CN102303854B - Purification method of monopotassium phosphate - Google Patents
Purification method of monopotassium phosphate Download PDFInfo
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- CN102303854B CN102303854B CN 201110214485 CN201110214485A CN102303854B CN 102303854 B CN102303854 B CN 102303854B CN 201110214485 CN201110214485 CN 201110214485 CN 201110214485 A CN201110214485 A CN 201110214485A CN 102303854 B CN102303854 B CN 102303854B
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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 trapezoid body inorganic salt with gloss, is applied to agricultural, medicine, the 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 the aspect such as lodging; Pharmaceutically be used for chemical reagent, medicinal chemicals, nutrition agent etc.; The potassium primary phosphate of food grade is for the manufacture of curing thing, monosodium glutamate, saleratus, and potassium primary phosphate can also be as seasonings of synthetic sake etc. in addition.
In prior art, the preparation method of potassium primary phosphate mainly contains neutralisation, crystallization process, ion exchange method and double decomposition.Wherein neutralisation technique is simple, and quality product is high, but because of its high cost, and causing can't scale operation; Though it is cheap and easy to get that crystallization process has raw material, simple operation and other advantages, defective are to exist in raw material the metallic impurity ion, have a strong impact on the quality of product due to the existence of foreign ion; Ion exchange method is expensive because of resin, thereby there is no 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 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, after filtering removal metallic impurity ion, SBA-15 molecular sieve chelate sorbent with the Repone K reaction, collects the potassium primary phosphate that obtains purifying from reaction product.
The purification process of described potassium primary phosphate of the present invention, concrete steps are as follows:
The 30-50wt% PHOSPHORIC ACID TECH.GRADE is filtered through SBA-15 molecular sieve chelate sorbent at 0.1-0.15MPa, 30-50 ℃ temperature, the phosphoric acid that obtains and Repone K at 50-70 ℃ of temperature stirring reaction 1-3 hour, reaction product is cooled to room temperature, filter, clean rear drying with ultrapure water, namely 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 namely obtains SBA-15 molecular sieve chelate sorbent.
Steeping fluid of the present invention refers to the 2-hydroxyquinoline is dissolved in the solution that forms in methyl alcohol or ethanol, wherein 2-hydroxyquinoline and methyl alcohol or with the mass volume ratio of ethanol 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%.After testing, the muriate in 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 primary industry level phosphoric acid, can effectively remove foreign ion wherein.
Reaction process of the present invention is simple to operate, cost, and yield improves, and the constant product quality that obtains is suitable for suitability for industrialized production.
Embodiment
The invention will be further described below by embodiment, 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 1000ml ethanol, at room temperature 250g SBA-15 molecular sieve is added in this steeping fluid, flood after 24 hours and filter, after cleaning 2 times with ultrapure water 1000ml, drying is 24 hours at 100 ℃ of temperature, namely obtains SBA-15 molecular sieve chelate sorbent 336g, the dress post, stand-by.
(2) purifying of potassium primary phosphate:
Be that the 30wt% PHOSPHORIC ACID TECH.GRADE is at 0.1MPa with 1000g concentration, pass into the SBA-15 molecular sieve chelate sorbent filtration that step (1) obtains at 30 ℃ of temperature, the phosphoric acid that obtains and 228g Repone K stirring reaction 1 hour at 50 ℃ of temperature, reaction product is cooled to room temperature, filter, clean rear drying with ultrapure water, namely obtain the potassium primary phosphate 395.6g of purifying, main content 99.3wt%, yield 94.99%.After testing, the muriate in product, metallic impurity ion content all meet the standard of pharmaceutical grade potassium primary phosphate, referring specifically 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 2000ml ethanol, at room temperature 250g SBA-15 molecular sieve is added in this steeping fluid, flood after 48 hours and filter, after cleaning 2 times with ultrapure water 800ml, drying is 24 hours at 100 ℃ of temperature, namely obtains SBA-15 molecular sieve chelate sorbent 325g, the dress post, stand-by.
(2) purifying of potassium primary phosphate:
Be that the 40wt% PHOSPHORIC ACID TECH.GRADE is at 0.12MPa with 1000g concentration, pass into the SBA-15 molecular sieve chelate sorbent filtration that step (1) obtains at 40 ℃ of temperature, the phosphoric acid that obtains and 334g Repone K stirring reaction 2 hours at 60 ℃ of temperature, reaction product is cooled to room temperature, filter, clean rear drying with ultrapure water, namely obtain the potassium primary phosphate 512.6g of purifying, main content 99.5wt%, yield 92.32%.After testing, the muriate in product, metallic impurity ion content all meet the standard of pharmaceutical grade potassium primary phosphate, referring specifically 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 2000ml methyl alcohol, at room temperature 250g SBA-15 molecular sieve is added in this steeping fluid, flood after 48 hours and filter, after cleaning 2 times with ultrapure water 800ml, drying is 24 hours at 100 ℃ of temperature, namely obtains SBA-15 molecular sieve chelate sorbent 321g, the dress post, stand-by.
(2) purifying of potassium primary phosphate:
Be that the 50wt% PHOSPHORIC ACID TECH.GRADE is at 0.15MPa with 1000g concentration, pass into the SBA-15 molecular sieve chelate sorbent filtration that step (1) obtains at 50 ℃ of temperature, the phosphoric acid that obtains and 900g Repone K stirring reaction 1 hour at 70 ℃ of temperature, reaction product is cooled to room temperature, filter, clean rear drying with ultrapure water, namely obtain the potassium primary phosphate 1388.1g of purifying, main content 99.1wt%, yield 95.30%.After testing, the muriate in product, metallic impurity ion content all meet the standard of pharmaceutical grade potassium primary phosphate, referring specifically 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)
Indicate the detection desired value of "-" in the potassium primary phosphate standard of ※ table 1 without calcium, magnesium, zinc etc.
Need to prove, above embodiment is only unrestricted in order to technical scheme of the present invention to be described.Although with reference to preferred embodiment, the present invention is had been described in detail, those of ordinary skill in the art is to be understood that, can modify or be equal to replacement the technical scheme of invention, and not break away from the scope of technical solution of the present invention, it all should be encompassed in claim scope of the present invention.
Claims (3)
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 at 0.1-0.15MPa, 30-50 ℃ temperature, the phosphoric acid that obtains and Repone K at 50-70 ℃ of temperature stirring reaction 1-3 hour, reaction product is cooled to room temperature, filter, clean rear drying with ultrapure water, namely obtain the potassium primary phosphate of purifying;
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, and drying namely obtains SBA-15 molecular sieve chelate sorbent;
Described steeping fluid refers to the 2-hydroxyquinoline is dissolved in the solution that forms in methyl alcohol or ethanol.
2. method according to claim 1, is characterized in that, the mass volume ratio of described 2-hydroxyquinoline and methyl alcohol or ethanol is 1:2-4, g/mL.
3. 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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| CN 201110214485 CN102303854B (en) | 2011-07-28 | 2011-07-28 | Purification method of monopotassium phosphate |
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| CN 201110214485 CN102303854B (en) | 2011-07-28 | 2011-07-28 | Purification method of monopotassium phosphate |
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| CN102303854B true CN102303854B (en) | 2013-05-15 |
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| CN104402666B (en) * | 2014-10-20 | 2016-06-15 | 太仓沪试试剂有限公司 | A kind of purification process of MOS level 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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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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