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Synthetic method for disulfide diisopropyl xanthate

A technology of diisopropyl xanthate disulfide and a synthesis method is applied in the field of chemistry, can solve the problems of a large amount of waste water containing salt and organic matter, cannot meet industrial production, low product yield and purity, etc., and achieves stable reaction. , easy to control, the effect of improving yield and purity

Inactive Publication Date: 2015-07-15
LANZHOU TAISHUN TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Above two kinds of methods all are to prepare diisopropyl xanthate disulfide compound with sodium isopropyl xanthate as starting raw material, wherein, the product yield and the purity that potassium persulfate oxidation method obtains are all lower, cannot To meet industrial production, the hydrogen peroxide oxidation method needs to be acidified with concentrated sulfuric acid first, then hydrogen peroxide oxidation, and then needs to add soda ash to neutralize the acid in the reaction solution. The economic cost is high, the process is cumbersome, and a large amount of salt and organic matter waste water

Method used

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  • Synthetic method for disulfide diisopropyl xanthate
  • Synthetic method for disulfide diisopropyl xanthate

Examples

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Embodiment 1

[0033] Example 1 The synthetic method of diisopropyl xanthate disulfide comprises the following steps:

[0034] ⑴Synthesis of alkali metal alkoxide:

[0035] Using isopropanol (60.06g, 1.0mol) as the starting material, tetrahydrofuran (180.18 g) was added as the reaction solvent, and alkali metal hydroxide (30.03g, 0.75mol) was added at room temperature, and then the temperature was raised to 65°C for Reflux the reaction, cool down to room temperature after 0.5h, and obtain the alkali metal alkoxide reaction solution.

[0036] Wherein: the weight of tetrahydrofuran is 3 times of the weight of isopropanol; the weight of alkali metal hydroxide is 0.5 times of the weight of isopropanol.

[0037] The alkali metal hydroxide is sodium hydroxide.

[0038] ⑵ Synthesis of xanthate intermediates:

[0039] Using the water seal pressure method, slowly add carbon disulfide dropwise to the alkali metal alkoxide reaction solution at -5°C, and stir for 8 hours to obtain the xanthate ...

Embodiment 2

[0050] Example 2 The synthetic method of diisopropyl xanthate disulfide comprises the following steps:

[0051] ⑴Synthesis of alkali metal alkoxide:

[0052]Using isopropanol (60.06g, 1.0mol) as the starting material, tetrahydrofuran (180.18 g) was added as the reaction solvent, and alkali metal hydroxide (30.03g, 0.75mol) was added at room temperature, and then the temperature was raised to 60°C for Reflux the reaction, cool down to room temperature after 2h, and obtain the alkali metal alkoxide reaction solution.

[0053] Wherein: the weight of tetrahydrofuran is 3 times of the weight of isopropanol; the weight of alkali metal hydroxide is 0.5 times of the weight of isopropanol.

[0054] The alkali metal hydroxide is sodium hydroxide.

[0055] ⑵ Synthesis of xanthate intermediates:

[0056] Using the water seal pressure method, at 5°C, slowly add carbon disulfide dropwise into the alkali metal alkoxide reaction solution, and stir for 10 hours to obtain the xanthate ...

Embodiment 3

[0067] Example 3 The synthetic method of diisopropyl xanthate disulfide comprises the following steps:

[0068] ⑴Synthesis of alkali metal alkoxide:

[0069] With isopropanol (60.06g, 1.0mol) as the starting material, tetrahydrofuran (360.36 g) was added as the reaction solvent, alkali metal hydroxide was added at room temperature, and then the temperature was raised to 70°C for reflux reaction, and the temperature was lowered to At room temperature, the alkali metal alkoxide reaction liquid is obtained.

[0070] Wherein: the weight of tetrahydrofuran is 6 times of the weight of isopropanol; the weight of alkali metal hydroxide is 0.6 times of the weight of isopropanol.

[0071] The alkali metal hydroxide is sodium hydroxide.

[0072] ⑵ Synthesis of xanthate intermediates:

[0073] Using the water seal pressure method, at 0°C, slowly add carbon disulfide dropwise into the alkali metal alkoxide reaction solution, and stir for 9 hours to obtain the xanthate intermediate...

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Abstract

The invention relates to a synthetic method for disulfide diisopropyl xanthate. The method comprises the following steps that 1, alkali metal alkoxide is synthesized, wherein isopropyl alcohol is used as a starting raw material, tetrahydrofuran is used as reaction solvent, alkali metal hydroxide is added for carrying out a backflow reaction, and then cooling is carried out to obtain an alkali metal alkoxide reaction solution; 2, an xanthate intermediate is synthesized, wherein a water seal pressing method is adopted for slowly dripping carbon disulfide into the alkali metal alkoxide reaction solution to obtain the xanthate intermediate; 3, the xanthate intermediate is activated, wherein water and iodine are added into the xanthate intermediate to carry out an activating reaction to obtain an activated xanthate intermediate; 4, hydrogen peroxide oxidizing is carried out, wherein hydrogen peroxide is slowly dripped into the activated xanthate intermediate to carry out a reaction in a heat-preserving mode to obtain disulfide diisopropyl xanthate mixed liquor; 5, reactive crystallization and purification are carried out, wherein the disulfide diisopropyl xanthate mixed liquor is distilled and cooled to separate out crystals, then water is added, and the disulfide diisopropyl xanthate mixed liquor is stirred and filtered to obtain the high-purity disulfide diisopropyl xanthate. According to the method, the process is simple, the cost is low, and the yield is high.

Description

technical field [0001] The invention relates to the field of chemistry, in particular to a synthesis method of diisopropyl xanthate disulfide. Background technique [0002] Compound disulfide diisopropyl xanthate (English name: dithiodiisopropyl xanthate, CAS number: 105-65-7, molecular formula: C 8 h 14 o 2 S 4 , molecular weight: 270.46) is a molecular weight regulator for synthetic rubber polymerization, lubricating oil additives, ore flotation agents, fungicides, herbicides and other intermediates; it can also be used as an accelerator in rubber processing, natural rubber and latex, styrene-butadiene Superaccelerator for rubber and latex, nitrile rubber and reclaimed rubber. It can also be used in the manufacture of adhesive plasters, medical and surgical rubber products, rubber shoes, waterproof cloth, natural glue and latex products, etc. [0003] The structural formula of diisopropyl xanthate disulfide is as follows: [0004] [0005] At present, the method of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C329/14
Inventor 彭维恩尚涛李卫平
Owner LANZHOU TAISHUN TECH CO LTD
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