SU1066988A1 - Process for preparing end forms of alkali metal alkylxanthogenates - Google Patents

Abstract

1. METHOD FOR OBTAINING THE FINAL FORMS OF ALKYLXANTOMBBNATES OF ALKALINE METALS by the interaction of carbon disulfide, alcohol and alkali in water with iselsovane supplement, so that, in order to increase the process, the latter is spent in the Presence as an additive dioxins alcohols in the amount of 2-3.5% by weight of the alkyl xanthate. 2. The method according to claim 1, about t l and h and iota, and with the fact that dioxaic spir-1. j is used in co, spiroef1 | rami trimethylcarbynap, meth11Lbutydiopa and dioxibic alcohols and 3-methylbutanediol, 3 in the small cohort of It (O, 1-0.2):

Description

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from 00

00 The invention relates to an improved method for producing alkali metal alkylxanthates for final forms, which are widely used in non-ferrous metallurgy as collector reagents for functional enrichment of sulfide ores of color and rare metals, as well as for the synthesis of sulfur ororganic compounds. A known method for producing alkaline metal alkylxanthates in the form of non-dusty and non-sticky pfs by using tiomamate and S-esters of xanthic acids C as additives. The disadvantage of this method is the high cost of these additives, as well as the limited field of application. The closest to the present invention is a method of obtaining alkali metal alkylxanthates for the final forms by the interaction of carbon disulfide, alcohol and alkali in water in the presence of addition or ester or tgshchinovoy acid alkyl ester t2J. The disadvantage of this method is the relatively high cost of additive additives. The purpose of the invention is to reduce the cost of the process, allowing the use of isoprene production from isobutylene and formaldehyde as an additive. The goal is achieved by the fact that according to the method for producing alkali metal alkylxanthates of the final forms, the principle is that dioxane alcohols in an amount of 2-3.5% by weight of the alkylxanthate are used as an additive in the xanthogenation stage :. Dioxane alcohols are preferably used in a mixture with trimethylcarbinsl, methylbutanediol and dioxane alcohols, 3-methylbutanediol || -1.3 in molar correlation 1: (0.1-0.2): (0.15 o, 2 Preferably, dioxane alcohols are preferably used and high-boiling components in a mixture of the following composition | wt.% 1 Dioxane alcohols 72-78 The ethyl alcohol trimethylcarOinol. a. and methylbutanediol6-10 Cc1 ortho esters of dioxai alcohols 3-6 3-Methylbutanediol-1, 310-15 in 3-5% of the mass of alkylxanthate. In the production of npeHia from 4,4-dimethyl-1,3-dioxane, which It is obtained by the condensation of isobutylene with formaldehyde, and a number of side high boiling products are formed: 3-methylbutanol-1,3, dioxane alcohols (4-methyloxyethyl-1,3-dioxane, 4,4-dimethyl-5-oxymethyl-1, 3- dioxane and 5- (2-OXI-2-PROPIL / -1, 3-dioxane and alcohol esters (1-.-tert.butoxy-3-methyl-3-butanol, 4-methyl-4- / 2-tert.butoxyethyl hl, 3-i -} 1, ioxa, n, 4-4-dimethyl-5- (tert butoxymethyl) -1, .3-dioxane, methyl tert-butyl ether, 1-methoxy-3-methyl-3- butanol), the composition is close to this mixture .. The implementation of the proposed method improves the quality of the target odukta and increase its output by formation of an additional quantity of xanthates at ksantogenirovanii dioxane alcohols, which leads to a complete conversion of the carbon disulfide to the reaction mixture and the sashm prevents formation on its basis byproducts osnovnymk of which are trithiocarbonate and thiosulfate. The content of the basic substance in the target product is up to 98% with the output of the latter up to 97%. In the case of xanthogenesis in the presence of dioxane alcohols and mainly alcohol esters and a diode, the sequential alkyl xanthates are obtained in the form of non-collapsible and non-contiguous powders. The achieved effect in this case is due to the fact that the high and low boiling point components of the additive, for example, alcohol esters and diol, which do not react with carbon disulfide, create my molecular liquid interlayers between the particles of dried xanthate, prevent the particles from separating from each other (dusting and provide hydrophobization of the powder, which causes incompatibility of the product during long-term storage. i The degree of dusting of the product, determined by the velocity of the fluidization stream, reaches 1.1-1.2 m / s. and {oynsanthogenates with a relative humidity of 80.0% of the environment do not exceed 8-10%. Example 1. A reactor with a capacity of 500 MP equipped with a stirrer, a reflux condenser and a thermometer, with an optimal molar ratio of reagents, is charged 29.4 g (0.53 mole). ) potassium hydroxide, 220 g (2.98 mol of isopropyl alcohol, 974 bg (0.58. Additionally, 1.82 g (2.0% of the isopropyl xanthate | dioxane alcohols as an additive) are added to the reactor. The reactor is placed in a water bath with TO-BO and mixed thoroughly until complete dissolution of the alkali. Then, the reaction mass is cooled to 20–300 Civ, while the mixer is turned on, 39.8 g (0.53 mol of carbon disulfide) are metered in for 15–20 minutes, while the temperature of the reaction mass is maintained no higher by adjusting the carbon disulfide feed rate and water bath temperature. After the addition of carbon disulfide, stirring is carried out for 5-10 mins, / a mixture of α-alcohol and water is distilled off from the reaction mass, and the resulting concentrated reaction mass in the form of a paste is dried in a vacuum box at a pressure of 150-20: 0 mm at 60-70 ° C. within 1 hour. / Get 88.5 G (97, 0% of the theory of isopropylxant, kgshi ogenate with the main substance content of 97.0%. Composition of cannular impurities, May.%: T, CgS3.52 Moisture and volatile Dusting of the resulting powder, determined by the gaseous flow, resulting in weight the test specimen in a pseudo-liquefied state is 0.9 m / s. Pa. The moisture content of the powder, determined after storage for 300 hours in a mixture with a relative humidity of 80.0%, is 9%. The estimated useful life is 3–4 g. p 2. Preparation of potassium isopropyl xanthate is carried out as described in Example 1, with the only difference that 3.2 g (3.5% of the dioxane alcohols formed according to xanthate} theory) are additionally charged to the reactor as an additive. Obtain 89.6 g (98.1% of the theory of potassium isrpropyl xanthate with a content of the main substance of 97.8%. The composition of mineral impurities, may.%: K f Iv l Sac to 2 S Moisture and volatiles Powder dusting is 1.1 1, 2 m / s, the equilibrium moisture content at a relative humidity of qpe of 80.0% is 7%, the powder does not cake during storage, the predicted practicality is no more than 4 g. I Example 3. Analogously to Example 1 of 70.0 g (1.25 1 mol) potassium hydroxide, 94.0 g (1.27 mol) of H-butyl alcohol and 91.0 g (1.2 mol) of carbon disulfide in the presence of 45.0 b (2.5 mol) of water and 8 , 8 g of mixture dioxane alcohols, alcohol esters of trimethylcarbinol, methylbutanediop and dioxane alcohols and 3-methylbutanediol (1: 0.1: 0.15 ratio) 202.8 g yield 86.3% of the theory of potassium butylxanthogenate containing the basic substance as an additive 89.0%. Powder dripping is 1.1 m / s, the equilibrium moisture content at 80% relative humidity is 9.8%. The powder does not cake during long term storage. The estimated useful life of at least 3g. Example 4. Analogously to example 3, in the presence of, as an additive, 6.6 g of a mixture of dioxane alcohols, alcoholic spirits of trimethylcarbinol, methylbutanediol and dioxane alcohols and 3-methylbutanediol (1: 0.2: 0.2 ratio) get 292-, 5 g (yield 86.1% of theory) potassium n-butyl xanthate with a basic substance content of 90%. The dusting of the powder contributes 1.1 m / s, an equilibrium moisture content of 8.0% at a relative humidity of 80%. Powder. Does not cake during storage. Example 5. Analogously to Example 1 ,, out of 25.44 g (0.636) of caustic soda; 191.0 g (3.18 mol) of isopropyl alcohol and 48.4 g (0.636 mol) of carbon disulfide in the presence of 35.4 g (1.91 mol) of water and as an additive 3.12 g 13% of the resulting xanthate ) mixtures of dioxane alcohols with high boiling point components, wt.% Dioxane alcohols. .72.0 Spirtoether of trimethylcarbinol and methylbutanediol 10, O Dioxane alcohol spirits3.0 3-Methylbutanediol 15.0. Get 96.1 g (yield 92.4% of theory) sodium isopropyl xanthate with. content of the main substance of 89.5%. The dusting of the powder is 1.0 m / s, the equilibrium moisture content is 10% at a relative humidity of 80%. The powder does not cake during storage. Example 6. Similarly, he will take 5, in the presence of as an additive 5.2 g (5% of the type of xanthate), a mixture of dioxane alcohols with high-boiling components, 97.7 g (yield 94.0% of theory) of sodium isoprpylxanthate with a content of main substance 91.6%. The dusting of the bedrock is 1.3 m / s, the equilibrium water content is 9.5%, and the osipate moisture content is 80%. The powder does not agglomerate.

Example 7, analogously to Example 1, of 41.0 g (0.73 mol / potassium hydroxide, 168.0 g (3.66 mol) of ethanol and 55.8 g (0.73 mol) of carbon disulfide in the presence of 35.6 g (i ", 97 mol) of water and, in addition to 3.5 g (3% of the resulting xanthate), a mixture of dioxane alcohols with high-boiling components of the composition, wt.%: Dioxane alcohols 78.0 Carbinoia trihydrate and methylbutanediol 6fO Dioxane slarts ethers 6.0 3 methylbutanediol get 112.3 g (yield 96.2% of potassium ethyl xanthate gene theory with basic substance content 95.8%, Dusting porsmac is 0.9m / s, equilibrium moisture content of 10% at a relative humidity of 80%. The powder is not caking during storage. The estimated useful life is 3-4 g.

Example 8. Analogously to Example 7, in the presence of 5.8 g (5% of KcaHToreHaTaj formed of a mixture of dioxanNew alcohols with high-boiling components, Nentami), 114.9 g (yield 97.5% of theory) of potassium ethylxanthogenate 1c with the content of the main substances 96.0%. Porisic dusting is 1.2 m / s, the equilibrium moisture content is 9%. The porosic does not clot during storage.

Under similar conditions, with an optimal ratio of reagents, samples of various xanthates are obtained.

Properties of the obtained samples are shown in the table.

IsoproshshantbgenaF

Kali

2.0 3.5

1 $ 0.1; 0.15

(1.9 g) 1: 0.2: 0.2

(3.1 g),

3.0

5.0

th-butylxanthengens

Kali

2.0

3.5

50 9 7 7.5

 97,81,2

6.9 7.5

97.91.1 98; 21.2 7.0

60

83.0 0.1

10 88.2 0.7

9 91.0 0.9

(4.9 g) l: 0.2tO, 2

(8.2 g)

Potassium Ethyloxants

2.0 3.5

1: 0.1: 0.15 12.3 g) 1: 0.2: 0.2

Continuation of the table

.3

8.0

1.2

92.6 92.5

Table continuation

Claims (3)

1. METHOD FOR PRODUCING ALKYL ALGANIC ALKALINE PRODUCTS METALS by the interaction of carbon disulfide, alcohol and alkali in water with the use of an additive, distinguished by the fact that, in order to reduce the cost of the process, the latter is carried out in the presence of an additive 72-78 rams of trimethylcarbinol, methylbutanediol and dioxane alcohols and 3-methylbutanediol-1,3 in a molar ratio of 1 "(0.1-0, 2) g '(0.15-0.27. 3. The method according to PP. 1 and 2, which is noteworthy because I use dioxane alcohols and high-boiling components as an additive in the following mixture, May -5% by weight of alkyl xanthogenate. 6-10 10-15, σ> о со оо оо