CN105584998A - Method for preparing disodium hydrogen phosphate by adopting raffinate of melamine purified phosphoric acid - Google Patents

Method for preparing disodium hydrogen phosphate by adopting raffinate of melamine purified phosphoric acid Download PDF

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Publication number
CN105584998A
CN105584998A CN201410722798.0A CN201410722798A CN105584998A CN 105584998 A CN105584998 A CN 105584998A CN 201410722798 A CN201410722798 A CN 201410722798A CN 105584998 A CN105584998 A CN 105584998A
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CN
China
Prior art keywords
melamine
phosphoric acid
hydrogen phosphate
raffinate
sodium hydrogen
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Pending
Application number
CN201410722798.0A
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Chinese (zh)
Inventor
周骏宏
吴慧芳
方进
田县利
朱博含
王兴艳
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Qiannan Normal University for Nationalities
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Qiannan Normal University for Nationalities
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Priority to CN2014106383017 priority Critical
Priority to CN201410638301 priority
Application filed by Qiannan Normal University for Nationalities filed Critical Qiannan Normal University for Nationalities
Priority to CN201410722798.0A priority patent/CN105584998A/en
Publication of CN105584998A publication Critical patent/CN105584998A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F5/00Compounds of magnesium
    • C01F5/14Magnesium hydroxide
    • C01F5/20Magnesium hydroxide by precipitation from solutions of magnesium salts with ammonia
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00Phosphorus; Compounds thereof
    • C01B25/01Treating phosphate ores or other raw phosphate materials to obtain phosphorus or phosphorus compounds
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F11/00Compounds of calcium, strontium, or barium
    • C01F11/18Carbonates

Abstract

The invention provides a method for preparing disodium hydrogen phosphate by adopting raffinate of melamine purified phosphoric acid. The method comprises the operation steps that melamine and phosphoric acid by a wet process are heated, a melamine phosphate double salt is generated, cooling and filtering are performed, water is added into a filter cake, namely the melamine phosphate double salt, heating is performed, sodium carbonate is added, immediate filtration is performed, the melamine is separated out, a filtrate is heated and concentrated, cooling crystallization is performed, crystals are separated out, and the disodium hydrogen phosphate is obtained. According to the method, the byproduct raffinate generated in the extraction and purification process of the phosphoric acid by the wet process can be utilized, the method has the advantages of being low in cost, simple in technology and reliable in product quality, and an effective way is provided for utilization of the industrial waste raffinate.

Description

A kind of method that adopts melamine purifying phosphoric acid raffinate sodium hydrogen phosphate processed
Affiliated technical field
The invention belongs to chemical field, is a kind of method that adopts melamine purifying phosphoric acid raffinate sodium hydrogen phosphate processed.
Background technology
Sodium hydrogen phosphate can be used for making citric acid, water softener, fabric weighting agent, fireproof agent, and for glaze, welding agent, medicine, pigment, food industry and produce other phosphate as industrial water quality treatment agent, printing and dyeing washing agent, quality improver, nertralizer, antibiotic nutrient chemical, biochemical treatment agent, food quality modifying agent.
The industrial production of sodium hydrogen phosphate, mainly contains two kinds of neutralisation, the precipitation method, and neutralisation adopts phosphoric acid to react with sodium carbonate or NaOH, through condensing crystallizing, obtains sodium hydrogen phosphate after separation. The precipitation method are to adopt calcium monohydrogen phosphate to react with sodium carbonate, and separation precipitation of calcium carbonate, gets product after the concentrating filter liquor of phosphoric acid disodium hydrogen, crystallization, separation.
If by neutralisation, can use thermal phosphoric acid, and phosphoric acid by wet process or other phosphorous raw material, take again purification separation measure as mud phosphorus, N-(phosphonomethyl) iminodiacetic acid wastewater, corn soaking waste water etc., can obtain sodium hydrogen phosphate.
Prepare perlate salt taking phosphoric acid by wet process as raw material, there is the production cost advantage lower than thermal phosphoric acid, but phosphoric acid by wet process has more, higher impurity, generally can only be used for producing the product of fertilizer grade, and the purity difference of sodium hydrogen phosphate will directly have influence on its range of application and use value. So, for phosphoric acid by wet process, the raffinate particularly producing after wet phosphoric acid purifying, so that improve its value, just must take to be used for preparing after control techniques removal of impurities phosphoric acid and the salt thereof of high-quality.
Summary of the invention
The present invention will solve phosphoric acid by wet process raffinate (abbreviation raffinate), and impurity is many, the problem of unfavorable effective utilization, and a kind of method that adopts melamine purifying phosphoric acid raffinate sodium hydrogen phosphate processed is provided, and the method has the advantages that technique is simple, cost is low.
To achieve these goals, the technical scheme that the present invention takes is: a kind of method that adopts melamine purifying phosphoric acid raffinate sodium hydrogen phosphate processed, comprises the following steps:
(1) prepare double salt: by the mixture heating of melamine and raffinate, keep uniform temperature and react a period of time, generating melamine phosphate double salt.
(2) filter: after cooling containing complex salt solution, filter, filter cake melamine phosphate double salt is for follow-up sodium hydrogen phosphate processed, and filtrate can be recycled.
(3) sodium hydrogen phosphate preparation: by after the heating of melamine phosphate feed liquid, slowly add sodium carbonate, in the time that PH reaches terminal, stop adding sodium carbonate, then isothermal reaction a period of time, obtain disodium phosphate soln and insoluble melamine.
(4) filter: filter while hot, filter residue is melamine, recycles.
(5) condensing crystallizing: by concentrated the heating of filtrate disodium phosphate soln, the cooling sodium hydrogen phosphate crystal of separating out, isolated by filtration obtains disodium hydrogen phosphate.
Embodiment 1
Take phosphoric acid by wet process 69.8g and melamine 52.2g, slowly add phosphoric acid by wet process when adding 600mL distilled water to be heated to 95 DEG C in melamine, maintain the temperature at 95 DEG C of reaction 1h, generate the melamine phosphate double salt of indissoluble and the solution containing various impurity. To be cooledly to room temperature, carry out suction filtration, filter cake is melamine phosphate double salt.
Put into the thermostat water bath of 55 DEG C after 300mL distilled water and heat to adding in melamine phosphate double salt, while reaching constant temperature, slowly add sodium carbonate, measure pH value simultaneously, in the time that reaching 8.8 left and right, PH stops adding sodium carbonate, again after isothermal reaction 30min, obtain disodium phosphate soln and insoluble melamine, isolated by filtration while hot, and water flush cake.
The washing lotion of disodium phosphate soln and flush cake is merged and obtain disodium phosphate soln, sodium hydrogen phosphate stoste obtained above is slowly heated, solution to be concentrated liquid level stops heating while there is epitaxial, slowly crystallisation by cooling, and isolation of crystalline obtains sodium hydrogen phosphate product.
Embodiment 2
Take melamine 55g, add in 500mL distilled water, while being heated to 95 DEG C, slowly add phosphoric acid by wet process 75g, maintain the temperature at 95 DEG C of reactions 1.5 hours, generate melamine phosphate double salt. To be cooledly to room temperature, carry out centrifugal filtration, filter cake is melamine phosphate double salt.
Put into the thermostat water bath of 55 DEG C after 300mL distilled water and heat to adding in melamine phosphate double salt, while reaching constant temperature, slowly add sodium carbonate, measure pH value simultaneously, in the time that reaching 8.8 left and right, PH stops adding sodium carbonate, again after isothermal reaction 40min, obtain disodium phosphate soln and insoluble melamine, isolated by filtration while hot, and water flush cake.
The washing lotion of disodium phosphate soln and flush cake is merged and obtain disodium phosphate soln, sodium hydrogen phosphate stoste obtained above is slowly heated, solution to be concentrated liquid level stops heating while there is epitaxial, slowly crystallisation by cooling, and isolation of crystalline obtains sodium hydrogen phosphate product.
Embodiment 3
Take respectively phosphoric acid by wet process 54g and melamine 40g, first in melamine, add 350mL water and be heated to 90 DEG C, slowly add phosphoric acid by wet process, maintain the temperature at 90 DEG C of reactions 1 hour, filter out melamine phosphate after being cooled to room temperature.
Put into the thermostat water bath of 60 DEG C after 300mL distilled water and heat to adding in melamine phosphate, while reaching constant temperature, slowly add sodium carbonate, measure pH value simultaneously, in the time that reaching 8.8 left and right, PH stops adding sodium carbonate, again after isothermal reaction 40min, obtain disodium phosphate soln and insoluble melamine, isolated by filtration while hot, and water flush cake.
The washing lotion of disodium phosphate soln and flush cake is merged and obtain disodium phosphate soln, sodium hydrogen phosphate stoste obtained above is slowly heated, solution to be concentrated liquid level stops heating while there is epitaxial, slowly crystallisation by cooling, and isolation of crystalline obtains sodium hydrogen phosphate product.

Claims (5)

1. one kind adopts the method for melamine purifying phosphoric acid raffinate sodium hydrogen phosphate processed.
2. the method for the sodium hydrogen phosphate processed of claim 1, is characterized in that using melamine.
3. the method for the sodium hydrogen phosphate processed of claim 2, is characterized in that making melamine and phosphoric acid to form insoluble double salt.
4. the method for the sodium hydrogen phosphate processed of claim 2, is characterized in that melamine and phosphoric acid form after insoluble double salt, separate with mother liquor, this double salt again with alkali reaction, generate sodium hydrogen phosphate.
5. the method for the sodium hydrogen phosphate processed of claim 1, is characterized in that the phosphorous raw material phosphoric acid and the accessory substance that make for wet chemistry method that use, and it contains more impurity.
CN201410722798.0A 2014-11-13 2014-12-04 Method for preparing disodium hydrogen phosphate by adopting raffinate of melamine purified phosphoric acid Pending CN105584998A (en)

Priority Applications (3)

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CN2014106383017 2014-11-13
CN201410638301 2014-11-14
CN201410722798.0A CN105584998A (en) 2014-11-13 2014-12-04 Method for preparing disodium hydrogen phosphate by adopting raffinate of melamine purified phosphoric acid

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CN201410722798.0A CN105584998A (en) 2014-11-13 2014-12-04 Method for preparing disodium hydrogen phosphate by adopting raffinate of melamine purified phosphoric acid

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CN105584998A true CN105584998A (en) 2016-05-18

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CN201410744065.7A Pending CN104445300A (en) 2014-11-14 2014-12-09 Method of preparing magnesium hydroxide and calcium carbonate and separating out phosphorus ores by taking phosphate tailings as raw materials through ammonia circulation process

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CN104828793B (en) * 2015-05-06 2016-07-27 贵州省化工研究院 A kind of phosphorus mine tailing extracts the phosphorus concentrate co-production method containing magnesium calcium carbonate
CN104860277B (en) * 2015-05-06 2018-01-30 贵州省化工研究院 It is a kind of to mid low grade phosphate rock de-magging processing method
CN104860334B (en) * 2015-05-06 2017-09-05 贵州省化工研究院 A kind of processing method for improving mid low grade phosphate rock quality and reclaiming calcium and magnesium
CN104860279A (en) * 2015-05-06 2015-08-26 贵州省化工研究院 Method for extracting phosphate concentrate from phosphate tailings and cooperatively producing calcium ammonium nitrate and magnesium ammonium sulphate
CN108314584A (en) * 2018-03-14 2018-07-24 贵州芭田生态工程有限公司 A method of the tailing generated using nitrophosphate fertilizer filter residue, calcium ammonium nitrate filter residue, phosphate rock floating prepares soil conditioner
CN109264686B (en) * 2018-10-16 2021-02-23 贵州盛源新材料股份有限公司 Process for enriching phosphate concentrate and simultaneously recovering calcium carbonate and magnesium hydroxide from medium-low grade phosphate ore or phosphate tailings
CN109354050B (en) * 2018-10-24 2021-04-16 沈阳辰兴化工技术有限公司 Method and device for preparing calcium carbonate and magnesium hydroxide by using dolomite
CN110106370A (en) * 2019-05-16 2019-08-09 攀枝花学院 The method of vanadium-bearing slag of high calcium and high phosphor pretreatment decalcification dephosphorization

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