The method of simultaneous receipt of chloroform and sodium formate

 

(57) Abstract:

The invention relates to the production of sodium formiate and obtaining thus purified chloroform. The method of simultaneous receipt of chloroform and sodium formate includes processing technical Chlorella resulting from the interaction of ethanol with gaseous chlorine, aqueous solution of sodium hydroxide. Target products produce by sedimentation and separation of the lower layer of chloroform and the top aqueous solution of sodium formiate, which expose oparka and drying by heating at a predetermined temperature to obtain commercial sodium formate. In the process of interaction of ethanol with gaseous chlorine perform simultaneous distillation of Chlorella in the rectifying mode. Thus from a bottom part of the output of the high-boiling components, which are subjected to neutralization. The result is improved quality of marketable sodium formate by reducing impurities in it crotonic aldehyde, of polymers of ethylene, etc. generated in the technical chorale on stage chlorination. At the same time achieve a high degree of purity of chloroform. 3 C.p. f-crystals.

The invention relates to the field of chemical engineers the openings, runways, roofs, etc. as a silage preservative mixtures as food additives in some types of feed, and so on) and obtain thus purified chloroform (as a basic semi-finished product or finished product).

The closest known prior art solution is a way of simultaneously receiving chloroform and sodium formate by processing technical Chlorella resulting from the interaction of ethanol with gaseous chlorine, aqueous sodium hydroxide solution, followed by separation of the target product by sedimentation and separation of the lower layer of chloroform and the top aqueous solution of sodium formiate, which expose oparka and drying by heating at a predetermined temperature to obtain commercial sodium formate (EN 2076854, 10.04.97).

The disadvantages of this method are as low as sodium formate due to the high content of impurities formed in the technical chorale.

The present invention is to increase the efficiency of production of sodium formate with high purity chloroform.

The problem is solved due to the fact that in the method of simultaneous polumutanty ethanol with gaseous chlorine, aqueous sodium hydroxide solution, followed by separation of the target product by sedimentation and separation of the lower layer of chloroform and the top aqueous solution of sodium formiate, which expose oparka and drying by heating at a predetermined temperature to obtain commercial sodium formate, according to the invention in the process of interaction of ethanol with gaseous chlorine perform simultaneous distillation of Chlorella in rectification mode with output from a bottom part of the high-boiling components subjected to neutralization.

However the output of the high-boiling components can be carried out with part of Chlorella formed during the interaction of ethanol with gaseous chlorine, mainly in the amount of 4-20%.

Derived high-boiling components may be exempt from associated Chlorella with additional distillation with return of the separated fractions containing chloral, in the process of interaction of ethanol with gaseous chlorine.

Disposal of high-boiling components withdrawn from the process of interaction of ethanol with gaseous chlorine and released from Chlorella, can be done by hydrolysis, mainly aqueous solution of hydroxytoluene efficiency by improving the quality of a commodity formate sodium by reducing the impurities in it (crotonic aldehyde, polymers of ethylene and other), resulting in a technical chorale due to chlorination components denatured synthetic alcohol or components hydrolysis of ethyl alcohol (fusel oils), and simultaneously maintaining a high degree of purity of chloroform.

The method of simultaneous receipt of chloroform and sodium formate is as follows.

Get technical chloral interaction of ethanol with gaseous chlorine, conduct its subsequent treatment with an aqueous solution of sodium hydroxide, followed by separation of the target product by sedimentation and separation of the lower layer of chloroform and the top aqueous solution of sodium formiate, which expose oparka and drying by heating at a predetermined temperature to obtain commercial sodium formate. In the process of interaction of ethanol with gaseous chlorine perform simultaneous distillation of Chlorella in rectification mode with output from a bottom part of the high-boiling components, which are subjected to neutralization. Conclusion high-boiling components is performed with part of Chlorella formed during the interaction of ethanol with gaseous chlorine, mainly in the amount of 4-20%. the return of the separated fractions, containing chloral, in the process of interaction of ethanol with gaseous chlorine. Disposal of high-boiling components withdrawn from the process of interaction of ethanol with gaseous chlorine and exempt from florala, carried out by hydrolysis, mainly aqueous solution of sodium hydroxide at boiling.

Example 1.

For simultaneous receipt of chloroform and sodium formiate use denatured synthetic alcohol that contains the main substance in the number 91, 3 wt.%, as impurities are present CROTONALDEHYDE and 0.37 wt. %, ethyl ester and 1.0 wt.%, polymers of ethylene, 0.1 wt.%, isopropanol, acetone and methyl ethyl ketone in an amount of 1.2 wt.%.

Chlorination of ethyl alcohol is carried out in a cascade of two devices - charator and perchlorate counterflow supply of reagents. The volume of charator 300 ml, the volume of perchlorate 200 ml. Temperature chloretone support within 89-97oC, perchlorate 59 - 65oC. Chlorine at a rate of 10 l/h served in charator through distillation capacity installed in the path of chlorine in charator. This tank gradually fills the reaction mass, which forcibly removed from charator. The reaction mass contains Vysoky mixture of charator served in the distillation column efficiency 5 theoretical plates. In the light fraction is taken away chloral - rectified, and cubic faction return to charator. Gas-vapor phase of the reflux condenser of the distillation column is sent to perchlorate, which serves the original alcohol at a rate of 10 ml/h of the Reaction mass from perchlorate gravity is directed in charator. Periodically from charator with an average rate of 1.8 ml/h (2.7 g/h) output high-boiling components with part of Chlorella formed during chlorination of ethanol, and sent to distillation capacity, which keep the temperature of 100-110oC. steady state in 1 ml of extracted high-boiling components with part of Chlorella spend 1 - 2 l of chlorine. Gas-vapor mixture from the distillation vessel without cooling is sent to XLERATOR, and non-volatile residue is collected and sent for disposal. Gas-vapor phase of perchlorate through a capacitor referred to trap hydrogen chloride to obtain hydrochloric acid.

90 h of process process 900 ml of synthetic ethanol and 0.9 m3chlorine. You get a 1.4 kg technical Chlorella content (wt.%) the basic substance of 78.8, dichloroacetamide 5,6, hydrogen chloride and 2.5 and 4.9 kg 27% hydrochloric acid is hanicheskih substances, mostly in the form of chlorocarbonic acids and aldehydes.

With the high-boiling components from charator output and return on chlorination{(2,790 - 195):[(2,790 - 195) +14,000,788]}100 = 4 wt.% Chlorella formed during chlorination of ethyl alcohol.

Technical chloral, released from the high-boiling components, is subjected to treatment with an aqueous solution of sodium hydroxide at a temperature of approximately 40oC. Just spent 300 g technical Chlorella containing 3000,788 = 236,4 g (1,603 mol) of trichloroacetaldehyde and 3000,056 = 16,8 g (0,149 mol) of dichloroacetamide.

Processing technical Chlorella spend 200 g of 40% aqueous sodium hydroxide solution (2.2 mol). Processing time of 1.5 hours the resulting mixture is separated by settling.

Get 190 g (1,590 mol) of chloroform containing 0.002 wt.% dichloropropylene. The output of chloroform 1,590 : 1,603100 = 99,19 wt.%. From the aqueous solution by evaporation and drying obtain 128 g of sodium formiate, containing no chlorinated organic components (less than 0.001%).

Non-volatile residue after the liberation from Chlorella containing 51,04 wt.% chlorine in the form of organochlorine substances, hydrolyzing an aqueous solution of sodium hydroxide. In a flask with a reverse holodilniki is heated to boiling and incubated for 2 h with stirring and at a low boil. The efficiency of hydrolysis of chloro-organic compounds in these conditions is 99%.

Example 2.

The simultaneous receipt of chloroform and sodium formate were carried out as in example 1, with increasing average speed selection high-boiling components from charator twice - 3.6 ml/h (5,4 g/h). Selected high-boiling components are exempt from Chlorella in the rectifying mode, light fraction Chlorella return in charator and cubic fraction is sent for disposal.

45 h process 450 ml of synthetic ethanol and 0.45 m3chlorine. You get 0.7 kg technical Chlorella content 79,0 wt. % of the basic substance. From the rectifying column bottom deduce 99 g of non-volatile residue containing 52 wt.% chlorine in the form of organochlorine substances.

With the high-boiling components from charator output and return on chlorination{ (5,445 - 99): [(5,445 - 99) + 700 0,79]}100 = 20,7% Chlorella formed during chlorination of ethyl alcohol.

Chloroform was obtained from technical Chlorella, released from the high-boiling components, contains as an impurity dichloropropylene at a concentration of less than 0.001 wt.% and does not require oleum clean.

1. The method of simultaneous receipt of chloroform and sodium formate by processing technical Chlorella resulting from the interaction of ethanol with gaseous chlorine, aqueous sodium hydroxide solution, followed by separation of the target product by sedimentation and separation of the lower layer of chloroform and the top aqueous solution of sodium formiate, which expose oparka and drying by heating at a predetermined temperature to obtain commercial sodium formate, characterized in that in the process of interaction of ethanol with gaseous chlorine perform simultaneous distillation of Chlorella in rectification mode with output from a bottom part of the high-boiling components, which are subjected to neutralization.

2. The method according to p. 1, characterized in that the output of the high-boiling components is performed with part of Chlorella formed during the interaction of ethanol with gaseous chlorine, mainly in the amount of 4 to 20%.

3. The method according to any of the p. 1 or 2, characterized in that the derived high-boiling components released from the associated Chlorella with additional distillation with return of the separated fractions containing chloral, in the process of interaction of ethanol with gay components, derived from the process of interaction of ethanol with gaseous chlorine and exempt from florala, carried out by hydrolysis, mainly aqueous solution of sodium hydroxide at boiling.

 

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