CN106241766A - A kind of without burnt high-pure anhydrous dipotassium hydrogen phosphate production system and technique - Google Patents
A kind of without burnt high-pure anhydrous dipotassium hydrogen phosphate production system and technique Download PDFInfo
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- CN106241766A CN106241766A CN201610672471.6A CN201610672471A CN106241766A CN 106241766 A CN106241766 A CN 106241766A CN 201610672471 A CN201610672471 A CN 201610672471A CN 106241766 A CN106241766 A CN 106241766A
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- hydrogen phosphate
- dipotassium hydrogen
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- phosphoric 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
- C01B25/30—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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- 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
- C01P2006/10—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
The invention discloses a kind of without burnt high-pure anhydrous dipotassium hydrogen phosphate production system and technique, the aspects such as without burnt high-purity major embodiment in the product without pyrophosphate or metaphosphate, other impurity contained is few, and dipotassium hydrogen phosphate content is high.Present system includes phosphoric acid, the potassium hydroxide storage tank being sequentially connected with, phosphoric acid, potassium hydroxide head tank, neutralizes reactor, fine filter, slip storage tank, evaporation concentration device, crystallization apparatus, centrifuge, conveyer device are evaporated under reduced pressure, two-part heats dynamic drying oven device indirectly, conveyer device, cools down furnace apparatus, conveyer device, pulverizing-screening system, packaging system.The present invention is reasonable in design, belongs to continuous production processes, and production efficiency is high.Compared with producing ADKP with nebulization, native system uses the mode of crystallization and heating indirectly to produce, and the generation of dust is greatly reduced, and product purity has had lifting by a relatively large margin, and without pyrophosphate or metaphosphate in product, energy consumption is also greatly reduced simultaneously.
Description
Technical field
The invention belongs to ADKP production technical field, be specifically related to a kind of without burnt high-pure anhydrous phosphoric acid hydrogen two
Potassium production system and technique.
Background technology
Dipotassium hydrogen phosphate is mainly used in medicine, fermentation, and antibacterial culturing and produce potassium pyrophosphate etc. is commonly used for analytical reagent,
Buffer agent and water quality treatment agent, in food industry for preparing the raw material of wheaten food aqueous alkali, fermentation agent, flavoring agent, swollen
Pine agent, the gentle alkaline agent of milk product, yeast food, as quality improver.
Current domestic ADKP uses spray drying method production technology substantially, and production scene dust is more, warp
Product bulk density after atomization is less, and substantially at about 0.4g/mL～0.5g/mL, dust recovery rate is relatively low, and most employing sky
So the clean energy resource such as gas or hydrogen is fuel, and energy consumption is relatively large, and production cost is of a relatively high, this anhydrous phosphorus of production technology gained
Acid hydrogen dipotassium product content is relatively low, substantially 98%～about 99.5%, is often detected the pyrophosphoric acid containing 1%～3%
Salt and metaphosphate, in product, the elementary metal impurities such as sodium calcium and magnesium ferro-aluminum is of a relatively high, sodium ion substantially at 3000ppm～
About 5000ppm, calcium and magnesium aluminium ion substantially at about 5ppm～25ppm, iron ion substantially at about 5ppm～40ppm, chlorine from
Son is substantially at about 20ppm～60ppm, and sulfate radical is at about 40ppm～100ppm.
Summary of the invention
It is an object of the invention to provide a kind of without burnt high-pure anhydrous dipotassium hydrogen phosphate production system, provide to utilize simultaneously and be somebody's turn to do
System produces the production technology without burnt high-pure anhydrous dipotassium hydrogen phosphate.
For achieving the above object, the present invention adopts the following technical scheme that
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 head tank
And potassium hydroxide head tank connects, phosphoric acid head tank and potassium hydroxide head tank are connected with neutralizing reactor, neutralization reactor and
Fine filter connects, and fine filter is connected with slip storage tank, and slip storage tank is connected with evaporation concentrator, evaporation concentrator and reduction vaporization
Crystallizer connects, and crystallizer is evaporated under reduced pressure and is connected with centrifuge, and centrifuge indirectly heats dynamic drying oven and is connected with two-part, and two
Segmentation indirectly heats dynamic drying oven and is connected with cooling stove, and cooling stove is connected with crushing and screening, can be formed without burnt high-pure anhydrous
The process units of dipotassium hydrogen phosphate.Described centrifuge is also connected with evaporation concentrator.
Utilize above-mentioned production system to produce the technique without burnt high-pure anhydrous dipotassium hydrogen phosphate, comprise the following steps:
(1) neutralize reaction: phosphoric acid with 85% and the alkali potassium of 48%, as raw material, are neutralized reaction in a kettle., control to expect
Slurry pH value is between 8.6～9.4, after fine filter filters, squeezes into slip storage tank, maintains storage tank slurry temperature at 85 DEG C～105
DEG C scope；
(2) evaporation and concentration: storage tank slip is squeezed into evaporation concentration device and concentrates, controls concentrated solution concentration
In 69wt%～72wt% scope；More preferably evaporation and concentration to urine concentration is 70wt%；
(3) be evaporated under reduced pressure crystallization: control vacuum in-0.08 MPa～-0.12MPa scope, feed temperature at 55 DEG C～70 DEG C,
Crystallization terminal solid-liquid ratio focuses on 1.90g/mL～2.00g/mL；After centrifugal, dipotassium hydrogen phosphate crystal moisture Control is 5%～10%；Enter
It is-0.11MPa that one step is preferably vacuum degree control in step (3), and feed liquid crystallization temperature is 55 DEG C, and crystallization terminal solid-liquid ratio focuses on
1.91g/mL；After centrifugal, dipotassium hydrogen phosphate crystal moisture Control is 7%.
(4) two-part indirectly heats and is dynamically dried: control leading portion indirect heat drying temperature at 150 DEG C～170 DEG C, back segment
Heat drying temperature is at 120 DEG C～140 DEG C indirectly；
(5) cooling crushing and screening packaging.
The present invention is reasonable in design, belongs to continuous production processes, and production efficiency is high.ADKP phase is produced with nebulization
Ratio, native system produces by the way of crystallization and indirect heating, the generation of dust is greatly reduced, and product purity has had larger amplitude
The raising of degree, bulk density significantly increases, and without pyrophosphate or metaphosphate in product, energy consumption is also greatly reduced simultaneously.
Accompanying drawing explanation
Fig. 1 is present system structural representation.
Detailed description of the invention is below in conjunction with embodiment the present invention will be further explained explanation, but the protection model of the present invention
Enclose and be not limited to that.
Embodiment 1
First by the potassium hydroxide addition neutralization reactor of the 48% of 6 tons, under agitation the phosphoric acid of addition 2.9 ton 85% is carried out instead
Should, regulation and control neutralizer pH value is 8.7, is maintained at 90 DEG C by slurry temperature after fine straining equipment fine straining, storage tank slip is squeezed into steaming
Send out enrichment facility to concentrate, be concentrated into 70wt%；Then concentrated solution is squeezed into reduction vaporization crystallization apparatus and carries out crystallization operation,
Vacuum is-0.11MPa, and crystallization temperature is 55 DEG C, and crystallization terminal feed liquid proportion is 1.91 g/mL, after centrifugal treating, after being centrifuged
Dipotassium hydrogen phosphate crystal moisture Control is 7%, and filtrate returns to evaporation concentration device, and dipotassium hydrogen phosphate crystal enters between two-part
Connecing the dynamic drying oven of heating and be dried process, leading portion indirect heat drying temperature is 155 DEG C, back segment indirect heat drying temperature
It it is 125 DEG C；It is packaged into finished product after the most cooled crushing and screening.This product dipotassium hydrogen phosphate content is 100.2% after testing, does not examines
Go out pyrophosphate and metaphosphate, product bulk density 0.78g/mL, sodium 396.24ppm, ferrum 0.83ppm, calcium 0.43ppm, magnesium
0.26ppm, aluminum 0.22ppm, sulfate radical does not detects, chloride ion 8ppm.
Embodiment 2
First by the potassium hydroxide addition neutralization reactor of the 48% of 6 tons, under agitation the phosphoric acid of addition 2.9 ton 85% is carried out instead
Should, regulation and control neutralizer pH value is 8.9, is maintained at 95 DEG C by slurry temperature after fine straining equipment fine straining, storage tank slip is squeezed into steaming
Send out enrichment facility to concentrate, be concentrated into 71wt%；Then concentrated solution is squeezed into reduction vaporization crystallization apparatus and carries out crystallization operation,
Vacuum is-0.10MPa, and crystallization temperature is 60 DEG C, and crystallization terminal feed liquid proportion is 1.92 g/mL, after centrifugal treating, after being centrifuged
Dipotassium hydrogen phosphate crystal moisture Control is 10%, and filtrate returns to evaporation concentration device, and dipotassium hydrogen phosphate crystal enters between two-part
Connecing the dynamic drying oven of heating and be dried process, leading portion indirect heat drying temperature is 160 DEG C, back segment indirect heat drying temperature
It it is 130 DEG C；It is packaged into finished product after the most cooled crushing and screening.This product dipotassium hydrogen phosphate content is 100.1% after testing, does not examines
Go out pyrophosphate and metaphosphate, product bulk density 0.77g/mL, sodium 402.37ppm, ferrum 0.86ppm, calcium 0.48ppm, magnesium
0.32ppm, aluminum 0.26ppm, sulfate radical does not detects, chloride ion 9ppm.
Embodiment 3
First by the potassium hydroxide addition neutralization reactor of the 48% of 6 tons, under agitation the phosphoric acid of addition 2.9 ton 85% is carried out instead
Should, regulation and control neutralizer pH value is 9.2, is maintained at 100 DEG C by slurry temperature after fine straining equipment fine straining, storage tank slip is squeezed into steaming
Send out enrichment facility to concentrate, be concentrated into 71wt%；Then concentrated solution is squeezed into reduction vaporization crystallization apparatus and carries out crystallization operation,
Vacuum is-0.09MPa, and crystallization temperature is 65 DEG C, and crystallization terminal feed liquid proportion is 1.94 g/mL, after centrifugal treating, after being centrifuged
Dipotassium hydrogen phosphate crystal moisture Control is 5%, and filtrate returns to evaporation concentration device, and dipotassium hydrogen phosphate crystal enters between two-part
Connecing the dynamic drying oven of heating and be dried process, leading portion indirect heat drying temperature is 165 DEG C, back segment indirect heat drying temperature
It it is 135 DEG C；It is packaged into finished product after the most cooled crushing and screening.This product dipotassium hydrogen phosphate content is 100.1% after testing, does not examines
Go out pyrophosphate and metaphosphate, product bulk density 0.76g/mL, sodium 405.75ppm, ferrum 0.94ppm, calcium 0.52ppm, magnesium
0.36ppm, aluminum 0.31ppm, sulfate radical does not detects, chloride ion 10ppm.
Embodiment 4
First by the potassium hydroxide addition neutralization reactor of the 48% of 6 tons, under agitation the phosphoric acid of addition 2.9 ton 85% is carried out instead
Should, regulation and control neutralizer pH value is 9.4, is maintained at 95 DEG C by slurry temperature after fine straining equipment fine straining, storage tank slip is squeezed into steaming
Send out enrichment facility to concentrate, be concentrated into 70wt%；Then concentrated solution is squeezed into reduction vaporization crystallization apparatus and carries out crystallization operation,
Vacuum is-0.10MPa, and crystallization temperature is 60 DEG C, and crystallization terminal feed liquid proportion is 1.91 g/mL, after centrifugal treating, after being centrifuged
Dipotassium hydrogen phosphate crystal moisture Control is 8%, and filtrate returns to evaporation concentration device, and dipotassium hydrogen phosphate crystal enters between two-part
Connecing the dynamic drying oven of heating and be dried process, leading portion indirect heat drying temperature is 160 DEG C, back segment indirect heat drying temperature
It it is 130 DEG C；It is packaged into finished product after the most cooled crushing and screening.This product dipotassium hydrogen phosphate content is 100.1% after testing, does not examines
Go out pyrophosphate and metaphosphate, product bulk density 0.78g/mL, sodium 396.18ppm, ferrum 0.88ppm, calcium 0.46ppm, magnesium
0.28ppm, aluminum 0.16ppm, sulfate radical does not detects, chloride ion 8ppm.
Claims (5)
1. one kind without burnt high-pure anhydrous dipotassium hydrogen phosphate production technology, it is characterised in that
(1) neutralize reaction: phosphoric acid with 85% and the alkali potassium of 48%, as raw material, are neutralized reaction in a kettle., control to expect
Slurry pH value is between 8.6～9.4, after fine filter filters, squeezes into slip storage tank, maintains storage tank slurry temperature at 85 DEG C～105
DEG C scope；
(2) evaporation and concentration: the slip in slip storage tank is squeezed into evaporation concentration device and concentrates, controls concentrated solution concentration and exists
69wt%～72wt% scope；
(3) be evaporated under reduced pressure crystallization: will concentrate after slip carry out be evaporated under reduced pressure crystallization, control vacuum-0.08 MPa～-
0.12MPa scope, feed liquid crystallization temperature is 55 DEG C～70 DEG C, and crystallization terminal solid-liquid ratio focuses on 1.90g/mL～2.00g/mL；From
After the heart, dipotassium hydrogen phosphate crystal moisture Control is 5%～10%；
(4) two-part heats the driest indirectly: the slip after crystallization being evaporated under reduced pressure carries out two-part and indirectly heats the most dry
Dry, control leading portion indirect heat drying temperature at 150 DEG C～170 DEG C simultaneously, back segment indirect heat drying temperature at 120 DEG C～
140℃；
(5) dried cooling crushing and screening packaging.
2. described in claim 1 without burnt high-pure anhydrous dipotassium hydrogen phosphate production technology, it is characterised in that step
Suddenly, in (2), evaporation and concentration to feed concentration is 70wt%.
3. described in claim 1 without burnt high-pure anhydrous dipotassium hydrogen phosphate production technology, it is characterised in that vacuum in step (3)
Degree controls to be-0.11MPa, and feed liquid crystallization temperature is 55 DEG C, and crystallization terminal solid-liquid ratio focuses on 1.91g/mL；Phosphoric acid hydrogen two after centrifugal
Potassium crystal moisture Control is 7%.
4. one kind without burnt high-pure anhydrous dipotassium hydrogen phosphate production system, it is characterised in that phosphoric acid storage tank divides with potassium hydroxide storage tank
Not being connected with phosphoric acid head tank and potassium hydroxide head tank, phosphoric acid head tank and potassium hydroxide head tank connect with neutralizing reactor
Connecing, neutralize reactor and be connected with fine filter, fine filter is connected with slip storage tank, and slip storage tank is connected with evaporation concentrator, evaporation
Concentrator is connected with crystallizer is evaporated under reduced pressure, and crystallizer is evaporated under reduced pressure and is connected with centrifuge, and centrifuge heats indirectly with two-part
Dynamically drying oven connects, and two-part indirectly heats dynamic drying oven and is connected with cooling stove, and cooling stove is connected with crushing and screening,
Form the production system without burnt high-pure anhydrous dipotassium hydrogen phosphate.
5. described in claim 4 without burnt high-pure anhydrous dipotassium hydrogen phosphate production system, it is characterised in that centrifuge also with evaporation
Concentrator connects.
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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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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107151005A (en) * | 2017-07-19 | 2017-09-12 | 江苏科伦多食品配料有限公司 | The preparation facilities and preparation method of a kind of high density ADKP |
| CN108264030A (en) * | 2018-03-16 | 2018-07-10 | 连云港西都生化有限公司 | A kind of preparation method of food grade phosphoric acid hydrogen dipotassium |
| 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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| 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 |
| CN102167298A (en) * | 2010-12-29 | 2011-08-31 | 武汉同源药业有限公司 | Preparation method of high-purity dipotassium phosphate crude drug |
| CN102249204A (en) * | 2011-06-15 | 2011-11-23 | 安徽恒星制药有限公司 | Method for preparing dipotassium phosphate |
| CN102862964A (en) * | 2012-09-08 | 2013-01-09 | 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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Patent Citations (4)
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| CN102167298A (en) * | 2010-12-29 | 2011-08-31 | 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 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107151005A (en) * | 2017-07-19 | 2017-09-12 | 江苏科伦多食品配料有限公司 | The preparation facilities and preparation method of a kind of high density ADKP |
| 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 |
| CN108264030A (en) * | 2018-03-16 | 2018-07-10 | 连云港西都生化有限公司 | A kind of preparation method of food grade phosphoric acid hydrogen dipotassium |
| 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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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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