WO2004002885A1 - Procede de fabrication de percarbonate de sodium - Google Patents

Procede de fabrication de percarbonate de sodium Download PDF

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Publication number
WO2004002885A1
WO2004002885A1 PCT/CN2003/000415 CN0300415W WO2004002885A1 WO 2004002885 A1 WO2004002885 A1 WO 2004002885A1 CN 0300415 W CN0300415 W CN 0300415W WO 2004002885 A1 WO2004002885 A1 WO 2004002885A1
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Prior art keywords
sodium
reaction
sodium carbonate
sodium percarbonate
hydrogen peroxide
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PCT/CN2003/000415
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English (en)
Chinese (zh)
Inventor
Zhigang Zhu
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Zhejiang Jinke Chemistry Co.,Ltd
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Priority to AU2003234899A priority Critical patent/AU2003234899A1/en
Publication of WO2004002885A1 publication Critical patent/WO2004002885A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C231/00—Preparation of carboxylic acid amides
    • C07C231/02—Preparation of carboxylic acid amides from carboxylic acids or from esters, anhydrides, or halides thereof by reaction with ammonia or amines
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B15/00—Peroxides; Peroxyhydrates; Peroxyacids or salts thereof; Superoxides; Ozonides
    • C01B15/055—Peroxyhydrates; Peroxyacids or salts thereof
    • C01B15/10—Peroxyhydrates; Peroxyacids or salts thereof containing carbon
    • C01B15/103—Peroxyhydrates; Peroxyacids or salts thereof containing carbon containing only alkali metals as metals
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C233/00—Carboxylic acid amides
    • C07C233/01—Carboxylic acid amides having carbon atoms of carboxamide groups bound to hydrogen atoms or to acyclic carbon atoms
    • C07C233/34—Carboxylic acid amides having carbon atoms of carboxamide groups bound to hydrogen atoms or to acyclic carbon atoms having the nitrogen atom of at least one of the carboxamide groups bound to a carbon atom of a hydrocarbon radical substituted by amino groups
    • C07C233/35—Carboxylic acid amides having carbon atoms of carboxamide groups bound to hydrogen atoms or to acyclic carbon atoms having the nitrogen atom of at least one of the carboxamide groups bound to a carbon atom of a hydrocarbon radical substituted by amino groups with the substituted hydrocarbon radical bound to the nitrogen atom of the carboxamide group by an acyclic carbon atom
    • C07C233/36—Carboxylic acid amides having carbon atoms of carboxamide groups bound to hydrogen atoms or to acyclic carbon atoms having the nitrogen atom of at least one of the carboxamide groups bound to a carbon atom of a hydrocarbon radical substituted by amino groups with the substituted hydrocarbon radical bound to the nitrogen atom of the carboxamide group by an acyclic carbon atom having the carbon atom of the carboxamide group bound to a hydrogen atom or to a carbon atom of an acyclic saturated carbon skeleton

Definitions

  • the invention relates to a method for preparing sodium percarbonate, and belongs to the technical field of preparation of oxygen-containing bleach. Background technique
  • Sodium percarbonate also known as sodium peroxycarbonate, has a molecular formula of Na 2 C0 3. L. 5HA, sodium carbonate peroxyhydrate, and the common name of sodium percarbonate in the industry is PCS.
  • PCS sodium percarbonate
  • Sodium percarbonate is usually prepared by the reaction of hydrogen peroxide and sodium carbonate aqueous solution, commonly known as wet crystallization processing method. The wet reaction includes the generation of an aqueous sodium carbonate solution and the reaction with an aqueous hydrogen peroxide solution.
  • the reaction conditions include the selection of sodium carbonate and hydrogen peroxide concentration, temperature, reaction time, and selected auxiliary agents.
  • Crystals formed in solution In order to reduce the solubility of sodium percarbonate in water, salting out agents such as sodium chloride and sodium sulfate are usually added to increase the yield and reduce the cost. The addition of a salting-out agent moves the reaction further to completion, which converts a larger portion of the reactant into the desired product. Synthetic reactions need to stabilize the active oxygen in sodium percarbonate, so it is also necessary to add an active oxygen stabilizer, called a crystallization aid.
  • Chinese patents CN1240407A and CN1156738 A disclose commonly used stabilizers.
  • the active oxygen content of crystalline sodium percarbonate obtained by the traditional wet method is generally 13-13.5%, and the bulk density is also large.
  • the synthesis reaction is fast, resulting in insufficient reaction, and the crystalline product obtained by the reaction has poor wet stability.
  • the consumption of sodium carbonate in the reaction is also high, and the waste liquid is discharged with some water pollution.
  • the object of the present invention is to provide a method for preparing sodium percarbonate, which can make sodium percarbonate have a high active oxygen content, good wet heat stability, and low raw material consumption.
  • the task of the present invention is achieved by the following technical solutions.
  • the sodium percarbonate is prepared by reacting a sodium carbonate solution with an aqueous hydrogen peroxide solution, which is characterized by the following steps:
  • an anhydrous sodium carbonate is added to an aqueous solution or a circulating mother liquor, and an aqueous sodium carbonate suspension is obtained through an emulsification and hydration reaction;
  • the hydrated sodium carbonate suspension and the hydrogen peroxide aqueous solution are introduced into the reaction kettle to react at a certain acceleration rate, and the sodium percarbonate crystal product is obtained by the reaction;
  • the third step is the solid-liquid separation of the crystals, the filtrate is recycled, and the crystals are post-processed into products; the molar ratio of the reaction between sodium carbonate and hydrogen peroxide is 1: 1. 3-1. 5;
  • a sodium-containing salting-out agent and a crystallization aid are added to the reaction.
  • the hydrated sodium carbonate suspension is prepared by adding anhydrous sodium carbonate to the circulating mother liquor, the amount of which is 20-5 OU'L hydration reaction temperature is 20-45 ° C_ emulsification hydration reaction time 5- 60 minutes;
  • the compound crystallization reaction temperature is 16-30 ° C, and the reaction time is 30-50 minutes.
  • the sodium percarbonate crystals are separated by filtration or centrifugation.
  • the crystals are dried at a temperature of 80-95 ° C, and then sieved to obtain a finished product.
  • the sodium-containing salting-out agent is one of sodium chloride and sodium sulfate, and the input amount is to maintain its concentration in the mother liquor of 17-22%;
  • the crystallization aid is selected from one or several mixtures of sodium silicate, organic phosphonic acid, magnesium sulfate, ethylenediaminetetraacetic acid or its sodium salt, and polypropionamide, and the input amount is 0.5 to the amount of sodium carbonate. 3%;
  • the hydrated sodium carbonate has a projecting acceleration of 800-1600 ml / h, and a hydrogen peroxide aqueous solution has a feeding rate of 210-660 ml / h.
  • the one-step reaction of the wet process is changed to a two-step reaction, and in particular, the reaction for preparing sodium carbonate hydrate is designed separately.
  • an anhydrous sodium carbonate is used to prepare an aqueous solution, or when anhydrous sodium carbonate is added to a circulating mother liquor, Using a high-speed emulsification shearer and agitator, the anhydrous sodium carbonate is hydrated with the water in the solution to form a hydrated sodium carbonate suspension.
  • the amount of anhydrous sodium carbonate used in the hydration reaction is the amount of mother liquor 20- 50 ° / » preferably 30-40 ° / » the hydration reaction time is 5- 50 minutes, preferably 10-30 minutes, and the hydration reaction temperature is 20-6 (TC , 25-45 ° C is preferred.
  • the degree of hydration of sodium carbonate in the 7-synthesis reaction is achieved by the temperature control of the suspension. When the temperature of the suspension is 32-35 ° C, sodium carbonate heptahydrate is formed, which is higher or lower than this. At temperature, sodium carbonate monohydrate or decahydrate will be formed, respectively.
  • the hydrated sodium carbonate suspension is mixed with a 25-70% hydrogen peroxide aqueous solution or added dropwise to the reactor at the same time to carry out the compounding reaction to form sodium percarbonate crystals. Since the sodium carbonate solution can fully react with hydrogen peroxide after emulsification and hydration, the amount of sodium carbonate dissolved in hydrogen peroxide water is greatly reduced, and the sodium carbonate content in the circulating fluid is reduced. During the preparation process, part of the circulating liquid is discharged, and the decrease of the content will reduce the loss of sodium carbonate, which will help reduce water pollution.
  • Another technical effect of the present invention is to utilize the characteristics of the hydration reaction as an exothermic reaction.
  • the temperature control of the emulsification hydration reaction only requires conventional water cooling, which will greatly reduce the heat of the second step reaction. The result is that during the crystallization reaction, only a small amount of frozen brine is needed to control the reaction temperature, thereby reducing the amount of frozen brine required.
  • the addition of a sodium-containing salting-out agent is indispensable.
  • the addition of sodium chloride or sodium sulfate can improve the yield of sodium percarbonate.
  • the addition of the salting-out agent can also reduce the sodium carbonate content in the mother liquor.
  • the salting-out agent is added to maintain its concentration in the circulating mother liquor of 15-22%, preferably ⁇ - 20 %.
  • the crystallization aid to be added in the present invention has the function of stabilizing active oxygen, such as sodium silicate, organic phosphonic acid, ethylenediaminetetraacetic acid and its sodium salt, a mixture of one or more kinds of polyacryl, etc. 5-3% ⁇ The amount of sodium carbonate in the reaction solution was added in an amount of 0.5-3%. The addition of crystallization aids makes the sodium percarbonate crystal particles have higher uniformity and purity, so that the product has better wet and thermal stability.
  • the thermal stability of the sodium percarbonate prepared by the invention is> 92% (105 ° C for 2 hours), and the wet stability is> 50%.
  • the product is very suitable for use in solid bleaching agents and phosphorus-free detergents.
  • Test method for wet stability 10 g of sodium percarbonate particles are mixed with 10 g of 4A zeolite, placed in an open culture subculture, and stored at 32 ° C and 80% relative humidity for 48 hours to calculate the sample active oxygen The remaining rate.
  • Example 1 14. 2 0. 82 957 512 95. 1 53. 3 Example 2 14. 5 0. 57 1072 762 94. 7 56. 1 Example 3 14. 3 0. 66 1032 432 95. 5 51. 7 Example 4 14. 2 0. 92 981 561 96. 3 52. 4 Example 5 13. 9 0. 43 760 523 96. 5 51. 6 Example 6 14. 2 0. 83 983 462 96. 6 53. 8 Example 7 14. 4 0. 55 940 625 95. 5 55. 4 Example 8 14. 6 0. 88 1060 912 94. 4 60. 2 Comparative test 13. 6 0. 92 810 430 92. 3 23.
  • the active oxygen content of the sodium percarbonate prepared by the present invention is over 14%, the product moisture content is reduced, the average particle size is increased, and especially the wet stability is greatly improved, and the effect is very significant. .
  • the implementation of the present invention can also reduce the consumption of sodium carbonate, reduce the process energy consumption, is beneficial to environmental protection, and is a preparation process with good economic and environmental benefits.
  • a hydrated sodium carbonate suspension was introduced at a total speed of 1200 ml per hour, while a concentration of 27.5% hydrogen peroxide solution was introduced at a total speed of 675 ML per hour, and the hydrogen peroxide in the mother liquor of the reactor was maintained at> 0.7%.
  • the temperature is maintained at 22-23 ° C, the process lasts about 40 minutes, and the feeding is completed.
  • the crystallization reaction product in the reaction kettle is separated from the mother liquor by a centrifuge, and the filtrate is recycled into the mother liquor tank for reuse. Dry in a fluidized bed at about 90 ° C for 30 minutes to obtain 409 g of finished product.
  • Example 1 The method steps are the same as in Example 1.
  • the different process conditions are as follows: In the first step, 840 g of mother liquor with 5% sodium carbonate content, 280 g of anhydrous sodium carbonate, 80 g of sodium chloride, reaction time 25 minutes, and reaction temperature 25 -3 (TC, to generate sodium carbonate decahydrate suspension; in the second step reaction, 450 g of 27.5% hydrogen peroxide solution, 1 g of seed crystals, hydrogen peroxide solution feed rate 430ml / h, sodium carbonate hydrate The suspension was fed at a speed of 800ml / h, the reaction time was 60 minutes, and the reaction temperature was 22-23 ° C. 410 g of sodium percarbonate was obtained.
  • Example three Example three
  • the method steps are the same as in Example 1, and the different process conditions are as follows:
  • the first step is a reaction, containing 840 g of sodium carbonate 7% mother liquor, adding 280 g of anhydrous sodium carbonate, 60 g of sodium chloride, 7 minutes of reaction time 25 minutes, hydration the reaction temperature of 25- 30 ° C, a suspension of sodium carbonate decahydrate generated;
  • the second reaction a concentration of 35 percent aqueous hydrogen peroxide 330 g seed 5 g, sodium carbonate hydrate suspension feed rate 960ml / h,
  • the hydrogen peroxide solution was fed at a speed of 400 ml / h, and the reaction time for crystallization was 50 minutes, and the reaction temperature was 22-23 ° C. 395 g of sodium percarbonate was obtained.
  • the method steps are the same as in Example 1, and the different process conditions are as follows:
  • the first step is a reaction, containing 840 g of sodium carbonate 7.2% mother liquor, adding 280 g of anhydrous sodium carbonate, 60 g of sodium chloride, and a hydration reaction time of 20 minutes.
  • the hydration reaction temperature is 32-35 ° C, and a sodium carbonate heptahydrate suspension is formed.
  • the method steps are the same as in Example 1, and the different process conditions are as follows:
  • the first step is reaction, 840 g of mother liquor containing 8% sodium carbonate, 280 g of anhydrous sodium carbonate, 68 g of sodium chloride, hydration reaction time 15 minutes, hydration reaction At a temperature of 38-43 ° C, a sodium carbonate monohydrate suspension is formed;
  • the second step reaction 320 g of a 35% hydrogen peroxide aqueous solution, 8 grams of seed crystals, and a hydrated sodium carbonate suspension feed rate of 1600 ml / h ; peroxidation
  • the hydrogen hydrogen solution was fed at a speed of 660 ml / h, the reaction time was 30 minutes, and the reaction temperature was 24-25 ° C. 394 g of sodium percarbonate crystals were obtained.
  • the method steps are the same as in Example 1.
  • the different process conditions are as follows:
  • the first step is reaction, 840 g of mother liquor containing 2% sodium carbonate, 280 g of anhydrous sodium carbonate, 32 g of sodium chloride, hydration reaction time 20 minutes, hydration reaction temperature 2 5 - 3 (TC, generates a suspension of sodium carbonate decahydrate;
  • the second reaction a concentration of over 235 g of 50% aqueous hydrogen peroxide solution, the seed crystal 5 grams of sodium carbonate hydrate suspension feed rate 1070ml / h, over Feeding rate of hydrogen oxide solution is 300ml / h, and the reaction time of feeding crystallization is 45 minutes
  • the reaction temperature was 22-23 ° C, and 415 g of sodium percarbonate was obtained.
  • Example 8 The method steps are the same as in Example 1.
  • the different process conditions are as follows: In the first step, 840 g of mother liquor containing 12% sodium carbonate, 280 g of anhydrous sodium carbonate, 16 g of sodium chloride, hydration reaction time 20 minutes, and hydration reaction At a temperature of 25-30 ° C, a suspension of sodium carbonate decahydrate is formed; in the second reaction step, 180 g of a 70% hydrogen peroxide aqueous solution, 2 g of seed crystals, a sodium hydrate feed rate of 107 Oml / h, and hydrogen peroxide The feed rate of the aqueous solution was 210 ml / h, the reaction time of the crystallization was 45 minutes, and the reaction temperature was 22-23 ° C. 423 g of sodium percarbonate was obtained.
  • Example eight The feed rate of the aqueous solution was 210 ml / h, the reaction time of the crystallization was 45 minutes, and the reaction temperature was 22-23
  • the method steps are the same as in Example 1, and the different process conditions are as follows:
  • the first step is a reaction, containing 840 g of sodium carbonate 12.3% mother liquor, adding 280 g of anhydrous sodium carbonate, 16 g of sodium chloride, and a reaction time of 20 minutes. 5 ⁇ , Hydration reaction temperature of 32-35 ° C, to generate a sodium carbonate heptahydrate suspension;
  • the second step of the reaction a concentration of 70% hydrogen peroxide aqueous solution 188 grams, seed 0. 5 grams.
  • the feed rate of 7J sodium carbonate suspension is 1070ml / h
  • the feed rate of aqueous hydrogen peroxide solution is 210ml / h
  • the reaction time of crystallization is 90 minutes
  • the reaction temperature is 22-23 ° C. 394 g of sodium percarbonate is obtained.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Detergent Compositions (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

L'invention se rapporte à un procédé de fabrication de percarbonate de sodium, qui a trait au domaine de la préparation des agents de blanchiment contenant de l'oxygène. Ledit procédé comprend une réaction entre une suspension de carbonate de sodium hydraté, qui est obtenue par émulsification et hydratation d'une solution de carbonate de sodium, et une solution aqueuse à 25 %-70 % de H2O2, puis par cristallisation. Au cours de la réaction, le chlorure de sodium ou le sulfate de sodium est ajouté en tant qu'agent de relarguage, et du silicate de sodium, de l'acide organophosphonique, et de l'acide tétra-acétique d'éthylènediamine ainsi que le sel de sodium de cet acide sont utilisés en tant que promoteur de cristallisation. L'hydratation et l'émulsification de la solution aqueuse de carbonate de sodium accélèrent sensiblement la cristallisation du peroxyde d'hydrogène restant, tout en réduisant la quantité de carbonate de sodium présente dans la solution mère. Les produits à base de percarbonate de sodium préparés conformément à cette invention sont obtenus à haut rendement avec une faible consommation de matières premières. Les produits de percarbonate de sodium préparés conformément à cette invention présentent l'avantage de posséder une teneur supérieure en oxygène activé, de présenter une taille de particules plus importante, et d'être dotés d'une stabilité hydrothermique supérieure en comparaison des produits obtenus selon un procédé de traitement par voie humide classique. La mise en oeuvre de cette invention est avantageuse d'un point de vue économique ainsi que d'un point de vue environnemental.
PCT/CN2003/000415 2002-06-27 2003-05-30 Procede de fabrication de percarbonate de sodium WO2004002885A1 (fr)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111717980A (zh) * 2020-06-19 2020-09-29 天津农学院 缓释增氧剂及其制备方法和应用

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EP1905738A1 (fr) * 2006-09-28 2008-04-02 Evonik Degussa GmbH Procédé de préparation de percarbonate de sodium sous forme de granules
CN101270233B (zh) * 2008-04-22 2010-12-15 浙江时代金科过氧化物有限公司 一种低堆密度颗粒型包膜过碳酸钠的制备方法
CN102642815A (zh) * 2012-03-05 2012-08-22 浙江金科过氧化物股份有限公司 过碳酸钠母液的循环回收利用方法
CN102634422B (zh) * 2012-03-31 2013-09-18 湖南洁宇日化新技术股份有限公司 含氧洗涤剂的制备方法
CN104743519B (zh) * 2015-01-21 2017-01-18 江西省博浩源化工有限公司 一种用十水碳酸钠和纯碱混合物制备过碳酸钠的方法
CN104528658B (zh) * 2015-01-21 2016-11-09 江西省博浩源化工有限公司 一种水合肼副产物制备过碳酸钠的方法及产品
CN104743520B (zh) * 2015-01-21 2016-05-18 江西省博浩源化工有限公司 一种用十水碳酸钠制备过碳酸钠的方法
CN104743518B (zh) * 2015-01-21 2017-02-22 江西省博浩源化工有限公司 一种制备过碳酸钠的助晶剂的使用方法
CN111285334A (zh) * 2018-12-10 2020-06-16 天津大学 具有致密球形结构的过氧碳酸钠及其制备方法
CN112591771A (zh) * 2020-12-17 2021-04-02 钟广新 一种碳酸氢钠及氯化铵的循环生产工艺

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JPS589805A (ja) * 1981-07-02 1983-01-20 Kao Corp 顆粒状過炭酸ナトリウムの製造方法
JPH0624713A (ja) * 1992-07-06 1994-02-01 Central Glass Co Ltd 水溶性に優れた過炭酸ソーダの製造方法
DE4338400A1 (de) * 1993-11-10 1995-05-11 Degussa Verfahren zur Herstellung von Natriumpercarbonat
EP0748764A1 (fr) * 1995-06-08 1996-12-18 AUSIMONT S.p.A. Procédé de préparation de percarbonate de sodium sous forme de granulés
EP0787682A1 (fr) * 1996-02-05 1997-08-06 Glatt Ingenieurtechnik GmbH Procédé de préparation de percarbonate de sodium en granules

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FR2746386B1 (fr) * 1996-03-19 1998-04-24 Atochem Elf Sa Nouveau percarbonate de sodium et son procede d'obtention
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Publication number Priority date Publication date Assignee Title
US4146571A (en) * 1976-10-22 1979-03-27 Treibacher Chemische Werke Preparation of sodium percarbonate
JPS589805A (ja) * 1981-07-02 1983-01-20 Kao Corp 顆粒状過炭酸ナトリウムの製造方法
JPH0624713A (ja) * 1992-07-06 1994-02-01 Central Glass Co Ltd 水溶性に優れた過炭酸ソーダの製造方法
DE4338400A1 (de) * 1993-11-10 1995-05-11 Degussa Verfahren zur Herstellung von Natriumpercarbonat
EP0748764A1 (fr) * 1995-06-08 1996-12-18 AUSIMONT S.p.A. Procédé de préparation de percarbonate de sodium sous forme de granulés
EP0787682A1 (fr) * 1996-02-05 1997-08-06 Glatt Ingenieurtechnik GmbH Procédé de préparation de percarbonate de sodium en granules

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111717980A (zh) * 2020-06-19 2020-09-29 天津农学院 缓释增氧剂及其制备方法和应用

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CN1330561C (zh) 2007-08-08
AU2003234899A1 (en) 2004-01-19
AU2003234900A1 (en) 2004-01-19
CN1463913A (zh) 2003-12-31

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