CN101759168B - Process for producing potassium phosphate with wet phosphoric acid - Google Patents
Process for producing potassium phosphate with wet phosphoric acid Download PDFInfo
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- CN101759168B CN101759168B CN2010100289367A CN201010028936A CN101759168B CN 101759168 B CN101759168 B CN 101759168B CN 2010100289367 A CN2010100289367 A CN 2010100289367A CN 201010028936 A CN201010028936 A CN 201010028936A CN 101759168 B CN101759168 B CN 101759168B
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- phosphoric acid
- potassium phosphate
- wet
- lead
- salt
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Abstract
The invention relates to a process for producing potassium phosphate with wet phosphoric acid. The process comprises the following steps that: 1) wet phosphoric acid is put into an ultrasonic reactor for ultrasonication at the temperature of 2-80 degree centigrade with the reaction time of 10-120 minutes; then the product is cooled to be at room temperature and precipitates are leached, thus obtaining a filter liquor; 2) potassium hydroxide, potassium carbonate or potassium bicarbonate is used to regulate the PH value of the filter liquor and generate precipitates, and a new filter liquor obtained after filtering is concentrated, evaporated, crystallized and then separated, thus obtaining potassium phosphate. The process is characterized in that wet phosphoric acid with low purity, purity and cost, lead-bearing material and potassium chloride are used as raw materials to react and generate potassium phosphate, which reduces production cost. Impurities in the raw materials interact and generate insoluble precipitates, and the insoluble precipitates can be easily separated. In the simple process, products are generated only by concentrating and crystallizing a neutralizer; potassium phosphate is directly prepared by utilizing phosphoric acid with the concentration of 5-40%, which solves the problems of low consistency of wet phosphoric acid and high energy consumption for concentration.
Description
Technical field
The present invention relates to a kind of technology with producing potassium phosphate with wet phosphoric acid.
Background technology
Domestic potassium phosphate salt adopt more thermal phosphoric acid or purification of phosphoric acid and Pottasium Hydroxide or salt of wormwood through neutralization, concentrate, crystallization makes, production cost is higher.Phosphoric acid by wet process and the Repone K lower with production cost replace thermal phosphoric acid to produce potassium phosphate salt, must carry out pre-treatment to phosphoric acid by wet process.Existing wet phosphoric acid purifying method such as solvent extration, ion exchange method, electroosmose process etc. all have shortcoming: facility investment is big; Operation is comparatively complicated; The purification cost is high.
Summary of the invention
Problem to be solved by this invention is to propose a kind of technology with producing potassium phosphate with wet phosphoric acid to above-mentioned prior art, and it utilizes lower concentration phosphoric acid by wet process direct production potassium phosphate salt, and technology is simple, need not purify and concentrate, and has reduced production cost.
The present invention by the problem of the above-mentioned proposition of solution the employing solution be: a kind of technology with producing potassium phosphate with wet phosphoric acid is characterized in that it comprises the steps:
1) phosphoric acid by wet process is added in the ultrasound reactor; By lead in phosphoric acid by wet process, the leaded thing and Repone K mol ratio is 2: 1: 1.8～2.5 reinforced, at 2～80 ℃ of following ultrasonication of temperature, reaction times 10～120min; Cool to room temperature elimination throw out obtains filtrating again;
2) with Pottasium Hydroxide, salt of wormwood or saleratus set-up procedure 1) gained filtrating pH=3.0～4.6 o'clock, produce deposition, filter and obtain filtrating, concentrate again, evaporative crystallization separates and obtain potassium phosphate salt, mother liquor is back to filter in the gained filtrating and reuses.
Press such scheme, described potassium phosphate salt is any one or multiple mixing in potassium primary phosphate, potassium phosphate,monobasic and the potassiumphosphate.
Press such scheme, described leaded thing is any one in lead ore, metallic lead, scrap lead cream and the lead salt.
Press such scheme, the P of described phosphoric acid by wet process
2O
5Mass percent concentration is 5～40%.
Press such scheme, the purity of described Repone K is technical grade or fertilizer grade.Repone K can add with solid form, also can aqueous solution form add.
Press such scheme, described Pottasium Hydroxide, salt of wormwood or saleratus purity are technical grades.Pottasium Hydroxide, salt of wormwood or saleratus can add with solid form, also can aqueous solution form add.
The present invention adopts metathesis process to produce potassium phosphate salt, can be with phosphoric acid by wet process, and P particularly
2O
5The phosphoric acid of (Vanadium Pentoxide in FLAKES) 5～40% concentration, leaded thing (lead ore, lead, scrap lead cream and lead salt), Repone K are raw material, directly change into potassium phosphate salt.Impurities in raw materials partly interacts and generates insoluble deposition, like PbCl
2, PbCO
3, CaF
2Etc. deposition.
The present invention has the following advantages:
1, can utilize purity low, phosphoric acid by wet process that concentration is low, cheap and leaded thing (lead ore, lead, scrap lead cream and lead salt) are that raw material reaction is produced potassium phosphate salt with Repone K, thereby reduce production costs;
2, impurities in raw materials partly interacts and generates insoluble deposition, easy-clear, and technology is simple, and neutralizer only needs condensing crystal promptly to get product simultaneously;
3, utilize the phosphoric acid of 5～40% concentration, the liquid phase that need not purify and concentrate, react concentrates and directly produces potassium phosphate salt, and it is low to have solved phosphoric acid by wet process concentration, concentrates the big problem of power consumption.
Embodiment
Below in conjunction with embodiment the present invention is described further, but can not be as to qualification of the present invention.
For a better understanding of the present invention, further illustrate content of the present invention, but content of the present invention not only is confined to following embodiment below in conjunction with embodiment.
Embodiment 1:
Phosphoric acid by wet process, lead ore and Repone K reacted potassium phosphate salt technology, it comprises the steps:
1. learn from else's experience and measure wherein P
2O
5Content is the phosphoric acid by wet process of 14.72% (mass percent); By plumbous in phosphoric acid by wet process, the lead ore, Repone K (technical grade) mol ratio be 2: 1: 2 reinforced, mixing liquid is put into ultrasound reactor, under 34～40 ℃ of temperature; Take out behind the reaction 40min; Cool to room temperature elimination throw out adds Pottasium Hydroxide regulation and control pH=4.59, produces Al (OH)
3And CaHPO
4Insoluble throw out, the elimination throw out.
2. filtrating is carried out evaporative crystallization.After solution reaches capacity, 40 ℃ Crystallization Separation is obtained potassium phosphate salt in temperature, mother liquor is back to filter in the gained filtrating and reuses.
The phosphoric acid potassium salt product of gained, composition is: P
2O
5Content is 49.38% (mass percent), K
2O content is 34.22% (mass percent), Cl
-Content is 1.10% (mass percent).
Embodiment 2:
Phosphoric acid by wet process, scrap lead cream and Repone K reacted potassium phosphate salt technology, it comprises the steps:
1. learn from else's experience and measure wherein P
2O
5Content is the phosphoric acid by wet process of 10.54% (mass percent); By the lead in phosphoric acid by wet process, the scrap lead cream, Repone K (technical grade) mol ratio be 2: 1: 2 reinforced, mixing liquid is put into ultrasound reactor, under 2～4 ℃ of temperature; Take out cool to room temperature elimination throw out behind the reaction 40min.Add Pottasium Hydroxide regulation and control pH=4.23, produce Al (OH)
3And CaHPO
4Insoluble throw out, the elimination throw out.
2. filtrating is carried out evaporative crystallization.After solution reaches capacity, 40 ℃ Crystallization Separation is obtained potassium phosphate salt in temperature.Mother liquor is back to filter in the gained filtrating and reuses.
The phosphoric acid potassium salt product of gained, composition is: P
2O
5Content is 51.18% (mass percent), K
2O content is 31.82% (mass percent), Cl
-Content is 1.5% (mass percent).
Embodiment 3:
Phosphoric acid by wet process, plumbous oxide or plumbic oxide and Repone K reacted potassium phosphate salt technology, it comprises the steps:
1. learn from else's experience and measure wherein P
2O
5Content is the phosphoric acid by wet process of 14.72% (mass percent); By the lead in phosphoric acid by wet process, the plumbous oxide, Repone K (technical grade) mol ratio be 2: 1: 1.8 reinforced; Mixing liquid is put into ultrasound reactor; Under 26～30 ℃ of temperature, take out cool to room temperature elimination throw out behind the reaction 60min.Add Pottasium Hydroxide regulation and control pH=4.23, produce Al (OH)
3And CaHPO
4Insoluble throw out, the elimination throw out.
2. filtrating is carried out evaporative crystallization.After solution reaches capacity, 40 ℃ Crystallization Separation is obtained potassium phosphate salt in temperature.Mother liquor is back to filter in the gained filtrating and reuses.
The phosphoric acid potassium salt product of gained, composition is: P
2O
5Content is 51.14% (mass percent), K
2O content is 32.23% (mass percent), Cl
-Content is 1.25% (mass percent).
Embodiment 4:
Phosphoric acid by wet process, lead salt and Repone K reacted potassium phosphate salt technology, it comprises the steps:
1. learn from else's experience and measure wherein P
2O
5Content is the phosphoric acid by wet process of 14.72% (mass percent), presses phosphoric acid by wet process, PbSO
4In lead, Repone K (technical grade) mol ratio be 2: 1: 2.4 reinforced, mixing liquid is put into ultrasound reactor, under 60～65 ℃ of temperature, take out cool to room temperature elimination throw out behind the reaction 110min.Add Pottasium Hydroxide regulation and control pH=4.23, produce Al (OH)
3And CaHPO
4Insoluble throw out, the elimination throw out.
2. filtrating is carried out evaporative crystallization.After solution reaches capacity, 40 ℃ Crystallization Separation is obtained potassium phosphate salt in temperature.Mother liquor is back to filter in the gained filtrating and reuses.
The phosphoric acid potassium salt product of gained, composition is: P
2O
5Content is 52.09% (mass percent), K
2O content is 31.15% (mass percent), Cl
-Content is 1.32% (mass percent).
Each cited raw material of the present invention can both be realized the present invention; And the bound value of each raw material, interval value can both realize the present invention; The bound value and the interval value of processing parameter of the present invention (like time, temperature, frequency, pH value etc.) can both be realized the present invention, do not enumerate embodiment one by one at this.
Claims (5)
1. the technology with producing potassium phosphate with wet phosphoric acid is characterized in that it comprises the steps:
1) phosphoric acid by wet process is added in the ultrasound reactor; By lead in phosphoric acid by wet process, the leaded thing and Repone K mol ratio is 2: 1: 1.8～2.5 reinforced; At 2～80 ℃ of following ultrasonication of temperature, reaction times 10～120min, cool to room temperature elimination throw out again; Obtain filtrating, described leaded thing is any one in lead ore, metallic lead, scrap lead cream and the lead salt;
2) with Pottasium Hydroxide, salt of wormwood or saleratus set-up procedure 1) gained filtrating pH=3.0～4.6 o'clock, produce deposition, filter and obtain filtrating, concentrate again, evaporative crystallization separates and obtain potassium phosphate salt, mother liquor is back to filter in the gained filtrating and reuses.
2. by the described technology of claim 1, it is characterized in that described potassium phosphate salt is any one or multiple mixing in potassium primary phosphate, potassium phosphate,monobasic and the potassiumphosphate with producing potassium phosphate with wet phosphoric acid.
3. by claim 1 or 2 described technologies, it is characterized in that the P of described phosphoric acid by wet process with producing potassium phosphate with wet phosphoric acid
2O
5Mass percent concentration is 5～40%.
4. by claim 1 or 2 described technologies with producing potassium phosphate with wet phosphoric acid, the purity that it is characterized in that described Repone K is technical grade or fertilizer grade.
5. by claim 1 or 2 described technologies, it is characterized in that described Pottasium Hydroxide, salt of wormwood or saleratus purity are technical grades with producing potassium phosphate with wet phosphoric acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010100289367A CN101759168B (en) | 2010-01-08 | 2010-01-08 | Process for producing potassium phosphate with wet phosphoric acid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010100289367A CN101759168B (en) | 2010-01-08 | 2010-01-08 | Process for producing potassium phosphate with wet phosphoric acid |
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| Publication Number | Publication Date |
|---|---|
| CN101759168A CN101759168A (en) | 2010-06-30 |
| CN101759168B true CN101759168B (en) | 2012-05-30 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010100289367A Expired - Fee Related CN101759168B (en) | 2010-01-08 | 2010-01-08 | Process for producing potassium phosphate with wet phosphoric acid |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102864303B (en) * | 2012-09-25 | 2014-04-09 | 武汉工程大学 | Method for leaching potassium in phosphorus potassium associated ore at low temperature by assisting with microwaves/ultrasonic waves |
| CN103072963B (en) * | 2012-12-28 | 2014-11-05 | 金正大生态工程集团股份有限公司 | Method for producing potassium dihydrogen phosphate through wet-process phosphoric acid |
| CN103738931A (en) * | 2013-11-26 | 2014-04-23 | 瓮福（集团）有限责任公司 | Method for production of potassium dihydrogen phosphate from phosphorus-containing acidic wastewater |
| CN103879980B (en) * | 2014-03-19 | 2016-02-17 | 钟林 | The method of potassium primary phosphate is produced with calcium hydrophosphate fodder |
| CN105217591B (en) * | 2015-09-22 | 2017-06-13 | 贵州开磷集团股份有限公司 | A kind of phosphoric acid by wet process prepares tripotassium phosphate method |
| CN107311134A (en) * | 2017-07-18 | 2017-11-03 | 禄丰天宝磷化工有限公司 | A kind of phosphoric acid method produces the production technology of feed grade potassium dihydrogen phosphate |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RO98062B1 (en) * | 1987-07-20 | 1989-10-30 | îNTREPRINDEREA CHIMICA "DUDESTI" | Process for obtaining reactive quality monopotassium phosphate with a reduced fluorine content |
| CN1008080B (en) * | 1986-02-21 | 1990-05-23 | 沈阳复合肥料技术开发公司 | Process for preparing dihydropotassium phosphate |
| CN1565963A (en) * | 2003-07-07 | 2005-01-19 | 绵阳市勤生技术开发有限公司 | Joint production process for potassium dihydrogen phosphate, sulphur group compound fertilizer and polyaluminium chloride |
| CN1830762A (en) * | 2006-03-30 | 2006-09-13 | 云南省化工研究院 | Method of continuously preparing potassium dihydrogen phosphate |
-
2010
- 2010-01-08 CN CN2010100289367A patent/CN101759168B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1008080B (en) * | 1986-02-21 | 1990-05-23 | 沈阳复合肥料技术开发公司 | Process for preparing dihydropotassium phosphate |
| RO98062B1 (en) * | 1987-07-20 | 1989-10-30 | îNTREPRINDEREA CHIMICA "DUDESTI" | Process for obtaining reactive quality monopotassium phosphate with a reduced fluorine content |
| CN1565963A (en) * | 2003-07-07 | 2005-01-19 | 绵阳市勤生技术开发有限公司 | Joint production process for potassium dihydrogen phosphate, sulphur group compound fertilizer and polyaluminium chloride |
| CN1830762A (en) * | 2006-03-30 | 2006-09-13 | 云南省化工研究院 | Method of continuously preparing potassium dihydrogen phosphate |
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|---|---|
| CN101759168A (en) | 2010-06-30 |
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Application publication date: 20100630 Assignee: Hubei Zhongning Chemical Co. Ltd. Assignor: Wuhan Institute of Technology Contract record no.: 2014420000144 Denomination of invention: Process for producing potassium phosphate with wet phosphoric acid Granted publication date: 20120530 License type: Exclusive License Record date: 20140716 |
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