CN1994871A - Method for preparing technical grade phosphate using wet method phosphoric acid as raw material - Google Patents
Method for preparing technical grade phosphate using wet method phosphoric acid as raw material Download PDFInfo
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- CN1994871A CN1994871A CN 200610163810 CN200610163810A CN1994871A CN 1994871 A CN1994871 A CN 1994871A CN 200610163810 CN200610163810 CN 200610163810 CN 200610163810 A CN200610163810 A CN 200610163810A CN 1994871 A CN1994871 A CN 1994871A
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Abstract
The invention discloses a making method of industry-grade phosphate based on wet process phosphoric acid as raw material, which comprises the following steps: desulfurizing; defluorinating; stripping arsenic; removing heavy metal; decoloring; extracting predisposed wet process phosphoric acid through compound organic solvent of ketone and phosphate ester; washing; reextracting; condensing; post-processing to obtain the product; adopting alkali solution of potassium carbonate, sodium carbonate or alkaline-earth metal as extractor.
Description
Technical field
The present invention relates to phosphatic preparation.Specifically, relating to a kind of is the method for feedstock production industrial grade phosphate with the phosphoric acid by wet process.
Background technology
Because the production of thermal phosphoric acid power consumption is high, along with energy day is becoming tight, people more and more are ready to adopt phosphoric acid by wet process to prepare the PHOSPHORIC ACID TECH.GRADE product salt.But the phosphoric acid by wet process impurities is higher, must earlier it be purified the production preparation that just can be used for industrial grade phosphate.To the purification of phosphoric acid by wet process, mainly contain chemical precipitation method, ion exchange method, the Phosphoric Acid Concentration method of purification, solvent extration and crystallization process, at present industrial general employing solvent extration.
Before the technology of solvent extration purification of wet process phosphoric acid can be traced back to 40 years.The initial solvent of using be can be miscible with water solvent, for example small molecular alcohol and ketone; Or with the immiscible short chain alcohol of water.The former need distill to discharge the acid after the purification, and energy consumption is big, the cost height; The latter needs a lot of levels just can reach satisfied effect of extracting, complex process.
Along with going deep into of research work, the extraction agent kind that drops into research at present and use is quite a lot of, and alcohols (propyl carbinol, isopropylcarbinol, amylalcohol), ethers (diisopropyl ether, diisobutyl ether), ketone (pimelinketone, methyl iso-butyl ketone (MIBK), methyl n-butyl ketone etc.), ester class (butylacetate, dibutyl phosphate, tributyl phosphate), sulfoxide class (dipropyl sulfoxide, dibutyl sulfoxide), amine (trioctylamine) etc. are arranged.Above-mentioned every kind of extraction agent has relative merits, and the requirement of raw material phosphoric acid also is not quite similar.For example, tributyl phosphate has in phosphoric acid concentration scope widely strong to phosphoric acid collection output capacity, and is good to the selectivity of metallic impurity, to anionic impurity (SO
4 2-, F
-) the good advantage of removal; But it costs an arm and a leg, at Cl
-, NO
3 -Can impel its hydrolysis when ion exists, cause damage, its proportion and viscosity are bigger, and the difficulty that is separated need be added thinner (kerosene, hexanaphthene etc.) during use.Again for example, though pimelinketone, methyl iso-butyl ketone (MIBK), butylacetate low price, be separated easily, only be applicable to that with high-concentration wet process phosphoric acid be come together the occasion of object, it requires raw material phosphoric acid P
2O
5Concentration generally must be greater than 54%.Ketones solvent is to cation impurity clearance height in the phosphoric acid by wet process, but HF, H
2SO
4Be difficult to remove.
At above-mentioned technical problem, the contriver has carried out arduous research meticulously, succeeded in developing a kind of purifying method of phosphoric acid by wet process, and the method that further prepares PHOSPHORIC ACID TECH.GRADE and food grade phosphoric acid, and applied for Chinese patent (application number: 200510048779.5).This technical costs is cheap, has effectively expanded the suitable concentration range of phosphate raw material.But when this technology manufacture level phosphoric acid salt of utilization, also there is following technical problem: 1. technical grade or the food grade phosphoric acid that obtains as reverse-extraction agent with water, technical process when being used to produce phosphoric acid salt is longer, phosphoric acid is concentrated repeatedly therein and dilutes, and has increased unnecessary energy consumption and expenditure; 2. water is the essential raw material of solvent extraction technology manufacture level or food grade phosphoric acid, but when being used to produce phosphoric acid salt because water and solvent density difference are very little, two-phase clarification velocity of separation is slow, the phase-splitting time is long, caused the big and high shortcoming of investment of back extraction processing apparatus volume thus, and in actually operating, may also exist solvent not separate the problems such as solvent loss that cause fully, therefore be necessary it is done further to improve.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, providing a kind of is the method for feedstock production industrial grade phosphate with the phosphoric acid by wet process.This method technology is reasonable, energy consumption is low, raw material subject range is wide, quality product is high.
Purpose of the present invention is achieved by following technical proposals.
The invention provides a kind of is the method for feedstock production industrial grade phosphate with the phosphoric acid by wet process, and this method comprises the step of following order:
(1) is raw material with the phosphoric acid by wet process, in phosphoric acid by wet process, adds earlier the ground phosphate rock desulfurization, add fluorine, arsenic and heavy metal in the mixture dephosphorylate of yellow soda ash and sodium sulphite then; Make it in an operation, finish tentatively removing of sulfate radical, fluorine, arsenic and heavy metal; Wherein, the addition of ground phosphate rock is pressed SO in the phosphoric acid
4 2-Stoichiometric 1.1~1.65 extraordinarily go into; The mass ratio of described yellow soda ash and sodium sulphite is 1.7~2.2: 1, and its addition is extraordinarily gone into according to 1.4~1.8 of the stoichiometric ratio of fluorine in the phosphoric acid; Temperature of reaction is 50 ℃~65 ℃, and the reaction times is 1.5~3.5 hours; Filter then;
(2) add activated carbon in the filtrate that step (1) obtains, the consumption of activated carbon is 0.2%~1.0wt% of phosphoric acid quality, and temperature of reaction is 50 ℃~70 ℃, 1~2.5 hour reaction times;
(3) step (2) gains are extracted, described extraction agent is cycloaliphatic ketone or contains the aliphatic ketone of two above saturated alkyls and the mixture of phosphoric acid ester, wherein the mass percent of phosphoric acid ester is 10%~80%, and cycloaliphatic ketone or the mass percent that contains the aliphatic ketone of two above saturated alkyls are 20%~90%; Organic phase compares 1.5~5.5 with the volume of water: 1, and temperature is 0 ℃~50 ℃;
(4) use aqueous phosphatic that the gains of step (3) are washed, described aqueous phosphatic is the purifying phosphoric acid salts solution for preparing from system itself.The volume of organic phase and salts solution is in a ratio of 3~10: 1, and temperature is 0 ℃~50 ℃;
(5) gains to step (4) carry out back extraction, and used reverse-extraction agent is the alkaline aqueous solution of alkali such as salt of wormwood, yellow soda ash, potassium hydroxide, sodium hydroxide or alkaline-earth metal, organic phase and water be in a ratio of 2~8: 1, temperature is 20 ℃~50 ℃;
(6) adopt thickening equipment with back extraction with reclaim the purification of phosphoric acid salt brine solution that is obtained behind the solvent and concentrate, crystallization filter or dry polymerization after can make required industrial grade phosphate.
Compare with prior art, the present invention has following outstanding beneficial effect:
1. the invention provides a kind of novel method for preparing industrial grade phosphate, this method divided for two steps carried out pre-treatment, not only can simplify technology effectively, make full use of the various aggreggate utilities that remove agent, reduced and filtered number of times and filter the P that is brought
2O
5Loss simultaneously, has reduced the consumption of discoloring agent effectively, has saved cost.
2. adopt the double solvents of ketone and phosphoric acid ester to carry out the extraction of phosphoric acid, the defective when having overcome independent use ketone or phosphoric acid ester on the performance as extraction agent.The use of double solvents has improved the separation factor of extraction agent to phosphoric acid, has expanded the scope of application of extraction agent, has reduced the biphase phase-splitting time.Ketone can not only play the effect of extraction agent, has also played the effect of phosphoric acid ester thinner simultaneously, and the two-phase phase-splitting is easy, is guaranteeing under the product quality premise, and the extraction yield is higher than the extraction yield of composite preceding single ketone or phosphoric acid ester.The continuous stalling characteristic of phosphoric acid ester has been improved the performance of ketone again, and ketone is increased the separation factor of phosphoric acid, and the suitable concentration range of raw material phosphoric acid also adopts single ketone extraction agent that relaxing by a relatively large margin arranged, and is more suitable for domestic phosphoric acid by wet process P
2O
5Production concentration generally can only reach 48~50% these present situations.
3. the recovery of extraction agent only needs simple stratified liquid and stripping, has simplified technology, has reduced energy consumption, has saved cost.
4. the phosphoric acid after directly adopting potassium hydroxide (sodium) or salt of wormwood alkaline aqueous solutions such as (sodium) back extraction from organic phase go out purifying as reverse-extraction agent, not only simplified the production technique of industrial grade phosphate, and, reduce the solvent loss and energy expenditure than using the soft water reverse-extraction agent can obtain better back extraction effect.
Description of drawings
Fig. 1 is the present invention prepares industrial grade phosphate with phosphoric acid by wet process a process flow diagram.
Embodiment
Embodiment 1
---preparation PHOSPHORIC ACID TECH.GRADE sodium dihydrogen
(wt%) composed as follows of raw materials used phosphoric acid by wet process:
Composition | P 2O 5 | F | SO 3 | Fe 2O 3 | Al 2O 3 | MgO | As | Pb | Org. |
Content % | 48.67 | 0.70 | 3.17 | 1.31 | 0.34 | 0.60 | 0.004 | 0.007 | 0.05 |
Serialization is produced, and technical process comprises pre-treatment, extraction, washing, back extraction, solvent recuperation successively, concentrates postprocessing working procedures as shown in Figure 1.
(1) pre-treatment
Pre-treatment divided for two steps carried out, and the first step adds ground phosphate rock and makes sweetening agent, adopts the mixture of yellow soda ash and sodium sulphite to slough fluorine, arsenic and heavy metal; Sweetening agent is pressed SO in the phosphoric acid
4 2-Stoichiometric 1.20 extraordinarily go into, defluorinate, arsenic and heavy metal agent are extraordinarily gone into according to 1.4 of the stoichiometric ratio of fluorine in the phosphoric acid, wherein yellow soda ash: sodium sulphite=2.2: 1,60 ℃ of temperature of reaction, in 3.5 hours reaction times, adopt flame filter press to separate then and remove solid slag.Second step was to add gac to make discoloring agent behind the waste residue that has filtered desulfurization, defluorinate, arsenic and heavy metal generation, the consumption of activated carbon is 0.5% of a phosphoric acid quality, temperature of reaction is 70 ℃, and in 2.0 hours reaction times, reaction finishes the back centrifugation and removes gac.
(2) extraction
Extraction is carried out in mixer-settler and/or extraction tower, and extraction agent is the mixture of pimelinketone and tributyl phosphate, and wherein the mass percent of tributyl phosphate is 80%, and the mass percent of pimelinketone is 20%; Processing parameter: compare 4.5: 1 of organic phase and water, temperature is 40 ℃.
(3) washing
Washing is carried out in mixer-settler and/or extraction tower, the purifying phosphoric acid salt brine solution that washings prepares from system itself.Compare 6: 1 of washing procedure organic phase and water, temperature is 40 ℃.
(4) back extraction
Back extraction is carried out in extraction clarifying tank and/or extraction tower, and extraction agent is 20% aqueous sodium hydroxide solution, compare 3: 1 of organic phase and water, and temperature of reaction is controlled at below 50 ℃; Strip liquor transfers to PH=4.2-4.6 with aqueous sodium hydroxide solution in storage tank.
(5) solvent recuperation
Reclaim most extraction agents in the back extraction operation by the stratified liquid mode.Extraction process is dissolved in the trace solvent that raffinate and back extraction operation be dissolved in purification of phosphoric acid salt and reclaims in the stripping mode.120 ℃ of stripping temperature, stripping pressure: normal pressure, stripping time: 30 minutes.
(6) concentrate
Purification of phosphoric acid sodium dihydrogen solution after adopting the concentrated back extraction of thickening equipment and reclaiming solvent promptly makes the PHOSPHORIC ACID TECH.GRADE sodium dihydrogen after crystallization, filtration, the oven dry.
The PHOSPHORIC ACID TECH.GRADE sodium dihydrogen that present embodiment is prepared, relevant components contents such as following table:
NaH 2PO 4.2H 2O | Basicity | Fe | SO 4 2- | As | Heavy metal (in Pb) | Cl |
98.4% | 19.6 | 0.03% | 0.21% | 0.003% | 0.002% | 0.03% |
Embodiment 2
---preparation PHOSPHORIC ACID TECH.GRADE disodium hydrogen
In the present embodiment, the composition of raw materials used phosphoric acid by wet process and flow process are with embodiment 1.The processing condition that present embodiment adopted with purify auxiliary agent (containing extraction agent) except that following all identical every with embodiment 1:
Sweetening agent is pressed SO in the phosphoric acid
4 2-Stoichiometric 1.35 extraordinarily go into, and defluorinate, arsenic and heavy metal agent are extraordinarily gone into according to 1.6 of the stoichiometric ratio of fluorine in the phosphoric acid.The consumption of activated carbon is 0.2% of a phosphoric acid quality.Back extraction is carried out in extraction clarifying tank and/or extraction tower, and extraction agent is 15% aqueous sodium carbonate, compare 4: 1 of organic phase and water, and temperature of reaction is controlled at below 50 ℃; Strip liquor transfers to PH=8.0-8.4 with technical grade yellow soda ash in storage tank.
The PHOSPHORIC ACID TECH.GRADE disodium hydrogen that present embodiment is prepared, relevant components contents such as following table:
Composition | Na 2HPO 4.12H 2O | SO 4 2- | Cl - | F | As |
Content % | 97.6 | 0.37 | 0.03 | 0.04 | 0.002 |
Embodiment 3
---preparation PHOSPHORIC ACID TECH.GRADE potassium dihydrogen
In the present embodiment, the composition of raw materials used phosphoric acid by wet process and flow process are with embodiment 1.The processing condition that present embodiment adopted with purify auxiliary agent (containing extraction agent) except that following all identical every with embodiment 1:
Back extraction is carried out in extraction clarifying tank and/or extraction tower, and extraction agent is 10% potassium hydroxide aqueous solution, compare 4: 1 of organic phase and water, and temperature of reaction is controlled at below 50 ℃; Strip liquor transfers to PH=4.2-4.6 with technical grade potassium hydroxide in storage tank.
The PHOSPHORIC ACID TECH.GRADE potassium dihydrogen that present embodiment is prepared, relevant components contents such as following table:
Composition | KH 2PO 4 | Cl - | Fe | As | Heavy metal (in Pb) |
Content % | 98.7 | 0.12 | 0.002 | 0.002 | 0.001 |
Embodiment 4
---preparation PHOSPHORIC ACID TECH.GRADE hydrogen dipotassium
In the present embodiment, the composition of raw materials used phosphoric acid by wet process and flow process are with embodiment 1.The processing condition that present embodiment adopted with purify auxiliary agent (containing extraction agent) except that following all identical every with embodiment 1:
Extraction agent is the mixture of methyl n-butyl ketone and tributyl phosphate, and wherein the mass percent of tributyl phosphate is 50%, and the mass percent of methyl n-butyl ketone is 50%; Processing parameter: compare 3.2: 1 of organic phase and water.
Back extraction is carried out in extraction clarifying tank and/or extraction tower, and extraction agent is 8% wet chemical, compare 4: 1 of organic phase and water, and temperature of reaction is controlled at below 50 ℃; Strip liquor transfers to PH=4.2~4.6 with salt of wormwood in storage tank.
The PHOSPHORIC ACID TECH.GRADE potassium dihydrogen that present embodiment is prepared, relevant components contents such as following table:
Composition | KH 2PO 4 | Cl - | Fe | As | Heavy metal (in Pb) |
Content % | 98.5 | 0.16 | 0.002 | 0.002 | 0.001 |
Embodiment 5
---preparation technical grade tripoly phosphate sodium STPP
In the present embodiment, the composition of raw materials used phosphoric acid by wet process and flow process are with embodiment 1.The processing condition that present embodiment adopted with purify auxiliary agent (containing extraction agent) except that following all identical every with embodiment 1:
Extraction agent is the mixture of methyl iso-butyl ketone (MIBK) and tributyl phosphate, and wherein the mass percent of tributyl phosphate is 20%, and the mass percent of methyl iso-butyl ketone (MIBK) is 80%; Processing parameter: compare 1.8: 1 of organic phase and water, temperature is 30 ℃.
Back extraction is carried out in extraction clarifying tank and/or extraction tower, and reverse-extraction agent is 15% aqueous sodium carbonate, compare 4: 1 of organic phase and water, and temperature of reaction is less than 50 ℃.Stratified liquid reclaims most extraction agents.Extraction process is dissolved in the trace solvent that raffinate and back extraction operation be dissolved in strip liquor and reclaims in the stripping mode.Strip liquor is regulated control neutralization value 2.75~2.85 (neutralization value refers to the degree that hydrogen ion is neutralized in the phosphoric acid, i.e. the ratio of the summation of sodium and disodium and a sodium) with yellow soda ash in storage tank.
The mixing solutions of concentrated phosphoric acid sodium dihydrogen and disodium-hydrogen is dried to water content less than 5% at 110 ℃.Grinding is sieved, and makes the tripoly phosphate sodium STPP product in 430 ℃ of high temperature polymerizations in the presence of catalyzer ammonium nitrate.
The technical grade tripoly phosphate sodium STPP that present embodiment is prepared, relevant components contents such as following table:
Project | Index |
Tripoly phosphate sodium STPP (Na 5P 3O 10) content, % | 96 |
Vanadium Pentoxide in FLAKES (P 2O 5) content, % | 57.8 |
Water insoluble matter content, % | 0.002 |
Iron (Fe) content, % | 0.0015 |
PH value (1% solution) | 9.8 |
Whiteness, % | 90 |
Arsenic (in As), ppm | 15 |
Claims (10)
1. one kind is the method for feedstock production industrial grade phosphate with the phosphoric acid by wet process, it may further comprise the steps: divided for two steps phosphoric acid by wet process was carried out desulfurization, defluorinate, dearsenification, removing heavy-metal and decolouring pre-treatment, compounded organic solvent with ketone and phosphoric acid ester extracts pretreated phosphoric acid by wet process then, again through washing, back extraction, concentrate and aftertreatment obtains industrial grade phosphate, it is characterized in that: used reverse-extraction agent is the alkaline aqueous solution of alkali such as salt of wormwood, yellow soda ash, potassium hydroxide, sodium hydroxide or alkaline-earth metal.
2. preparation method according to claim 1 is characterized in that: desulfurization, defluorinate, dearsenification, removing heavy-metal are once finished at an in-process, decolour after having filtered desulfurization and defluorinate, waste residue that arsenic and heavy metal produced again.Sweetening agent is ground phosphate rock and/or barium carbonate, and defluorinate, arsenic and heavy metal agent are the mixture of sodium sulphite and yellow soda ash, and discoloring agent is an activated carbon.
3. preparation method according to claim 1 and 2 is characterized in that: described sweetening agent is pressed SO in the phosphoric acid
4 2-Stoichiometric 1.1~1.65 extraordinarily go into, described defluorinate, arsenic and heavy metal agent are extraordinarily gone into by 1.4~1.8 of the stoichiometric ratio of fluorine in the phosphoric acid, yellow soda ash wherein: sodium sulphite=1.7~2.2: 1,50~65 ℃ of temperature of reaction, 1.5~3.5 hours reaction times.
4. preparation method according to claim 2 is characterized in that: described decolorizing with activated carbon agent, its activated carbon specific surface area 8 00~1200m
2/ g, the consumption of activated carbon are 0.2%~1.0% of phosphoric acid quality, and temperature of reaction is 50~70 ℃, 1~2.5 hour reaction times.
5. preparation method according to claim 1, it is characterized in that: the compounded organic solvent of described ketone and phosphoric acid ester is cycloaliphatic ketone or contains the aliphatic ketone of two above saturated alkyls and the mixture of phosphoric acid ester, processing parameter: organic phase compares 1.5~5.5: 1 with water, and temperature is 0 ℃~50 ℃.
6. preparation method according to claim 5 is characterized in that: the mass percent of phosphoric acid ester is 10~80%, and cycloaliphatic ketone or the mass percent that contains the aliphatic ketone of two above saturated alkyls are 20~90%.
7. preparation method according to claim 5 is characterized in that: described cycloaliphatic ketone or the aliphatic ketone that contains two above saturated alkyls can be a kind of in cyclohexanone, methyl iso-butyl ketone (MIBK), methyl n-butyl ketone or the ethyl propyl ketone.
8. preparation method according to claim 5 is characterized in that: described phosphoric acid ester is selected from a kind of in tributyl phosphate or the dibutyl phosphate.
9. preparation method according to claim 1 is characterized in that: the purifying phosphoric acid salts solution that the washings that washing procedure uses prepares from system itself, processing parameter: organic phase compares 3~10: 1 with water, 0 ℃~50 ℃ of temperature.
10. preparation method according to claim 1, it is characterized in that: used reverse-extraction agent is the alkaline aqueous solution of alkali such as salt of wormwood, yellow soda ash, potassium hydroxide, sodium hydroxide or alkaline-earth metal, organic phase and water be in a ratio of 2~8: 1, temperature is 20 ℃~50 ℃.
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CN103332665A (en) * | 2013-07-09 | 2013-10-02 | 清华大学 | Method used for removing impurity ions from phosphoric acid-containing organic solvent |
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DE19703884C2 (en) * | 1997-02-03 | 1999-04-29 | Bk Giulini Chem Gmbh & Co Ohg | Process for purifying wet process phosphoric acid |
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CN111777052A (en) * | 2020-07-24 | 2020-10-16 | 瓮福(集团)有限责任公司 | Fine desulfurization method for phosphoric acid |
CN111777052B (en) * | 2020-07-24 | 2023-04-25 | 瓮福(集团)有限责任公司 | Fine desulfurization method for phosphoric acid |
CN114988380A (en) * | 2022-06-28 | 2022-09-02 | 新希望化工投资有限公司 | Method for producing food-grade monopotassium phosphate and co-producing high-purity gypsum by using feed-grade calcium hydrophosphate |
CN115124009A (en) * | 2022-06-28 | 2022-09-30 | 新希望化工投资有限公司 | Method for producing magnesium hydrogen phosphate and potassium dihydrogen phosphate and co-producing high-purity gypsum by using calcium hydrogen phosphate reclaimed material |
CN115215310A (en) * | 2022-06-28 | 2022-10-21 | 新希望化工投资有限公司 | Impurity removal and recovery method of crude phosphoric acid |
CN115215310B (en) * | 2022-06-28 | 2023-10-27 | 新希望化工投资有限公司 | Impurity removal and recovery method for crude phosphoric acid |
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