CN109796029A - A kind of preparation method of ammonium sulphate nitrate - Google Patents
A kind of preparation method of ammonium sulphate nitrate Download PDFInfo
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- CN109796029A CN109796029A CN201910168718.4A CN201910168718A CN109796029A CN 109796029 A CN109796029 A CN 109796029A CN 201910168718 A CN201910168718 A CN 201910168718A CN 109796029 A CN109796029 A CN 109796029A
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- ammonium sulphate
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Abstract
The present invention relates to a kind of preparation methods of ammonium sulphate nitrate, ammonia, nitric acid and sulfuric acid solution are passed through in tubular reactor, reaction generates the mixed solution containing ammonium nitrate and ammonium sulfate, by flash separator gas-liquid separation, liquid, which enters, is stirred slot, it is stirred in slot and diammonium hydrogen phosphate is added, the enough long-times of uniform stirring, to form 1:1 type, 1:2 type or 1:3 type ammonium sulphate nitrate double salt；Mixed slurry after reaction is evaporated, evaporating temperature, vacuum degree are controlled；Slurry after evaporation carries out vacuum filter, and filtrate returns in mixing channel and continues to participate in reaction, and filter cake obtains finished product ammonium sulphate nitrate after being dried.The ammonium nitrate generated in tubular reactor in the present invention chemically reacts in aqueous solution with ammonium sulfate, can generate the ammonium sulphate nitrate double salt of variform, chemical property is stablized, prevented from caking.
Description
Technical field
The present invention relates to technical field of chemical fertilizer production, especially a kind of preparation method of ammonium sulphate nitrate.
Background technique
Ammonium sulphate nitrate is a kind of widely used nitrogenous fertilizer, and containing two kinds of elements of nitrogen and sulphur, nitrogen has ammonium nitrogen and nitre again
Two kinds of forms of state nitrogen are especially suitable for the various crops of happiness nitrate nitrogen, sulphur, such as Cruciferae and green onion garlic, are generally taken as and chase after
Fertilizer use, can soil apply, can also be with fertigation.Different from ammonium sulfate, ammonium sulphate nitrate does not form apparent acidity in the soil,
Close to physiological neutral fertilizer, NO3--N translocation rate is high, and fertilizer efficiency is faster than ammonium sulfate.
Ammonium sulphate nitrate be generally yellowish coloured particles, it is complete it is water-soluble compared with ammonium nitrate, ammonium sulphate nitrate has hygroscopicity small, changes
The features such as property is stablized, prevented from caking, nonflammable explosive, this is because ammonium nitrate and ammonium sulfate form stable double salt,
Ammonium sulphate nitrate double salt through being reported has 1:1 type, 1:2 type and 1:3 type, wherein, tradition the most stable with 1:2 type ammonium sulphate nitrate
Production method on, melted after liquid ammonium nitrate is mixed in a certain ratio with solid ammonium sulfate, the matter of liquid ammonium nitrate
Concentration is measured 99% or more, being formed by most of ammonium sulphate nitrate is 1:1 type product, and contains a large amount of simple substance ammonium sulfate or nitre
Sour ammonium causes its physicochemical property to be still not sufficiently stable, and is easy agglomeration.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of preparation methods of ammonium sulphate nitrate, utilize ammonia, nitric acid and sulphur
Strong exothermal reaction of the acid solution in tubular reactor generates the mixed solution containing ammonium nitrate and ammonium sulfate, in diammonium hydrogen phosphate
Under the action of, uniform stirring reaction enough for a long time, generates 1:1 type, 1:2 type or 1:3 type ammonium sulphate nitrate.
In order to solve the above technical problems, the technical scheme adopted by the invention is that: a kind of preparation method of ammonium sulphate nitrate, should
Method the following steps are included:
1) ammonia, nitric acid and sulfuric acid solution are passed through in tubular reactor, it is molten that reaction generates the mixing containing ammonium nitrate and ammonium sulfate
Liquid, by flash separator gas-liquid separation, liquid, which enters, is stirred slot, is stirred in slot and diammonium hydrogen phosphate is added, uniformly
Stirring long-time enough, to form the ammonium sulphate nitrate double salt of 1:1 type, 1:2 type or 1:3 type or combinations thereof；
2) mixed slurry after reaction is evaporated, controls evaporating temperature, vacuum degree；
3) slurry after evaporating carries out vacuum filter, and filtrate returns and continues to participate in reaction in mixing channel, and filter cake obtains after being dried
To finished product ammonium sulphate nitrate.
Preferably, in step 1), the mass concentration of nitric acid solution is 60-65%, and the mass concentration of sulfuric acid solution is 90-
98%。
Preferably, in step 1), the ratio between the amount of substance of pure nitric acid, bright sulfur acid is 3- in ammonia and nitric acid and sulfuric acid solution
4:1-2:1.
Preferably, it in step 1), is stirred in slot and diammonium hydrogen phosphate is added, by weight, ammonium nitrate solution 50-65
Part, 30-50 parts of ammonium sulfate, 0.0001-5 parts of diammonium hydrogen phosphate.
Preferably, in step 1), being stirred to react the time is 30-120 minutes.
Preferably, in step 2), evaporating temperature control is 160-200 DEG C, vacuum degree 70-100Kpa.
Preferably, in step 3), the finished product ammonium sulphate nitrate moisture after drying is not higher than 2%.
The present invention provides a kind of preparation methods of ammonium sulphate nitrate, have the beneficial effect that:
1, in the production of traditional ammonium sulphate nitrate, the liquid ammonium nitrate of 99% or more mass concentration mixes in proportion with solid ammonium sulfate,
Under the extremely low environment of moisture content, ammonium nitrate and ammonium sulfate are simple physical mixed, and chemical reaction occurs and generates stabilization
Double salt is seldom, and the ammonium nitrate generated in the present invention chemically reacts in aqueous solution with ammonium sulfate, can generate variform
Ammonium sulphate nitrate double salt, chemical property stablize, it is prevented from caking；
2, it compared with conventional production methods, is reacted in tubular reactor using ammonia with nitric acid and sulfuric acid solution, the heat of generation
Be conducive to ammonium nitrate and generate reacting for ammonium sulphate nitrate double salt with ammonium sulfate, improves reaction rate and yield, double salt average yield
Greater than 70%, and conventional production methods are used, the yield of double salt is less than 10%, and substantially 1:1 type double salt；
3, a certain amount of diammonium hydrogen phosphate is added in mixing channel, on the one hand making aqueous solution is in alkalescent, is had under weakly alkaline environment
Conducive to the generation of ammonium sulphate nitrate double salt；On the other hand, due to the presence of ammonium ion in diammonium hydrogen phosphate, nitre sulphur is effectively inhibited
Inverse decomposition of the sour ammonium to ammonium sulfate and ammonium nitrate.
Detailed description of the invention
Fig. 1 schematic structural diagram of the device of the invention；
Wherein: nitric acid storage tank 1, tubular reactor 2, flash separator 3 are stirred slot 4, flash tank 5, level-one evaporator 6, and two
Grade evaporator 7, high-tower melting granulation device 9 neutralize scrubbing tower 8, gas ammonia access tube 21, nitric acid access tube 22, sulfuric acid access tube
23, ammonia sulfate crystal discharge port 41, diammonium hydrogen phosphate discharge port 42, middle pressure steam access tube 71.
Specific embodiment
Combined with specific embodiments below, further details of elaboration is made to the present invention, but embodiments of the present invention are not
It is confined to the range of embodiment expression.These embodiments are merely to illustrate the present invention, range and is not intended to limit the present invention.
Embodiment 1
Ammonia, nitric acid and sulfuric acid solution are passed through in tubular reactor, nitric acid solution mass concentration is 65%, sulfuric acid solution quality
Concentration is 98%, and the ratio between the amount of substance of pure nitric acid, bright sulfur acid is 4:2:1 in ammonia and nitric acid and sulfuric acid solution, and reaction, which generates, to be contained
The mixed solution of ammonium nitrate and ammonium sulfate, by flash separator gas-liquid separation, liquid, which enters, is stirred slot, is stirred slot
In diammonium hydrogen phosphate is not added, uniform stirring enters vapo(u)rization system after sixty minutes in mixing channel, control evaporating temperature is 180 DEG C,
Vacuum degree 80Kpa, the reaction slurry that evaporation removes most of moisture enter vacuum type belt filter and carry out cold filtration, obtain
Ammonium sulphate nitrate filter cake is finally dried to obtain ammonium sulphate nitrate finished product, and filtrate returns in mixing channel and continues to participate in reaction.By finished product
Ammonium sulphate nitrate carries out X-ray diffraction (XRD), and unit is (wt.%), as a result as follows, and the yield of double salt is 22.82%, wherein 1:2 type
Double salt yield is 1.78%:
Ammonium nitrate 56.91
Ammonium sulfate 19.07
1:1 type double salt 20.5
1:2 type double salt 1.78
1:3 type double salt 0.54
Water 1.2
Embodiment 2
Ammonia, nitric acid and sulfuric acid solution are passed through in tubular reactor, nitric acid solution mass concentration is 65%, sulfuric acid solution quality
Concentration is 98%, and the ratio between the amount of substance of pure nitric acid, bright sulfur acid is 4:2:1 in ammonia and nitric acid and sulfuric acid solution, and reaction, which generates, to be contained
The mixed solution of ammonium nitrate and ammonium sulfate, by flash separator gas-liquid separation, liquid, which enters, is stirred slot, diammonium hydrogen phosphate
Mass percent be 3%, uniform stirring enters vapo(u)rization system after sixty minutes in mixing channel, control evaporating temperature is 180 DEG C,
Vacuum degree 80Kpa, the reaction slurry that evaporation removes most of moisture enter vacuum type belt filter and carry out cold filtration, obtain
Ammonium sulphate nitrate filter cake is finally dried to obtain ammonium sulphate nitrate finished product, and filtrate returns in mixing channel and continues to participate in reaction.By finished product
Ammonium sulphate nitrate carries out X-ray diffraction (XRD), and unit is (wt.%), as a result as follows, and the yield of double salt is 78.46%, wherein 1:2 type
Double salt yield is 55.06%:
Ammonium nitrate 11.63
Ammonium sulfate 5.31
Phosphate 3.5
1:1 type double salt 12.2
1:2 type double salt 55.06
1:3 type double salt 11.2
Water 1.1
Embodiment 3
Ammonia, nitric acid and sulfuric acid solution are passed through in tubular reactor, nitric acid solution mass concentration is 65%, sulfuric acid solution quality
Concentration is 98%, and the ratio between the amount of substance of pure nitric acid, bright sulfur acid is 4:2:1 in ammonia and nitric acid and sulfuric acid solution, and reaction, which generates, to be contained
The mixed solution of ammonium nitrate and ammonium sulfate, by flash separator gas-liquid separation, liquid, which enters, is stirred slot, diammonium hydrogen phosphate
Mass percent be 5%, uniform stirring enters vapo(u)rization system after sixty minutes in mixing channel, control evaporating temperature is 180 DEG C,
Vacuum degree 80Kpa, the reaction slurry that evaporation removes most of moisture enter vacuum type belt filter and carry out cold filtration, obtain
Ammonium sulphate nitrate filter cake is finally dried to obtain ammonium sulphate nitrate finished product, and filtrate returns in mixing channel and continues to participate in reaction.By finished product
Ammonium sulphate nitrate carries out X-ray diffraction (XRD), and unit is (wt.%), as a result as follows, and the yield of double salt is 94.11%, wherein 1:2
Type double salt yield is 86.56%:
Ammonium nitrate 0
Ammonium sulfate 0
Phosphate 4.89
1:1 type double salt 3.77
1:2 type double salt 86.56
1:3 type double salt 3.78
Water 1
Embodiment 4
Ammonia, nitric acid and sulfuric acid solution are passed through in tubular reactor, nitric acid solution mass concentration is 65%, sulfuric acid solution quality
Concentration is 98%, and the ratio between the amount of substance of pure nitric acid, bright sulfur acid is 3:1:1 in ammonia and nitric acid and sulfuric acid solution, and reaction, which generates, to be contained
The mixed solution of ammonium nitrate and ammonium sulfate, by flash separator gas-liquid separation, liquid, which enters, is stirred slot, diammonium hydrogen phosphate
Mass percent be 3%, in mixing channel after uniform stirring 120 minutes enter vapo(u)rization system, control evaporating temperature be 170 DEG C,
Vacuum degree 100Kpa, the reaction slurry that evaporation removes most of moisture enter vacuum type belt filter and carry out cold filtration, obtain
To ammonium sulphate nitrate filter cake, finally it is dried to obtain ammonium sulphate nitrate finished product, filtrate returns in mixing channel and continues to participate in reaction.It will be at
Product ammonium sulphate nitrate carries out X-ray diffraction (XRD), and unit is (wt.%), as a result as follows, and the yield of double salt is 80.78%, wherein 1:
2 type double salt yields are 9.2%:
Ammonium nitrate 10.29
Ammonium sulfate 4.62
Phosphate 3.21
1:1 type double salt 60.06
1:2 type double salt 9.2
1:3 type double salt 11.52
Water 1.1
Embodiment 5
Ammonia, nitric acid and sulfuric acid solution are passed through in tubular reactor, nitric acid solution mass concentration is 65%, sulfuric acid solution quality
Concentration is 98%, and the ratio between the amount of substance of pure nitric acid, bright sulfur acid is 3:1:1 in ammonia and nitric acid and sulfuric acid solution, and reaction, which generates, to be contained
The mixed solution of ammonium nitrate and ammonium sulfate, by flash separator gas-liquid separation, liquid, which enters, is stirred slot, diammonium hydrogen phosphate
Mass percent be 5%, in mixing channel after uniform stirring 120 minutes enter vapo(u)rization system, control evaporating temperature be 170 DEG C,
Vacuum degree 100Kpa, the reaction slurry that evaporation removes most of moisture enter vacuum type belt filter and carry out cold filtration, obtain
To ammonium sulphate nitrate filter cake, finally it is dried to obtain ammonium sulphate nitrate finished product, filtrate returns in mixing channel and continues to participate in reaction.It will be at
Product ammonium sulphate nitrate carries out X-ray diffraction (XRD), and unit is (wt.%), as a result as follows, and the yield of double salt is 94.04%, wherein 1:
2 type double salt yields are 7.76%:
Ammonium nitrate 0
Ammonium sulfate 0
Phosphate 4.96
1:1 type double salt 78.53
1:2 type double salt 7.76
1:3 type double salt 7.75
Water 1
Embodiment 6
The device that embodiment 1-5 is used, including nitric acid storage tank 1, the nitric acid storage tank 1 pass through pipeline and tubular reactor 2, sudden strain of a muscle
It steams separator 3, be stirred slot 4, flash tank 5, level-one evaporator 6, secondary evaporimeter 7 and high-tower melting granulation device 9 successively
Connection, the nitric acid storage tank 1 also by pipeline and neutralization scrubbing tower 8 and are stirred slot 4 and are sequentially communicated.
Preferably, the tubular reactor 2 is equipped with gas ammonia access tube 21, nitric acid access tube 22 and sulfuric acid access tube 23, institute
It states and is stirred slot 4 equipped with ammonia sulfate crystal discharge port 41 and diammonium hydrogen phosphate discharge port 42.
Preferably, the flash separator 3 is connected to by pipeline with scrubbing tower 8 is neutralized.
Preferably, the secondary evaporimeter 7 be equipped with middle pressure steam access tube 71, it is described be stirred slot 4 by pipeline with
Flash tank 5, level-one evaporator 6 and secondary evaporimeter 7 are sequentially communicated by pipeline.
Preferably, the neutralization scrubbing tower 8 is formed into a loop by pipeline and level-one evaporator 6.Neutralize the washing of scrubbing tower 8
Process steam enters the utilization of level-one evaporator 6, and the process steam condensate liquid of the level-one evaporator 6, which enters, neutralizes scrubbing tower 8 again
It utilizes.
The above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations；Although referring to aforementioned each reality
Applying example, invention is explained in detail, those skilled in the art should understand that: it still can be to aforementioned each
Technical solution documented by embodiment is modified, or equivalent substitution of some or all of the technical features；And
These are modified or replaceed, the range for technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution.
Claims (10)
1. a kind of preparation method of ammonium sulphate nitrate, it is characterised in that: the method includes following procedure:
1) ammonia, nitric acid and sulfuric acid solution are passed through in tubular reactor, it is molten that reaction generates the mixing containing ammonium nitrate and ammonium sulfate
Liquid, by flash separator gas-liquid separation, liquid, which enters, is stirred slot, is stirred in slot and diammonium hydrogen phosphate is added, uniformly
Stirring enough for a long time, forms the mixed slurry of the ammonium sulphate nitrate double salt of 1:1 type, 1:2 type or 1:3 type or combinations thereof；
2) mixed slurry after reaction is evaporated；
3) slurry after evaporating carries out vacuum filter, and filtrate, which returns to be stirred in slot, continues to participate in reaction, and filter cake is dried
After obtain finished product ammonium sulphate nitrate.
2. a kind of preparation method of ammonium sulphate nitrate according to claim 1, it is characterised in that: in the step 1), nitre
The mass concentration of acid solution is 60%-65%, and the mass concentration of sulfuric acid solution is 90%-98%.
3. a kind of preparation method of ammonium sulphate nitrate according to claim 1, it is characterised in that: in the step 1), ammonia
The ratio between amount of substance of gas and nitric acid, sulfuric acid is 3-4:1-2:1.
4. a kind of preparation method of ammonium sulphate nitrate according to claim 1, it is characterised in that: in the step 1), stir
It mixes and diammonium hydrogen phosphate is added in mixing channel, be stirred in slot substance by weight, 50-65 parts of ammonium nitrate solution, ammonium sulfate
30-50 parts, 0.0001-5 parts of diammonium hydrogen phosphate.
5. a kind of preparation method of ammonium sulphate nitrate according to claim 1, it is characterised in that: when the step 1) stirs
Between be 30-120 minutes.
6. a kind of preparation method of ammonium sulphate nitrate according to claim 1, it is characterised in that: the step 2 evaporates item
Part are as follows: 160-200 DEG C of temperature, vacuum degree 70-100Kpa.
7. a kind of preparation method of ammonium sulphate nitrate according to claim 1, it is characterised in that: after the step 3) drying
Finished product ammonium sulphate nitrate moisture≤2%.
8. the device that preparation method described in claims 1-7 any one uses, it is characterised in that: described includes nitric acid storage tank
(1), it is characterised in that: the nitric acid storage tank (1) by pipeline and tubular reactor (2), flash separator (3), be stirred
Slot (4), flash tank (5), level-one evaporator (6), secondary evaporimeter (7) and high-tower melting granulation device (9) are sequentially communicated, described
Nitric acid storage tank (1) also by pipeline and neutralization scrubbing tower (8) and is stirred slot (4) and is sequentially communicated.
9. a kind of device for producing particle ammonium sulphate nitrate according to claim 8, it is characterised in that: the tubular reactor
(2) it is equipped with gas ammonia access tube (21), nitric acid access tube (22) and sulfuric acid access tube (23), described be stirred slot (4) are equipped with sulphur
Sour ammonium crystal discharge port (41) and diammonium hydrogen phosphate discharge port (42).
10. a kind of device for producing particle ammonium sulphate nitrate according to claim 8, it is characterised in that: the flash separation
Device (3) is connected to by pipeline with scrubbing tower (8) are neutralized, and the secondary evaporimeter (7) is equipped with middle pressure steam access tube (71), described
It is stirred slot (4) and is successively connected with flash tank (5), level-one evaporator (6) and secondary evaporimeter (7) by pipeline by pipeline
Logical, the neutralization scrubbing tower (8) is formed into a loop by pipeline and level-one evaporator (6).
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| CN107556061A (en) * | 2010-11-02 | 2018-01-09 | 艾德凡斯化学公司 | The production method of ammonium sulfate nitrate |
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2019
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| US2795495A (en) * | 1953-10-24 | 1957-06-11 | Rubrchemie Ag | Non-caking ammonium sulfate nitrate |
| US6689181B2 (en) * | 2000-11-15 | 2004-02-10 | Honeywell International Inc. | Ammonium sulfate nitrate |
| US20100242556A1 (en) * | 2009-03-31 | 2010-09-30 | Smith Michael R | Pastillation of Ammonium Sulfate Nitrate |
| CN107556061A (en) * | 2010-11-02 | 2018-01-09 | 艾德凡斯化学公司 | The production method of ammonium sulfate nitrate |
| CN102603387A (en) * | 2012-03-19 | 2012-07-25 | 深圳市芭田生态工程股份有限公司 | Method for producing compound fertilizer by high tower tubular reactor |
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