CN101559929A - Stable preparation method of sodium peroxydisulfate - Google Patents
Stable preparation method of sodium peroxydisulfate Download PDFInfo
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- CN101559929A CN101559929A CNA2008100179815A CN200810017981A CN101559929A CN 101559929 A CN101559929 A CN 101559929A CN A2008100179815 A CNA2008100179815 A CN A2008100179815A CN 200810017981 A CN200810017981 A CN 200810017981A CN 101559929 A CN101559929 A CN 101559929A
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- sodium
- peroxide
- crystallisate
- peroxydisulfate
- hydrogen peroxide
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Abstract
The invention relates to a stable preparation method of sodium peroxydisulfate by sodium sulfate, sodium chloride, an aqueous solution of hydogen peroxide and a certain crystallizing agent. The method comprises the following steps: 1, adding the well-prepared crystallizing agent to the aqueous solution of hydogen peroxide and then adding anhydrous sodium sulfate; 2, adding the sodium chloride to reaction liquid in the first step, controlling the reaction temperature and reacting to prepare a solid peroxide crystal; and 3, separating the solid peroxide crystal to obtain a filtrate as mother liquor, and drying the crystal to obtain a product. The prepared sodium peroxydisulfate has a hydogen peroxide decomposition rate within 2 percent, and the product has higher content of hydogen peroxide and extremely good stability.
Description
Technical field
The invention belongs to solid oxygen-bearing bleaching agent technical field, relate to a kind of stable preparation method of sodium peroxydisulfate.
Background technology
Sodium peroxydisulfate is the adducts of sodium sulfate, hydrogen peroxide and sodium-chlor, and outward appearance is white crystal particle or powder.Its molecular formula is 4Na
2SO
42H
2O
2NaCl, soluble in water, in water, be dissociated into salt and hydrogen peroxide.Have bleaching, sterilization and help the function of washing, the product degradation production is environmentally friendly.Therefore, can be used as SYNTHETIC OPTICAL WHITNER and fish oxygenation agent use in the washing composition.
German patent DE 2530539 has been announced the common preparation method of this adducts: adopt to react in anhydrous sodium sulphate and the sodium-chlor input aqueous hydrogen peroxide solution to make, reaction conditions comprises the concentration of three kinds of proportion of raw materials, hydrogen peroxide, the selected and reaction times of temperature of reaction.The crystallization from building-up reactions solution of this solid peroxide produces, and goes out crystallisate by filtration or centrifugation, obtains finished product after the final drying.But the finished product stability that makes under this condition is poor, can not long storage.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of stable sodium peroxydisulfate is to solve problems of the prior art.
The technical solution adopted in the present invention is:
The first step behind the crystallization auxiliary that adding prepares in aqueous hydrogen peroxide solution, adds anhydrous sodium sulphate again;
Second step added sodium-chlor in the first step reaction solution, control reaction temperature, and reaction makes the solid peroxide crystallisate;
The 3rd step, separate solid superoxide crystallisate, filtrate is mother liquor, and the crystallisate drying is handled and is obtained product;
The mass ratio of anhydrous sodium sulphate and hydrogen peroxide is: 1: 0.27～1.2;
The add-on of anhydrous sodium sulphate is 25～80% of a mother liquor quality;
5～15 ℃ of crystallization reaction temperature, 30～180 minutes reaction times.
Described crystallisate adopts and filters or centrifugation, and crystallisate is dry down after screening is finished product 60～120 ℃ of temperature.
The sodium-chlor input amount is that to keep its concentration in mother liquor be 3～20%.
Described crystallization auxiliary is a sodium polyphosphate, polypropylene acid sodium, one or more several mixtures of hydroxy ethylene diphosphonic acid, Amino Trimethylene Phosphonic Acid, ethylenediamine tetramethylene phosphonic acid organic phosphoric acid or its sodium salt, Polyscrylamide, input amount is 0.1～3% of an anhydrous sodium sulphate consumption.
The testing method of stability: a little product is positioned in the unlimited culture dish, in 100 ℃ constant temperature oven, placed 3 hours, calculate the rate of decomposition of the content of hydrogen peroxide of sample.
Below be the contrast test result of the sodium peroxydisulfate of the sodium peroxydisulfate for preparing of the present invention and general technology preparation:
| Project | Content of hydrogen peroxide (%) | Rate of decomposition (%) | Remarks |
| Experiment 1 | 9.2 | 1.83 | |
| Experiment 2 | 9.1 | 1.74 | |
| Experiment 3 | 9.36 | 1.5 | |
| Experiment 4 | 9.47 | 1.7 | |
| The contrast experiment 1 | 9.01 | 9.21 | |
| The contrast experiment 2 | 9.29 | 8.64 |
Draw from above-mentioned test result comparative analysis, all in 2%, the content of hydrogen peroxide of product is higher and stable very good for the hydrogen peroxide decomposition rate of the sodium peroxydisulfate of the present invention preparation, can long-term storage and can not influence functional quality.
Embodiment
Embodiment 1:
Get 455 milliliters of content and be 27.5% hydrogen peroxide, add crystallization auxiliary 2 grams that prepare, stir cooling, when treating that temperature is reduced to 10 ℃, drop into 132 gram anhydrous sodium sulphate and 125 gram sodium-chlor, maintain the temperature at 10 ℃ of reaction dischargings after 60 minutes, use the B suction filtration, wet product 50 ℃ of oven dry in constant temperature oven get product 140 grams.
Embodiment 2:
Get 435 milliliters in the mother liquor of embodiment 1, adding 25ml content is 50% hydrogen peroxide, add crystallization auxiliary 2 grams that prepare, stir cooling, when treating that temperature is reduced to 10 ℃, drop into 132 gram anhydrous sodium sulphate and 13 gram sodium-chlor, keep 10 ℃ of reaction dischargings after 120 minutes of temperature, use the B suction filtration, wet product 50 ℃ of oven dry in constant temperature oven get product 155 grams.
Embodiment 3:
Get 300 milliliters of content and be 27.5% hydrogen peroxide, add crystallization auxiliary 3 grams that prepare, stir cooling, when treating that temperature is reduced to 10 ℃, drop into 240 gram anhydrous sodium sulphate and 40 gram sodium-chlor, keep 10 ℃ of reaction dischargings after 120 minutes of temperature, use the B suction filtration, wet product 50 ℃ of oven dry in constant temperature oven get product 215 grams.
Embodiment 4:
Get 220 milliliters in the mother liquor of embodiment 3, adding 45ml content is 50% hydrogen peroxide, add crystallization auxiliary 3 grams that prepare, stir cooling, when treating that temperature is reduced to 10 ℃, drop into 240 gram anhydrous sodium sulphate and 23 gram sodium-chlor, keep 10 ℃ of reaction dischargings after 80 minutes of temperature, use the B suction filtration, wet product 50 ℃ of oven dry in constant temperature oven get product 290 grams.
The contrast experiment 1:
Testing program is identical with embodiment 1, but does not add the crystallization auxiliary for preparing.
The contrast experiment 2:
Testing program is identical with embodiment 3, but does not add the crystallization auxiliary for preparing.
Claims (4)
1, a kind of stable preparation method of sodium peroxydisulfate makes stable peroxide sodium sulfate by sodium sulfate, sodium-chlor and aqueous hydrogen peroxide solution and certain crystallization auxiliary, it is characterized in that following these steps to carrying out:
1.1 after in aqueous hydrogen peroxide solution, adding the crystallization auxiliary for preparing, add anhydrous sodium sulphate again;
1.2 in the first step reaction solution, add sodium-chlor, control reaction temperature, reaction makes the solid peroxide crystallisate;
1,3 separate solid superoxide crystallisate, filtrate is mother liquor, and the xln drying is handled and is obtained product.
2, a kind of stable preparation method of sodium peroxydisulfate as claimed in claim 1 is characterized in that the mass ratio of anhydrous sodium sulphate and hydrogen peroxide is: 1: 0.27～1.2; The add-on of anhydrous sodium sulphate is 25～80% of a mother liquor quality; The sodium-chlor input amount is 3～20% for keeping its concentration in mother liquor.
3, a kind of stable preparation method of sodium peroxydisulfate as claimed in claim 1 is characterized in that described crystallisate adopts filtration or centrifugation, and crystallisate is dry down after screening is finished product 60～120 ℃ of temperature.
4, a kind of stable preparation method of sodium peroxydisulfate as claimed in claim 1, it is characterized in that described crystallization auxiliary is a sodium polyphosphate, polypropylene acid sodium, one or more several mixtures of hydroxy ethylene diphosphonic acid, Amino Trimethylene Phosphonic Acid, ethylenediamine tetramethylene phosphonic acid organic phosphoric acid or its sodium salt and Polyscrylamide, input amount are 0.1～3% of anhydrous sodium sulphate consumption.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100179815A CN101559929A (en) | 2008-04-16 | 2008-04-16 | Stable preparation method of sodium peroxydisulfate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100179815A CN101559929A (en) | 2008-04-16 | 2008-04-16 | Stable preparation method of sodium peroxydisulfate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101559929A true CN101559929A (en) | 2009-10-21 |
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| CNA2008100179815A Pending CN101559929A (en) | 2008-04-16 | 2008-04-16 | Stable preparation method of sodium peroxydisulfate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107128880A (en) * | 2017-05-31 | 2017-09-05 | 山西宝清化工有限公司 | Sodium peroxydisulfate and its preparation method and application |
| CN108083298A (en) * | 2018-01-15 | 2018-05-29 | 东南大学 | It is a kind of to prepare the nanocrystalline method of potassium sulfate |
-
2008
- 2008-04-16 CN CNA2008100179815A patent/CN101559929A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107128880A (en) * | 2017-05-31 | 2017-09-05 | 山西宝清化工有限公司 | Sodium peroxydisulfate and its preparation method and application |
| CN108083298A (en) * | 2018-01-15 | 2018-05-29 | 东南大学 | It is a kind of to prepare the nanocrystalline method of potassium sulfate |
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Open date: 20091021 |