CN1657407A - Mixed extractant of purification wet phosphoric acid and dilute phosphoric dechlorine technology - Google Patents
Mixed extractant of purification wet phosphoric acid and dilute phosphoric dechlorine technology Download PDFInfo
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- CN1657407A CN1657407A CN 200410039484 CN200410039484A CN1657407A CN 1657407 A CN1657407 A CN 1657407A CN 200410039484 CN200410039484 CN 200410039484 CN 200410039484 A CN200410039484 A CN 200410039484A CN 1657407 A CN1657407 A CN 1657407A
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- phosphoric acid
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Abstract
A mixed extractant for purifying wet phosphoric acid is the mixture of n-butanol (60-70 vol%), tributyl phosphate (20-30) and methylisopropyl methanone (10-20) and has high extracting power and impurities-removing power. Said purified phosphoric acid can be used to prepare nano-class silver chloride by adding silver nitrate to it, reaction, and depositing.
Description
1, technical field
The invention belongs to the wet phosphoric acid purifying technical field
2, background technology
The purification acid product of solvent extraction phosphoric acid purification technology can satisfy PHOSPHORIC ACID TECH.GRADE or preparation feed and phosphatic requirement mostly, can reach food grade so that the standard of pharmaceutical grade through special processing.The difference of various Technologies is choosing at solvent species mainly.
This technology appears at the twenties in last century the earliest, and the seventies Europe and day present technique be comparative maturity, and has realized industrialization.China is slow in the development aspect this, and according to incompletely statistics, also there is not large-scale industrial production in China.
The common solvent that solvent extration adopts has:
(1) Fatty Alcohol(C12-C14 and C12-C18) that Fatty Alcohol(C12-C14 and C12-C18) is commonly used has propyl carbinol, isopropylcarbinol, primary isoamyl alcohol etc., and their carbonatoms is 4～5, and it is strong that cation impurity removes ability, and lower concentration phosphoric acid is had higher extracting power, but the solubleness in water is big, solvent recuperation expense height.Senior lipid acid such as n-Octanol, n-Heptyl alcohol, nonyl alcohol do not have extracting power substantially in low strength range.The extraction agent that Japan's Japan Cao Da method (Toyo process), West Asia, Rome IPROCHIM-ICECHIM method etc. are used is propyl carbinol, it is solvent that the Phorex method of France's nitrogen and chemical company (APC) adopts isopropylcarbinol, and USS agricultural chemicals company (USSAgu-Chemicais) adopts n-Heptyl alcohol to make solvent.
(2) ether solvent that ether is commonly used has diisopropyl ether, n-propyl isopropyl ether, di-n-propyl ether, n-butyl ether etc., but industrial the most commonly used with diisopropyl ether.It is big that ether has the interior extracting power of high concentration region, and cation impurity removes characteristics such as ability is strong.The Cleaning method of Israel mining company (IMI) has used diisopropyl ether to be extraction agent.
(3) ketones solvent that ketone and ester are general has methyl iso-butyl ketone (MIBK), methyl ethyl ketone, pimelinketone etc., and the ester class has propyl acetate, ethyl ester, N-BUTYL ACETATE etc.Their characteristics are similar with the ether extration agent, are raw material with the high-concentration phosphoric acid all, and it is strong that cation impurity removes power, and anionic impurity removes not exclusively, and the purifying phosphoric acid that makes can only reach technical grade.
(4) phosphoric acid ester tributyl phosphate (TBP) is important extraction agent, that uses in phosphoric acid extraction is also a lot, as Belgian Prayon method, the Phone-Poulenc Centrale Liqueur method of France etc., the characteristics of TBP are percentage extraction height of phosphoric acid in phosphoric acid concentration widely, to the decreasing ratio height of sulfate radical and fluorion, the solubleness in water is little, and solvent recuperation is easy.
(5) Jiang Yuming such as dibutyl sulfoxide, trialkylphosphine oxide, Li Daochun etc. have studied and have utilized the processing condition of dibutyl sulfoxide for the extraction agent purification of wet process phosphoric acid, purify sour P
2O
5Yield be 55.5%; Studied the extraction ability of trialkylphosphine oxide, experiment shows that trialkyl phosphine has stronger extracting power, and still along with the increase of aqueous phase acidity, its extracting power obviously descends.
(6) mixed solvent make mixed extractant that good extracting power and removal of impurities ability all be arranged in the high-concentration and low-concentration scope, so the research of mixed solvent is more according to the extraction ability of different solvents.The Wang Chun of Beijing Mine and Metallurgy General Inst, the big magnitude people of king have studied the extraction process that utilizes hexalin-pimelinketone mixed solvent to purify the YUNLAN Phosphor Fertilizer Plant phosphoric acid by wet process, and after level Four extraction, three grades of back extractions, the percentage extraction of phosphoric acid is 52.1%, and back extraction ratio is 99%.The research of building medium people in Dong Zhanneng, week also is mixed solvent, and its extraction section is respectively ten grades, ten one-levels, and stripping section is 2 grades, and sour yield is about 60%.It is extraction agent that Belgian Prayon adopts diisopropyl ether and tributyl phosphate mixed solvent, and sour yield reaches 70%～95%; It is the flow process of extraction agent that IMI has also adopted diisopropyl ether-propyl carbinol (or own amylalcohol) mixed solvent, purifies sour yield greater than 80%.
The Cl that contains some amount in the phosphoric acid behind the solvent extraction purification
-, the general method of underpressure distillation that adopts removes in the modern industry, needs to consume a large amount of heats.
3, summary of the invention
1) extraction agent that adopts of the present invention is the mixture of propyl carbinol and tbp, methyl isopropyl level ketone, and three's ratio (volume ratio) is a propyl carbinol 60%～70%, tbp 20%～30%, methyl isopropyl level ketone 10%～20%.This mixed extractant has the advantages that good extracting power and removal of impurities ability are all arranged in the high-concentration and low-concentration scope.
2) the present invention takes the dilute phosphoric acid after the 0.4mol/l～1.0mol/l silver nitrate solution of equivalent precipitates above method purification, and the reaction times is controlled at 1min～2min, not only the Cl in the dilute phosphoric acid
-Content can be less than the level of 0.0001% (weight ratio), and precipitated product is the silver chloride ultra-fine micropowder about 50nm.
4, embodiment
The embodiment of mixed extractant:
Example one: the proportioning of mixed extractant (volume ratio) is propyl carbinol 60%, tbp 30%, methyl isopropyl level ketone 10%, through the P of raw phosphoric acid after engaging sulphate, defluorinate, the dearsenification
2O
5Concentration is 25%, is in a ratio of 1: 1, and extraction temperature is 20 ℃, the powerful stirring, and the percentage extraction of Pyatyi cross current solvent extraction is about 75%, the percentage extraction of Pyatyi counter-current extraction is about 70%.
Example two: the proportioning of mixed extractant (volume ratio) is propyl carbinol 70%, tbp 20%, methyl isopropyl level ketone 10%, through the P of raw phosphoric acid after engaging sulphate, defluorinate, the dearsenification
2O
5Concentration is 25%, is in a ratio of 1: 1, and extraction temperature is 20 ℃, the powerful stirring, and the percentage extraction of Pyatyi cross current solvent extraction is about 80%, the percentage extraction of Pyatyi counter-current extraction is about 72%.
Example three: the proportioning of mixed extractant (volume ratio) is propyl carbinol 60%, tbp 30%, methyl isopropyl level ketone 10%, through the P of raw phosphoric acid after engaging sulphate, defluorinate, the dearsenification
2O
5Concentration is 35%, is in a ratio of 1: 1, and extraction temperature is 20 ℃, the powerful stirring, and the percentage extraction of Pyatyi cross current solvent extraction is about 88%, the percentage extraction of Pyatyi counter-current extraction is about 82%.
Example four: the proportioning of mixed extractant (volume ratio) is propyl carbinol 70%, tbp 20%, methyl isopropyl level ketone 10%, through the P of raw phosphoric acid after engaging sulphate, defluorinate, the dearsenification
2O
5Concentration is 35%, is in a ratio of 1: 1, and extraction temperature is 20 ℃, the powerful stirring, and the percentage extraction of Pyatyi cross current solvent extraction is about 94%, the percentage extraction of Pyatyi counter-current extraction is about 88%.
Example five: the proportioning of mixed extractant (volume ratio) is propyl carbinol 60%, tbp 20%, methyl isopropyl level ketone 60%, through the P of raw phosphoric acid after engaging sulphate, defluorinate, the dearsenification
2O
5Concentration is 25%, is in a ratio of 1: 1, and extraction temperature is 20 ℃, the powerful stirring, and the percentage extraction of Pyatyi cross current solvent extraction is about 72%, the percentage extraction of Pyatyi counter-current extraction is about 68%.
Example six: the proportioning of mixed extractant (volume ratio) is propyl carbinol 60%, tbp 20%, methyl isopropyl level ketone 20%, through the P of raw phosphoric acid after engaging sulphate, defluorinate, the dearsenification
2O
5Concentration is 35%, is in a ratio of 1: 1, and extraction temperature is 20 ℃, the powerful stirring, and the percentage extraction of Pyatyi cross current solvent extraction is about 85%, the percentage extraction of Pyatyi counter-current extraction is about 80%.
After the organic phase washing after this extraction agent extraction, back extraction, the foreign matter content in the phosphoric acid removes Cl
-Generally can reach the food grade phosphoric acid standard outward.
Dilute phosphoric acid dechlorination embodiment after this extraction agent extraction of process and organic phase washing, the back extraction:
Example seven: press Cl in the dilute phosphoric acid
-Equivalent than the silver nitrate solution that adds 0.4mol/l, filter immediately, wash, dry behind the reaction 1min, the white precipitate that obtains is the silver chloride superfine powder about 50nm, Cl in the dilute phosphoric acid
-Content is less than 0.0001%.
Example eight: press Cl in the dilute phosphoric acid
-Equivalent than the silver nitrate solution that adds 0.4mol/l, filter immediately, wash, dry behind the reaction 2min, the white precipitate that obtains is the silver chloride superfine powder about 70nm, Cl in the dilute phosphoric acid
-Content is less than 0.0001%.
Example nine: press Cl in the dilute phosphoric acid
-Equivalent than the silver nitrate solution that adds 1.0mol/l, filter immediately, wash, dry behind the reaction 1min, the white precipitate that obtains is the silver chloride superfine powder about 40nm, Cl in the dilute phosphoric acid
-Content is less than 0.0001%.
Example ten: press Cl in the dilute phosphoric acid
-Equivalent than the silver nitrate solution that adds 1.0mol/l, filter immediately, wash, dry behind the reaction 2min, the white precipitate that obtains is the silver chloride superfine powder about 60nm, Cl in the dilute phosphoric acid
-Content is less than 0.0001%.
Claims (3)
1, a kind of novel phosphoric acid by wet process mixed extractant and dilute phosphoric acid dechlorination technology.
2, according to right 1, the extraction agent that it is characterized in that extracting phosphoric acid by wet process is the mixture of propyl carbinol and tbp, methyl isopropyl ketone, three's ratio (volume ratio) is a propyl carbinol 60%～70%, tbp 20%～30%, methyl isopropyl ketone 10%～20%.
3, according to right 1, it is characterized in that the phosphoric acid of this purification process preparation is dilute phosphoric acid, remove Cl in the dilute phosphoric acid
-Precipitation agent adopt the 0.4mol/l～1.0mol/l Silver Nitrate (AgNO of equivalent
3) solution, the reaction times is controlled at 1min～2min, and throw out is the ball shaped nano level silver chloride about 50nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410039484 CN1657407A (en) | 2004-02-16 | 2004-02-16 | Mixed extractant of purification wet phosphoric acid and dilute phosphoric dechlorine technology |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410039484 CN1657407A (en) | 2004-02-16 | 2004-02-16 | Mixed extractant of purification wet phosphoric acid and dilute phosphoric dechlorine technology |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1308228C (en) * | 2005-10-31 | 2007-04-04 | 宜宾天原股份有限公司 | Process for purifying producing extracting solvent of food grade phosphoric acid by wet method phosphoric acid and extracting process thereof |
| CN102815685A (en) * | 2012-08-10 | 2012-12-12 | 清华大学 | Wet-method phosphoric acid staged extraction and purification process |
| CN106348273A (en) * | 2016-08-17 | 2017-01-25 | 湖北三宁化工股份有限公司 | Extraction agent for preparing industrial phosphoric acid through hydrochloric acid method and extraction method thereof |
| CN108928808A (en) * | 2018-07-03 | 2018-12-04 | 昆明川金诺化工股份有限公司 | A kind of solvent extraction new method of purifying low-concentration phosphoric acid by wet process |
-
2004
- 2004-02-16 CN CN 200410039484 patent/CN1657407A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1308228C (en) * | 2005-10-31 | 2007-04-04 | 宜宾天原股份有限公司 | Process for purifying producing extracting solvent of food grade phosphoric acid by wet method phosphoric acid and extracting process thereof |
| CN102815685A (en) * | 2012-08-10 | 2012-12-12 | 清华大学 | Wet-method phosphoric acid staged extraction and purification process |
| CN102815685B (en) * | 2012-08-10 | 2014-01-01 | 清华大学 | Wet-method phosphoric acid staged extraction and purification process |
| CN106348273A (en) * | 2016-08-17 | 2017-01-25 | 湖北三宁化工股份有限公司 | Extraction agent for preparing industrial phosphoric acid through hydrochloric acid method and extraction method thereof |
| CN108928808A (en) * | 2018-07-03 | 2018-12-04 | 昆明川金诺化工股份有限公司 | A kind of solvent extraction new method of purifying low-concentration phosphoric acid by wet process |
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