The method of obtaining chlorinated solvents
(57) Abstract:The invention relates to the production of cheap solvents for degreasing metals and chemical cleaning. The solvents get through the distillation of high-boiling waste production of vinyl chloride. Before distillation waste type trichloride and/or tetrachloride in such quantity to get azeotropic mixture trichlorethene with dichloroethane and tetrachlorethene with trichloroethane and/or tetrachlorethane. The technical result - waste production of vinyl chloride. The invention relates to the field of processing chlorophenothane waste, as well as to the field of production of solvents for degreasing metals and chemical cleaning.Know the use for degreasing metals and dry cleaning trichloroethene /trichloroethylene/, tetrachlorethene /perchloroethylene, trichloroethane and CFC /Traeger Y. A. and other Major chlorinated solvents. M.: Chemistry, 1984, S. 192-207/. Due to lower cost the most widely trichloride and tetrachloride, although trichloroethane and freon as far as their physical-chemical properties and detergency /Traeger Y. A., and others, see above, S. 207/.FL. Handbook edited Osina L. A. M.: Chemistry,. 1978, S. 68/. High-boiling waste of vinyl chloride are composed mainly of dichloroethane, trichloroethane, tetrachlorethene and tetrachlorethane. Select the rectification of the mixture of individual trichloroethane, tetrachloride and tetrachlorethane is not possible, because they form an azeotropic mixture.A method of refining high-boiling waste of vinyl chloride /patent SU 633465 A, 16.11.1973/, which consists of stages of evaporation, heat treatment residue, condensing the vaporous components and their distillation. The result is a distillate containing 1,2-dichloroethane and dichlorethylene formed during the heat treatment, as well as CBM product consisting of trichloroethane with the above-mentioned impurities. The distillate return in the production of vinyl chloride and CBM product sent as raw materials for the production of perchloroethylene.The disadvantage of this method of recycling is the lack of a final marketable product.The above mentioned disadvantage is eliminated by the fact that in the method of processing high-boiling waste production of vinyl chloride by distillation to the original waste before distillation to relax what chloretone and tetrachlorethene with trichloroethane and/or tetrachlorethane, then get organochlorine solvents, consisting mainly of these azeotropic mixtures.It is known that the solvent capacity of azeotropic mixtures is higher than that of each component, introducing the mixture /Greenberg S. A. and other Solvents for paints and varnishes. L.: Chemistry, 1980, S. 103-104/.The azeotropic mixtures have another advantage over individual solvents. Trichloride boils at 87oWith, and its azeotropic mixture with dichloromethane /39% trichlorethene and 61% of dichloroethane/ - if 82oC. Tetrachloride boils at 121oWith, and its azeotropic mixture with trichloroethane or tetrachlorethane /57% tetrachlorethane and 43% of trichloroethane and/or tetrachlorethane/ - at 112oWith /Industrial organochlorine products, see above, C. 102,139,180/. Lowering the boiling temperature is favorable for regeneration of the solvent.In order to avoid losses trichlorethene and tetrachlorethene distillation to provide a slight excess of dichloroethane and trichloroethane in the resulting azeotropic solvents. As a result, the solvents have a boiling within, respectively, 82-84oC and 112-114oWith, because dichloroethane boils at 83,5oAnd trichloroethane - when 113,9oC.the s contain 15.2% dichloroethane, 1.6% of 1-chloro-2-brometea, 60.3 per cent of trichloroethane, and 5.5% tetrachlorethane, 2.7% tetrachlorethane and 14.7% other chlorohydrocarbons having a boiling point above 114oC.On the power of the column, adds 95 kg/h trichlorethene. The main product is taken 247 kg/h fraction 82-84oC, which consists essentially of azeotropic mixtures trichloroethane and dichloroethane with a small surplus /3 kg/h/ dichloroethane. This fraction is the first solvent.Side shoulder strap column select 700 kg/h fraction 107-115oWith, which is the second solvent and has the composition: 2.3% of 1-chloro-2-brometea, 86.1% trichloroethane, 7,9% tetrachlorethane and 3.7% of tetrachlorethane and other chlorohydrocarbons.148 kg/h VAT residue is directed to thermal deactivation.Example 2. In a distillation column is distilled 1 t/h of high-boiling waste of vinyl chloride as described in example 1. On the power of the column add 775 kg/h tetrachlorethene.The main product is taken 247 kg/h fraction 82-84oWith, which is the first solvent.Side shoulder strap column select 1460 kg/h fraction 112-114oWith, which is the second solvent and is essentially azeotrope is Ronny deduce the fraction 85-111oWith 16 kg/h, which is added to 145 kg/h VAT residue and is directed to thermal deactivation.Example 3. In the evaporator dry cleaning machines during normal operation accumulate 50-60 kg of waste cleaning, is then pumped into the evaporator 200 kg high-boiling waste of vinyl chloride, the composition of which is specified in example 1. To reduce the Flammability of the solvent here add 20 kg trichlorethene. Conduct regular distillation, getting 190 kg of solvent with a boiling within 82-115oC. first with 82oWith Argonauts azeotrope of dichloroethane with trichlorethane, and then the remaining components of the solvent.Unload the waste cleaning and guide them in the disposal.Example 4. The solvent receive, as described in example 3. In a tank of pure solvent dry cleaning machines add up to 155 kg tetrachlorethene getting azeotrope with the last three - and tetrachlorethane. The method of obtaining chlorinated solvents by distillation of high-boiling waste of vinyl chloride, characterized in that the waste before distillation add trichloride and/or tetrachloride in such quantity to get the azeotropic mixture of t is
FIELD: chemical technology.
SUBSTANCE: invention relates to a method for treatment of waste from manufacture of organochlorine substances from resinification products by distillation of volatile components. Method involves distilling volatile components as azeotrope with water in the presence of inert inorganic filling agent and accessory agent reducing adhesion of resinification products to equipment. Method provides excluding formation of resinification products and cake and to achieve the complete separation of volatile components from resinous substances.
EFFECT: improved method of treatment of waste.
5 cl, 1 tbl, 12 ex
SUBSTANCE: method includes supply of initial mixture and dimethylsulfoxide (DMSO) as separating agent, taken in ratio 7-7.5:1 to initial mixture, into extraction rectification column (1) efficiency 50 t.t., initial mixture being supplied on 30 t.t., separating agent on 10 t.t. of column (plate numeration from top of column), phlegm number in column constitutes 1.5-2, taking of benzol in distillate and mixture benzol-perfluorobenzol (PFB) - tertiary amyl alcohol (TAA)-DMSO from column (1) cube , supply of mixture PFB-TA-DMSO on 25 t.t. of column of separating agent regeneration (2) with efficiency 50 t.t., phlegm number in column being 1-3, removal separating agent from column cube and its supply to column (1), supply of column (2) distillate, representing aseotropic mixture PFB-TAA, for separation into complex of two columns (3) and (4) with efficiency 35 t.t., with removal from column cubes of TAA and PFB, respectively, aesotropic mixture being supplied on 18 t.t. of column (3), phlegm numbers of columns (3) and (4) being equal 0.5-1.5 and 1-2 respectively, re-cycle of aseotrope PFB-TAA, which is separated in distillate of column (4) into column(3) feeding, ratio of re-cycle of column (4) and feeding of column (3) being (1-1.1):0.66, pressure in columns (1)-(3) is 300 mm of mercury, pressure in column (4) - 760 mm of mercury.
EFFECT: simplification of technology, increase of ecological compatibility of process and quality of obtained products.
1 tbl, 1 dwg, 1 ex
FIELD: technological processes.
SUBSTANCE: invention relates to method for separation of components in azeotropic or azeotrope-like mixture, which represents a flow outging from polymerisation reactor, including contact of extractant, including at least one hydrocarbon with mixture, containing at least one C4-C7isoolefin and dissolvent, including one or more fluorohydrocarbons, to produce a product of contact, which represents a dissolvent, including one or more fluorohydrocarbons, substantially free of at least one C4-C7isoolefin, where one or several fluorohydrocarbons comply with the formula CxHyFz, in which x stands for integer number from 1 to 40 and y and z stand for integer numbers from one and more, and hydrocarbon is selected from alkanes, including linear, cyclic, branched alkanes, alkenes, aromatic compounds from C4 to C22 or their mixtures. Method for separation is carried out in extractive distillation system, including section of polymerisation reactor, from where azeotropic or azeotrope-like mixture is withdrawn, one column with section for entry of extractant, including at least one hydrocarbon, at least one condensation heat exchanger, from where product of contact is withdrawn, and at least one evaporation heat exchanger. Invention also relates to azeotropic mixture for separation, including 1,1,1,2-tetrafluoroethane and isobutylene at 0.84 mole fraction of 1,1,1,2-tetrafluoroethane at 25°C and 684 kPa and at 0.88 mole fraction of 1,1,1,2-tetrafluoroethane at 75°C and 2378 kPa; to azeotrope-like mixture for separation, including 1,1,1,2-tetrafluoroethane and isobutylene in the range from 0.8504 to 0.9968 mole fraction of 1,1,1,2-tetrafluoroethane at 25°C and from 663.29 to 683.99 kPa, and in the range from 0.8851 to 0.9958 mole fraction of 1,1,1,2-tetrafluoroethane at 75°C and from 2349.5 to 2377.5 kPa; to azeotropic mixture for separation, including 1,1-difluoroethane and isobutylene at approximatelt 0.87 mole fraction of 1,1-difluoroethane at 25°C and 603 kPa and at approximately 0.94 mole fraction of 1,1-difluoroethane at 75°C and 2091 kPa; to azeotropic mixture for separation, including 1,1-difluoroethane and isolbutylene in the range from 0.7536 to 0.813 mole fraction of 1,1-difluoroethane at 25°C and from 596.98 to 603.10 kPa and in the range from 0.7670 to 0.9325 mole fraction of 1,1-difluoroethane at 75°C and from 2054.0 to 2090.6 kPa.
EFFECT: production of substantially pure dissolvent, which may be used in polymerisation of C4-C7isoolefin at higher temperatures with considerable reduction of contamination in polymerisation reactor.
19 cl, 4 dwg, 7 tbl
SUBSTANCE: invention discloses a method of producing an azeotropic composition containing fluorohydroolefin with 3-8 carbon atoms via dehydrofluorination of a fluorine-containing hydrocarbon. The invention also discloses methods of separating fluorohydroolefins from fluorine-containing hydrocarbons and from hydrogen fluoride.
EFFECT: invention enables to obtain fluorohydroolefins without using a catalyst.
9 cl, 33 ex, 35 tbl, 2 dwg
SUBSTANCE: described are methods of separating any of HFC-1225ye, HFC-1234ze, HFC-1234yf or HFC-1243zf from HF. One of methods includes separation of mixture, which contains HF and fluorolefin, where said method includes a) supply of composition, containing HF and fluorolefin, to first distillation column; b) discharge of azeotropic composition, containing HF and fluorolefin as first distillate and either i) HF, or i) fluorolefin as composition of vat residue of first column; c) condensation of first distillate with formation of two liquid phases: i) HF-saturated phase and ii) fluorolefin-enriched phase; and d) recirculation of first liquid phase, enriched with the same compound, which is removed as vat residue of first column, where said first liquid phase is either i) HF-enriched phase, or ii) fluorolefin-enriched phase, back into first distillation column.
EFFECT: invention presents more efficient method of HF separation from olefins.
33 cl, 13 ex, 14 tbl, 8 dwg
SUBSTANCE: one of the versions involves: a. feeding a composition containing HF and HFO-1234ze into a first distillation column; b. removing the azeotropic composition containing HF and HFO-1234ze as a first distillate and either i) HF or ii) HFO-1234ze as a composition of distillation residues of the first column; c. condensation of the first distillate to form 2 liquid phases which are i) a phase rich in HF and ii) a phase rich in HFO-1234ze; and d. recycling the first liquid phase rich in the same compound, which is removed as distillation residues of the first column, said first liquid phase being either i) a phase rich in HF or ii) a phase rich in HFO-1234ze, back into the first distillation column. The invention also relates to a method of separating HFO-1234yf from HFO-1234ze to form an azeotropic mixture containing HF and HFO-1234ze.
EFFECT: invention provides a novel method of separating HF from HFO-1234ze.
17 cl, 9 ex, 9 tbl
SUBSTANCE: invention relates to a range of versions of separating a mixture containing HF and HFO-1234yf. One of the versions involves: a. feeding a composition containing HF and HFO-1234yf into a first distillation column; b. removing the azeotropic composition containing HF and HFO-1234yf in form of a first distillate and either i) HF or ii) HFO-1234yf in form of a composition of first still residues; c. condensation of the first distillate to form two liquid phases which are i) a phase rich in HF and ii) a phase rich in HFO-1234yf; and d. recycling the first liquid phase rich in the same compound, which is removed in form of still residues of the first column, said liquid phase being either i) a phase rich in HF or ii) a phase rich in HFO-1234yf, back into the first distillation column.
EFFECT: present invention provides a novel method of separating HF and HFO-1234yf.
14 cl, 9 ex, 9 tbl, 8 dwg