CN106348273B - A kind of extractant and its extracting process of hydrochloric acid legal system industrial phosphoric acid - Google Patents
A kind of extractant and its extracting process of hydrochloric acid legal system industrial phosphoric acid Download PDFInfo
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- CN106348273B CN106348273B CN201610686625.7A CN201610686625A CN106348273B CN 106348273 B CN106348273 B CN 106348273B CN 201610686625 A CN201610686625 A CN 201610686625A CN 106348273 B CN106348273 B CN 106348273B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/46—Preparation involving solvent-solvent extraction
- C01B25/461—Preparation involving solvent-solvent extraction the phosphoric acid present in the medium obtained after reaction being first extracted from the liquid phase formed or separated then re-extracted as free acid by using water or as a phosphate by using a basic compound
- C01B25/465—Preparation involving solvent-solvent extraction the phosphoric acid present in the medium obtained after reaction being first extracted from the liquid phase formed or separated then re-extracted as free acid by using water or as a phosphate by using a basic compound the extracting agent being an ester or a mixture of esters
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Abstract
The invention discloses the extractant and extraction process of hydrochloric acid legal system industrial phosphoric acid, its component and mass fraction are：One or both of tributyl phosphate or three butoxyethyl phosphates 10%~50%, one or more 15%~40% in n-butanol, isooctanol, cyclohexanol, isopropanol, isoamyl alcohol, one or both of n-butyl ether, isopropyl ether, Di Iso Propyl Ether 10%~30%, one or more 5%~30% in high-carbon ketone, fatty amine or quaternary ammonium salt, the one or more 1%~10% in Oleth phosphate, sodium octyl sulfate, α sodium olefin sulfonates, sodium lignin sulfonate, stearyl sulfosuccinamic acid disodium, Texapon Special.The extractant applicable elements of the present invention are wide, and solvent loss is small, and recovery is convenient, and extraction yield is up to more than 80%.
Description
Technical field
The present invention relates to phosphoric acid preparing technical field, and in particular to when preparing industrial phosphoric acid using hydrochloric acid method used one
Kind composite extractant.
Background technology
Phosphoric acid is a kind of important industrial chemicals, is widely used in the industries such as chemical fertilizer, food, coating, electronics industry.Phosphoric acid
Mainly there are two kinds of production technologies of Re Fa and wet method.Thermal phosphoric acid is after producing yellow phosphorus with electric furnace process, then it is oxidized, absorb and obtain,
Gained phosphoric acid purity is higher, but high to ingredient requirement, and energy consumption is big.Phosphoric acid by wet process is with sour decomposing phosphate rock, after separation of solid and liquid
Obtain phosphoric acid, adaptable wide, low power consumption and other advantages.Typical phosphoric acid by wet process is come decomposing phosphate rock, technics comparing with sulfuric acid
Maturation, but China's sulphur inadequate resource, sulphur is in short supply, and many enterprises process units by-product hydrochloric acid, cheap, market
It is not smooth, therefore develop and replace sulfuric acid decomposition phosphorus ore that there is very high practical value to produce the technique of phosphoric acid by wet process with hydrochloric acid.
Chinese patent ZL200510019049.2 discloses a kind of hydrochloric acid decomposing medium and low grade process industry phosphoric acid
Method, this method use calcium phosphate+ forage with decomposing phosphate rock by chlorhydric acid after separation of solid and liquid, concentrate, then with tributyl phosphate with
Isopropyl ether extracts, then concentrates, and decolourizes, 85% PHOSPHORIC ACID TECH.GRADE is made.But extractant used in this method can preferentially extract
Take out Fe3+With Cl-The complex of formation, cause finished product phosphoric acid Fe3+Content is higher；On the other hand, to be concentrated twice twice
Extract, and to be cooled to less than 10 DEG C after concentrating for second to carry out second of extraction, cause energy consumption higher.Investment is big, removes
The shortcomings of miscellaneous efficiency is low, dangerous big, high energy consumption, is unfavorable for large-scale industrial production.Chinese patent 201110006702 is public
Opened a kind of method of the step of hydrochloric acid method one extraction from mid low grade phosphate rock process industry phosphoric acid, the method be with decomposing phosphate rock by chlorhydric acid,
Monocalcium chlorophosphate is first prepared, and then adds phosphoric acid,diluted mashing, after filtered purification, then is beaten and dissolves with hydrochloric acid, with phosphoric acid
Tributyl extracts, concentrated, decolourizing and to obtain industrial phosphoric acid, and the method has that extraction efficiency is not high, loss is larger etc. asks in actual applications
Topic, so far there are no realizes industrialized production.
It is to select a kind of suitable extractant with the key of hydrochloric acid legal system industrial phosphoric acid, is capable of the extraction phosphorus of high selectivity
Acid, and being particularly substantial amounts of chlorion to other impurities ion has repellency.
The content of the invention
It is an object of the invention to provide a kind of extractant that industrial phosphoric acid is prepared suitable for hydrochloric acid decomposition method, the extractant
There is very high selectivity to phosphoric acid, a large amount of existing chlorions in system are not extracted substantially, and raw phosphoric acid is only needed by de-
Fluorine decolourizes directly be extracted after pretreatment, without being removed in advance to other impurity metal ions, enormously simplify work
Skill.
The present invention implementation be：A kind of hydrochloric acid method prepares the extractant of industrial phosphoric acid, and component and mass fraction are：Phosphorus
One or both of sour tributyl or three butoxyethyl phosphates 10%~50%, it is n-butanol, isooctanol, cyclohexanol, different
One or both of one or more 15%~40%, n-butyl ether, isopropyl ether, Di Iso Propyl Ether in propyl alcohol, isoamyl alcohol
10%~30%, the one or more 5%~30% in high-carbon ketone, fatty amine or quaternary ammonium salt, Oleth phosphate,
In sodium octyl sulfate, α-sodium olefin sulfonate, sodium lignin sulfonate, stearyl sulfosuccinamic acid disodium, Texapon Special
One or more 1%~10%.
The high-carbon ketone is methyl isopropyl ketone, isobutyrone, hexone or cyclohexanone.
The fatty amine or season be by salt：Dioctadecyl dimethyl ammonium chloride, hexadecyltrimethylammonium chloride, ten alkane
Base dimethyl tertiary amine, trioctylamine or tetramethyl DBSA ammonium.
Compared with prior art, advantage of the invention is that：
1st, a kind of composite extractant for preparing industrial phosphoric acid the present invention be directed to hydrochloric acid method and developing, it is capable of the extraction of selectivity
Take phosphoric acid and hardly carry chlorion secretly, laid a good foundation for the industrial applications of hydrochloric acid legal system phosphoric acid.
2nd, composite extractant of the invention has high repellency to impurity anions, metal ion, thus raw material acid is pre-
Desulfurization, removing heavy-metal are not needed in handling process, simple defluorinate need to be only carried out to raw material acid and decolourizes to enter after pretreatment
Row extracting operation, and defluorinate also only needs suitably to reduce free fluorine, and this just enormously simplify pre-treatment step, reduce life
Produce cost.
3rd, using the extractant of the present invention, for raw phosphoric acid after extracting, washing, directly concentration can obtain composite industrial level phosphorus
The Standard of acid.
4th, after esters, alcohols, ethers in being formulated are mixed in the ratio described in claim 1, its extraction yield is significantly
Improving, phosphoric acid extraction rate reaches more than 80%, and with single extractant phosphoric acid extraction rate 10~50%；The composite extractant pair
Metal ion, and Ca2+There is obvious repellency, and with single extractant then to Ca2+Without obvious repellency.
5th, the boiling point of extractant each component is close and moderate, water-soluble relatively low, and solvent loss is small, and recovery is convenient, can be in room
Temperature is lower to be extracted.
6th, extractant of the invention can extract at room temperature, save energy consumption and solvent loss.
The purpose of the present invention is implemented to comprise the following steps：
(1) acidolysis ore deposit：Hydrochloric acid is added in acidolysis groove, stirs lower addition ground phosphate rock, reaction 0.1~3 is small at 40~60 DEG C
When.Hydrochloric acid dosage is 1.0~1.2 times of required hydrochloric acid theoretical amount when the CaO in ground phosphate rock reacts completely with hydrochloric acid.Reaction terminates
After be filtrated to get acid hydrolysis solution.
(2) pre-process：Acid hydrolysis solution after clarification is concentrated into H3PO4Mass fraction 10~30% or so, adds appropriate carbonic acid
Sodium defluorinate, after 70 DEG C are reacted 2 hours, sedimentation, take supernatant liquor to add decolorizing with activated carbon, filtering, obtain thick purifying phosphoric acid solution.
(3) extract：Thick purifying phosphoric acid solution adverse current obtained by step (2) is added to the extractant of the present invention, extractant：Slightly
Volume ratio=0.5~5 of purifying phosphoric acid：1, six stage countercurrent extractions, work of the extraction phase dissolved with sodium carbonate are carried out at normal temperatures
Industry level phosphoric acid carries out four-stage counter-current washing, extraction phase：Wash phase volume ratio=10~50：1.
(4) it is stripped：Extraction phase overflow after washing enters back extraction groove, according to extraction phase：Aqueous phase=6:1 volume ratio adds
Soft water carries out four-stage counter-current back extraction, H in the strip liquor of acquisition3PO4Mass fraction 20% or so.
(5) purification eventually：Sulfate radical and fluorinion concentration in strip liquor obtained by determination step (4), add stoichiometry 100%
Barium carbonate, reaction 3 hours after, sedimentation, extract supernatant liquor, add activated carbon decolorizing, filtering, filtrate is concentrated to phosphoric acid matter
Fraction is measured up to 85%, produces industrial phosphoric acid.
In described step (3), extractant：Volume ratio=0.5~5 of thick purifying phosphoric acid：1；Extraction phase：Dissolved with carbonic acid
The volume ratio of the PHOSPHORIC ACID TECH.GRADE of sodium is 10~50：1.More preferably in step (3), extractant：The body of thick purifying phosphoric acid
Product ratio=2：1；Extraction phase：The volume ratio of PHOSPHORIC ACID TECH.GRADE dissolved with sodium carbonate is 25：1.
Embodiment
The effect of extracting of extractant of the present invention is described further below by specific embodiment, skill of the invention
Art scheme is not limited with embodiment.Mid low grade phosphate rock powder composition (mass percent, %) such as following table used in following embodiments:
Embodiment 1
Take the hydrochloric acid that mass concentration is 21% or so to add in acidolysis groove, stir lower addition ground phosphate rock, hydrochloric acid dosage is phosphorus
1.2 times of required hydrochloric acid theoretical amount when CaO in miberal powder reacts completely with hydrochloric acid.Lower 50 DEG C of strong stirring reacts 2 hours, reaction
Filtered after end, obtain acid hydrolysis solution.
Acid hydrolysis solution after clarification is concentrated into H3PO4Mass fraction 20% or so, proper amount of sodium carbonate defluorinate is added, at 70 DEG C
After reaction 2 hours, sedimentation, take supernatant liquor to add decolorizing with activated carbon, filtering, obtain thick purifying phosphoric acid solution.
Above-mentioned thick purifying phosphoric acid solution adverse current is added to the extractant of the present invention, extractant：The volume ratio of thick purifying phosphoric acid
=1：1, six stage countercurrent extractions are carried out at normal temperatures.The extractant each component mass fraction is：Tributyl phosphate 30%, positive fourth
Alcohol 40%, isopropyl ether 20%, hexadecyltrimethylammonium chloride 5%, cyclohexanone 5%.Extraction phase is used dissolved with sodium carbonate
85% industrial phosphoric acid carries out four-stage counter-current washing, extraction phase：Wash phase volume ratio=25：1.
Extraction phase overflow after washing enters back extraction groove, according to extraction phase：Aqueous phase=6:1 volume ratio adds soft water and carried out
Four-stage counter-current is stripped, H in the strip liquor of acquisition3PO4Mass fraction 20%.
Sulfate radical and fluorinion concentration in strip liquor obtained by above-mentioned steps are determined, adds the barium carbonate of stoichiometry 100%,
After reaction 3 hours, sedimentation, supernatant liquor is extracted, add activated carbon decolorizing, filtering, filtrate is concentrated to phosphoric acid quality fraction and reached
85%, produce industrial phosphoric acid.
The present embodiment phosphoric acid extraction rate 81.3%, loss of extractant is calculated, be 85% finished product phosphoric acid consumption extraction per ton after conversion
Take agent 38.4kg.
The relevant component content (mass percent, %) of industrial phosphoric acid obtained by the implementation case see the table below：
Embodiment 2
Take the hydrochloric acid that mass concentration is 21% or so to add in acidolysis groove, stir lower addition ground phosphate rock, hydrochloric acid dosage is phosphorus
1.1 times of required hydrochloric acid theoretical amount when CaO in miberal powder reacts completely with hydrochloric acid.The lower 60 DEG C of reactions of strong stirring 0.5 hour, instead
Filtered after should terminating, obtain acid hydrolysis solution.
Acid hydrolysis solution after clarification is concentrated into H3PO4Mass fraction 25% or so, proper amount of sodium carbonate defluorinate is added, at 70 DEG C
After reaction 2 hours, sedimentation, take supernatant liquor to add decolorizing with activated carbon, filtering, obtain thick purifying phosphoric acid solution.
Above-mentioned thick purifying phosphoric acid solution adverse current is added to the extractant of the present invention, extractant：The volume ratio of thick purifying phosphoric acid
=2：1, six stage countercurrent extractions are carried out at normal temperatures.The extractant each component mass fraction is：Tributyl phosphate 15%, isopropyl
Alcohol 30%, cyclohexanone 30%, n-butyl ether 20%, DBSA ammonium 5%.85% work of the extraction phase dissolved with sodium carbonate
Industry phosphoric acid carries out four-stage counter-current washing, extraction phase：Wash phase volume ratio=30：1.
Extraction phase overflow after washing enters back extraction groove, according to extraction phase：Aqueous phase=6:1 volume ratio adds soft water and carried out
Four-stage counter-current is stripped, H in the strip liquor of acquisition3PO4Mass fraction 22%.
Sulfate radical and fluorinion concentration in strip liquor obtained by above-mentioned steps are determined, adds the barium carbonate of stoichiometry 100%,
After reaction 3 hours, sedimentation, supernatant liquor is extracted, add activated carbon decolorizing, filtering, filtrate is concentrated to phosphoric acid quality fraction and reached
85%, produce industrial phosphoric acid.
The present embodiment phosphoric acid extraction rate 84.62%, loss of extractant is calculated, be 85% finished product phosphoric acid consumption extraction per ton after conversion
Take agent 36.1kg.
The relevant component content (mass percent, %) of industrial phosphoric acid obtained by the implementation case see the table below：
Embodiment 3
Take the hydrochloric acid that mass concentration is 21% or so to add in acidolysis groove, stir lower addition ground phosphate rock, hydrochloric acid dosage is phosphorus
1.05 times of required hydrochloric acid theoretical amount when CaO in miberal powder reacts completely with hydrochloric acid.The lower 50 DEG C of reactions of strong stirring 2 hours, instead
Filtered after should terminating, obtain acid hydrolysis solution.
Acid hydrolysis solution after clarification is concentrated into H3PO4Mass fraction 20% or so, proper amount of sodium carbonate defluorinate is added, at 70 DEG C
After reaction 2 hours, sedimentation, take supernatant liquor to add decolorizing with activated carbon, filtering, obtain thick purifying phosphoric acid solution.
Above-mentioned thick purifying phosphoric acid solution adverse current is added to the extractant of the present invention, extractant：The volume ratio of thick purifying phosphoric acid
=3：1, six stage countercurrent extractions are carried out at normal temperatures.The extractant each component mass fraction is：N-butanol 40%, diisobutyl
Ketone 30%, n-butyl ether 20%, Oleth phosphate 10%.85% industrial phosphorus of the extraction phase dissolved with sodium carbonate
Acid carries out four-stage counter-current washing, extraction phase：Wash phase volume ratio=20：1.
Extraction phase overflow after washing enters back extraction groove, according to extraction phase：Aqueous phase=6:1 volume ratio adds soft water and carried out
Four-stage counter-current is stripped, H in the strip liquor of acquisition3PO4Mass fraction 20%.
Sulfate radical and fluorinion concentration in strip liquor obtained by above-mentioned steps are determined, adds the barium carbonate of stoichiometry 100%,
After reaction 3 hours, sedimentation, supernatant liquor is extracted, add activated carbon decolorizing, filtering, filtrate is concentrated to phosphoric acid quality fraction and reached
85%, produce industrial phosphoric acid.
The present embodiment phosphoric acid extraction rate 86.23%, loss of extractant is calculated, be 85% finished product phosphoric acid consumption extraction per ton after conversion
Take agent 41.3kg.
The relevant component content (mass percent, %) of industrial phosphoric acid obtained by the implementation case see the table below：
Claims (6)
- A kind of 1. extractant of hydrochloric acid legal system industrial phosphoric acid, it is characterised in that the raw material composition including following percetage by weight：Phosphorus One or both of sour tributyl or three butoxyethyl phosphates 10%~50%；N-butanol, isooctanol, cyclohexanol, isopropyl One or more 15%~40% in alcohol, isoamyl alcohol；One or both of n-butyl ether, isopropyl ether, Di Iso Propyl Ether 10%~ 30%；One or more 5%~30% in high-carbon ketone, fatty amine or quaternary ammonium salt；Oleth phosphate, octyl sulfate Sodium, α-sodium olefin sulfonate, sodium lignin sulfonate, stearyl sulfosuccinamic acid disodium, one kind in Texapon Special or Several 1%~10%.
- 2. the extractant of hydrochloric acid legal system industrial phosphoric acid according to claim 1, it is characterised in that the high-carbon ketone is methyl Isopropyl-ketone, isobutyrone, hexone or cyclohexanone.
- 3. the extractant of hydrochloric acid legal system industrial phosphoric acid according to claim 1, it is characterised in that the fatty amine or quaternary ammonium Salt is：Dioctadecyl dimethyl ammonium chloride, hexadecyltrimethylammonium chloride, ten alkyl dimethyl tertiary amines or trioctylamine or four Methyl DBSA ammonium.
- 4. the extraction process of the extractant using the hydrochloric acid legal system industrial phosphoric acid according to claim 1 or 2 or 3, its feature It is,（1）Acidolysis ore deposit：Hydrochloric acid is added in acidolysis groove, lower addition ground phosphate rock is stirred, is reacted 0.1 ~ 3 hour at 40 ~ 60 DEG C, hydrochloric acid Dosage is 1.0 ~ 1.2 times of required hydrochloric acid theoretical amount when CaO and the hydrochloric acid in ground phosphate rock react completely, filtering after reaction terminates, Clarification obtains acid hydrolysis solution；（2）Pretreatment：Acid hydrolysis solution after clarification is concentrated into H3PO4Mass fraction 10 ~ 30%, sodium carbonate defluorinate is added, at 70 DEG C After reaction 2 hours, sedimentation, take supernatant liquor to add decolorizing with activated carbon, filtering, obtain thick purifying phosphoric acid solution；（3）Extraction：Thick purifying phosphoric acid solution adverse current obtained by step (2) is added to the salt according to claim 1 or 2 or 3 The extractant of acid system industrial phosphoric acid, carries out six stage countercurrent extractions at normal temperatures, and obtained extraction phase is used dissolved with sodium carbonate Industrial phosphoric acid carries out four-stage counter-current washing, H in the industrial phosphoric acid dissolved with sodium carbonate3PO4Mass fraction 10 ~ 30%；（4）Back extraction：Extraction phase overflow after washing enters back extraction groove, according to extraction phase：Aqueous phase=6：1 volume ratio adds soft water Four-stage counter-current back extraction is carried out, H in the strip liquor of acquisition3PO4Mass fraction in 15%-25%；（5）Purification eventually：Sulfate radical and fluorinion concentration in strip liquor obtained by determination step (4), add the carbon of stoichiometry 100% Sour barium, after reacting 3 hours, sedimentation, supernatant liquor is extracted, add activated carbon decolorizing, filtering, filtrate is concentrated to phosphoric acid quality and divided Number produces industrial phosphoric acid up to 85%.
- 5. the extraction process of the hydrochloric acid legal system industrial phosphoric acid described in claim 4, it is characterised in that step（3）In, extractant： Volume ratio=0.5 ~ 5 of thick purifying phosphoric acid：1；Extraction phase：The volume ratio of PHOSPHORIC ACID TECH.GRADE dissolved with sodium carbonate is 10 ~ 50：1.
- 6. the extraction process of the hydrochloric acid legal system industrial phosphoric acid described in claim 5, it is characterised in that step（3）In, extractant： Volume ratio=2 of thick purifying phosphoric acid：1；Extraction phase：The volume ratio of PHOSPHORIC ACID TECH.GRADE dissolved with sodium carbonate is 25：1.
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| 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 |
| CN109133241B (en) * | 2018-09-18 | 2024-04-12 | 神木富油能源科技有限公司 | FU type composite extractant suitable for coal tar hydrogenation wastewater treatment and application of FU type composite extractant in coal tar hydrogenation wastewater treatment |
| CN110252274B (en) * | 2019-06-14 | 2022-09-02 | 湖北三宁碳磷基新材料产业技术研究院有限公司 | Preparation method of catalyst for synthesizing diphenyl carbonate by ester exchange |
| CN112850675A (en) * | 2021-02-04 | 2021-05-28 | 武汉工程大学 | Method for extracting chloride ions from wet-process phosphoric acid solution by hydrochloric acid method |
| CN114835094B (en) * | 2022-03-17 | 2024-04-26 | 中国科学院过程工程研究所 | Method for preparing wet-process phosphoric acid and calcium sulfate by acidolysis and in-situ extraction of phosphorus from phosphorus ore |
| CN115089999B (en) * | 2022-06-08 | 2024-05-10 | 广东工业大学 | Application of composite extractant in recycling waste acid in waste aluminum chemical polishing solution |
| CN115475411A (en) * | 2022-09-30 | 2022-12-16 | 武汉工程大学 | Method for extracting and purifying wet-process phosphoric acid by using isopropyl ether-fatty alcohol mixed solution |
| CN116216672A (en) * | 2022-12-16 | 2023-06-06 | 贵州芭田生态工程有限公司 | Method for removing sulfate radical in phosphoric acid preparation process |
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| US3367749A (en) * | 1963-02-20 | 1968-02-06 | Monsanto Co | Purifying phosphoric acid using an amine extractant |
| EP0176613A1 (en) * | 1984-10-01 | 1986-04-09 | East China Institute Of Chemical Technology | A process for producing phosphoric acid and/or phosphates from wet-process phosphoric acid and an extractant used therein |
| CN1003909B (en) * | 1986-09-19 | 1989-04-19 | 华中师范大学 | A kind of novel liquid extraction agent and extracting process thereof of phosphoric acid extraction |
| RU2208576C1 (en) * | 2002-05-14 | 2003-07-20 | Открытое акционерное общество "Научно-исследовательский институт по удобрениям и инсектофунгицидам им. проф. Я.В.Самойлова" | Organic extractant restoration process in pure phosphoric acid production |
| CN1657407A (en) * | 2004-02-16 | 2005-08-24 | 申士富 | Mixed extractant of purification wet phosphoric acid and dilute phosphoric dechlorine technology |
| CN101857216B (en) * | 2010-06-29 | 2012-04-25 | 贵州川恒化工有限责任公司 | Method for extracting and purifying wet-process phosphorous acid to produce industrial-grade phosphorous acid |
| CN102616765B (en) * | 2012-01-11 | 2014-01-01 | 吴杰 | Method of using composite extracting agent for extraction and refining of phosphoric acid prepared through wet process |
| CN104069646B (en) * | 2014-06-11 | 2016-01-06 | 陈锂 | A kind of extractant of purification of wet process phosphoric acid and the method with its extraction phosphoric acid by wet process |
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