CN101033202A - Organic acid stabilizer and preparation of its percarbonateamide - Google Patents
Organic acid stabilizer and preparation of its percarbonateamide Download PDFInfo
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- CN101033202A CN101033202A CN 200710010259 CN200710010259A CN101033202A CN 101033202 A CN101033202 A CN 101033202A CN 200710010259 CN200710010259 CN 200710010259 CN 200710010259 A CN200710010259 A CN 200710010259A CN 101033202 A CN101033202 A CN 101033202A
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- urea
- hydrogen peroxide
- percarbamide
- aqueous solution
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- 238000002360 preparation method Methods 0.000 title claims 2
- 239000003381 stabilizer Substances 0.000 title description 16
- 150000007524 organic acids Chemical class 0.000 title 1
- 239000011248 coating agent Substances 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims abstract description 5
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims description 7
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 2
- 229940095064 tartrate Drugs 0.000 claims 2
- 229910021529 ammonia Inorganic materials 0.000 claims 1
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 abstract description 22
- AQLJVWUFPCUVLO-UHFFFAOYSA-N urea hydrogen peroxide Chemical compound OO.NC(N)=O AQLJVWUFPCUVLO-UHFFFAOYSA-N 0.000 abstract description 13
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 abstract description 12
- 239000004202 carbamide Substances 0.000 abstract description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 9
- 239000001301 oxygen Substances 0.000 abstract description 9
- 229910052760 oxygen Inorganic materials 0.000 abstract description 9
- 238000006243 chemical reaction Methods 0.000 abstract description 6
- 239000007864 aqueous solution Substances 0.000 abstract description 4
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 239000000843 powder Substances 0.000 abstract description 4
- 238000004659 sterilization and disinfection Methods 0.000 abstract description 4
- 238000003786 synthesis reaction Methods 0.000 abstract description 4
- 239000013078 crystal Substances 0.000 abstract description 3
- 238000002474 experimental method Methods 0.000 abstract description 3
- 239000012847 fine chemical Substances 0.000 abstract description 3
- 238000004061 bleaching Methods 0.000 abstract description 2
- 230000001954 sterilising effect Effects 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 2
- 239000006076 specific stabilizer Substances 0.000 abstract 1
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 4
- 239000011975 tartaric acid Substances 0.000 description 4
- 235000002906 tartaric acid Nutrition 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- 239000005711 Benzoic acid Substances 0.000 description 3
- 235000010233 benzoic acid Nutrition 0.000 description 3
- VTIIJXUACCWYHX-UHFFFAOYSA-L disodium;carboxylatooxy carbonate Chemical compound [Na+].[Na+].[O-]C(=O)OOC([O-])=O VTIIJXUACCWYHX-UHFFFAOYSA-L 0.000 description 3
- 229940045872 sodium percarbonate Drugs 0.000 description 3
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 description 1
- -1 Dipotassium Hydrogen Phosphate Tartrate Benzoate Chemical compound 0.000 description 1
- 235000011054 acetic acid Nutrition 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- NGPZJQXXJCDBDS-UHFFFAOYSA-N dodecane-1-sulfonic acid;sodium Chemical compound [Na].CCCCCCCCCCCCS(O)(=O)=O NGPZJQXXJCDBDS-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000005457 ice water Substances 0.000 description 1
- 239000001630 malic acid Substances 0.000 description 1
- 235000011090 malic acid Nutrition 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- MZSDGDXXBZSFTG-UHFFFAOYSA-M sodium;benzenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C1=CC=CC=C1 MZSDGDXXBZSFTG-UHFFFAOYSA-M 0.000 description 1
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- Detergent Compositions (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
过碳酰胺是一种精细化工新产品，它是过氧化氢和尿素的晶体加合物，外观为白色结晶粉末，理论活性氧含量为17.02％，易溶于水，水溶液兼具过氧化氢和尿素水溶液的性质，稳定性好，释放氧缓慢，效用时间长，具有广泛的用途(如漂白，杀菌，消毒等)，而且有广泛的应用前景。本文主要介绍了用27.5％的过氧化氢和尿素，再加入特定的稳定剂，包膜剂，采用条件实验考察了过碳酰胺的合成，获得最佳工艺反应条件。Percarbamide is a new fine chemical product. It is a crystal adduct of hydrogen peroxide and urea. It is a white crystalline powder with a theoretical active oxygen content of 17.02%. It is easily soluble in water. The aqueous solution contains both hydrogen peroxide and The properties of urea aqueous solution, good stability, slow release of oxygen, long effective time, has a wide range of uses (such as bleaching, sterilization, disinfection, etc.), and has a wide range of application prospects. This article mainly introduces the use of 27.5% hydrogen peroxide and urea, and then adds a specific stabilizer and coating agent, and uses conditional experiments to investigate the synthesis of percarbamide, and obtains the best process reaction conditions.
Description
技术领域technical field
本项发明涉及过碳酰胺的合成方法及其新型稳定剂的筛选。该合成法路线简洁、操作简单、产率高，无污染，废液可循环使用。This invention relates to the synthesis method of percarbamide and the screening of novel stabilizer. The synthesis method has simple route, simple operation, high yield, no pollution, and the waste liquid can be recycled.
背景技术Background technique
过碳酰胺是一种精细化工新产品，它是过氧化氢和尿素的晶体加合物，外观为白色结晶粉末，理论活性氧含量为17.02％，易溶于水，水溶液兼具过氧化氢和尿素水溶液的性质，稳定性好，释放氧缓慢，效用时间长，具有广泛的用途(如漂白，杀菌，消毒等)，而且有广泛的应用前景。但这种重要精细化工产品在工业上还处于空白，急待开发和应用。目前，过碳酸钠成套装置生产能力达到20kt/a，世界总需求量为700kt/a，生产能力远远满足不了市场需求，单就洗衣粉的添加剂(10％-20％)，每年需求50-100kt，而过碳酸纳每年产量不足万吨。过碳酰胺为新产品，由于其在性能上的优势，在价格上肯定比过碳酸钠高。因此，过碳酰胺会成为一种更新换代的产品已是必然，但现在过碳酰胺的生产国只有美国，日本等。近年来国外的开发和应用以获得很大进展，国内虽有很多过氧化氢和尿素的生产厂家，但是稳定剂的好坏直接影响产品的稳定性。Percarbamide is a new fine chemical product. It is a crystal adduct of hydrogen peroxide and urea. It is a white crystalline powder with a theoretical active oxygen content of 17.02%. It is easily soluble in water. The aqueous solution contains both hydrogen peroxide and The properties of urea aqueous solution, good stability, slow release of oxygen, long effective time, has a wide range of uses (such as bleaching, sterilization, disinfection, etc.), and has a wide range of application prospects. However, this important fine chemical product is still in a blank in the industry and needs to be developed and applied urgently. At present, the production capacity of sodium percarbonate complete set has reached 20kt/a, and the world's total demand is 700kt/a. The production capacity is far from meeting the market demand. The additive (10%-20%) of washing powder alone requires 50- 100kt, while the annual output of sodium percarbonate is less than 10,000 tons. Percarbamide is a new product, and due to its performance advantages, its price must be higher than that of sodium percarbonate. Therefore, it is inevitable that percarbamide will become a replacement product, but now the only producers of percarbamide are the United States and Japan. In recent years, the development and application abroad have made great progress. Although there are many manufacturers of hydrogen peroxide and urea in China, the quality of the stabilizer directly affects the stability of the product.
发明内容Contents of the invention
合成工艺流程是由原料尿素和过氧化氢在稳定剂和包膜剂存在的条件下，经合成，包膜结晶，过滤，烘干制成成品，过滤后的母液保存下来，用于下次合成(如下图所示)。重要是稳定剂的筛选。The synthesis process is made of raw materials urea and hydrogen peroxide in the presence of stabilizers and coating agents, which are synthesized, coated and crystallized, filtered, and dried to make finished products. The filtered mother liquor is preserved for the next synthesis (As shown below). Important is the screening of stabilizers.
过碳酰胺易分解。在制取过碳酰胺时，由于尿素或过氧化氢中会存在少许金属离子.应加入稳定剂以除去金属离子，稳定剂的加入量为尿素的加入量的0.5～1.0％为最佳，但越少越好。在用稳定剂的量相同时，反应温35℃，反应时间30min，投料比为0.70∶1情况下，几种不同稳定剂对过碳酰胺产率的影响如下表1：Percarbamide is easy to decompose. When preparing percarbamide, due to the presence of a little metal ions in urea or hydrogen peroxide, a stabilizer should be added to remove metal ions. The less the better. When using the same amount of stabilizer, 35°C of reaction temperature, 30min in the reaction time, and a feed ratio of 0.70: 1, several different stabilizers have the following table 1 on the impact of percarbamide yield:
表1.稳定剂对反应的影响
由表1可以发现，用过氧化氢与尿素合成过碳酰胺，在酸性条件下该加合效应能较顺利进行，且产品稳定性较好，产品产率也较高。比较稳定剂苯甲酸，酒石酸，磷酸氢二钾发现，最佳稳定剂为酒石酸。As can be found from Table 1, the synthesis of percarbamide with hydrogen peroxide and urea can be carried out more smoothly under acidic conditions, and the product stability is better, and the product yield is also higher. Comparing the stabilizers benzoic acid, tartaric acid, and dipotassium hydrogen phosphate found that the best stabilizer was tartaric acid.
稳定剂包括：苯甲酸，酒石酸，乙酸，丙酮，苹果酸，柠檬酸，磷酸氢二钾，氯化钾等。Stabilizers include: benzoic acid, tartaric acid, acetic acid, acetone, malic acid, citric acid, dipotassium hydrogen phosphate, potassium chloride, etc.
包膜剂：十二烷基磺酸钠，苯基磺酸钠等。Coating agent: sodium dodecylsulfonate, sodium phenylsulfonate, etc.
本发明表明，在适当的稳定剂中，用尿素与过氧化氢混合可以得到稳定的过碳酰胺。最高产率高于70％，活性氧含量高于16.3％。The present invention shows that stable percarbamides can be obtained by mixing urea with hydrogen peroxide in a suitable stabilizer. The highest yield is higher than 70%, and the active oxygen content is higher than 16.3%.
具体实施方式Detailed ways
实例1Example 1
500ml容器中，加入过氧化氢和相应量的尿素，控制在一定反应温度，待尿素完全溶解后，加入少量稳定剂苯甲酸，待反应将结束时，加入少包膜剂十二烷基磺酸钠，共搅拌35分钟则反映结束，将所得溶液用冰水混合物冷却3-4小时，得白色糊状液体，抽滤，得白色粉末状结晶，并在30℃的烘干器中烘干，即得到产品。产率为77.36％；活性氧含量16.47％。In a 500ml container, add hydrogen peroxide and a corresponding amount of urea, and control the reaction temperature at a certain temperature. After the urea is completely dissolved, add a small amount of stabilizer benzoic acid. When the reaction is about to end, add the less coating agent dodecylsulfonic acid Sodium, stirring for 35 minutes to complete the reaction, cooling the resulting solution with ice-water mixture for 3-4 hours to obtain a white paste liquid, suction filtration to obtain white powder crystals, and drying in a dryer at 30 ° C. That is, the product is obtained. The yield is 77.36%; the active oxygen content is 16.47%.
实例2Example 2
按照实例1的实验方法。稳定剂换成酒石酸。得到产品与实例1一样。产率为75.36％；活性氧含量16.20％。According to the experimental method of example 1. The stabilizer was replaced by tartaric acid. Obtaining product is the same as example 1. The yield is 75.36%; the active oxygen content is 16.20%.
实例3Example 3
按照实例1的实验方法。稳定剂换成柠檬酸。得到产品与实例1一样。产率为76.36％；活性氧含量16.40％。According to the experimental method of example 1. The stabilizer was replaced with citric acid. Obtaining product is the same as example 1. The yield is 76.36%; the active oxygen content is 16.40%.
Claims (4)
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200710010259 CN101033202A (en) | 2007-01-31 | 2007-01-31 | Organic acid stabilizer and preparation of its percarbonateamide |
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| CN 200710010259 CN101033202A (en) | 2007-01-31 | 2007-01-31 | Organic acid stabilizer and preparation of its percarbonateamide |
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| CN101033202A true CN101033202A (en) | 2007-09-12 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104127384A (en) * | 2014-08-07 | 2014-11-05 | 河北天成药业股份有限公司 | Carbamide peroxide for injection and production process thereof |
| CN104529831A (en) * | 2014-12-18 | 2015-04-22 | 西南化工研究设计院有限公司 | Preparation method of urea peroxide with high active oxygen content, high stability and high anti-moisture ability |
| CN106245310A (en) * | 2016-08-16 | 2016-12-21 | 朱玲 | A kind of 6 amino 1 hexanol absorbent-type hydrogen peroxide bleaching stabilizers |
| CN111296467A (en) * | 2020-03-30 | 2020-06-19 | 山东消博士消毒科技股份有限公司 | Compound hydrogen peroxide sterilization powder and manufacturing device thereof |
-
2007
- 2007-01-31 CN CN 200710010259 patent/CN101033202A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104127384A (en) * | 2014-08-07 | 2014-11-05 | 河北天成药业股份有限公司 | Carbamide peroxide for injection and production process thereof |
| CN104127384B (en) * | 2014-08-07 | 2016-05-11 | 河北天成药业股份有限公司 | A kind of injection Carbamaid peroxide and production technology thereof |
| CN104529831A (en) * | 2014-12-18 | 2015-04-22 | 西南化工研究设计院有限公司 | Preparation method of urea peroxide with high active oxygen content, high stability and high anti-moisture ability |
| CN106245310A (en) * | 2016-08-16 | 2016-12-21 | 朱玲 | A kind of 6 amino 1 hexanol absorbent-type hydrogen peroxide bleaching stabilizers |
| CN111296467A (en) * | 2020-03-30 | 2020-06-19 | 山东消博士消毒科技股份有限公司 | Compound hydrogen peroxide sterilization powder and manufacturing device thereof |
| CN111296467B (en) * | 2020-03-30 | 2022-03-08 | 山东消博士消毒科技股份有限公司 | Compound hydrogen peroxide sterilization powder and manufacturing device thereof |
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Open date: 20070912 |