Classifications

• • C—CHEMISTRY; METALLURGY
  • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
  • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
  • C02F1/00—Treatment of water, waste water, or sewage
  • C02F1/28—Treatment of water, waste water, or sewage by sorption
  • C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
  • C01B32/00—Carbon; Compounds thereof
  • C01B32/30—Active carbon
  • C01B32/312—Preparation
  • C01B32/318—Preparation characterised by the starting materials
  • C01B32/33—Preparation characterised by the starting materials from distillation residues of coal or petroleum; from petroleum acid sludge
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
  • C01B32/00—Carbon; Compounds thereof
  • C01B32/30—Active carbon
  • C01B32/312—Preparation
  • C01B32/342—Preparation characterised by non-gaseous activating agents

Definitions

• the invention relates to a process for the preparation of a solid carbon-containing material having a sorption capacity for metal ions.
• the preparation of a solid carbon-containing material having a sorption capacity for metal ions is known in itself.
• a process is described in which polymers of vinyl aromatic hydrocarbons are reacted with a compound made up of sulphur and chlorine in the presence of a catalyst and the resulting polymer sulphides or polymer polysulphides are oxidized or reduced..
• Reduction results in the formation of thiol resins which have a high affinity for ions of heavy metals.
• a disadvantage to the known metal adsorbing material is its high price. This is due both to the high price of the starting materials and the relatively complex process to be used for the preparation of the desired thiol resins.
• a solid carbon-containing material having a sorption capacity for metal ions can be obtained in an inexpensive and simple manner by mixing the carbon-containing starting material with sulphur, heating the mixture for some time to a temperature of about 120 o -500 o C., and subsequently treating it with an aqueous solution of alkali metal hydroxide an a temperature not exceeding about 200° C. Tt should be
• waste materials such as waste rubber, but also peat, liqnite, coal, asphalt or petroleum coke. They are preferably used in a finely divided state, in the form of for instance chips or grains having a diameter of not more than a few millimeters.
• the rubber to be used may be of synthetic or natural origin. It will generally occur in the form of worn tyres of automobiles or other motor vehicles or means of transport, and in the form of worn objects that are partly or entirely made of rubber, such as conveyor belts. The rubber objects may be cut up or ground in any convenient manner, possibly after removal of metal parts, for instance from the beads of automobile tyres.
• the process according to the invention is usually so carried out that before, during or after the carbon-containing starting material is cut up, it is mixed with 0.1 to 5 parts by weight of sulphur and subsequently heated for a number of hours in an oven at a temperature in the range of about 120 to 500 o C. Preference, however, is given to a treatment with 0.5 to 1.5 parts by weight of sulphur per part by weight of starting material at a temperature between about 200 and 300 o C. '
• the subsequent treatment of the sulphurized material with an aqueous solution of an alkali metal hydroxide can suitably be carried out at a temperature not exceeding about 200 C.; above 100 C.the treatment is usually done in an autoclave. It is preferred that use should be made of a sodium hydroxide solution, for instance a 10% NaOH solution, by which with proper stirring the treatment can be completed within a few hours at a temperature of 800C. or higher.
• the material successively treated with sulphur and an aqueous solution of NaOH is finally filtered and/or washed with (acidified) water, after which it is ready for use.
• the physical appearance of the novel adsorbing materials according to the invention may vary from gel form to porous solid matter.
• Treatment of the same starting material at a temperature above 400° C. results in obtaining a material having a porous structure.
• the material produced with the process according to the invention not only shows the property of a cation exchanger, but is also capable of binding metals that occur in the form of anionic complexes.
• the material according to the invention appears to have a high reducing capacity, which is particularly manitest in the sorption of ions of noble metals, such as gold and silver, and cf metals of the platinum group. It is also found possible for instance to reduce Cr0 4 2- to Cr 3+ . This means that the novel material according to the invention can also be looked upon as an inexpensive reducing agent.
• Another useful application of the material according to the invention consists in the removal of mercury from concentrated sulphuric acid, as obtained by roasting zinc sulphide.
• the invention also provides a process in which prior or subsequent to thermal treatment the starting material is subjected to a treatment with sulphur or oleum, or still heated in the presence of air or some other oxygen-containing gas.
• Brown coal briquettes were crushed and ground into grains measuring 1 to 2 mm.
• Example VIII The grains, which had strongly swollen in the aqueous NaOH solution, were successively washed with water and acidified with dilute sulphuric acid (5% by weight of H 2 SO 4 ). After they had again been washed with water, their properties were determined. The results are given in Example VIII and Example IX.
• coal grains containing 24% volatile material measuring 1 to 2 mm were mixed with 100 parts by weight of sulphur and subsequently heated for 8 hours in a rotating steel oven, with the temperature being gradually raised from 120°C to 300° C.
• the mixture thus obtained was heated for 4 hours at 300° C.
• the resulting grains were still heated for 5 hours at 90 C.with an aqueous solution of 10% by weight NaOH and 10% by weight Na 2 S.
• the grains were successively washed with water, excess acid and water.
• this material contained strongly acid groups in an amount of as little as 50 meq/l.
• 25 ml of grains had been introduced into a 20 cm column, they were found capable of sorbing all silver from a fixing bath containing 1 g Aq per litre.
• Example I A To illustrate the strong metal adsorbing capacity of the material prepared by the process according to the invention the product prepared in Example I A was tested for its capacity of retaining mercury from a HgCl 4 ions-containing solution.
• Example II Through a column of the product prepared in Example I A 20 cm in bed weight and having a bed volume of 25 ml there was passed an aqueous solution containing 100 mg Hg 2+ and 10 grammes of NaCl per litre.
• Example VI 25 ml of granular material prepared in the way described in Example It were introduced into a 20 cm column, as used in Example VI Through the column there was passed a solution of 1 mg Cu in 25% by weight sulphuric acid. After a passage of 40 bed volumes over a period of 8 hours no copper could be found in the effwens of the column.
• the solution was subsequently replaced by a 5% sulphurie acid containing about 100 mg Ag per litre.

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• Chemical & Material Sciences (AREA)
• Organic Chemistry (AREA)
• Engineering & Computer Science (AREA)
• Inorganic Chemistry (AREA)
• Environmental & Geological Engineering (AREA)
• Water Supply & Treatment (AREA)
• Life Sciences & Earth Sciences (AREA)
• Chemical Kinetics & Catalysis (AREA)
• General Chemical & Material Sciences (AREA)
• Oil, Petroleum & Natural Gas (AREA)
• Materials Engineering (AREA)
• Hydrology & Water Resources (AREA)
• Solid-Sorbent Or Filter-Aiding Compositions (AREA)
• Carbon And Carbon Compounds (AREA)

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• 1977
  • 1977-06-22 NL NL7706879A patent/NL7706879A/xx not_active Application Discontinuation
• 1978
  • 1978-06-09 DE DE7878200033T patent/DE2860365D1/de not_active Expired
  • 1978-06-09 EP EP78200033A patent/EP0000214B1/fr not_active Expired
  • 1978-06-13 US US05/915,242 patent/US4203868A/en not_active Expired - Lifetime
  • 1978-06-21 JP JP7531178A patent/JPS5410296A/ja active Pending

Patent Citations (6)

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