CN102303854A - Purification method of monopotassium phosphate - Google Patents
Purification method of monopotassium phosphate Download PDFInfo
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- CN102303854A CN102303854A CN201110214485A CN201110214485A CN102303854A CN 102303854 A CN102303854 A CN 102303854A CN 201110214485 A CN201110214485 A CN 201110214485A CN 201110214485 A CN201110214485 A CN 201110214485A CN 102303854 A CN102303854 A CN 102303854A
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Abstract
The invention discloses a purification method of monopotassium phosphate. According to the invention, industrial phosphoric acid is filtered by an SBA-15 molecular sieve chelate adsorbent to remove impurity ions and then reacts with potassium chloride, so that purified monopotassium phosphate is collected from reaction products; the main body content of monopotassium phosphate obtained by the purification method disclosed by the invention is larger than 99wt%, and the yield of monopotassium phosphate is more than 90%; and through analysis and detection, the contents of chlorides and metal impurity ions in the product meet the standard of medicinal monopotassium phosphate. In the invention, the SBA-15 molecular sieve is used as a carrier, and the prepared SBA-15 molecular sieve chelate adsorbent has strong adsorption capacity to the metal impurity ions in a raw material industrial phosphoric acid, thereby effectively removing the impurity ions therein; and the purification method has the advantages that reaction process operation is simple, cost is reduced, yield is improved and the obtained product is stable in quality, thus the purification method is suitable for industrial production.
Description
Technical field
The present invention relates to a kind of purification process of potassium primary phosphate.
Background technology
Potassium primary phosphate is a kind of broad-spectrum colourless or white band glossy trapezoid body inorganic salt, is applied to agricultural, medicine, industries such as food.On agricultural, use as non-chlorine type phosphorus, potassium two high effect composite fertilizers, be applicable to various soil and crop, resisting hot dry wind and preventing that from there is unusual effect aspect such as lodging; Pharmaceutically be used for chemical reagent, medicinal chemicals, nutrition agent etc.; The potassium primary phosphate of food grade is used for making and cures thing, monosodium glutamate, saleratus, and potassium primary phosphate can also be as the seasonings of synthetic sake etc. in addition.
In the prior art, the preparation method of potassium primary phosphate mainly contains neutralisation, crystallization process, ion exchange method and double decomposition.Wherein neutralisation technology is simple, and quality product is high, but too high because of its cost, and causing can't scale operation; Be easy to get though crystallization process has low in raw material cost, simple operation and other advantages, defective are to exist in the raw material metallic impurity ion, because the existence of foreign ion has a strong impact on the quality of product; Ion exchange method costs an arm and a leg because of resin, thereby does not have the value of popularization; And the double decomposition complex operation, raw materials cost is very high, more is unworthy promoting.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of purification process of potassium primary phosphate, and to overcome unstable product quality in the prior art, the metallic impurity ion content is high, complex operation, the deficiency that raw materials cost is higher.
Technical conceive of the present invention is such:
With PHOSPHORIC ACID TECH.GRADE,, SBA-15 molecular sieve chelate sorbent, from reaction product, collects the potassium primary phosphate that obtains purifying after filtering removal metallic impurity ion with the Repone K reaction.
The purification process of described potassium primary phosphate of the present invention, concrete steps are following:
The 30-50wt% PHOSPHORIC ACID TECH.GRADE is filtered through SBA-15 molecular sieve chelate sorbent under 0.1-0.15MPa, 30-50 ℃ temperature; Phosphoric acid that obtains and Repone K under 50-70 ℃ of temperature stirring reaction 1-3 hour; Reaction product is cooled to room temperature; Filter; Clean after drying with ultrapure water, promptly obtain the potassium primary phosphate of purifying.
According to the method described above; The preparation process of described SBA-15 molecular sieve chelate sorbent comprises the steps: the SBA-15 molecular sieve was flooded in steeping fluid 24-48 hour, filters, and cleans this SBA-15 molecular sieve with ultrapure water; Drying promptly obtains SBA-15 molecular sieve chelate sorbent.
Steeping fluid of the present invention is meant the 2-hydroxyquinoline is dissolved in the solution of forming in methyl alcohol or the ethanol, wherein 2-hydroxyquinoline and methyl alcohol or with the alcoholic acid mass volume ratio be 1: 2-4, g/ml.
The mol ratio of described phosphoric acid and Repone K is 1: 1-1.2, mol/mol.
The potassium primary phosphate main content that obtains with aforesaid method of the present invention is greater than 99wt%, and yield is greater than 90%.Through detecting, the muriate in the product, metallic impurity ion content all reach the standard of pharmaceutical grade potassium primary phosphate.
The present invention's beneficial effect compared with prior art:
The present invention adopts the SBA-15 molecular sieve as carrier, and the SBA-15 molecular sieve chelate sorbent for preparing has very strong adsorptive power for the metallic impurity ion in the primary industry level phosphoric acid, can effectively remove foreign ion wherein.
Reaction process of the present invention is simple to operate, and cost reduces, and yield improves, and the constant product quality that obtains is suitable for suitability for industrialized production.
Embodiment
Through embodiment the present invention is described further below, but embodiment does not limit protection scope of the present invention.
Embodiment 1
(1) preparation of SBA-15 molecular sieve chelate sorbent post:
Get 500g 2-hydroxyquinoline; Add dissolving composition steeping fluid in the 1000ml ethanol; At room temperature 250g SBA-15 molecular sieve is added in this steeping fluid; Flood 24 hours after-filtration; After ultrapure water 1000ml cleaning 2 times, drying is 24 hours under 100 ℃ of temperature, promptly obtains SBA-15 molecular sieve chelate sorbent 336g; The dress post, for use.
(2) purifying of potassium primary phosphate:
With 1000g concentration is that the 30wt% PHOSPHORIC ACID TECH.GRADE is at 0.1MPa; Feed the SBA-15 molecular sieve chelate sorbent filtration that step (1) obtains under 30 ℃ of temperature; Phosphoric acid that obtains and 228g Repone K stirring reaction 1 hour under 50 ℃ of temperature; Reaction product is cooled to room temperature; Filter, clean after drying, promptly obtain the potassium primary phosphate 395.6g of purifying with ultrapure water; Main content 99.3wt%, yield 94.99%.Through detecting, the muriate in the product, metallic impurity ion content all meet the standard of pharmaceutical grade potassium primary phosphate, specifically referring to table 1.
Embodiment 2
(1) preparation of SBA-15 molecular sieve chelate sorbent post:
Get 500g 2-hydroxyquinoline; Add dissolving composition steeping fluid in the 2000ml ethanol; At room temperature 250g SBA-15 molecular sieve is added in this steeping fluid; Flood 48 hours after-filtration; After ultrapure water 800ml cleaning 2 times, drying is 24 hours under 100 ℃ of temperature, promptly obtains SBA-15 molecular sieve chelate sorbent 325g; The dress post, for use.
(2) purifying of potassium primary phosphate:
With 1000g concentration is that the 40wt% PHOSPHORIC ACID TECH.GRADE is at 0.12MPa; Feed the SBA-15 molecular sieve chelate sorbent filtration that step (1) obtains under 40 ℃ of temperature; Phosphoric acid that obtains and 334g Repone K stirring reaction 2 hours under 60 ℃ of temperature; Reaction product is cooled to room temperature; Filter, clean after drying, promptly obtain the potassium primary phosphate 512.6g of purifying with ultrapure water; Main content 99.5wt%, yield 92.32%.Through detecting, the muriate in the product, metallic impurity ion content all meet the standard of pharmaceutical grade potassium primary phosphate, specifically referring to table 1.
Embodiment 3
(1) preparation of SBA-15 molecular sieve chelate sorbent post:
Get 500g 2-hydroxyquinoline; Add dissolving composition steeping fluid in the 2000ml methyl alcohol; At room temperature 250g SBA-15 molecular sieve is added in this steeping fluid; Flood 48 hours after-filtration; After ultrapure water 800ml cleaning 2 times, drying is 24 hours under 100 ℃ of temperature, promptly obtains SBA-15 molecular sieve chelate sorbent 321g; The dress post, for use.
(2) purifying of potassium primary phosphate:
With 1000g concentration is that the 50wt% PHOSPHORIC ACID TECH.GRADE is at 0.15MPa; Feed the SBA-15 molecular sieve chelate sorbent filtration that step (1) obtains under 50 ℃ of temperature; Phosphoric acid that obtains and 900g Repone K stirring reaction 1 hour under 70 ℃ of temperature; Reaction product is cooled to room temperature; Filter, clean after drying, promptly obtain the potassium primary phosphate 1388.1g of purifying with ultrapure water; Main content 99.1wt%, yield 95.30%.Through detecting, the muriate in the product, metallic impurity ion content all meet the standard of pharmaceutical grade potassium primary phosphate, specifically referring to table 1.
The analytical results of table 1 potassium primary phosphate standard and embodiment product
(carrying out the standard Q/CYDZ 2008-2010 of pharmaceutical grade potassium primary phosphate)
There is not the detection desired value that calcium, magnesium, zinc etc. indicate "-" in the potassium primary phosphate standard of ※ table 1
Need to prove that above embodiment is only unrestricted in order to technical scheme of the present invention to be described.Although the present invention is described in detail with reference to preferred embodiment; Those of ordinary skill in the art is to be understood that; Can make amendment or be equal to replacement the technical scheme of invention, and not break away from the scope of technical scheme of the present invention, it all should be encompassed in the claim scope of the present invention.
Claims (5)
1. the purification process of a potassium primary phosphate is characterized in that, comprises the steps:
The 30-50wt% PHOSPHORIC ACID TECH.GRADE is filtered through SBA-15 molecular sieve chelate sorbent under 0.1-0.15MPa, 30-50 ℃ temperature; Phosphoric acid that obtains and Repone K under 50-70 ℃ of temperature stirring reaction 1-3 hour; Reaction product is cooled to room temperature; Filter; Clean after drying with ultrapure water, promptly obtain the potassium primary phosphate of purifying.
2. method according to claim 1; It is characterized in that; The preparation process of described SBA-15 molecular sieve chelate sorbent comprises the steps: the SBA-15 molecular sieve was flooded in steeping fluid 24-48 hour; Filter; Clean this SBA-15 molecular sieve with ultrapure water; Drying promptly obtains SBA-15 molecular sieve chelate sorbent.
3. method according to claim 2 is characterized in that, described steeping fluid is meant the 2-hydroxyquinoline is dissolved in the solution of forming in methyl alcohol or the ethanol.
4. method according to claim 3 is characterized in that, described 2-hydroxyquinoline and methyl alcohol or alcoholic acid mass volume ratio are 1: 2-4, g/ml.
5. method according to claim 1 is characterized in that, the mol ratio of described phosphoric acid and Repone K is 1: 1-1.2.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201110214485 CN102303854B (en) | 2011-07-28 | 2011-07-28 | Purification method of monopotassium phosphate |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201110214485 CN102303854B (en) | 2011-07-28 | 2011-07-28 | Purification method of monopotassium phosphate |
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| CN102303854A true CN102303854A (en) | 2012-01-04 |
| CN102303854B CN102303854B (en) | 2013-05-15 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104402666A (en) * | 2014-10-20 | 2015-03-11 | 太仓沪试试剂有限公司 | Purification method for MOS-grade chloroform |
| CN106044839A (en) * | 2016-08-23 | 2016-10-26 | 太仓沪试试剂有限公司 | Silver nitrate purification method |
| CN106167253A (en) * | 2016-08-05 | 2016-11-30 | 常熟市圆启晶体材料有限公司 | A kind of method that potassium dihydrogen phosphate recrystallization purifies |
| CN107311133A (en) * | 2017-06-23 | 2017-11-03 | 太仓沪试试剂有限公司 | A kind of preparation method of potassium dihydrogen phosphate |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86101186A (en) * | 1986-02-21 | 1987-01-31 | 沈阳化学工业污染防治研究中心 | A kind of novel method of producing potassium primary phosphate |
-
2011
- 2011-07-28 CN CN 201110214485 patent/CN102303854B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86101186A (en) * | 1986-02-21 | 1987-01-31 | 沈阳化学工业污染防治研究中心 | A kind of novel method of producing potassium primary phosphate |
Non-Patent Citations (2)
| Title |
|---|
| 《磷肥与复肥》 20040131 杨林等 "磷酸二氢钾的制备方法综述" 第54-56页 1-5 第19卷, 第1期 * |
| 杨林等: ""磷酸二氢钾的制备方法综述"", 《磷肥与复肥》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104402666A (en) * | 2014-10-20 | 2015-03-11 | 太仓沪试试剂有限公司 | Purification method for MOS-grade chloroform |
| CN106167253A (en) * | 2016-08-05 | 2016-11-30 | 常熟市圆启晶体材料有限公司 | A kind of method that potassium dihydrogen phosphate recrystallization purifies |
| CN106044839A (en) * | 2016-08-23 | 2016-10-26 | 太仓沪试试剂有限公司 | Silver nitrate purification method |
| CN107311133A (en) * | 2017-06-23 | 2017-11-03 | 太仓沪试试剂有限公司 | A kind of preparation method of potassium dihydrogen phosphate |
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| CN102303854B (en) | 2013-05-15 |
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Address after: 200072 Zhabei District, Shanghai, Shanghai Road, No. 1, building 801, No. Applicant after: Sinopharm Chemical Reagent Co., Ltd. Address before: 200002 No. 52, Ningbo Road, Shanghai, Huangpu District Applicant before: Sinopharm Chemical Reagent Co., Ltd. |
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