CN100393610C - Preparation method of potassium borale peroxide and its application - Google Patents
Preparation method of potassium borale peroxide and its application Download PDFInfo
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- CN100393610C CN100393610C CNB2006100098787A CN200610009878A CN100393610C CN 100393610 C CN100393610 C CN 100393610C CN B2006100098787 A CNB2006100098787 A CN B2006100098787A CN 200610009878 A CN200610009878 A CN 200610009878A CN 100393610 C CN100393610 C CN 100393610C
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Abstract
The present invention relates to a preparation method of potassium borate peroxide and an application thereof, which has an appearance of white powders and freely flows and is stable under the normal temperature. An active oxygen content is from 18% to 22%. The present invention is prepared by boric acid, potassium hydroxide, catalysts, stabilizing agents, hydrogen peroxide, etc. is mainly used for flax ' strong bleaching 'for replacing the existing sodium chlorite, thereby, forms a new 'double oxygen bleaching 'process of flax bleaching, solves the problem of serious environment pollution brought by the traditional sodium chlorite bleaching and sodium hypochlorite bleaching, simultaneously solves the problem of micro chloric compounds contained in flax products, and has large social benefits and economic benefits. In addition, the product can be widely used for the bleaching of other bast fibers and cotton fibers, and can also be applied to the bleaching of other printing and dyeing industry and paper-making industry.
Description
The technical field is as follows:
the invention relates to a preparation method of potassium peroxyborate.
Background art:
china is a big country for producing linen products, the existing production capacity reaches seventy-ten thousand spindles, the annual output of linen yarns reaches 1400 ten thousand tons, and 40 billion yards of linen is at the top of the world. For many years, China still continues to use the technology of 'bleaching with oxygen, namely' bleaching with sodium chlorite and sodium hypochlorite ', and' bleaching with hydrogen peroxide 'lightly'. The process generates trace chlorine-containing compounds, greatly influences the product quality, and the discharged wastewater seriously pollutes the environment, wherein the pollutants are chlorine compounds and nitrates.
The invention content is as follows:
the invention aims to provide a preparation method of potassium peroxyborate with high activeoxygen content, stability at normal temperature and strong oxidation bleaching performance. The invention is realized by the following method: 1. a preparation method of potassium peroxyborate is characterized by comprising the following steps:
1) the reaction equation of the potassium peroxyborate is as follows:
2) raw material proportioning
Boric acid and borax: 20 to 28 portions of
Sulfuric acid or hydrochloric acid: 0.5 to 1.0 portion
Potassium hydroxide: 16 to 26 portions of
Hydrogen peroxide: 40.6 to 69.8 portions
Hydrogen peroxide stabilizer: 0.5 to 1.0 part of acetanilide
Catalyst: 0.2 to 0.5 portion of sulfate or nitrite
A stabilizer: 0.5 to 1.0 part of silicate, trisilicate or polysilicate
Deionized water: 10 to 30 portions of
3) Preparation method and process conditions
Firstly, adding 10-30 parts of deionized water into a reaction kettle, then adding 20-28 parts of boric acid and borax according to a ratio of 3: 1, adjusting the pH value to 1-5 by using 0.5-1.0 part of sulfuric acid or hydrochloric acid to dissolve the boric acid and borax, controlling the temperature to be 20-70 ℃, stirring for 20-60 minutes, then adding 0.2-0.5 part of sulfate or nitrite, and then adding silicate, trisilicate or polysilicate: 0.5-1.0 part of potassium hydroxide is stirred, 16-26 parts of potassium hydroxide is added to react for 1-2 hours, after the reaction is finished, 40.6-69.8 parts of hydrogen peroxide and 0.5-1.0 part of stabilizing agent are added to carry out redox reaction at the reaction temperature of 0-40 ℃ for 1-8 hours, and finally, the potassium peroxyborate is precipitated, filtered and dried to obtain the product.
4. The main technical indexes of the product prepared by the invention are as follows:
appearance: white powder, free flowing.
Active oxygen content (%): 18 to 22
pH value: 9.5 to 10.5
5. Advantages of the preparation method of the invention
In addition, before the oxidation-reduction reaction is carried out, a stabilizing agent N-acetanilide is added into the hydrogen peroxide, so that the stability of the hydrogen peroxide is further improved, the ineffective decomposition of the hydrogen peroxide in the reaction process is reduced, the generation rate of the potassium peroxide is improved, and the production cost of the potassium peroxide is reduced. The method reduces the amount of the added deionized water as much as possible and improves the yield of the potassium oxide borate.
The potassium peroxyborate prepared by the invention is a novel bleaching agent, and has no related products at home and abroad.
The specific implementation mode is as follows:
example 1:
firstly, adding 30-40 g of deionized water into a reaction kettle, then adding 40.6-51.2 g of a mixture of boric acid and borax according to a ratio of 3: 1, stirring, then adding 1.5-2.0 g of sulfuric acid, adjusting the pH value to 2-4, stirring for 20 minutes at the temperature of 40-60 ℃, adding 0.4-0.6 g of sodium nitrate, and stirring for 20-30 minutes. And then adding 55.5-62.2 g of potassium hydroxide for reaction, wherein the temperature is controlled to be 50-70 ℃, and the time is 1.5-2.0 hours. And after the reaction is finished, adding 75.5-90.2 g of hydrogen peroxide and 0.5g N-acetanilide to react for 2-3 hours at 30-40 ℃, and precipitating, filtering and drying reactants to obtain the product. The active oxygen content of the potassium peroxyborate prepared by the method reaches 19.2 percent.
Example 2:
adding 30-40 g of deionized water into a reaction kettle, then adding 40.6-51.2 g of a mixture of boric acid and borax according to a ratio of 3: 1, stirring, then adding 1.5-2.0 g of sulfuric acid, adjusting the pH value to 2-4, stirring for 20 minutes at the temperature of 40-60 ℃, adding 0.5-0.7 g of sodium sulfate, and stirring for 20-30 minutes. And then adding 55.5-65.2 g of potassium hydroxide for reaction, wherein the temperature is controlled to be 50-70 ℃, and the time is 1.5-2.0 hours. And after the reaction is finished, adding 75.5-90.2 g of hydrogen peroxide and 0.5g N-acetanilide to react for 4-6 hours at 30-40 ℃, and precipitating, filtering and drying reactants to obtain the product. The active oxygen content of the potassium peroxyborate prepared by the method reaches 19.5 percent.
Example 3:
adding 30-40 g of deionized water into a reaction kettle, then adding 40.6-51.2 g of a mixture of boric acid and borax according to a ratio of 3: 1, stirring, then adding 1.0-1.5 g of sulfuric acid, adjusting the pH value to 2-4, stirring for 20 minutes at the temperature of 40-50 ℃, adding 0.5-0.6 g of sodium sulfate, and stirring for 20-30 minutes. And then adding 52.0-60.2 g of potassium hydroxide for reaction, wherein the temperature is controlled to be 50-70 ℃, and the time is 1.5-2.0 hours. And after the reaction is finished, adding 75.5-90.2 g of hydrogen peroxide and 0.5g N-acetanilide to react for 2-3 hours at 30-40 ℃, and precipitating, filtering and drying reactants to obtain the product. The active oxygen content of the potassium peroxyborate prepared by the method reaches 18.5 percent.
Example 4:
adding 30-40 g of deionized water into a reaction kettle, then adding 40.6-51.2 g of a mixture of boric acid and borax according to a ratio of 3: 1, stirring, then adding 1.0-1.5 g of sulfuric acid, adjusting the pH value to 2-4, stirring for 20 minutes at the temperature of 40-50 ℃, adding 0.5-0.6 g of sodium sulfate, and stirring for 20-30 minutes. And then adding 52.0-60.2 g of potassium hydroxide for reaction, wherein the temperature is controlled to be 50-70 ℃, and the time is 1.5-2.0 hours. And after the reaction is finished, adding 75.5-90.2 g of hydrogen peroxide and 0.5g N-acetanilide to react for 4-5 hours at 30-40 ℃, and precipitating, filtering and drying reactants to obtain the product. The active oxygen content of the potassium peroxyborate prepared by the method reaches 18.9 percent.
Example 5:
adding 35-40 g of deionized water into a reaction kettle, then adding 40.6-51.2 g of potassium hydroxide, stirring for 20 minutes at the temperature of 20-40 ℃, adding 0.5-0.6 g of sodium sulfate, and stirring for 20-30 minutes. Then adding 45.2-52.6 boric acid to react, controlling the temperature at 50-70 ℃ and the time at 1.5-2.0 hours. And after the reaction is finished, adding 75.5-90.2 g of hydrogen peroxide and 0.5g N-acetanilide to react for 4-6 hours at 30-40 ℃, and precipitating, filtering and drying reactants to obtain the product. The active oxygen content of the potassium peroxyborate prepared by the method reaches 18.2 percent.
Example 6:
adding 38-40 g of deionized water into a reaction kettle, then adding 40.6-51.2 g of a mixture of boric acid and borax according to a ratio of 3: 1, stirring, then adding 1.0-1.5 g of sulfuric acid, adjusting the pH value to 3-4, stirring for 20 minutes at a temperature controlled between 40-50 ℃, adding 0.5-0.6 g of sodium sulfate, and stirring for 20-30 minutes. And then adding 52.0-60.2 g of potassium hydroxide for reaction, wherein the temperature is controlled to be 50-70 ℃, and the time is 1.5-2.0 hours. After the reaction is finished, 85.5-109.2 g of hydrogen peroxide and 0.5g N-acetanilide are added to react for 4-5 hours at the temperature of 30-40 ℃, and the product is obtained after the reactants are precipitated, filtered and dried. The active oxygen content of the potassium peroxyborate prepared by the method reaches 20.1 percent.
Example 7:
adding 38-40 g of deionized water into a reaction kettle, then adding 47.6-51.2 g of a mixture of boric acid and borax according to a ratio of 3: 1, stirring, then adding 1.0-1.5 g of sulfuric acid, adjusting the pH value to 3-4, stirring for 20 minutes at a temperature controlled between 40-50 ℃, adding 0.5-0.6 g of sodium nitrate, and stirring for 20-30 minutes. And then adding 52.0-60.2 g of potassium hydroxide for reaction, wherein the temperature is controlled to be 50-70 ℃, and the time is 1.5-2.0 hours. After the reaction is finished, 85.5-109.2 g of hydrogen peroxide and 0.5g N-acetanilide are added to react for 6-8 hours at the temperature of 30-40 ℃, and the product is obtained after the reactants are precipitated, filtered and dried. The active oxygen content of the potassium peroxyborate prepared by the method reaches 20.5 percent.
Example 8:
adding 38-40 g of deionized water into a reaction kettle, then adding 47.6-51.2 g of a mixture of boric acid and borax according to a ratio of 3: 1, stirring, adding 1.6-1.9 g of sulfuric acid, adjusting the pH value to 3-4, controlling the temperature to be 40-50 ℃, stirring for 20 minutes, adding 0.5-0.6 g of sodium nitrate, and stirring for 20-30 minutes. And then adding 52.0-60.2 g of potassium hydroxide for reaction, wherein the temperature is controlled to be 40-50 ℃ and the time is 1.5-2.0 hours. And after the reaction is finished, adding 98.5-117.2 g of hydrogen peroxide and 0.7g N-acetanilide to react for 2-4 hours at 10-20 ℃, and precipitating, filtering and drying reactants to obtain the product. The active oxygen content of the potassium peroxyborate prepared by the method reaches 21.2 percent.
Example 9:
adding 39-42 g of deionized water into a reaction kettle, then adding 45.0-50.0 g of boric acid, stirring, then adding 0.4-0.6 g of sulfuric acid, adjusting the pH value to 3-4, stirring for 20 minutes at the temperature of 20-30 ℃, adding 0.5-0.6 g of sodium sulfate, and stirring for 20-30 minutes. Then 43.0-46.2 g of potassium hydroxide is added for reaction, the temperature is controlled at 20-40 ℃, and the time is 0.5-1.0 hour. And after the reaction is finished, adding 85.5-95.2 g of hydrogen peroxide and 0.6g N-acetanilide to react for 2-4 hours at 20-30 ℃, and precipitating, filtering and drying reactants to obtain the product. The active oxygen content of the potassium peroxyborate prepared by the method reaches 20.6 percent.
Example 10:
adding 39-42 g of deionized water into a reaction kettle, then adding 45.0-50.0 g of boric acid, stirring, then adding 0.4-0.6 g of sulfuric acid, adjusting the pH value to 3-4, stirring for 20 minutes at the temperature of 20-30 ℃, adding 0.5-0.6 g of sodium sulfate, and stirring for 20-30 minutes. Then 43.0-46.2 g of potassium hydroxide is added for reaction, the temperature is controlled at 20-40 ℃, and the time is 0.5-1.0 hour. After the reaction is finished, adding 115.5-120.2 g of hydrogen peroxide and 0.6g N-acetanilide to react for 7-8 hours at 20-30 ℃, and precipitating, filtering and drying reactants to obtain the product. The active oxygen content of the potassium peroxyborate prepared by the method reaches 21.7 percent.
Claims (1)
1. A preparation method of potassium peroxyborate is characterized by comprising the following steps:
1) the reaction equation of the potassium peroxyborate is as follows:
2) raw material proportioning
Boric acid and borax: 20 to 28 portions of
Sulfuric acid or hydrochloric acid: 0.5 to 1.0 portion
Potassium hydroxide: 16 to 26 portions of
Hydrogen peroxide: 40.6 to 69.8 portions
Hydrogen peroxide stabilizer: 0.5 to 1.0 part of acetanilide
Catalyst: 0.2 to 0.5 portion of sulfate or nitrite
A stabilizer: 0.5 to 1.0 part of silicate, trisilicate or polysilicate
Deionized water: 10 to 30 portions of
3) Preparation method and process conditions
Firstly, adding 10-30 parts of deionized water into a reaction kettle, then adding 20-28 parts of boric acid and borax according to a ratio of 3: 1, adjusting the pH value to 1-5 by using 0.5-1.0 part of sulfuric acid or hydrochloric acid to dissolve the boric acid and borax, controlling the temperature to be 20-70 ℃, stirring for 20-60 minutes, then adding 0.2-0.5 part of sulfate or nitrite, and then adding silicate, trisilicate or polysilicate: 0.5-1.0 part of potassium hydroxide is stirred, 16-26 parts of potassium hydroxide is added to react for 1-2 hours, after the reaction is finished, 40.6-69.8 parts of hydrogen peroxide and 0.5-1.0 part of stabilizing agent are added to carry out redox reaction at the reaction temperature of 0-40 ℃ for 1-8 hours, and finally, the potassium peroxyborate is precipitated, filtered and dried to obtain the product.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2006100098787A CN100393610C (en) | 2006-03-31 | 2006-03-31 | Preparation method of potassium borale peroxide and its application |
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| CNB2006100098787A CN100393610C (en) | 2006-03-31 | 2006-03-31 | Preparation method of potassium borale peroxide and its application |
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| CN1830759A CN1830759A (en) | 2006-09-13 |
| CN100393610C true CN100393610C (en) | 2008-06-11 |
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| CNB2006100098787A Expired - Fee Related CN100393610C (en) | 2006-03-31 | 2006-03-31 | Preparation method of potassium borale peroxide and its application |
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| CN117778014B (en) * | 2023-12-22 | 2024-08-16 | 哈尔滨工业大学 | Application of active oxygen carrying oxidant in removing organic pollutants in soil |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB913688A (en) * | 1958-04-28 | 1962-12-28 | Solvay | Sodium perborate |
| GB940262A (en) * | 1959-01-13 | 1963-10-30 | Laporte Chemical | Improvements in or relating to the preparation of sodium perborate trihydrate |
| US4211759A (en) * | 1971-01-13 | 1980-07-08 | Produits Chimiques Ugine Kuhlmann | High-density sodium perborate and method of preparation |
| GB2188914A (en) * | 1986-04-08 | 1987-10-14 | May Helan Vivien | Production of sodium perborate |
| CN1056324A (en) * | 1990-05-08 | 1991-11-20 | 徐钢 | One-step technology for decolouring, boiling and bleaching with sodium hydrosulfide |
| CN1369430A (en) * | 2002-03-18 | 2002-09-18 | 陶华西 | Method for preparing sodium perborate monohydrate |
-
2006
- 2006-03-31 CN CNB2006100098787A patent/CN100393610C/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB913688A (en) * | 1958-04-28 | 1962-12-28 | Solvay | Sodium perborate |
| GB940262A (en) * | 1959-01-13 | 1963-10-30 | Laporte Chemical | Improvements in or relating to the preparation of sodium perborate trihydrate |
| US4211759A (en) * | 1971-01-13 | 1980-07-08 | Produits Chimiques Ugine Kuhlmann | High-density sodium perborate and method of preparation |
| GB2188914A (en) * | 1986-04-08 | 1987-10-14 | May Helan Vivien | Production of sodium perborate |
| CN1056324A (en) * | 1990-05-08 | 1991-11-20 | 徐钢 | One-step technology for decolouring, boiling and bleaching with sodium hydrosulfide |
| CN1369430A (en) * | 2002-03-18 | 2002-09-18 | 陶华西 | Method for preparing sodium perborate monohydrate |
Non-Patent Citations (4)
| Title |
|---|
| 硼砂法合成过硼酸钠方法的改进. 杨传世，刘春兰.中国化工，第12期. 1997 |
| 硼砂法合成过硼酸钠方法的改进. 杨传世，刘春兰.中国化工，第12期. 1997 * |
| 过硼酸钠在纸浆漂白中的应用. 劳嘉葆.造纸化学品，第3期. 1996 |
| 过硼酸钠在纸浆漂白中的应用. 劳嘉葆.造纸化学品，第3期. 1996 * |
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