CN109678126A - A kind of method that hydrochloric acid method prepares calcium hydrophosphate fodder - Google Patents
A kind of method that hydrochloric acid method prepares calcium hydrophosphate fodder Download PDFInfo
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- CN109678126A CN109678126A CN201811598670.2A CN201811598670A CN109678126A CN 109678126 A CN109678126 A CN 109678126A CN 201811598670 A CN201811598670 A CN 201811598670A CN 109678126 A CN109678126 A CN 109678126A
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- hydrochloric acid
- added
- filtrate
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- liquor
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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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses a kind of methods that hydrochloric acid method prepares calcium hydrophosphate fodder, comprising the following steps: hydrochloric acid is added in ground phosphate rock by S1, stirs after hydrochloric acid is added, and after standing, carries out first time filtering, obtains liquor B;S3 is added milk of lime into liquor B or calcium carbonate, pH value is adjusted to 0.8-1.0, adds vulcanized sodium and polyacrylamide flocculant, after precipitating completely, carries out second and filters, obtain filtrate D;5, filtrate D carry out defluorinate process, carry out third time filtering, obtain filtrate F;Milk of lime and calcium carbonate soln are added into filtrate F by S7, until pH value is 5.3-6.0, stirs evenly simultaneously, obtain mixed liquor G;S8 carries out third time filtering to mixed liquor G, obtains filter cake H;S9, filter cake H are washed with acetone soln, obtain filter residue;Filter residue is dried to measurement, obtains product calcium monohydrogen phosphate.In the present invention, defluorination effect is good, and fluorine content is lower than the requirement of national standard 0.18% in the calcium monohydrogen phosphate of generation, can be safe to use, no security risk.
Description
Technical field
The present invention relates to the sides that calcium monohydrogen phosphate preparation field more particularly to a kind of hydrochloric acid method prepare calcium hydrophosphate fodder
Method.
Background technique
Calcium monohydrogen phosphate is white monoclinic system crystal powder, and odorless, tasteless exists usually in the form of dihydrate,
Stablize in air.Calcium monohydrogen phosphate is heated to 75 DEG C and starts to lose the crystallization water as anhydride, and high temperature then becomes pyrophosphate, readily soluble
In dilute hydrochloric acid, dust technology and acetic acid, it is slightly soluble in water, does not dissolve in ethyl alcohol.
Calcium monohydrogen phosphate makees hardening agent and leavening agent uses, and China's regulation can be used for biscuit, dispensed food for baby, most ambassador
Dosage is 1.0g;Calcium monohydrogen phosphate also can be used as quality improver, for Flour product of fermenting, need appropriate use by production.
Calcium monohydrogen phosphate is as food feed additive, to supplement the phosphorus in poultry and livestock feed, calcium constituent.Calcium monohydrogen phosphate is in food
Industry is used as raising agent, is used for biscuit, milk replacer, and usage amount is needed by normal production, it may also be used for bread manufacture is trained with yeast
Support agent.
Calcium monohydrogen phosphate is used for the auxiliary fodder of poultry, can promote feed digestion, make poultry weight gain, to increase production meat
Amount, milk production, egg production, while can also treat the rickets, osteomalacia, anemia etc. of livestock.Calcium monohydrogen phosphate can also be used in point
Reagent, stabilizer for plastics, food and feed additive are analysed, and in glass industry production.
Country is clearly stipulate that fluorinated volume will be lower than 0.18% in calcium monohydrogen phosphate, therefore how reduce phosphorus in process of production
The fluorinated volume of sour hydrogen calcium, is problem to be solved.
Summary of the invention
To solve technical problem present in background technique, the present invention proposes that a kind of hydrochloric acid method prepares calcium hydrophosphate fodder
Method.
The method that a kind of hydrochloric acid method proposed by the present invention prepares calcium hydrophosphate fodder, comprising the following steps:
Hydrochloric acid is added in ground phosphate rock by S1, stirs after hydrochloric acid is added, and keeps reaction 3-5 hours, obtains mixed liquor A;
S2, mixed liquor A stand 2-3 hours, carry out first time filtering, obtain liquor B;
S3 is added milk of lime into liquor B or calcium carbonate, the pH value of liquor B is adjusted to 0.8-1.0, obtains mixing thing liquid C;
Vulcanized sodium and polyacrylamide flocculant is added into mixed liquor C in S4, after precipitating completely, carries out second of mistake
Filter, obtains filtrate D;
S5, filtrate D carry out defluorinate process;Sodium chloride is added into filtrate D, completely after precipitating, it is molten to add sodium hydroxide
Liquid and modified polyacrylamide solution, obtain mixed liquor E;
S6 after liquid E to be mixed is precipitated completely, carries out third time filtering, obtains filtrate F;
Milk of lime and calcium carbonate soln are added into filtrate F by S7, until pH value is 5.3-6.0, stirs evenly, obtain simultaneously
Mixed liquor G;
S8 carries out third time filtering to mixed liquor G, obtains filter cake H and filtrate K;
S9, filter cake H are washed with acetone soln, obtain filter residue;Filter residue is dried to measurement, obtains product calcium monohydrogen phosphate;
S10, it is whether up to standard using the fluorine content in fluorine ion selective electrode determining calcium monohydrogen phosphate;If up to standard, carry out
Storage.
Preferably, in S1, hydrochloric acid is the concentrated hydrochloric acid that mass percent is 37.5%.
Preferably, in S1, every 1g ground phosphate rock is corresponding to be added 0.5-1ml hydrochloric acid.
Preferably, in S1, reaction temperature is 70-80 degrees Celsius.
Preferably, in S1, mixing speed 200-400r/min.
Preferably, in S4, separation is carried out using band filter and is removed slag.
Preferably, in S9, drying condition is 80 degrees Celsius.
Preferably, S7, mixing speed 400r/min.
In the present invention, hydrochloric acid is the concentrated hydrochloric acid that mass percent is 37.5%, and every 1g ground phosphate rock corresponds to and 0.5- is added
1ml hydrochloric acid is conducive to improve production efficiency to guarantee the process of ground phosphate rock being sufficiently acidified;Reaction temperature is that 70-80 is Celsius
Degree guarantees that reaction is abundant;Mixing speed is 300r/min, guarantees being uniformly mixed for ground phosphate rock, so that ground phosphate rock and hydrochloric acid is complete
Full connected, to improve the acidification efficiency of ground phosphate rock;Meanwhile mixing speed is moderate, guarantees production safety,
In S5, filtrate D carries out defluorinate process;Sodium chloride is added into filtrate D, generates Na2SiF6Precipitating;Precipitating completely
Afterwards, adding sodium hydroxide solution and modified polyacrylamide solution turns fluorine further with the progress for promoting F to react with Si
Turn to SiF6 2-, Na is generated again2SiF6Precipitating realizes depth defluorinate, while reducing the viscosity of phosphoric acid again, accelerates Na2SiF6It is heavy
The sedimentation and filtering in shallow lake, defluorination effect is good, and defluorinate is high-efficient.
In the present invention, in S7, mixing speed 400r/min guarantees that neutralization reaches most preferably, to guarantee to neutralize
The accuracy of pH value afterwards guarantees the accuracy to reaction controlling;
In S9, filter cake H is washed with acetone soln, and obtained filter residue is dried to weighing apparatus under 80 degrees Celsius of drying condition
Amount, obtains product calcium monohydrogen phosphate, wherein the molecular structure of calcium monohydrogen phosphate itself will not be destroyed under 80 degrees Celsius of drying condition,
Guarantee product quality;Meanwhile guaranteeing that drying efficiency reaches highest, improve whole work efficiency, energy conservation and environmental protection.
In the present invention, defluorination effect is good, and fluorine content is lower than the requirement of national standard 0.18%, energy in the calcium monohydrogen phosphate of generation
Enough safe to use, no security risks.
Specific embodiment
Embodiment 1
The method that a kind of hydrochloric acid method proposed by the present invention prepares calcium hydrophosphate fodder, comprising the following steps:
Hydrochloric acid is added in ground phosphate rock by S1, stirs after hydrochloric acid is added, and keeps reaction 3-5 hours, obtains mixed liquor A;
S2, mixed liquor A stand 2-3 hours, carry out first time filtering, obtain liquor B;
S3 is added milk of lime into liquor B or calcium carbonate, the pH value of liquor B is adjusted to 0.8-1.0, obtains mixing thing liquid C;
Vulcanized sodium and polyacrylamide flocculant is added into mixed liquor C in S4, after precipitating completely, carries out second of mistake
Filter, obtains filtrate D;
S5, filtrate D carry out defluorinate process;Sodium chloride is added into filtrate D, completely after precipitating, it is molten to add sodium hydroxide
Liquid and modified polyacrylamide solution, obtain mixed liquor E;
S6 after liquid E to be mixed is precipitated completely, carries out third time filtering, obtains filtrate F;
Milk of lime and calcium carbonate soln are added into filtrate F by S7, until pH value is 5.3-6.0, stirs evenly, obtain simultaneously
Mixed liquor G;
S8 carries out third time filtering to mixed liquor G, obtains filter cake H and filtrate K;
S9, filter cake H are washed with acetone soln, obtain filter residue;Filter residue is dried to measurement, obtains product calcium monohydrogen phosphate;
S10, it is whether up to standard using the fluorine content in fluorine ion selective electrode determining calcium monohydrogen phosphate;If up to standard, carry out
Storage.
In the present invention, in S5, filtrate D carries out defluorinate process;Sodium chloride is added into filtrate D, generates Na2SiF6Precipitating;It is complete
After full precipitating, add sodium hydroxide solution and modified polyacrylamide solution, with the progress for promoting F to react with Si, make fluorine into
One step is converted into SiF6 2-, Na is generated again2SiF6Precipitating realizes depth defluorinate, while reducing the viscosity of phosphoric acid again, accelerates
Na2SiF6The sedimentation and filtering of precipitating, defluorination effect is good, and defluorinate is high-efficient.
In the present invention, defluorination effect is good, and fluorine content is lower than the requirement of national standard 0.18%, energy in the calcium monohydrogen phosphate of generation
Enough safe to use, no security risks.
Embodiment 2
The method that a kind of hydrochloric acid method proposed by the present invention prepares calcium hydrophosphate fodder, comprising the following steps:
Hydrochloric acid is added in ground phosphate rock by S1, stirs after hydrochloric acid is added, and keeps reaction 3-5 hours, obtains mixed liquor A;Hydrochloric acid
It is the concentrated hydrochloric acid that mass percent is 37.5%, and every 1g ground phosphate rock corresponds to and 0.5-1ml hydrochloric acid is added;Wherein, reaction temperature
It is 70-80 degrees Celsius, mixing speed 200-400r/min;
S2, mixed liquor A stand 2-3 hours, carry out first time filtering, obtain liquor B;
S3 is added milk of lime into liquor B or calcium carbonate, the pH value of liquor B is adjusted to 0.8-1.0, obtains mixing thing liquid C;
Vulcanized sodium and polyacrylamide flocculant is added into mixed liquor C in S4, after precipitating completely, carries out second of mistake
Filter, obtains filtrate D;Wherein, filtering separate using band filter and be removed slag, low energy consumption for band filter, occupied area is small,
Work efficiency is high, automatization level is high, be dehydrated and filter effect is good.
S5, filtrate D carry out defluorinate process;Sodium chloride is added into filtrate D, completely after precipitating, it is molten to add sodium hydroxide
Liquid and modified polyacrylamide solution, obtain mixed liquor E;
S6 after liquid E to be mixed is precipitated completely, carries out third time filtering, obtains filtrate F;
Milk of lime and calcium carbonate soln are added into filtrate F by S7, until pH value is 5.3-6.0, stirs evenly, obtain simultaneously
Mixed liquor G;
S8 carries out third time filtering to mixed liquor G, obtains filter cake H and filtrate K;
S9, filter cake H are washed with acetone soln, obtain filter residue;Filter residue is dried to measurement, obtains product calcium monohydrogen phosphate;
S10, it is whether up to standard using the fluorine content in fluorine ion selective electrode determining calcium monohydrogen phosphate;If up to standard, carry out
Storage.
In the present invention, hydrochloric acid is the concentrated hydrochloric acid that mass percent is 37.5%, and every 1g ground phosphate rock corresponds to and 0.5- is added
1ml hydrochloric acid is conducive to improve production efficiency to guarantee the process of ground phosphate rock being sufficiently acidified;Reaction temperature is that 70-80 is Celsius
Degree guarantees reaction sufficiently, and mixing speed is the acidification efficiency that 200-400r/min improves ground phosphate rock, and guarantees ground phosphate rock and hydrochloric acid
Full contact.
In S5, filtrate D carries out defluorinate process;Sodium chloride is added into filtrate D, generates Na2SiF6Precipitating;Completely after precipitating,
Adding sodium hydroxide solution and modified polyacrylamide solution is further converted to fluorine with the progress for promoting F to react with Si
SiF6 2-, Na is generated again2SiF6Precipitating realizes depth defluorinate, while reducing the viscosity of phosphoric acid again, accelerates Na2SiF6Precipitating
Sedimentation and filtering, defluorination effect is good, and defluorinate is high-efficient.
In the present invention, defluorination effect is good, and fluorine content is lower than the requirement of national standard 0.18%, energy in the calcium monohydrogen phosphate of generation
Enough safe to use, no security risks.
Embodiment 3
The method that a kind of hydrochloric acid method proposed by the present invention prepares calcium hydrophosphate fodder, comprising the following steps:
The concentrated hydrochloric acid that mass percent is 37.5% is added in ground phosphate rock, stirs after hydrochloric acid is added, and at 80 degrees Celsius by S1
Under the conditions of, it reacts 3-5 hours, obtains mixed liquor A;Wherein, every 1g ground phosphate rock is corresponding is added 0.5-1ml hydrochloric acid, and mixing speed is
300r/min。
S2, mixed liquor A stand 2-3 hours, carry out first time filtering, obtain liquor B;Wherein, using band filter into
Row separation is removed slag;
S3 is added milk of lime into liquor B or calcium carbonate, the pH value of liquor B is adjusted to 0.8-1.0, obtains mixing thing liquid C;
Vulcanized sodium and polyacrylamide flocculant is added into mixed liquor C in S4, after precipitating completely, carries out second of mistake
Filter, obtains filtrate D;Wherein, separation is carried out using band filter to remove slag;
S5, filtrate D carry out defluorinate process;Sodium chloride is added into filtrate D, completely after precipitating, it is molten to add sodium hydroxide
Liquid and modified polyacrylamide solution, obtain mixed liquor E;
S6 after liquid E to be mixed is precipitated completely, carries out third time filtering, obtains filtrate F;
Milk of lime and calcium carbonate soln are added into filtrate F, stirs evenly, mixing speed 400r/min works as pH value by S7
When for 5.3-6.0, mixed liquor G is obtained;
S8 carries out third time filtering to mixed liquor G, obtains filter cake H and filtrate K;
S9, filter cake H are washed with acetone soln, obtain filter residue;Under 80 degrees Celsius of drying condition, filter residue is dried to weighing apparatus
Amount, obtains product calcium monohydrogen phosphate;
S10, it is whether up to standard using the fluorine content in fluorine ion selective electrode determining calcium monohydrogen phosphate;If up to standard, carry out
Storage.
In the present invention, hydrochloric acid is the concentrated hydrochloric acid that mass percent is 37.5%, and every 1g ground phosphate rock corresponds to and 0.5- is added
1ml hydrochloric acid is conducive to improve production efficiency to guarantee the process of ground phosphate rock being sufficiently acidified;Reaction temperature is that 70-80 is Celsius
Degree guarantees that reaction is abundant;Mixing speed is 300r/min, guarantees being uniformly mixed for ground phosphate rock, so that ground phosphate rock and hydrochloric acid is complete
Full connected, to improve the acidification efficiency of ground phosphate rock;Meanwhile mixing speed is moderate, guarantees production safety,
In S5, filtrate D carries out defluorinate process;Sodium chloride is added into filtrate D, generates Na2SiF6Precipitating;Precipitating completely
Afterwards, adding sodium hydroxide solution and modified polyacrylamide solution turns fluorine further with the progress for promoting F to react with Si
Turn to SiF6 2-, Na is generated again2SiF6Precipitating realizes depth defluorinate, while reducing the viscosity of phosphoric acid again, accelerates Na2SiF6It is heavy
The sedimentation and filtering in shallow lake, defluorination effect is good, and defluorinate is high-efficient.
In the present invention, in S7, mixing speed 400r/min guarantees that neutralization reaches most preferably, to guarantee to neutralize
The accuracy of pH value afterwards guarantees the accuracy to reaction controlling;
In S9, filter cake H is washed with acetone soln, and obtained filter residue is dried to weighing apparatus under 80 degrees Celsius of drying condition
Amount, obtains product calcium monohydrogen phosphate, wherein the molecular structure of calcium monohydrogen phosphate itself will not be destroyed under 80 degrees Celsius of drying condition,
Guarantee product quality;Meanwhile guaranteeing that drying efficiency reaches highest, improve whole work efficiency, energy conservation and environmental protection.
In the present invention, defluorination effect is good, and fluorine content is lower than the requirement of national standard 0.18%, energy in the calcium monohydrogen phosphate of generation
Enough safe to use, no security risks.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (8)
1. a kind of method that hydrochloric acid method prepares calcium hydrophosphate fodder, which comprises the following steps:
Hydrochloric acid is added in ground phosphate rock by S1, stirs after hydrochloric acid is added, and keeps reaction 3-5 hours, obtains mixed liquor A;
S2, mixed liquor A stand 2-3 hours, carry out first time filtering, obtain liquor B;
S3 is added milk of lime into liquor B or calcium carbonate, the pH value of liquor B is adjusted to 0.8-1.0, obtains mixing thing liquid C;
Vulcanized sodium and polyacrylamide flocculant is added into mixed liquor C in S4, after precipitating completely, carries out second and filters,
Obtain filtrate D;
S5, filtrate D carry out defluorinate process;Sodium chloride is added into filtrate D, completely precipitating after, add sodium hydroxide solution and
Modified polyacrylamide solution, obtains mixed liquor E;
S6 after liquid E to be mixed is precipitated completely, carries out third time filtering, obtains filtrate F;
Milk of lime and calcium carbonate soln are added into filtrate F by S7, until pH value is 5.3-6.0, stirs evenly, are mixed simultaneously
Liquid G;
S8 carries out third time filtering to mixed liquor G, obtains filter cake H and filtrate K;
S9, filter cake H are washed with acetone soln, obtain filter residue;Filter residue is dried to measurement, obtains product calcium monohydrogen phosphate;
S10, it is whether up to standard using the fluorine content in fluorine ion selective electrode determining calcium monohydrogen phosphate;If up to standard, stored.
2. the method that hydrochloric acid method according to claim 1 prepares calcium hydrophosphate fodder, which is characterized in that in S1, hydrochloric acid
The concentrated hydrochloric acid for being 37.5% for mass percent.
3. the method that hydrochloric acid method according to claim 1 prepares calcium hydrophosphate fodder, which is characterized in that in S1, every 1g
Ground phosphate rock is corresponding to be added 0.5-1ml hydrochloric acid.
4. the method that hydrochloric acid method according to claim 1 prepares calcium hydrophosphate fodder, which is characterized in that in S1, reaction
Temperature is 70-80 degrees Celsius.
5. the method that hydrochloric acid method according to claim 1 prepares calcium hydrophosphate fodder, which is characterized in that in S1, stirring
Speed is 300-400r/min.
6. the method that hydrochloric acid method according to claim 1 prepares calcium hydrophosphate fodder, which is characterized in that in S4, use
Band filter carries out separation and removes slag.
7. the method that hydrochloric acid method according to claim 1 prepares calcium hydrophosphate fodder, which is characterized in that in S9, drying
Condition is 80 degrees Celsius.
8. the method that hydrochloric acid method according to claim 1 prepares calcium hydrophosphate fodder, which is characterized in that S7, stirring speed
Degree is 100r/min.
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Cited By (1)
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CN111003699A (en) * | 2019-12-30 | 2020-04-14 | 龙蟒大地农业有限公司 | Method for producing feed-grade calcium hydrophosphate and co-producing industrial-grade calcium chloride by hydrochloric acid method |
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CN111003699A (en) * | 2019-12-30 | 2020-04-14 | 龙蟒大地农业有限公司 | Method for producing feed-grade calcium hydrophosphate and co-producing industrial-grade calcium chloride by hydrochloric acid method |
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