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Preparation method of dihydrate hexamethylene-1,6-disodium dithiosulfate

A technology of disodium dithiosulfate and hexamethylene dihydrate is applied in the field of preparation of hexamethylene dihydrate 1,6-dithiosulfate disodium salt, which can solve the problem of low reaction yield and adaptability , long reaction time and other problems, to achieve the effect of high reaction yield, simple and convenient separation

Active Publication Date: 2014-05-28
HEZE JIACHENG CHEM CO LTD
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  • Abstract
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Problems solved by technology

Chinese patent CN200610060884 reports that sodium thiosulfate and dichloro (or dibromo) hexane are directly heated and reacted under ethanol as a solvent. According to this method, gas with pungent odor will be produced during the reaction process, and the reaction yield is low. At the same time, the product is separated The resulting liquid is not further utilized and is not suitable for production applications
"Synthetic Rubber Industry" reported on pages 152-154 of No. 3, 2001, that water was directly used as solvent for reflux reaction, and after cooling and crystallization, dihydrate hexamethylene-1,6-dithiosulfuric acid disodium salt was precipitated; Chinese patent CN200510074134 .9 The reaction operation process is further given in detail. The reaction is carried out in a water solvent, and the reaction is controlled by adjusting the pH value. The reaction yield reaches 93%, but the patent does not propose dihydrated hexamethylene 1,6-dithiosulfuric acid The effective separation method of disodium salt, the reaction mixed solution adopts cooling overnight crystallization to obtain flocculent precipitation, by means of a kind of sintered glass separation, repeat the example 1 method of this patent, the reaction time required for making solvent with water is longer (boiling for 9 hours ), the obtained precipitate is very fine and difficult to be separated by conventional separation means, and after the mother liquor is further concentrated, the obtained product is basically in the form of a slurry, which is extremely difficult to separate. This patent is difficult to realize industrial production
None of the above-mentioned technologies mentioned reasonable treatment measures for the mother liquor, and it is difficult to adapt to the current environmental protection chemical production requirements

Method used

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  • Preparation method of dihydrate hexamethylene-1,6-disodium dithiosulfate

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Into the 2000L reaction kettle that is equipped with stirring, reflux condenser, online pH meter, high level tank, drop into 1020kg and prepare ethanol aqueous solution that ethanol content is 60%, 420kg sodium thiosulfate pentahydrate, 120kg 1.6-dichlorohexane mix and stir . Pump 50L of prepared 5% sodium hydroxide aqueous solution into the high-level tank, and the pH value is measured at about 8.0 at this time. Begin to heat up, reflux reaction, the temperature is at 84 ℃. With the progress of the reaction, the online pH meter found that the pH value was constantly decreasing. At this time, 5% aqueous sodium hydroxide solution was added dropwise to keep the pH value between 7.5-8.0. After about 7 hours of reflux reaction, no 5% aqueous sodium hydroxide solution was added dropwise at this time, and the pH of the reaction solution was between 7.5-8.0, and basically no longer dropped. At this time, about 42 L of 5% sodium hydroxide aqueous solution was used. Reduc...

Embodiment 2

[0022] In the 2000L reactor that stirring, reflux condenser, on-line pH meter, high level tank are installed, drop into by centrifuging and reclaiming mother liquor 1040kg in the implementation example 1, add 60kg95% ethanol, add 40kg purified water, drop into 384kg pentahydrate thiosulfate again Sodium sulfate, drop into 120kg 1.6-dichlorohexane and mix and stir. Pump 50L of prepared 5% sodium hydroxide aqueous solution into the high-level tank, slowly add 5% sodium hydroxide aqueous solution to the reaction mixture, and adjust the pH value between 7.5-8.0. Begin to heat up, reflux reaction, the temperature is at 85 ℃. With the progress of the reaction, the online pH meter found that the pH value was constantly decreasing. At this time, 5% aqueous sodium hydroxide solution was added dropwise to keep the pH value between 7.5-8.0. After about 7 hours of reflux reaction, it was found that colorless transparent crystals were precipitated (sodium chloride crystals). At this time,...

Embodiment 3

[0024] In the 2000L reactor that is equipped with stirring, reflux condenser, on-line pH meter, high level tank, drop into 1020kg and prepare ethanol aqueous solution that ethanol content is 50%, 653kg sodium thiosulfate pentahydrate, 204kg 1.6-dichlorohexane are mixed and stirred . Pump 250L of prepared 1% sodium hydroxide aqueous solution into the high-level tank, and the pH value at this time is measured to be around 8.0. Begin to heat up, reflux reaction, the temperature is at 80 ℃. Along with the progress of the reaction, the online pH meter found that the pH value was constantly decreasing. At this time, 1% aqueous sodium hydroxide solution was added dropwise to keep the pH value at 7.5. After about 7 hours of reflux reaction, no 1% aqueous sodium hydroxide solution was added dropwise at this time, and the pH of the reaction solution was at 7.5, which basically did not drop. At this time, about 210 L of 1% sodium hydroxide aqueous solution was used. Reduce the sti...

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Abstract

The invention relates to a preparation method of dihydrate hexamethylene-1,6-disodium dithiosulfate. The preparation method comprises the following steps: firstly, adding ethanol water with the ethanol content of 50-70% or recycled mother liquor into a reaction kettle, then adding sodium thiosulfate pentahydrate and 1,6-dichlorohexane, stirring and warming to prepare a sodium hydroxide water solution, when the sodium hydroxide water solution is not dripped any longer, continuously stirring in a backflow manner, reducing the temperature to be below 40 DEG C while stirring at a low speed, discharging and centrifugally separating, drying, oiling, smashing and packaging to obtain an anti-reversion agent finished product. The preparation method has the benefits that the product prepared through the technology has the purity reaching 99% and the yield of more than 95%, and is simple and convenient to separate and high in reaction yield; mother liquor in the production process can be repeatedly used; the preparation method is green and environment-friendly, does not need to process emissions, and is suitable for the current green and environment-friendly chemical industry production requirement.

Description

(1) Technical field [0001] The invention belongs to the field of organic chemistry and relates to a preparation method of dihydrated hexamethylene 1,6-dithiosulfuric acid disodium salt. (2) Background technology [0002] Dihydrated hexamethylene-1,6-dithiosulfate disodium salt is a new type of anti-reversion agent, which can improve the anti-reversion performance of sulfur vulcanized rubber materials. The use of this product can increase the simultaneous vulcanization of rubber products quality and longevity of the product. [0003] The preparation of dihydrate hexamethylene-1,6-dithiosulfate disodium salt is generally carried out by reacting sodium thiosulfate with 1,6-dihalogenated (usually dichloro)hexane. Experiments have shown that the results of different reaction conditions vary greatly, and some existing small-scale test reports still need further corrections in technology. Chinese patent CN200610060884 reports that sodium thiosulfate and dichloro (or dibromo) hexa...

Claims

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Application Information

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IPC IPC(8): C07C381/02
Inventor 王平生赵士杰刘志强崔平刚
Owner HEZE JIACHENG CHEM CO LTD
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