CN106800285A - The production method of calcium hydrophosphate fodder - Google Patents
The production method of calcium hydrophosphate fodder Download PDFInfo
- Publication number
- CN106800285A CN106800285A CN201710014804.0A CN201710014804A CN106800285A CN 106800285 A CN106800285 A CN 106800285A CN 201710014804 A CN201710014804 A CN 201710014804A CN 106800285 A CN106800285 A CN 106800285A
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- Prior art keywords
- reaction
- calcium
- hydrophosphate fodder
- calcium hydrophosphate
- production method
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/32—Phosphates of magnesium, calcium, strontium, or barium
- C01B25/322—Preparation by neutralisation of orthophosphoric acid
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/28—Ammonium phosphates
Abstract
The present invention relates to a kind of production method of calcium monohydrogen phosphate, a kind of production method of calcium hydrophosphate fodder is specifically disclosed.Comprise the following steps：A, phosphoric acid by wet process and ground phosphate rock and/or phosphate ore pulp carry out extractive reaction, and are incubated curing；B, filtering reaction slurry；C, filtrate and milk of lime carry out neutralization reaction；D, filter slurry, filter cake through pneumatic conveying drying, be crushed into calcium hydrophosphate fodder product.It is an advantage of the invention that：1）The intermediate product calcium dihydrogen phosphate of neutralization reagent milk of lime next life producing feed-stage calcium monohydrogen phosphate is substituted with raw materials for production ground phosphate rock, the consumption of milk of lime is eliminated, the production cost of calcium hydrophosphate fodder is substantially reduced；2）The filter residue produced while generation calcium dihydrogen phosphate can realize the abundant recovery of phosphor resource as the raw material of production high value added product MAP.
Description
Technical field
The present invention relates to a kind of production method of calcium monohydrogen phosphate, especially a kind of calcium monohydrogen phosphate as feed addictive
Production method.
Background technology
Calcium hydrophosphate fodder refers to and meets relevant criterion, can be applied in feed manufacturing as phosphorus, the phosphorus of the replenishers of calcium
Sour hydrogen calcium.Because phosphorus calcium ratio therein and phosphorus calcium in animal skeleton are than closest, and can all be dissolved in animal hydrochloric acid in gastric juice,
Calcium hydrophosphate fodder is one of best feed mineral additive generally acknowledged both at home and abroad at present.Animal growth and development can be accelerated,
Shorten fattening period, quick weightening；The breeding rate and survival rate of livestock and poultry can be improved, while there is the enhancing disease-resistant tolerance to cold of livestock and poultry,
Rickets, dysentery characterized by white mucous stool disease, paralysed disease disease to livestock and poultry have preventive and therapeutic effect.
The production technology of usual calcium hydrophosphate fodder is：Using the phosphorus ore and direct reaction of sulfuric acid that conform to quality requirements,
Phosphoric acid by wet process is obtained, after metering into one section of neutralization chamber, is neutralized with milk of lime, filtering filter residue is used to produce the fertilizer of low value
Calcium monohydrogen phosphate（White fertilizer）, the iron after being neutralized by one section in phosphoric acid, aluminium, the impurity such as sulfate radical is purified；Filtrate enters two sections
Neutralization chamber, with milk of lime continue neutralize, filter liquor return preparing lime milk, filter cake through pneumatic conveying drying, be crushed into product.Its
Exemplary steps can be summarized as follows：
（1）Phosphoric acid by wet process is obtained by phosphorus ore and sulfuric acid reaction；
（2）In one section of neutralization chamber, phosphoric acid by wet process carries out neutralization reaction with milk of lime, obtains reaction slurry；
（3）Filtering reaction slurry obtains one section of filtrate and filter residue；
（4）In two sections of neutralization chambers, one section of filtrate carries out neutralization reaction with milk of lime, obtains slurry；
（5）Filter slurry obtains two sections of filtrates and filter cake, filter cake through pneumatic conveying drying, be crushed into calcium hydrophosphate fodder product.
The main chemical reactions being directed to are as follows：
H3PO4 + Ca(OH)2→ Ca(H2PO4)2+ H2O
Ca(H2PO4)2+ Ca(OH)2 →CaHPO4+ H2O
One section of filtrate main component in above-mentioned calcium monohydrogen phosphate production process is calcium dihydrogen phosphate, and its cardinal principle for being formed is：
Phosphoric acid is neutralized by toward addition milk of lime in one section of reactive tank so that the pH reductions of system, and then makes the iron in system,
Aluminium impurity is precipitated out in the form of calcium phosphate precipitation, while milk of lime and phosphatase reaction generation calcium dihydrogen phosphate filtrate（One section
Filtrate）, the appearance of substantial amounts of soluble calcium salt causes the impurity anions such as sulfate radical in phosphoric acid by wet process with the shape of calcium precipitation
Formula leaves system.
The main chemical reactions being related to are as follows：
H3PO4 + Ca(OH)2→ Ca(H2PO4)2+ H2O
Ca2+ +SO4 2- = CaSO4 ↓
Fe3+ + PO4 3- =FePO4 ↓
Al3+ + PO4 3- =AlPO4 ↓
Milk of lime consumption during this accounts for the 50% of whole calcium hydrophosphate fodder production technology milk of lime consumption, while there are about
20~30% phosphoric acid by wet process loses in the form of phosphate（In one section of N-process, the phosphate radical of the calcium phosphate precipitation of formation
Source by phosphoric acid by wet process provide, thus result in phosphoric acid by wet process and largely lose）.In addition, also in the presence of following defect：1st, it is secondary
The hydrate filtering that filter residue is entirely almost iron, aluminium is produced, press filtration is difficult, and it is more to eat liquid, has a strong impact on milk of lime consumption and clear liquid
Yield.2nd, by-product filter residue particle is tiny, and crystallinity is poor, often filtration difficulty, blocks filter cloth, and plant maintenance is difficult.3rd, by-product
Filter residue is entirely almost the hydrate of iron, aluminium, and grade is extremely low, therefore is simply possible to use in the white fertilizer of production low value, causes phosphor resource
Waste.Disadvantage mentioned above is the important factor in order for influenceing calcium hydrophosphate fodder production cost.
Can the current hydrogen calcium market competitive pressure be big, by rational technique adjustment reduction calcium dihydrogen phosphate filtrate（One section
Neutralize filtrate）Production cost, and reduce phosphoric acid by wet process loss turn into one be worth research problem.
The content of the invention
To overcome problem above present in prior art, the invention provides a kind of production work of calcium hydrophosphate fodder
Skill.
The technical solution adopted in the present invention is：The production technology of calcium hydrophosphate fodder, comprises the following steps：
A, one-section abstraction reaction：Phosphoric acid by wet process carries out extractive reaction with ground phosphate rock and/or phosphate ore pulp, and is incubated curing, must react
Slurry；
B, filtering reaction slurry obtain one section of filtrate and filter residue；
C, two sections of neutralization reactions, one section of filtrate carry out neutralization reaction with milk of lime, obtain slurry；
D, filter slurry obtain two sections of filtrates and filter cake, filter cake through drying, be crushed into calcium hydrophosphate fodder product.
The present invention is actually that one section of neutralization reaction of phosphoric acid by wet process in existing process and milk of lime is replaced with into wet method phosphorus
Acid carries out extractive reaction with ground phosphate rock.The main component of phosphorus ore is fluorapatite, in addition also containing impurity such as a small amount of iron, aluminium,
Because the impurity such as fluorine, iron, aluminium can not enter final calcium hydrophosphate fodder product, it is therefore necessary to try to remove them.This
In invention, main reaction is that fluorapatite generates calcium dihydrogen phosphate with wet-process phosphoric acid reaction, and phosphoric acid constantly quilt is carried out with reaction
Consumption, a small amount of acid very weak hydrofluoric acid of generation（7mol phosphoric acid is often consumed, 1mol hydrofluoric acid is generated）, therefore entering with reaction
The pH value of row solution constantly increases（Acidity is constantly reduced）, with the increase of pH value, iron, aluminium in phosphoric acid by wet process and in phosphorus ore
Impurity can be separated out in the form of calcium phosphate precipitation（Iron, the cardinal principle that aluminium is precipitated under certain acidity be because solubility product causes,
This is the chemical precipitation law of standard, will be generated when acidity is reduced to the precipitation acidity of ferric phosphate, aluminum phosphate corresponding
Precipitation）.A large amount of calcium ions occur during calcium dihydrogen phosphate is formed such that solution simultaneously, so that can be with the fluorine in phosphorus ore, wet method phosphorus
Sulfate radical in acid combines to form corresponding deposit.It is miscellaneous that reaction can obtain hardly iron content, aluminium, fluorine, sulfate radical etc. after terminating
The calcium dihydrogen phosphate filtrate of matter.
The main chemical reactions being related to are as follows：
Ca5（PO4）3F + 7H3PO4=5Ca（H2PO4）2+ HF
Ca2+ + 2F- =CaF2 ↓
Ca2+ + SO4 2- = CaSO4 ↓
Fe3+ + PO4 3- = FePO4 ↓
Al3+ + PO4 3- = AlPO4 ↓
Additional additive milk of lime is substituted with ground phosphate rock, production cost is not only substantially reduced, whole set process is formed well
One body circulation.Wherein ground phosphate rock is not only to play simple neutralization because wherein phosphorus also by phosphoric acid by wet process extraction
And enter in product, therefore ground phosphate rock effect in the present invention is substantially raw materials for production（And not neutralization reagent）, with list
The scheme that pure consumption large quantities of lime breast is neutralized to phosphoric acid by wet process is entirely different.The method is replaced with ground phosphate rock
Phosphoric acid by wet process is neutralized for milk of lime, but ground phosphate rock is also in itself raw materials for production, therefore from whole calcium hydrophosphate fodder
Production technology circulation from the point of view of be then the consumption for eliminating milk of lime so that the mode of production of intermediate product calcium dihydrogen phosphate from
Raw material（Phosphoric acid by wet process）With neutralization reagent（Milk of lime）The mode of production, enter to turn to raw material（Phosphoric acid by wet process）Plus raw material（Ground phosphate rock）
The mode of production, this benefit industrially to be brought is huge.
The main component of the accessory substance filter residue of generation be the complete phosphorus ore of unreacted, calcirm-fluoride, ferric phosphate, aluminum phosphate and by
The a small amount of calcium dihydrogen phosphate filtrate eaten liquid in filter residue and carry secretly；The hydrate proportion very little of iron, aluminium, warm in the filter residue
Larger precipitating crystalline can be formed after curing, liquid measure reduction is eaten, it is easier to which press filtration, calcium dihydrogen phosphate filtrate yields increase, together
When be not easily blocked filter plant, reduce cost of equipment maintenance, and recyclable as high value added product MAP（Rather than low
The white fertilizer of value）Raw materials for production enter MAP production system phosphorus ore extraction tank, mixing with sulfuric acid carries out extractive reaction
Reclaim the phosphorus in filter residue.So that the phosphorus of nearly all addition is all converted and enters phosphorus in whole calcium hydrophosphate fodder production system
Sour hydrogen calcium product is recovered and enters monoammonium phosphate product, and almost without phosphorus damage, realizes the abundant recovery of phosphorus.In the present invention, need
Add enough de-magging phosphorus ore filter cakes to promote the abundant reaction of de-magging phosphoric acid by wet process, and reach the purpose of regulation pH.
As a further improvement on the present invention, raw material of the filter residue that will be obtained in step B as MAP production technology
Use.The typical production process of MAP is ground phosphate rock（Slurry）Mixing with sulfuric acid carries out extractive reaction, and reaction slurry is consolidated
Liquid is separated, and obtains wet dilute phosphoric acid, and liquefied ammonia carries out neutralization reaction with wet dilute phosphoric acid, and reaction slurry is by multiple-effect（Three times or
Twice）Powdery or granular monoammonium phosphate product is obtained by operations such as drying, screening, anti-caking parcel, coolings after concentration concentrate.
The main component of the filter residue that step C of the present invention is obtained is the complete phosphorus ore of unreacted, calcirm-fluoride, ferric phosphate, aluminum phosphate
And a small amount of calcium dihydrogen phosphate filtrate carried secretly because filter residue eats liquid；The filter residue can be directly entered MAP production system
Phosphorus ore extraction tank, the phosphorus carried out during extractive reaction reclaims filter residue is mixed with sulfuric acid.So that whole calcium hydrophosphate fodder production body
The phosphorus of nearly all addition is all converted into calcium monophosphate product or is recovered and enters monoammonium phosphate product in system, almost without phosphorus
Damage.
As a further improvement on the present invention, the extractive reaction temperature of step B is maintained more than 60 DEG C.The purpose of temperature control
It is, in order to improve reactivity, to shorten the reaction time.
As a further improvement on the present invention, the feed postition of ground phosphate rock and/or phosphate ore pulp is in step B：While stirring
Add ground phosphate rock and/or phosphate ore pulp in phosphoric acid by wet process, add speed be able to maintain that the pH=1.5 of material in reaction vessel~
2.5.Ground phosphate rock or phosphate ore pulp are preferably that, as the carrying out of reaction is slowly added in reactive tank, its reason is ground phosphate rock and wet method phosphorus
It is slow that the reaction of acid has the decline of acidity in a process, therefore course of reaction, and being slowly added to ground phosphate rock can prevent from adding
Enter much excessive phosphorus ore（Excessively it is unfavorable for improve production efficiency and causes the waste of resource）.And can be by controlling adding for phosphorus ore
Enter speed, the pH of reaction system is controlled 1.5~2.5, it is ferric phosphate, the precipitation acidity of aluminum phosphate that the pH value range is corresponding
Scope.
As a further improvement on the present invention, the insulation curing time in step B is 50~90min.It is incubated the mesh of curing
Be that the crystallization for making deposit is fully grown up, precipitation is abundant.The impurity level being mixed into filtrate is effectively reduced, while can drop
Low precipitation matter eats liquid measure, is easy to subsequent filter operation, therefore should ensure that enough curing times.
As a further improvement on the present invention, the smashing fineness of ground phosphate rock used is in step B：325 mesh sieve percent of pass are big
In 90%.Mog is improved so that ground phosphate rock fully reacts with phosphoric acid by wet process, and is favorably improved reaction rate.
As a further improvement on the present invention, the filter residue obtained in step C is washed, the washing lotion for obtaining and step C
In obtain one section of filtrate mixing carry out follow-up two sections of neutralization reactions.Contain a small amount of calcium dihydrogen phosphate filtrate component in filter residue,
Can be recycled by washing.
As a further improvement on the present invention, phosphoric acid by wet process used is obtained by low magnesium phosphorus ore and sulfuric acid reaction in step A.By
Magnesium in phosphoric acid by wet process cannot be removed by reaction, therefore in order to ensure the quality of final feed calcium hydrophosphate product, should
Content of magnesium in phosphoric acid by wet process is reduced, can use the low content of magnesium phosphoric acid by wet process as obtained in low magnesium phosphorus ore and sulfuric acid reaction.
The ground phosphate rock that uses or phosphate ore pulp can also be crushed using low magnesium phosphorus ore and be obtained in the present invention simultaneously, or using sulfuric acid,
Phosphoric acid etc. carries out the low magnesium phosphorus ore obtained after de-magging pretreatment to high-magnesium-phosphorus ore, to ensure final feed calcium hydrophosphate product
Quality.
The beneficial effects of the invention are as follows：1）Neutralization reagent milk of lime next life producing feed-stage phosphorus is substituted with raw materials for production ground phosphate rock
The intermediate product calcium dihydrogen phosphate of sour hydrogen calcium, eliminates the consumption of milk of lime, makes the production cost of calcium hydrophosphate fodder significantly
Reduce；2）The filter residue produced while generation calcium dihydrogen phosphate can be real as the raw material of production high value added product MAP
The abundant recovery of existing phosphor resource.
Specific embodiment
With reference to embodiment, the present invention is further described.
Explanation：The degree of material refers both to mass percent without special instruction in following examples and comparative example.
Embodiment one：
Phosphorus ore（P2O5%=30%, MgO=1.0%）It is the percent of pass of 325 mesh sieve 90% to use wet milk to be fully ground to fineness, is added to
Phosphoric acid by wet process（P2O5=200g/l）In, maintenance reaction temperature is 70 DEG C；Ground phosphate rock control reaction slurry is gradually added into while stirring
2.0 or so, reaction terminates follow-up continuation of insurance temperature curing 60min must react slurry to the pH stable of material；Reaction slurry was carried out
Filter, obtains calcium dihydrogen phosphate filtrate（One section of filtrate）And filter residue, filter residue is directly entered MAP extracting system.The phosphoric acid for obtaining
Calcium dihydrogen filtrate into carrying out neutralization reaction in neutralization chamber with milk of lime, reacted slurry by be filtrated to get two sections of filtrates and
Filter cake, filter cake through pneumatic conveying drying, be crushed into calcium hydrophosphate fodder product.
One section of filtrate (calcium dihydrogen phosphate) leading indicator obtained by the program is as follows：
Ca(H2PO4)2=150g/l, Fe2O3=0.5g/l, Al2O3=0.5g/l, F-=0.2g/l, SO4 2-=0.8g/l。
Comparative example two：
Toward phosphoric acid by wet process（P2O5=200g/l）Middle addition milk of lime (CaO%=10%) carries out neutralization reaction, regulation reaction slurry pH=
2.0, fully obtain reacting slurry after reaction, filtering reaction slurry obtains calcium dihydrogen phosphate filtrate（One section of filtrate）, the phosphoric acid for obtaining
Calcium dihydrogen filtrate into carrying out neutralization reaction in neutralization chamber with milk of lime, reacted slurry by be filtrated to get two sections of filtrates and
Filter cake, filter cake through pneumatic conveying drying, be crushed into calcium hydrophosphate fodder product.
One section of filtrate (calcium dihydrogen phosphate) leading indicator obtained by the program is as follows：
Ca(H2PO4)2=150g/l, Fe2O3=0.4g/l, Al2O3=0.6g/l, F-=0.2g/l, SO4 2-=0.9g/l。
The solution of the present invention can be seen that compared with prior art by the contrast of above example, gained intermediate product
The quality of calcium dihydrogen phosphate filtrate is suitable with the quality of prior art gained calcium dihydrogen phosphate filtrate, but the present invention can exempt lime
The consumption of breast, accessory substance filter residue can be used to produce the advantage of high value added product MAP.
Claims (7)
1. the production method of calcium hydrophosphate fodder, comprises the following steps：
A, one-section abstraction reaction：Phosphoric acid by wet process carries out extractive reaction with ground phosphate rock and/or phosphate ore pulp, is fully incubated after reaction ripe
Change, obtain reaction slurry；
B, filtering reaction slurry obtain one section of filtrate and filter residue；
C, two sections of neutralization reactions, one section of filtrate carry out neutralization reaction with milk of lime, obtain slurry；
D, filter slurry obtain two sections of filtrates and filter cake, filter cake through drying, be crushed into calcium hydrophosphate fodder product.
2. the production method of calcium hydrophosphate fodder according to claim 1, it is characterised in that：By what is obtained in step B
Filter residue is used as the raw material of MAP production technology.
3. the production method of calcium hydrophosphate fodder according to claim 1, it is characterised in that：The extraction of step A is anti-
Temperature is answered to maintain more than 60 DEG C.
4. the production method of calcium hydrophosphate fodder according to claim 1, it is characterised in that：In step A ground phosphate rock and/
Or the feed postition of phosphate ore pulp is：Ground phosphate rock and/or phosphate ore pulp are added while stirring in phosphoric acid by wet process, adding speed for can
PH=1.5~2.5 of maintenance reaction material in container.
5. the production method of calcium hydrophosphate fodder according to claims 1 to 4, it is characterised in that：Insulation in step A
Curing time is 50~90min.
6. the production method of calcium hydrophosphate fodder according to claims 1 to 4, it is characterised in that：Phosphorus used in step A
The smashing fineness of miberal powder is that 325 mesh sieve percent of pass are more than 90%.
7. the production method of calcium hydrophosphate fodder according to claims 1 to 4, it is characterised in that：To be obtained in step B
Filter residue washed, the washing lotion for obtaining mixes with the one section of filtrate obtained in step B carries out follow-up two sections of neutralization reactions.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108046228A (en) * | 2017-12-29 | 2018-05-18 | 四川绵竹三佳饲料有限责任公司 | A kind of preparation method of high-purity phosphoric acid hydrogen calcium |
| CN109678126A (en) * | 2018-12-26 | 2019-04-26 | 四川龙蟒磷化工有限公司 | A kind of method that hydrochloric acid method prepares calcium hydrophosphate fodder |
| CN115504444A (en) * | 2022-09-30 | 2022-12-23 | 昆明川金诺化工股份有限公司 | Method for treating phosphorite chemical magnesium removal liquid |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1174812A (en) * | 1996-08-26 | 1998-03-04 | 四川联合大学 | Industrial monoammonium phosphate and productive method for industrial monoammunium phosphate and calcium hydrogen phosphate fodder |
| CN1283584A (en) * | 1999-08-04 | 2001-02-14 | 四川大学 | Process for preparing calcium hydrogen phosphate from middle-and low-grade phosphorus ore |
| CN105197905A (en) * | 2015-09-24 | 2015-12-30 | 中化化肥有限公司成都研发中心 | Production method for extracting phosphorite cogeneration feed grade monocalcium phosphate and industrial grade monoammonium phosphate |
-
2017
- 2017-01-10 CN CN201710014804.0A patent/CN106800285A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1174812A (en) * | 1996-08-26 | 1998-03-04 | 四川联合大学 | Industrial monoammonium phosphate and productive method for industrial monoammunium phosphate and calcium hydrogen phosphate fodder |
| CN1283584A (en) * | 1999-08-04 | 2001-02-14 | 四川大学 | Process for preparing calcium hydrogen phosphate from middle-and low-grade phosphorus ore |
| CN105197905A (en) * | 2015-09-24 | 2015-12-30 | 中化化肥有限公司成都研发中心 | Production method for extracting phosphorite cogeneration feed grade monocalcium phosphate and industrial grade monoammonium phosphate |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108046228A (en) * | 2017-12-29 | 2018-05-18 | 四川绵竹三佳饲料有限责任公司 | A kind of preparation method of high-purity phosphoric acid hydrogen calcium |
| CN109678126A (en) * | 2018-12-26 | 2019-04-26 | 四川龙蟒磷化工有限公司 | A kind of method that hydrochloric acid method prepares calcium hydrophosphate fodder |
| CN115504444A (en) * | 2022-09-30 | 2022-12-23 | 昆明川金诺化工股份有限公司 | Method for treating phosphorite chemical magnesium removal liquid |
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Application publication date: 20170606 |