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    • 1. 发明授权
    • Production of purified strong wet-process phosphoric acid
    • 生产纯净的强力湿法磷酸
    • US4435372A
    • 1984-03-06
    • US458403
    • 1983-01-17
    • Alva W. FrazierEwell F. Dillard
    • Alva W. FrazierEwell F. Dillard
    • C01B25/226C01B25/237C05B1/02C01B25/16
    • C01B25/226C01B25/237C05B1/02
    • The concentration of impurities in wet-process phosphoric acid limits the usefulness of the acid for the production of fertilizers, feedgrade phosphate and detergents. The aluminum, magnesium, and fluoride impurities are removed with the calcium sulfate hemihydrate filter cake by hydrolyzing and recycling the off-gas scrubber solutions in the presence of a ferric iron catalyst. The aluminum and magnesium are reduced to less than 0.1 percent in the acid product by the precipitation of (Ca,Mg)Al.sub.2 F.sub.8 .multidot.2H.sub.2 O, which is acid insoluble and suitable for storage with the byproduct calcium sulfate. Ferric iron also serves as a catalyst for the simultaneous precipitation of (Na,K).sub.2 SiF.sub.6. Subsequent additions of potassium as, for example, in the teachings of Gilbert (U.S. Pat. No. 3,338,675), can then be applied to obtain a purified phosphoric acid product suitable for most commercial applications.
    • 湿法磷酸中的杂质浓度限制了酸生产肥料,磷酸盐和去污剂的有用性。 通过在三价铁催化剂存在下水解和循环废气洗涤器溶液,用硫酸钙半水合物滤饼除去铝,镁和氟化物杂质。 酸性产物中的铝和镁通过析出(Ca,Mg)Al 2 F 8 x 2 H 2 O在酸性产物中降至小于0.1%,这是酸不溶性的,适合与副产物硫酸钙一起储存。 铁还用作(Na,K)2 SiF 6同时沉淀的催化剂。 随后可以例如在吉尔伯特(Gilbert)(美国专利号3,338,675)的教导中添加钾,以获得适合于大多数商业应用的纯化的磷酸产品。
    • 2. 发明授权
    • Production of urea phosphate
    • 生产尿素磷酸盐
    • US4461913A
    • 1984-07-24
    • US376809
    • 1982-05-10
    • Harry T. LewisEwell F. Dillard
    • Harry T. LewisEwell F. Dillard
    • C07F15/04C07C126/08C07C127/01
    • C07F15/04
    • A two-stage continuous crystallization process for production of urea phosphate by reaction of impure wet-process orthophosphoric acid (about 54 percent P.sub.2 O.sub.5) and urea with simultaneous addition of a selected acidifying agent (sulfuric acid, hydrochloric acid, or phosphoric acid) to clarified mother liquor used as recycle in the process. Addition of the acidifying agent decreases pH in the crystallization process whereby the solubility of a contaminating water-insoluble iron phosphate-urea salt [FeH.sub.3 (PO.sub.4).sub.2.2CO(NH.sub.2).sub.2 ] is increased, purity of the crystalline urea phosphate product is improved significantly, and the useful storage life of the recycle mother liquor is prolonged.
    • 通过不纯的湿法正磷酸(约54%P 2 O 5)和尿素的反应生产尿素磷酸盐的两阶段连续结晶方法,同时加入选定的酸化剂(硫酸,盐酸或磷酸)澄清 在这个过程中用作回收的母液。 酸化剂的添加降低了结晶过程中的pH值,由此污染的水不溶性磷酸铁 - 尿素盐[FeH 3(PO 4)2.2 CO(NH 2)2]的溶解度增加,结晶尿素磷酸盐产品的纯度显着提高 ,延长了循环母液的有效保存期。
    • 3. 发明授权
    • Stabilized ammonium orthophosphate suspensions
    • 稳定的正磷酸铵悬浮液
    • US5022913A
    • 1991-06-11
    • US399032
    • 1989-08-28
    • Ewell F. DillardJames R. Burnell
    • Ewell F. DillardJames R. Burnell
    • C05B7/00C05G3/00
    • C05G3/007C05B7/00
    • An improved batch process for the production, in equipment readily available at the fertilizer dealer level, of high-analysis stable ammonium orthophosphate suspension fertilizers effected by the ammoniation of solid intermediates derived from wet-process orthophosphoric acids or combinations of the solid intermediates with such wet-process type acid or other impure phosphoric acids. Fluorosilicic acid, a by-product of the phosphate industry which is readily available and relatively inexpensive, is utilized as a source of fluoride. The fluorosilicic acid is added to the batch formulation prior to the ammoniation step thereby allowing the fluorosilicic acid to be converted to ammonium fluoride. Subsequently, the metallic impurities are allowed to precipitate as fluoride compounds instead of the usual troublesome impurity-phosphate-water gels which have been identified as causing complete destruction of suspension fluidity during storage. This specific sequencing of process steps produce suspensions which can be stored for substantial periods of time without becoming thixotropic and/or so thick that they have to be diluted before use as is the case in suspensions prepared by prior art procedures.
    • 在化肥经销商层面上易于获得的设备中,通过氨化来自湿法正磷酸的固体中间体或固体中间体与这种湿润的固体中间体的氨化,得到了高分析稳定的正磷酸铵悬浮肥料 过程类型的酸或其他不纯的磷酸。 氟硅酸是磷酸盐工业的副产物,其易于获得并且相对便宜,被用作氟化物源。 在氨化步骤之前将氟硅酸加入批料中,由此使氟硅酸转化为氟化铵。 随后,允许金属杂质作为氟化物而不是常规麻烦的杂质 - 磷酸盐 - 水凝胶沉淀,这些凝胶已经被鉴定为在储存期间引起悬浮液流动性的完全破坏。 工艺步骤的这种特异性测序产生悬浮液,其可以储存相当长的一段时间,而不会变得触变和/或如此厚,使得它们在使用前必须如现有技术方法制备的悬浮液中那样稀释。
    • 5. 发明授权
    • Production of purified strong wet-process phosphoric acid
    • 生产纯净的强力湿法磷酸
    • UST103202I4
    • 1983-07-05
    • US417804
    • 1982-09-13
    • Alva W. FrazierEwell F. Dillard
    • Alva W. FrazierEwell F. Dillard
    • C01B25/226C01B25/237C05B1/02
    • C01B25/237C01B25/226C05B1/02
    • The concentration of impurities in wet-process phosphoric acid limits the usefulness of the acid for the production of fertilizers, feed-grade phosphate and detergents. The aluminum, magnesium, and fluoride impurities are removed with the calcium sulfate hemihydrate filter cake by hydrolyzing and recycling the off-gas scrubber solutions in the presence of a ferric iron catalyst. The aluminum and magnesium are reduced to less than 0.1 percent in the acid product by the precipitation of (Ca,Mg)Al.sub.2 F.sub.8.2H.sub.2 O, which is acid insoluble and suitable for storage with the byproduct calcium sulfate. Ferric iron also serves as a catalyst for the simultaneous precipitation of (Na,K).sub.2 SiF.sub.6. Subsequent additions of potassium as, for example, in the teachings of Gilbert (U.S. Pat. No. 3,338,675), can then be applied to obtain a purified phosphoric acid product suitable for most commercial applications. The added potassium serves two purposes in the 40 to 55 percent P.sub.2 O.sub.5 acid since ferric iron is reduced to 0.25 percent Fe.sub.2 O.sub.3 by the precipitation of Fe.sub.3 KH.sub.14 (PO.sub.4).sub.8.4H.sub.2 O and the SiF.sub.6.sup.= is reduced to about 0.2 percent by the precipitation of K.sub.2 SiF.sub.6. This subsequent precipitate contains about 50 percent P.sub.2 O.sub.5 and is as effective as superphosphate [Ca(H.sub.2 PO.sub.4).sub.2.H.sub.2 O] in supporting plant growth.