CN101234755A - Method for producing monoammonium phosphate by metathesis method - Google Patents

Method for producing monoammonium phosphate by metathesis method Download PDF

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CN101234755A
CN101234755A CNA2008100448135A CN200810044813A CN101234755A CN 101234755 A CN101234755 A CN 101234755A CN A2008100448135 A CNA2008100448135 A CN A2008100448135A CN 200810044813 A CN200810044813 A CN 200810044813A CN 101234755 A CN101234755 A CN 101234755A
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reaction
monoammonium phosphate
phosphate
raw material
operating mode
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张志强
周成明
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SICHUAN JIANWEI MINGFENG CHEMICAL CO Ltd
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SICHUAN JIANWEI MINGFENG CHEMICAL CO Ltd
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Abstract

The invention provides a method for manufacturing ammonium diacid phosphate by double decomposition, which follows the steps of material preparation by computation, calcium superphosphate preparation, double decomposition reaction, PH value vernier regulation and drying and grinding in sequence. The invention is remarkably characterized by that calcium superphosphate is prepared by firstly using rock phosphate and sulfuric acid and then carried out the double decomposition reaction with ammonium sulfate to manufacture ammonium diacid phosphate products, which avoids the defect in traditional 'neutralization method' that large quantity of metal ion such as iron, aluminum and magnesium are precipitated as the form of hydrogen phosphate of water insoluble and large quantity of phosphorus element are drained away; the thickness of hydrogen ion in original state of reaction liquid and the water solubility of dihydric phosphate such as iron, aluminum and magnesium are preserved. The method can use low, middle and high grade of phosphorite as material and manufacture ammonium diacid phosphate products with a quality that can realize or higher than the international II class standard; the total yield of phosphorus reaches up to 95 percent; the consumption of sulfuric acid material reduces by 30 percent; the method has a good effect of energy saving and emissions reduction and remarkable economic efficiency.

Description

Method with producing monoammonium phosphate by metathesis method
Technical field:
The present invention relates to produce the technical field of monoammonium phosphate, specifically a kind of method that adopts producing monoammonium phosphate by metathesis method.
Background technology:
Monoammonium phosphate has another name called and is that primary ammonium phosphate, its chemical formula are NH 4H 2PO 4, it is a kind ofly to continue to use in agriculture production for a long time, produce the phosphorus-ammonium compound fertilizer material that good harvest has vital role to ensureing farm crop.Except that being used as chemical fertilizer, it also can be used as fire extinguishing fire retardant and chemistry interpolation auxiliary agent as a kind of important phosphoric acid salt Chemicals, has been widely used in numerous production technical field such as agriculture production, food mfg and chemical and medicine industry.Up to now, in phosphate chemical industry, always be for a long time and adopt fertilizer phosphoric acid and NH 3Carry out the Technology of neutralization reaction and produce monoammonium phosphate product.For example: the disclosed name of Chinese patent CN1063157C is called " production method of industrial monoammonium phosphate and industrial monoammonium phosphate and calcium hydrogen phosphate fodder ", the disclosed name of CN1235794C is called " co-production method of diammonium phosphate and monoammonium phosphate and washings neutralizing device " and the disclosed name of CN1792778A is called patent documentations such as " utilizing the titanium dioxide spent acid to produce the method for high-purity phosphoric acid one ammonium ", and above-mentioned patent documentation is disclosed all to be to adopt " neutralisation " to manufacture the technology of monoammonium phosphate.Need not to dare not or would not speak up, the traditional technology that existing " neutralisation " continued to use produced the fertilizer monoammonium phosphate exists following technical bug:
(1) at fertilizer phosphoric acid and NH 3Carry out in the process of neutralization reaction, particularly reaction solution is when pH1.5 proceeds to the stage of pH4.5, being present in a large amount of metal ions such as iron in the fertilizer phosphoric acid, aluminium, magnesium can separate out and a large amount of phosphoric that runs off with the form of water-insoluble hydrophosphate, will have a strong impact on the total phosphorus yield.Add up according to investigations: the total phosphorus yield that existing " neutralisation " produces monoammonium phosphate generally only is about 80%.
(2) the existing producer that adopts " neutralisation " to manufacture monoammonium phosphate makes product can reach the technical indicator of " water-soluble phosphorus accounts for available phosphorus 〉=75% " of GB II class defined, can only select the higher-grade phosphorus ore for use is raw materials for production, and this is to run counter to the fundamental state policy of comprehensive utilization of resources Sustainable development.
(3) adopt 1 ton of monoammonium phosphate product of the every production of " neutralisation " technology need consume 1.3 tons of sulfuric acid raw materials, because sulphur market value continuous rise causes vitriolic production cost per ton up to 1600 yuan recently, directly causes the production cost of monoammonium phosphate sharply to rise.
How could scientifically fully utilize mid low grade phosphate rock and (refer to contain P 2O 5Be 25 ∽ 20%) produce the monoammonium phosphate that reaches or be higher than GB II class standard, be the key subjects of pendulum in face of vast phosphorous chemical industry researcher always, this problem also to be solved by this invention just.
Summary of the invention:
The objective of the invention is to propose that a kind of can generally to be suitable for basic, normal, high grade phosphorus mine be raw material, adopt double decomposition production can reach or be higher than the method for the monoammonium phosphate product of GB II class quality standard, distinguishing feature of the present invention is: it has thoroughly given up traditional " neutralisation ", look for another way, propose that a kind of [major ingredient is Ca with ground phosphate rock 5F (PO 4) 3] and the calcium superphosphate that makes of sulfuric acid reaction carry out the new technology that replacement(metathesis)reaction is produced monoammonium phosphate product with ammonium sulfate again.The present invention is achieved by the following technical solution:
Its step is in the following order carried out:
(1) metering is got the raw materials ready: take by weighing raw material by following weight part:
1 part in ground phosphate rock,
Contain H 2SO 40.5 part of 95% sulfuric acid 0.3 ∽,
Contain (NH 4) 2SO 40.35 part of 99% ammonium sulfate 0.22 ∽,
(2) preparation calcium superphosphate:
Take the ground phosphate rock raw material of 40 ∽ 60% by weight and put into reaction tank, by 3 ∽ 4 of used ground phosphate rock raw material weight water extraordinarily, under the operating mode that dilution is stirred, add sulfuric acid gradually, feed steam heating, control reaction temperature is 85 ℃ of 75 ∽, reaction 6 ∽ 8 hours under the operating mode that stirs
Ca 5F(PO 4) 3+5H 2SO 4-3H 3PO 4+5CaSO 4↓+HF
Filter, filter residue discharges waste after rinsing, and filtrate is imported in the reaction tank, again the ground phosphate rock raw material of surplus is put into reaction tank under the stirring operating mode, and feeding steam heating, control reaction temperature are 85 ℃ of 75 ∽, and reaction 6 ∽ 8 hours under the operating mode that stirs,
Ca 5F(PO 4) 3+7H 3PO 4-5Ca(H 2PO 4) 2+HF
Filter once more, collect clear filtrate, promptly make calcium superphosphate solution, filter residue foldback metering material preparation step is augmented the raw material reuse,
(3) replacement(metathesis)reaction: the calcium superphosphate solution that makes is sent in the reaction tank, under the stirring operating mode, added ammonium sulfate, feed to be steam heated to boil and carries out replacement(metathesis)reaction, make monoammonium phosphate solution,
Ca(H 2PO 4) 2+(NH 4) 2SO 4-2NH 4H 2PO 4+CaSO 4↓
Filter, filter residue discharges after rinsing, and washing lotion is stand-by,
(4) little adjust pH: add small amount of N H gradually 4OH, the pH value of regulating control monoammonium phosphate solution is 4 ∽ 5, elimination precipitates the residue impurity of separating out again, makes qualified monoammonium phosphate liquid,
(5) oven dry is pulverized: the qualified monoammonium phosphate liquid that will make technology is routinely pulverized through oven dry, can make the monoammonium phosphate product that quality reaches or be higher than GB II class standard.
Substantive distinguishing features of the present invention and marked improvement are: its traditional technology that " neutralisation " used for a long time produces monoammonium phosphate of thoroughly having sublated, look for another way, propose originally a kind ofly to prepare calcium superphosphate with ground phosphate rock and sulfuric acid and carry out the new technology that replacement(metathesis)reaction is produced monoammonium phosphate product with ammonium sulfate again.Avoided traditional " neutralisation " in the neutralization reaction process, to have a large amount of iron, aluminium, metal ions such as magnesium are separated out and the mortality defective of a large amount of phosphoric that run off with water-insoluble hydrophosphate form, can keep reaction solution original state hydrogen ion concentration and also just keep iron in the reaction solution, aluminium, dihydrogen phosphates such as magnesium water-soluble, can ensure well that the water-soluble phosphorus in the quality product is up to standard, and grade and foreign matter content to the phosphorus ore raw material all do not have harsh requirement, the total phosphorus yield is increased to more than 95% by 80%, the quantity that monoammonium phosphate product per ton consumes the sulfuric acid raw material reduces about 0.5 ton, and total cost of production can reduce more than 1000 yuan.
The method with producing monoammonium phosphate by metathesis method that the present invention proposes is compared with existing " neutralisation " has following advantage:
1. technical process of the present invention is simple and direct, need not the newly added equipment investment, continues to use existing common process equipment, and the phosphorus ore that can generally be suitable for basic, normal, high grade is a raw material, all can produce the monoammonium phosphate product that quality reaches or be higher than GB II class standard;
2. total phosphorus yield of the present invention can improve resource utilization greatly up to more than 95%, and effects of energy saving and emission reduction is remarkable, has splendid social effect;
3. the 1 ton of monoammonium phosphate product of the every production of double decomposition that adopts the present invention to propose consumes the sulfuric acid material quantity and can be reduced to 0.8 ton by " neutralisation " 1.3 tons, and product per ton can reduce production costs more than 1000 yuan, has huge economic benefit.
Safe and reliable to operation, the operation of the present invention produce and manage very convenient, the constant product quality of being produced, it is significant to further development China phosphoric acid salt chemical industry enterprise.
Description of drawings:
Accompanying drawing is technological process of production figure of the present invention.
Embodiment:
Embodiment one:
The method that the present invention proposes with producing monoammonium phosphate by metathesis method, it successively in the following order step carry out:
(1) metering is got the raw materials ready: take by weighing raw material by following weight part:
Contain P 2O 51 part in 30% ground phosphate rock,
Contain H 2SO 40.5 part in 95% sulfuric acid,
Contain (NH 4) 2SO 40.35 part in 99% ammonium sulfate.
(2) preparation calcium superphosphate:
Take 60% ground phosphate rock raw material at first by weight and put into the reaction tank that is fitted with agitator and steam heater, 4 water extraordinarily by used ground phosphate rock raw material weight, under the operating mode that dilution is stirred, add sulfuric acid gradually, feeding steam heating, control reaction temperature are 80 ℃, under the operating mode that evenly stirs continuously, carried out following chemical reaction 7 hours:
Ca 5F(PO 4) 3+5H 2SO 4-3H 3PO 4+5CaSO 4↓+HF
Filter, filter residue discharges waste after rinsing, collect clear filtrate, the filtrate input is fitted with in the reaction tank of agitator and steam heater, under the stirring operating mode, again the ground phosphate rock raw material of surplus 40% is put into reaction tank, feeding steam heating, control reaction temperature are 80 ℃, under the operating mode that evenly stirs continuously, carry out following reaction 7 hours:
Ca 5F(PO 4) 3+7H 3PO 4-5Ca(H 2PO 4) 2+HF
Filter, collect clear filtrate, promptly make calcium superphosphate solution.
Collect above-mentioned filter residue, foldback metering material preparation step is augmented the raw material reuse.
(3) replacement(metathesis)reaction: the calcium superphosphate solution that makes is sent in the reaction tank that is fitted with agitator and steam heater, under the stirring operating mode, progressively added ammonium sulfate, feed to be steam heated to boil and carries out following replacement(metathesis)reaction:
Ca(H 2PO 4) 2+(NH 4) 2SO 4-2NH 4H 2PO 4+CaSO 4↓
Treat to filter after replacement(metathesis)reaction finishes, filter residue is cleaned the back discharging, make monoammonium phosphate solution.
(4) little adjust pH: add small amount of N H gradually 4OH, the pH value of regulating control monoammonium phosphate solution is 4.5, the residue impurity that the elimination precipitation is separated out promptly makes qualified monoammonium phosphate liquid.
(5) oven dry is pulverized: the qualified monoammonium phosphate liquid that will make technology is routinely pulverized through oven dry, can make the monoammonium phosphate product that quality reaches or be higher than GB II class standard.
Embodiment two:
The present invention propose the method with producing monoammonium phosphate by metathesis method, its step is in the following order carried out:
(1) metering is got the raw materials ready: take by weighing raw material by following weight part:
Contain P 2O 51 part in 25% ground phosphate rock,
Contain H 2SO 40.4 part in 95% sulfuric acid,
Contain (NH 4) 2SO 40.3 part in 99% ammonium sulfate.
(2) preparation calcium superphosphate:
Take 50% ground phosphate rock raw material at first by weight and put into the reaction tank that is fitted with agitator and steam heater, 3.5 water extraordinarily by used ground phosphate rock raw material weight, under the operating mode that dilution is stirred, add sulfuric acid gradually, feeding steam heating, control reaction temperature are 75 ℃, under the operating mode that evenly stirs continuously, carried out following chemical reaction 8 hours:
Ca 5F(PO 4) 3+5H 2SO 4-3H 3PO 4+5CaSO 4↓+HF
Filter, filter residue discharges waste after rinsing, collect clear filtrate, the filtrate input is fitted with in the reaction tank of agitator and steam heater, under the stirring operating mode, again the ground phosphate rock raw material of surplus 50% is put into reaction tank, feeding steam heating, control reaction temperature are 75 ℃, under the operating mode that evenly stirs continuously, carry out following reaction 8 hours:
Ca 5F(PO 4) 3+7H 3PO 4-5Ca(H 2PO 4) 2+HF
Filter, collect clear filtrate, promptly make calcium superphosphate solution.
Collect above-mentioned filter residue, foldback metering material preparation step is augmented the raw material reuse.
(3) replacement(metathesis)reaction: the calcium superphosphate solution that makes is sent in the reaction tank that is fitted with agitator and steam heater, under the stirring operating mode, progressively added ammonium sulfate, feed to be steam heated to boil and carries out following replacement(metathesis)reaction:
Ca(H 2PO 4) 2+(NH 4) 2SO 4-2NH 4H 2PO 4+CaSO 4↓
Treat to filter after replacement(metathesis)reaction finishes, filter residue is cleaned the back discharging, make monoammonium phosphate solution.
(4) little adjust pH: add small amount of N H gradually 4OH, the pH value of regulating control monoammonium phosphate solution is 5, elimination precipitates the residue impurity of separating out again, promptly makes qualified monoammonium phosphate liquid.
(5) oven dry is pulverized: the qualified monoammonium phosphate liquid that will make technology is routinely pulverized through oven dry, can make the monoammonium phosphate product that quality reaches or be higher than GB II class standard.
Embodiment three:
Its step is in the following order carried out:
(1) metering is got the raw materials ready: take by weighing raw material by following weight part:
Contain P 2O 51 part in 20% ground phosphate rock,
Contain H 2SO 40.3 part in 95% sulfuric acid,
Contain (NH 4) 2SO 40.22 part in 99% ammonium sulfate.
(2) preparation calcium superphosphate:
Take 55% ground phosphate rock raw material at first by weight and put into the reaction tank that is fitted with agitator and steam heater, 3 water extraordinarily by used ground phosphate rock raw material weight, under the operating mode that dilution is stirred, add sulfuric acid gradually, feeding steam heating, control reaction temperature are 85 ℃, under the operating mode that evenly stirs continuously, carried out following chemical reaction 6 hours:
Ca 5F(PO 4) 3+5H 2SO 4-3H 3PO 4+5CaSO 4↓+HF
Filter, filter residue discharges waste after rinsing, collect clear filtrate, the filtrate input is fitted with in the reaction tank of agitator and steam heater, under the stirring operating mode, again the ground phosphate rock raw material of surplus 45% is put into reaction tank, feeding steam heating, control reaction temperature are 85 ℃, under the operating mode that evenly stirs continuously, carry out following reaction 6 hours:
Ca 5F(PO 4) 3+7H 3PO 4-5Ca(H 2PO 4) 2+HF
Filter, collect clear filtrate, promptly make calcium superphosphate solution.
Collect above-mentioned filter residue, foldback metering material preparation step is augmented the raw material reuse.
(3) replacement(metathesis)reaction: the calcium superphosphate solution that makes is sent in the reaction tank that is fitted with agitator and steam heater, under the stirring operating mode, progressively added ammonium sulfate, feed to be steam heated to boil and carries out following replacement(metathesis)reaction:
Ca(H 2PO 4) 2+(NH 4) 2SO 4-2NH 4H 2PO 4+CaSO 4↓
Treat to filter after replacement(metathesis)reaction finishes, filter residue is cleaned the back discharging, make monoammonium phosphate solution.
(4) little adjust pH: add small amount of N H gradually 4OH, the pH value of regulating control monoammonium phosphate solution is 4, the residue impurity that the elimination precipitation is separated out promptly makes qualified monoammonium phosphate liquid.
(5) oven dry is pulverized: the monoammonium phosphate liquid technology process oven dry pulverizing routinely with making can make the monoammonium phosphate product that quality reaches or be higher than GB II class standard.

Claims (2)

1. method with producing monoammonium phosphate by metathesis method, it successively in the following order step carry out:
(1) metering is got the raw materials ready: take by weighing raw material by following weight part:
1 part in ground phosphate rock,
Contain H 2SO 40.5 part of 95% sulfuric acid 0.3 ∽,
Contain (NH 4) 2SO 40.35 part of 99% ammonium sulfate 0.22 ∽,
(2) preparation calcium superphosphate:
Take the ground phosphate rock raw material of 40 ∽ 60% by weight and put into reaction tank, by 3 ∽ 4 of used ground phosphate rock raw material weight water extraordinarily, under the operating mode that dilution is stirred, add sulfuric acid gradually, feed steam heating, control reaction temperature is 85 ℃ of 75 ∽, reaction 6 ∽ 8 hours under the operating mode that stirs, filter, filtrate is imported in the reaction tank, under the stirring operating mode, again the ground phosphate rock raw material of surplus is put into reaction tank, feed steam heating, control reaction temperature is 85 ℃ of 75 ∽, and reaction 6 ∽ 8 hours under the operating mode that stirs, filter once more, collect clear filtrate, promptly make calcium superphosphate solution
(3) replacement(metathesis)reaction: the calcium superphosphate solution that makes is sent in the reaction tank, under the stirring operating mode, added ammonium sulfate, feed to be steam heated to boil and carries out replacement(metathesis)reaction, make monoammonium phosphate solution,
(4) little adjust pH: add small amount of N H gradually 4OH, the pH value of regulating control monoammonium phosphate solution is 4 ∽ 5, promptly makes qualified monoammonium phosphate liquid,
(5) oven dry is pulverized: the qualified monoammonium phosphate liquid that will make technology is routinely pulverized through oven dry, can make the monoammonium phosphate product that quality reaches or be higher than GB II class standard.
2. the method with producing monoammonium phosphate by metathesis method according to claim 1 is characterized in that: in the metering material preparation step, take by weighing raw material by following weight part:
1 part in ground phosphate rock,
Contain H 2SO 40.4 part in 95% sulfuric acid,
Contain (NH 4) 2SO 40.3 part in 99% ammonium sulfate.
CNA2008100448135A 2008-02-25 2008-02-25 Method for producing monoammonium phosphate by metathesis method Pending CN101234755A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104649241A (en) * 2015-01-23 2015-05-27 湖北宜化肥业有限公司 Method for producing monoammonium phosphate by utilizing medium and low grade phosphorus ore
CN106241764A (en) * 2016-08-23 2016-12-21 贵阳开磷化肥有限公司 It is that MAP method prepared by raw material by the sulfur waste liquor of ammonium of anhydrous hydrogen fluoride workshop and the sewage treatment slag in phosphoric acid production workshop
CN106564919A (en) * 2016-11-08 2017-04-19 贵州省化工研究院 Method for directly preparing magnesium ammonium sulfate through phosphorite magnesium removal
CN108087018A (en) * 2017-11-24 2018-05-29 惠水县凡趣创意科技有限公司 A kind of preparation formula of dihydric phosphate Explosion suppressant
CN113086957A (en) * 2021-04-30 2021-07-09 陕西科原环保节能科技有限公司 Method for producing ammonium dihydrogen phosphate

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104649241A (en) * 2015-01-23 2015-05-27 湖北宜化肥业有限公司 Method for producing monoammonium phosphate by utilizing medium and low grade phosphorus ore
CN104649241B (en) * 2015-01-23 2017-01-25 湖北宜化肥业有限公司 Method for producing monoammonium phosphate by utilizing medium and low grade phosphorus ore
CN106241764A (en) * 2016-08-23 2016-12-21 贵阳开磷化肥有限公司 It is that MAP method prepared by raw material by the sulfur waste liquor of ammonium of anhydrous hydrogen fluoride workshop and the sewage treatment slag in phosphoric acid production workshop
CN106564919A (en) * 2016-11-08 2017-04-19 贵州省化工研究院 Method for directly preparing magnesium ammonium sulfate through phosphorite magnesium removal
CN108087018A (en) * 2017-11-24 2018-05-29 惠水县凡趣创意科技有限公司 A kind of preparation formula of dihydric phosphate Explosion suppressant
CN113086957A (en) * 2021-04-30 2021-07-09 陕西科原环保节能科技有限公司 Method for producing ammonium dihydrogen phosphate

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