JP3975075B2 - Method for producing stable sodium percarbonate - Google Patents
Method for producing stable sodium percarbonate Download PDFInfo
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- JP3975075B2 JP3975075B2 JP2001352855A JP2001352855A JP3975075B2 JP 3975075 B2 JP3975075 B2 JP 3975075B2 JP 2001352855 A JP2001352855 A JP 2001352855A JP 2001352855 A JP2001352855 A JP 2001352855A JP 3975075 B2 JP3975075 B2 JP 3975075B2
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- sodium percarbonate
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Description
【０００１】
【発明の属する技術分野】
本発明は、安定な過炭酸ナトリウムの製造方法に関する。更に詳細には、ゼオライトを含有する洗剤に配合するのに好適な過炭酸ナトリウムの製造方法に関する。
【０００２】
【従来技術】
過炭酸ナトリウムは、色柄物の漂白にも使用できること、生地を傷めないこと等のために、単独で、或いは洗剤に配合されて使用されている酸素系漂白剤である。
過炭酸ナトリウムを配合した洗剤は、洗濯と同時に漂白を行うことができ、有用であるが、ゼオライトが配合された洗剤中では、過炭酸ナトリウムは不安定であり、分解して有効酸素を失ってしまう。
そこで、一般的には、過炭酸ナトリウム粒子とゼオライトとが直接、接触しないように、過炭酸ナトリウム粒子をある種の化合物で被覆することが行われている。例えば、特開昭59-193999号公報には、過炭酸ナトリウムをメタホウ酸ソーダと珪酸アルカリ金属塩の水溶液で被覆する方法が、特開平7-69606号公報には、珪酸塩、硫酸マグネシウム、及びアルカリ金属の硫酸塩の水溶液で被覆する方法が開示されている。
【０００３】
これらの被覆方法は、乾燥させた過炭酸ナトリウム粒子の表面に、被覆剤水溶液を噴霧、或いは滴下する方法であるため、(1)被覆剤水溶液が、過炭酸ナトリウム粒子表面に多数に存在する微小な空隙から過炭酸ナトリウム粒子内部に浸透してしまい、粒子表面への被覆効率が低下するという問題がある。また、(2)一旦乾燥させた過炭酸ナトリウム粒子に、被覆剤水溶液を噴霧、或いは滴下するので被覆処理の後、再び乾燥を行わなくてはならず、乾燥設備面、及びエネルギー消費面で問題がある。
【０００４】
【発明が解決しようとする課題】
本発明者は、上記欠点、即ち、被覆剤を均一に、しかも効率よく過炭酸ナトリウム粒子表面に被覆でき、かつ乾燥工程でのエネルギー負荷の少ない被覆方法について検討を重ねた結果、特定の無機化合物の粉末を湿潤過炭酸ナトリウム粒子表面に塗した後、その無機化合物を水和物として固定化することによって、均一な被膜を効率よく形成させることができることを見出し、本発明を完成させた。
【０００５】
【課題を解決するための手段】
即ち、本発明は、湿潤過炭酸ナトリウム粒子と、平均粒径が5〜200μの、無水炭酸ナトリウム粉末又は無水硫酸ナトリウム粉末とを混合して、該湿潤過炭酸ナトリウム粒子表面に該無水化合物粉末を吸着させ、該無水化合物を過炭酸ナトリウム粒子表面に該化合物の水和物の被膜として固定化することを特徴とする、安定な過炭酸ナトリウムの製造方法に関する。
【０００６】
また、湿潤過炭酸ナトリウム粒子と、平均粒径が5〜200μの、無水炭酸ナトリウム粉末又は無水硫酸ナトリウム粉末とを混合して、該湿潤過炭酸ナトリウム粒子表面に該無水化合物粉末を吸着させた後、該混合系内に水を噴霧、または滴下して、該無水化合物を過炭酸ナトリウム粒子表面に該化合物の水和物の被膜として固定化することを特徴とする、安定な過炭酸ナトリウムの製造方法に関する。
前記湿潤過炭酸ナトリウムの含水率は5〜20％である。
湿潤過炭酸ナトリウム粒子と、無水炭酸ナトリウム粉末又は無水硫酸ナトリウム粉末の混合系内に噴霧、または滴下する水は、珪酸塩、又は／及びマグネシウム塩を溶解、或いは懸濁させて用いることができる。
【０００７】
【発明の実施の形態】
本発明で用いる湿潤過炭酸ナトリウムは、過酸化水素と炭酸ナトリウムとを水溶液中で反応させた後、脱水機で脱水して得られるものをそのまま、或いは含水率を調整して用いることができるが、含水率5〜20％の湿潤過炭酸ナトリウムを用いることが好ましい。
本発明においては、湿潤過炭酸ナトリウム粒子と特定粒径の、無水炭酸ナトリウム粉末又は無水硫酸ナトリウム粉末とを混合して、該湿潤過炭酸ナトリウム粒子表面に無水炭酸ナトリウム又は無水硫酸ナトリウムを吸着させるが、用いる無水炭酸ナトリウム粉末又は無水硫酸ナトリウム粉末の平均粒径は、好ましくは、5〜200μであり、より好ましくは、5〜50μである。
【０００８】
湿潤過炭酸ナトリウム粒子と無水炭酸ナトリウム粉末又は無水硫酸ナトリウム粉末との混合には、転動水平式混合機、破砕転動式造粒機、連続混合機等が使用できるが、転動水平式混合機が良い。
噴霧、または滴下する水に、珪酸塩、又は／及びマグネシウム塩を溶解、或いは懸濁させて用いることができるが、珪酸塩としては、オルト珪酸ナトリウム、セスキ珪酸ナトリウム、メタ珪酸ナトリウム、及び水ガラス１〜３号等の珪酸塩であり、マグネシウム塩としては、硫酸マグネシウム、塩化マグネシウム等である。更にまた、噴霧、または滴下する水に、ベンゼンスルホン酸ナトリウム、p-トルエンスルホン酸ナトリウム、m-キシレンスルホン酸ナトリウム等の芳香族炭化水素スルホン酸塩、四硼酸ナトリウム、オクタ硼酸ナトリウム、ペンタ硼酸ナトリウム、メタ硼酸ナトリウム等の硼酸塩等の公知過炭酸ナトリウム被覆剤を溶解、或いは懸濁させても良い。
【０００９】
本発明では、湿潤過炭酸ナトリウムと、無水炭酸ナトリウム粉末又は無水硫酸ナトリウム粉末を添加、混合するが、該湿潤過炭酸ナトリウムに炭酸ナトリウムの水溶液又は硫酸ナトリウムの水溶液を添加、混合した場合には、水分過多の状態となり、過炭酸ナトリウム粒子がブロック化し、乾燥自体困難な状態となってしまう。本発明では過炭酸ナトリウム粒子がブロック化を起こすことはない。
【００１０】
本発明の作用機構は明らかでないが、例えば、無水炭酸ナトリウムを用いた場合、湿潤過炭酸ナトリウム粒子表面に吸着した無水炭酸ナトリウムが、湿潤過炭酸ナトリウム中の水分、或いは系内に噴霧、或いは滴下される水分と反応し、過炭酸ナトリウム粒子表面に炭酸ナトリウムの水和物の被膜を形成する際、過炭酸ナトリウム粒子表面が該反応で発熱するため、被膜が過炭酸ナトリウム粒子表面に均一に展開しやすくなると共に強固に固定化されて、安定な過炭酸ナトリウムを得ることができるものと推定される。
【００１１】
【実施例】
以下に本発明を実施例で説明する。
（以下の実施例において使用する、湿潤過炭酸ナトリウム）
炭酸ナトリウムと過酸化水素とを塩化ナトリウムを共存させた水溶液中で反応させた後、脱水して、含水率10％の湿潤過炭酸ナトリウムを得た。
【００１２】
比較例１
上記の方法で得た、湿潤過炭酸ナトリウムを乾燥して、有効酸素14.1％、平均粒径550μの過炭酸ナトリウムを得た。該過炭酸ナトリウムを次に示す試験方法に従って、対ゼオライト安定性を測定したところ、24％であった。
【００１３】
（対ゼオライト安定性の試験方法）
サンプル1.0g（被覆過炭酸ナトリウム0.9gに市販ゼオライト0.1gを混合したもの）を、50ml容プラスチック容器に入れ、蓋（ピンポール付き）をして、50℃、70%RHの条件下に48時間放置した後、有効酸素残存率を次式で求めた。有効酸素の測定は、過マンガン酸カリウム滴定法を用いた。
有効酸素残存率(%)＝（保存後の有効酸素／保存前の有効酸素）×100
【００１４】
実施例１
含水率が10％の湿潤過炭酸ナトリウム5000gと、平均粒径が100μの無水炭酸ナトリウム500gを転動水平式混合機（以下の実施例においては、単に混合機という）に入れ、水118mlを噴霧添加した後、3分間混合した。混合後、内容物を取り出し、流動層乾燥機で乾燥させ、有効酸素12.9％、平均粒径643μの過炭酸ナトリウム粒子を得た。この過炭酸ナトリウムの対ゼオライト安定性は、67.5％であった。
【００１５】
実施例２
含水率が10％の湿潤過炭酸ナトリウム5000gと、平均粒径が20μの無水炭酸ナトリウム500gを混合機に入れ、水118mlを噴霧添加した後、3分間混合した。混合後、内容物を取り出し、流動層乾燥機で乾燥させ、有効酸素12.8％、平均粒径728μの過炭酸ナトリウム粒子を得た。この過炭酸ナトリウムの対ゼオライト安定性は、71％であった。
【００１６】
実施例３
含水率が10％の湿潤過炭酸ナトリウム4986gと、平均粒径が100μの無水炭酸ナトリウム500gを混合機に入れ、そこに3号珪酸ナトリウム43.1gを水94mlに溶解してから添加し、3分間混合した。混合後、内容物を取り出し、流動層乾燥機で乾燥させ、有効酸素12.8％、平均粒径609μの過炭酸ナトリウム粒子を得た。この過炭酸ナトリウムの対ゼオライト安定性は、69.9％であった。
【００１７】
実施例４
含水率が10％の湿潤過炭酸ナトリウム4986gと、平均粒径が20μの無水炭酸ナトリウム500gを混合機に入れ、そこに3号珪酸ナトリウム43.1gを水94mlに溶解してから添加し、3分間混合した。混合後、内容物を取り出し、流動層乾燥機で乾燥させ、有効酸素12.8％、平均粒径699μの過炭酸ナトリウム粒子を得た。この過炭酸ナトリウムの対ゼオライト安定性は、75.7％であった。
【００１８】
実施例５
含水率が10％の湿潤過炭酸ナトリウム4986gと、平均粒径が20μの無水炭酸ナトリウム500gを混合機に入れ、そこに硫酸マグネシウム7水塩25.5gを水41mlに溶解し添加、更に3号珪酸ナトリウム43.1gを水41mlに溶解してから添加し、3分間混合した。混合後、内容物を取り出し、流動層乾燥機で乾燥させ、有効酸素12.5％、平均粒径765μの過炭酸ナトリウム粒子を得た。この過炭酸ナトリウムの対ゼオライト安定性は、82％であった。
【００１９】
実施例６
含水率が12％の湿潤過炭酸ナトリウム5000gと、平均粒径が100μの無水炭酸ナトリウム500gを混合機に入れ、3分間混合した。混合後、内容物を取り出し、流動層乾燥機で乾燥させ、有効酸素12.7％、平均粒径650μの過炭酸ナトリウム粒子を得た。この過炭酸ナトリウムの対ゼオライト安定性は、62.5％であった。
【００２０】
実施例７
含水率が10％の湿潤過炭酸ナトリウム5000gと、平均粒径が100μの無水硫酸ナトリウム500gを混合機に入れ、水118mlを噴霧添加した後、3分間混合した。混合後、内容物を取り出し、流動層乾燥機で乾燥させ、有効酸素12.7％、平均粒径705μの過炭酸ナトリウム粒子を得た。この過炭酸ナトリウムの対ゼオライト安定性は、65％であった。
【００２１】
【発明の効果】
本発明によれば、被覆剤を均一に、しかも効率よく過炭酸ナトリウム粒子表面に被覆でき、かつ乾燥工程が１回で済むため、被覆過炭酸ナトリウムの品質、及び設備面、或いはエネルギー面において有利な過炭酸ナトリウムの被覆方法となる。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a method for producing stable sodium percarbonate. More specifically, the present invention relates to a method for producing sodium percarbonate suitable for blending with a detergent containing zeolite.
[0002]
[Prior art]
Sodium percarbonate is an oxygen-based bleaching agent that can be used for bleaching colored fabrics, does not damage the fabric, and used alone or in combination with detergents.
Detergents containing sodium percarbonate can be bleached at the same time as washing and are useful, but in detergents containing zeolite, sodium percarbonate is unstable and decomposes to lose active oxygen. End up.
Therefore, in general, the sodium percarbonate particles are coated with a certain compound so that the sodium percarbonate particles and the zeolite are not in direct contact with each other. For example, JP-A-59-193999 discloses a method of coating sodium percarbonate with an aqueous solution of sodium metaborate and an alkali metal silicate, and JP-A-7-69606 discloses a silicate, magnesium sulfate, and A method of coating with an aqueous solution of an alkali metal sulfate is disclosed.
[0003]
Since these coating methods are methods in which a coating aqueous solution is sprayed or dripped onto the surface of dried sodium percarbonate particles, (1) a small amount of coating aqueous solution exists on the surface of the sodium percarbonate particles. There is a problem that the permeation into the inside of the sodium percarbonate particles from a small gap and the coating efficiency on the particle surface is reduced. (2) Since the aqueous coating agent solution is sprayed or dripped onto the once dried sodium percarbonate particles, it must be dried again after the coating process, which is a problem in terms of drying equipment and energy consumption. There is.
[0004]
[Problems to be solved by the invention]
As a result of repeated investigations on the above-mentioned drawbacks, that is, coating methods that can uniformly and efficiently coat the coating agent on the surface of the sodium percarbonate particles and have a low energy load in the drying process, The present invention was completed by coating the wet sodium percarbonate particles on the surface of the wet sodium percarbonate particles and then immobilizing the inorganic compound as a hydrate to efficiently form a uniform film.
[0005]
[Means for Solving the Problems]
That is, the present invention mixes wet sodium percarbonate particles with anhydrous sodium carbonate powder or anhydrous sodium sulfate powder having an average particle size of 5 to 200 μm, and the anhydrous compound powder is placed on the surface of the wet sodium percarbonate particles. The present invention relates to a method for producing stable sodium percarbonate, wherein the anhydrous compound is adsorbed and immobilized on a surface of sodium percarbonate particles as a hydrate film of the compound.
[0006]
Further, after mixing wet sodium percarbonate particles with anhydrous sodium carbonate powder or anhydrous sodium sulfate powder having an average particle size of 5 to 200 μm, the anhydrous compound powder is adsorbed on the surface of the wet sodium percarbonate particles. , Spraying or dripping water into the mixed system to fix the anhydrous compound on the surface of the sodium percarbonate as a hydrated film of the compound, thereby producing a stable sodium percarbonate Regarding the method.
The moisture content of the wet sodium percarbonate is 5 to 20%.
Water sprayed or dripped into a mixed system of wet sodium percarbonate particles and anhydrous sodium carbonate powder or anhydrous sodium sulfate powder can be used by dissolving or suspending a silicate or / and magnesium salt.
[0007]
DETAILED DESCRIPTION OF THE INVENTION
The wet sodium percarbonate used in the present invention can be obtained by reacting hydrogen peroxide and sodium carbonate in an aqueous solution and then dehydrating with a dehydrator as it is or with the water content adjusted. It is preferable to use wet sodium percarbonate having a water content of 5 to 20%.
In the present invention, wet sodium percarbonate particles are mixed with anhydrous sodium carbonate powder or anhydrous sodium sulfate powder having a specific particle size, and the anhydrous sodium carbonate or anhydrous sodium sulfate is adsorbed on the surface of the wet sodium percarbonate particles. The average particle diameter of the anhydrous sodium carbonate powder or anhydrous sodium sulfate powder used is preferably 5 to 200 μm, more preferably 5 to 50 μm.
[0008]
For mixing wet sodium percarbonate particles with anhydrous sodium carbonate powder or anhydrous sodium sulfate powder, rolling horizontal mixers, crushing rolling granulators, continuous mixers, etc. can be used. The machine is good.
Silicates and / or magnesium salts can be dissolved or suspended in sprayed or dripped water. Examples of silicates include sodium orthosilicate, sodium sesquisilicate, sodium metasilicate, and water glass. Examples of silicates such as Nos. 1 to 3 include magnesium sulfate and magnesium chloride. In addition, water sprayed or dripped into an aromatic hydrocarbon sulfonate such as sodium benzenesulfonate, sodium p-toluenesulfonate, sodium m-xylenesulfonate, sodium tetraborate, sodium octaborate, sodium pentaborate A known sodium percarbonate coating agent such as borate such as sodium metaborate may be dissolved or suspended.
[0009]
In the present invention, wet sodium percarbonate and anhydrous sodium carbonate powder or anhydrous sodium sulfate powder are added and mixed, but when an aqueous solution of sodium carbonate or aqueous solution of sodium sulfate is added to and mixed with the wet sodium percarbonate, It becomes a state of excessive moisture, so that sodium percarbonate particles are blocked, and drying itself becomes difficult. In the present invention, sodium percarbonate particles do not block.
[0010]
Although the action mechanism of the present invention is not clear, for example, when anhydrous sodium carbonate is used, anhydrous sodium carbonate adsorbed on the surface of wet sodium percarbonate particles is sprayed or dripped into the moisture in the wet sodium percarbonate or into the system. When a sodium carbonate hydrate film is formed on the surface of the sodium percarbonate particles by reacting with the water that is generated, the sodium percarbonate particle surface generates heat due to the reaction, so that the film spreads uniformly on the surface of the sodium percarbonate particles. It is presumed that stable sodium percarbonate can be obtained while being easily fixed and firmly fixed.
[0011]
【Example】
Hereinafter, the present invention will be described with reference to examples.
(Wet sodium percarbonate used in the following examples)
Sodium carbonate and hydrogen peroxide were reacted in an aqueous solution coexisting with sodium chloride and then dehydrated to obtain wet sodium percarbonate having a water content of 10%.
[0012]
Comparative Example 1
The wet sodium percarbonate obtained by the above method was dried to obtain sodium percarbonate having 14.1% effective oxygen and an average particle size of 550 μm. The sodium percarbonate was measured for stability to zeolite according to the following test method and found to be 24%.
[0013]
(Test method for stability to zeolite)
Sample 1.0g (mixed sodium percarbonate 0.9g mixed with commercially available zeolite 0.1g) is put in a 50ml plastic container, covered with a pin pole, and kept under conditions of 50 ℃ and 70% RH for 48 hours. After being allowed to stand, the effective oxygen residual rate was determined by the following formula. The measurement of effective oxygen used the potassium permanganate titration method.
Effective oxygen residual rate (%) = (effective oxygen after storage / effective oxygen before storage) x 100
[0014]
Example 1
Put 5000g of wet sodium percarbonate with a water content of 10% and 500g of anhydrous sodium carbonate with an average particle size of 100μ into a rolling horizontal mixer (simply called a mixer in the following examples) and spray 118ml of water. After addition, mixed for 3 minutes. After mixing, the contents were taken out and dried with a fluidized bed dryer to obtain sodium percarbonate particles having an effective oxygen content of 12.9% and an average particle size of 643 μm. The sodium percarbonate stability to zeolite was 67.5%.
[0015]
Example 2
5000 g of wet sodium percarbonate having a water content of 10% and 500 g of anhydrous sodium carbonate having an average particle diameter of 20 μ were put into a mixer, and 118 ml of water was added by spraying, followed by mixing for 3 minutes. After mixing, the contents were taken out and dried with a fluidized bed dryer to obtain sodium percarbonate particles having an effective oxygen content of 12.8% and an average particle size of 728μ. The sodium percarbonate stability to zeolite was 71%.
[0016]
Example 3
Add 4986 g of wet sodium percarbonate with a water content of 10% and 500 g of anhydrous sodium carbonate with an average particle size of 100μ to a mixer, add 43.1 g of sodium silicate 3 in 94 ml of water, and add for 3 minutes. Mixed. After mixing, the contents were taken out and dried with a fluidized bed dryer to obtain sodium percarbonate particles having an effective oxygen content of 12.8% and an average particle size of 609 μm. The sodium percarbonate stability to zeolite was 69.9%.
[0017]
Example 4
Add 4986 g of wet sodium percarbonate with a water content of 10% and 500 g of anhydrous sodium carbonate with an average particle size of 20μ to a mixer, add 43.1 g of sodium silicate 3 in 94 ml of water and add it for 3 minutes. Mixed. After mixing, the contents were taken out and dried with a fluidized bed dryer to obtain sodium percarbonate particles having an effective oxygen content of 12.8% and an average particle size of 699 μm. The sodium percarbonate stability to zeolite was 75.7%.
[0018]
Example 5
Add 4986 g of wet sodium percarbonate with a water content of 10% and 500 g of anhydrous sodium carbonate with an average particle size of 20μ to a mixer, add 25.5 g of magnesium sulfate heptahydrate in 41 ml of water, and add No. 3 silicic acid. 43.1 g of sodium was dissolved in 41 ml of water and then added and mixed for 3 minutes. After mixing, the contents were taken out and dried with a fluidized bed dryer to obtain sodium percarbonate particles having an effective oxygen content of 12.5% and an average particle size of 765 μm. The sodium percarbonate stability to zeolite was 82%.
[0019]
Example 6
5000 g of wet sodium percarbonate having a water content of 12% and 500 g of anhydrous sodium carbonate having an average particle size of 100 μ were put into a mixer and mixed for 3 minutes. After mixing, the contents were taken out and dried with a fluidized bed dryer to obtain sodium percarbonate particles having an effective oxygen content of 12.7% and an average particle size of 650 μm. The sodium percarbonate stability to zeolite was 62.5%.
[0020]
Example 7
5000 g of wet sodium percarbonate having a water content of 10% and 500 g of anhydrous sodium sulfate having an average particle size of 100 μ were put into a mixer, and 118 ml of water was added by spraying, followed by mixing for 3 minutes. After mixing, the contents were taken out and dried with a fluidized bed dryer to obtain sodium percarbonate particles having an effective oxygen content of 12.7% and an average particle size of 705 μm. The sodium percarbonate stability to zeolite was 65%.
[0021]
【The invention's effect】
According to the present invention, the coating agent can be uniformly and efficiently coated on the surface of the sodium percarbonate particles, and only one drying step is required, which is advantageous in terms of the quality of the coated sodium percarbonate, equipment, and energy. This is a method for coating sodium percarbonate.
Claims (5)
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001352855A JP3975075B2 (en) | 2001-11-19 | 2001-11-19 | Method for producing stable sodium percarbonate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001352855A JP3975075B2 (en) | 2001-11-19 | 2001-11-19 | Method for producing stable sodium percarbonate |
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| Publication Number | Publication Date |
|---|---|
| JP2003146626A JP2003146626A (en) | 2003-05-21 |
| JP3975075B2 true JP3975075B2 (en) | 2007-09-12 |
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| JP2001352855A Expired - Fee Related JP3975075B2 (en) | 2001-11-19 | 2001-11-19 | Method for producing stable sodium percarbonate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008545609A (en) * | 2005-06-01 | 2008-12-18 | ソルヴェイ（ソシエテ アノニム） | Coated sodium percarbonate particles, methods for their production, their use and detergent compositions containing them |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1939276A1 (en) * | 2006-12-29 | 2008-07-02 | Solvay SA | Use of a blend containing percarbonate for detergents and dishwashing formulations |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008545609A (en) * | 2005-06-01 | 2008-12-18 | ソルヴェイ（ソシエテ アノニム） | Coated sodium percarbonate particles, methods for their production, their use and detergent compositions containing them |
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| JP2003146626A (en) | 2003-05-21 |
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