WO2016074348A1 - Procédé de préparation d'acide hypophosphoreux avec du ferrophosphore - Google Patents

Procédé de préparation d'acide hypophosphoreux avec du ferrophosphore Download PDF

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Publication number
WO2016074348A1
WO2016074348A1 PCT/CN2015/071520 CN2015071520W WO2016074348A1 WO 2016074348 A1 WO2016074348 A1 WO 2016074348A1 CN 2015071520 W CN2015071520 W CN 2015071520W WO 2016074348 A1 WO2016074348 A1 WO 2016074348A1
Authority
WO
WIPO (PCT)
Prior art keywords
hypophosphorous acid
phosphorus
ferrophosphorus
acid
sulfuric acid
Prior art date
Application number
PCT/CN2015/071520
Other languages
English (en)
Chinese (zh)
Inventor
周骏宏
孙成斌
阮代锬
罗骏
张娇
王娇
熊玉霞
方进
房群莉
刘方方
张秀
Original Assignee
周骏宏
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 周骏宏 filed Critical 周骏宏
Publication of WO2016074348A1 publication Critical patent/WO2016074348A1/fr

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Classifications

    • 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
    • C01B25/165—Hypophosphorous acid; Salts thereof

Definitions

  • the invention belongs to the field of chemical industry, and is a method for producing hypophosphorous acid by using an electro-furnace method to produce phosphorus iron (or similar substance) produced by yellow phosphorus as a raw material.
  • hypophosphorous acid also known as hypophosphorous acid
  • hypophosphorous acid is reductive and widely used in electroless plating, or in the production of nickel-hydrogen battery cathodes, food production, organic synthesis, medicine, and the like.
  • the conventional preparation method of hypophosphorous acid generally adopts a two-step preparation method of preparing soluble hypophosphite and then acidifying by metathesis reaction to obtain hypophosphorous acid.
  • yellow phosphorus is reacted with barium hydroxide to form a calcium hypophosphite solution, and then sulfuric acid is added to form barium sulfate precipitate, and the precipitate is filtered to obtain hypophosphorous acid.
  • sulfuric acid is added to form barium sulfate precipitate, and the precipitate is filtered to obtain hypophosphorous acid.
  • the reaction of yellow phosphorus with lime, caustic soda, sodium hypophosphite, ion-exchange membrane electrodialysis, ion exchange, electrolysis, etc. to produce hypophosphorous acid.
  • Phosphorus iron is a kind of waste slag produced in the production of phosphorus chemical industry or a substance containing phosphorus and iron, such as yellow phosphorus, calcium phosphate fertilizer by-product phosphorus iron.
  • Phosphorus iron generally has a metallic luster of silver-gray (or yellowish) solids, which is relatively hard and brittle and has a certain ferromagnetism. Through the chemical element analysis of ferrophosphorus, the results show that the largest content is iron, iron accounted for 55% to 75%, followed by phosphorus, and phosphorus accounts for 10% to 20%.
  • ferrophosphorus contains a large amount of iron and phosphorus, its chemical properties are extremely stable. It does not oxidize slowly in the air like iron. It does not oxidize white smoke or even burn in the air like phosphorus. Phosphorus can be It persists in the air for a long time. It is indicated that there is no single state of phosphorus and iron in the ferrophosphorus. X-ray diffraction analysis of the ferrophosphorus showed that there were two forms of Fe 2 P and Fe 3 P in the ferrophosphorus.
  • the conventional utilization of ferrophosphorus can be used as an alloying agent and deoxidizer for steelmaking.
  • the chemical utilization is generally carried out by mixing soda ash with ferrophosphorus powder and then calcining at a high temperature, then leaching with water, and the filtrate is concentrated, crystallized and dried to obtain trisodium phosphate. The product, the filter residue is washed and dried to obtain iron oxide.
  • hypophosphorous acid that is, the reaction of yellow phosphorus with lime milk and soda ash, to produce sodium hypophosphite, and then converted to hypophosphorous acid.
  • the reaction of yellow phosphorus with alkali is a disproportionation reaction, which causes disproportionation of phosphine while producing hypophosphite, resulting in a decrease in yield and an increase in the difficulty of treating phosphine.
  • the chemical nature of yellow phosphorus is active and easily reacts with air, which also increases the difficulty of production control.
  • ferrophosphorus As a by-product of yellow phosphorus, ferrophosphorus is generally used as iron-containing waste, and its economic benefits are very low. There has been no better technology to increase the economic value of ferrophosphorus.
  • the invention solves the defects of low utilization value of the original ferrophosphorus, less utilization channels, or long processing process, and the disadvantages of the production method of the hypophosphorous acid and the single material selection and the high processing cost, and proposes a new utilization mode of the phosphorus iron and A new method for the manufacture of hypophosphorous acid, which has the characteristics of low cost, full utilization of waste resources or by-products, and simple process.
  • the technical solution adopted by the present invention is: a method for preparing hypophosphorous acid using phosphorus iron, comprising the following steps:

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Removal Of Specific Substances (AREA)
  • Fertilizers (AREA)

Abstract

L'invention concerne un procédé de préparation d'acide hypophosphoreux avec du ferrophosphore qui consiste à : pulvériser le ferrophosphore, effectuer un trempage à l'acide sulfurique, filtrer, extraire, éliminer l'acide sulfurique, extraire en retour et concentrer afin d'obtenir l'acide hypophosphoreux. Le procédé utilise les sous-produits ou les déchets de production de phosphore dans l'industrie chimique et présente les caractéristiques d'un faible coût, d'un procédé simple et d'une bonne qualité de produit.
PCT/CN2015/071520 2014-11-15 2015-01-26 Procédé de préparation d'acide hypophosphoreux avec du ferrophosphore WO2016074348A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN201410646509.3A CN104386659B (zh) 2014-11-15 2014-11-15 一种用磷化工废料生产次磷酸的方法
CN201410646509.3 2014-11-15

Publications (1)

Publication Number Publication Date
WO2016074348A1 true WO2016074348A1 (fr) 2016-05-19

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Application Number Title Priority Date Filing Date
PCT/CN2015/071520 WO2016074348A1 (fr) 2014-11-15 2015-01-26 Procédé de préparation d'acide hypophosphoreux avec du ferrophosphore

Country Status (2)

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CN (1) CN104386659B (fr)
WO (1) WO2016074348A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113061354A (zh) * 2021-02-25 2021-07-02 中科院过程工程研究所南京绿色制造产业创新研究院 改性磷铁粉及其制备方法与应用

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107522170B (zh) * 2017-09-14 2020-01-10 四川大学 一种硫酸钙还原方法

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1341779A (zh) * 2001-09-07 2002-03-27 南开大学 电解法制备次磷酸的方法
CN101181983A (zh) * 2007-12-12 2008-05-21 湖北兴发化工集团股份有限公司 一种生产次磷酸的方法
CN101481102A (zh) * 2008-01-11 2009-07-15 桑达-阿比克有限责任公司 从含磷矿泥获得次磷酸钠的方法

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1341779A (zh) * 2001-09-07 2002-03-27 南开大学 电解法制备次磷酸的方法
CN101181983A (zh) * 2007-12-12 2008-05-21 湖北兴发化工集团股份有限公司 一种生产次磷酸的方法
CN101481102A (zh) * 2008-01-11 2009-07-15 桑达-阿比克有限责任公司 从含磷矿泥获得次磷酸钠的方法

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
MAO, ANZHANG;: "Review on Preparation of Hypophosphorous Acid and Hypophosphite and Recovery of Byproduct", GUANGDONG CHEMICAL INDUSTRY, 31 December 2004 (2004-12-31), pages 1 - 3 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113061354A (zh) * 2021-02-25 2021-07-02 中科院过程工程研究所南京绿色制造产业创新研究院 改性磷铁粉及其制备方法与应用

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CN104386659B (zh) 2019-10-25
CN104386659A (zh) 2015-03-04

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