CN103787292A - Method for preparing agricultural monopotassium phosphate by taking pretreatment acid as raw material - Google Patents
Method for preparing agricultural monopotassium phosphate by taking pretreatment acid as raw material Download PDFInfo
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- CN103787292A CN103787292A CN201410021745.6A CN201410021745A CN103787292A CN 103787292 A CN103787292 A CN 103787292A CN 201410021745 A CN201410021745 A CN 201410021745A CN 103787292 A CN103787292 A CN 103787292A
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Abstract
The invention discloses a method for preparing agricultural monopotassium phosphate by taking pretreatment acid as a raw material, belonging to the field of phosphorus chemical industry. The method comprises the following steps: uniformly mixing the pretreatment acid, water and industrial potassium chloride; adding epoxy chloropropane for reacting fully, and separating an organic phase from a water phase, wherein the temperature of the water phase is 80-120 DEG C; adding potassium-containing alkali into the water phase to adjust the pH value to 4.8-6.0, and filtering to obtain a solid phase and a water phase; adding industrial phosphoric acid into the water phase to adjust the pH value to 4.4-4.7; cooling to the room temperature for crystalizing; filtering to obtain a solid product, namely, monopotassium phosphate.
Description
Technical field
The present invention relates to phosphorous chemical industry field, relate in particular to a kind of method of preparing agricultural potassium primary phosphate take pre-treatment acid as raw material.
Background technology
Pre-treatment acid is the upstream raw material of extraction process manufacture phosphoric acid, and compared with industrial phosphoric acid, pre-treatment acid concentration is lower, and concentration impurity ion is higher, low many of price.
Potassium primary phosphate is due to its good chemical property, and purposes is very extensive.Industrial as buffer reagent, casate, the raw material of potassium metaphosphate processed, the nutrient chemical of brewer's yeast, reinforcer, raising agent, fermentation assistant etc.; In agricultural, as efficient phosphorus potassium complex fertilizer, be widely used in the almost crop of all types such as all types of cash crop, grain, melon and fruit, vegetables.
Potassium primary phosphate is the king of potash fertilizer, and the utilization ratio of its effective constituent almost can reach 100%, has the dual function of phosphate fertilizer and potash fertilizer concurrently, and effect of increasing production is surprising, and application of phosphoric acid potassium dihydrogen can drop into less fecund and go out.
The preparation method of potassium primary phosphate mainly contains several as follows at present: neutralisation, extraction process, direct method and double decomposition.Neutralisation produce potassium primary phosphate be industrialization the earliest, the widest production technique of range of application of production technique is the simplest, environmental pollution is less a kind of maturation.
The main raw material of neutralisation is industrial phosphoric acid and potassium hydroxide, and therefore process costs is higher.Patent (publication number is: CN102936007A) has been reported a kind of method for production of phosphate salt, the method has realized the object with metal-salt hydrochlorate alternative metals oxide compound, carbonate or oxyhydroxide in phosphate production, effectively reduce the raw materials cost of phosphate production, but when the method is applied to pre-treatment acid, because iron ion content in pre-treatment acid is higher, causing the potassium dihydrogen phosphate crystal crystallization obtaining is needle-like, crystal water ratio is too high, thereby makes in potassium dihydrogen phosphate crystal chloride ion content too high.
By to the consulting of domestic and international patent and the publication published, do not find take pre-treatment acid as raw material, use the method for patent (publication number is: CN102936007A) report to prepare the relevant report of potassium primary phosphate technique.
Summary of the invention
The object of this invention is to provide a kind of method of preparing agricultural potassium primary phosphate take pre-treatment acid as raw material.
The method is mainly for pre-treatment acid, and take the pre-treatment acid of Wengfu group as example, this pre-treatment acid main component is phosphoric acid, its quality percentage composition 70%-80%, iron ion quality percentage composition 0.01%-1%.The technical scheme that realizes technical purpose of the present invention is as follows:
Pre-treatment acid, water are mixed with industrial potassium chloride, after adding epichlorohydrin reaction fully, separate organic phase and water, water temperature is at 80 ~ 120 ℃, then regulate pH value to 4.8-6.0 to adding in water containing the alkali of potassium, filter to obtain solid phase and water, in water, add industrial phosphoric acid to regulate pH value to 4.4 ~ 4.7 again, and be cooled to crystallizing at room temperature, after filtering, gained solid phase prod is potassium dihydrogen phosphate product.
The described alkali containing potassium is the one of potassium hydroxide, salt of wormwood and saleratus.
Described pre-treatment acid, its phosphoric acid quality percentage composition is 70% ~ 80%, iron ion quality percentage composition is 0.01 ~ 1%.
Beneficial effect of the present invention is: the concentration that has reduced iron ion in technique, eliminate the impact of iron ion on potassium primary phosphate crystallisation process, realize the object of preparing potassium primary phosphate take pre-treatment acid as raw material, greatly reduced the production cost of potassium primary phosphate.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope picture of the prepared potassium dihydrogen phosphate crystal of the direct method that adopts patent (publication number is: CN102936007A) to report;
Fig. 2 is the scanning electron microscope picture of the potassium dihydrogen phosphate crystal prepared of the inventive method.
Embodiment
Below in conjunction with embodiment, the present invention will be further described in detail.
Embodiment 1:
Pre-treatment acid, water are mixed with industrial potassium chloride, after adding epichlorohydrin reaction fully, separate organic phase and water, water temperature is at 100 ℃, then in water, add the alkali adjusting pH value to 5.0 containing potassium, then filter to obtain solid phase and water, then in water, add industrial phosphoric acid to regulate pH value to 4.5, be then cooled to crystallizing at room temperature, after filtering, gained solid phase prod is potassium dihydrogen phosphate product.
Press such scheme, the described alkali containing potassium is potassium hydroxide, salt of wormwood and saleratus.
Press such scheme, described pre-treatment acid, its phosphorus acid content is 75%, iron ion content is 0.4%.
Now the chloride ion content in potassium dihydrogen phosphate product is 0.1%.
Embodiment 2:
Pre-treatment acid, water are mixed with industrial potassium chloride, after adding epichlorohydrin reaction fully, separate organic phase and water, water temperature is at 120 ℃, then in water, add the alkali adjusting pH value to 6.0 containing potassium, then filter to obtain solid phase and water, then in water, add industrial phosphoric acid to regulate pH value to 4.7, be then cooled to crystallizing at room temperature, after filtering, gained solid phase prod is potassium dihydrogen phosphate product.
Press such scheme, the described alkali containing potassium is salt of wormwood.
Press such scheme, described pre-treatment acid, its phosphorus acid content is 80%, iron ion content is 1%.
Now the chloride ion content in potassium dihydrogen phosphate product is 0.2%.
Embodiment 3:
Pre-treatment acid, water are mixed with industrial potassium chloride, after adding epichlorohydrin reaction fully, separate organic phase and water, water temperature is at 80 ℃, then in water, add the alkali adjusting pH value to 4.8 containing potassium, then filter to obtain solid phase and water, then in water, add industrial phosphoric acid to regulate pH value to 4.4, be then cooled to crystallizing at room temperature, after filtering, gained solid phase prod is potassium dihydrogen phosphate product.
Press such scheme, the described alkali containing potassium is potassium hydroxide.
Press such scheme, described pre-treatment acid, its phosphorus acid content is 70%, iron ion content is 0.01.
Now the chloride ion content in potassium dihydrogen phosphate product is 0.2%.
Embodiment 4:
Pre-treatment acid, water are mixed with industrial potassium chloride, after adding epichlorohydrin reaction fully, separate organic phase and water, water temperature is at 100 ℃, then in water, add the alkali adjusting pH value to 5.6 containing potassium, then filter to obtain solid phase and water, then in water, add industrial phosphoric acid to regulate pH value to 4.6, be then cooled to crystallizing at room temperature, after filtering, gained solid phase prod is potassium dihydrogen phosphate product.
Press such scheme, the described alkali containing potassium is potassium hydroxide, salt of wormwood and saleratus.
Press such scheme, described pre-treatment acid, its phosphorus acid content is 77.85%, iron ion content is 0.39%.
Now the chloride ion content in potassium dihydrogen phosphate product is 0.1%.
Claims (3)
1. prepare the method for agricultural potassium primary phosphate take pre-treatment acid as raw material for one kind, it is characterized in that the method is that pre-treatment acid, water are mixed with industrial potassium chloride, after adding epichlorohydrin reaction fully, separate organic phase and water, water temperature is between 80 ~ 120 ℃, then regulate pH value to 4.8-6.0 to adding in water containing the alkali of potassium, filter to obtain solid phase and water, in water, add industrial phosphoric acid to regulate pH value to 4.4 ~ 4.7 again, and be cooled to crystallizing at room temperature, after filtering, gained solid phase prod is potassium dihydrogen phosphate product.
2. the method for claim 1, is characterized in that the described alkali containing potassium is the one of potassium hydroxide, salt of wormwood and saleratus.
3. the method for claim 1, is characterized in that described pre-treatment acid, and its phosphorus acid content is 70% ~ 80%, and iron ion content is 0.01 ~ 1%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201410021745.6A CN103787292A (en) | 2014-01-17 | 2014-01-17 | Method for preparing agricultural monopotassium phosphate by taking pretreatment acid as raw material |
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| CN201410021745.6A CN103787292A (en) | 2014-01-17 | 2014-01-17 | Method for preparing agricultural monopotassium phosphate by taking pretreatment acid as raw material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114132908A (en) * | 2021-12-30 | 2022-03-04 | 贵州越都化工有限公司 | Process for producing potassium dihydrogen phosphate by extraction method |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4885148A (en) * | 1988-09-06 | 1989-12-05 | Phosphate Engineering & Construction Co., Inc. | Production of monobasic potassium phosphate with low chloride content from potassium chloride and phosphoric acid produced from the commercial wet process |
| CN101979311A (en) * | 2010-11-15 | 2011-02-23 | 中化重庆涪陵化工有限公司 | Method for producing industrial monopotassium phosphate and nitrogen, phosphorus and potassium compound fertilizer by using wet-process purified phosphoric acid as raw material through extraction |
| CN102602905A (en) * | 2012-03-16 | 2012-07-25 | 瓮福（集团）有限责任公司 | Method for producing monopotassium phosphate |
| CN102936007A (en) * | 2012-10-30 | 2013-02-20 | 武汉工程大学 | Preparation method of phosphate |
| CN103072963A (en) * | 2012-12-28 | 2013-05-01 | 山东金正大生态工程股份有限公司 | Method for producing potassium dihydrogen phosphate through wet-process phosphoric acid |
-
2014
- 2014-01-17 CN CN201410021745.6A patent/CN103787292A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4885148A (en) * | 1988-09-06 | 1989-12-05 | Phosphate Engineering & Construction Co., Inc. | Production of monobasic potassium phosphate with low chloride content from potassium chloride and phosphoric acid produced from the commercial wet process |
| CN101979311A (en) * | 2010-11-15 | 2011-02-23 | 中化重庆涪陵化工有限公司 | Method for producing industrial monopotassium phosphate and nitrogen, phosphorus and potassium compound fertilizer by using wet-process purified phosphoric acid as raw material through extraction |
| CN102602905A (en) * | 2012-03-16 | 2012-07-25 | 瓮福（集团）有限责任公司 | Method for producing monopotassium phosphate |
| CN102936007A (en) * | 2012-10-30 | 2013-02-20 | 武汉工程大学 | Preparation method of phosphate |
| CN103072963A (en) * | 2012-12-28 | 2013-05-01 | 山东金正大生态工程股份有限公司 | Method for producing potassium dihydrogen phosphate through wet-process phosphoric acid |
Non-Patent Citations (1)
| Title |
|---|
| 蒋丽红等: ""湿法磷酸生产磷酸二氢钾杂质净化率研究"", 《化工矿物与加工》, no. 3, 31 March 2003 (2003-03-31), pages 10 - 12 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114132908A (en) * | 2021-12-30 | 2022-03-04 | 贵州越都化工有限公司 | Process for producing potassium dihydrogen phosphate by extraction method |
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Application publication date: 20140514 |