CN104445121B - Mono-ammonium phosphate produced by using wet process phosphoric acid and production method of mono-ammonium phosphate - Google Patents

Mono-ammonium phosphate produced by using wet process phosphoric acid and production method of mono-ammonium phosphate Download PDF

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Publication number
CN104445121B
CN104445121B CN201410673845.7A CN201410673845A CN104445121B CN 104445121 B CN104445121 B CN 104445121B CN 201410673845 A CN201410673845 A CN 201410673845A CN 104445121 B CN104445121 B CN 104445121B
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phosphoric acid
map
content
phosphorus
ammonium phosphate
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CN104445121A (en
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魏发展
廖吉星
朱飞武
石秀明
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Guizhou Kailin Group Co Ltd
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Guizhou Kailin Group Co Ltd
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Abstract

The invention relates to the technical field of mono-ammonium phosphate prepared by using wet process phosphoric acid, and in particular to mono-ammonium phosphate produced by using wet process phosphoric acid and a production method of the mono-ammonium phosphate. When an ammonia gas is introduced or liquid ammonia is added into impurities in phosphoric acid prepared by using the wet process phosphoric acid, the neutralization in mixed liquor is adjusted to 0.5-0.8 to generate a large amount of precipitates from the impurities in the phosphoric acid, separation treatment is carried out by using a separator, after phosphoric acid with higher purity is obtained, the ammonia gas or the liquid ammonia is introduced in the phosphoric acid, and the pH value of the phosphoric acid is controlled to obtain mono-ammonium phosphate slurry with higher purity, so that the purity of a mono-ammonium phosphate product is improved and the total nutrient in the mono-ammonium phosphate is 60.15-60.36%, wherein counted by phosphorus pentoxide, the phosphorus content is 49.0-51.0%, the content of water soluble phosphorus is 47.62-48.15%, the nitrogen content is 9.0-11.0%, the fluorine content is 0.48-0.68%, the quality of the ammonium phosphate is improved, and the environmental pollution of the ammonium phosphate resulting from a fertilization effect is avoided.

Description

A kind of MAP of utilization Wet-process Phosphoric Acid Production and its production method
Technical field
The present invention relates to phosphoric acid by wet process prepares MAP technical field, especially one kind is using wet The MAP of method phosphoric acid production and its production method.
Background technology
MAP is a kind of efficient compound fertilizer in addition to Diammonium phosphate (DAP), because its nutrient is high, Also have a wide range of applications in all kinds of plant fertilisings.With agrotechnical continuous development, people The growth mechanism of plant is had deeper into understanding, the fertilizer efficiency to fertilizer and impurity content require Also more and more higher.At present for the requirement of the water-soluble phosphorus in MAP be account for the 90% of total phosphorus with On, it is higher than 1% that the requirement to Oil repellent must not be.And traditional employing Wet-process Phosphoric Acid Production phosphorus In the technique of a sour ammonium, it is directly to be reacted with ammonia with phosphoric acid by wet process, by controlling ammonia and phosphoric acid Mol ratio adjusts total nutrient, and then impurity in phosphoric acid by wet process is fully entered in product, leads to The impurity contents such as the total nutrient of product, water-soluble phosphorus and fluorine are difficult to control to it is impossible to meet market Demand.
And Oil repellent present in MAP is higher so that the range of fertilizer is subject to Limitation, simultaneously use when, due to Determination of Multi-Impurities presence so that Fertilization Effect and The impact that theory of barrel short plate is brought to crop is more obvious, result in crop growth environment and is subject to Serious pollution, for this reason, this researcher is by long-term exploration and research, will be using wet method phosphorus The technique that acid produces monoammonium phosphate product provides a kind of new selection, reduces monoammonium phosphate product Production cost.
Content of the invention
In order to solve above-mentioned technical problem present in prior art, the present invention provides a kind of utilization The MAP of Wet-process Phosphoric Acid Production, having total nutrient is 60.15-60.36%, wherein, water-soluble Property phosphorus content be 47.62-48.15%, nitrogen content is 9.0-11.0%%, and Oil repellent is The feature of 0.48-0.68%.
Another object of the present invention is to provide a kind of phosphoric acid one of utilization Wet-process Phosphoric Acid Production The production method of ammonium, the method passes through the amount to the ammonia being passed through and PH in preparation technology The control of value and adjustment, and then make a large amount of impurity in the phosphoric acid of phosphoric acid by wet process phosphoric acid acquisition It is removed, and then the prepared purity of monoammonium phosphate product of raising phosphoric acid by wet process and total nutrient contain Amount, meanwhile, reduces Oil repellent in monoammonium phosphate product so that Oil repellent in manufacturing process Less than 0.7%.
It is achieved particular by technical scheme below:
A kind of MAP of utilization Wet-process Phosphoric Acid Production, the Oil repellent of this MAP is 0.48-0.68%.
The total nutrient of described MAP is 60.15-60.36%, and wherein phosphorus content is with five oxidations Two phosphorus meters, content is 49.0-51.0%, and in phosphorus content, the content of water-soluble phosphorus is 47.62-48.15%, nitrogen content is 9.0-11.0%%, and Oil repellent is 0.48-0.68%.
The total nutrient of described MAP be 60.23%, wherein phosphorus content in terms of phosphorus pentoxide, Content is 50.10%, and in phosphorus content, the content of water-soluble phosphorus is 48.03%, and nitrogen content is 10.13%, Oil repellent is 0.53%.
This utilizes the production method of the MAP of Wet-process Phosphoric Acid Production, comprises the following steps:
(1) preneutralization:Phosphoric acid is placed in preneutralization groove, is passed through ammonia thereto, and adopt The mode stirring when being passed through is taken to be passed through, mixing speed during stirring is 30-50r/min, When the mol ratio of the ammonia being passed through and phosphoric acid is 0.5-0.7, continue at mixing speed stirring Reason 20-30min, and hyperthermic treatment is carried out to preneutralization groove, programming rate is 0.3-0.6 DEG C/min Hyperthermic treatment, and detect the pH value of mixed liquor in preneutralization groove, treat that pH value reaches 0.5-0.8, Stop hyperthermic treatment, obtain solidliquid mixture, stand-by;
(2) separate:By step 1) solidliquid mixture that obtains is placed in centrifugal separator and carries out Centrifugation, the rotating speed of centrifugal separator is 3000-4000r/min, centrifugation 20-30min Afterwards, obtain solid and liquid, solid is transported to compound fertilizer production technology, liquid is stand-by;
(3) neutralize again:Liquid is placed in mixing channel, and continues to be passed through in mixing channel Ammonia, and take the mode stirring when being passed through to carry out, mixing speed is 30-50r/min, treats Being passed through to the mol ratio of ammonia in solution and phosphoric acid is 0.98-1.05, and adjustment pH value is 4.2-4.6, Obtain MAP slip, stand-by:
(4) granulate:By step 3) the MAP slip pump that obtains by pipeline extract to So that MAP slip carries out spraying granulation process in comminutor in comminutor, obtain phosphorus Acid one ammonium just finished product, stand-by;
(5) it is dried:By step 4) just finished product is placed in drier for the MAP that obtains, Using 90 DEG C of temperature dried process 30-40s, obtain finished product MAP.
Described phosphoric acid be sulfuric acid decomposition phosphorus ore be obtained phosphoric acid, decomposing phosphorite by using nitric acid be obtained phosphorus One of phosphoric acid that acid, decomposing phosphate rock by chlorhydric acid are obtained.
In described separating step, centrifugal separator can also be filtered with filter press or hypergravity One of machine is replacing.
Described ammonia can also be replaced with liquefied ammonia.
Compared with prior art, the technique effect of the present invention is embodied in:
1. ammonia or addition are being passed through by the impurity in the phosphoric acid prepared to phosphoric acid by wet process During liquefied ammonia, when the degree of neutralization in adjustment mixed liquor is 0.5-0.8, and then lead to the impurity in phosphoric acid Obtain substantial amounts of precipitation, and then separating treatment is carried out by seperator, obtain the higher phosphorus of purity After acid, then it is passed through ammonia or liquefied ammonia thereto, and controls its pH value, and then obtain phosphoric acid The higher slip of one ammonium purity, and then improve the purity of monoammonium phosphate product so that phosphoric acid one Total nutrient in ammonium is 60.15-60.36%, and in terms of phosphorus pentoxide, content is wherein phosphorus content 49.0-51.0%, in phosphorus content, the content of water-soluble phosphorus is 47.62-48.15%, nitrogen content For 9.0-11.0%%, Oil repellent is 0.48-0.68%, improves the quality of MAP, it is to avoid Fertilization Effect makes the phenomenon that MAP causes environment pollution.
2. pass through the adjustment of above-mentioned technique and control in MAP production process, and then make Must purifying phosphoric acid and the Oil repellent reducing in MAP be obtained largely improving, carry The high quality as crop fertilizer for the MAP.
Specific embodiment
Technical scheme is further limited with reference to specific embodiment Fixed, but claimed scope is not only limited to description.
The present invention fully analyzes the composition of phosphoric acid by wet process, and in phosphoric acid, fluorine, magnesium, aluminium, iron etc. are miscellaneous In matter ion and ammonia course of reaction, reaction under the conditions of degree of neutralization is for 0.5-0.8 generates different answering Heterocompound.It is difficult to the physical property dissolving using complex compound, realize solid-liquor separation, Gu Mutually it is used for the production of composite fertilizer, the secondary neutralization of liquid phase ammonification, obtain high water-soluble phosphorus low fluorine content High-quality MAP.
Embodiment 1
A kind of MAP of utilization Wet-process Phosphoric Acid Production, the Oil repellent of this MAP is 0.53%.
This utilizes the production method of the MAP of Wet-process Phosphoric Acid Production, comprises the following steps:
(1) preneutralization:Phosphoric acid is placed in preneutralization groove, is passed through ammonia thereto, and adopt The mode stirring when being passed through is taken to be passed through, mixing speed during stirring is 30r/min, treats When the mol ratio of the ammonia being passed through and phosphoric acid is 0.5, continue to mixing speed stir process 20min, and hyperthermic treatment is carried out to preneutralization groove, programming rate is 0.3 DEG C/min hyperthermic treatment, And detect the pH value of mixed liquor in preneutralization groove, treat that pH value reaches 0.5, stop hyperthermic treatment, Obtain solidliquid mixture, stand-by;
(2) separate:By step 1) solidliquid mixture that obtains is placed in centrifugal separator and carries out Centrifugation, the rotating speed of centrifugal separator is 3000r/min, after centrifugation 20min, obtains Solid and liquid, solid is transported to compound fertilizer production technology, and liquid is stand-by;
(3) neutralize again:Liquid is placed in mixing channel, and continues to be passed through in mixing channel Ammonia, and take the mode stirring when being passed through to carry out, mixing speed is 30r/min, waits to lead to Entering to the mol ratio of ammonia in solution and phosphoric acid is 0.98, and adjustment pH value is 4.2, obtains phosphoric acid One ammonium slip, stand-by:
(4) granulate:By step 3) the MAP slip pump that obtains by pipeline extract to So that MAP slip carries out spraying granulation process in comminutor in comminutor, obtain phosphorus Acid one ammonium just finished product, stand-by;
(5) it is dried:By step 4) just finished product is placed in drier for the MAP that obtains, Using 90 DEG C of temperature dried process 30s, obtain finished product MAP.
Described phosphoric acid is the phosphoric acid that sulfuric acid decomposition phosphorus ore is obtained.
MAP is detected, its result is that the total nutrient of described MAP is 60.23%, in terms of phosphorus pentoxide, content is 50.10% to wherein phosphorus content, in phosphorus content, The content of water-soluble phosphorus is 48.03%, and nitrogen content is 10.13%, and Oil repellent is 0.53%.
Embodiment 2
A kind of MAP of utilization Wet-process Phosphoric Acid Production, the Oil repellent of this MAP is 0.48%.
This utilizes the production method of the MAP of Wet-process Phosphoric Acid Production, comprises the following steps:
(1) preneutralization:Phosphoric acid is placed in preneutralization groove, is passed through ammonia thereto, and adopt The mode stirring when being passed through is taken to be passed through, mixing speed during stirring is 50r/min, treats When the mol ratio of the ammonia being passed through and phosphoric acid is 0.7, continue to mixing speed stir process 30min, and hyperthermic treatment is carried out to preneutralization groove, programming rate is 0.6 DEG C/min hyperthermic treatment, And detect the pH value of mixed liquor in preneutralization groove, treat that pH value reaches 0.8, stop hyperthermic treatment, Obtain solidliquid mixture, stand-by;
(2) separate:By step 1) solidliquid mixture that obtains is placed in centrifugal separator and carries out Centrifugation, the rotating speed of centrifugal separator is 4000r/min, after centrifugation 30min, obtains Solid and liquid, solid is transported to compound fertilizer production technology, and liquid is stand-by;
(3) neutralize again:Liquid is placed in mixing channel, and continues to be passed through in mixing channel Ammonia, and take the mode stirring when being passed through to carry out, mixing speed is 50r/min, waits to lead to Entering to the mol ratio of ammonia in solution and phosphoric acid is 1.05, and adjustment pH value is 4.6, obtains phosphoric acid One ammonium slip, stand-by:
(4) granulate:By step 3) the MAP slip pump that obtains by pipeline extract to So that MAP slip carries out spraying granulation process in comminutor in comminutor, obtain phosphorus Acid one ammonium just finished product, stand-by;
(5) it is dried:By step 4) just finished product is placed in drier for the MAP that obtains, Using 90 DEG C of temperature dried process 40s, obtain finished product MAP.
Described phosphoric acid is the phosphoric acid that decomposing phosphorite by using nitric acid is obtained.
MAP is detected it can be deduced that:Total nutrient is 60.15%, wherein phosphorus content In terms of phosphorus pentoxide, content is 50.06%, and in phosphorus content, the content of water-soluble phosphorus is 47.62%, nitrogen content is 10.09%, and Oil repellent is 0.48%.
Embodiment 3
A kind of MAP of utilization Wet-process Phosphoric Acid Production, the Oil repellent of this MAP is 0.68%.
This utilizes the production method of the MAP of Wet-process Phosphoric Acid Production, comprises the following steps:
(1) preneutralization:Phosphoric acid is placed in preneutralization groove, is passed through ammonia thereto, and adopt The mode stirring when being passed through is taken to be passed through, mixing speed during stirring is 40r/min, treats When the mol ratio of the ammonia being passed through and phosphoric acid is 0.6, continue to mixing speed stir process 25min, and hyperthermic treatment is carried out to preneutralization groove, programming rate is 0.5 DEG C/min hyperthermic treatment, And detect the pH value of mixed liquor in preneutralization groove, treat that pH value reaches 0.7, stop hyperthermic treatment, Obtain solidliquid mixture, stand-by;
(2) separate:By step 1) solidliquid mixture that obtains is placed in centrifugal separator and carries out Centrifugation, the rotating speed of centrifugal separator is 3500r/min, after centrifugation 25min, obtains Solid and liquid, solid is transported to compound fertilizer production technology, and liquid is stand-by;
(3) neutralize again:Liquid is placed in mixing channel, and continues to be passed through in mixing channel Ammonia, and take the mode stirring when being passed through to carry out, mixing speed is 40r/min, waits to lead to Entering to the mol ratio of ammonia in solution and phosphoric acid is 0.99, and adjustment pH value is 4.4, obtains phosphoric acid One ammonium slip, stand-by:
(4) granulate:By step 3) the MAP slip pump that obtains by pipeline extract to So that MAP slip carries out spraying granulation process in comminutor in comminutor, obtain phosphorus Acid one ammonium just finished product, stand-by;
(5) it is dried:By step 4) just finished product is placed in drier for the MAP that obtains, Using 90 DEG C of temperature dried process 35s, obtain finished product MAP.
Described phosphoric acid is the phosphoric acid that decomposing phosphate rock by chlorhydric acid is obtained.
MAP is detected, its result is:Total nutrient is 60.36%, wherein phosphorus content In terms of phosphorus pentoxide, content is 50.16%, and in phosphorus content, the content of water-soluble phosphorus is 48.15%, nitrogen content is 10.2%, and Oil repellent is 0.68%.
Embodiment 4
On the basis of embodiment 1,, all with embodiment 1, one kind utilizes Wet-process Phosphoric Acid Production for other MAP production method, in described separating step, centrifugal separator can also with pressure Filter is replacing.
Embodiment 5
On the basis of embodiment 2,, all with embodiment 2, one kind utilizes Wet-process Phosphoric Acid Production for other MAP production method, in described separating step, centrifugal separator can also be with super Gravity filter is replacing.
Embodiment 6
On the basis of embodiment 3,, all with embodiment 3, one kind utilizes Wet-process Phosphoric Acid Production for other MAP production method, described ammonia can also replace with liquefied ammonia.
Here it is important to point out that, above example is only limitted to technical scheme is done Further explanation and explanation, are not the further restriction to technical scheme, The essential characteristics of the non-protruding that those skilled in the art make on this basis and non-significant are entered The improvement of step, belongs to the protection category of the present invention.

Claims (7)

1. a kind of MAP production method of utilization Wet-process Phosphoric Acid Production is it is characterised in that the Oil repellent of this MAP is 0.48-0.68%;
Comprise the following steps:
(1) preneutralization:Phosphoric acid is placed in preneutralization groove, is passed through ammonia thereto, and take the mode stirring when being passed through to be passed through, mixing speed during stirring is 30-50r/min, when the mol ratio of the ammonia being passed through and phosphoric acid is 0.5-0.7, continues to mixing speed stir process 20-30min, and hyperthermic treatment is carried out to preneutralization groove, programming rate is 0.3-0.6 DEG C/min hyperthermic treatment, and detect pH of mixed in preneutralization groove, treat that pH reaches 0.5-0.8, stop hyperthermic treatment, obtain solidliquid mixture, stand-by;
(2) separate:The solidliquid mixture that step (1) is obtained is placed in centrifugal separator and is centrifuged, the rotating speed of centrifugal separator is 3000-4000r/min, after centrifugation 20-30min, obtains solid and liquid, solid is transported to compound fertilizer production technology, liquid is stand-by;
(3) neutralize again:Liquid is placed in mixing channel, and continues to be passed through ammonia in mixing channel, and take the mode stirring when being passed through to carry out, mixing speed is 30-50r/min, and waiting to be passed through to the mol ratio of ammonia in solution and phosphoric acid is 0.98-1.05, and adjustment pH value is 4.2-4.6, obtain MAP slip, stand-by:
(4) granulate:The MAP slip that step (3) is obtained is extracted to comminutor by pipeline with pump so that MAP slip carries out spraying granulation process in comminutor, obtains MAP just finished product, stand-by;
(5) it is dried:Just finished product is placed in drier the MAP that step (4) is obtained, and using 90 DEG C of temperature dried process 30-40s, obtains finished product MAP.
2. the MAP production method of utilization Wet-process Phosphoric Acid Production as claimed in claim 1 is it is characterised in that the Oil repellent of this MAP is 0.53%.
3. the MAP production method of utilization Wet-process Phosphoric Acid Production as claimed in claim 1, it is characterized in that, the total nutrient of described MAP is 60.15-60.36%, wherein phosphorus content is in terms of phosphorus pentoxide, content is 49.0-51.0%, and in phosphorus content, the content of water-soluble phosphorus is 47.62-48.15%, nitrogen content is 9.0-11.0%%, and Oil repellent is 0.48-0.68%.
4. the MAP production method of utilization Wet-process Phosphoric Acid Production as claimed in claim 2 or claim 3, it is characterized in that, the total nutrient of described MAP is 60.23%, wherein phosphorus content is in terms of phosphorus pentoxide, content is 50.10%, and in phosphorus content, the content of water-soluble phosphorus is 48.03%, nitrogen content is 10.13%, and Oil repellent is 0.53%.
5. the MAP production method using Wet-process Phosphoric Acid Production as claimed in claim 1 is it is characterised in that one of phosphoric acid of being obtained of the phosphoric acid that is obtained of phosphoric acid that described phosphoric acid is sulfuric acid decomposition phosphorus ore to be obtained, decomposing phosphorite by using nitric acid, decomposing phosphate rock by chlorhydric acid.
6. the MAP production method of utilization Wet-process Phosphoric Acid Production as claimed in claim 1 is it is characterised in that in described separating step, centrifugal separator also to be replaced with one of filter press or hypergravity filter.
7. as claim 1 using the MAP production method of Wet-process Phosphoric Acid Production it is characterised in that described ammonia is also replaced with liquefied ammonia.
CN201410673845.7A 2014-11-21 2014-11-21 Mono-ammonium phosphate produced by using wet process phosphoric acid and production method of mono-ammonium phosphate Expired - Fee Related CN104445121B (en)

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CN105084333B (en) * 2015-08-17 2017-05-03 湖北楚星化工股份有限公司 Production process of granulated mono ammonium phosphate (GMAP)
CN105540562A (en) * 2015-12-30 2016-05-04 川恒生态科技有限公司 Method for directly producing high-nutrition monoammonium phosphate from hemi-hydrate process wet process phosphoric acid
CN106744763A (en) * 2017-02-14 2017-05-31 瓮福(集团)有限责任公司 The method that powdery monoammonium phosphate is produced with phosphoric acid by wet process " step "
CN107200315B (en) * 2017-06-28 2023-07-21 四川省高宇化工有限公司 Method and device for producing monoammonium phosphate based on multi-neutralization wet-process phosphoric acid
CN108751152B (en) * 2018-05-30 2022-03-18 湖北三宁化工股份有限公司 Method for improving pH value of industrial monoammonium phosphate produced by wet-process phosphoric acid
CN110844897B (en) * 2019-12-13 2023-08-29 中山市中环环保废液回收有限公司 Treatment method of waste phosphoric acid on running water treatment line

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