CN104528675B - Utilize method and the whipping appts of wet purification phosphoric acid production crystal phosphoric acid one ammonium - Google Patents
Utilize method and the whipping appts of wet purification phosphoric acid production crystal phosphoric acid one ammonium Download PDFInfo
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Abstract
The present invention relates to the preparation field of monoammonium phosphate, specifically, it relates to a kind of method and whipping appts utilizing wet purification phosphoric acid production crystal phosphoric acid one ammonium, eliminate in thermal phosphoric acid required pretreatment technology, and save investment, simplify operation. Comprising the following steps: after (1) adds the mother liquor of predetermined amount in neutralizing well, then add through measuring the purification of wet process phosphoric acid mixing that purity is 85%, to mixed solution, the mass concentration of phosphoric acid is 35-45%; (2) starting whipping appts, add ammonia by multiple spot and add liquefied ammonia neutralization, control adds the speed of liquefied ammonia, continues to add stopping neutralization when the 80-100 minute pH value to solution reaches 4.2��4.6; (3), after qualified after testing, the crystallisation by cooling stage is entered; (4) after crystallization completes, slurry dewatering, drying are obtained crystal phosphoric acid one ammonium, and the mother liquor deviate from is delivered to mother liquor storage groove and recycles.
Description
Technical field
The present invention relates to the preparation field of monoammonium phosphate, specifically, it relates to a kind of method and whipping appts utilizing wet purification phosphoric acid production crystal phosphoric acid one ammonium.
Background technology
Monoammonium phosphate Ammoniumdihydrogenphosphate; Ammoniumphosphate, monobasic, molecular formula: NH4H2PO4Molecular weight: 115.03 monoammonium phosphates are also known as primary ammonium phosphate. Water white transparency tetragonal spheroidal crystal, density 1.803 (19 DEG C). Fusing point 190 DEG C, soluble in water, it is slightly soluble in alcohol, it is insoluble to acetone. The aqueous solution, in acid, should make fodder additives, high-efficiency compound fertilizer. [
Monoammonium phosphate (MAP) is a kind of water soluble quick-acting composite fertilizer, available phosphorus (AP2O5) it is about 5.44:1 with the ratio of total nitrogen (TN) content, it is one of the main kind of high-concentration phosphate compound fertilizers. This product generally topdresses, and is also produce ternary compound fertilizer, the fertile topmost basic material of BB; This product is widely used in various food crop and the cash crop such as paddy rice, wheat, corn, Chinese sorghum, cotton, melon and fruit, vegetables; It is widely used in the various soil properties such as red soil, yellow earth, brown earth, yellow moist soil, black earth, cinnamon soil, purple soil, Baijiang soil; It is particularly suitable for the drought areas such as NORTHWEST CHINA, North China, northeast to use.
The raw material producing monoammonium phosphate is phosphoric acid and ammonia, can produce phosphorus ammonium with ammonia neutralising phosphoric acid. By different phosphoric acid production methods, can being divided into thermal phosphoric acid and phosphoric acid by wet process, take yellow phosphorus as raw material, through oxidation, the phosphoric acid that aquation etc. are reacted and produced is called thermal phosphoric acid. According to the P at different temperature2O5Different hydration reactions, can obtain ortho-phosphoric acid (referred to as phosphoric acid), tetra-sodium and metaphosphoric acid etc. multiple, but wherein the most important thing is ortho-phosphoric acid. The phosphoric acid obtained with sulfuric acid, nitric acid or decomposing phosphate rock by chlorhydric acid is referred to as phosphoric acid by wet process, and is method the most basic in Wet-process Phosphoric Acid Production by the method for the obtained phosphoric acid of sulfuric acid decomposing phosphate rock. Due to economic benefit, for the phosphoric acid of processed fertilizer ammonium phosphate, big multiplex phosphoric acid by wet process.
Ammonium neutralization reaction: phosphoric acid has three hydrogen atoms, they can successively with ammonia react generation ammonium neutralization reaction, generate monoammonium phosphate (MAP) NH successively4H2PO4, diammonium phosphate (DAP) (NH4)2HPO4, triammonium phosphate (NH4)3PO4. Reactional equation is as follows:
H3PO4(l)+NH3(g)==NH4H2PO4(s) �� H298=126kJ
H3PO4(l)+2NH3(g)==(NH4)2HPO4(s) �� H298=203kJ
H3PO4(l)+3NH3(g)==(NH4)3PO4(s) �� H298=256kJ
Pure ammonium phosphate salt is all white crystal, and wherein stable with monoammonium phosphate, crystal habit is tetragonal spheroidal, is heated to more than 130 DEG C and just can decompose releasing ammonia, becomes tetra-sodium even metaphosphoric acid; Diammonium phosphate is more stable, and crystal habit is oblique system, starts when temperature reaches 90 DEG C to decompose and releases ammonia, becomes monoammonium phosphate. Monoammonium phosphate and diammonium phosphate are all high concentration N phosphorus composite fertilizers. Triammonium phosphate is then very unstable, and crystal habit is rhombic system, just can release ammonia at normal temperatures, become diammonium phosphate, should not make commercial fertilizer and use.
With phosphoric acid by wet process the difference is that, thermal phosphoric acid can obtain the higher phosphoric acid of purity, and phosphoric acid by wet process then can only obtain the phosphoric acid containing certain impurity. Meanwhile, containing excessive arsenic and heavy metal in thermal phosphoric acid, it is easy to form residual in the product, finally can cause environmental pollution. And the process of phosphorous acid production by BEP crystal phosphoric acid one ammonium needs through pre-treatment, with the excessive arsenic removed in thermal phosphoric acid and heavy metal. Throw out, for add sodium sulphite in thermal phosphoric acid, to produce the throw out of arsenic and heavy metal, then is removed, to reach the object of dearsenification and removing heavy-metal by pretreated technique by filtering. And flow process is complicated, cost height. Meanwhile, in the process of phosphorous acid production by BEP monoammonium phosphate, electricity consumption is high, mixed effect is poor, crystallization time length, effect are undesirable.
And the cost of Wet-process Phosphoric Acid Production crystal phosphoric acid one ammonium is lower, but its product purity is not as the purity height of crystal phosphoric acid one ammonium of phosphorous acid production by BEP, even if after follow-up cleaning section, its purity is still undesirable.
In view of this, special proposition the present invention.
Summary of the invention
It is an object of the invention to provide a kind of method utilizing brand-new wet purification phosphoric acid production crystal phosphoric acid one ammonium, eliminate in thermal phosphoric acid required pretreatment technology, and save investment, simplify operation.
2nd object of the present invention is to provide the whipping appts used in a kind of described method utilizing wet purification phosphoric acid production crystal phosphoric acid one ammonium. Because the whipping appts used in prior art stirs for bilayer, and two layers of blade structure stirred are identical, and its mixing effect is not good, electricity consumption is high, mixed effect is poor. Original whipping appts has been carried out the improvement more rationalized by the present invention, and the mixing effect after change is good, and after each production cycle completes, reactor sidewall and bottom produce without buildup. Energy consumption is low, and the use power of existing stirring rake is lower than original stirring rake. Overall stirring intensity reduces, and the destruction of crystallization is little, product advantages of good crystallization.
In order to realize the above-mentioned purpose of the present invention, spy by the following technical solutions:
Utilize a method for wet purification phosphoric acid production crystal phosphoric acid one ammonium, comprise the following steps:
(1) after adding the mother liquor of predetermined amount in neutralizing well, then adding through measuring the purification of wet process phosphoric acid mixing that purity is 85%, to mixed solution, the mass concentration of phosphoric acid is 35-45%;
(2) starting whipping appts, add ammonia by multiple spot and add liquefied ammonia neutralization, control adds the speed of liquefied ammonia, continues to add stopping neutralization when the 80-100 minute pH value to solution reaches 4.2��4.6;
(3), after qualified after testing, the crystallisation by cooling stage is entered;
(4) after crystallization completes, slurry dewatering, drying are obtained crystal phosphoric acid one ammonium, and the mother liquor deviate from is delivered to mother liquor storage groove and recycles.
In prior art, it is that single-point adds ammonia, its mass transfer effect is poor, and a kind of method utilizing brand-new wet purification phosphoric acid production crystal phosphoric acid one ammonium provided by the invention, wherein add ammonia by multiple spot and add liquefied ammonia neutralization, using multiple pipe that adds to carry out adding ammonia when specifically adding liquefied ammonia, such mass transfer effect is good, reaction efficiency height.
Eliminate in thermal phosphoric acid required pretreatment technology, and save investment, simplify operation. And mother liquor is recycled, be conducive to cost-saving and resource.
Further, in step (1), in described mixed solution, the mass concentration of phosphoric acid is 38-40%.
Further, in step (2), the time adding liquefied ammonia is that 90 minutes pH value to solution reach 4.3��4.5.
Further, in step (3), when beginning to cool down, adopt naturally cooling; When starching temperature and drop to 68-72 DEG C, open reacting kettle jacketing water coolant and carry out forcing cooling; Until when temperature is down to normal temperature, cooling time is controlled to 80-100 minute.
The present invention also provides the whipping appts used in a kind of method utilizing wet purification phosphoric acid production crystal phosphoric acid one ammonium, comprises stir storehouse and stirring rake; Described stirring rake is included in described stir storehouse from the stationary shaft running through setting under upper, and the agitating vane being located on described stationary shaft;
Described stirring rake is provided with the first agitating vane and the 2nd agitating vane, is all set on described stationary shaft; The blade surface level of described first agitating vane L-shaped structure, its one end is fixedly connected with central shaft, and its other end is horizontal-extending; The blade of described 2nd agitating vane is arc, and its one end is fixedly connected with central shaft, and its other end is horizontal-extending.
Because the whipping appts used in prior art stirs for bilayer, and two layers of blade structure stirred are identical, so slurries are in the process of flowing rotation like this, the stirring extent of its levels is completely identical, it is arranged in stir storehouse and forms a big whirlpool rotated to identical direction, fundamentally slurries fully can not be stirred, its mixing effect is good and because the stirring like this of short period of time can not reach the mixing effect of expection, so churning time length electricity consumption is high and mixed effect is poor.
Original whipping appts has been carried out the improvement more rationalized by the present invention, the structure arranging the first agitating vane and the 2nd agitating vane is completely different, first agitating vane is three wider agitating vanes of level completely, slurries in it completely are thoroughly stirred by it at the middle part of stir storehouse, and it is located at the blade that the 2nd agitating vane bottom stir storehouse is set to arc, like this, when the slurries on upper strata fall bottom, the drive of the 2nd agitating vane, its rotary motion trace changes completely, the slurries of lower floor can be stirred to brand-new direction again again, like this can fully by even for the slurry agitation in stir storehouse, and mass transfer effect is good, make the uniformity coefficient of xln finally obtained better. and each production cycle complete after reactor sidewall and bottom produce without buildup. energy consumption is low, the use power reduction of stirring rake, and overall stirring intensity reduces, and the destruction of crystallization is little, product advantages of good crystallization.
Further, described first agitating vane and described 2nd agitating vane are turbine type blade, and described first agitating vane is located at the top of described 2nd agitating vane, and described 2nd agitating vane is located at the bottom of described stir storehouse.
Further, vertical with the bearing of trend of described stationary shaft in direction described in the width of described first its blade of agitating vane; Direction described in the width of the blade of described 2nd agitating vane of arc is parallel with the bearing of trend of described central shaft.
In order to can well by the slurry agitation of lower floor, it is possible to the direction, width place arranging the blade that first mixes blade is vertical with the bearing of trend of stationary shaft, is also exactly so-called radial-flow type blade, refers to that the main discharge opeing direction of blade is vertical with stir shaft. The direction, width of blade place that can arrange the 2nd agitating vane is parallel with the bearing of trend of stationary shaft, is also exactly so-called axial-flow type blade, refers to that the main discharge opeing direction of blade is parallel with stir shaft.
Further, the width of blade of described first agitating vane is greater than the width of blade of described 2nd agitating vane.
Little in order to reduce the destruction to crystallization, it is possible to the width of blade arranging the 2nd agitating vane is less, can prevent from well like this destroying the xln formed, avoid making it again be grown to bigger xln, affect the homogeneity of final xln.
Further, the width of the blade on described 2nd agitating vane is the 1/4-1/5 of the width of the blade on described first agitating vane.
Further, the blade on described first agitating vane and described 2nd agitating vane is all uniformly distributed; Blade quantity��4 on described first agitating vane, and more than the blade quantity on described, the blade quantity on described 2nd agitating vane is minimum is 2.
Preferably, it is possible to arranging the blade quantity on the first agitating vane is 3, and the blade quantity on the 2nd agitating vane is 2.
Compared with prior art, the useful effect of the present invention is:
(1) eliminate phosphoric acid pretreatment technology, save investment, simplify operation;
(2) single-point adds ammonia and becomes multiple spot and add ammonia, and mass transfer effect is good.
(3) changing the period of crystallisation by cooling, and the destruction of stirring rake is little, crystallization effect is good, and visual appearance is good.
(4) structure arranging the first agitating vane and the 2nd agitating vane is completely different, and the mixing effect after change is good, and after each production cycle completes, reactor sidewall and bottom produce without buildup. Energy consumption is low, and the use power of existing stirring rake is lower than original stirring rake. Overall stirring intensity reduces, and the destruction of crystallization is little, product advantages of good crystallization.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, it is briefly described to the accompanying drawing used required in embodiment or description of the prior art below.
Fig. 1 is a kind of method process flow sheet utilizing wet purification phosphoric acid production crystal phosphoric acid one ammonium provided by the invention;
Fig. 2 is the structural representation of the whipping appts of offer in the present invention;
Fig. 3 is the structural representation of the first agitating vane in whipping appts provided by the invention;
Fig. 4 is the structural representation of the 2nd agitating vane in whipping appts provided by the invention;
1. the first agitating vane, 2. the 2nd agitating vane, 3. stationary shaft.
Embodiment
Embodiment of the present invention being described in detail below in conjunction with embodiment, but it will be understood to those of skill in the art that, the following example is only for illustration of the present invention, and should not be considered as limiting the scope of the invention. Unreceipted concrete condition person in embodiment, conveniently the condition of condition or manufacturers's suggestion carries out. Agents useful for same or the unreceipted production firm person of instrument, be and can buy, by commercially available, the conventional products obtained.
As shown in Figure 1, a kind of method utilizing wet purification phosphoric acid production crystal phosphoric acid one ammonium, comprises the following steps:
(1) after adding the mother liquor of predetermined amount in neutralizing well, then adding through measuring the purification of wet process phosphoric acid mixing that purity is 85%, to mixed solution, the mass concentration of phosphoric acid is 35-45%;
Preferably, in described mixed solution, the mass concentration of phosphoric acid is 38-40%.
(2) starting whipping appts, add ammonia by multiple spot and add liquefied ammonia neutralization, control adds the speed of liquefied ammonia, continues to add stopping neutralization when the 80-100 minute pH value to solution reaches 4.2��4.6;
Preferably, the time adding liquefied ammonia is that 90 minutes pH value to solution reach 4.3��4.5.
(3), after qualified after testing, the crystallisation by cooling stage is entered;
Preferably, when beginning to cool down, adopt naturally cooling; When starching temperature and drop to 68-72 DEG C, open reacting kettle jacketing water coolant and carry out forcing cooling; Until when temperature is down to normal temperature, cooling time is controlled to 80-100 minute.
(4) after crystallization completes, slurry dewatering, drying are obtained monoammonium phosphate crystal, and the mother liquor deviate from is delivered to mother liquor storage groove and recycles.
In prior art, it is that single-point adds ammonia, its mass transfer effect is poor, and a kind of method utilizing brand-new wet purification phosphoric acid production crystal phosphoric acid one ammonium provided by the invention, wherein add ammonia by multiple spot and add liquefied ammonia neutralization, using multiple pipe that adds to carry out adding ammonia when specifically adding liquefied ammonia, such mass transfer effect is good, reaction efficiency height.
Eliminate in thermal phosphoric acid required pretreatment technology, and save investment, simplify operation. And mother liquor is recycled, be conducive to cost-saving and resource.
As shown in Figure 2-4, the present invention also provides the whipping appts used in a kind of method utilizing wet purification phosphoric acid production crystal phosphoric acid one ammonium, comprises stir storehouse and stirring rake; Described stirring rake is included in described stir storehouse from the stationary shaft 3 running through setting under upper, and the agitating vane being located on described stationary shaft 3;
Described stirring rake is provided with the first agitating vane 1 and the 2nd agitating vane 2, is all set on described stationary shaft 3; The blade surface level of described first agitating vane 1 L-shaped structure, its one end is fixedly connected with central shaft, and its other end is horizontal-extending; The blade of described 2nd agitating vane 2 is arc, and its one end is fixedly connected with central shaft, and its other end is horizontal-extending.
Because the whipping appts used in prior art stirs for bilayer, and two layers of blade structure stirred are identical, so slurries are in the process of flowing rotation like this, the stirring extent of its levels is completely identical, it is arranged in stir storehouse and forms a big whirlpool rotated to identical direction, fundamentally slurries fully can not be stirred, its mixing effect is good and because the stirring like this of short period of time can not reach the mixing effect of expection, so churning time length electricity consumption is high and mixed effect is poor.
Original whipping appts has been carried out the improvement more rationalized by the present invention, the structure arranging the first agitating vane 1 and the 2nd agitating vane 2 is completely different, first agitating vane 1 is three wider agitating vanes of level completely, slurries in it completely are thoroughly stirred by it at the middle part of stir storehouse, and it is located at the blade that the 2nd agitating vane 2 bottom stir storehouse is set to arc, like this, when the slurries on upper strata fall bottom, the drive of the 2nd agitating vane 2, its rotary motion trace changes completely, the slurries of lower floor can be stirred to brand-new direction again again, like this can fully by even for the slurry agitation in stir storehouse, and mass transfer effect is good, make the uniformity coefficient of xln finally obtained better. and each production cycle complete after reactor sidewall and bottom produce without buildup. energy consumption is low, the use power reduction of stirring rake, and overall stirring intensity reduces, and the destruction of crystallization is little, product advantages of good crystallization.
Preferably, described first agitating vane 1 and described 2nd agitating vane 2 are turbine type blade, and described first agitating vane 1 is located at the top of described 2nd agitating vane 2, and described 2nd agitating vane 2 is located at the bottom of described stir storehouse.
Preferably, vertical with the bearing of trend of described stationary shaft 3 in direction described in the width of described first its blade of agitating vane 1; Direction described in the width of the blade of described 2nd agitating vane 2 of arc is parallel with the bearing of trend of described central shaft.
In order to can well by the slurry agitation of lower floor, it is possible to the direction, width place arranging the blade that first mixes blade is vertical with the bearing of trend of stationary shaft 3, is also exactly so-called radial-flow type blade, refers to that the main discharge opeing direction of blade is vertical with stir shaft. The direction, width of blade place that can arrange the 2nd agitating vane 2 is parallel with the bearing of trend of stationary shaft 3, is also exactly so-called axial-flow type blade, refers to that the main discharge opeing direction of blade is parallel with stir shaft.
Preferably, the width of blade of described first agitating vane 1 is greater than the width of blade of described 2nd agitating vane 2.
Little in order to reduce the destruction to crystallization, it is possible to the width of blade arranging the 2nd agitating vane 2 is less, can prevent from well like this destroying the xln formed, avoid making it again be grown to bigger xln, affect the homogeneity of final xln.
Preferably, the width of the blade on described 2nd agitating vane 2 is the 1/4-1/5 of the width of the blade on described first agitating vane 1.
Preferably, the blade on described first agitating vane 1 and described 2nd agitating vane 2 is all uniformly distributed; Blade quantity��4 on described first agitating vane 1, and more than the blade quantity on described, the blade quantity on described 2nd agitating vane 2 is minimum is 2.
Preferably, it is possible to the blade quantity arranged on the first agitating vane 1 is 3, the blade quantity on the 2nd agitating vane 2 is 2.
Embodiment 1
Utilize a method for wet purification phosphoric acid production crystal phosphoric acid one ammonium, comprise the following steps:
(1) after adding the mother liquor of predetermined amount in neutralizing well, then adding through measuring the purification of wet process phosphoric acid mixing that purity is 85%, to mixed solution, the mass concentration of phosphoric acid is 35-45%;
(2) starting whipping appts, add ammonia by multiple spot and add liquefied ammonia neutralization, control adds the speed of liquefied ammonia, continues to add stopping neutralization when the 80-100 minute pH value to solution reaches 4.2��4.6;
(3), after qualified after testing, the crystallisation by cooling stage is entered;
(4) after crystallization completes, slurry dewatering, drying are obtained crystal phosphoric acid one ammonium, and the mother liquor deviate from is delivered to mother liquor storage groove and recycles.
Embodiment 2
Utilize a method for wet purification phosphoric acid production crystal phosphoric acid one ammonium, comprise the following steps:
(1) after adding the mother liquor of predetermined amount in neutralizing well, then adding through measuring the purification of wet process phosphoric acid mixing that purity is 85%, to mixed solution, the mass concentration of phosphoric acid is 40%;
(2) starting whipping appts, add ammonia by multiple spot and add liquefied ammonia neutralization, control adds the speed of liquefied ammonia, continues to add stopping neutralization when 90 minutes pH value to solution reach 4.3;
(3), after qualified after testing, the crystallisation by cooling stage is entered; When beginning to cool down, adopt naturally cooling; When starching temperature and drop to 70 DEG C, open reacting kettle jacketing water coolant and carry out forcing cooling; Until when temperature is down to normal temperature, being controlled to 90 minutes cooling time.
(4) after crystallization completes, slurry dewatering, drying are obtained monoammonium phosphate crystal, and the mother liquor deviate from is delivered to mother liquor storage groove and recycles.
Embodiment 3
Utilize the whipping appts used in the method for wet purification phosphoric acid production crystal phosphoric acid one ammonium, it is characterised in that, comprise stir storehouse and stirring rake; Described stirring rake is included in described stir storehouse from the stationary shaft 3 running through setting under upper, and the agitating vane being located on described stationary shaft 3;
Described stirring rake is provided with the first agitating vane 1 and the 2nd agitating vane 2, is all set on described stationary shaft 3; The blade surface level of described first agitating vane 1 L-shaped structure, its one end is fixedly connected with central shaft, and its other end is horizontal-extending; The blade of described 2nd agitating vane 2 is arc, and its one end is fixedly connected with central shaft, and its other end is horizontal-extending.
Embodiment 4
Utilize the whipping appts used in the method for wet purification phosphoric acid production crystal phosphoric acid one ammonium, it is characterised in that, comprise stir storehouse and stirring rake; Described stirring rake is included in described stir storehouse from the stationary shaft 3 running through setting under upper, and the agitating vane being located on described stationary shaft 3;
Described stirring rake is provided with the first agitating vane 1 and the 2nd agitating vane 2, is all set on described stationary shaft 3; The blade surface level of described first agitating vane 1 L-shaped structure, its one end is fixedly connected with central shaft, and its other end is horizontal-extending; The blade of described 2nd agitating vane 2 is arc, and its one end is fixedly connected with central shaft, and its other end is horizontal-extending;
Described first agitating vane 1 is located at the top of described 2nd agitating vane 2, and described 2nd agitating vane 2 is located at the bottom of described stir storehouse;
Described in the width of described first its blade of agitating vane 1 vertical with the bearing of trend of described stationary shaft 3 in direction; Direction described in the width of the blade of described 2nd agitating vane 2 of arc is parallel with the bearing of trend of described central shaft;
The width of blade of described first agitating vane 1 is greater than the width of blade of described 2nd agitating vane 2, and described first agitating vane 1 comprises 3 blades, and described 2nd agitating vane 2 comprises 2 blades.
Experimental example 1
The appearance requirement of product is colourless or white crystal or powder by industrial grade monoammonium phosphate, it does not have grain size number is made specified in more detail.
But user in sales process is it is frequently desirable to crystalline particle is too thinless, and with wanting evenly. Meanwhile, in process of production, crystalline particle is meticulous, when drying, it is easy to produce airborne dust, and the product loss caused when dried tail gas discharges is also bigger, and the receipts rate of product reduces, and consumes and increases.
Prior art and the embodiment of the present invention 1 and 3 combine the crystalline particle produced and contrast such as following table:
| Product cut size distributes | More than 120 orders | 60 orders are to 120 orders | Below 60 orders |
| Prior art | 3% to 5% | 60% to 75% | 20% to 40% |
| Basis is special obtains technology | 1% to 3% | 90% to 95% | It is less than 10% |
According to upper table it will be clear that, its size-grade distribution of monoammonium phosphate crystal produced by method provided by the invention and device is more even, more than 90% is distributed between 60-120 order, and the excessive or excessively little crystal grain more than 120 orders or below 60 orders is less.
Although illustrate and describing the present invention with specific embodiment, but it will be appreciated that can make when not deviating from the spirit and scope of the present invention many other change and amendment. Therefore, it means that comprise all such changes and modifications belonging in the scope of the invention in the following claims.
Claims (9)
1. one kind utilizes the method for wet purification phosphoric acid production crystal phosphoric acid one ammonium, it is characterised in that, comprise the following steps:
(1) after adding the mother liquor of predetermined amount in neutralizing well, then adding through measuring the purification of wet process phosphoric acid mixing that purity is 85%, to mixed solution, the mass concentration of phosphoric acid is 35-45%;
(2) starting whipping appts, add ammonia by multiple spot and add liquefied ammonia neutralization, control adds the speed of liquefied ammonia, continues to add stopping neutralization when the 80-100 minute pH value to solution reaches 4.2��4.6;
(3) after qualified after testing, enter the crystallisation by cooling stage: when beginning to cool down, adopt naturally cooling; When starching temperature and drop to 68-72 DEG C, open reacting kettle jacketing water coolant and carry out forcing cooling; Until when temperature is down to normal temperature, cooling time is controlled to 80-100 minute;
(4) after crystallization completes, slurry dewatering, drying are obtained monoammonium phosphate crystal, and the mother liquor deviate from is delivered to mother liquor storage groove and recycles.
2. the method utilizing wet purification phosphoric acid production crystal phosphoric acid one ammonium according to claim 1, it is characterised in that,
In step (1), in described mixed solution, the mass concentration of phosphoric acid is 38-40%.
3. the method utilizing wet purification phosphoric acid production crystal phosphoric acid one ammonium according to claim 1, it is characterised in that,
In step (2), the time adding liquefied ammonia is that 90 minutes pH value to solution reach 4.3-4.5.
4. the whipping appts used in the method utilizing wet purification phosphoric acid production crystal phosphoric acid one ammonium according to any one of claim 1-3, it is characterised in that, comprise stir storehouse and stirring rake; Described stirring rake is included in described stir storehouse from the stationary shaft running through setting under upper, and the agitating vane being located on described stationary shaft;
Described stirring rake is provided with the first agitating vane and the 2nd agitating vane, is all set on described stationary shaft; The blade surface level of described first agitating vane L-shaped structure, its one end is fixedly connected with central shaft, and its other end is horizontal-extending; The blade of described 2nd agitating vane is arc, and its one end is fixedly connected with central shaft, and its other end is horizontal-extending.
5. the whipping appts used in the method utilizing wet purification phosphoric acid production crystal phosphoric acid one ammonium according to claim 4, it is characterized in that, described first agitating vane is located at the top of described 2nd agitating vane, and described 2nd agitating vane is located at the bottom of described stir storehouse.
6. the whipping appts used in the method utilizing wet purification phosphoric acid production crystal phosphoric acid one ammonium according to claim 4, it is characterised in that, vertical with the bearing of trend of described stationary shaft in direction described in the width of described first its blade of agitating vane; Direction described in the width of the blade of described 2nd agitating vane of arc is parallel with the bearing of trend of described central shaft.
7. the whipping appts used in the method utilizing wet purification phosphoric acid production crystal phosphoric acid one ammonium according to claim 4, it is characterised in that, the width of blade of described first agitating vane is greater than the width of blade of described 2nd agitating vane.
8. the whipping appts used in the method utilizing wet purification phosphoric acid production crystal phosphoric acid one ammonium according to claim 7, it is characterised in that,
The width of the blade on described 2nd agitating vane is the 1/4-1/5 of the width of the blade on described first agitating vane.
9. the whipping appts used in the method utilizing wet purification phosphoric acid production crystal phosphoric acid one ammonium according to claim 4, it is characterised in that, the blade on described first agitating vane and described 2nd agitating vane is all uniformly distributed; Blade quantity��4 on described first agitating vane, and more than the blade quantity on described, the blade quantity on described 2nd agitating vane is minimum is 2.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101792134A (en) * | 2010-02-10 | 2010-08-04 | 侯炎学 | Process for producing industrial grade monoammonium phosphate |
| CN101857211A (en) * | 2010-06-04 | 2010-10-13 | 广西明利集团有限公司 | Method for preparing industrial grade monoammonium phosphate from wet-process phosphoric acid |
| CN201906575U (en) * | 2010-12-07 | 2011-07-27 | 鞍钢集团矿业公司 | Anti-sediment calcium oxide medicine drum |
| CN202028358U (en) * | 2011-03-25 | 2011-11-09 | 潍坊金瑞生物科技有限公司 | Stirring device used for ofloxacin dosing tank |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101792134A (en) * | 2010-02-10 | 2010-08-04 | 侯炎学 | Process for producing industrial grade monoammonium phosphate |
| CN101857211A (en) * | 2010-06-04 | 2010-10-13 | 广西明利集团有限公司 | Method for preparing industrial grade monoammonium phosphate from wet-process phosphoric acid |
| CN201906575U (en) * | 2010-12-07 | 2011-07-27 | 鞍钢集团矿业公司 | Anti-sediment calcium oxide medicine drum |
| CN202028358U (en) * | 2011-03-25 | 2011-11-09 | 潍坊金瑞生物科技有限公司 | Stirring device used for ofloxacin dosing tank |
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