The method of chemical recycling of polychlorinated biphenyls |
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IPC classes for russian patent The method of chemical recycling of polychlorinated biphenyls (RU 2175964):
       
 The way dechlorination substituted compounds chloroaromatics / 2152921
The invention relates to a method dechlorination substituted chloroaromatics compounds by the action of a reducing agent (zinc, magnesium or aluminum) and catalytic amounts generated in situ complex compounds of Nickel with bidentate nitrogen-containing ligands (2,2'-BIPYRIDILIUM or 1,10 - phenanthroline) in the bipolar solvent in the presence of a source of protons at a temperature of 70-150°C.
 The method of obtaining dichloro-di-p-xylylene / 2101272
The invention relates to organic chemistry, in particular the production of intermediate for the synthesis of poly-n-xylylene used for surface treatment of metal parts in electronics
 Method for the chemical treatment of polychlorinated biphenyls / 2087458
The invention relates to the field of organic chemistry, in particular to a method for the chemical treatment of polychlorinated biphenyls, which until recently was used in electrotechnical products as an insulating and heat transfer materials
 The way to obtain di(p-anisyl)-ideaware of halide / 2033990
The invention relates to the pharmaceutical industry, specifically to a method for producing di-(p-anisyl)-yedoniah halide of General formula
 H3CO I OCH Hal where Hal is Br, I
 The way to clean octafluorocyclobutane / 2160246
The invention relates to a method of cleaning OCTAFLUOROCYCLOBUTANE from unsaturated impurities, including contacting the modified aluminum oxide in the gas phase at elevated temperatures with subsequent condensation
 The method of purification of 1,1,1-ferrichloride / 2157362
The invention relates to a method of purification of 1,1,1-ferrichloride from chloride vinylidene by contact with chlorine
 The allocation method pentafluoroethane (options) / 2131407
The invention relates to methods of allocation Pentafluoroethane (also known as HFC-125), particularly to the method of separation of HFC-125 from a mixture comprising HFC-125 and at least CHLOROPENTAFLUOROETHANE (also known as CFC-115) as a component (that is, the crude mixture contains at least HFC-125 and CFC-115)
 The method of purification of 1,1-differetn / 2098399
The invention relates to the chemical industry and can be used to remove impurities of vinyl chloride 1,1-differetn (HFC 152a) - ozone-safe refrigerant) used as a refrigerant, porofor, raw materials for the synthesis of organofluorine products
 The method of purification of chloroform / 2096400
 The method of purification of 1,1,1-ferrichloride / 2068403
The invention relates to the chemical industry and can be used to remove impurities chloride vinylidene of 1,1,1-ferrichloride (halon V, or hydrochlorofluorocarbons НСFC-V), which is used as ozone-component fluids, aerosols, poroporo, solvents, and as an inhalation anesthetic
 The method of producing chlorobenzene / 2039731
The invention relates to methods for organochlorine substances and can be used in chemical industry for production improvement of chlorobenzene
 Method for purifying octafluorocyclobutane, method for its preparing and applying / 2245316
Invention relates to a method for purifying octafluorocyclobutane. Method is carried out by interaction of crude octafluorocyclobutane containing impurities with the impurity-decomposing agent at increased temperature and then with adsorbent that is able to eliminate indicated impurities up to the content less 0.0001 wt.-% from the mentioned crude octafluorocyclobutane. Impurity-decomposing agent comprises ferric (III) oxide and compound of alkaline-earth metal in the amount from 5 to 40 wt.-% of ferric oxide and from 60 to 95 wt.-% of compound of alkaline-earth metal as measured for the complete mass of the impurity-decomposing agent. Ferric (III) oxide represents γ-form of iron hydroxyoxide and/or γ-form of ferric (III) oxide. Impurity represents at least one fluorocarbon taken among the group consisting of 2-chloro-1,1,1,2,3,3,3-heptafluoropropane, 1-chloro-1,1,2,2,3,3,3-heptafluoropropane, 1-chloro-1,1,2,2,3,3,3-heptafluoropropane, 1-chloro-1,2,2,2-tetrafluoroethane, 1-chloro-1,1,2,2-tetrafluoroethane, 1,2-dichloro-1,1,2,2-tetrafluoroethane, hexafluoropropene and 1H-heptafluoropropane. Adsorbent represents at least one of representatives taken among the group including activated carbon, carbon molecular sieves and activated coal. Crude octafluorocyclobutane interacts with the mentioned impurity-decomposing agent at temperature from 250oC to 380oC. Invention proposes gas, etching gas and purifying gas including octafluorocyclobutane with purity degree 99.9999 wt.-% and above and comprising fluorocarbon impurity in the concentration less 0.0001 wt.-%. Invention provides enhancing purity of octafluorocyclobutane.
 Method for purifying octafluoropropane / 2245317
Invention relates to a method for purifying octafluoropropane. Method is carried out by interaction of crude octafluoropropane comprising impurities with the impurity-decomposing agent at increased temperature and then with adsorbent that are able to remove indicated impurities up to the content less 0.0001 wt.-% from indicated crude octafluoropropane. The impurity-decomposing agent comprises ferric (III) oxide and compound of alkaline-earth metal in the amount from 5 to 40 wt.-% of ferric oxide and from 60 to 95 wt.-% of compound of alkaline-earth metal as measured for the complete mass of the impurity-decomposing agent. Ferric (III) oxide represents γ-form of iron hydroxyoxide and/or γ-form of ferric (III) oxide. Impurities represent at least one compound taken among the group consisting of chloropentafluoroethane, hexafluoropropene, chlorotrifluoromethane, dichlorodifluoromethane and chlorodifluoromethane. Adsorbent represents at least one substance taken among the group consisting of activated coal, molecular sieves and carbon molecular sieves. Crude octafluoropropane comprises indicated impurities in the amount from 10 to 10 000 mole fr. by mass. Invention proposes gas, etching gas and purifying gas comprising octafluoropropane with purity degree 99.9999 wt.-% and above and containing chlorine compound in the concentration less 0.0001 wt.-%. Invention provides enhancing purity of octafluoropropane.
Method of detoxification of polychlorinated organic wastes / 2255930
Invention relates to detoxifying polychlorinated organic wastes containing toxic high-boiling substances. For this aim, wastes are hydrogenised on supported palladium catalyst at 60-130°C and pressure 10-50 atm in presence of 10-20% sodium hydroxide solution in biphasic water/hydrocarbon system. According to invention, hydrocarbon solution of waste, prior to be subjected to hydrogenation, is filtered at 70-100°C through filter of nonwoven polymeric material allowing waste particles at least 1 μm in size to be retained, after which reaction mixture is charged with lower aliphatic alcohol in amount 1 to 20 wt %.
Method for processing chloroaromatic hydrocarbon / 2263100
Invention is designated for detoxification of chloroaromatic hydrocarbons or their mixtures by dechlorination method resulting to preparing benzene. Dechlorination process of chloroaromatic hydrocarbons is carried out by hydropyrolysis at temperature 700-850°C and in the mole ratio hydrogen : chloroaromatic hydrocarbons = (7-10):1 under pressure 0.1-5 MPa. Benzene is separated by rectification and the following recirculation unreacted chloroaromatic hydrocarbons. Formed hydrogen chlorine is adsorbed with alkali solution. Invention provides simplified technology, excluding toxic reagents and solvents in using and absence of toxic waste.
Method for detoxifying polychlorobiphenils / 2266890
Invention relates to processing organochlorine wastes in chemical industry, in particular, to detoxifying polychlorobiphenyls. Method involves chemical treatment of polychlorobiphenyls by dechlorination method under atmosphere pressure and preferably at temperature 25-50°C. As reagent method involves using hydroxyl-containing compounds representing polyesters and isocyanate in the mass ratio polychlorobiphenyls : polyesters : isocyanate = 1:(1.25-1.4):(2.6-2.75), respectively. Invention represent an ecologically safety method due to absence of harmful exhausts in atmosphere.
Method of processing polychloroorganic waste / 2315030
Invention relates to processing of polychloroorganic wastes via hydrodechlorination with molecular hydrogen at elevated pressure and temperature in presence of an alkali agent, aromatic and/or alicyclic hydrocarbons, water, and catalyst - supported palladium. According to invention, process is carried out in presence of aliphatic and/or alicyclic C4-C6-alcohols at hydrogen-to-alcohol volume ratio (5-10):1.
Method for tetrachloromethane purification / 2323922
According to the said method, chlorine gas solution in liquid tetrachloromethane is exposed to UV radiation in a reactor made of transparent material. Method provides for preparing tetrachlormethane, which contains less than 10 mg/ml of compounds with carbon-hydrogen bonds and double bonds.
 Method of hydrodechlorination of chloraromatic compounds and catalyst for method realisation / 2339606
Method of hydrodechlorination of chloraromatic compounds, in particular polychlorbenzoles, is realised at temperatures higher than 100°C in presence of palladium catalyst on solid carrier. Catalyst, used in method, contains palladium from 4·10-4 to 1·10-2 wt %, and size of not less than 90% of metal particles lies within range 2-5 nm.
Selectively reacting olefins containing terminal cf2 group in mixture / 2399607
Invention relates to a method of reducing molar ratio (1) of a first component selected from a group consisting of compounds of formula Y1Y2C=CF2, where each of Y1 and Y2 independently denotes H, F, Cl, Br, C1-C6alkyl or C1-C6 halogenalkyl containing not more than 3 chlorine atoms, 2 bromine atoms and 1 iodine atom, and (2) a second component selected from a group consisting of saturated compounds of formula CdHeFfClgBrhIk, where d is an integer ranging from 1 to 10, e+f+g+h+k equals 2d+2, provided that g equals 0, 1, 2 or 3, h equals 0, 1 or 2 and k equals 0 or 1, and unsaturated compounds of formula Y3Y4C=CY5Y6, where each of Y3, Y5 and Y6 independently denotes H, F, Cl, Br, C1-C6 alkyl or C1-C6 halogen alkyl containing not more than 3 chlorine atoms, 2 bromine atoms and 1 iodine atom, provided that Y5 and Y6 do not denote F at the same time and Y4 denotes C1-C6 alkyl or C1-C6 halogenalkyl containing not more than 3 chlorine atoms, 2 bromine atoms and 1 iodine atom in a mixture. Said method involves bringing said mixture into contact with at least one selective removal agent selected from a group consisting of SO3 and RSO3H, where R is selected from a group consisting of F, Cl, OH, C1-C8 alkyl, C1-C8 fluoroalkyl or C1-C8 fluoroalkoxyalkyl containing not more than two ester oxygen atoms, with subsequent selective reaction of said selective removal agent with said first component. The invention also relates to a method of extracting at least one product selected from a group consisting of saturated saturated compounds of formula CdHeFfClgBrhIk, where d is an integer ranging from 1 to 10, e+f+g+h+k equals 2d+2, provided that g equals 0, 1, 2 or 3, h equals 0, 1 or 2 and k equals 0 or 1, and unsaturated compounds of formula Y3Y4C=CY5Y6, where each of Y3, Y5 and Y6 independently denotes H, F, Cl, Br, C1-C6 alkyl or C1-C6 halogen alkyl containing not more than 3 chlorine atoms, 2 bromine atoms and 1 iodine atom, provided that Y5 and Y6 do not denote F at the same time and Y4 denotes C1-C6 alkyl or C1-C6 halogenalkyl containing not more than 3 chlorine atoms, 2 bromine atoms and 1 iodine atom in a mixture which contains (i) said at least one product and (ii) an olefin impurity selected from a group consisting of compounds of formula Y1Y2C=CF2, where each of Y1 and Y2 independently denotes H, F, Cl, Br, C1-C6 alkyl or C1-C6 halogen alkyl containing not more than 3 chlorine atoms, 2 bromine atoms and 1 iodine atom. The method involves (a) bringing said mixture into contact with at least one selective removal agent selected from a group consisting of SO3 and RSO3H, where R is selected from a group consisting of F, Cl, OH, C1-C8 alkyl, C1-C8 fluoroalkyl and C1-C8 fluoroalkoxyalkyl containing not more than two ether oxygen atoms, with subsequent selective reaction of said selective removal agent with olefin impurity, resulting in reduction of the radio of the olefin impurity to the said at least one product; and (b) separation of said at least one product and olefin impurity formed during the reaction using the selective removal agent obtained at step (a).
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(57) Abstract: The invention relates to a method for the chemical treatment of polychlorinated biphenyls (PCBs) by the interaction of technical PCB General formula< / BR> where n+m=3-5, with polyethylene glycol (PEG) in the presence of potassium hydroxide and/or sodium in an open system at elevated temperatures. As PEG use glycols normal structure of the General formula H(och2CH2)andHE where a= 3, 13, 35, 65. The process is conducted at a molar ratio policlorodifenil : polyglycol : alkali metal hydroxide= 1 : 2 - 5 : 2 - 5. In the disposal of PCBs receive intermediate products containing two CNS Deputy molecule of diphenyl. table 2. The invention relates to chemical methods of disposal of polychlorinated biphenyls (PCBs), sometimes referred to in the literature as PCBs (polychlorinated biphenyls), the General formula: < / BR> where n + m = 3...5. Until recently, PCBs were used in electrical products as an insulating and heat transfer materials. Today it is established that PCBs are highly toxic (immunotoxicity, the ability to accumulate in organisms, embryotoxic and aracne (inflammation of the sebaceous glands) [Melnikov N. N., Belan, S. R. // Chem. prom. 1989. N 5. C. 328-333], and in some studies the results of analytical measurements on the impact of PCBs on the development of wildlife (human and animal) [Tarasov centuries // the Main achievements in education and science. Collection of scientific papers. M.: Mir, 1995. Vol. 173. C. 24-42]. In addition, the operating conditions (especially at elevated temperatures) PCB partially transformed into chlorinated dioxins, one of the most dangerous in its biological activity substances that can be one of the reasons long-term contamination of the biosphere. These facts were the basis for the prohibition of the international community in 1977, the production and use of PCBs in Russia the production of PCBs ceased only in 1990. Currently, Russia has accumulated more than 400,000 t PCB, which makes the problem of finding an efficient and economically feasible methods of disposal of PCBs relevant. Among the chemical methods of disposal of PCB-known methods of rehabilitation dehalogenase: under the action of metallic sodium in an inert atmosphere [U.S. Pat. 4340471 (1982) USA // S. A. 1982. Vol. 97. 150192 f], metallic sodium in an environment of ammonia [U.S. Pat. 635283 (1995) EUR. // C. A. 1995. Vol. 122. P 141540 a]. Thus the origin is a polymeric substance. The disadvantages of these methods are, first, the use of processes flammable reagents (sodium in an inert atmosphere, sodium in ammonia) [Pozarovzryvobezopasnost substances and materials and their means of fighting Ed. by A. N. Baratova, A. J., Korolenko. M.: Chemistry, 1990. So 2. C. 32], secondly, the need for warehousing and storage of organic compounds obtained as a result of processing, in designated areas that require additional material costs. Currently, due to the significant accumulation of PCBs in the world and in Russia, in particular, methods of rehabilitation dehalogenase is not practicable. The second group of chemical methods aimed at the neutralization and disposal of PCBs, includes the substitution of chlorine atoms in the source PCB to the fluorine atoms under the action of fluorides of alkali metals [U.S. Pat. 2488216 (1949, USA) / / S. A. 1950. Vol. 44. 1629]. It is known that substitution of Cl for F in organic compounds significantly reduces the toxicity of the latter [Clayton J. W. // J. Fluor. Chem. Rev. 1967. N 1. P. 197], and they polyporpylene biphenyls in accordance with some known dielectric characteristics can be used in the same as that of PCBs. However, substitution visokoi temperature. All of this requires significant energy and material costs. The purpose of the invention is to find new, more effective methods of chemical recycling of PCBs, which consists not only in the disposal of PCBs, but also intermediates for the synthesis of practically useful products and substances, ready to use in production. It is known that polyethylene glycol (PEG) of various molecular weights are good catalysts of migration in different processes, for example, in the formation of aromatic ethers [Angeletti E., Tundo P., Venturello P. // J. Chem. Soc., Perkin Trans. 1. 1982. N 5. P. 1137-1141]: < / BR> X = Cl, Br, I. This method is embedded in the purification of transformer oils from PCB traces and formed of them dioxins in Italy [Tundo P., Facchetti, S., W. Tumiatti, Fortunati U. G. // Chemosphere. 1985. Vol. 14. N 5. P. 403-410]. The process is carried out at a temperature not exceeding 100oC in the presence of peroxide catalyst is sodium peroxide: < / BR> In the course of reactions rehabilitation dehalogenase tetrachlorodibenzodioxin and produces a mixture of products consisting of mono-, di-, trichloropropane of dibenzoxepines and non-chlorinated dioxin. Similarly protocarnivorous oils in this way is the formation of solid products by side reactions (prototype): < / BR> n = 1, 2; m = 2, 3; a = 130. The disadvantages of this method are: 1. the lack of purposeful involvement of PCBs and PEG in the reaction of formation of products of alkoxysilane; 2. the reaction proceeds in a flammable mixture with peroxide catalyst - Na2O2[Pozarovzryvobezopasnost substances and materials and their means of fighting Ed. by A. N. Baratova, A. J., Korolenko. M.: Chemistry, 1990. So 2. C. 35]; 3. the process of alkoxysilane PCBs is carried out in flammable solvents (n-hexane, n-decane); 4. selected products of substitution of the chlorine atoms on the alkoxy group is not characterized; 5. there are no proposals on the application of both primary and secondary products alkoxysilane. The basis of the present invention laid the reaction of PCBs with PEG of different molecular masses in the presence of hydroxides of alkali metals: < / BR> n = 1, 2; m = 2, 3; a= 3, 13; 35; 65; M = K, Na. The reaction starts with the formation of alcoholate, potassium and/or sodium melts/solutions of PEG of different molecular masses in an open system when heated to 120-140oC. after the formation of the alcoholate in the reactor is brought PCB, and the mixture is stirred for 3-5 h at the is m excess of sodium alcoholate and/or potassium in the mixture flows through the substitution of two chlorine atoms in the alkoxy anion in the original PCB, apparently, due to steric factors. All the synthesized products are soluble in water, which enables their use as lubricating fluids (coolant) [Klamann D. Lubricants and related products. M.: Chemistry, 1988. S. 121]. The presence in the products alkoxysilane PCB functional groups enables the involvement of the latter in the oligomerization reaction with foramerican perfluoroine carbonic acid [Ed. mon. N 1659399 (USSR) // Appl. 26.12.88, Publ. 01.03.91] . As a result of oligomerization produced products that are used as lubricants and made for anti-adhesion compositions [U.S. Pat. 3250806 (1966) USA // Rehim. 1967. N 14. NP]. The advantages of this method are: 1. no need to use solvents and catalysts in this reaction; 2. quantitative yields of products of double alkoxysilane PCB; 3. the simplicity of the hardware design process; 4. known possible use of the compounds obtained; 5. depending on the application, you might receive as a solid (with the highest PEG) and liquid products (with the lowest PEG). The EXPERIMENTAL PART is Lenovo oil (for solids). The depth of the transformations and the course of the reaction was controlled by TLC on Silufol plates (the disappearance of the spot of the original connection). The conditions of the reaction, downloads, outputs, and data of IR spectroscopy and elemental analysis of the obtained compounds are given in table. 1, 2. Example 1. In a three-neck flask with a capacity of 0.25 ml, equipped with a mechanical stirrer, reflux condenser and addition funnel, download 30.0 g (0.2 mol) of triethylene glycol (PEG-3 MM/150) and 11.2 g (0.2 mol) of potassium hydroxide (KOH). The reactor is placed in a glycerin bath and with vigorous stirring, heated to 120oC. At this temperature, to the resulting homogeneous mass within 1 h was added dropwise 25.6 g (0.1 mol) of trichlorodiphenyl (TCD, OST 6-01-24 - 85). The reaction mass is stirred at a temperature of 120oC for 3 h, after which bring in the reactor 100 ml of water. In the resulting solution is added with stirring to 25 ml of ethyl acetate. The mixture is cooled and separated the upper organic layer. Extraction of the aqueous layer is repeated with 25 ml of ethyl acetate. Both extracts are combined and dried with MgSO4liquid portion is separated, the ethyl acetate is distilled off. The remaining product is subjected to distillation in a vacuum oil pump. Get 45.logically spend interaction 45.0 g (0.03 mol) of PEG-35 (MM=1500), 1.2 g (0.03 mol) of NaOH and 3.3 g (0.01 mol) of pentachlorobiphenyl (PCBs, OST 6-01-17-85) at a temperature of 130oC for 4 h After all treatments emit 61.8 g (99%) wazeliniarzy product is white, which represent trichlorogalactosucrose PCBs (distilled in a vacuum oil pump is not subjected to). Example 3. Similarly spend interaction 60.0 g (0.4 mol) of PEG-3 (MM=150), 11.2 g (0.2 mol) of KOH, 8.0 g (0.2 mol) of NaOH and 32.7 g (0.1 mol) of pentachlorobiphenyl (PCBs) at a temperature of 140oC for 5 h After all treatments emit 54.0 g (97%) of a light brown viscous product, representing trichlorogalactosucrose PCB, so Kip. 340-362oC / 4 mm RT. Art. Example 4. Similarly spend interaction 30.0 g (0.05 mol) of PEG-13 (MM=600), 2.8 g (0.05 mol) of KOH and 3.3 g (0.01 mol) of pentachlorobiphenyl (PCBs) at a temperature of 130oC for 3 h After all treatments emit 13.8 g (95%) of a bright yellow viscous product, representing trichlorogalactosucrose PCB (connection resulting from degassing, distillation in a vacuum oil pump is not subjected to). Example 5. Similarly spend the interaction of 3.3 g (0.01 mol) P the solid product is a light yellow color. The output is 59.6 g (99%), so pl. 54-55oC. Method for the chemical treatment of polychlorinated biphenyls (PCBs), which consists in the interaction of technical PCB General formula < / BR> where n+m=3...5, with polyethylene glycol (PEG) in the presence of potassium hydroxide and/or sodium in an open system at elevated temperature to obtain a product containing two CNS Deputy molecule of diphenyl, characterized in that as the PEG use glycols normal structure of the General formula H(och2CH2)aHE where a=3, 13, 35, 65, the process is conducted at a molar ratio policlorodifenil : polyglycol : alkali metal hydroxide=1: 2-5:2-5.
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