• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    Crude wet process phosphoric acid is pretreated, to ensure against impurity precipitation and objectionable coloration during the downstream processing, e.g., liquid-liquid extraction thereof, by first homogeneously admixing same with an impurity adsorbent, next mixing the liquid dispersion which results with a liquid suspension of a flocculating agent, maintaining the resulting admixture under nonshearing agitation until same separates into a flocculated phase and a liquid solution phase, and then separating therefrom the flocculated phase and a purified, product acid liquid solution phase.
    公开号:SU1181529A3
    申请号:SU802869458
    申请日:1980-01-23
    公开日:1985-09-23
    发明作者:Ниней Ги；Бутэн Жан；Шамбон Морис
    申请人:Рон-Пуленк Эндюстри (Фирма)；
    IPC主号:
    专利说明:

    The invention relates to methods for the purification of phosphoric acid obtained by the sulfuric acid decomposition of phosphate raw materials from calcium sulfate impurities and organic substances, which can be further used for liquid extraction with organic solvents.
    During the decomposition of phosphate raw materials with sulfuric acid, phosphoric acid is partially converted into impurities contained in the feedstock, as well as substances introduced during the pretreatment, acid decomposition and pulpation of the suspension. Impurities are inorganic and organic substances, for example, magnesium compounds of iron, aluminum, fluorides, silicates, etc. Organic substances contained in phosphoric acid get into it from the feedstock (humic acids) and as a result of physico-chemical processing of phi ( acids, amines, hydrocarbons). The concentration of impurities contained in phosphoric acid is saturated or supersaturated, and therefore the acid solution is in an unstable state.
    The subsequent processing of such an acid, for example, liquid extraction with organic solvents, causes a number of difficulties due to the precipitation of salts in the apparatus upon contact with organic solvents and the accumulation of organic impurities at the interface of two liquid phases with the formation of an intermediate colored organic phase. The devices must be periodically cleaned of impurity deposits, and the intermediate organic phase must be separated.
    A known method for the purification of phosphoric acid from organic impurities is followed by the separation of gypsum, which includes the treatment of acid with flocculant, which is polyacrylamide, and activated carbon. A purified acid is obtained, suitable for the production of sodium tripolyphosphate.
    In the activated carbon layer, more than 5% of PjOj is delayed. It is removed while the coal is regenerated by washing with soda lj.
    The disadvantage of this method is the loss of phosphoric acid in the coal layer, which is neutralized by soda.
    The closest to the invention to the technical essence and the achieved result is a method of purification of phosphoric acid from organic impurities, including treating the acid simultaneously with a reducing agent, an adsorbent (activated carbon), flocculant (polyacrylamide and crystalline mineral matter (gypsum), keeping the mixture under stirring for 0.5 h followed by separation of the precipitate of impurities from the product by decantation 2j.
    An acid is obtained in which the content of organic impurities is 0.85 - 1.3 units.5 suitable for the production of tripolyphosphate. However, the residual content of organic impurities does not allow the use of this acid for solvent extraction.
    The disadvantages of this method are also the additional consumption of reagents - a reducing agent and acid-insoluble crystallites and insufficient purification of the acid from organic impurities (purification degree 42.2 - 62.2%).
    The purpose of the invention is to increase the degree of purification of phosphoric acid from organic impurities and to simplify the process by eliminating the treatment of the acid with a reducing agent and insoluble in it with sulfates.
    The goal is achieved by the fact that according to the method of purification of phosphoric acid from organic impurities, the acid is sequentially treated first with an adsorbent for 0.5-2 hours, then with flocculant-polyacrylamide for 0.5 3 hours, the mixture is incubated with stirring, followed by separation of the product from sediment impurities by decantation. In this case, bentonite is used as an adsorbent.
    The proposed method allows to achieve a degree of purification from organic impurities of 75.5%. In addition, the acid is also purified from calcium sulfate,
    The table shows the effect of the sequential treatment of the acid with the adsorbent and flocculant on the residual content of organic impurities.
    The source acid contains g / l CaO and 16.6 g / l organic matter content of 2.25 units
    3
    (The unit of organic impurities is determined by a colorimetric indicator of a tributic phosphate solution containing organic impurities extracted from phosphoric acid. The comparison solution is pure 100% tributyl phosphate.)
    From the data given in the table, it follows that with an adsorbent and flocculant treatment time of less than 30 minutes, the degree of purification from organic impurities is insufficient, and with an adsorbent processing time of more than 2 hours and flocculation more than 3 hours, the degree of purification from organic impurities does not increase, and decantation rate decreases.
    Example 1. Phosphoric acid (28%; CaO 0.26%; 8041.7%, organic impurities 2 units), having a temperature of 40 ° C, is fed to a collection (At a flow rate of 500 l / h. The collection has a turbine agitator with a displaced center (800 revolutions per rev / m. This collection is fed with a suspension (5% by weight of a mixture of WYV bentonite (one part by weight) and FGNFR4 bentonite (two weight parts), in phosphoric acid at a flow rate of 20 l / h. Hold 30 min. the slurry is guided sequentially into a homogenizer and a holding tank, equipped with a sloping three 5294
    with a pastel mixer (rotation speed 24 rpm), and an aqueous suspension of FlocogyT LB37 flocculant of 1 g / l concentration at a flow rate of 1 l / h is added to the homogenate at a flow rate of 1 l / h. From the bottom of the holding tank after 30 min, the suspension is fed to a decanter equipped with a scraper device (0.2 rpm). From the bottom of the decanter it is removed: from the coagulum separated from phosphoric acid, which in turn is combined with the original acid. From the top part, purified acid is removed,%, PjOj 28; CaO 0.24; 1.6; organic impurities 0.7 units.
    Example 2. Phosphoric acid in example 1 (caO 4.9 g / l, 864 16.6 g / l, organic impurities 2.25 units) are treated with the same reagents as in example 1.
    The mixture of acid and adsorbent is first stirred for 15 s at a speed of 310 rpm, then 29 min. 45 s with a speed of 210 rpm. Then flocculants are introduced and mixed for 2 minutes at a speed of 100 rpm and 45 minutes at a speed of 100 rpm. After decanting for 120 minutes, the acid contains, g / l: CaO 1.23; 50 organic impurities 0,55 units.
    The invention provides an acid suitable for solvent extraction with organic solvents.
    20
    20
    1.05
    权利要求:
    Claims (2)
    [1]
    ,1. METHOD FOR CLEANING PHOSPHORIC ACID FROM ORGANIC IMPURITIES, including treating the acid with an adsorbent and a flocculant, using polyacrylamide, keeping the resulting suspension under stirring, followed by separation of the product from the precipitate of impurities by decantation, characterized in that, in order to increase the degree of purification from impurities and simplify the method by eliminating the treatment of the acid with reducing agents and insoluble sulfates in it, the acid is sequentially treated first with an adsorbent for 0.5 t 2 hours, then flocculant for 0.5 to 3 hours. S
    [2]
    2. The method according to p. ^ Characterized in that bentonite is used as an adsorbent.
    (L s
    SL é ζ ©>
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    同族专利:
    公开号 | 公开日
    US4369169A|1983-01-18|
    IT8047673D0|1980-01-22|
    ATA38080A|1991-05-15|
    ZA80411B|1981-01-28|
    BR8000411A|1980-10-21|
    GR73131B|1984-02-07|
    GB2039869B|1983-01-26|
    FR2447347A1|1980-08-22|
    CA1134119A|1982-10-26|
    FI67205C|1985-02-11|
    MA18711A1|1980-10-01|
    EG14670A|1984-06-30|
    JPS55104908A|1980-08-11|
    NL8000439A|1980-07-28|
    IL59186D0|1980-05-30|
    ES487930A1|1980-07-16|
    BE881307A|1980-07-23|
    GB2039869A|1980-08-20|
    MX7288E|1988-04-15|
    IT1188894B|1988-01-28|
    FI800183A|1980-07-25|
    FR2447347B1|1983-02-04|
    DE3002359A1|1980-07-31|
    FI67205B|1984-10-31|
    IN151181B|1983-03-05|
    IL59186A|1983-12-30|
    DE3002359C2|1982-05-19|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    US2968528A|1957-07-01|1961-01-17|Int Minerals & Chem Corp|Process for producing clarified phosphoric acid|
    US2936888A|1958-07-07|1960-05-17|Int Minerals & Chem Corp|Production of clarified acidic phosphatic solutions|
    US3186793A|1960-10-10|1965-06-01|Internat Minerals & Chemicals|Clarification of acidic phosphatic solutions|
    US3099622A|1960-10-25|1963-07-30|Int Minerals & Chem Corp|Production of clarified acidic phosphatic solutions|
    NL295743A|1962-07-25|
    GB1103224A|1964-07-28|1968-02-14|Marchon Products Ltd|Improvements in the manufacture of phosphoric acid|
    US3644091A|1970-03-17|1972-02-22|Exxon Research Engineering Co|Clarification of phosphoric acid|
    AU7108374A|1973-12-21|1976-01-15|Fertiliazantes Fosfatados Mexi|Phosphoric acid|
    DE2447390C3|1974-10-04|1983-11-17|Hoechst Ag, 6230 Frankfurt|Process for purifying wet phosphoric acid|
    UST971006I4|1977-09-14|1978-06-06|Tennessee Valley Authority|Purification of phosphoric acid solutions|
    US4256570A|1979-03-19|1981-03-17|International Minerals & Chemical Corporation|Purification of phosphoric acid|FR2507170A2|1976-02-26|1982-12-10|Ind Chimiques Maghrebines|Phosphoric acid clarification and defluorination - by treatment with pre-wetted clay|
    US4291005A|1979-04-23|1981-09-22|American Cyanamid Company|Settling out suspended solids in phosphoric acid product solutions|
    DE3212675A1|1982-04-05|1983-10-06|Hoechst Ag|METHOD FOR SEPARATING HEAVY METAL COMPOUNDS FROM INTERMEDIATE PRODUCTS OF THE FABRICATION OF PHOSPHOROUS AGENTS|
    US4585636A|1984-10-17|1986-04-29|Negev Phosphates Ltd.|Process for the manufacture of purified phosphoric acid|
    US4643883A|1986-01-22|1987-02-17|International Minerals & Chemical Corp.|Method of decolorizing wet process phosphoric acid|
    DE3806822A1|1988-03-03|1989-09-14|Hoechst Ag|CONTINUOUS PROCESS FOR COMPLETELY REMOVING ORGANIC IMPURITIES AND COMPLETELY DISCHARGING PRE-CLEANED WET PHOSPHORIC ACIDS|
    DE3913853A1|1989-04-27|1990-10-31|Hoechst Ag|METHOD FOR PROCESSING PHOSPHORIC ACID|
    US9187327B2|2011-01-04|2015-11-17|Nalco Company|Phosphoric acid production gypsum filtration flocculant pre-dilutionwith post-filtration phosphoric acid|
    JP6060398B2|2014-03-31|2017-01-18|日本碍子株式会社|Method for removing phosphorus in wastewater and apparatus for removing phosphorus in wastewater|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    FR7901752A|FR2447347B1|1979-01-24|1979-01-24|
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