CN106853962A - A kind of feed-level calcium biphosphate and preparation method thereof - Google Patents
A kind of feed-level calcium biphosphate and preparation method thereof Download PDFInfo
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- CN106853962A CN106853962A CN201611173002.6A CN201611173002A CN106853962A CN 106853962 A CN106853962 A CN 106853962A CN 201611173002 A CN201611173002 A CN 201611173002A CN 106853962 A CN106853962 A CN 106853962A
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- parts
- calcium
- phosphoric acid
- acid solution
- feed
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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
- C01B25/328—Defluorination during or after the preparation
Abstract
The invention discloses a kind of feed-level calcium biphosphate, according to weight meter, it is made up of 20 30 parts of phosphorus ore, 5 15 parts of calcium hydroxide, 5 15 parts of calcium carbonate, 5 15 parts of sulfuric acid, 5 15 parts of industrial waste acid, 26 parts of activated carbon grain.Present invention process is simple, easy to implement and raw material sources are extensive, can shorten the production technology time, energy consumption is low, low cost, industrialization large-scale production is applicable to, with wide market prospects and good economic results in society.
Description
Technical field
The present invention relates to a kind of feed-level calcium biphosphate and preparation method thereof, belong to feed additive production technology neck
Domain.
Background technology
The principal item of feed-grade calcium phosphate salt has tricalcium phosphate, and calcium monohydrogen phosphate, calcium dihydrogen phosphate belong to mineral matter element
Nutritive additive.Wherein, calcium dihydrogen phosphate (MCP) is a kind of excellent high efficiency phosphatic feed additive, phosphorous height,
Water-soluble rate is high, is widely used in the feed addictive of aquiculture animal and livestock and poultry cultivation animal.Because calcium dihydrogen phosphate is water-soluble
Phosphorus content is higher, and content accounts for more than total phosphorus 90wt%, is conducive to absorption of the aquatic livestock to calcium phosphorus, digestibility 90% with
On, excretion is few, the features such as be conducive to environmental protection.At home and abroad find broad application.
At present, both at home and abroad generally using wet processing and dry process production feed-level calcium biphosphate.Wherein wet method work
Skill is that solid material is added in phosphoric acid solution obtained in wet method, and generation is dissolved in the calcium dihydrogen phosphate of water, by vacuum concentration, cold
But after crystallizing, separating out calcium dihydrogen phosphate crystal, re-dry, crushings, screening obtain product, and it is long that the method has a technological process, phosphorus damage
Lose greatly, high energy consumption, investment are big, and production capacity is small, cost is high to wait not enough.Dry process is then using phosphoric acid and C obtained in hot method
The solid materials such as aCO3 react, and after obtaining calcium dihydrogen phosphate slurry, product, this side are obtained by drying, broken, screening etc.
There is the deficiencies such as equipment volume is huge, granularity is small, power consumption is big in method.Therefore, in the prior art, generally existing technological process
Length, high energy consumption, investment be big and the low feature of productivity ratio.
The content of the invention
It is an object of the present invention to provide a kind of feed-level calcium biphosphate and preparation method thereof.The invention can shorten life
Production. art time, low cost.
Technical scheme：A kind of feed-level calcium biphosphate, according to weight meter, by phosphorus ore 20-30 parts, hydroxide
Calcium 5-15 parts, calcium carbonate 5-15 parts, sulfuric acid 5-15 parts, industrial waste acid 5-15 parts, activated carbon grain 2-6 parts of composition.
Foregoing feed-level calcium biphosphate, according to weight meter, by 25 parts of phosphorus ore, 10 parts of calcium hydroxide, 10 parts of calcium carbonate,
10 parts of sulfuric acid, 10 parts of industry spent acid, 4 parts of compositions of activated carbon grain.
Foregoing feed-level calcium biphosphate and preparation method thereof, includes following steps：
（1）Sulfuric acid and spent acid are mixed to prepare nitration mixture A；
（2）By obtained nitration mixture A and phosphorus ore hybrid reaction, heating stirring 2-6 hours, phosphoric acid solution B is obtained；
（3）Obtained phosphoric acid solution B is added into activated carbon grain, calcium hydroxide, water 2-4kg, defluorinate removal of impurities is carried out, 3-5 is stood small
When, clean phosphoric acid solution C is obtained；
（4）Calcium carbonate and obtained phosphoric acid solution C neutralization reactions, heating are concentrated, filter, clean, dried, obtained final product.
Foregoing feed-level calcium biphosphate and preparation method thereof, includes following steps：
（1）Sulfuric acid and spent acid are mixed to prepare nitration mixture A；
（2）Obtained nitration mixture A and phosphorus ore hybrid reaction, heating stirring 4 hours are obtained phosphoric acid solution B；
（3）Obtained phosphoric acid solution B is added into activated carbon grain, calcium hydroxide, water 3kg, defluorinate removal of impurities is carried out, 4 hours are stood, system
Obtain phosphoric acid solution C totally；
（4）By calcium carbonate and obtained phosphoric acid solution C neutralization reactions, heating, concentration, filtering, cleaning, drying, obtain final product.
It is in foregoing feed-level calcium biphosphate and preparation method thereof, the calcium carbonate and obtained phosphoric acid solution C and anti-
The heating-up temperature answered is 40-60 DEG C.
Beneficial effects of the present invention：Compared with prior art, feed of the invention has advantages below：
1. calcium hydroxide used in the present invention and calcium carbonate greatly reduce the production time as raw material, increase economic efficiency.
2. present invention process is simple, it is easy to implement, and raw material sources are extensively, is applicable to industrialization large-scale production,
With wide market prospects and good economic results in society.
3. the spent acid used by the present invention replaces phosphoric acid commonly used in the prior art, cheap, and obtained fertilizer efficiency
Height, its pH value is in faintly acid, with improvement basic soil effect.
4. the obtained fertilizer of the present invention can both be administered alone or can be used in mixed way with other nutrients, if making with nitrogenous fertilizer mixing
With with certain nitrogen fixation.
Experimental example production time, pH value and production cost
1 process and material therefor
1.1 wet processings：Method（Solid material is added in phosphoric acid solution obtained in wet method, generation is dissolved in the biphosphate of water
Calcium, by the way that after vacuum concentration, crystallisation by cooling, precipitation calcium dihydrogen phosphate crystal, re-dry, crushing, screening obtain product）；
Dry process：Method（Reacted using solid materials such as phosphoric acid obtained in hot method and CaCO3, obtain calcium dihydrogen phosphate material
After slurry, product is obtained by drying, broken, screening etc.）；
Preparation method of the invention：It is prepared by embodiment 2；
1.2 test methods：Production time, pH value and production cost are observed by testing production tracing.
1.3 observation statistical indicators
（1）Production for production time, pH value and production cost respectively carries out Experimental Comparison, and production time, PH are counted respectively
Value and production cost.
（2）Production to production time, pH value and production cost carries out five Experimental Comparisons（Average）.
1.4 results
Result see the table below 1.
The production time of table 1, pH value and production cost statistics table（The product of production identical weight packaging）
| Technique and preparation method | Production time（My god） | PH value | Production cost（Unit） |
| Wet processing | 20 | 5 | 60 |
| Dry process | 21 | 4 | 65 |
| Preparation method of the invention | 16 | 3 | 55 |
More than experiment understand, the present invention compared with prior art, with speed of production is fast, low cost and other advantages.
Invention is further described with reference to embodiment, but is not intended as the foundation to present invention limitation.
Specific embodiment
Embodiments of the invention 1.
A kind of feed-level calcium biphosphate, according to weight meter, by phosphorus ore 20-30 parts, calcium hydroxide 5-15 parts, calcium carbonate 5-
15 parts, sulfuric acid 5-15 parts, industrial waste acid 5-15 parts, activated carbon grain 2-6 parts of composition.
Described feed-level calcium biphosphate and preparation method thereof, includes following steps：
（1）Sulfuric acid and spent acid are mixed to prepare nitration mixture A；
（2）By obtained nitration mixture A and phosphorus ore hybrid reaction, heating stirring 2-6 hours, phosphoric acid solution B is obtained；
（3）Obtained phosphoric acid solution B is added into activated carbon grain, calcium hydroxide, water 2-4kg, defluorinate removal of impurities is carried out, 3-5 is stood small
When, clean phosphoric acid solution C is obtained；
（4）Calcium carbonate and obtained phosphoric acid solution C neutralization reactions, heating are concentrated, filter, clean, dried, obtained final product.
Embodiments of the invention 2.
A kind of feed-level calcium biphosphate, according to weight meter, by 25 parts of phosphorus ore, 10 parts of calcium hydroxide, 10 parts of calcium carbonate, sulphur
10 parts of acid, 10 parts of industry spent acid, 4 parts of compositions of activated carbon grain.
（1）Sulfuric acid and spent acid are mixed to prepare nitration mixture A；
（2）Obtained nitration mixture A and phosphorus ore hybrid reaction, heating stirring 4 hours are obtained phosphoric acid solution B；
（3）Obtained phosphoric acid solution B is added into activated carbon grain, calcium hydroxide, water 3kg, defluorinate removal of impurities is carried out, 4 hours are stood, system
Obtain phosphoric acid solution C totally；
（4）By calcium carbonate and obtained phosphoric acid solution C neutralization reactions, heating, concentration, filtering, cleaning, drying, obtain final product.
Embodiments of the invention 3.
A kind of feed-level calcium biphosphate, according to weight meter, by 20 parts of phosphorus ore, 5 parts of calcium hydroxide, 5 parts of calcium carbonate, sulfuric acid
5 parts, 5 parts of industry spent acid, 2 parts of activated carbon grain composition.
（1）Sulfuric acid and spent acid are mixed to prepare nitration mixture A；
（2）Obtained nitration mixture A and phosphorus ore hybrid reaction, heating stirring 2 hours are obtained phosphoric acid solution B；
（3）Obtained phosphoric acid solution B is added into activated carbon grain, calcium hydroxide, water 2kg, defluorinate removal of impurities is carried out, 3 hours are stood, system
Obtain phosphoric acid solution C totally；
（4）By calcium carbonate and obtained phosphoric acid solution C neutralization reactions, heating, concentration, filtering, cleaning, drying, obtain final product.
Embodiments of the invention 4.
A kind of feed-level calcium biphosphate, according to weight meter, by 30 parts of phosphorus ore, 15 parts of calcium hydroxide, 15 parts of calcium carbonate, sulphur
15 parts of acid, 15 parts of industry spent acid, 6 parts of compositions of activated carbon grain.
（1）Sulfuric acid and spent acid are mixed to prepare nitration mixture A；
（2）Obtained nitration mixture A and phosphorus ore hybrid reaction, heating stirring 6 hours are obtained phosphoric acid solution B；
（3）Obtained phosphoric acid solution B is added into activated carbon grain, calcium hydroxide, water 4kg, defluorinate removal of impurities is carried out, 5 hours are stood, system
Obtain phosphoric acid solution C totally；
（4）By calcium carbonate and obtained phosphoric acid solution C neutralization reactions, heating, concentration, filtering, cleaning, drying, obtain final product.
The calcium carbonate is 40-60 DEG C with the heating-up temperature of obtained phosphoric acid solution C neutralization reactions.
Claims (5)
1. a kind of feed-level calcium biphosphate, it is characterised in that：According to weight meter, by phosphorus ore 20-30 parts, calcium hydroxide 5-15
Part, calcium carbonate 5-15 parts, sulfuric acid 5-15 parts, industrial waste acid 5-15 parts, activated carbon grain 2-6 parts of composition.
2. feed-level calcium biphosphate according to claim 1, it is characterised in that：According to weight meter, by 25 parts of phosphorus ore, hydrogen
10 parts of calcium oxide, 10 parts of calcium carbonate, 10 parts of sulfuric acid, 10 parts of industry spent acid, 4 parts of compositions of activated carbon grain.
3. a kind of feed-level calcium biphosphate as claimed in claim 1 or 2 and preparation method thereof, it is characterised in that：Include
Following steps：
（1）Sulfuric acid and spent acid are mixed to prepare nitration mixture A；
（2）By obtained nitration mixture A and phosphorus ore hybrid reaction, heating stirring 2-6 hours, phosphoric acid solution B is obtained；
（3）Obtained phosphoric acid solution B is added into activated carbon grain, calcium hydroxide, water 2-4kg, defluorinate removal of impurities is carried out, 3-5 is stood small
When, clean phosphoric acid solution C is obtained；
（4）Calcium carbonate and obtained phosphoric acid solution C neutralization reactions, heating are concentrated, filter, clean, dried, obtained final product.
4. feed-level calcium biphosphate according to claim 3 and preparation method thereof, it is characterised in that：Include following step
Suddenly：
（1）Sulfuric acid and spent acid are mixed to prepare nitration mixture A；
（2）Obtained nitration mixture A and phosphorus ore hybrid reaction, heating stirring 4 hours are obtained phosphoric acid solution B；
（3）Obtained phosphoric acid solution B is added into activated carbon grain, calcium hydroxide, water 3kg, defluorinate removal of impurities is carried out, 4 hours are stood, system
Obtain phosphoric acid solution C totally；
（4）By calcium carbonate and obtained phosphoric acid solution C neutralization reactions, heating, concentration, filtering, cleaning, drying, obtain final product.
5. feed-level calcium biphosphate according to claim 3 or 4 and preparation method thereof, it is characterised in that：The carbonic acid
Calcium is 40-60 DEG C with the heating-up temperature of obtained phosphoric acid solution C neutralization reactions.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108163826A (en) * | 2018-01-12 | 2018-06-15 | 南京牧奇亚生物科技有限公司 | Feed-grade calcium phosphate salt and preparation method thereof |
| CN110483125A (en) * | 2019-08-02 | 2019-11-22 | 史丹利化肥当阳有限公司 | Utilize the method for waste phosphoric acid production S-based compound fertilizer raw material |
Citations (8)
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|---|---|---|---|---|
| CN1107661A (en) * | 1994-03-01 | 1995-09-06 | 云南精细化工公司 | Catalytic technology for processing calcium hydrogen phosphate as feed |
| CN1153137A (en) * | 1996-08-23 | 1997-07-02 | 四川绵竹龙蟒矿物质饲料集团有限公司 | Method for producing toothpaste grade calcium hydrophosphate |
| CN1155513A (en) * | 1996-01-23 | 1997-07-30 | 魏如铎 | Method for producing calcium hydrophosphate and monocalcium phosphate as feeds |
| CN1305946A (en) * | 2001-03-28 | 2001-08-01 | 四川龙蟒集团有限责任公司 | Process for preparing feed-class calcium dihydrogen phosphate and high-phosphorus products |
| CN1308015A (en) * | 2001-01-18 | 2001-08-15 | 天津化工研究设计院 | Depuration method for the production process of large-grain feed-level calcium hydrogen phosphate crystal |
| CN101058414A (en) * | 2007-06-06 | 2007-10-24 | 四川绵竹新清华化工有限责任公司 | Reused process for waste water in calcium hydrogen orthophosphate production |
| CN102815681A (en) * | 2012-06-21 | 2012-12-12 | 中化云龙有限公司 | Method for producing feed-grade calcium dihydrogen phosphate from wet-process phosphoric acid |
| CN103303886A (en) * | 2013-06-28 | 2013-09-18 | 山东鲁北企业集团总公司 | Novel method for producing industrial phosphoric acid by purification with wet process phosphoric acid |
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- 2016-12-18 CN CN201611173002.6A patent/CN106853962A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1107661A (en) * | 1994-03-01 | 1995-09-06 | 云南精细化工公司 | Catalytic technology for processing calcium hydrogen phosphate as feed |
| CN1155513A (en) * | 1996-01-23 | 1997-07-30 | 魏如铎 | Method for producing calcium hydrophosphate and monocalcium phosphate as feeds |
| CN1153137A (en) * | 1996-08-23 | 1997-07-02 | 四川绵竹龙蟒矿物质饲料集团有限公司 | Method for producing toothpaste grade calcium hydrophosphate |
| CN1308015A (en) * | 2001-01-18 | 2001-08-15 | 天津化工研究设计院 | Depuration method for the production process of large-grain feed-level calcium hydrogen phosphate crystal |
| CN1305946A (en) * | 2001-03-28 | 2001-08-01 | 四川龙蟒集团有限责任公司 | Process for preparing feed-class calcium dihydrogen phosphate and high-phosphorus products |
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| CN102815681A (en) * | 2012-06-21 | 2012-12-12 | 中化云龙有限公司 | Method for producing feed-grade calcium dihydrogen phosphate from wet-process phosphoric acid |
| CN103303886A (en) * | 2013-06-28 | 2013-09-18 | 山东鲁北企业集团总公司 | Novel method for producing industrial phosphoric acid by purification with wet process phosphoric acid |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108163826A (en) * | 2018-01-12 | 2018-06-15 | 南京牧奇亚生物科技有限公司 | Feed-grade calcium phosphate salt and preparation method thereof |
| CN110483125A (en) * | 2019-08-02 | 2019-11-22 | 史丹利化肥当阳有限公司 | Utilize the method for waste phosphoric acid production S-based compound fertilizer raw material |
| CN110483125B (en) * | 2019-08-02 | 2022-03-04 | 史丹利化肥当阳有限公司 | Method for producing raw material for sulfur-based compound fertilizer by using waste phosphoric acid |
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Application publication date: 20170616 |