CN104817480B - Reuse of Bunte salt in sodium hydrosulfite waste residue - Google Patents
Reuse of Bunte salt in sodium hydrosulfite waste residue Download PDFInfo
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- CN104817480B CN104817480B CN201510110479.9A CN201510110479A CN104817480B CN 104817480 B CN104817480 B CN 104817480B CN 201510110479 A CN201510110479 A CN 201510110479A CN 104817480 B CN104817480 B CN 104817480B
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- bunte salts
- waste residue
- acidolysis
- sodium hydrosulfite
- acid
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Abstract
The invention discloses a reuse method for Bunte salt in sodium hydrosulfite waste residue. The main processes include (1) acidolysis of Bunte salt, (2) oxidation of acidolysis product, (3) alkali neutralization, and (4) product precipitation. The method provided by the invention converts the waste Bunte salt in sodium hydrosulfite waste residue into high value-added sodium hydroxyethyl sulfonate, and turns waste into treasure, and the purity of the product can reach 95%. With the characteristics of mild reaction conditions and simple operation process, the method solves enterprise environmental pollution, and at the same time brings economic benefits and social benefits to enterprises.
Description
Technical field
The present invention relates to a kind of method that the conversion of bunte salts is recycled in sodium hydrosulfite waste residue, turns bunte salts through conversion
The sodium isethionate with higher economic worth is turned to, belongs to refuse reclamation property.
Background technology
At present, the method for domestic production sodium hydrosulfite mainly has two kinds, sodium formate method and zinc powder method.Because sodium formate method has
The advantages of low production cost, steady quality, sodium formate method production insurance powder yield occupies the 4/5 of Nationwide Insurance Enterprise's powder total output.Should
Contain substantial amounts of debirs in waste liquid after method production sodium hydrosulfite, serious pollution is produced to environment.The country is to insurance
Powder waste residue is used without unified standard, while the processing cost of costliness causes enterprise to hang back.
Sodium formate therein is simply carried out conversion recovery by patent CN1164527A, for other materials then can only be carried out
Emission treatment.Patent CN102050471A reclaims sodium formate and Asia using steps such as ultrafiltration, nanofiltration, condensing crystallizing, centrifugal filtrations
Sodium sulfate, equipment investment is expensive, but the Organic substance of high added value then can not be recycled.Patent CN101214930A is public
The method using sodium hydrosulfite residual liquid lignin co-production sodium sulfonate is opened, the method does not also turn high value added product in waste residue
Change and utilize.Containing sodium isethionate and bunte salts in sodium hydrosulfite waste residue, sodium isethionate can serve as in surfactant
Mesosome, daily use chemicals and medicine intermediate, with higher economic worth.
The content of the invention
It is contemplated that a kind of method that bunte salts changes into sodium isethionate is disclosed, it is according to this step conversion that nation is special
Salt changes into the sodium isethionate with higher economic worth, and main technological steps are as follows：
Mainly comprise the following steps（1）The acidolysis of bunte salts；（2）The oxidation of acid hydrolysate；（3）The neutralization of alkali；（4）The analysis of product
Go out.Finally product is carried out into sucking filtration, be dried, weighed.
Step（1）The acid that the acidolysis of middle bunte salts is used is hydrochloric acid, sulphuric acid, nitric acid, phosphoric acid, and the usage amount of acid is that nation is special
0.03-0.06 times of salt quality, the temperature of acidolysis is 70-90 DEG C, and the acidolysis time is 1.5-3h.
Step（2）The oxidant that the oxidation of middle acid hydrolysate is used is hydrogen peroxide, and the usage amount of hydrogen peroxide is bunte salts
0.5-0.8 times of quality, the temperature of oxidation is 10-30 DEG C, and oxidization time is 1.5-3h.
Step（3）The alkali that the neutralization of middle alkali is used is sodium hydroxide, potassium hydroxide, and the usage amount of alkali is bunte salts quality
0.3-0.4 times.
Step（4）The organic solvent that the precipitation of middle product is used is methanol, ethanol, and the usage amount of alcohol is bunte salts quality
1-3 times.
Specific embodiment
Embodiment 1
（1）Weigh bunte salts 100g to be placed in round-bottomed flask, add 100g water to be dissolved, matter is taken in the state of stirring
The hydrochloric acid solution 30mL of amount fraction 10% is instilled in flask, controls 85-90 DEG C of acidolysis temperature, response time 3h；
（2）Solution of the acidolysis after complete is cooled down, temperature control is made at 10-15 DEG C, slow Deca 80g dioxygen
Water, controls the response time for 3h after dripping；
（3）Sodium hydroxide is added after having reacted is neutralized in reaction bulb, the quality for adding sodium hydroxide is 30g；
（4）Ethanol 100mL is slowly added to in the solution after neutralization, white flock precipitate can be slowly washed out in solution,
This is precipitated as sodium isethionate.Precipitation is carried out into sucking filtration, washing, the heavy m=64g of drying, yield is 78%, product purity 98%.
Embodiment 2
（1）Weigh bunte salts 100g to be placed in round-bottomed flask, add 100g water to be dissolved, matter is taken in the state of stirring
The sulfuric acid solution 20mL of amount fraction 30% is instilled in flask, controls 85-90 DEG C of acidolysis temperature, response time 3h；
（2）Solution of the acidolysis after complete is cooled down, temperature control is made at 10-15 DEG C, slow Deca 60g dioxygen
Water, controls the response time for 2.5h after dripping；
（3）Sodium hydroxide is added after having reacted is neutralized in reaction bulb, the quality for adding sodium hydroxide is 30g；
（4）Ethanol 100mL is slowly added to in the solution after neutralization, white flock precipitate can be slowly washed out in solution,
This is precipitated as sodium isethionate.Precipitation is carried out into sucking filtration, washing, the heavy m=69g of drying, yield is 84%, product purity 97%.
Embodiment 3
（1）Weigh bunte salts 100g to be placed in round-bottomed flask, add 100g water to be dissolved, matter is taken in the state of stirring
The salpeter solution 20mL of amount fraction 20% is instilled in flask, controls 70-75 DEG C of acidolysis temperature, response time 1.5h；
（2）Solution of the acidolysis after complete is cooled down, temperature control is made at 10-15 DEG C, slow Deca 50g dioxygen
Water, controls the response time for 1.5h after dripping；
（3）Potassium hydroxide is added after having reacted is neutralized in reaction bulb, the quality for adding potassium hydroxide is 40g；
（4）Ethanol 200mL is slowly added to in the solution after neutralization, white flock precipitate can be slowly washed out in solution,
This is precipitated as sodium isethionate.Precipitation is carried out into sucking filtration, washing, the heavy m=72g of drying, yield is 87%, product purity 97%.
Embodiment 4
（1）Weigh bunte salts 100g to be placed in round-bottomed flask, add 100g water to be dissolved, matter is taken in the state of stirring
The hydrochloric acid solution 15mL of amount fraction 30% is instilled in flask, controls 80-85 DEG C of acidolysis temperature, response time 2h；
（2）Solution of the acidolysis after complete is cooled down, temperature control is made at 25-30 DEG C, slow Deca 70g dioxygen
Water, controls the response time for 3h after dripping；
（3）Potassium hydroxide is added after having reacted is neutralized in reaction bulb, the quality for adding potassium hydroxide is 40g；
（4）Ethanol 300mL is slowly added to in the solution after neutralization, white flock precipitate can be slowly washed out in solution,
This is precipitated as sodium isethionate.Precipitation is carried out into sucking filtration, washing, the heavy m=74g of drying, yield is 90%, product purity 95%.
Claims (5)
1. in a kind of sodium hydrosulfite waste residue bunte salts recycling, it is characterized in that, comprise the following steps：
（1）The acidolysis of bunte salts, described bunte salts is hydroxyethylthio sodium sulfate, described acid be hydrochloric acid, sulphuric acid, nitric acid,
Phosphoric acid；
（2）The oxidation of acid hydrolysate, described oxidant is hydrogen peroxide；
（3）The neutralization of alkali, described alkali is sodium hydroxide, potassium hydroxide；
（4）The precipitation of product, described organic solvent is methanol, ethanol.
2. in a kind of sodium hydrosulfite waste residue according to claim 1 bunte salts recycling, it is characterized in that, step（1）Middle nation
The acidolysis of special salt, the usage amount of acid is 0.03-0.06 times of bunte salts quality, and the temperature of acidolysis is 70-90 DEG C, and the acidolysis time is
1.5-3h。
3. in a kind of sodium hydrosulfite waste residue according to claim 1 bunte salts recycling, it is characterized in that, step（2）Middle acid
The oxidation of solution product, the usage amount of hydrogen peroxide is 0.5-0.8 times of bunte salts quality, and the temperature of oxidation is 10-30 DEG C, during oxidation
Between be 1.5-3h.
4. in a kind of sodium hydrosulfite waste residue according to claim 1 bunte salts recycling, it is characterized in that, step（3）Middle alkali
Neutralization, the usage amount of alkali is 0.3-0.4 times of bunte salts quality.
5. in a kind of sodium hydrosulfite waste residue according to claim 1 bunte salts recycling, it is characterized in that, step（4）Middle product
The precipitation of product, the usage amount of alcohol is 1-3 times of bunte salts quality.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510110479.9A CN104817480B (en) | 2015-03-13 | 2015-03-13 | Reuse of Bunte salt in sodium hydrosulfite waste residue |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510110479.9A CN104817480B (en) | 2015-03-13 | 2015-03-13 | Reuse of Bunte salt in sodium hydrosulfite waste residue |
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| Publication Number | Publication Date |
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| CN104817480A CN104817480A (en) | 2015-08-05 |
| CN104817480B true CN104817480B (en) | 2017-04-19 |
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| CN201510110479.9A Expired - Fee Related CN104817480B (en) | 2015-03-13 | 2015-03-13 | Reuse of Bunte salt in sodium hydrosulfite waste residue |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105537232B (en) * | 2015-12-03 | 2018-01-23 | 浙江嘉成化工有限公司 | A kind of processing method of sodium hydrosulfite production residue |
| CN108569989B (en) * | 2018-05-25 | 2020-06-02 | 中南大学 | Method for preparing thiourethane and co-producing 2-mercaptoethanol or O-alkylthio ethyl xanthate |
| CN111518001B (en) * | 2020-04-28 | 2021-02-23 | 烟台市金河保险粉厂有限公司 | Method for preparing 2-mercaptoethanol from sodium hydrosulfite production waste liquid |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CS163273B2 (en) * | 1971-03-29 | 1975-08-29 | ||
| CN102050471B (en) * | 2010-11-05 | 2012-05-23 | 烟台大学 | Method for recycling sodium formate and sodium sulfite from waste sodium hydrosulfite liquid with sodium formate method |
| CN103694101B (en) * | 2013-11-07 | 2015-08-19 | 济南大学 | A kind of method of comprehensive utilization of sodium hydrosulfite waste residue |
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