EP0999878A1 - Method for eliminating halogenated and non halogenated waste - Google Patents
Method for eliminating halogenated and non halogenated wasteInfo
- Publication number
- EP0999878A1 EP0999878A1 EP98940244A EP98940244A EP0999878A1 EP 0999878 A1 EP0999878 A1 EP 0999878A1 EP 98940244 A EP98940244 A EP 98940244A EP 98940244 A EP98940244 A EP 98940244A EP 0999878 A1 EP0999878 A1 EP 0999878A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- halogenated
- carbon
- metal oxide
- waste
- waste materials
- Prior art date
- Legal status (The legal status 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 status listed.)
- Granted
Links
Classifications
-
- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D3/00—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances
- A62D3/30—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by reacting with chemical agents
- A62D3/37—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by reacting with chemical agents by reduction, e.g. hydrogenation
-
- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D3/00—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances
- A62D3/30—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by reacting with chemical agents
- A62D3/34—Dehalogenation using reactive chemical agents able to degrade
-
- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D2101/00—Harmful chemical substances made harmless, or less harmful, by effecting chemical change
- A62D2101/04—Pesticides, e.g. insecticides, herbicides, fungicides or nematocides
-
- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D2101/00—Harmful chemical substances made harmless, or less harmful, by effecting chemical change
- A62D2101/20—Organic substances
- A62D2101/22—Organic substances containing halogen
Definitions
- the present invention relates to a method for the disposal of halogenated and non-halogenated waste materials.
- EP 0 306 540 describes a process for the production of energy from substituted hydrocarbons, such as those e.g. as CCI4, CHCI3, C2H2CI4, PCB, PVC, polyvinylidene chloride etc. in pure or bound form.
- the waste material is thermally decomposed in an inductively heatable reactor in the presence of a metal oxide which is difficult to smelt and an electrically conductive material, for example electrode coke or electrographite, and in contact with water vapor at temperatures between 800 and 1,100 ° C.
- a proportion of the metal oxide that corresponds to the chlorine content of the waste materials is converted into volatile metal chloride.
- a portion of the released carbon is converted into carbon monoxide and the portion of the carbon that does not react with the metal oxide is converted into water gas (CO + H 2) with the aid of a stoichiometric amount of water vapor.
- the object of the present invention is to develop a method which allows various halogenated and non-halogenated waste materials to be disposed of in an environmentally friendly manner.
- This object is achieved according to the invention by a process for the disposal of halogenated non-halogenated waste materials, in which the halogenated and non-halogenated waste materials are reacted with metal oxide-containing products with the exclusion of oxygen at temperatures of 800 ° C. to 1100 ° C.
- the process described here is used for the environmentally neutral recycling of halogenated and non-halogenated waste materials.
- the volume of the waste used is largely reduced, so that as few residues as possible remain and the largest possible amount of metals / metal compounds is obtained.
- the aim is to achieve the most positive energy balance possible during implementation.
- carbon-containing, halogenated waste materials are reacted.
- carbon dioxide is added as the fluidizing gas.
- the reactor can also be charged with carbon in the form of graphite and / or coal.
- a halogenatable product containing metal oxide is preferably used as the metal oxide-containing starting material.
- products which contain CaO, T1O2, SiO2, Al2O3 and / or F ⁇ 2O3 or a mixture thereof are used as halogenatable, metal oxide-containing reactants.
- metal oxide-containing waste materials such as e.g. Silicon-containing residues from the metalworking industry, filter dust, fly ash, fly sands, pile of heaps, electroplating sludge, slag, slate residues etc. are used.
- Simple quartz sand which consists of about 98% silicon dioxide (Si ⁇ 2), is the simplest material imaginable
- All of the above materials are characterized in that they contain a relatively high content of halogenatable metal oxides (CaO, SiO2, TiO2 > I2O3, Fe2O3, etc.).
- halogenated waste materials solvents such as: carbon tetrachloride, chloroform, methylene chloride, tetra- and trichlorethylene, tetrachloroethane, coolants or refrigerants, PCB, pesticides, fungicides and herbicides, halogenated plastics such as PVC can be used.
- a proportion of the metal oxide that corresponds to the chlorine content of the waste materials is converted into metal chloride by the above-mentioned process.
- Ecologically and economically valuable metal chlorides are formed, with silicon and titanium tetrachloride (SiCI ⁇ TiCl4> being particularly preferred products.
- Used oils, lubricants, greases, varnishes, paints, tars, waxes, plastics, coolants and solvents, brake fluid or similar non-halogenated substances and materials must be disposed of.
- reaction or reaction products formed thermodynamically preferred under these process parameters are primarily gaseous hydrogen (H 2 ) in addition to lower percentages of methane (CH).
- gaseous substances such as carbon monoxide (CO), and the carbon dioxide (CO 2 ) known as so-called greenhouse gas, is negligible under the preferred reaction conditions. Only at temperatures above 1100 ° C can CO or CO 2 be formed by chemical decomposition processes.
- the implementation takes place in a fluidized bed reactor. This can either be made of special ceramics, silicon carbide (SiC) or specially alloyed steels.
- the reactor can be brought to the necessary operating temperatures either by using electrical heating elements (e.g. heating halves) or by using induction heating.
- the temperatures required for the implementation are in the range of 800 ° C to 1100 ° C.
- the reaction itself takes place with the exclusion of oxygen.
- Carbon dioxide (CO2) is used as the fluidizing gas.
- the halogenated compounds are broken down into their simplest components by the high temperatures, in the case of chlorinated hydrocarbons hydrogen chloride, hydrogen, alkanes and chlorine gas are formed.
- the chlorine gas and the hydrogen chloride serve as chlorinating agents for the metal oxide-containing products or wastes.
- Products of this chlorination reaction are the thermodynamically preferred metal chlorides.
- hydrogen and carbon monoxide are formed, which can be used as synthesis gas either for the production of electrical energy or for other chemical syntheses, such as methanol synthesis.
- Reaction equation 1 The carbon dioxide (CO2) used as the fluidizing gas is completely converted to carbon monoxide (CO) by reaction with the carbon of the decomposed hydrocarbons and by an additional bed of carbon or graphite in the head of the reactor.
- halogenated metal compounds produced are initially in gaseous form.
- solid, ie crystalline metal compounds can be obtained by cooling to room temperature, or liquid metal compounds by condensation at low temperatures.
- the purity of these compounds is 96% and can e.g. by fractional distillation, or rectification.
- Fig. 1 a diagram of the plant for the disposal of halogenated waste.
- a fluidization gas CO2 is blown into the fluidized bed reactor 5.
- the reactor 5 is heated by means of a reactor heater 6 to a temperature between 800 ° C and 1100 ° C, so that there is a reaction between the halogenated waste and the metal oxide-containing substances in the reactor.
- the products formed are separated in a solid separator 7 and the solid metal chlorides formed, in particular AICI3 and FeC ⁇ , are over a
- Line 8 discharged.
- the remaining gases are cleaned by an activated carbon filter 9 and then compressed by a blower 10.
- the gases are then cooled in a cooling container 12, which has a coolant inlet 11 and a coolant outlet 13, so that the remaining metal chlorides are eliminated. It is mainly SiCI ⁇
- the gases are then fed to a condenser 15 and in one
- Gas wash column 16 subjected to an alkaline gas wash.
- the column 16 has a circulation pump 17 for the washing liquid.
- the remaining synthesis gas, a mixture of CO and H2 is via line 18 in the upper
- Table 1 Slate analysis from Martelange, Belgian-Luxembourg border area
- the slate waste is crushed using a jaw crusher. Average grain sizes in the range of 3 - 8 mm are advantageous.
- Fluidizing gas is used to generate and maintain the
- the temperature of the fluidizing gas is advantageously brought to about 500 ° C.
- Perchlorethylene (C2CI4, ' PER) is used as the halogenated waste product.
- the PER is introduced as a kind of aerosol from a partial fluidization gas stream directly into the reaction zone of the reactor. There the PER is broken down into its components. The difference between PER and others Solvents is that there are no hydrogen atoms in the molecule. As a result, the formation of hydrochloric acid (HCI) is not possible.
- HCI hydrochloric acid
- Chlorinating agent The chlorine gas reacts in the fluidized bed with the formation of metal chlorides (generally Me x C) with the metal oxides of the slate.
- metal chlorides generally Me x C
- metal oxides of the slate For example, aluminum chloride (AICI3), iron III chloride (FeC ⁇ ) and silicon tetrachloride
- the elemental carbon (C) obtained during the thermal decomposition of the chlorinated hydrocarbons reacts either with the fluidizing gas (CO2) or with the bound oxygen of the metal oxides to form carbon monoxide.
- Reaction equation 3 describes the chlorination of silicon dioxide with the formation of silicon tetrachloride and carbon monoxide.
- reaction equation 4 It becomes clear from reaction equation 4 that various metal chlorides are formed in addition to carbon monoxide. All substances are initially gaseous at temperatures around 1000 ° C. Immediately after the reactor, the gases cool down very quickly to around 800 ° C through the ambient air.
- Separation devices such as cyclones or activated carbon filters make it possible to separate and retain dust or crystalline metal chlorides, but mainly aluminum chloride and iron chloride, from the process gas stream. Supported by a blower, the gas flow is drawn through the filters. This has the consequence that a slight negative pressure already on Reactor outlet is to be noted, which is in the range of about 0.01-0.05 bar under normal pressure.
- the residual gases contain gaseous silicon tetrachloride and carbon monoxide. Since the silicon tetrachloride changes to the solid state at temperatures below - 68 ° C, the process gas must be cooled down to temperatures of around - 50 ° C. This is done by pre-cooling with liquid nitrogen and post-cooling using a cooling mixture in a condensation column. The cold mixture used is an acetone / dry ice mixture, which can generate temperatures down to a maximum of - 86 ° C.
- the gaseous silicon tetrachloride is reflected in the above Temperatures in the condenser are low and is collected in a storage container.
- the degree of purity of the condensed silicon tetrachloride is approximately 96%. Any foreign substances that may be present can be removed by a subsequent fractional distillation. The result of the purification by distillation would be a silicon tetrachloride solution with a degree of purity of approx. 99%.
- the process gas is fed to an alkaline gas wash with a 10% potassium hydroxide solution according to the countercurrent principle.
- the gas purified in this way only contains carbon monoxide.
- Example of use 2 Disposal of vinyl chloride
- the process engineering design of the system corresponds to the design that was also used for the disposal of perchlorethylene (PER).
- PER perchlorethylene
- AICI3, FeC ⁇ The process engineering separation of aluminum and iron chloride (AICI3, FeC ⁇ ) takes place on the one hand by centrifugal force separation in a cyclone and on the other hand by separation in special filters.
- the silicon tetrachloride is separated off in the manner already described.
- reaction equation 8 it can be seen from reaction equation 8 that in addition to the metal chlorides, a synthesis gas consisting of carbon monoxide and hydrogen is formed.
- the ratio between hydrogen and carbon monoxide is 1: 2.3.
- Example of use 3 Disposal of hydrocarbon (KW) or halogenated hydrocarbon (HKW) waste in the presence of calcium oxide
- the various feed materials such as Oils, greases, PCBs, CFCs, solvents or the like are fed through a dosing device, e.g. an eccentric screw pump, conveyed into the reaction zone.
- a dosing device e.g. an eccentric screw pump
- the residence time of the feed materials or that of the cleavage products formed is determined by the height of the reaction zone.
- reaction equation 1 Calcium chloride (CaCl) is essentially formed as the reaction product, which remains in the reactor as slag or melt.
- reaction equation 1 takes into account all essential products that are formed during the disposal or recycling of a halogenated hydrocarbon. The individual products were calculated thermodynamically and verified experimentally.
- carbon is also discharged from the reactor in the form of fine soot particles.
- the separation of the other gaseous components hydrogen and methane, or hydrogen and carbon monoxide (CO), is carried out by gravity separators, e.g. a high performance cyclone.
- the gases cleaned in this way can still be passed through activated carbon filters. If there are still foreign components in the process gas, they can be removed either by targeted condensation or by gas scrubbing.
Landscapes
- Business, Economics & Management (AREA)
- Toxicology (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Emergency Management (AREA)
- Health & Medical Sciences (AREA)
- Processing Of Solid Wastes (AREA)
- Fire-Extinguishing Compositions (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Silicon Compounds (AREA)
Abstract
Description
Claims
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP02004190A EP1219324B1 (en) | 1997-07-23 | 1998-07-20 | Method for elimination of halogenated and non halogenated waste |
Applications Claiming Priority (5)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
LU90109A LU90109B1 (en) | 1997-07-23 | 1997-07-23 | Process for disposing (non)-halogenated waste e.g. carbon tetra:chloride - comprises reacting waste with products containing metal oxide with exclusion of oxygen |
LU90109 | 1997-07-23 | ||
LU90191 | 1997-12-24 | ||
LU90191A LU90191A7 (en) | 1997-07-23 | 1997-12-24 | Process for the disposal of halogenated and non-halogenated waste materials |
PCT/EP1998/004508 WO1999004861A1 (en) | 1997-07-23 | 1998-07-20 | Method for eliminating halogenated and non halogenated waste |
Related Child Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP02004190A Division EP1219324B1 (en) | 1997-07-23 | 1998-07-20 | Method for elimination of halogenated and non halogenated waste |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0999878A1 true EP0999878A1 (en) | 2000-05-17 |
EP0999878B1 EP0999878B1 (en) | 2002-02-27 |
Family
ID=26640365
Family Applications (2)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP98940244A Expired - Lifetime EP0999878B1 (en) | 1997-07-23 | 1998-07-20 | Method for eliminating halogenated and non halogenated waste |
EP02004190A Expired - Lifetime EP1219324B1 (en) | 1997-07-23 | 1998-07-20 | Method for elimination of halogenated and non halogenated waste |
Family Applications After (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP02004190A Expired - Lifetime EP1219324B1 (en) | 1997-07-23 | 1998-07-20 | Method for elimination of halogenated and non halogenated waste |
Country Status (16)
Country | Link |
---|---|
US (1) | US6645449B2 (en) |
EP (2) | EP0999878B1 (en) |
JP (1) | JP4208412B2 (en) |
CN (1) | CN1198669C (en) |
AT (2) | ATE213657T1 (en) |
AU (1) | AU747426B2 (en) |
BR (1) | BR9810858A (en) |
CA (1) | CA2295907C (en) |
DE (2) | DE59803209D1 (en) |
DK (2) | DK1219324T3 (en) |
ES (2) | ES2172185T3 (en) |
HK (1) | HK1047900B (en) |
LU (1) | LU90191A7 (en) |
PT (2) | PT1219324E (en) |
RU (1) | RU2200601C2 (en) |
WO (1) | WO1999004861A1 (en) |
Families Citing this family (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE10055360B4 (en) * | 2000-11-08 | 2004-07-29 | Mühlen, Heinz-Jürgen, Dr.rer.Nat. | Process for the gasification of liquid to pasty organic substances and mixtures |
AT508100A2 (en) * | 2009-03-30 | 2010-10-15 | Erema | NEUTRALIZATION BY FILLER |
CN102061008A (en) * | 2010-11-09 | 2011-05-18 | 佛山市高明区(中国科学院)新材料专业中心 | Method for reducing bromide content in pyrolysis gas of waste printed circuit board by high-temperature shock heating |
CN104147745B (en) * | 2014-08-22 | 2017-02-15 | 上海化工研究院 | Method for removing volatile halocarbons in environment through chemical conversion |
RU2667566C1 (en) * | 2017-09-04 | 2018-09-21 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Ярославский государственный технический университет" ФГБОУВО "ЯГТУ" | Method of preparation of galvanic sludge for its utilization |
CN110251877A (en) * | 2019-05-21 | 2019-09-20 | 山东大学 | A method of using silicon carbide as the mechanochemical reaction of catalyst degradation hexachloro-benzene |
Family Cites Families (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
NL7710901A (en) * | 1977-10-05 | 1979-04-09 | Esmil B V Stationsstraat 48 | PROCESS FOR THE SIMULTANEOUS PROCESSING OF USED METAL AND / OR METAL WASTE FROM HALOGENATED HYDROCARBONS. |
US4435379A (en) * | 1982-08-18 | 1984-03-06 | The Dow Chemical Company | Process for treating chlorinated hydrocarbons |
US4541907A (en) * | 1984-04-16 | 1985-09-17 | Aluminum Company Of America | Process for decomposing chlorinated hydrocarbon compounds |
US4631183A (en) | 1985-06-25 | 1986-12-23 | Hydro-Quebec | Process for the destruction of toxic organic products |
DE3623492A1 (en) * | 1986-07-11 | 1988-01-21 | Hagenmaier Hans Paul | METHOD FOR DEGRADING HALOGENATED AROMATES |
ATE118688T1 (en) * | 1986-11-27 | 1995-03-15 | Suppan Friedrich | METHOD AND SYSTEM FOR GENERATING ENERGY FROM TOXIC WASTE MATERIALS WITH THE SIMULTANEOUS DISPOSAL OF THEM. |
JPH06104183B2 (en) * | 1989-06-09 | 1994-12-21 | 三井・デュポンフロロケミカル株式会社 | Catalytic decomposition method of chlorofluoroalkane |
US5608136A (en) * | 1991-12-20 | 1997-03-04 | Kabushiki Kaisha Toshiba | Method and apparatus for pyrolytically decomposing waste plastic |
US5280757A (en) * | 1992-04-13 | 1994-01-25 | Carter George W | Municipal solid waste disposal process |
US5222448A (en) * | 1992-04-13 | 1993-06-29 | Columbia Ventures Corporation | Plasma torch furnace processing of spent potliner from aluminum smelters |
US5673635A (en) * | 1995-06-12 | 1997-10-07 | L.E. Maxwitat | Process for the recycling of organic wastes |
-
1997
- 1997-12-24 LU LU90191A patent/LU90191A7/en unknown
-
1998
- 1998-07-20 AT AT98940244T patent/ATE213657T1/en not_active IP Right Cessation
- 1998-07-20 CA CA002295907A patent/CA2295907C/en not_active Expired - Fee Related
- 1998-07-20 US US09/463,349 patent/US6645449B2/en not_active Expired - Fee Related
- 1998-07-20 JP JP2000503903A patent/JP4208412B2/en not_active Expired - Fee Related
- 1998-07-20 PT PT02004190T patent/PT1219324E/en unknown
- 1998-07-20 ES ES98940244T patent/ES2172185T3/en not_active Expired - Lifetime
- 1998-07-20 BR BR9810858-1A patent/BR9810858A/en not_active IP Right Cessation
- 1998-07-20 DK DK02004190.1T patent/DK1219324T3/en active
- 1998-07-20 CN CNB988074494A patent/CN1198669C/en not_active Expired - Fee Related
- 1998-07-20 ES ES02004190T patent/ES2337769T3/en not_active Expired - Lifetime
- 1998-07-20 EP EP98940244A patent/EP0999878B1/en not_active Expired - Lifetime
- 1998-07-20 WO PCT/EP1998/004508 patent/WO1999004861A1/en active IP Right Grant
- 1998-07-20 DE DE59803209T patent/DE59803209D1/en not_active Expired - Fee Related
- 1998-07-20 AT AT02004190T patent/ATE452689T1/en active
- 1998-07-20 DK DK98940244T patent/DK0999878T3/en active
- 1998-07-20 DE DE59814426T patent/DE59814426D1/en not_active Expired - Lifetime
- 1998-07-20 PT PT98940244T patent/PT999878E/en unknown
- 1998-07-20 AU AU88626/98A patent/AU747426B2/en not_active Ceased
- 1998-07-20 RU RU2000102922/12A patent/RU2200601C2/en not_active IP Right Cessation
- 1998-07-20 EP EP02004190A patent/EP1219324B1/en not_active Expired - Lifetime
-
2003
- 2003-01-02 HK HK03100019.4A patent/HK1047900B/en not_active IP Right Cessation
Non-Patent Citations (1)
Title |
---|
See references of WO9904861A1 * |
Also Published As
Publication number | Publication date |
---|---|
ES2172185T3 (en) | 2002-09-16 |
DE59803209D1 (en) | 2002-04-04 |
ATE452689T1 (en) | 2010-01-15 |
DK1219324T3 (en) | 2010-04-06 |
ATE213657T1 (en) | 2002-03-15 |
BR9810858A (en) | 2000-07-25 |
AU747426B2 (en) | 2002-05-16 |
EP1219324A3 (en) | 2004-04-07 |
HK1047900B (en) | 2010-09-03 |
WO1999004861A1 (en) | 1999-02-04 |
US20030149325A1 (en) | 2003-08-07 |
AU8862698A (en) | 1999-02-16 |
ES2337769T3 (en) | 2010-04-29 |
PT999878E (en) | 2002-07-31 |
EP0999878B1 (en) | 2002-02-27 |
DK0999878T3 (en) | 2002-06-10 |
JP2001510814A (en) | 2001-08-07 |
JP4208412B2 (en) | 2009-01-14 |
EP1219324A2 (en) | 2002-07-03 |
DE59814426D1 (en) | 2010-02-04 |
PT1219324E (en) | 2010-03-25 |
RU2200601C2 (en) | 2003-03-20 |
CA2295907C (en) | 2005-10-18 |
EP1219324B1 (en) | 2009-12-23 |
HK1047900A1 (en) | 2003-03-14 |
CN1265043A (en) | 2000-08-30 |
CN1198669C (en) | 2005-04-27 |
LU90191A7 (en) | 1999-06-24 |
CA2295907A1 (en) | 1999-02-04 |
US6645449B2 (en) | 2003-11-11 |
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