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Preparation method of xanthate

A technology of xanthate and raw materials, which is applied in the field of preparation of xanthate compounds, can solve problems such as unfavorable alkali dispersion or dissolution, difficult separation of xanthate, and strong pungent odor, so as to avoid irritating Odor, high conversion rate of raw materials, light odor effect

Active Publication Date: 2016-03-09
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] However, solvents such as carbon disulfide, raw material alcohol, benzene, toluene, xylene, ethylbenzene, ethylene dichloride, acetone, sherwood oil, water, gasoline, kerosene in the prior art, or high boiling point, and xanthate Difficulty separating (raw material alcohol, benzene, toluene, xylene, ethylbenzene, gasoline, kerosene), or promoting the occurrence of side reactions (carbon disulfide, water), or participating in the reaction during the reaction (dichloroethane, acetone), or It is not conducive to the dispersion or dissolution of alkali, and the reaction efficiency is low (benzene, toluene, xylene, ethylbenzene, gasoline, kerosene, petroleum ether). Although the purity and yield of xanthate synthesized by solvent method are slightly higher than those of kneading method, However, there is still a strong pungent smell of xanthate products, and there is still room for improvement in purity and yield, especially if the carbon chain is C 6 The yields of high-grade xanthate, ethyl xanthate and dixanthate compounds are low, so there are few reports on the commercial preparation of xanthate compounds by solvent method

Method used

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  • Preparation method of xanthate

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Experimental program
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Effect test

Embodiment 1 10

[0049] The preparation of embodiment 1 sodium dodecyl xanthate

[0050] Add 17.78 parts of tetrahydrofuran with a purity of 99% into the reactor, start stirring, add 18.63 parts of dodecanol with a purity of 99%, stir for 10 minutes, and add 4.2 parts of granular sodium hydroxide with a purity of 96% in batches. In a container, fully stir for 20 minutes at 5-20°C. Then slowly add 7.84 parts of carbon disulfide, and then stir and react at 10-20°C for 3 hours after the addition. After the reaction was completed, the reaction mixture was distilled and dried to obtain a sodium dodecyl xanthate product with a purity of 99.1%. The product had a light odor and was non-irritating. The yield based on dodecyl alcohol was 97.5%.

Embodiment 2

[0051] The preparation of embodiment 2 hexyloxyethyl xanthate potassium

[0052] Add 13.33 parts of tetrahydrofuran with a purity of 99% into the reactor, start stirring, and add a total of 6.6 parts of flake potassium hydroxide (purity 85%) into the reactor in batches, stir well; slowly add 14.92 parts at 5 to 20°C Parts of ethylene glycol monohexyl ether with a purity of 98% were added, and stirring was continued for 10 minutes after the addition was complete. Then slowly add 7.74 parts of carbon disulfide, and then stir and react at 10-22°C for 2.5 hours after the addition. After the reaction was completed, the reaction mixture was distilled and dried to obtain a potassium hexyloxyethyl xanthate product with a purity of 98.2%. The product had a light odor and was non-irritating. The product yield based on ethylene glycol monohexyl ether was 97.2%.

Embodiment 3

[0053] Embodiment 3 diethylene glycol and sodium hydroxide prepare sodium dixanthate

[0054] Add 13.33 parts of tetrahydrofuran with a purity of 99% into the reactor, start stirring, and add 4.3 parts of granular sodium hydroxide (purity 96%) in batches to the reactor, stir well; slowly add 5.31 Parts of diethylene glycol with a purity of 99% were stirred and reacted for 20 minutes after the addition was completed. Then slowly add 7.91 parts of carbon disulfide, and then stir and react at 10-22°C for 2.5 hours after the addition. After the reaction was completed, the reaction mixture was distilled and dried to obtain a sodium diethylene glycol dixanthate product with a purity of 99.2%. The product had a light smell and was non-irritating. The yield based on diethylene glycol was 97.1%. .

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Abstract

The invention discloses a preparation method of xanthate. According to the preparation method, tetrahydrofuran is taken as the reaction medium, monohydric alcohol or dihydric alcohol and caustic alkali carry out reactions at a temperature of 0 to 30 DEG C, finally desolvation is performed to obtain high purity xanthate, and the yield is high. The obtained xanthate has the advantages of little odor, higher purity, and higher yield, and is especially suitable for being used to prepare high grade xanthate with a carbon chain having a carbon number of 6 or more, ethyl xanthate, and dixanthate.

Description

technical field [0001] The invention relates to a preparation method of xanthate compounds. Background technique [0002] Xanthate, commonly known as "xanthate", the basic formula is: [0003] [0004] In the formula, R is an alkyl group with different carbon chain lengths, aryl group, alkoxy group, cycloalkyl group, etc., and the R group with more than 4 carbon atoms is called high-level xanthate, and the one with less than 4 carbon atoms is called low-level xanthate. Medicine; Me is generally sodium or potassium. In 1815, Zeise synthesized xanthate for the first time; in 1925, Keller discovered that xanthate could be used as a flotation collector for sulfide minerals. At present, xanthate is still the most widely used sulfide ore collector. [0005] The methods of synthesizing xanthate mainly include "kneading method" and "solvent method". The kneading method is currently the main method for synthesizing xanthate. It directly adds alcohol and carbon disulfide to the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C329/14
CPCC07C329/14
Inventor 刘广义黄耀国
Owner CENT SOUTH UNIV
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