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Preparation method of sodium polysulfide

A sodium polysulfide and sodium hydroxide technology, which is applied in the preparation of organic compounds, chemical instruments and methods, sulfur compounds, etc., can solve the problems of increased production costs, large storage costs, and poor market prospects for sodium thiosulfate. problem, to achieve the effect of saving resources

Active Publication Date: 2018-12-04
LIAONING HONGSHAN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The output of waste liquid is large, and the storage cost is large; there are many impurities, the purification cost is high and difficult, and the production cost of the product increases; as a by-product, the market prospect of sodium thiosulfate is not good

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] A kind of preparation method of sodium polysulfide, carries out successively according to following steps:

[0026] Step 1: preparing sodium polysulfide;

[0027] a1, take Na respectively 2 S·9H 2 17.6 grams of O, 9.1 grams of sublimed sulfur, 15.6 grams of solid sodium hydroxide, and 192 grams of water are added to the reactor;

[0028] a2. Stir and heat, heat up to 85°C, dissolve the material, keep stirring for 3 hours;

[0029] a3, after the insulation reaction finishes, stop heating, cool down to room temperature, filter the reaction solution, filter out unreacted sulfur, detect the sodium polysulfide content 62g / L to the filtrate, and the polysulfide index is 2.0;

[0030] Step 2: refining p-aminobenzaldehyde;

[0031] b1. Weigh 25 grams of p-aminotoluene and 160 ml of ethanol into a three-necked flask, start stirring, heating, condensing, and raise the temperature to 80°C, maintain a large reflux, and continue stirring for 30 minutes;

[0032] b2. Weigh 136 g...

Embodiment 2

[0044] A kind of preparation method of sodium polysulfide, carries out successively according to following steps:

[0045] Step 1: preparing sodium polysulfide;

[0046] a1, take Na respectively 2 S·9H 2 O19.5 grams, sublimated sulfur 10.1 grams, solid sodium hydroxide 13.2 grams, water 123 grams, join in the reactor;

[0047] a2. Stir and heat, heat up to 85°C, dissolve the material, keep stirring for 3 hours;

[0048] a3, after the insulation reaction finishes, stop heating, cool down to room temperature, filter the reaction solution, filter out unreacted sulfur, detect the sodium polysulfide content 62g / L to the filtrate, and the polysulfide index is 2.7;

[0049] Step 2: refining p-aminobenzaldehyde;

[0050] b1. Weigh 25 grams of p-aminotoluene and 160 ml of ethanol into a three-neck flask, start stirring, heating, condensing, and raise the temperature to 80°C, maintain a large reflux, and continue stirring for 30 minutes;

[0051] b2. Weigh 160 grams of sodium polys...

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Abstract

The invention discloses a preparation method of sodium polysulfide and belongs to the technical field of chemical products. The preparation method comprises: 1, preparation of sodium polysulfide, 2, refining of p-aminobenzaldehyde, and 3, separation and recycling of a residual liquid to prepare sodium polysulfide. The preparation method utilizes the reaction of sodium sulfide, caustic soda and sulfur to prepare sodium polysulfide. The raw materials react to produce p-aminobenzaldehyde, and a water phase separated from the reaction product is used as a waste liquid mainly containing sodium sulfide, sodium polysulfide, sodium thiosulfate, sodium hydroxide, water, sodium hydrosulfide, unreacted sulfur, and the like. The waste liquid is subjected to suction filtration so that the unreacted sulfur is removed. The filtrate, sodium sulfide, caustic soda and sulfur undergo a reaction to produce sodium polysulfide. The method realizes recycling of the separated waste liquid and saves resources.

Description

technical field [0001] The invention belongs to the technical field of chemical products and relates to a preparation method of sodium polysulfide. Background technique [0002] Sodium polysulfide is a chemical substance, mainly used as a polymerization terminator, as a depilatory agent for raw hides in the tanning industry, and as an insecticide in agriculture. The traditional process is to prepare sodium polysulfide by reacting caustic soda and sulfur. The sodium polysulfide prepared by this process method is first prepared by feeding reaction to p-aminobenzaldehyde, and the water phase obtained by liquid separation after the reaction is used as waste liquid. The main components in the waste liquid are sodium thiosulfate, sodium sulfide, water, hydrogen peroxide Sodium etc. [0003] The waste liquid produced by the traditional process adopts the treatment method of purifying sodium thiosulfate as a by-product. Large amount, many impurities, low content of sodium thiosul...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C221/00C07C223/06C01B17/34
CPCC01B17/34C07C221/00C07C223/06
Inventor 王文娟胡修波徐桂苹万里海吕鑫寇瑞林陈志广李丹宋昕洋杨萍
Owner LIAONING HONGSHAN CHEM
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