CN104528675A - Method and stirring device for producing crystalline monoammonium phosphate by using wet-process purified phosphoric acid - Google Patents
Method and stirring device for producing crystalline monoammonium phosphate by using wet-process purified phosphoric acid Download PDFInfo
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Abstract
The invention relates to the field of preparation of monoammonium phosphate, particularly a method and stirring device for producing crystalline monoammonium phosphate by using wet-process purified phosphoric acid. The method cancels the pretreatment technique required by hot-process phosphoric acid, saves the investment and simplifies the operation. The method comprises the following steps: (1) adding a preset amount of mother solution into a neutralizing tank, and adding metered purified wet-process phosphoric acid with the purity of 85% until the mass concentration of phosphoric acid in the mixed solution is 35-45%; (2) starting a stirring device, adding liquid ammonia for neutralization by multipoint ammonification, continuously adding the liquid ammonia for 80-100 minutes while controlling the liquid ammonia addition speed, and stopping neutralization when the pH value reaches 4.2-4.6; (3) sending the qualified product into a cooling crystallization stage; and (4) after finishing crystallization, dehydrating and drying the slurry to obtain crystalline monoammonium phosphate, and sending the mother solution to a mother solution storage tank for cyclic use.
Description
Technical field
The present invention relates to the preparation field of monoammonium phosphate, in particular to a kind of method and the whipping appts that utilize Wet Phosphoric Acid Market production crystal phosphoric acid one ammonium.
Background technology
Monoammonium phosphate Ammonium dihydrogenphosphate; Ammoniumphosphate, monobasic, molecular formula: NH
4h
2pO
4molecular 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, be slightly soluble in alcohol, be 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 (AP
2o
5) be about 5.44:1 with the ratio of total nitrogen (TN) content, be one of principal item of high-concentration phosphate compound fertilizers.This product generally topdresses, and is also to 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; Be 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; Be 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 be divided into thermal phosphoric acid and phosphoric acid by wet process, take yellow phosphorus as raw material, and through oxidation, the phosphoric acid that aquation etc. are reacted and produced is called thermal phosphoric acid.According to the P at different temperature
2o
5different 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 the method for the phosphoric acid obtained with sulfuric acid decomposition phosphorus ore is method the most basic in Wet-process Phosphoric Acid Production.Due to economic benefit, for the phosphoric acid of processed fertilizer ammonium phosphate, large 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) successively---NH
4h
2pO
4, diammonium phosphate (DAP)---(NH
4)
2hPO
4, triammonium phosphate---(NH
4)
3pO
4.Reactional equation is as follows:
H
3PO
4(l)+NH
3(g)＝＝NH4H
2PO
4(s)△H298＝—126kJ
H
3PO
4(l)+2NH
3(g)＝＝(NH4)
2HPO
4(s)△H298＝—203kJ
H
3PO
4(l)+3NH
3(g)＝＝(NH4)
3PO
4(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 decomposes releasing ammonia, becomes tetra-sodium even metaphosphoric acid; Diammonium phosphate is more stable, and crystal habit is oblique system, starts to decompose to release ammonia when temperature reaches 90 DEG C, 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 unlike, 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, easily formed residual in the product, finally can cause environmental pollution.And need through pre-treatment in the process of phosphorous acid production by BEP crystal phosphoric acid one ammonium, to remove excessive arsenic 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 removes by filtering, to reach the object of dearsenification and removing heavy-metal by pretreated technique.And flow process is complicated, cost is high.Meanwhile, in the process of phosphorous acid production by BEP monoammonium phosphate, power consumption is high, mixed effect is poor, crystallization time is long, effect is undesirable.
And the cost of Wet-process Phosphoric Acid Production crystal phosphoric acid one ammonium is lower, but its product purity is high not as the purity 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
The object of the present invention is to provide a kind of method utilizing brand-new Wet Phosphoric Acid Market to produce crystal phosphoric acid one ammonium, eliminate pretreatment technology required in thermal phosphoric acid, and save investment, simplify operation.
The second object of the present invention is to provide a kind of described Wet Phosphoric Acid Market that utilizes to produce the whipping appts used in the method for crystal phosphoric acid one ammonium.Because the whipping appts used in prior art stirs for bilayer, and the paddle blade structure of two-layer stirring is identical, its mixing effect is bad, power consumption is high, mixed effect is poor.The present invention has carried out the improvement more rationalized to original whipping appts, 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, little to the destruction of crystallization, product advantages of good crystallization.
In order to realize above-mentioned purpose of the present invention, spy by the following technical solutions:
Utilize Wet Phosphoric Acid Market to produce a method for crystal phosphoric acid one ammonium, comprise the following steps:
(1) add the mother liquor of predetermined amount in neutralizing well after, 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) start whipping appts, add liquefied ammonia neutralization by multiple spot ammonification, control adds the speed of liquefied ammonia, continues to add when within 80-100 minute, the pH value to solution reaches 4.2 ~ 4.6 to stop neutralization;
(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 tank recycle.
In prior art, it is single-point ammonification, its mass transfer effect is poor, and a kind of method utilizing brand-new Wet Phosphoric Acid Market to produce crystal phosphoric acid one ammonium provided by the invention, wherein add liquefied ammonia neutralization by multiple spot ammonification, use multiple pipe that adds to carry out ammonification when specifically adding liquefied ammonia, such mass transfer effect is good, and reaction efficiency is high.
To 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 dropping to 68-72 DEG C, open reacting kettle jacketing water coolant and carry out pressure cooling; Until when temperature is down to normal temperature, control cooling time as 80-100 minute.
The present invention also provides a kind of Wet Phosphoric Acid Market that utilizes to produce the whipping appts used in the method for crystal phosphoric acid one ammonium, comprises stir storehouse and stirring rake; Described stirring rake is included in from the stationary shaft running through setting under upper in described stir storehouse, and is located at the agitating vane on described stationary shaft;
Described stirring rake is provided with the first agitating vane and the second 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, its other end horizontal-extending; The blade of described second agitating vane is arc, and its one end is fixedly connected with central shaft, its other end horizontal-extending.
Because the whipping appts used in prior art stirs for bilayer, and the paddle blade structure of two-layer stirring is identical, so such slurries are in the process of flowing rotation, the stirring extent of its levels is identical, be arranged on the whirlpool rotated to equidirectional that formation one in stir storehouse is large, fundamentally slurries can not be stirred fully, its mixing effect is bad and because the stirring like this of short period of time can not reach the mixing effect of expection, so the long power consumption of churning time is high and mixed effect is poor.
The present invention has carried out the improvement more rationalized to original whipping appts, the structure arranging the first agitating vane and the second agitating vane is completely different, first agitating vane is the wider agitating vanes of three of level completely, slurries in it fully thoroughly stir at the middle part of stir storehouse by it, and the second agitating vane be located at bottom stir storehouse is set to the blade of arc, like this, when the slurries on upper strata fall bottom, the drive of the second agitating vane, its rotary motion trace changes completely, the slurries of lower floor can be stirred by 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 the 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, little to the destruction of crystallization, product advantages of good crystallization.
Further, described first agitating vane and described second agitating vane are turbine type blade, and described first agitating vane is located at the top of described second agitating vane, and described second 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; Described in the width of the blade of described second agitating vane of arc, direction is parallel with the bearing of trend of described central shaft.
In order to can well by the slurry agitation of lower floor, can arranging first, to mix the direction, width place of the blade of blade vertical with the bearing of trend of stationary shaft, and namely 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 second agitating vane is parallel with the bearing of trend of stationary shaft, namely 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 second agitating vane.
Little in order to reduce the destruction of crystallization, the width of blade that can arrange the second agitating vane is less, can prevent from well like this destroying the xln formed, and avoids making it regrow as larger xln, affects the homogeneity of final xln.
Further, the width of the blade on described second 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 second 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 second agitating vane is minimum is 2.
Preferably, the blade quantity that can arrange on the first agitating vane is 3, and the blade quantity on the second agitating vane is 2.
Compared with prior art, beneficial effect of the present invention is:
(1) eliminate phosphoric acid pretreatment technology, save investment, simplify operation;
(2) single-point ammonification becomes multiple spot ammonification, and mass transfer effect is good.
(3) change 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 second 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, little to the destruction of crystallization, 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, be 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 Phosphoric Acid Market to produce crystal phosphoric acid one ammonium provided by the invention;
The structural representation of whipping appts of Fig. 2 for providing 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 second agitating vane in whipping appts provided by the invention;
1. the first agitating vane, 2. the second agitating vane, 3. stationary shaft.
Embodiment
Below in conjunction with embodiment, embodiment of the present invention are described in detail, but it will be understood to those of skill in the art that the following example only for illustration of the present invention, and should not be considered as limiting the scope of the invention.Unreceipted actual conditions person in embodiment, the condition of conveniently conditioned disjunction manufacturers suggestion is carried 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 Phosphoric Acid Market to produce crystal phosphoric acid one ammonium, comprises the following steps:
(1) add the mother liquor of predetermined amount in neutralizing well after, 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%;
Preferably, in described mixed solution, the mass concentration of phosphoric acid is 38-40%.
(2) start whipping appts, add liquefied ammonia neutralization by multiple spot ammonification, control adds the speed of liquefied ammonia, continues to add when within 80-100 minute, the pH value to solution reaches 4.2 ~ 4.6 to stop neutralization;
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 dropping to 68-72 DEG C, open reacting kettle jacketing water coolant and carry out pressure cooling; Until when temperature is down to normal temperature, control cooling time as 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 tank recycle.
In prior art, it is single-point ammonification, its mass transfer effect is poor, and a kind of method utilizing brand-new Wet Phosphoric Acid Market to produce crystal phosphoric acid one ammonium provided by the invention, wherein add liquefied ammonia neutralization by multiple spot ammonification, use multiple pipe that adds to carry out ammonification when specifically adding liquefied ammonia, such mass transfer effect is good, and reaction efficiency is high.
To 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 a kind of Wet Phosphoric Acid Market that utilizes to produce the whipping appts used in the method for crystal phosphoric acid one ammonium, comprises stir storehouse and stirring rake; Described stirring rake is included in from the stationary shaft 3 running through setting under upper in described stir storehouse, and is located at the agitating vane on described stationary shaft 3;
Described stirring rake is provided with the first agitating vane 1 and the second 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, its other end horizontal-extending; The blade of described second agitating vane 2 is arc, and its one end is fixedly connected with central shaft, its other end horizontal-extending.
Because the whipping appts used in prior art stirs for bilayer, and the paddle blade structure of two-layer stirring is identical, so such slurries are in the process of flowing rotation, the stirring extent of its levels is identical, be arranged on the whirlpool rotated to equidirectional that formation one in stir storehouse is large, fundamentally slurries can not be stirred fully, its mixing effect is bad and because the stirring like this of short period of time can not reach the mixing effect of expection, so the long power consumption of churning time is high and mixed effect is poor.
The present invention has carried out the improvement more rationalized to original whipping appts, the structure arranging the first agitating vane 1 and the second agitating vane 2 is completely different, first agitating vane 1 is the wider agitating vanes of three of level completely, slurries in it fully thoroughly stir at the middle part of stir storehouse by it, and the second agitating vane 2 be located at bottom stir storehouse is set to the blade of arc, like this, when the slurries on upper strata fall bottom, the drive of the second agitating vane 2, its rotary motion trace changes completely, the slurries of lower floor can be stirred by 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 the 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, little to the destruction of crystallization, product advantages of good crystallization.
Preferably, described first agitating vane 1 and described second agitating vane 2 are turbine type blade, and described first agitating vane 1 is located at the top of described second agitating vane 2, and described second 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; Described in the width of the blade of described second agitating vane 2 of arc, direction is parallel with the bearing of trend of described central shaft.
In order to can well by the slurry agitation of lower floor, can arranging first, to mix the direction, width place of the blade of blade vertical with the bearing of trend of stationary shaft 3, and namely 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 second agitating vane 2 is parallel with the bearing of trend of stationary shaft 3, namely 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 second agitating vane 2.
Little in order to reduce the destruction of crystallization, the width of blade that can arrange the second agitating vane 2 is less, can prevent from well like this destroying the xln formed, and avoids making it regrow as larger xln, affects the homogeneity of final xln.
Preferably, the width of the blade on described second 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 second 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 second agitating vane 2 is minimum is 2.
Preferably, the blade quantity that can arrange on the first agitating vane 1 is 3, and the blade quantity on the second agitating vane 2 is 2.
Embodiment 1
Utilize Wet Phosphoric Acid Market to produce a method for crystal phosphoric acid one ammonium, comprise the following steps:
(1) add the mother liquor of predetermined amount in neutralizing well after, 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) start whipping appts, add liquefied ammonia neutralization by multiple spot ammonification, control adds the speed of liquefied ammonia, continues to add when within 80-100 minute, the pH value to solution reaches 4.2 ~ 4.6 to stop neutralization;
(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 tank recycle.
Embodiment 2
Utilize Wet Phosphoric Acid Market to produce a method for crystal phosphoric acid one ammonium, comprise the following steps:
(1) add the mother liquor of predetermined amount in neutralizing well after, 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 40%;
(2) start whipping appts, add liquefied ammonia neutralization by multiple spot ammonification, control adds the speed of liquefied ammonia, continues to add when within 90 minutes, the pH value to solution reaches 4.3 to stop neutralization;
(3), after qualified after testing, the crystallisation by cooling stage is entered; When beginning to cool down, adopt naturally cooling; When starching temperature and dropping to 70 DEG C, open reacting kettle jacketing water coolant and carry out pressure cooling; Until when temperature is down to normal temperature, cooling time, control was 90 minutes.
(4) after crystallization completes, slurry dewatering, drying are obtained monoammonium phosphate crystal, and the mother liquor deviate from is delivered to mother liquor storage tank recycle.
Embodiment 3
Utilize Wet Phosphoric Acid Market to produce the whipping appts used in the method for crystal phosphoric acid one ammonium, it is characterized in that, comprise stir storehouse and stirring rake; Described stirring rake is included in from the stationary shaft 3 running through setting under upper in described stir storehouse, and is located at the agitating vane on described stationary shaft 3;
Described stirring rake is provided with the first agitating vane 1 and the second 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, its other end horizontal-extending; The blade of described second agitating vane 2 is arc, and its one end is fixedly connected with central shaft, its other end horizontal-extending.
Embodiment 4
Utilize Wet Phosphoric Acid Market to produce the whipping appts used in the method for crystal phosphoric acid one ammonium, it is characterized in that, comprise stir storehouse and stirring rake; Described stirring rake is included in from the stationary shaft 3 running through setting under upper in described stir storehouse, and is located at the agitating vane on described stationary shaft 3;
Described stirring rake is provided with the first agitating vane 1 and the second 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, its other end horizontal-extending; The blade of described second agitating vane 2 is arc, and its one end is fixedly connected with central shaft, its other end horizontal-extending;
Described first agitating vane 1 is located at the top of described second agitating vane 2, and described second agitating vane 2 is located at the bottom of described stir storehouse;
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; Described in the width of the blade of described second agitating vane 2 of arc, direction 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 second agitating vane 2, and described first agitating vane 1 comprises 3 blades, and described second agitating vane 2 comprises 2 blades.
Experimental example 1
The appearance requirement of industrial grade monoammonium phosphate to product is colourless or white crystal or powder, does not make specified in more detail to grain size number.
But user often wishes that crystalline particle is too thinless in sales process, and with wanting evenly.Meanwhile, in process of production, crystalline particle is meticulous, when drying, easily produces airborne dust, and the product loss caused during dried tail gas discharge is also larger, and the yield 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 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% | Be less than 10% |
Can be clear that according to upper table, its size-grade distribution of monoammonium phosphate crystal of being 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 too small crystal grain more than 120 orders or below 60 orders is less.
Although illustrate and describe the present invention with specific embodiment, however it will be appreciated that can to make when not deviating from the spirit and scope of the present invention many other change and amendment.Therefore, this means to comprise all such changes and modifications belonged in the scope of the invention in the following claims.
Claims (10)
1. utilize Wet Phosphoric Acid Market to produce a method for crystal phosphoric acid one ammonium, it is characterized in that, comprise the following steps:
(1) add the mother liquor of predetermined amount in neutralizing well after, 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) start whipping appts, add liquefied ammonia neutralization by multiple spot ammonification, control adds the speed of liquefied ammonia, continues to add when within 80-100 minute, the pH value to solution reaches 4.2 ~ 4.6 to stop neutralization;
(3), after qualified after testing, the crystallisation by cooling stage is entered;
(4) after crystallization completes, slurry dewatering, drying are obtained monoammonium phosphate crystal, and the mother liquor deviate from is delivered to mother liquor storage tank recycle.
2. the method utilizing Wet Phosphoric Acid Market to produce crystal phosphoric acid one ammonium according to claim 1, is characterized in that,
In step (1), in described mixed solution, the mass concentration of phosphoric acid is 38-40%.
3. the method utilizing Wet Phosphoric Acid Market to produce crystal phosphoric acid one ammonium according to claim 1, is characterized 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 method utilizing Wet Phosphoric Acid Market to produce crystal phosphoric acid one ammonium according to claim 1, is characterized in that,
In step (3), when beginning to cool down, adopt naturally cooling; When starching temperature and dropping to 68-72 DEG C, open reacting kettle jacketing water coolant and carry out pressure cooling; Until when temperature is down to normal temperature, control cooling time as 80-100 minute.
5. the Wet Phosphoric Acid Market that utilizes according to any one of claim 1-4 produces the whipping appts used in the method for crystal phosphoric acid one ammonium, it is characterized in that, comprises stir storehouse and stirring rake; Described stirring rake is included in from the stationary shaft running through setting under upper in described stir storehouse, and is located at the agitating vane on described stationary shaft;
Described stirring rake is provided with the first agitating vane and the second 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, its other end horizontal-extending; The blade of described second agitating vane is arc, and its one end is fixedly connected with central shaft, its other end horizontal-extending.
6. the Wet Phosphoric Acid Market that utilizes according to claim 5 produces the whipping appts used in the method for crystal phosphoric acid one ammonium, it is characterized in that, described first agitating vane is located at the top of described second agitating vane, and described second agitating vane is located at the bottom of described stir storehouse.
7. the Wet Phosphoric Acid Market that utilizes according to claim 5 produces the whipping appts used in the method for crystal phosphoric acid one ammonium, it is characterized 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; Described in the width of the blade of described second agitating vane of arc, direction is parallel with the bearing of trend of described central shaft.
8. the Wet Phosphoric Acid Market that utilizes according to claim 5 produces the whipping appts used in the method for crystal phosphoric acid one ammonium, and it is characterized in that, the width of blade of described first agitating vane is greater than the width of blade of described second agitating vane.
9. the Wet Phosphoric Acid Market that utilizes according to claim 8 produces the whipping appts used in the method for crystal phosphoric acid one ammonium, it is characterized in that,
The width of the blade on described second agitating vane is the 1/4-1/5 of the width of the blade on described first agitating vane.
10. the Wet Phosphoric Acid Market that utilizes according to claim 5 produces the whipping appts used in the method for crystal phosphoric acid one ammonium, it is characterized in that, the blade on described first agitating vane and described second 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 second agitating vane is minimum is 2.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510051664.5A CN104528675B (en) | 2015-01-30 | 2015-01-30 | Utilize method and the whipping appts of wet purification phosphoric acid production crystal phosphoric acid one ammonium |
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|---|---|---|---|
| CN201510051664.5A CN104528675B (en) | 2015-01-30 | 2015-01-30 | Utilize method and the whipping appts of wet purification phosphoric acid production crystal phosphoric acid one ammonium |
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| Publication Number | Publication Date |
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| CN104528675A true CN104528675A (en) | 2015-04-22 |
| CN104528675B CN104528675B (en) | 2016-06-01 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108002392A (en) * | 2017-11-20 | 2018-05-08 | 湖北六国化工股份有限公司 | The method that ammonium fluosilicate co-producing white carbon black is prepared using phosphoric acid plant fluorinated tail gas |
| RU2812559C1 (en) * | 2023-06-10 | 2024-01-30 | Общество с ограниченной ответственностью "Алмаз Тех" (ООО "Алмаз Тех") | Method of producing monoammonium phosphate |
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| 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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| 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 |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108002392A (en) * | 2017-11-20 | 2018-05-08 | 湖北六国化工股份有限公司 | The method that ammonium fluosilicate co-producing white carbon black is prepared using phosphoric acid plant fluorinated tail gas |
| CN108002392B (en) * | 2017-11-20 | 2019-11-19 | 湖北六国化工股份有限公司 | The method for preparing ammonium fluosilicate co-producing white carbon black using phosphoric acid plant fluorinated tail gas |
| RU2812559C1 (en) * | 2023-06-10 | 2024-01-30 | Общество с ограниченной ответственностью "Алмаз Тех" (ООО "Алмаз Тех") | Method of producing monoammonium phosphate |
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