CN106241766B - It is a kind of without burnt high-pure anhydrous dipotassium hydrogen phosphate production system and technique - Google Patents
It is a kind of without burnt high-pure anhydrous dipotassium hydrogen phosphate production system and technique Download PDFInfo
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- CN106241766B CN106241766B CN201610672471.6A CN201610672471A CN106241766B CN 106241766 B CN106241766 B CN 106241766B CN 201610672471 A CN201610672471 A CN 201610672471A CN 106241766 B CN106241766 B CN 106241766B
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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
- C01B25/30—Alkali metal phosphates
- C01B25/305—Preparation from phosphorus-containing compounds by alkaline treatment
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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
- C01B25/30—Alkali metal phosphates
- C01B25/308—Methods for converting an alkali metal orthophosphate into another one; Purification; Decolorasing; Dehydrating; Drying
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/10—Solid density
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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
- C01P2006/82—Compositional purity water content
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Abstract
Pyrophosphate or metaphosphate are free of in the product without burnt high-pure anhydrous dipotassium hydrogen phosphate production system and technique, no high-purity major embodiment of coke the invention discloses a kind of, and contained other impurity are few, the aspect such as dipotassium hydrogen phosphate content height.Present system includes sequentially connected phosphoric acid, potassium hydroxide storage tank, phosphoric acid, potassium hydroxide head tank, neutralization reaction kettle, fine filter, slurry storage tank, evaporation concentration device, crystallization apparatus, centrifuge, conveying device is evaporated under reduced pressure, the dry furnace apparatus of two-part indirect heating dynamic, conveying device, cooling furnace apparatus, conveying device, pulverizing-screening system, packaging system.The present invention has rational design, belongs to continuous production processes, high production efficiency.Compared with spray-on process produces anhydrous potassium dihydrogen phosphate, this system is produced by the way of crystallization and indirect heating, the generation of dust is greatly reduced, product purity has promotion by a relatively large margin, and pyrophosphate or metaphosphate are free of in product, while energy consumption is also greatly reduced.
Description
Technical field
The invention belongs to anhydrous potassium dihydrogen phosphate production technical fields, and in particular to a kind of without burnt high-pure anhydrous phosphoric acid hydrogen two
Potassium production system and technique.
Background technique
Dipotassium hydrogen phosphate is mainly used for medicine, fermentation, Bacteria Culture and produces potassium pyrophosphate etc., is commonly used for analytical reagent,
Buffer and water quality treatment agent are used to prepare the raw material of wheaten food buck in food industry, ferment and use agent, flavoring agent is swollen
Loose agent, the mild alkaline agent of dairy products, yeast food, as quality improver.
Country's anhydrous potassium dihydrogen phosphate uses spray drying process production technology substantially at present, and production scene dust is more, warp
Product heap density after atomization is smaller, and substantially in 0.4g/mL~0.5g/mL or so, dust recovery rate is lower, and most using day
The right clean energy resourcies such as gas or hydrogen are fuel, and energy consumption is relatively large, and production cost is relatively high, anhydrous phosphorus obtained by this production technology
Sour hydrogen dipotassium product content is relatively low, substantially 98%~99.5% or so, is often detected the pyrophosphoric acid containing 1%~3%
Salt and metaphosphate, the elementary metal impurities such as sodium calcium and magnesium ferro-aluminum are relatively high in product, sodium ion substantially 3000ppm~
5000ppm or so, calcium and magnesium aluminium ion substantially in 5ppm~25ppm or so, iron ion substantially in 5ppm~40ppm or so, chlorine from
Son is substantially in 20ppm~60ppm or so, and sulfate radical is in 40ppm~100ppm or so.
Summary of the invention
The purpose of the present invention is to provide a kind of without burnt high-pure anhydrous dipotassium hydrogen phosphate production system, while providing to utilize and be somebody's turn to do
Production technology of the system production without burnt high-pure anhydrous dipotassium hydrogen phosphate.
To achieve the above object, the present invention adopts the following technical scheme:
It is a kind of without burnt high-pure anhydrous dipotassium hydrogen phosphate production system, phosphoric acid storage tank and potassium hydroxide storage tank respectively with phosphoric acid height
Position slot and the connection of potassium hydroxide head tank, phosphoric acid head tank and potassium hydroxide head tank are connect with neutralization reaction kettle, neutralization reaction
Kettle is connect with fine filter, and fine filter is connect with slurry storage tank, and slurry storage tank is connect with evaporation concentrator, evaporation concentrator and decompression
Crystallizing evaporator connection is evaporated under reduced pressure crystallizer and connect with centrifuge, and centrifuge and two-part indirect heating dynamic drying oven connect
It connects, two-part indirect heating dynamic drying oven is connect with cooling furnace, and cooling furnace is connect with crushing and screening, can be formed without burnt high-purity
The process units of anhydrous potassium dihydrogen phosphate.The centrifuge is also connect with evaporation concentrator.
Technique using the production of above-mentioned production system without burnt high-pure anhydrous dipotassium hydrogen phosphate, comprising the following steps:
(1) neutralization reaction: using 85% phosphoric acid and 48% alkali potassium as raw material, carry out neutralization reaction in a kettle, control
Slurry pH value processed is between 8.6~9.4, after fine filter filters, squeezes into slurry storage tank, maintain storage tank slurry temperature 85 DEG C~
105 DEG C of ranges；
(2) it is concentrated by evaporation: storage tank slurry being squeezed into evaporation concentration device and is concentrated, control concentrate concentration
In 69wt%~72wt% range；Further preferably being concentrated by evaporation to urine concentration is 70wt%；
(3) crystallization is evaporated under reduced pressure: control vacuum degree in -0.08 MPa~-0.12MPa range, feed liquid temperature 55 DEG C~
70 DEG C, crystallization terminal solid-liquid ratio focuses on 1.90g/mL~2.00g/mL；After centrifugation dipotassium hydrogen phosphate crystal water sub-control system 5%~
10%；Vacuum degree control is -0.11MPa further preferably in step (3), and feed liquid crystallization temperature is 55 DEG C, crystallizes terminal feed liquid
Specific gravity is in 1.91g/mL；Dipotassium hydrogen phosphate crystal water sub-control system is 7% after centrifugation.
(4) two-part indirect heating dynamic is dry: control leading portion indirect heating drying temperature is at 150 DEG C~170 DEG C, back segment
Indirect heating drying temperature is at 120 DEG C~140 DEG C；
(5) cooling crushing and screening packaging.
The present invention has rational design, belongs to continuous production processes, high production efficiency.Anhydrous potassium dihydrogen phosphate phase is produced with spray-on process
Than this system is produced by way of crystallizing with indirect heating, the generation of dust is greatly reduced, product purity has larger amplitude
The raising of degree, heap density significantly increase, and pyrophosphate or metaphosphate are free of in product, while energy consumption is also greatly reduced.
Detailed description of the invention
Fig. 1 is present system structural schematic diagram.
Specific embodiment is below with reference to embodiment the present invention will be further explained explanation, but protection model of the invention
It encloses and is not limited to that.
Embodiment 1
First 6 tons of 48% potassium hydroxide is added in neutralization reaction kettle, 2.9 ton 85% of phosphoric acid is added under stiring and carries out
Reaction, regulation neutralizer pH value are 8.7, are maintained at 90 DEG C by slurry temperature after refined filtration equipment refined filtration, storage tank slurry is squeezed into
Evaporation concentration device is concentrated, and 70wt% is concentrated into；Then concentrate is squeezed into reduction vaporization crystallization apparatus and carries out crystallization behaviour
To make, vacuum degree is -0.11MPa, and crystallization temperature is 55 DEG C, and crystallization terminal feed liquid specific gravity is 1.91 g/mL, after centrifugal treating, from
For dipotassium hydrogen phosphate crystal water sub-control system 7%, filtrate returns to evaporation concentration device after the heart, and dipotassium hydrogen phosphate crystal enters two sections
Formula indirect heating dynamic drying oven is dried, and leading portion indirect heating drying temperature is 155 DEG C, and back segment indirect heating is dry
Temperature is 125 DEG C；Finished product is packaged into after cooling crushing and screening again.The product dipotassium hydrogen phosphate content is detected 100.2%,
It is not detected pyrophosphate and metaphosphate, product heap density 0.78g/mL, sodium 396.24ppm, iron 0.83ppm, calcium 0.43ppm,
Magnesium 0.26ppm, aluminium 0.22ppm, sulfate radical are not detected, chloride ion 8ppm.
Embodiment 2
First 6 tons of 48% potassium hydroxide is added in neutralization reaction kettle, 2.9 ton 85% of phosphoric acid is added under stiring and carries out
Reaction, regulation neutralizer pH value are 8.9, are maintained at 95 DEG C by slurry temperature after refined filtration equipment refined filtration, storage tank slurry is squeezed into
Evaporation concentration device is concentrated, and 71wt% is concentrated into；Then concentrate is squeezed into reduction vaporization crystallization apparatus and carries out crystallization behaviour
To make, vacuum degree is -0.10MPa, and crystallization temperature is 60 DEG C, and crystallization terminal feed liquid specific gravity is 1.92 g/mL, after centrifugal treating, from
For dipotassium hydrogen phosphate crystal water sub-control system 10%, filtrate returns to evaporation concentration device after the heart, and dipotassium hydrogen phosphate crystal enters two sections
Formula indirect heating dynamic drying oven is dried, and leading portion indirect heating drying temperature is 160 DEG C, and back segment indirect heating is dry
Temperature is 130 DEG C；Finished product is packaged into after cooling crushing and screening again.The product dipotassium hydrogen phosphate content is detected 100.1%,
It is not detected pyrophosphate and metaphosphate, product heap density 0.77g/mL, sodium 402.37ppm, iron 0.86ppm, calcium 0.48ppm,
Magnesium 0.32ppm, aluminium 0.26ppm, sulfate radical are not detected, chloride ion 9ppm.
Embodiment 3
First 6 tons of 48% potassium hydroxide is added in neutralization reaction kettle, 2.9 ton 85% of phosphoric acid is added under stiring and carries out
Reaction, regulation neutralizer pH value are 9.2, are maintained at 100 DEG C by slurry temperature after refined filtration equipment refined filtration, storage tank slurry is squeezed into
Evaporation concentration device is concentrated, and 71wt% is concentrated into；Then concentrate is squeezed into reduction vaporization crystallization apparatus and carries out crystallization behaviour
To make, vacuum degree is -0.09MPa, and crystallization temperature is 65 DEG C, and crystallization terminal feed liquid specific gravity is 1.94 g/mL, after centrifugal treating, from
For dipotassium hydrogen phosphate crystal water sub-control system 5%, filtrate returns to evaporation concentration device after the heart, and dipotassium hydrogen phosphate crystal enters two sections
Formula indirect heating dynamic drying oven is dried, and leading portion indirect heating drying temperature is 165 DEG C, and back segment indirect heating is dry
Temperature is 135 DEG C；Finished product is packaged into after cooling crushing and screening again.The product dipotassium hydrogen phosphate content is detected 100.1%,
It is not detected pyrophosphate and metaphosphate, product heap density 0.76g/mL, sodium 405.75ppm, iron 0.94ppm, calcium 0.52ppm,
Magnesium 0.36ppm, aluminium 0.31ppm, sulfate radical are not detected, chloride ion 10ppm.
Embodiment 4
First 6 tons of 48% potassium hydroxide is added in neutralization reaction kettle, 2.9 ton 85% of phosphoric acid is added under stiring and carries out
Reaction, regulation neutralizer pH value are 9.4, are maintained at 95 DEG C by slurry temperature after refined filtration equipment refined filtration, storage tank slurry is squeezed into
Evaporation concentration device is concentrated, and 70wt% is concentrated into；Then concentrate is squeezed into reduction vaporization crystallization apparatus and carries out crystallization behaviour
To make, vacuum degree is -0.10MPa, and crystallization temperature is 60 DEG C, and crystallization terminal feed liquid specific gravity is 1.91 g/mL, after centrifugal treating, from
For dipotassium hydrogen phosphate crystal water sub-control system 8%, filtrate returns to evaporation concentration device after the heart, and dipotassium hydrogen phosphate crystal enters two sections
Formula indirect heating dynamic drying oven is dried, and leading portion indirect heating drying temperature is 160 DEG C, and back segment indirect heating is dry
Temperature is 130 DEG C；Finished product is packaged into after cooling crushing and screening again.The product dipotassium hydrogen phosphate content is detected 100.1%,
It is not detected pyrophosphate and metaphosphate, product heap density 0.78g/mL, sodium 396.18ppm, iron 0.88ppm, calcium 0.46ppm,
Magnesium 0.28ppm, aluminium 0.16ppm, sulfate radical are not detected, chloride ion 8ppm.
Claims (3)
1. a kind of without burnt high-pure anhydrous dipotassium hydrogen phosphate production technology, which is characterized in that
(1) neutralization reaction: using 85% phosphoric acid and 48% alkali potassium as raw material, carry out neutralization reaction in a kettle, control material
PH value is starched between 8.6~9.4, after fine filter filters, slurry storage tank is squeezed into, maintains storage tank slurry temperature 85 DEG C~105
DEG C range；
(2) it is concentrated by evaporation: the slurry in slurry storage tank being squeezed into evaporation concentration device and is concentrated, control concentrate concentration exists
70wt% range；
(3) crystallization is evaporated under reduced pressure: the slurry after concentration is subjected to reduction vaporization crystallization, control vacuum degree in -0.11MPa range,
Feed liquid crystallization temperature is 55 DEG C, and crystallization terminal solid-liquid ratio focuses on 1.91g/mL；Dipotassium hydrogen phosphate crystal water sub-control system exists after centrifugation
7%；
(4) two-part indirect heating dynamic is dry: it is dry that the progress two-part indirect heating dynamic of the slurry after crystallizing will be evaporated under reduced pressure
It is dry, while controlling leading portion indirect heating drying temperature at 150 DEG C~170 DEG C, back segment indirect heating drying temperature 120 DEG C~
140℃；
(5) cooling crushing and screening packaging after drying.
2. a kind of without burnt high-pure anhydrous dipotassium hydrogen phosphate production system, which is characterized in that phosphoric acid storage tank and potassium hydroxide storage tank point
It is not connect with phosphoric acid head tank and potassium hydroxide head tank, phosphoric acid head tank and potassium hydroxide head tank and neutralization reaction kettle connect
It connects, neutralization reaction kettle is connect with fine filter, and fine filter is connect with slurry storage tank, and slurry storage tank is connect with evaporation concentrator, evaporation
Inspissator is connect with crystallizer is evaporated under reduced pressure, and crystallizer is evaporated under reduced pressure and connect with centrifuge, centrifuge and two-part indirect heating
The connection of dynamic drying oven, two-part indirect heating dynamic drying oven are connect with cooling furnace, and cooling furnace is connect with crushing and screening
Form the production system without burnt high-pure anhydrous dipotassium hydrogen phosphate.
3. as claimed in claim 2 without burnt high-pure anhydrous dipotassium hydrogen phosphate production system, which is characterized in that centrifuge also with evaporation
Inspissator connection.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610672471.6A CN106241766B (en) | 2016-08-16 | 2016-08-16 | It is a kind of without burnt high-pure anhydrous dipotassium hydrogen phosphate production system and technique |
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| CN201610672471.6A CN106241766B (en) | 2016-08-16 | 2016-08-16 | It is a kind of without burnt high-pure anhydrous dipotassium hydrogen phosphate production system and technique |
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| CN107151005B (en) * | 2017-07-19 | 2019-05-21 | 江苏科伦多食品配料有限公司 | A kind of preparation facilities and preparation method of high density anhydrous potassium dihydrogen phosphate |
| CN108264030B (en) * | 2018-03-16 | 2021-04-20 | 连云港西都食品配料有限公司 | Preparation method of food-grade dipotassium hydrogen phosphate |
| CN110482510A (en) * | 2019-09-20 | 2019-11-22 | 瓮福达州化工有限责任公司 | A kind of preparation process of food grade phosphoric acid hydrogen dipotassium |
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| CN102167298B (en) * | 2010-12-29 | 2012-08-29 | 武汉同源药业有限公司 | Preparation method of high-purity dipotassium phosphate crude drug |
| CN102101663A (en) * | 2011-04-06 | 2011-06-22 | 襄樊巨力化工实业有限公司 | Method for preparing food-grade low-water insoluble disodium dihydrogen pyrophosphate |
| CN102249204A (en) * | 2011-06-15 | 2011-11-23 | 安徽恒星制药有限公司 | Method for preparing dipotassium phosphate |
| CN102862964B (en) * | 2012-09-08 | 2014-07-23 | 湖北三宁化工股份有限公司 | Device and method for producing monopotassium phosphate by using double decomposition |
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Effective date of registration: 20190704 Address after: 443007 No. 66-6 Gongting Avenue, Gongting District, Yichang City, Hubei Province Patentee after: HUBEI XINGFA PHOSPHORUS CHEMICAL INDUSTRY RESEARCH INSTITUTE CO., LTD. Address before: 443711 Hunan Road, Gufu Town, Xingshan County, Yichang City, Hubei Province Patentee before: Hubei Xingfa Chemical Group Corp., Ltd. |
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