S4, stirring B solution to be added in B solution, after question response is complete, solid-liquid separation, Obtain the nitrogenous fertilizer of amide containing state nitrogen and nitrate nitrogen, wherein, above-mentioned waste water containing concentrated nitric acid is 0.4 with the volume ratio of above-mentioned B solution:1;
S5, preparation C solution:Described C solution is by molten after the water after nitrogenous fertilizer in phosphoamide, cleaning S4 and S4 solid-liquid separation Liquid forms, and wherein, cleans the volume of the water after nitrogenous fertilizer in S4 and the volume sum of solution after S4 solid-liquid separation and phosphoamide Ratio be 1:2.6;
Concentrated nitric acid waste water will be contained while S6, stirring C solution to be added in C solution, after question response is complete, solid-liquid separation, Obtain the nitrogenous fertilizer of amide containing state nitrogen and nitrate nitrogen, wherein, above-mentioned waste water containing concentrated nitric acid is 2.6 with the volume ratio of above-mentioned C solution:1;
The mixing speed of above-mentioned stirring is 260r/min;Above-mentioned waste water containing concentrated nitric acid is concentrated nitric acid copper-containing wastewater.
In order to weigh the actual processing effect to waste water for the method containing concentrated nitric acid waste water for the above-mentioned process, spy is to dense containing concentrated nitric acid Degree identical waste water is respectively adopted embodiment 1-6, comparative example 1-4 and alkali neutralization method and is processed, and remaining after detection process Nitrogen content, result is as shown in table 1.
Remaining nitrogen content after the process of table 1 different disposal method
As shown in Table 1, remaining nitrogen content is processed after waste water containing concentrated nitric acid in waste water 0.1% using the method that the present invention provides Hereinafter, the remaining nitrogen content after processing far below comparative example 1-4 and alkali neutralization method, illustrates that the method for the present invention has conversion rate of nitrogen High advantage;Meanwhile, the waste water of concentration containing concentrated nitric acid and quality all same is adopted with embodiment 1-6, comparative example 1-4 and alkali neutralization Method is processed, and result shows, the method reaction that the present invention provides only needs 0.5-2 hour completely, and in comparative example 1-4 and alkali All longer with the response time of method, method of the present invention efficiency high is described, further, its water consumption is compared, send out The water consumption of the existing present invention is minimum, has saved and has also saved cost while water resource.
In summary, the method that a kind of process that the present invention provides contains concentrated nitric acid waste water has efficient, reliability, technological process Simply, advantage easy and simple to handle and with low cost, reaction only needs 0.5-2 hour, and conversion rate of nitrogen is high, after treatment containing concentrated nitric acid In waste water, the mass percent of contained remaining nitrogen is only 0.01-0.1%.
Although illustrate and describing the present invention with specific embodiment, but it will be appreciated that without departing substantially from the present invention's Many other changes can be made in the case of spirit and scope and change.It is, therefore, intended that in the following claims Including all such changes and modifications belonging in the scope of the invention.

Claims (10)

1. a kind of method processing containing concentrated nitric acid waste water is it is characterised in that comprise the following steps:
First prepare containing carbonyl alkaline matter solution, then, stirring under conditions of, will contain concentrated nitric acid waste water be added to molten In liquid, after question response is complete, solid-liquid separation, obtain the nitrogenous fertilizer of amide containing state nitrogen and nitrate nitrogen.
2. the method processing containing concentrated nitric acid waste water according to claim 1 is it is characterised in that the described basic species containing carbonyl The solvent of the solution of matter is water, or, the solution after solid-liquid separation and the water after cleaning nitrogenous fertilizer;
Preferably, in the solution of the described alkaline matter containing carbonyl, the body of the described alkaline matter containing carbonyl and described solvent Long-pending ratio is 1-2:1;
Preferably, described waste water containing concentrated nitric acid and the volume ratio of the solution of the described alkaline matter containing carbonyl are 1-2:1.
3. the method processing containing concentrated nitric acid waste water according to claim 2 is it is characterised in that comprise the following steps:
S1, the aqueous solution of the alkaline matter containing carbonyl for the preparation are as solution A;
S2, stirring under conditions of, concentrated nitric acid waste water will be contained and be added in solution A, after question response is complete, solid-liquid separation, obtain Amide containing state nitrogen and the nitrogenous fertilizer of nitrate nitrogen;
S3, preparation B solution:Described B solution is by the water after nitrogenous fertilizer in the alkaline matter containing carbonyl, cleaning S2 and S2 solid-liquid separation Solution composition afterwards;
S4, stirring under conditions of, concentrated nitric acid waste water will be contained and be added in B solution, after question response is complete, solid-liquid separation, obtain Amide containing state nitrogen and the nitrogenous fertilizer of nitrate nitrogen.
4. the method processing containing concentrated nitric acid waste water according to claim 3 is it is characterised in that further comprising the steps of:
S5, preparation C solution:Described C solution is by the water after nitrogenous fertilizer in the alkaline matter containing carbonyl, cleaning S4 and S4 solid-liquid separation Solution composition afterwards;
S6, stirring under conditions of, concentrated nitric acid waste water will be contained and be added in C solution, after question response is complete, solid-liquid separation, obtain Amide containing state nitrogen and the nitrogenous fertilizer of nitrate nitrogen.
5. the process according to any one of claim 1-4 contain concentrated nitric acid waste water method it is characterised in that described containing carbonyl Alkaline matter be amide, or the mixture of carboxylic acid and amide.
6. the method processing containing concentrated nitric acid waste water according to claim 5 is it is characterised in that described carboxylic acid is formic acid, second Acid, propanoic acid and butanoic acid any one or at least two mixture;
Described amide be Methanamide, propionic acid amide. and phosphoamide any one or at least two mixture.
7. the process according to any one of claim 1-4 contains the method for concentrated nitric acid waste water it is characterised in that described stirring Mixing speed is 10-200r/min.
8. the process according to any one of claim 1-4 contain concentrated nitric acid waste water method it is characterised in that described containing dense nitre Sour waste water is concentrated nitric acid copper-containing wastewater.
9. the method processing containing concentrated nitric acid waste water according to claim 1 and 2 is it is characterised in that comprise the following steps:
S1, prepare the aqueous solution of alkaline matter containing carbonyl as solution A, wherein, the described alkaline matter containing carbonyl and water Volume ratio is 1-2:1;
Concentrated nitric acid waste water will be contained while S2, stirring solution A to be added in solution A, after question response is complete, solid-liquid separation, obtain Amide containing state nitrogen and the nitrogenous fertilizer of nitrate nitrogen, wherein, described waste water containing concentrated nitric acid is 1-2 with the volume ratio of described solution A:1;
S3, preparation B solution:Described B solution is by the water after nitrogenous fertilizer in the alkaline matter containing carbonyl, cleaning S2 and S2 solid-liquid separation Solution composition afterwards, wherein, the volume sum of the water after nitrogenous fertilizer in cleaning S2 and the solution after S2 solid-liquid separation is contained with described The ratio of the volume of the alkaline matter of carbonyl is 1:1-2;
Concentrated nitric acid waste water will be contained while S4, stirring B solution to be added in B solution, after question response is complete, solid-liquid separation, obtain Amide containing state nitrogen and the nitrogenous fertilizer of nitrate nitrogen, wherein, described waste water containing concentrated nitric acid is 1-2 with the volume ratio of described B solution:1;
S5, preparation C solution:Described C solution is by the water after nitrogenous fertilizer in the alkaline matter containing carbonyl, cleaning S4 and S4 solid-liquid separation Solution composition afterwards, wherein, the volume sum of the water after nitrogenous fertilizer in cleaning S4 and the solution after S4 solid-liquid separation is contained with described The ratio of the volume of the alkaline matter of carbonyl is 1:1-2;
Concentrated nitric acid waste water will be contained while S6, stirring C solution to be added in C solution, after question response is complete, solid-liquid separation, obtain Amide containing state nitrogen and the nitrogenous fertilizer of nitrate nitrogen, wherein, described waste water containing concentrated nitric acid is 1-2 with the volume ratio of described C solution:1;
The mixing speed of described stirring is 10-200r/min;Described waste water containing concentrated nitric acid is concentrated nitric acid copper-containing wastewater.
10. the nitrogenous fertilizer of a kind of amide containing state nitrogen and nitrate nitrogen is it is characterised in that described nitrogenous fertilizer is by any one of claim 1-9 Methods described prepares.
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