CN105731407B - The method of Wet-process Phosphoric Acid Production ammonium dihydrogen phosphate - Google Patents
The method of Wet-process Phosphoric Acid Production ammonium dihydrogen phosphate Download PDFInfo
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- CN105731407B CN105731407B CN201610220771.0A CN201610220771A CN105731407B CN 105731407 B CN105731407 B CN 105731407B CN 201610220771 A CN201610220771 A CN 201610220771A CN 105731407 B CN105731407 B CN 105731407B
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- crystal
- dihydrogen phosphate
- ammonium dihydrogen
- phosphoric acid
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/28—Ammonium phosphates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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Abstract
The invention discloses a kind of method of Wet-process Phosphoric Acid Production ammonium dihydrogen phosphate, concretely comprise the following steps：Using phosphoric acid by wet process neutralizer as initial feed, it is 1.36 1.38g/cm to be concentrated into density3Concentrate after pour into crystallization reaction begun to cool down in crystallizer, the crystal seed that particle mean size is 120 280 μm is added in 95 DEG C control ammonium dihydrogen phosphate crystallization nucleation under the stir speed (S.S.) of 240 350r/min, being cooled to 70 DEG C of 10 360min of thermostatical crystallizations reaction makes fine crystals uniform growth, being cooled to 50 DEG C of 10 180min of thermostatical crystallizations reaction makes crystal fully grow up, being cooled to 35 40 DEG C of 10 180min of thermostatical crystallizations reaction again makes crystal grow up completely, then filter, washing, it is dry, obtain complete crystal form, even particle size distribution and the ammonium dihydrogen phosphate crystal that particle mean size is 730 1000 μm.The present invention has the advantages that the reaction time is short, crystal grain is small and even particle size distribution, high income and economic benefit are obvious.
Description
Technical field
The invention belongs to industry cooling crystallization technique field, and in particular to a kind of side of Wet-process Phosphoric Acid Production ammonium dihydrogen phosphate
Method.
Background technology
Ammonium dihydrogen phosphate abbreviation MAP, molecular formula NH4H2PO4, water white transparency tetragonal system crystal is soluble easily in water, is slightly soluble in
Alcohol, insoluble in acetone, relatively stablizes, is heated to having fraction decomposition at 100 DEG C in atmosphere.Ammonium dihydrogen phosphate industry, food,
The sector applications such as medicine are relatively broad, not the still primary raw material of dry powder fire extinguishing agent and be instant capacity high efficiency composition drip irrigation fertilizer
Material, phosphorus ore belongs to non-renewable resources, as international market increasingly increases ammonium dihydrogen phosphate product demand, and world Gao Pin
The rapid exhaustion of position phosphate rock resource, causes holding at high price for the product.
In recent years, it is right although ammonium dihydrogen phosphate has done some researchs in some domestic schools, enterprise, research institution etc.
Less in ammonium dihydrogen phosphate crystallisation by cooling process study, the research to product crystal form is fewer and fewer.It is reported that Sichuan connection in 2001
Close university and invented the method that PHOSPHORIC ACID TECH.GRADE, food grade phosphoric acid and ammonium dihydrogen phosphate are prepared with phosphoric acid by wet process, make phosphoric acid by wet process
Rational classified utilization is obtained, the added value of phosphorus also increases；The same year Sichuan Long Mang, Group Co., Ltd was wet with extracting first
Method phosphoric acid production ammonium dihydrogen phosphate, product have reached the quality standard of ammonium dihydrogen phosphate；Dang Yagu, Fei Dejun are equal to 2010
《Inorganic chemicals industry》In " research of Wet-process Phosphoric Acid Production fine monoammonium phosphate crystallization improver " ammonia neutralisation purification wet method phosphorus is discussed
The effect of acid, has filtered out suitable crystallization improver；The 50kt/a ammonium dihydrogen phosphate devices of Hubei Ezhong Chemical Industry Co., Ltd.
It is constructed and put into operation in May, 2011.Except Hubei auspicious cloud in 2012（Group）Chemical inc and Wuhan Engineering Univ
Cooperate beyond the method for crystallising of research bulky grain ammonium dihydrogen phosphate, the change of ammonium dihydrogen phosphate is mainly focused in these above-mentioned researchs
The property learned Quality Research, and it is very few to its physical Quality Research.
In conclusion the quality of ammonium dihydrogen phosphate was not only influenced by product composition, but also influenced by product external quality.By
During crystallisation by cooling, reaction temperature cooling is more, and reactive crystallization speed is also accelerated when cooling down too fast based on Temperature fall, brilliant
Karyomorphism into speed be far longer than its growth speed, nucleus is not had enough growths, new nucleus produces again, so as to cause
Ammonium dihydrogen phosphate product grain size differs, or even crystal adhesion, has seriously affected the quality of product.Therefore, develop energy consumption it is low,
The method of crystal perfection and the ammonium dihydrogen phosphate of even particle size distribution is even more important.
The content of the invention
The technical problem to be solved by the present invention is to provide a kind of method of Wet-process Phosphoric Acid Production ammonium dihydrogen phosphate, party's legal system
The ammonium dihydrogen phosphate product crystal form obtained is perfect, and granularity is small and is evenly distributed, and yield is higher.
The present invention is to solve above-mentioned technical problem to adopt the following technical scheme that, the side of Wet-process Phosphoric Acid Production ammonium dihydrogen phosphate
Method, it is characterised in that concretely comprise the following steps：Using phosphoric acid by wet process neutralizer as initial feed, it is 1.36- to be concentrated into density
1.38g/cm3Concentrate after pour into crystallization reaction begun to cool down in crystallizer, under the stir speed (S.S.) of 200-350r/min in
95 DEG C add the crystal seed that particle mean size is 120-280 μm and control ammonium dihydrogen phosphate crystallization nucleation, and the wherein addition of crystal seed is dense
The 0.1%-6% of contracting liquid quality, being cooled to 70 DEG C of thermostatical crystallization reaction 10-360min makes fine crystals uniform growth, is cooled to 50
DEG C thermostatical crystallization reaction 10-180min makes crystal fully grow up, then is cooled to 35-40 DEG C of thermostatical crystallization 10-180min and makes crystal
Growth completely, is then filtered, and is washed, dry, and it is 730-1000 μm to obtain complete crystal form, even particle size distribution and particle mean size
Ammonium dihydrogen phosphate crystal.
Further preferably, the specific preparation process of the crystal seed is：It is using phosphoric acid by wet process neutralizer as initial feed, its is dense
It is 1.36-1.38g/cm to be reduced to density3Concentrate after pour into and start crystallization reaction in crystallizer, question response temperature is down to naturally
A large amount of nucleus are produced at 80-90 DEG C, filters, washs, it is 120- that drying, which obtains particle mean size, after thermostatical crystallization growth 15-35min
280 μm of crystal seed.
Further limit, the addition of the crystal seed is the 0.3%-2% of concentrate quality.
Further preferably, the rate of temperature fall of temperature-fall period is 0.4-0.7 DEG C/min.
Further preferably, being cooled to 70 DEG C of thermostatical crystallization reaction 30-100min makes fine crystals uniform growth.
Further preferably, being cooled to 50 DEG C of thermostatical crystallization reaction 20-60min makes crystal fully grow up.
Further preferably, being cooled to 35-40 DEG C of thermostatical crystallization reaction 20-60min makes crystal grow up completely.
Further preferably, the crystal wash solution used in washing process is acetone.
Ammonium dihydrogen phosphate new crystalline technology provided by the invention makes crystal have time enough in each stage of reaction, makes production
Product are sufficiently grown up, and are avoided since reaction cooling is too fast, a large amount of fine crystals cannot sufficiently grow up, and cause to react
Liquid carries many fine crystals secretly, solves that ammonium dihydrogen phosphate size distribution is uneven and the technical barrier of the easy adhesion of crystal, has
Effect improves the yield and crystal form quality of crystalline product.The present invention is with the reaction time is short, crystal grain is small and size distribution is equal
Even, the advantages that high income and economic benefit are obvious.
Brief description of the drawings
Fig. 1 is the SEM figures of the ammonium dihydrogen phosphate crystal of existing industrial crystallization；
Fig. 2 is the SEM figures of ammonium dihydrogen phosphate crystal made from the embodiment of the present invention 1；
Fig. 3 is the particle size distribution figure of ammonium dihydrogen phosphate crystal made from distinct methods.
Embodiment
The above of the present invention is described in further details by the following examples, but this should not be interpreted as to this
The scope for inventing above-mentioned theme is only limitted to following embodiment, and all technologies realized based on the above of the present invention belong to this hair
Bright scope.
Embodiment 1
The density of phosphoric acid by wet process neutralizer is concentrated into 1.37g/cm3After pour into crystallization reaction begun to cool down in crystallizer,
It is 270r/min in stir speed (S.S.), under conditions of falling temperature gradient is 0.6 DEG C/min, it is 140 that 2.19g particle mean sizes are added in 95 DEG C
μm crystal seed, control ammonium dihydrogen phosphate crystallization nucleation, temperature to be crystallized be down to 70 DEG C start thermostatical crystallizations reaction 40min make crystal
Uniform growth, it is an isothermal reaction point that 50 DEG C are down to from 70 DEG C, and thermostatical crystallization reaction 60min makes crystal fully grow up, followed by
Continuous Jiang Wei to 40 DEG C of thermostatical crystallization reaction 30min, filtering, is washed with absolute ethyl alcohol, and drying to weight obtains 58.27g di(2-ethylhexyl)phosphates
Hydrogen ammonium product, its purity are 98.71%, and complete crystal form, any surface finish, granularity is small and is evenly distributed.
Embodiment 2
The density of phosphoric acid by wet process neutralizer is concentrated into 1.36g/cm3After pour into crystallization reaction begun to cool down in crystallizer,
It is 300r/min in stir speed (S.S.), under conditions of falling temperature gradient is 0.6 DEG C/min, it is 260 that 4.83g particle mean sizes are added in 95 DEG C
μm crystal seed, control ammonium dihydrogen phosphate crystallization nucleation, temperature to be crystallized be down to 70 DEG C start thermostatical crystallizations reaction 60min make crystal
Uniform growth, it is an isothermal reaction point that 50 DEG C are down to from 70 DEG C, and thermostatical crystallization reaction 35min makes crystal fully grow up, followed by
Continuous to be cooled to 38 DEG C of thermostatical crystallization reaction 55min, filtering, is washed with absolute ethyl alcohol, and drying to weight obtains 74.21g di(2-ethylhexyl)phosphates
Hydrogen ammonium product, its purity are 98.64%, and complete crystal form, any surface finish, granularity is small and is evenly distributed.
Embodiment 3
The density of phosphoric acid by wet process neutralizer is concentrated into 1.38g/cm3After pour into crystallization reaction begun to cool down in crystallizer,
It is 330r/min in stir speed (S.S.), under conditions of falling temperature gradient is 0.5 DEG C/min, it is 190 that 7.34g particle mean sizes are added in 95 DEG C
μm crystal seed, control ammonium dihydrogen phosphate crystallization nucleation, temperature to be crystallized be down to 70 DEG C start thermostatical crystallizations reaction 80min make crystal
Uniform growth, it is an isothermal reaction point that 50 DEG C are down to from 70 DEG C, and thermostatical crystallization reaction 50min makes crystal fully grow up, followed by
Continuous to be cooled to 36 DEG C of thermostatical crystallization reaction 40min, filtering, is washed with absolute ethyl alcohol, and drying to weight obtains 77.91g di(2-ethylhexyl)phosphates
Hydrogen ammonium product, its purity are 98.69%, and complete crystal form, any surface finish, granularity is small and is evenly distributed.
Embodiment 4
The density of phosphoric acid by wet process neutralizer is concentrated into 1.37g/cm3After pour into crystallization reaction begun to cool down in crystallizer,
It is 230r/min in stir speed (S.S.), under conditions of falling temperature gradient is 0.7 DEG C/min, it is 210 that 2.19g particle mean sizes are added in 95 DEG C
μm crystal seed, control ammonium dihydrogen phosphate crystallization nucleation, temperature to be crystallized be down to 70 DEG C start thermostatical crystallizations reaction 75min make crystal
Uniform growth, it is an isothermal reaction point that 50 DEG C are down to from 70 DEG C, and thermostatical crystallization reaction 50min makes crystal fully grow up, followed by
Continuous to be cooled to 39 DEG C of thermostatical crystallization reaction 35min, filtering, is washed with absolute ethyl alcohol, and drying to weight obtains 61.35g di(2-ethylhexyl)phosphates
Hydrogen ammonium product, its purity are 98.50%, and complete crystal form, any surface finish, granularity is small and is evenly distributed.
Basic principle, main features and advantages embodiment above describes the present invention, the technical staff of the industry should
Understand, the present invention is not limited to the above embodiments, and the above embodiments and description only describe the original of the present invention
Reason, under the scope for not departing from the principle of the invention, various changes and modifications of the present invention are possible, these changes and improvements are each fallen within
In the scope of protection of the invention.
Claims (3)
1. the method for Wet-process Phosphoric Acid Production ammonium dihydrogen phosphate, it is characterised in that concretely comprise the following steps：It is first using phosphoric acid by wet process neutralizer
Beginning raw material, it is 1.36-1.38g/cm to be concentrated into density3Concentrate after pour into crystallization reaction begun to cool down in crystallizer,
The crystal seed that particle mean size is 120-280 μm is added in 95 DEG C control ammonium dihydrogen phosphate knot under the stir speed (S.S.) of 200-350r/min
Crystalline substance nucleation, the wherein addition of crystal seed are the 0.1%-6% of concentrate quality, are cooled to 70 DEG C of thermostatical crystallization reaction 30-100min
Make fine crystals uniform growth, being cooled to 50 DEG C of thermostatical crystallization reaction 20-60min makes crystal fully grow up, then is cooled to 35-40
DEG C thermostatical crystallization 20-60min makes crystal grow up completely, and the rate of temperature fall of temperature-fall period is 0.4-0.7 DEG C/min, is then filtered,
Washing, it is dry, obtain the ammonium dihydrogen phosphate crystal that complete crystal form, even particle size distribution and particle mean size are 730-1000 μm, institute
The specific preparation process for stating crystal seed is：Using phosphoric acid by wet process neutralizer as initial feed, it is 1.36-1.38g/ to be concentrated into density
cm3Concentrate after pour into and start crystallization reaction in crystallizer, question response temperature produces a large amount of brilliant when being down to 80-90 DEG C naturally
Core, thermostatical crystallization filter after growing 15-35min, wash, and drying obtains the crystal seed that particle mean size is 120-280 μm.
2. the method for Wet-process Phosphoric Acid Production ammonium dihydrogen phosphate according to claim 1, it is characterised in that：The crystal seed adds
Enter the 0.3%-2% that amount is concentrate quality.
3. the method for Wet-process Phosphoric Acid Production ammonium dihydrogen phosphate according to claim 1, it is characterised in that：Used in washing process
Crystal wash solution be acetone.
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| CN201610220771.0A CN105731407B (en) | 2016-04-11 | 2016-04-11 | The method of Wet-process Phosphoric Acid Production ammonium dihydrogen phosphate |
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| CN105731407B true CN105731407B (en) | 2018-04-27 |
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| CN103569982B (en) * | 2013-11-08 | 2015-05-20 | 武汉工程大学 | Method for crystallizing large-grained industrial ammonium dihydrogen phosphate |
| CN103754851B (en) * | 2014-01-08 | 2016-05-04 | 瓮福（集团）有限责任公司 | A kind of preparation method of LITHIUM BATTERY crystal phosphoric acid ammonium dihydrogen |
| CN104058378B (en) * | 2014-07-09 | 2015-11-18 | 昆明隆祥化工有限公司 | The method of monoammonium phosphate and magnesium ammonium phosphate is produced with the acid of wet method concentrated phosphoric acid slag |
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