The method of obtaining 1,1,1,3,3-pentachlorobutane

 

(57) Abstract:

The invention relates to the production of 1,1,1,3,3-pentachlorobutane. The method is realized by the interaction between carbon tetrachloride and 2-chlorpro-1-Yong in the presence of catalyst telomerization. As the catalyst used is at least one compound of copper(I) or copper(II). The reaction is carried out at a temperature of from 40 to 200oC. Preferably the process is conducted in the presence of a solvent, which selects a nitrile, amide or trialkylphosphines. The technical result is an increase in the output of 1,1,1,3,3-pentachlorobutane. 9 C.p. f-crystals, 5 PL.

The invention relates to a method for producing 1,1,1,3,3-pentachlorobutane, in particular by reaction of telomerization between carbon tetrachloride and 2-chlorpro-1-Yong.

1,1,1,3,3-Pentachlorobutane is an important industrial interest, because it leads, by fluoridation, to the appropriate pentafluorophenol derived (HFC-365 mfc) used, in particular, as gazonapolnitel or solvent of the third generation that do not have a destructive effect on the ozone layer and does not contribute to global warming of the planet due to the greenhouse effect.

Another way of obtaining 1,1,1,3,3-pentachlorobutane described recently Kotora and his team (React. Kinet. Catal. Lett., 44 (2), 415-419 [1991] ), consists in the introduction into the interaction 1,1,1-trichloroethane to 1,1-dichlorethene in the presence of monovalent chloride of copper and amine. The resulting output is low (8%), and this method of synthesis, therefore, is also unsuitable for use in industry.

Consequently, the invention relates to a developing method, which allows, in one stage, using readily available reagents to obtain 1,1,1,3,3-pentachlorobutane with high output.

Thus, the invention relates to a method for producing 1,1,1,3,3-pentachlorobutane by the reaction between carbon tetrachloride and 2-chlorpro-1-Yong in the presence of a catalyst comprising at least one compound of copper(I) or a compound of copper(II). Generally preferred compounds of copper(II).

The connection of copper(I) or a compound of copper(II) is preferably chosen among halides 2">

Of the halides of copper(I) or copper(II), in particular, are applied fluorides, chlorides, bromides or iodides. Preferred are the chlorides and iodides. Particularly preferred chloride copper(II).

Mixed salts of copper(I) or copper(II), in particular, are used hydroxhloride. Preferred hydroxychloride copper-(II).

From carboxylates of copper(I) or copper(II), in particular, are used salts formed with the carboxylic acids such as acetic acid, propionic acid, butyric acid, cyclohexanedione acid or benzoic acid. Preferred are acetates of copper(I) or copper(II), that is, salts formed with acetic acid. Particularly preferred cyclohexanebutyrate copper-(II).

Of the complexes formed with copper(I) or copper(II), in particular, are used complexes obtained with neutral ligands, such as phosphines, such as triphenylphosphine, or with acetylacetone. Preferred acetylacetonate copper(II).

Preferably the catalyst is chosen among the acetate of copper(I) or acetate of copper(II), cyclohexanebutyrate copper(II) chloride complex of monovalent copper with triphenylphosphine, acetylaceton preferred are chloride copper(II), acetate of copper(II), hydroxychloride copper(II), cyclohexanebutyrate copper(II) acetylacetonate copper(II).

In the case of periodical way molar ratio between the input connection of copper and 2-chlorpro-1-Yong is usually higher than or equal to 0.001, tend to be higher than or equal to 0.002. Preferably it is greater than or equal to 0.005. The molar ratio between the input connection of copper and 2-chlorpro-1-Yong often lower than or equal to 5, mostly less than or equal to 1. Preferably it is less than or equal to 0.5. Especially preferably, this ratio is higher or equal to 0.01 and less than or equal to 0.1.

In the case of ongoing way molar ratio between the insertion catalyst and 2-chlorpro-1-Yong is approximately the same extent as in the case of periodical way, but, however, it can reach values of 50.

It is clear that the amount of catalyst expressed in the case of periodically carried out method in relation to the initial quantity of used 2-chlorpro-1-ene in the case of ongoing fashion with respect to a constant amount in the reactor 2-chlorpro-1-ene.

The molar ratio between techno is equal to or higher than 0.1, mostly equal to or above 0.5. Preferably it is greater than or equal to 1. Typically, this ratio, however, is equal to or lower than 20, mostly equal to or below 10. Preferably, this ratio is equal to or lower than 8.

Usually the reaction is carried out at a temperature higher than or equal to room temperature. Preferably a temperature equal to or above the 40oWith and preferably equal to or above 80oC. Typically, the reaction temperature does not exceed 200oC. Mostly, especially when using hydroxychloride copper-(II) as catalyst, the reaction temperature is higher or equal to 90oWith, preferably it is higher than or equal to 100oC. Usually it is lower than or equal to 150oWith, rather it is lower than or equal to 140aboutC. When using hydroxychloride copper-(II) in particular, it is preferable to carry out the reaction at a temperature close to 130oC.

Duration of response in case of periodical way or the residence time in the case of continuously implemented method depends on various parameters such as reaction temperature, concentration of reactants and catalyst in the reaction mixture and the molar ratio. Usually depending on these parameters, the time of stay or equal to atmospheric pressure and equal to or lower than 15 bar. Preferably it is less than or equal to 10 bar. As the reaction telomerization usually carried out in the liquid phase, the pressure depending on the temperature of the reaction medium, preferably chosen in such a way as to maintain the reaction medium mainly in the condensed phase.

In the first variant of the method according to the invention the reaction is carried out in the presence of a solvent. Can be used any solvent in which the reactants form a target product with an acceptable output. Preferably the solvent for the reaction is alcohol, nitrile, amide, lactone, trialkylphosphines, trialkylphosphine or other polar solvent.

Used as solvent for the reaction of alcohols, in particular, are used methanol, ethanol, isopropanol and tert.-butanol. Used as solvent for the reaction of NITRILES, in particular, are used aliphatic NITRILES, particularly acetonitrile, propionitrile or adiponitrile, and aromatic NITRILES, especially benzonitrile or tolunitrile. Among the NITRILES are preferred propionitrile and adiponitrile. Used as solvent for the reaction of amides are used in icon. You can also specify hexamethylphosphoramide. Used as solvent for the reaction of lactones, in particular, call-butyrolactone. Used as solvent for the reaction of trialkylphosphines can, in particular, include compounds of formula (R1R2R3)PO, in which Rl, R2, and R3 denote the same or different, preferably linear, alkyl groups with 3-10 carbon atoms. In particular, use three(n-butyl)phosphine oxide, three(n-hexyl)phosphine oxide, tri-(n-octyl)phosphine oxide, n-octyl-di(n-hexyl)phosphine oxide and n-hexyl di(n-octyl)phosphine oxide and mixtures thereof. Used as solvent for the reaction of trialkylphosphates can, in particular, include compounds of the formula (RO)3RO in which R is preferably a linear alkyl group with 3 to 10 carbon atoms. In particular, the use of tributyl phosphate. As other polar solvents can also specify 1,3-dimethyl-2-imidazolidinone, dimethylsulfoxide and tetrahydrofuran. Preferably the solvent is an amine or trialkylphosphines. Good results are in particular achieved by the use of N-methylpyrrolidone, N, N-dimethylacetamide, and using the mixture of three(n-hexyl)phosphine oxide, three(n-octodiol solvent in the first variant of the method according to the invention is not critical. But too diluted solution is not conducive to high yields and a high degree of conversion. Preferably the molar ratio of solvent to 2-chlorpro-1-ENU is equal to or higher than 0.05. Preferably, this ratio is equal to or higher than 0.1. The molar ratio of solvent to 2-chlorpro-1-ENU usually equal to or lower than 20, mostly equal to or below 15. Preferably, this ratio is equal to or higher than 0.2 and equal to or lower than 10. In the reaction medium, the amount of solvent may vary in a molar ratio in the range of values from about 5-fold to 500-fold amount of the catalyst, preferably from about 10-fold to 200-fold.

In the second, preferred, embodiment of the method according to the invention the reaction is carried out in the presence of socializaton. Acetalization can be selected, in particular, among amines, amides and trialkylphosphines. As used as acetalization amines can be called aliphatic amines or aromatic amines. Of the aliphatic amines are primary amines, secondary amines and tertiary amines. As Amin usually use alkanolamine, bonds alkylamines, such as, for example, ethanolamine, n-butylamine, tert.-butylamine, n-cuts the Dean or aniline. As used as acetalization amides can be called N-organic and N,N-dimethylformamide. As used as acetalization of trialkylphosphines can be called a connection, which is used as a solvent according to the first variant embodiment of the invention. The preferred socialization are aliphatic bonds alkylamines, such as n-butylamine, tert.-butylamine, n-Propylamine and Isopropylamine. Particularly preferred Isopropylamine and tert.-butylamine. Other preferred acetalization are trialkylphosphines.

Compounds of copper(II) is particularly preferred when the reaction is carried out in the presence of socializaton. Very good results are achieved when using the acetate of copper(II) and tert.-of butylamine as socializaton.

In this second, preferred, embodiment of the method according to the invention, the reaction temperature may be equal to or below 120oC. In particular, the presence of socializaton allows the reaction at a temperature equal to or below the 100oWith, while maintaining a high degree of conversion and excellent selectivity. It is especially recommended temperature, bliski equal to 0.001. Preferably, this ratio is equal to or higher than 0,005. Typically, this ratio is equal to or below 1, mostly equal to or lower than 0.5. Preferably this ratio is greater than or equal to 0.01 and less than or equal to 0.25. Especially preferably, this ratio is higher or equal to 0.1 and less than or equal to 0.2. The number of socializaton may change in the molar ratio in the range of values from about 0.1 times to about 25 times the amount of catalyst, preferably about 0.5-fold to about 20-fold.

The presence of socializaton in the reaction mixture does not preclude the use of nitrile or other compounds as the solvent.

In this second embodiment of the method according to the invention the carbon tetrachloride may serve as both a reagent and solvent. The molar ratio between carbon tetrachloride and 2-chlorpro-1-Yong then greater than or equal to 2, tend to be higher than or equal to 4. Preferably, this ratio is higher or equal to 4.5. However, to avoid too much dilution of the reagents, this ratio is usually lower than or equal to 10 and preferably it is less than or equal to 8. Preferably this ratio is below or equal to 6.

The method according from the x reagents usually with a selectivity of over 90%.

Obtained according to the proposed invention method 1,1,1,3,3-pentachlorobutane is a precursor of the corresponding pentafluorophenol analog 1,1,1,3,3-pentafluorobutane (HFC-365 mfc), which can be obtained by treatment with hydrogen fluoride in the presence of a catalyst, such as a salt of antimony, salt, titanium salt tantalum or salt of tin.

The following examples illustrate the invention without limiting its scope. In these examples, the reactants, solvent and catalyst is introduced into the autoclave with a capacity of 300 ml, the inner wall of which is covered with Teflon. Then the device is hermetically closed, placed in a vertical furnace and the temperature is gradually increased and is supported at the desired value within a few hours. Mixing is provided by a core of a magnetic stirrer placed inside the autoclave. Upon completion of the reaction, the autoclave is allowed to cool, take a sample of fluid with a syringe and analyze its chromatographic method for determination of the degree of conversion of 2-chlorpro-1-ene and selectivity of transformation in 1,1,1,3,3-pentachlorobutane.

The following tables, the conversion rate represents the ratio, expressed as PR is nanii reaction, and used by a number; the selectivity of transformation in 1,1,1,3,3-pentachlorobutane represents the ratio, expressed in percentage, between the number of formed 1,1,1,3,3-pentachlorobutane and the number of 1,1,1,3,3-pentachlorobutane, which would be formed if the entire 2-chlorpro-1-ene turned into 1,1,1,3,3-pentachlorobutane.

Examples 1-4

In these examples, 1,1,1,3,3-pentachlorobutane get in the presence of various NITRILES in the presence of a mixture containing 20% CuCl and 80% CuClO (below denoted CuCl-CuClOH), as compounds of copper. The molar ratio of 2-chlorpro-1-ene/CCL4/Sys-lO/nitrile is 1/2/0,01/1.The reaction is carried out at a temperature of 130oWith over 13 hours. The results are presented in table I.

Example 5

Repeat example 1 using molar ratios of 2-chlorpro-1-ene/nitrile 1/0,5. Reach the degree of conversion of 85% and a selectivity of 85%.

Example 6

Repeat example 1 using molar ratios of 2-chlorpro-1-ene/nitrile 1/4. Reach the degree of conversion of 90% and a selectivity of 89%.

Example 7

Repeat example 6, using anhydrous chloride of copper(II) as catalyst. Reach the degree of conversion of 92% and a selectivity of 98%.

4/propionitrile is 1/2/4. The results obtained are presented in table II.

Example 10

In this example repeats example 6 at a temperature of 150oC. Achieve a degree of conversion of 99% and a selectivity of 91%.

Examples 11 and 12

In these examples, 1,1,1,3,3-pentachlorobutane get in the presence of various amines in the presence of CuCl-CuClOH. The molar ratio of 2-chlorpro-1-ene/CCL4/CuCl-CuClOH/Amin is 1/5/0,05/0,1. The reaction is carried out at a temperature of 90oC for two hours. The results are presented in table III.

Example 13

Repeat example 12 using acetate of copper(II) as catalyst and the reaction time is 1 hour at a temperature of 90oC. the Molar ratio of 2-chlorpro-1-ene/CCL4/C(COOCH3)2/Amin is 1/5/0,05/0,15. Reach the degree of conversion of 96% and a selectivity of 97%.

Examples 14-20

Repeat example 11 using various copper compounds. The results are presented in table IV.

Example 21 (not according to invention)

Repeat example 6, but in the absence of copper compounds. Not see education 1,1,1,3,3-pentachlorobutane.

Examples 22-25

1,1,1,3,3-Penna. The duration of reaction is 2 hours. The molar ratio of the reagents, the reaction temperature and the obtained results are presented in table V.

Examples 26 and 27

1,1,1,3,3-Pentachlorobutane obtained from 2-chlorpro-1-ene and carbon tetrachloride in the presence of acetylacetonate copper(II) as catalyst and a mixture of four trialkylphosphine [three(n-hexyl)phosphine oxide, three(n-octyl)phosphine oxide, n-octyl-di(n-hexyl)phosphine oxide and n-hexyl di(n-octyl)-phosphine oxide] , manufactured by CYTEC under the name of CYANEX923. The duration of reaction is 2 hours. The molar ratio of the reagents, the reaction temperature and the results obtained are also presented in table V.

Example 28

Repeat example 24 using acetate of copper(II) as catalyst. Reach the degree of conversion of 55% and the selectivity of transformation in 1,1,1,3,3-pentachlorobutane 94%.

Example 29

1,1,1,3,3-Pentachlorobutane get in the presence of CuCl2as the catalyst and using N-methylpyrrolidone as solvent. The molar ratio of 2-chlorpro-1-ene/CCl4/CuCl2/N-organic is 1/2,2/0,05/3,3. After reaction for 5 hours while the temperature is">

1. The method of obtaining 1,1,1,3,3-pentachlorobutane by the reaction between carbon tetrachloride and 2-chlorpro-1-Yong in the presence of catalyst telomerization, characterized in that the catalyst comprises at least one compound of copper (I) or a compound of copper (II).

2. The method according to p. 1, characterized in that the connection of copper is chosen among the halides of copper, mixed with copper salts, carboxylates of copper complexes with phosphine or acetylacetone, or mixtures thereof.

3. The method according to p. 2, characterized in that the catalyst is chosen among the acetate of copper (II), hydroxychloride copper (II), cyclohexanebutyrate copper (II) acetylacetonate copper (II) chloride copper (II).

4. The method according to any of paragraphs.1-3, characterized in that the reaction is carried out in the presence of a solvent.

5. The method according to any of paragraphs.1-4, characterized in that the reaction is carried out in the presence of socializaton.

6. The method according to p. 5, characterized in that socialization is Amin.

7. The method according to p. 6, characterized in that the amine is Isopropylamine or tert.-butylamine.

8. The method according to any of paragraphs.1-7, characterized in that the reaction is carried out at a temperature higher than or equal to 40oC and lower than or equal to 200oC.

10. The method according to p. 9, characterized in that the solvent is chosen among N-methylpyrrolidone, N, N-dimethylacetamide, three(n-hexyl)phosphine oxide, three(n-octyl)phosphine oxide, n-octyl-di(n-hexyl)phosphine oxide, n-hexyl di(n-octyl)phosphine oxide and mixtures thereof.

Priority points:

05.05.1997 - PP.1-8;

05.05.1997 and 24.02.1998 - p. 9;

24.02.1998 - p. 10.

 

Same patents:

The invention relates to new derivatives of tamilcanadian with the General formula (I) wherein R' represents 2-thienyl or 3-thienyl radical, R represents ceanorhaditis or a radical of the formula-C(O) - and R2 is optional saturated or unsaturated cyclic hydrocarbon radical or aryl radical

The invention relates to the field of chlorinated organic synthesis, in particular, to a method of obtaining hexachlorethane, which is used in the process of casting aluminum parts

The invention relates to the chlorination of paraffin

The invention relates to techniques for the chlorination of paraffin hydrocarbons with gaseous chlorine
The invention relates to a technology for organochlorine products, namely the method for producing a solid chloroparaffin brand HP-1100, used as additives to polymeric materials to reduce their Flammability

The invention relates to the production of tertiary butyl chloride, used as intermediate in organic synthesis
The invention relates to a method for producing a solid chloroparaffin with the General average formula CnH2n+2-xClxwhere x = 21 - 24

The invention relates to the field of synthesis of halide Akilov, which are used as solvents and as intermediates in the industries of organic synthesis, for example in the synthesis of CHLOROSILANES

The invention relates to methods of chlorination of paraffins, widely used in polymer compositions as plasticizers in the production of building materials, paints and varnishes, synthetic films and leathers, rubber industry, as well as ontamarama additives to various polymers

The invention relates to a process for the preparation of adducts of fluorinated hydrocarbons and olefins having the formula RR1R2CCR1F or FR1R2CCR1R2CH2)2where R is selected from the group consisting of CH3CH2F, C2H4F, F(CF2)nCH2CH2where n is an integer from 1 to 10; each of R1independently selected from the group consisting of H, C1, F and CF3and each of R2independently selected from the group consisting of H, F and CF3

FIELD: chemistry.

SUBSTANCE: invention relates to a method for selective production of C6F13I through telomerisation of fluoroalkyl iodide of formula RfI (where Rf is a C2-4 fluoroalkyl group) as telogen and tetrafluoroethylene (CF2CF2) as taxogen, involving a step for liquid-phase telomerisation which involves supply of a homogeneous liquid mixture of telogen and taxogen from the bottom part of tube reactor, movement of the mixture from the bottom part of the reactor towards its top part in the presence of a radical initiator with dwell time in the reactor of at least 5 minutes. The reaction system is kept in liquid-phase state under conditions where there is separation of gas and liquid, so that taxogen being fed into the reactor is considerably consumed in the reaction in the reactor and the reaction product is released from the top part of the reactor. The radical initiator is a peroxide-type or azo-compound, and molar ratio RfI/CF2CF2 in the liquid mixture of reagents lies between 20 and 200.

EFFECT: high output of telomere, having one given length of the carbon chain.

7 cl, 1 dwg, 2 ex

FIELD: chemistry.

SUBSTANCE: invention relates to a method of producing fluorinated organic compounds involving reaction of methylfluoride with at least one fluorinated olefin, having structural formula where R denotes F, Cl, C1-C2 fluorinated alkyl or fluorinated alkenyl containing 2 carbon atoms, to obtain at least one product containing at least 3 carbon atoms, where the said reaction takes place in gas phase and in the presence of a Lewis acid as a catalysts, which is used to saturate activated carbon.

EFFECT: cheap method of producing fluorinated organic compounds.

10 cl, 14 ex

FIELD: chemistry.

SUBSTANCE: invention relates to a method for synthesis of partially halogenated propane or partially fluorinated butane, involving: reaction of partially fluorinated methane, which is selected from a group comprising CH2F2 to CH3F, with fluoro-olefin, which is selected from a group comprising CF2=CF2, ClFC=CF2 and CF3CF2=CF2, in the presence of a catalyst - modified aluminium chloride, where the modified aluminium chloride has formula AlCl3-xFx, in which x ranges from approximately 1.0 to approximately 2.8 or modified aluminium bromide, where the modified aluminium bromide has formula AlBr3-yFy, in which y ranges from approximately 2.7 to 2.95. During the process, the catalyst is first fed into a reaction vessel and then partially fluorinated methane is fed into the reaction vessel. Further, said partially fluorinated methane can react with said fluoro-olefin at temperature between 0C and 100C, where molar ratio of said partially fluorinated methane to said fluoro-olefin is at least 1:1, and where the reaction is carried out in an inert solvent which is the reaction product - partially fluorinated propane or partially fluorinated butane.

EFFECT: reduced amount of by-products.

30 cl, 2 tbl, 6 ex

FIELD: chemistry.

SUBSTANCE: method of producing tetrafluoropropenes involves reduction of a compound (I), selected from 1-chloro-2,2,3,3,3-pentafluoropropane (CF3CF2CH2Cl; HCFC-235cb); 2,2,3,3,3-pentafluoropropane (CF3CF2CH3; HFC-245cb) and 1-chloro-2,3,3,3-tetrafluoro-1-propene (CF3CF=CHCl). The compound (I) is obtained by reacting a compound of formula CF2=CY2, where Y independently denotes F or O, with chlorofluoromethane (CF2FCl).

EFFECT: high conversion and selectivity.

10 cl, 3 tbl, 33 ex

FIELD: chemistry.

SUBSTANCE: invention relates to a method of producing 1,4-diiodoperfluorobutane by reacting 1,2-diidoperfluroethane with tetrafluoroethylene, which involves heating 1,2-diidoperfluorethane, feeding tetrafluoroethylene into a reactor with 1,2-diiodoperfluoroethane, holding the obtained mixture at high temperature and pressure. The process is carried out in two steps: at the first step, temperature of the process is equal to 180-200C and pressure of tetrafluoroethylene in the reactor is equal to 1.3-1.7 MPa, and at the second step, temperature in the reactor is equal to 150-170C and pressure in the reactor is equal to 0.7-1.0 MPa. The obtained crude 1,4-diiodoperfluorobutane undergoes fractionation at low pressure to extract the 1,2-diiodoperfluoroethane fraction which is returned to the step for producing 1,4-diiodoperfluorobutane, and the fraction of the desired product.

EFFECT: high selectivity of the process with respect to 1,4-diiodoperfluorobutane, possibility of conducting the process without the intermediate operation for removing gaseous products during synthesis, and low consumption of raw materials.

2 cl, 6 ex

FIELD: chemistry.

SUBSTANCE: perfluorocarbons are obtained by decarboxylation and dimerisation of C6-C9 perfluorinated acids, said perfluorocarbons being treated in 0.5-2 hours with ethanol or isopropanol solution containing 0.5-4.5 wt % fluorine-containing surfactants of general formula , where RF is optionally a radical C6F13-, C8F17-, or , where n=1-2. The solvent is then distilled off, followed by drying and moulding.

EFFECT: use of the disclosed method provides a composition having a wide operating temperature range, which enables use of lubricants in unstable weather conditions.

1 ex, 1 tbl

FIELD: chemistry.

SUBSTANCE: invention relates to a method of producing perfluorocarbon-based ski lubricant for treating plastic skis. The method is characterised by that it involves distilling a halocarbon, grinding and drying. Before distilling the solvent via decarboxylation and dimerisation of C6-C9 perfluoro acids at temperature of 180C-210C, perfluorocarbons are obtained; the obtained powdered mixture of perfluorocarbons is saturated with 0.5% perfluoropolyoxapropylene carboxylic acid solution for 2 hours, followed by distillation of the halocarbon; the obtained lubricant composition is dried, crystallised and ground to 0.5-0.8 mcm using a dismembrator and pelletisation.

EFFECT: disclosed invention provides a ski lubricant with high water repellence and wear resistance, with low power consumption during production, as well as high environmental safety during production and use.

4 ex, 1 tbl

FIELD: chemical technology.

SUBSTANCE: invention relates to technology manufacturing halide-substituted hydrocarbons, in particular, to stabilization of halogenated paraffins that are used as plasticizers, antipyrenes and special additives for polymeric materials and rubber mixtures, and in leather industry and in manufacturing depressants and lubricants also. Method is carried out by addition of stabilizing system comprising epoxy-compound and chelate compound forming chelate with iron ions. Stabilizing system comprises additionally acceptor of hydrogen chloride as a stabilizing agent that represents aliphatic carboxylic acid ketene comprising carbon number in chain in the ranges (C10-C23) and alkaline-earth metal of the 2-d group of periodic system in the following ratio of components as measured for the parent halogenated paraffin, wt.-%: chelate compound, 0.03-0.50; acceptor of hydrogen chloride as a stabilizing agent, 0.05-0.30; epoxy-compound, 0.20-0.80. Addition of indicated components of stabilizing system to halogenated paraffin is carried out simultaneously or successively at temperature in the ranges 40-90oC. Stabilizing system can comprise additionally also antioxidant - a stabilizing agent of phenol type representing sterically hindered di- or trialkylphenol or its derivative, or their mixtures taken in the mount 0.01-0.15 wt.-%. Addition of indicated antioxidant - stabilizing agent is carried out before blowing or steaming acid mixtures at temperature in the ranges 40-90oC in common or separately with chelate compound. Halogenated paraffin represents chlorinated paraffin with mass part of chlorine in the ranges 12-75%. Invention provides enhancing quality of stabilized halogenated paraffins by indices "color index" and "mass part of acids", reducing consumption norm of epoxy-compound.

EFFECT: improved stabilizing method.

8 cl, 1 tbl, 16 ex

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention relates to manufacturing chloro-containing hydrocarbons, in particular, tert.-butyl chloride used for preparing addition agents and as activator for dehydrogenation catalysts. Method for preparing involves interaction gaseous isobutylene and hydrogen chloride in the presence of catalyst in the amount 0.02-0.3 wt.-% of parent reagents mass. Water is used as a catalyst. Process is carried out at volume rate of feeding reagents from 1400 h-1 to 1500 h-1, at temperature from 0oC to -5oC and in the mole ratio isobutylene : hydrogen chloride = (1.01-1.015):1 in the bubbling reactor. Method provides elevating yield of tert.-butyl chloride up to 99.2-99.5 wt.-%.

EFFECT: improved preparing method, enhanced yield.

2 cl, 1 tbl, 4 ex

FIELD: industrial organic synthesis.

SUBSTANCE: invention is dealing with production of chlorohydrocarbons exhibiting plasticizing properties in polymer compositions in production of synthetic building materials, varnishes and paints, artificial films and leathers, in rubber industry, and as fire-retardant additives in polymers. Process comprises chlorination of waste obtained in production of C14-C32 fraction by ethylene-α-olefin oligomerization. Chlorination is accomplished in two steps: addition chlorination at 35-55°C followed by substitution chlorination at 40-105°C. Chlorohydrocarbons thus obtained can, in particular, be used as secondary plasticizer in polyvinylchloride compositions.

EFFECT: reduced expenses due to using production waste.

4 tbl, 30 ex

Up!