CN110255580A - High-concentration sulfuric acid ammonium Recycling Mother Solution processing method - Google Patents
High-concentration sulfuric acid ammonium Recycling Mother Solution processing method Download PDFInfo
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- CN110255580A CN110255580A CN201910713977.0A CN201910713977A CN110255580A CN 110255580 A CN110255580 A CN 110255580A CN 201910713977 A CN201910713977 A CN 201910713977A CN 110255580 A CN110255580 A CN 110255580A
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- sulfuric acid
- acid ammonium
- processing method
- concentration
- solution processing
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/02—Preparation, purification or separation of ammonia
-
- 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
- C01F5/00—Compounds of magnesium
- C01F5/40—Magnesium sulfates
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
- C05D5/00—Fertilisers containing magnesium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Analytical Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention belongs to resource and environment fileds, it is related to a kind of high-concentration sulfuric acid ammonium Recycling Mother Solution processing method, the following steps are included: magnesia powder is added in the ammonium sulfate liquor that concentration is 80~300g/L in (1), heat ammonia still process, Adlerika and ammonia are obtained, ammonia is passed through absorption plant and is recycled;(2) Adlerika described in heating evaporation when there is crystal precipitation, then is cooled and separated, dries, obtains sulfuric acid magnesium products;(3) by the isolated mother liquor return step (1), it is made to carry out heating ammonia still process with the magnesia powder.It is practically free of impurity in the sulfuric acid magnesium products that the present invention obtains, purification & isolation process is reduced compared with other techniques, there is significant economic effect and huge social benefit.
Description
Technical field
The invention belongs to resource and environment fileds, are related to a kind of high-concentration sulfuric acid ammonium Recycling Mother Solution processing method.
Background technique
Ammonium sulphate waste liquor is mainly derived from chemical production field and total amount is huge, and the processing method of ammonium sulphate waste liquor is mainly adopted
Evaporation process is taken to separate salt in solid form.Existing method uses single-action or multiple-effect evaporation method, and needs constantly to mention
For heating steam, steam consumption is high.But energy prices increasingly go up in recent years, lead to cost promotion in traditional evaporation process.
Publication No. discloses a kind of useless with the mixing of ammonium sulfate magnesium sulfate for the Chinese invention patent application of CN107056341A
The method that liquid produces sulfuric acid monohydrate fertiliser containing magnesium and ammonium hydroxide, due to joined in magnesium sulfate ammonium sulfate mixed waste liquor ammonia still process step
Therefore excessive magnesia powder after ammonia still process step, also contains unreacted magnesia and a small amount of Mg in waste liquid
(OH)2, the waste of resource is not only caused, increases solid generation of giving up, also reduces the purity of sulfuric acid magnesium products.Especially in height
G., jelly-like slurry is formd in the processing of concentration ammonium sulfate, further reduced reaction efficiency.
Therefore, this field needs a kind of high-concentration sulfuric acid ammonium Recycling Mother Solution processing method being simple and efficient.
Summary of the invention
The purpose of the present invention is in view of the drawbacks of the prior art, provide a kind of high-concentration sulfuric acid ammonium Recycling Mother Solution processing side
Method.
Specifically, high-concentration sulfuric acid ammonium Recycling Mother Solution processing method of the invention, comprising the following steps:
(1) high-concentration sulfuric acid ammonium salt solution ammonia still process
Magnesia powder is added in the ammonium sulfate liquor that concentration is 80~300g/L, heats ammonia still process, obtains Adlerika
And ammonia, ammonia is passed through absorption plant and is recycled;
(2) magnesium sulfate evaporative crystallization
Adlerika described in heating evaporation when there is crystal precipitation, then is cooled and separated, dries, and obtains magnesium sulfate production
Product;
(3) magnesium sulfate mother liquid recycling
By in above-mentioned isolated sulfuric acid mother liquid of magnesium return step (1), it is made to carry out heating steaming with the magnesia powder
Ammonia.
Preferably, in the magnesia powder in MgO and the ammonium sulfate liquor molar ratio of ammonium ion be 1:(2.01~
5)。
Preferably, heating temperature is 60~95 DEG C in the high-concentration sulfuric acid ammonium salt solution ammonia still process step, when heating a length of 4~
6h, pressure are -0.02MPa to -0.09MPa.
Preferably, heating temperature is 70 DEG C in the high-concentration sulfuric acid ammonium salt solution ammonia still process step.
Preferably, in step (2), the temperature of Adlerika described in heating evaporation is 80~100 DEG C.
Preferably, in step (2), the temperature after cooling is 60~80 DEG C.
Preferably, in step (2), the temperature after cooling is 70 DEG C.
Preferably, in step (2), the temperature of the drying is 40~60 DEG C.
Preferably, the sulfuric acid magnesium products are epsom salt.
Technical solution of the present invention have it is following the utility model has the advantages that
(1) high-concentration sulfuric acid ammonium Recycling Mother Solution processing method of the invention is suitable for the circulation benefit of high-concentration sulfuric acid ammonium mother liquor
With, wherein ammonium ion generates ammonia, and sulfate ion generates magnesium sulfate fertilizer, realizes in high-concentration sulfuric acid ammonium mother liquor
The resource utilization of each ingredient;
(2) high-concentration sulfuric acid ammonium Recycling Mother Solution processing method of the invention is in ammonia still process step due to the magnesia of addition
Amount is small relative to the amount of ammonium ion in solution, therefore, impurity is practically free of in the sulfuric acid magnesium products of acquisition, with other technique phases
Than reducing purification & isolation process, there is significant economic effect and huge social benefit.
Detailed description of the invention
By reading the following detailed description of the preferred embodiment, various other advantages and benefits are common for this field
Technical staff will become clear.The drawings are only for the purpose of illustrating a preferred embodiment, and is not considered as to the present invention
Limitation.
Fig. 1 is the process flow chart of high-concentration sulfuric acid ammonium Recycling Mother Solution processing method of the present invention.
Specific embodiment
In order to fully understand the purpose of the present invention, feature and effect, by following specific embodiments, the present invention is made detailed
It describes in detail bright.For process of the invention in addition to following the description, remaining is all made of the conventional method or device of this field.Following nouns
Term is unless otherwise stated, all have the normally understood meaning of those skilled in the art.
Specifically, as shown in Figure 1, high-concentration sulfuric acid ammonium Recycling Mother Solution processing method of the invention, comprising the following steps:
(1) high-concentration sulfuric acid ammonium salt solution ammonia still process
Magnesia powder is added in the ammonium sulfate liquor that concentration is 80~300g/L, heats, obtains Adlerika and ammonia
Ammonia is passed through absorption plant and recycled by gas.The chemical reaction of generation is as follows:
Preferably, the concentration of the ammonium sulfate liquor is 170~180g/L.
Preferably, in the magnesia powder in MgO and the ammonium sulfate liquor molar ratio of ammonium ion be 1:(2.01~
5)。
The present invention hardly has impurity (impurity in thus obtained sulfuric acid magnesium products by using a small amount of magnesia
Content is extremely low, can be ignored), purification & isolation process is reduced compared with other techniques, have significant economic effect and
Huge social benefit.
Preferably, the heating temperature of the high-concentration sulfuric acid ammonium salt solution ammonia still process step is 60~90 DEG C, preferably 70 DEG C, is added
A length of 4~6h when hot, pressure are -0.02MPa to -0.09MPa.
In the Chinese invention patent of Publication No. CN 107056341A, magnesium sulfate ammonium sulfate mixed waste liquor ammonia still process step
Temperature is high, and energy consumption is high;And the heating temperature of high-concentration sulfuric acid ammonium salt solution ammonia still process step of the present invention is only 70 DEG C or so, energy consumption is significantly
It reduces.
It is further preferred that carrying out the high-concentration sulfuric acid ammonium salt solution ammonia still process step using Rotary Evaporators, wherein water-bath
Pot heating temperature is 70 DEG C, 4~6h of time of ammonia distillation, controls 0.02~0.09Mpa of negative pressure, and the ammonia for reacting generation enters absorption dress
It sets and recycles.Wherein, the absorption plant is the receiving flask of Rotary Evaporators, contains water (absorbent) in receiving flask, generates
Ammonia be only absorbed by the water as ammonium hydroxide, realize recycling for ammonia.
(2) magnesium sulfate evaporative crystallization
Adlerika described in heating evaporation is cooled and separated, dries when there is crystal precipitation, obtains magnesium sulfate production
Product.
Preferably, the temperature of Adlerika described in heating evaporation is 80~100 DEG C.
Preferably, Adlerika described in heating evaporation then stops heating, is cooled to 60 when there is the precipitation of a small amount of crystal
~80 DEG C, preferably 70 DEG C, are then separated by solid-liquid separation.
Wherein, the separation is carried out using separation means commonly used in the art, and the present invention is not specifically limited herein.
Wherein, the magnesium sulfate obtained after separation is epsom salt wet product.
Wherein, the temperature of the drying is 40~60 DEG C, when a length of 0.5~1h of the drying, under the drying condition,
Finally obtain the epsom salt for meeting national standard agricultural magnesium sulfate GB/T26568-2011 requirement.
Wherein, the magnesium sulfate obtained after separation is epsom salt wet product, can also be obtained under other drying conditions
Magnesium sulfate containing the different crystallizations water, 10~60 minutes are dried such as at 100~400 DEG C, and available to meet national standard agricultural
The magnesium sulfate monohydrate that magnesium sulfate GB/T26568-2011 is required.Those skilled in the art can according to need the temperature to drying
It is selected with the time, to obtain corresponding sulfuric acid magnesium products.
(3) magnesium sulfate mother liquid recycling
It will be steamed in sulfuric acid mother liquid of magnesium return step (1) isolated described in step (2) with the magnesia powder
Ammonia.
Contain a large amount of ammonium sulfate in the sulfuric acid mother liquid of magnesium obtained after separation, by will be in mother liquor return step (1)
Make further ammonia still process processing, realizes the effective use of resource.
Preferably, high-concentration sulfuric acid ammonium Recycling Mother Solution processing method of the invention further includes that the sulfuric acid magnesium products that will be obtained claim
The step of packing again.
High-concentration sulfuric acid ammonium Recycling Mother Solution processing method of the invention is suitable for recycling for high-concentration sulfuric acid ammonium mother liquor,
Wherein, ammonium ion generates ammonia, and sulfate ion generates magnesium sulfate fertilizer, realizes the money of each ingredient in ammonium sulfate liquor
Sourceization utilizes.In addition, the amount for the magnesia that the present invention is added in ammonia still process step is small relative to the amount of ammonium ion in solution, because
This, hardly has impurity in the sulfuric acid magnesium products of acquisition, purification & isolation process is reduced compared with other techniques, has significant
Economic effect and huge social benefit.
Embodiment
The present invention is further illustrated below by the mode of embodiment, but does not therefore limit the present invention to the reality
It applies among a range.In the following examples, the experimental methods for specific conditions are not specified, according to conventional methods and conditions.Following implementation
Raw material used in example is that regular market purchase obtains.
Embodiment 1
Light-magnesite powder is added in the ammonium sulfate that concentration is 80g/L, in magnesia powder (in terms of MgO) and solution
The molar ratio of ammonia is 1:2.01.Ammonia still process is carried out using Rotary Evaporators, wherein water-bath heating temperature is 70 DEG C, time of ammonia distillation
For 4h, control negative pressure is 0.07Mpa, and the ammonia for reacting generation enters absorption plant and recycles.
After ammonia still process, the Adlerika from step (1) is heated to 100 DEG C of evaporations, when steaming to there is a small amount of crystallization
When precipitation, stop heating, be cooled to 70 DEG C, after being separated by solid-liquid separation, solid phase is epsom salt wet product, and mother liquor returns to rotation and steams
It sends out and continues reaction cycle utilization in instrument.
The epsom salt wet product that will be obtained dries 1h at 40 DEG C of low temperature, finally obtains and meets the agricultural sulphur of national standard
The epsom salt that sour magnesium GB/T26568-2011 is required.
Embodiment 2
Light-magnesite powder, magnesia powder (in terms of MgO) and solution is added in the ammonium sulfate that concentration is 300g/L
The molar ratio of middle ammonia is 1:5.Ammonia still process is carried out using Rotary Evaporators, wherein water-bath heating temperature is 70 DEG C, and time of ammonia distillation is
6h, control negative pressure are 0.05Mpa, and the ammonia for reacting generation enters absorption plant and recycles.
After ammonia still process, the Adlerika from step (1) is heated to 100 DEG C of evaporations, when steaming to there is a small amount of crystallization
When precipitation, stop heating, be cooled to 70 DEG C, after being separated by solid-liquid separation, solid phase is epsom salt wet product, and liquid returns to rotation and steams
It sends out and continues reaction cycle utilization in instrument.
By obtained epsom salt and ammonium sulfate wet product, 1h is dried at 40 DEG C of low temperature, obtains meeting national standard agriculture
The epsom salt required with magnesium sulfate GB/T26568-2011.
Embodiment 3
Light-magnesite powder, magnesia powder (in terms of MgO) and solution is added in the ammonium sulfate that concentration is 200g/L
The molar ratio of middle ammonia is 1:3.Ammonia still process is carried out using Rotary Evaporators, wherein water-bath heating temperature is 70 DEG C, and time of ammonia distillation is
4h, control negative pressure are 0.09Mpa, and the ammonia for reacting generation enters absorption plant and recycles.
After ammonia still process, the Adlerika from step (1) is heated to 100 DEG C of evaporations, when steaming to there is a small amount of crystallization
When precipitation, stop heating, be cooled to 70 DEG C, after being separated by solid-liquid separation, solid phase is epsom salt wet product, and liquid returns to rotation and steams
It sends out and continues reaction cycle utilization in instrument.
By obtained epsom salt and ammonium sulfate wet product, 0.5h is dried at 50 DEG C of low temperature, obtains meeting national standard
The epsom salt that agricultural magnesium sulfate GB/T26568-2011 is required.
Comparative example
A method of seven water magnesium sulfuric acid fertilizer and ammonium hydroxide being produced with ammonium sulfate magnesium sulfate mixed waste liquor, steps are as follows:
(1) magnesium sulfate ammonium sulfate mixed waste liquor ammonia still process
Magnesium sulfate ammonium sulfate (ammonium sulfate concentrations 200g/L) mixed waste liquor is added in reactor, stirring, metering are opened
Light-magnesite powder is added, wherein NH in MgO and solution is added4 +Molar ratio is 1:0.9;Being passed through and being steam heated to temperature is 105
DEG C, ammonia, which goes out reactor and enters absorption tower, produces ammonium hydroxide, and solution is the impurity such as silicon, calcium a small amount of in magnesium sulfate and light-burning magnesium powder;
After ammonia still process, the Adlerika from step (1) is heated to 100 DEG C of evaporations, when steaming to there is a small amount of crystallization
When precipitation, stop heating, be cooled to 70 DEG C, after being separated by solid-liquid separation, solid phase is epsom salt wet product, and liquid returns to rotation and steams
It sends out and continues reaction cycle utilization in instrument.
By obtained epsom salt and ammonium sulfate wet product, 1h is dried at 40 DEG C of low temperature, obtains epsom salt.
Physicochemical property test
The epsom salt that embodiment 1-3 and comparative example are prepared using disodium ethylene diamine tetraacetate volumetric method below
The purity of product is tested, and test result is shown in Table 1.
The purity test result of 1 epsom salt product of table summarizes
Product | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example |
Epsom salt % | 99.5 | 99.4 | 99.5 | 96 |
High-concentration sulfuric acid ammonium Recycling Mother Solution processing method of the invention is in ammonia still process step due to the amount of the magnesia of addition
Amount relative to ammonium ion in solution is small, therefore, in the sulfuric acid magnesium products of acquisition the purity of epsom salt 99% or more,
Compared with the prior art without carrying out purification & isolation to product, there is significant economic effect and huge social benefit.
The present invention is hereinbefore disclosed with preferred embodiment, but it should be understood by those skilled in the art that, these
Embodiment is only used for describing the present invention, but should not be understood as limiting the scope of the invention.It should be noted that all implement with these
Example equivalent variation and displacement, should all be set as being covered by scope of the presently claimed invention.Therefore, protection scope of the present invention
It should be subject to range defined in claims.
Claims (9)
1. a kind of high-concentration sulfuric acid ammonium Recycling Mother Solution processing method, which comprises the following steps:
(1) high-concentration sulfuric acid ammonium salt solution ammonia still process
Magnesia powder is added in the ammonium sulfate liquor that concentration is 80~300g/L, heats ammonia still process, obtains Adlerika and ammonia
Ammonia is passed through absorption plant and recycled by gas;
(2) magnesium sulfate evaporative crystallization
Adlerika described in heating evaporation when there is crystal precipitation, then is cooled and separated, dries, obtains sulfuric acid magnesium products;
(3) magnesium sulfate mother liquid recycling
By in above-mentioned isolated sulfuric acid mother liquid of magnesium return step (1), it is made to carry out heating ammonia still process with the magnesia powder.
2. high-concentration sulfuric acid ammonium Recycling Mother Solution processing method according to claim 1, which is characterized in that the magnesia powder
The molar ratio of middle MgO and ammonium ion in the ammonium sulfate liquor is 1:(2.01~5).
3. high-concentration sulfuric acid ammonium Recycling Mother Solution processing method according to claim 1, which is characterized in that the high concentration sulphur
Heating temperature is 60~90 DEG C in acid ammonium solution ammonia still process step, when heating a length of 4~6h, pressure be -0.02MPa to -
0.09MPa。
4. high-concentration sulfuric acid ammonium Recycling Mother Solution processing method according to claim 3, which is characterized in that the high concentration sulphur
Heating temperature is 70 DEG C in acid ammonium solution ammonia still process step.
5. high-concentration sulfuric acid ammonium Recycling Mother Solution processing method according to claim 1, which is characterized in that in step (2), add
The temperature of Adlerika described in thermal evaporation is 80~100 DEG C.
6. high-concentration sulfuric acid ammonium Recycling Mother Solution processing method according to claim 1, which is characterized in that in step (2), institute
Stating temperature after cooling is 60~80 DEG C.
7. high-concentration sulfuric acid ammonium Recycling Mother Solution processing method according to claim 6, which is characterized in that in step (2), institute
Stating temperature after cooling is 70 DEG C.
8. high-concentration sulfuric acid ammonium Recycling Mother Solution processing method according to claim 7, which is characterized in that in step (2), institute
The temperature for stating drying is 40~60 DEG C.
9. high-concentration sulfuric acid ammonium Recycling Mother Solution processing method according to claim 8, which is characterized in that the magnesium sulfate produces
Product are epsom salt.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112645369A (en) * | 2020-12-30 | 2021-04-13 | 莱州市中大贵合化工有限公司 | Production process for producing magnesium sulfate fertilizer by using sulfamic acid waste acid |
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CN106904642A (en) * | 2017-01-19 | 2017-06-30 | 南阳东方应用化工研究所 | A kind of magnesium processes treatment liquid containing ammonium sulfate technique waste water and the method for reclaiming magnesium sulfate |
CN107055569A (en) * | 2017-06-26 | 2017-08-18 | 孙东江 | A kind of comprehensive utilization process of liquid containing ammonium sulfate industrial wastewater |
-
2019
- 2019-08-02 CN CN201910713977.0A patent/CN110255580A/en active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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US4292043A (en) * | 1979-02-15 | 1981-09-29 | Bayer Antwerpen | Process for working up effluent containing ammonium sulphate |
CN106904642A (en) * | 2017-01-19 | 2017-06-30 | 南阳东方应用化工研究所 | A kind of magnesium processes treatment liquid containing ammonium sulfate technique waste water and the method for reclaiming magnesium sulfate |
CN107055569A (en) * | 2017-06-26 | 2017-08-18 | 孙东江 | A kind of comprehensive utilization process of liquid containing ammonium sulfate industrial wastewater |
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Cited By (1)
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CN112645369A (en) * | 2020-12-30 | 2021-04-13 | 莱州市中大贵合化工有限公司 | Production process for producing magnesium sulfate fertilizer by using sulfamic acid waste acid |
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