Classifications

• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
  • C01G21/00—Compounds of lead
  • C01G21/02—Oxides
  • C01G21/06—Lead monoxide [PbO]
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
  • C01G21/00—Compounds of lead
  • C01G21/02—Oxides
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
  • C01G21/00—Compounds of lead
  • C01G21/20—Sulfates

Definitions

• This invention relates to the manufacture of
• Typical derivatives are tri-basic lead sulphate, tetra-basic lead silico sulphate, lead silicon sulphate, dibasic lead phosphite, lead phthalate, dibasic lead stearate and lead stearate.
• the stabilizers aforementioned are presently manufactured by a process which involves the production
• PVC are manufactured by reacting litharge with dilute acetic acid, and the dibasic lead acetate so formed is reacted with sodium sulphate.
• a process for the 0 manufacture of hydrated lead oxides in the bivalent state characterized by the steps of CIJL reacting metallic lead with acetic acid at a temperature up to 200 C under an atmosphere of an oxygen containing gas of between 1 and 10 atmospheres absolute pressure to form lead acetate, then 5 (2) reacting the lead acetate with a source of ammonium ion under an absolute pressure between 1 and 5 atmospheres up to 100 C to precipitate hydrated lead oxides.
• the acetic acid may be present in concentrations of up to 50% wt.-, preferably up to 25% wt. and if added as Q ammonium acetate concentrations of up to 50% wt. , preferably 35% wt. should be used.
• the process may include the additional step of adding sulphuric acid and/or ammonium sulphate to the hydrated lead oxides 5 to produce tri- or tetra- basic lead sulphate. Additionally the tri- or tetra- basic lead sulphate can be separated and dried.
• a particularly preferred form of the invention is a process for the manufacture of tri- and tetra- basic 0 lead sulphates, characterized by the steps of (11 reacting excess metallic lead with an aqueous solution containing between 5% and 30% by weight of ammonium acetate at a temperature between 50°C and 200°C under an atmosphere of oxygen of between 1 and IQ atmospheres absolute pressure 5 to form lead acetate, then C21 reacting the lead acetate so formed with ammonia under an absolute pressure between 1 and 5 atmospheres at a temperature between 15°C and 1QQ°C, preferably 60°C to 90°C, to precipitate lead oxides.
• step CIL the concentration of the aqueous solution of ammonium acetate is between 15% and 25% by weight, the temperature is between 80°C and 120°C, and the pressure is between 3 and 5 atmospheres absolute.
• the concentration of the aqueous solution of ammonium acetate is 20% by weight, the temperature is 100°C, and the pressure is 2.5 atmospheres absolute, and in step (.2) the temperature is 80°C and the pressure is 3 atmospheres absolute.
• Example -1 An aqueous solution of ammonium acetate at a concentration of 35% by weight and a temperature of 1Q0 C was reacted for 1 hour with excess metallic lead in a closed reactor through which oxygen was passed.
• the ammonium acetate dissociates and the acetic acid formed reacted with the lead under an atmosphere of oxygen at 5 atmospheres absolute pressure to produce a lead acetate solution and ammonia.
• the ammonia was carried away and condensed and the oxygen stream was returned to the reactor.
• the temperature of the aqueous solution of lead acetate was adjusted to 80 C, and it was transferred to a precipitator, into which ammonia including that recovered from the previous stage was directed until a pressure of 3 atmospheres absolute was achieved. Hydrated lead oxides were precipitated, and ammonium acetate solution was formed.
• Example 2 The same procedure as disclosed in Example 1 was followed.
• the resulting solid was incorporated as a stabilizer in polyvinyl chloride resin, which was then passed through an extruder to form test pieces.
• the liquid was heated in a stripping circuit to drive off any dissolved ammonia, which was recovered for re-use and to adjust the concentration of ammonium acetate to 35% by weight. It was then directed to the reactor for the first stage of a repetition of the process on a fresh batch of metallic lead.
• the test pieces provided by the process according to the present invention were found to be more effectively stabilized without sacrifice of any desirable properties of the resin. Furthermore, the tribasic lead sulphate resulting from the process according to the present invention was substantially free (less than 5 ppm) of elemental lead,mono basic lead sulphate and unreacted lead oxides.

Landscapes

• Chemical & Material Sciences (AREA)
• Organic Chemistry (AREA)
• Inorganic Chemistry (AREA)
• Inorganic Compounds Of Heavy Metals (AREA)
• Pigments, Carbon Blacks, Or Wood Stains (AREA)
• Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
• Compositions Of Macromolecular Compounds (AREA)
• Photoreceptors In Electrophotography (AREA)
• Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
• Chemical And Physical Treatments For Wood And The Like (AREA)
• Oxygen, Ozone, And Oxides In General (AREA)

Priority Applications (4)

Applications Claiming Priority (2)

Publications (1)

Family

ID=3770694

Family Applications (1)

Country Status (17)

Cited By (1)

Citations (2)

Family Cites Families (7)

• 1985
  • 1985-07-19 NZ NZ212810A patent/NZ212810A/en unknown
  • 1985-07-23 ZA ZA855565A patent/ZA855565B/xx unknown
  • 1985-07-25 US US06/845,691 patent/US4673561A/en not_active Expired - Fee Related
  • 1985-07-25 BR BR8506857A patent/BR8506857A/pt unknown
  • 1985-07-25 IN IN578/MAS/85A patent/IN165108B/en unknown
  • 1985-07-25 EP EP19850903785 patent/EP0190226A4/en not_active Withdrawn
  • 1985-07-25 WO PCT/AU1985/000167 patent/WO1986000878A1/en not_active Ceased
  • 1985-07-25 JP JP60503475A patent/JPS61502813A/ja active Pending
  • 1985-07-25 KR KR1019860700144A patent/KR900000680B1/ko not_active Expired
  • 1985-07-26 CA CA000487572A patent/CA1255876A/en not_active Expired
  • 1985-07-26 ES ES85545620A patent/ES8700214A1/es not_active Expired
  • 1985-07-26 GR GR851848A patent/GR851848B/el unknown
  • 1985-07-26 PT PT80875A patent/PT80875B/pt not_active IP Right Cessation
  • 1985-07-29 PH PH32574A patent/PH21397A/en unknown
• 1986
  • 1986-03-20 DK DK129686A patent/DK129686D0/da not_active Application Discontinuation
  • 1986-03-21 NO NO861134A patent/NO861134L/no unknown
  • 1986-03-24 FI FI861256A patent/FI81327C/fi not_active IP Right Cessation

Patent Citations (2)

Non-Patent Citations (2)

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