CN1042820C - Production method of feed-grade monocalcium phosphate - Google Patents
Production method of feed-grade monocalcium phosphate Download PDFInfo
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- CN1042820C CN1042820C CN96116482A CN96116482A CN1042820C CN 1042820 C CN1042820 C CN 1042820C CN 96116482 A CN96116482 A CN 96116482A CN 96116482 A CN96116482 A CN 96116482A CN 1042820 C CN1042820 C CN 1042820C
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- phosphoric acid
- calcium phosphate
- drying
- secondary calcium
- raw material
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Abstract
The present invention discloses a production method of feed-grade monocalcium phosphate, which is characterized in that calcium hydrogen phosphate is used as a raw material, and the refined concentrated phosphoric acid is prepared through solid-phase direct conversion reaction, and technological processes of crushing, drying and screening. The production method is simple and easy to implement, low in cost, excellent in product quality and wide in market development prospect.
Description
The present invention relates to a kind of production method of fodder grade calcium phosphate.
As the mono-calcium phosphate of fodder additives,, be subjected to people's common concern in the nature of things because it is easily absorbed by the aquatic product animal.
At present with regard to fodder grade calcium phosphate [Ca (H
2PO
4)
2H
2O] production, generally adopt thermal phosphoric acid or wet method concentrated phosphoric acid and the direct neutralisation of lime powder both at home and abroad, though method is simple, but because this method is subjected to the influence of raw material phosphoric acid price bigger, cost is more and more higher, has limited the promotion and application of this product in feedstuff industry to a great extent.In addition, though with the Wet-process Phosphoric Acid Production fodder grade calcium phosphate should be a kind of desirable method, but because the quality index of the detrimental impurity element of product is difficult to reach requirement in production technique, add inevitably and will carry out condensing crystal, so the energy consumption height, so still there is not direct report so far by the Wet-process Phosphoric Acid Production fodder grade calcium phosphate.
Based on the present situation of above-mentioned domestic and international production mono-calcium phosphate, the branch of industry of China wishes relevant scientific worker, provides a kind of raw material cheap and easy to get, produces the simple and feasible novel method of producing fodder grade calcium phosphate that is suitable for China's actual conditions.
Purpose of the present invention is exactly the above-mentioned shortcoming at prior art, and a kind of production method of simple and easy to do fodder grade calcium phosphate is provided according to the needs of branch of industry.
Design of the present invention is such:
The contriver finds in being engaged in phosphide research for a long time, can very produce pure secondary calcium phosphate (it is Lin Suanergai industrial title) economically with phosphoric acid by wet process, and this is the water insolubility owing to secondary calcium phosphate, separates bringing great convenience to purifying products.Therefore, the contriver imagines the pure secondary calcium phosphate of direct usefulness and makes raw material, perhaps directly with CaCO
2Ore is a raw material, goes out pure secondary calcium phosphate (for prior art) with Wet-process Phosphoric Acid Production and for raw material, carries out the direct conversion reaction of solid phase with the purified strong phosphoric acid and produce fodder grade calcium phosphate [Ca (H
2PO
4)
2H
2O] method.
According to above-mentioned design, about content of the present invention and concrete production method are described below:
In chemical equation ratio uniform mixing, the conversion of windrow solid phase, pulverizing, drying make fodder grade calcium phosphate with purified strong phosphoric acid and secondary calcium phosphate.
Specific embodiments is as follows:
1. mix and the solid phase conversion
Secondary calcium phosphate (promptly crossing 40 mesh sieve holes) with particle diameter≤0.5mm adds in one horizontal pair of ribbon solid blender earlier, under agitation, in proportion the purified strong phosphoric acid is added in the blender in the spray mode by pump and shower nozzle, the reinforced back of finishing continues to stir 3～5 minutes, to guarantee that calcium hydrogen phosphate particle mixes with the strong phosphoric acid uniform contact, discharging, turning slaking 48～72hr guarantees that the solid phase conversion reaction between phosphoric acid and the secondary calcium phosphate is complete.Its chemical equation is as follows:
Wherein n=1.0～2.3 (being equivalent to refining strong phosphoric acid concentration is 85～70%)
In the windrow maturing process, can determine the completeness of solid phase conversion reaction by the pH value of measuring half-finished 5% aqueous solution, when PH 〉=3.0, show that the solid phase conversion reaction finishes.
When the secondary calcium phosphate that adopts carries out drying when sloughing crystal water about 80% in advance, adopting concentration simultaneously is that 85% refining strong phosphoric acid is when being raw material, free-water part is≤4% in the work in-process after the solid phase conversion is finished, to need not drying again during the product post-treatment is handled at this moment, and only need pulverizing, screening to get final product.
2. pulverize, drying
Work in-process after the solid phase conversion reaction (windrow slaking) fully can lump unavoidably because of reaction heat and the more high reason of water content, therefore should pulverize earlier, carry out drying again, and arrangement helps improving the finished product output capacity of drying installation like this.The coarse grain of not crossing 40 mesh sieve holes can return the new pulverizing of amount in the pulverizer, makes finished product by drying installation then.
Said purification of phosphoric acid can be that concentration is that the hot method industrial phosphoric acid of 85%wt, concentration are the mud phosphoric acid of 70%wt, or concentration reaches a kind of in the wet method concentrated phosphoric acid of 80%wt;
Said secondary calcium phosphate raw material, the ratio of components of its major ingredient is:
P
2O
5〉=40%, F≤0.18%, Ca 〉=22%; The secondary calcium phosphate of common feedstuffs level.
The ratio of said purified strong phosphoric acid and secondary calcium phosphate (is converted to P by chemical equation
2O
5Mol ratio) be 0.8～1: 1, should press reaction with same mole.Often be converted to weight ratio in the practicality, so that operation.
The work in-process that solid phase conversion reaction (being that industrial custom is called the turning slaking) obtains through pulverizing, drying, sieve all technological processs and obtain finished product.
Wherein: drying mode can be chosen arbitrarily, but the present invention recommends to adopt air stream drying, and this moment, drying temperature was 70～90 ℃;
Assurance 98% above product is crossed 40 mesh sieve holes (fineness requirement of product) during screening.
When adopting the secondary calcium phosphate drying to slough 80%wt left and right sides crystal water technology earlier, wherein drying should adopt air stream drying, and drying temperature is 140～160 ℃.
Further illustrate content of the present invention below in conjunction with drawings and Examples, but embodiment does not limit protection scope of the present invention.
Fig. 1---one of process implementing scheme of the present invention.
Fig. 2---two of process implementing scheme of the present invention.
Wherein:
1---blender
2---the solid state reaction aerobic fermentation tank
3---pulverizer
4---drying installation
5---sifter
According to Fig. 1 purified strong phosphoric acid and secondary calcium phosphate are placed blender 1 abundant stirring and evenly mixing by the weight ratio or the mol ratio of reactional equation, then compound is discharged in the aerobic fermentation tank 2, slaking 48～72hr, when the pH value by measuring half-finished 5% the aqueous solution greater than 3.0 the time, solid phase conversion reaction (slaking) is finished, the work in-process that slaking is finished are delivered to pulverizing in the pulverizer 3 earlier, enter in the drying installation drying and dehydrating again to water content≤4% of product, through sifter 5, the material of crossing 40 mesh sieve holes is product of the present invention, and the material of not crossing 40 mesh sieve holes then returns in the pulverizer 3 to be pulverized again, dry.
The process program of Fig. 2 and Fig. 1 is similar substantially, and its difference only is that Fig. 2 is the secondary calcium phosphate (CaHPO that will enter
42H
2O) crystal water sloughed about 80% of raw material elder generation drying device 4, mol ratio by reaction equation takes by weighing weight and refining strong phosphoric acid (85%wt) abundant stirring and evenly mixing in blender 1 then, and technologies such as remaining solid state reaction (windrow slaking), pulverizing, screening are all with shown in Figure 1.Because the drying dehydration of the secondary calcium phosphate that adopts in Fig. 2 technology elder generation, therefore can guarantee water-content≤4% in the product after the slaking, so no longer need drying in the technology afterwards.Obviously the equipment capacity of the technology of Fig. 2 is greater than the throughput of the processing unit of Fig. 1.Therefore, factory should pay the utmost attention to the operational path of Fig. 2 on the layout of production equipment.But as refining strong phosphoric acid (85%wt) source has any problem, and can obtain concentration easily and be the mud phosphoric acid of 70%wt the time, the technology of Fig. 1 remains one of more satisfactory production fodder grade calcium phosphate embodiment.
Get 50 kilograms of secondary calcium phosphates and (wherein contain P
2O
541.3%, F 0.14%, H
2O 0.3%, fineness 98.8% is crossed 40 mesh sieve holes) and 30 kilograms of (85%wt) thermal phosphoric acids, place blender to mix 5 minutes, be discharged into turning slaking 56hr in the aerobic fermentation tank, work in-process are PH=3.0 after measured, and free moisture content=9.3% is through pulverizing, in 80 ℃ of downstream dryings, get finished product 72kg, its quality is composed as follows:
P
2O
5(always)=54.1%, P
2O
5(water)/P
2O
5(always)=92.3%, Ca=16.85%, F=0.1%, H
2O=1.3%, fineness 98.5% is crossed 40 mesh sieve holes.
Get 50 kilograms of secondary calcium phosphates (industrial Lin Suanergai that claims again, it is formed with embodiment 1) and 36 kilograms of (concentration is 70%wt) mud phosphoric acid (making by the tankage in the phosphorus production process), produce by the 1 identical mode of enforcement, can get 74 kilograms of finished products, its quality is composed as follows:
P
2O
5(always)=53.1%, P
2O
5(water)/P
2O
5(always)=91%, Ca=16.8%, F=0.12%, H
2O=3.2%, product fineness 98% is crossed 40 mesh sieve holes.
Get 80 kilograms of secondary calcium phosphates (it is formed with embodiment 1) and, must consist of P in advance prior to 150 ℃ of downstream drying and dehydratings
2O
566 kilograms of the secondary calcium phosphates of=50.2% dehydration add 48 kilograms of (concentration is 85%wt) thermal phosphoric acids and placed behind the blender stirring and evenly mixing 5 minutes, are discharged into turning slaking 72hr in the aerobic fermentation tank.
Again through pulverize, sieve 112 kilograms of finished products, its quality is composed as follows:
P
2O
5(always)=55.2%, P
2O
5(water)/P
2O
5(always)=94.8%, Ca=16.9%, F=0.11%, H
2O=1.2%, product fineness 99.3% is crossed 40 mesh sieve holes.
Therefore, according to design of the present invention, can produce the fodder grade calcium phosphate product easily.
Point out in passing because at present country does not have the unified standard of fodder grade calcium phosphate as yet, for this reason enterprise will to advise that the expert formulates the unified national standard of fodder grade calcium phosphate as follows:
P
2O
5(always) 〉=53.1%;
P
2O
5(water)/P
2O
5(always) 〉=90%;
Ca ≤17％；
F ≤0.15％；
H
2O ≤4％；
PH ≥3.0；
Fineness 〉=98% is crossed 40 mesh sieve holes;
Outward appearance is the white crystalline powder of good fluidity.
Product of the present invention is all excellent above-mentioned standard, has satisfied the specification of quality of branch of industry to fodder grade calcium phosphate fully.
In a word, method of the present invention has the vast market development prospect.
Claims (2)
1. the production method of a fodder grade calcium phosphate is characterized in that:
With purified strong phosphoric acid and secondary calcium phosphate be raw material by the mixed of reaction formula evenly after, place aerobic fermentation tank to carry out the solid phase conversion reaction, again through pulverize, dry, all technological processs of screening make product of the present invention;
Wherein:
(1) said refining strong phosphoric acid is that concentration is that hot method industrial phosphoric acid, the concentration of 85% (wt) is that the mud phosphoric acid of 70% (wt) or concentration are greater than 80%wt) the wet method concentrated phosphoric acid in a kind of;
(2) ratio of components of said its main component of secondary calcium phosphate is:
P
2O
5≥40％,F≤0.18％,Ca≥22％；
(3) material rate of said refining strong phosphoric acid and secondary calcium phosphate is by being converted to P
2O
5After mol ratio be: " 0.8-1: 1 ";
(4) mixing in one horizontal pair of ribbon blender of said raw material finished, solid phosphoric acid hydrogen calcium adds earlier in the blender, and then under agitation, phosphoric acid adds with the form of spray, continued to mix the material that can obtain to mix 3-5 minute behind reinforced the finishing;
(5) said solid phase conversion reaction is that the material that will mix places aerobic fermentation tank to turn over to push away slaking 48～72 hours;
(6) said dry system adopts air stream drying, and drying temperature is 70～90 ℃.
2. the method for claim 1 is characterized in that: raw material secondary calcium phosphate elder generation drying is sloughed 80% crystal water, the appropriate to the occasion employing air stream drying that dewaters, and drying temperature is 140～160 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96116482A CN1042820C (en) | 1996-08-23 | 1996-08-23 | Production method of feed-grade monocalcium phosphate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96116482A CN1042820C (en) | 1996-08-23 | 1996-08-23 | Production method of feed-grade monocalcium phosphate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1146426A CN1146426A (en) | 1997-04-02 |
| CN1042820C true CN1042820C (en) | 1999-04-07 |
Family
ID=5123583
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN96116482A Expired - Fee Related CN1042820C (en) | 1996-08-23 | 1996-08-23 | Production method of feed-grade monocalcium phosphate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1042820C (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102079515A (en) * | 2010-03-22 | 2011-06-01 | 云南天创科技有限公司 | High efficiency low consumption thick slurry method for preparing high-quality monocalcium phosphate monohydrate |
| CN103435024A (en) * | 2013-08-08 | 2013-12-11 | 瓮福（集团）有限责任公司 | Method for producing feed grade calcium hydrophosphate |
| CN103803520B (en) * | 2014-02-27 | 2015-06-24 | 武汉工程大学 | Production method for feed-grade calcium monohydrogenphosphate |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2296495A (en) * | 1939-09-14 | 1942-09-22 | Blockson Chemical Co | Manufacture of anhydrous monocalcium phosphate |
| US3401014A (en) * | 1965-11-26 | 1968-09-10 | Olin Mathieson | Preparation of pure monocalcium phosphate |
| US4454103A (en) * | 1982-04-21 | 1984-06-12 | Stauffer Chemical Company | High acid monocalcium phosphate and process for preparing the same |
-
1996
- 1996-08-23 CN CN96116482A patent/CN1042820C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2296495A (en) * | 1939-09-14 | 1942-09-22 | Blockson Chemical Co | Manufacture of anhydrous monocalcium phosphate |
| US3401014A (en) * | 1965-11-26 | 1968-09-10 | Olin Mathieson | Preparation of pure monocalcium phosphate |
| US4454103A (en) * | 1982-04-21 | 1984-06-12 | Stauffer Chemical Company | High acid monocalcium phosphate and process for preparing the same |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1146426A (en) | 1997-04-02 |
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Free format text: CORRECT: PATENTEE; FROM: LOMON MINERALS AND FEEDS(GROUP) CO., LTD,MIANZHU, SICHUAN TO: SICHUAN LOMON GROUP CO., LTD. |
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| CP03 | Change of name, title or address |
Address after: Sichuan city in Mianzhu province of South Road Patentee after: Longmang Group Co., Ltd., Sichuan Prov Address before: Sichuan province Mianzhu County South high respect Temple Patentee before: Longmang Mineral Material Fodder Group Co., Ltd., Mianzhu County, Sichuan Prov. |
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Granted publication date: 19990407 |