• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    The invention relates to a process for the production of compact, coarse sodium percarbonate which comprises reacting hydrogen peroxide at 10 to 20 DEG C, with an input solution containing sodium carbonate and saturated with sodium percarbonate in the presence of 100 to 200 g of sodium chloride per litre of solution, at least one active oxygen stabiliser and from 0.1 to 1.9 g of sodium hexametaphosphate per litre of solution, the ratio of soda to sodium hexametaphosphate in the input solution being from 65:1 to 500:1, hydrogen peroxide being added to the soda input solution or suspension in a quantity which is substantially equivalent to the sodium carbonate dissolved and/or suspended in the input solution at a temperature maintained at substantially one and the same level throughout the entire precipitation process, subsequently reducing the over-saturation of dissolved sodium percarbonate formed by precipitation of the sodium percarbonate during and for up to 60 minutes after addition of the hydrogen peroxide, and separating off and drying the salt obtained. Optionally the mother liquor accumulating is returned to the working stage for the soda input solution.
    公开号:SU957757A3
    申请号:SU782680502
    申请日:1978-11-01
    公开日:1982-09-07
    发明作者:Книппшильд Герд；Шустер Хуберт；Клебе Ханс
    申请人:Дегусса (Фирма)；
    IPC主号:
    专利说明:

    The invention relates to methods for producing percarbonate, which is used as a bleach in synthetic detergents.
    A known method for producing sodium percarbonate 5 by reacting a solution or suspension of soda with an aqueous solution of hydrogen peroxide in the presence of sodium chloride [1].
    Closest to the proposed invention in technical essence and the achieved result is a method for producing sodium percarbonate by reacting sodium carbonate contained in a saturated solution of 5 sodium percarbonate with hydrogen peroxide at a temperature of up to 30 ° C in the presence of sodium chloride, an active oxygen stabilizer, for example magnesium sulfate , in the amount of 3-10 and 2-8 g / l of 20 sodium hexametaphosphate, followed by separation of the product precipitate [2]. The disadvantage of these methods is that they do not provide 25 obtain a coarse product.
    The purpose of the invention is the increase in particle size of the precipitate of the product.
    The goal is achieved according to the method for producing sodium percarbonate 2, which consists in the fact that the sodium carbonate contained in a saturated solution of sodium percarbonate is reacted with hydrogen peroxide at 10-20 ° C in the presence of sodium chloride, an active oxygen stabilizer such as magnesium sulfate and 0 , 1-1.9 g / l of sodium hexametate phosphate, and the weight ratio between sodium carbonate and sodium hexametaphosphate is maintained equal to (65-500): 1, respectively, followed by separation of the product precipitate.
    The method is as follows.
    An initial aqueous solution is prepared containing g / l: sodium percarbonate 40-100, sodium hexametaphosphate 0.11.9, sodium chloride 100-200 and saturated with magnesium sulfate. In the preparation of the initial solution, you can use the mother liquor obtained after separation of the finished product, which also contains 40-100 g / l of sodium percarbonate. A necessary condition for this is to maintain the weight ratio between sodium carbonate contained in sodium percarbonate and sodium hexametafsophate equal to (65-500): 1. The solution or suspension obtained in this way by introducing ·) into interaction with hydrogen peroxide taken in an amount equivalent to the amount contained in the initial solution, the amount of sodium carbonate. The process is carried out at 10-20 ° C for up to 60 min, after which the precipitated sodium percarbonate is separated and su & at, and the mother liquor is sent to the beginning of the process.
    It was experimentally established that in order to achieve this goal it is necessary to introduce 0.1-1.9 g / l sodium hexametaphosphate into the initial solution. The introduction of the latter more than 1.9 g / l leads to the fact that the addition of hydrogen peroxide does not reduce the supersaturation of the initial solution with sodium percarbonate, i.e. the crystallization process may stop (according to the prototype, product precipitation occurs at a higher content of sodium hexametaphosphate and at a higher temperature in the form of fine crystalline particles), the introduction of sodium hexametaphosphate less than 0.1 g / l leads to spontaneous crystallization, and therefore a fine crystalline product is obtained.
    In addition, when implementing the method, it is important to maintain the weight ratio between sodium carbonate and sodium hexametaphosphate equal to (65500): 1, respectively. So, with an increase in the indicated ratio to 600: 1, the product sharply rises : 35 the content of fine crystalline particles, in particular when the ratio of these components is 500: 1, the fraction of particles in the product with a size of less than 0.2 mm is 11%, and with a ratio of 600 : 1 - 28%.
    . The lower limit of the weight ratio between sodium carbonate and sodium hexametaphosphate is set equal to 65: 1, since a further decrease in the soda content does not allow to obtain a coarse-grained product.
    It was experimentally established that when using the indicated solution compositions, the treatment of the latter with hydrogen peroxide should be carried out at 1020 ° C. Using temperatures above 20 ° C leads to a large loss of active oxygen, i.e. product quality is lower than in the prototype. A temperature below 10 ° C is impractical, since it does not lead to a noticeable increase in the fineness of crystalline grains and requires additional cooling costs.
    PRI me R , 1. In a thermostated two-liter beaker equipped with a stirrer, prepare a solution saturated with sodium percarbonate and · containing, g / l: sodium chloride 200, magnesium sulfate 4.5 and sodium hexametaphosphate 0.1, at The weight ratio between the sodium carbonate contained in sodium percarbonate and sodium hexametaphosphate is maintained at 500: 1, respectively. The initial solution at 10 ° C is introduced into interaction with hydrogen peroxide, taken in an equivalent amount to the amount of sodium carbonate contained in the solution. The resulting crystalline precipitate of sodium percarbonate is separated using a centrifuge and dried.
    Get a product with the following characteristics: active oxygen 13.94%; composition by fractions: particles with a size of less than 0.2 mm 11%, 0.2 mm 38%, 0.4 mm - 15%, 0.5 mm - 29%, 0.8 mm - 6¾.
    With an increase in the weight ratio of sodium carbonate and sodium hexametaphosphate to 600: 1, respectively, under the conditions of this experiment, a product with a content of fine crystalline grains (with a particle size of less than 0.2 mm) is obtained 28%.
    Example 2 The method is carried out analogously to example 1, however, the initial solution contains 1.9 g / l of hexametaphosphate, sodium, and the weight ratio between sodium carbonate and sodium hexametaphosphate is maintained equal to 110: 1, respectively, and the process is carried out at 20 ° C. The fraction of fine crystalline particles (with grain size less than 0.2 mm) in the product is 9%.
    Example 3. The method is carried out analogously to example 1, but the weight ratio between sodium carbonate and sodium hexametaphosphate is maintained at 65: 1 and the process is carried out at 20 ° C. In the resulting product, the fraction of fine crystalline particles (with grain size less than 0.2 mm) is 8%.
    Reproduction of the prototype method leads to spontaneous crystallization of the product (the product is crystalline), or product isolation was not observed at all.
    Thus, the method according to this invention allows to stably obtain a coarse-grained product with a fine crystalline phase content (with a particle size of less than 0.2 mm) of not more than 9-11%, while the prototype makes it possible to obtain only a fine-grained product.
    权利要求:
    Claims (3)
    [1]
    The invention relates to methods for producing percarbonate, which is used as a bleaching agent in detergents. A known method of producing sodium percarbonate by reacting a solution or suspension of soda with an aqueous solution of hydrogen peroxide in the presence of sodium chloride 1. The closest to the proposed invention in its technical essence and the achieved result is a method for producing sodium percarbonate by reacting sodium carbonate contained in a saturated solution of sodium percarbonate with water peroxide of the genus at a temperature up to 30 ° C in the presence of sodium chloride, an active oxygen stabilizer, for example sulfate magnesium, in the amount of 3-10 and 2-8 g / sodium sodium hexametaphosphate, followed by separation of the precipitate of product 2. The disadvantage of these methods is that they do not provide a coarse-grained product. The purpose of the invention is to increase the particle size of the product sediment. The goal is achieved according to the method for producing sodium percarbonate, which implies that sodium carbonate contained in a saturated solution of sodium percarbonate is reacted with hydrogen peroxide at 10-20 ° C in the presence of sodium chloride, an active oxygen stabilizer such as magnesium sulfate and 0, 1-1.9 g / l of sodium phosphate hexamete, the weight ratio between sodium carbonate and sodium hexametaphosphate being maintained at (65-500): 1, respectively, followed by separation of the product precipitate. The method is carried out as follows. An initial aqueous solution is prepared containing g / l: sodium percarbonate 40-100, sodium hexametaphosphate 0.11, 9, sodium chloride 100-200 and saturated with magnesium sulfate. In preparing the initial solution, the mother solution obtained after separation of the finished product, which also contains 40-100 g / l of sodium percarbonate, can be used. A prerequisite for this is to maintain the weight ratio between sodium carbonate contained in sodium percarbonate and sodium hexametaphosphate (65-500): 1. The solution or suspension thus obtained is brought into contact with hydrogen peroxide, taken in an amount equivalent to containing sodium carbonate in the initial solution. The process is carried out at 10–20 ° C for up to 60 minutes, after which the precipitated sodium percarbonate is separated and the iiaT su, and the mother liquor is sent to the beginning of the process. It was established experimentally that in order to achieve this goal, it is necessary to introduce 0.1-1.9 g / l of sodium hexametaphosphate into the initial solution. The introduction of the latter more than 1.9 g / l leads to the fact that the addition of hydrogen peroxide does not reduce the saturation of the initial solution with sodium percarbonate, i.e. The crystallization process can stop (on the prototype type, product precipitation occurs at a higher content of sodium hexametaphosphate and at a higher temperature in the form of fine-crystalline particles), the introduction of sodium hexametaphosphate less than 0.1 g / l leads to spontaneous crystallization, and consequently get crystalline product. In addition, when carrying out the process, it is important to maintain the weight ratio between sodium carbonate and sodium hexametaphosphate equal to (65500); 1 respectively. Thus, with an increase in this ratio up to 600: 1; the content of fine-crystalline chagtits in the product increases dramatically, in particular, when the ratio of these components is 500: 1 the fraction of particles in the product with a size of less than 0.2 mm is 11%, and at a ratio of 600: 1 - 28 % . The lower limit of the weight ratio between sodium carbonate and sodium hexametaphosphate is set to 65: 1, since a further decrease in the soda content does not allow the coarse-crystalline product to be obtained. It was established experimentally that when using the indicated composition of the solution, the treatment with the last one with hydrogen peroxide should be carried out at 1020 ° C. The use of temperature above leads to a large loss of active oxygen, i.e. the quality of the product is lower than in the prototype. The temperature is lower. It is not feasible, since it does not lead to a noticeable increase in the grain size of the crystal grains and requires additional costs for cooling. Example 1. In a two-liter thermostated tumbler equipped with a stirrer, a solution of sodium percarbonate starch prepared and containing, g / l: sodium chloride 200, magnesium sulfate 4.5 and sodium hexametaphosphate 0.1, while The weight ratio between sodium carbonate contained in sodium percarbonate and sodium hexametaphosphate is maintained at 500: 1, respectively. The stock solution is reacted with hydrogen peroxide, taken in equivalent amount to the amount of sodium carbonate contained in the solution. The resulting crystalline sodium percarbonate precipitate is separated using a centrifuge and dried. Get the product, with the following characteristics: active oxygen 13,94%; composition by fraction: particles with a size less than. 0.2 mm 11%, 0.2 mm 38%, 0.4 mm - 15%, 0.5 mm - 29%, 0.8 mm - 6%. By increasing the weight ratio of sodium carbonate and sodium hexametaphosphate to 600: 1, respectively, under the conditions of this experiment, a product with a content of fine-grained grains (with a particle size less than 0.2 mm) of 2-8% is obtained. Example
    [2]
    2. The method is carried out analogously to example 1, however, the initial solution contains 1.9 g / l of hexametaphosphate. sodium, and the weight ratio between sodium carbonate and sodium hexametaphosphate is 110: 1, respectively, and the process is carried out at. The share of fine-crystalline particles (with a grain size of less than 0.2 mm) in the product is 9%. Example
    [3]
    3. The method is carried out analogously to example 1, but the weight ratio between sodium carbonate and sodium hexametaphosphate is maintained at 65: 1 and the process is carried out at 20 ° C. In the resulting product, the proportion of fine-crystalline particles (with a grain size of less than 0.2 mm) is 8%. Reproduction of the prototype method leads to spontaneous crystallization of the product (fine-crystalline product), or no product separation was observed at all. Thus, the method according to the invention allows to stably obtain a coarse-grained product with a fine-crystalline phase content (with a particle size of less than 0.2 mm) of not more than 9-11%, while the prototype can only produce a fine-grained product. The method of obtaining sodium parcarbonate by reacting sodium carbonate containing sodium percarbonate in saturated solution with hydrogen peroxide at 10-20 ° C in the presence of sodium chloride, active oxygen stabilizer and sodium hexametaphosphate. With subsequent separation of the product precipitate, I distinguish .59577576
    u and with the fact that, in order to increase the sources of information,
    neither the size of the sediment particles, hexametae taken time during examination
    sodium phosphate is used in amount; 1. Patent (Ivetsii 90295,
    ve 0.1-1.9 g / l solution with support-cells. 42 i 20 / pub. 1937,: the weight ratio between Carbog 2. German Federal Republic 2328803,
    nat sodium and hexametaphosphate nat-5kl, C 01 B 15/10, published, 1971 (look at (65-500): respectively, totype),
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    同族专利:
    公开号 | 公开日
    IL56390D0|1979-03-12|
    DE2800760A1|1979-07-19|
    PL212677A1|1979-11-05|
    SE7900158L|1979-07-10|
    FR2414022B1|1982-11-19|
    CA1106136A|1981-08-04|
    AT386590B|1988-09-12|
    CH638464A5|1983-09-30|
    JPS6327292B2|1988-06-02|
    ATA16279A|1988-02-15|
    IL56390A|1981-09-13|
    PL114221B1|1981-01-31|
    JPS54101798A|1979-08-10|
    DE2800760C2|1983-01-27|
    ZA786759B|1979-11-28|
    GB2011874B|1982-05-26|
    BE873347A|1979-07-09|
    DD141013A5|1980-04-09|
    ES475099A1|1979-04-16|
    IT1160954B|1987-03-11|
    SE439152B|1985-06-03|
    IT7869696D0|1978-11-24|
    GB2011874A|1979-07-18|
    PT68751A|1978-12-01|
    FR2414022A1|1979-08-03|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    DE2328803C3|1973-06-06|1982-11-25|Peroxid-Chemie GmbH, 8023 Höllriegelskreuth|Process for the production of an abrasion-resistant, coarse-grained sodium percarbonate|
    DE2644148C3|1976-09-30|1983-05-11|Degussa Ag, 6000 Frankfurt|Continuous process for the production of a compact, coarse-grained sodium percarbonate|
    DE2644147C3|1976-09-30|1983-05-19|Degussa Ag, 6000 Frankfurt|Process for the production of a compact, coarse-grained sodium percarbonate|
    AT356627B|1976-10-22|1980-05-12|Treibacher Chemische Werke Ag|METHOD FOR PRODUCING SODIUM PERCARBONATE|JPS5833164B2|1980-07-04|1983-07-18|Kao Soap Co|
    JPS58182855U|1982-05-31|1983-12-06|
    JPS58186557U|1982-06-04|1983-12-12|
    JPS6339827Y2|1982-07-05|1988-10-19|
    DE59301882D1†|1992-10-16|1996-04-18|Solvay Interox Gmbh|Sodium percarbonates stabilized by coating|
    DE4306399C2|1993-03-02|1995-06-14|Degussa|Process for the preparation of stabilized sodium percarbonate|
    DE4311944A1|1993-04-10|1994-10-13|Degussa|Coated sodium percarbonate particles, process for their preparation and detergent, cleaning and bleaching compositions containing them|
    US5560896A|1993-08-31|1996-10-01|Degussa Aktiengesellschaft|Method for producing granulated sodium percarbonate|
    IT1276685B1|1995-06-08|1997-11-03|Ausimont Spa|PROCESS FOR THE PRODUCTION OF SODIUM PERCARBONATE IN GRANULAR FORM|
    DE19717729A1|1997-04-26|1998-10-29|Degussa|Coated sodium percarbonate particles, process for their preparation and their use|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    DE2800760A|DE2800760C2|1978-01-09|1978-01-09|Process for the production of sodium percarbonate from a soda solution or suspension|
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