JP6942603B2 - Purified sugar manufacturing equipment and manufacturing method - Google Patents

Purified sugar manufacturing equipment and manufacturing method Download PDF

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JP6942603B2
JP6942603B2 JP2017202557A JP2017202557A JP6942603B2 JP 6942603 B2 JP6942603 B2 JP 6942603B2 JP 2017202557 A JP2017202557 A JP 2017202557A JP 2017202557 A JP2017202557 A JP 2017202557A JP 6942603 B2 JP6942603 B2 JP 6942603B2
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JP2019071862A (en
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英也 八尾
英也 八尾
修大 荻野
修大 荻野
直己 越川
直己 越川
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本発明は、精製糖の製造装置および製造方法に関する。 The present invention relates to an apparatus and a method for producing purified sugar.

蔗糖の精製工程では、通常、サトウキビ等から製造された原料糖を洗糖し、温水に溶解後、石灰と炭酸ガスを加えて形成した炭酸カルシウムの微細結晶に不純物を凝集させる炭酸飽充工程を経て、活性炭やイオン交換樹脂(例えば、特許文献1参照)を用いて脱色を行い、糖液を得る。この脱色された糖液を結晶化して、精製糖を得る。 In the sucrose refining step, a carbonic acid filling step is usually performed in which raw sugar produced from sugar cane or the like is washed, dissolved in warm water, and then impurities are aggregated into fine crystals of calcium carbonate formed by adding lime and carbon dioxide gas. After that, decolorization is performed using activated carbon or an ion exchange resin (see, for example, Patent Document 1) to obtain a sugar solution. This decolorized sugar solution is crystallized to obtain purified sugar.

炭酸飽充工程は、種々の不純物を除去する上で重要な工程であり、蔗糖の精製において必須の工程であるとされている。この炭酸飽充工程では、多量の石灰および炭酸ガスを使用する。炭酸ガスを得るためには燃料を燃焼させる必要があり、エネルギーを多量に消費する。また、通常はボイラー等の排気ガス中の炭酸ガスを利用するが、ボイラー等が稼働していない場合には、炭酸ガスの供給ができない問題がある。炭酸飽充工程では、さらに、石炭のコストや、生じた有機物を含む炭酸カルシウムの多量の廃棄物等が問題となっている。これらの点から、炭酸飽充工程の省略化が望まれている。 The carbonic acid saturation step is an important step in removing various impurities, and is considered to be an indispensable step in the purification of sucrose. This carbon dioxide filling step uses a large amount of lime and carbon dioxide. In order to obtain carbon dioxide, it is necessary to burn fuel, which consumes a large amount of energy. Further, although carbon dioxide gas in the exhaust gas of a boiler or the like is normally used, there is a problem that carbon dioxide gas cannot be supplied when the boiler or the like is not in operation. In the carbonic acid satiation process, the cost of coal and a large amount of waste of calcium carbonate including organic substances generated are further problems. From these points, it is desired to omit the carbonation saturation step.

炭酸飽充工程に代わる方法として、マグネシア吸着剤を用いる方法(例えば、特許文献2参照)も知られているが、原料糖の不純物の除去および脱色に関しては不十分である。 A method using a magnesia adsorbent as an alternative to the carbonic acid saturation step (see, for example, Patent Document 2) is also known, but it is insufficient in removing impurities and decolorizing the raw sugar.

特開2015−136336号公報Japanese Unexamined Patent Publication No. 2015-136336 特開昭61−274787号公報Japanese Unexamined Patent Publication No. 61-274787

本発明の目的は、炭酸飽充工程の省略化が可能であり、炭酸飽充工程を含む精製方法と同等以上の品質で精製糖を得ることができる精製糖の製造装置および製造方法を提供することにある。 An object of the present invention is to provide a refined sugar production apparatus and a production method capable of omitting a carbon dioxide saturation step and obtaining a refined sugar with a quality equal to or higher than that of a purification method including a carbonic acid saturation step. There is.

本発明は、原料糖の溶解液をろ過処理するろ過手段と、得られたろ過液を活性炭で処理する活性炭処理手段と、得られた活性炭処理液を、OH形の強塩基性陰イオン交換樹脂およびH形の弱酸性陽イオン交換樹脂を含むイオン交換樹脂により脱塩処理するイオン交換処理手段と、を備え、前記ろ過手段の前段に、前記溶解液を酸化マグネシウムで処理する酸化マグネシウム処理手段をさらに備え、炭酸飽充を行わない、精製糖の製造装置である。 In the present invention, a filtering means for filtering a solution of raw sugar, an activated charcoal treatment means for treating the obtained filtered liquid with activated charcoal, and an OH-type strongly basic anion exchange resin for treating the obtained activated charcoal liquid are used. And an ion exchange treatment means for desalting with an ion exchange resin containing an H-type weakly acidic cation exchange resin, and a magnesium oxide treatment means for treating the solution with magnesium oxide is provided in front of the filtration means. Further prepared, it is a refined sugar production apparatus that does not perform carbonic acid saturation.

前記精製糖の製造装置において、前記酸化マグネシウムは、比表面積100m/g以上の多孔質酸化マグネシウムであることが好ましい。 In the purified sugar production apparatus, the magnesium oxide is preferably porous magnesium oxide having a specific surface area of 100 m 2 / g or more.

前記精製糖の製造装置において、前記ろ過手段の後段に、得られたろ過液を弱酸性陽イオン交換樹脂により処理してpH6〜8の範囲に調整する弱酸性陽イオン交換処理手段をさらに備えることが好ましい。 In the purified sugar production apparatus, a weakly acidic cation exchange treatment means for treating the obtained filtrate with a weakly acidic cation exchange resin to adjust the pH to a range of 6 to 8 is further provided after the filtering means. Is preferable.

前記精製糖の製造装置において、前記弱酸性陽イオン交換処理手段における前記弱酸性陽イオン交換樹脂の官能基の30〜60モル%が、ナトリウム形およびカリウム形のうちの少なくとも1つであることが好ましい。 In the purified sugar production apparatus, 30 to 60 mol% of the functional groups of the weakly acidic cation exchange resin in the weakly acidic cation exchange treatment means may be at least one of sodium form and potassium form. preferable.

また、本発明は、原料糖の溶解液をろ過処理するろ過工程と、得られたろ過液を活性炭で処理する活性炭処理工程と、得られた活性炭処理液を、OH形の強塩基性陰イオン交換樹脂およびH形の弱酸性陽イオン交換樹脂を含むイオン交換樹脂により脱塩処理するイオン交換処理工程と、を含み、前記ろ過工程の前段に、前記溶解液を酸化マグネシウムで処理する酸化マグネシウム処理工程をさらに含み、炭酸飽充工程を含まない、精製糖の製造方法である。 Further, in the present invention, a filtration step of filtering a solution of raw sugar, an activated charcoal treatment step of treating the obtained filtered solution with activated charcoal, and an OH-type strongly basic anion using the obtained activated charcoal-treated solution are used. the ion exchange resin containing exchange resin and H-shaped weakly acidic cation exchange resin and an ion exchange treatment step of desalting, only contains, in front of the filtration process, magnesium oxide treating the solution with magnesium oxide It is a method for producing a purified sugar , which further includes a treatment step and does not include a carbon dioxide saturation step.

前記精製糖の製造方法において、前記酸化マグネシウムは、比表面積100m/g以上の多孔質酸化マグネシウムであることが好ましい。 In the method for producing purified sugar, the magnesium oxide is preferably porous magnesium oxide having a specific surface area of 100 m 2 / g or more.

前記精製糖の製造方法において、前記ろ過工程の後段に、得られたろ過液を弱酸性陽イオン交換樹脂により処理してpH6〜8の範囲に調整する弱酸性陽イオン交換処理工程をさらに含むことが好ましい。 In the method for producing purified sugar, a weakly acidic cation exchange treatment step of treating the obtained filtrate with a weakly acidic cation exchange resin to adjust the pH to a range of 6 to 8 is further included in the subsequent stage of the filtration step. Is preferable.

前記精製糖の製造方法において、前記弱酸性陽イオン交換処理工程における前記弱酸性陽イオン交換樹脂の官能基の30〜60モル%が、ナトリウム形およびカリウム形のうちの少なくとも1つであることが好ましい。 In the method for producing a purified sugar, 30 to 60 mol% of the functional group of the weakly acidic cation exchange resin in the weakly acidic cation exchange treatment step is at least one of sodium form and potassium form. preferable.

本発明により、炭酸飽充工程の省略化が可能であり、炭酸飽充工程を含む精製方法と同等以上の品質で精製糖を得ることができる。 According to the present invention, the carbonic acid saturation step can be omitted, and the refined sugar can be obtained with a quality equal to or higher than that of the purification method including the carbonic acid saturation step.

本発明の実施形態に係る精製糖の製造装置の一例を示す概略構成図である。It is a schematic block diagram which shows an example of the purified sugar production apparatus which concerns on embodiment of this invention. 本発明の実施形態に係る精製糖の製造装置の他の例を示す概略構成図である。It is a schematic block diagram which shows another example of the refined sugar production apparatus which concerns on embodiment of this invention. 本発明の実施形態に係る精製糖の製造装置の他の例を示す概略構成図である。It is a schematic block diagram which shows another example of the refined sugar production apparatus which concerns on embodiment of this invention.

本発明の実施の形態について以下説明する。本実施形態は本発明を実施する一例であって、本発明は本実施形態に限定されるものではない。 Embodiments of the present invention will be described below. The present embodiment is an example of carrying out the present invention, and the present invention is not limited to the present embodiment.

本発明の実施形態に係る精製糖の製造装置の一例の概略を図1に示し、その構成について説明する。精製糖の製造装置1は、原料糖の溶解液をろ過するろ過手段として、ろ過装置12と、ろ過手段で得られたろ過液を活性炭で処理する活性炭処理手段として、活性炭処理装置14と、活性炭処理手段で得られた活性炭処理液をイオン交換樹脂により脱塩処理するイオン交換処理手段として、イオン交換処理装置16と、を備える。精製糖の製造装置1は、原料糖を溶解して溶解液を得る溶解手段として、溶解槽10と、イオン交換処理手段で得られたイオン交換処理液を結晶化させる結晶化手段として、結晶化装置18とのうち少なくとも1つをさらに備えてもよい。また、イオン交換処理手段で得られたイオン交換処理液を濃縮して液糖を得る濃縮手段として、濃縮装置20をさらに備えてもよい。 An outline of an example of an apparatus for producing purified sugar according to an embodiment of the present invention is shown in FIG. 1, and its configuration will be described. The refined sugar production apparatus 1 includes a filtration apparatus 12 as a filtration means for filtering a solution of raw sugar, an activated carbon treatment apparatus 14 as an activated carbon treatment means for treating the filtrate obtained by the filtration means with activated carbon, and an activated carbon. An ion exchange treatment device 16 is provided as an ion exchange treatment means for desalting the activated carbon treatment liquid obtained by the treatment means with an ion exchange resin. The purified sugar production apparatus 1 is crystallized as a dissolution means for dissolving the raw sugar to obtain a dissolution liquid, and as a crystallization means for crystallizing the ion exchange treatment liquid obtained by the ion exchange treatment means. At least one of the devices 18 may be further provided. Further, a concentrator 20 may be further provided as a concentrating means for concentrating the ion exchange treatment liquid obtained by the ion exchange treatment means to obtain a liquid sugar.

図1の精製糖の製造装置1において、溶解槽10の出口とろ過装置12の入口とは配管22により接続され、ろ過装置12の出口と活性炭処理装置14の入口とは配管24により接続され、活性炭処理装置14の出口とイオン交換処理装置16の入口とは配管26により接続され、イオン交換処理装置16の出口と結晶化装置18の入口とは配管28により接続され、結晶化装置18の出口には配管30が接続されている。配管28から分岐した配管32が濃縮装置20の入口に接続され、濃縮装置20の出口には配管34が接続されている。ろ過装置12と活性炭処理装置14との間にろ過液を貯留するための貯留槽、活性炭処理装置14とイオン交換処理装置16との間に活性炭処理液を貯留するための貯留槽、イオン交換処理装置16と結晶化装置18との間にイオン交換処理液を貯留するための貯留槽等が設けられてもよい。 In the purified sugar production apparatus 1 of FIG. 1, the outlet of the dissolution tank 10 and the inlet of the filtration device 12 are connected by a pipe 22, and the outlet of the filtration device 12 and the inlet of the activated carbon treatment apparatus 14 are connected by a pipe 24. The outlet of the activated carbon treatment device 14 and the inlet of the ion exchange treatment device 16 are connected by a pipe 26, the outlet of the ion exchange treatment device 16 and the inlet of the crystallization device 18 are connected by a pipe 28, and the outlet of the crystallization device 18 is connected. A pipe 30 is connected to the pipe 30. The pipe 32 branched from the pipe 28 is connected to the inlet of the concentrator 20, and the pipe 34 is connected to the outlet of the concentrator 20. A storage tank for storing the filtered liquid between the filtration device 12 and the activated carbon treatment device 14, a storage tank for storing the activated carbon treatment liquid between the activated carbon treatment device 14 and the ion exchange treatment device 16, and an ion exchange treatment. A storage tank or the like for storing the ion exchange treatment liquid may be provided between the device 16 and the crystallization device 18.

本実施形態に係る精製糖の製造方法および精製糖の製造装置1の動作について説明する。 The method for producing purified sugar and the operation of the device 1 for producing purified sugar according to the present embodiment will be described.

原料糖が溶解槽10に供給され、溶解槽10において原料糖が温水等に溶解されて溶解液が得られる(溶解工程)。原料糖の溶解液は、配管22を通してろ過装置12に供給され、ろ過装置12において溶解液のろ過処理が行われる(ろ過工程)。ろ過工程で得られたろ過液は、配管24を通して活性炭処理装置14に供給され、活性炭処理装置14において活性炭で処理される(活性炭処理工程)。活性炭処理工程で得られた活性炭処理液は、配管26を通してイオン交換処理装置16に供給され、イオン交換処理装置16においてイオン交換樹脂により脱塩処理される(イオン交換処理工程)。イオン交換処理工程で得られたイオン交換処理液の少なくとも一部は、配管28を通して結晶化装置18に供給され、結晶化装置18において結晶化が行われる(結晶化工程)。結晶化工程で得られた結晶は精製糖として配管30を通して排出される。一方、イオン交換処理工程で得られたイオン交換処理液の一部または全ては、配管28から分岐した配管32を通して濃縮装置20に供給され、濃縮装置20において濃縮され、液糖とされてもよい(濃縮工程)。濃縮工程で得られた液糖は配管34を通して排出される。濃縮工程で得られた液糖について、必要に応じて、さらに殺菌処理、ろ過処理等が行われてもよい。 The raw sugar is supplied to the dissolution tank 10, and the raw sugar is dissolved in warm water or the like in the dissolution tank 10 to obtain a dissolution liquid (dissolution step). The dissolution liquid of the raw material sugar is supplied to the filtration device 12 through the pipe 22, and the filtration device 12 performs the filtration treatment of the dissolution liquid (filtration step). The filtrate obtained in the filtration step is supplied to the activated carbon treatment device 14 through the pipe 24, and is treated with activated carbon in the activated carbon treatment device 14 (activated carbon treatment step). The activated carbon treatment liquid obtained in the activated carbon treatment step is supplied to the ion exchange treatment device 16 through the pipe 26, and is desalted by the ion exchange resin in the ion exchange treatment device 16 (ion exchange treatment step). At least a part of the ion exchange treatment liquid obtained in the ion exchange treatment step is supplied to the crystallization device 18 through the pipe 28, and crystallization is performed in the crystallization device 18 (crystallization step). The crystals obtained in the crystallization step are discharged as purified sugar through the pipe 30. On the other hand, a part or all of the ion exchange treatment liquid obtained in the ion exchange treatment step may be supplied to the concentrator 20 through the pipe 32 branched from the pipe 28 and concentrated in the concentrator 20 to be a liquid sugar. (Concentration step). The liquid sugar obtained in the concentration step is discharged through the pipe 34. The liquid sugar obtained in the concentration step may be further sterilized, filtered, or the like, if necessary.

本実施形態に係る精製糖の製造方法および精製糖の製造装置により、炭酸飽充工程の省略化が可能であり、炭酸飽充工程を含む精製方法と同等以上の品質で精製糖を得ることができる。炭酸飽充を行わなくても、高品質の精製糖が得られ、炭酸飽充を実施しないことにより、石灰、炭酸ガス等の薬品コスト、エネルギーコスト等の製造コストの削減が可能となる。また、原料糖工場等でボイラー等が稼働しない時期(例えば休糖期)でも精製糖を製造することが可能となる。原料糖を洗糖する洗糖工程の省略化が可能であり、洗糖によるロス分がなくなり、精製の歩留まりが向上する。イオン交換樹脂により脱塩処理することにより、結晶化工程における結晶化効率が高くなり、精製糖の収率向上、品質向上が達成され、精製の歩留まりが向上すると考えられる。 By the method for producing refined sugar and the apparatus for producing refined sugar according to the present embodiment, the carbon dioxide saturation step can be omitted, and the refined sugar can be obtained with a quality equal to or higher than that of the purification method including the carbonic acid saturation step. can. High-quality refined sugar can be obtained without carbon dioxide saturation, and by not performing carbon dioxide saturation, it is possible to reduce the cost of chemicals such as lime and carbon dioxide, and the production cost such as energy cost. Further, it is possible to produce purified sugar even when the boiler or the like does not operate in the raw sugar factory or the like (for example, the sugar rest period). It is possible to omit the sugar washing process of washing the raw sugar, eliminate the loss due to sugar washing, and improve the refining yield. It is considered that the desalting treatment with an ion exchange resin increases the crystallization efficiency in the crystallization step, improves the yield and quality of the purified sugar, and improves the purification yield.

従来の蔗糖の精製方法では、液糖を得るために結晶化した精製糖を再度溶解して、液状にする場合があったが、本実施形態に係る精製糖の製造方法および精製糖の製造装置によれば、イオン交換処理で脱塩処理されるため、イオン交換処理工程で得られたイオン交換処理液を濃縮することにより、高品質の液糖が得られる。 In the conventional method for purifying sucrose, crystallized purified sugar may be re-dissolved to make it liquid in order to obtain liquid sugar. However, the method for producing purified sugar and the apparatus for producing purified sugar according to the present embodiment. According to the above, since the desalting treatment is carried out by the ion exchange treatment, high quality sucrose can be obtained by concentrating the ion exchange treatment liquid obtained in the ion exchange treatment step.

原料糖は、サトウキビ、テンサイ等から製造されたもので、蔗糖(スクロース)を含む。蔗糖は、グルコース(ブドウ糖)とフルクトース(果糖)が結合した二糖類である。 The raw sugar is produced from sugar cane, sugar beet, etc., and contains sucrose. Sucrose is a disaccharide in which glucose (dextrose) and fructose (fructose) are bound.

溶解工程では、溶解槽10において原料糖が水等の溶媒に溶解されて溶解液が得られる。必要に応じて、60〜90℃程度、好ましくは70〜90℃程度に加温してもよい。溶解槽10には、撹拌羽根等の撹拌手段を設けてもよい。水等の溶媒は、例えば、原料糖100重量部に対して40〜100重量部用いればよい。 In the dissolution step, the raw sugar is dissolved in a solvent such as water in the dissolution tank 10 to obtain a dissolution liquid. If necessary, it may be heated to about 60 to 90 ° C., preferably about 70 to 90 ° C. The melting tank 10 may be provided with a stirring means such as a stirring blade. The solvent such as water may be used, for example, 40 to 100 parts by weight with respect to 100 parts by weight of the raw sugar.

溶解工程の後、必要に応じて、pH調整剤により、pH6〜8の範囲に調整してもよい(pH調整工程)。pH調整剤としては、例えば、塩酸等の酸や、炭酸ナトリウム等のアルカリ剤を用いればよい。pH調整は、溶解槽10または配管22において行われてもよいし、溶解槽10とろ過装置12との間にpH調整槽を別途設け、pH調整槽において行われてもよい。 After the dissolution step, if necessary, the pH may be adjusted to the range of 6 to 8 with a pH adjuster (pH adjustment step). As the pH adjuster, for example, an acid such as hydrochloric acid or an alkaline agent such as sodium carbonate may be used. The pH adjustment may be performed in the dissolution tank 10 or the pipe 22, or may be performed in the pH adjustment tank by separately providing a pH adjustment tank between the dissolution tank 10 and the filtration device 12.

ろ過工程では、原料糖の溶解液のろ過処理が行われ、不溶物が除去される。ろ過方法としては、特に制限はないが、例えば、ろ過助材として珪藻土、パーライト等がプレコートされたフィルタを用いてろ過処理を行えばよい。ろ過工程では、例えば、珪藻土等のろ過助材がプレコートされたフィルタに上向流、下向流、横向流で溶解液を通液させればよい。 In the filtration step, the solution of the raw sugar is filtered to remove insoluble matter. The filtration method is not particularly limited, and for example, the filtration treatment may be performed using a filter precoated with diatomaceous earth, pearlite or the like as a filtration aid. In the filtration step, for example, the solution may be passed through a filter precoated with a filtration auxiliary material such as diatomaceous earth by an upward flow, a downward flow, or a lateral flow.

活性炭処理工程では、ろ過工程で得られたろ過液が活性炭で処理されて、主に脱色処理される。活性炭としては、例えば、粒状活性炭、粉状活性炭等が挙げられ、経済性、操作性等の点から粒状活性炭を用いることが好ましい。活性炭処理工程では、例えば、粒状活性炭が充填された充填塔に上向流、下向流でろ過液を通液させればよい。 In the activated carbon treatment step, the filtrate obtained in the filtration step is treated with activated carbon and mainly decolorized. Examples of the activated carbon include granular activated carbon, powdered activated carbon and the like, and it is preferable to use granular activated carbon from the viewpoint of economy, operability and the like. In the activated carbon treatment step, for example, the filtered liquid may be passed through a packed tower filled with granular activated carbon by an upward flow or a downward flow.

粒状活性炭は、体積平均粒径200〜2000μmの活性炭である。粒状活性炭としては、例えば、ダイヤホープMS−10(カルゴンカーボン社製)、NORIT GAC1240(キャボットノリット社製)等を用いることができる。 The granular activated carbon is an activated carbon having a volume average particle diameter of 200 to 2000 μm. As the granular activated carbon, for example, Diahope MS-10 (manufactured by Calgon Carbon Co., Ltd.), NORIT GAC1240 (manufactured by Cabot Norit Co., Ltd.) and the like can be used.

イオン交換処理工程では、活性炭処理工程で得られた活性炭処理液がイオン交換樹脂により脱塩処理される。イオン交換処理工程では、脱色処理を行うこともできる。 In the ion exchange treatment step, the activated carbon treatment liquid obtained in the activated carbon treatment step is desalted with an ion exchange resin. In the ion exchange treatment step, decolorization treatment can also be performed.

イオン交換樹脂としては、OH形等の強塩基性陰イオン交換樹脂、H形等の弱酸性陽イオン交換樹脂等が用いられる。イオン交換処理工程における処理方法としては、例えば、以下の(1)〜(4)の方法が挙げられる。
(1)OH形強塩基性陰イオン交換樹脂の単床塔で処理した後、H形弱酸性陽イオン交換樹脂の単床塔で処理する。
(2)OH形強塩基性陰イオン交換樹脂とH形弱酸性陽イオン交換樹脂とを混合充填した混床塔で処理する。
(3)OH形強塩基性陰イオン交換樹脂の単床塔で処理した後、OH形強塩基性陰イオン交換樹脂とH形弱酸性陽イオン交換樹脂とを混合充填した混床塔で処理する。
(4)OH形強塩基性陰イオン交換樹脂とナトリウム(Na)形またはカリウム(K)形陽イオン交換樹脂とを混合充填または複層床とした第1塔と、OH形強塩基性陰イオン交換樹脂とH形弱酸性陽イオン交換樹脂とを混合充填した混床塔(第2塔)で処理する。
As the ion exchange resin, a strong basic anion exchange resin such as OH type, a weakly acidic cation exchange resin such as H type, and the like are used. Examples of the treatment method in the ion exchange treatment step include the following methods (1) to (4).
(1) After treatment with a single bed tower of an OH type strongly basic anion exchange resin, treatment is performed with a single bed tower of an H type weakly acidic cation exchange resin.
(2) The treatment is carried out in a mixed bed tower in which an OH-type strong basic anion exchange resin and an H-type weakly acidic cation exchange resin are mixed and filled.
(3) After treating with a single bed tower of OH type strongly basic anion exchange resin, it is treated with a mixed bed tower in which OH type strongly basic anion exchange resin and H type weakly acidic cation exchange resin are mixed and filled. ..
(4) The first column in which an OH-type strong basic anion exchange resin and a sodium (Na) -type or potassium (K) -type cation exchange resin are mixed and filled or made into a multi-layer bed, and an OH-type strong basic anion. The treatment is carried out in a mixed bed tower (second tower) in which the exchange resin and the H-type weakly acidic cation exchange resin are mixed and filled.

これらのうち、処理液の品質等の点から(4)の処理方法が好ましい。後述する、図3の精製糖の製造装置5のように、酸化マグネシウム処理液のろ過液を弱酸性陽イオン交換処理する場合には、(3)の処理方法でもよい。 Of these, the treatment method (4) is preferable from the viewpoint of the quality of the treatment liquid and the like. When the filtered solution of the magnesium oxide-treated solution is subjected to a weakly acidic cation exchange treatment as in the purified sugar production apparatus 5 of FIG. 3, which will be described later, the treatment method of (3) may be used.

OH形強塩基性陰イオン交換樹脂としては、アクリル系のOH形強塩基性陰イオン交換樹脂、スチレン系のOH形強塩基性陰イオン交換樹脂等が挙げられる。アクリル系のOH形強塩基性陰イオン交換樹脂としては、例えば、アンバーライト(登録商標、以下同様))IRA958、IRA458RF(ダウケミカル社製)、PUROLITE(登録商標、以下同様)A860、A850(ピュロライト社製)等が挙げられる。アクリル系のOH形強塩基性陰イオン交換樹脂のうち、特にゲル型樹脂は、交換容量が大きく、処理できる蔗糖溶液の量が多くなることから有利である。ゲル型アクリル系強塩基性陰イオン交換樹脂としては、アンバーライト IRA458RF(ダウケミカル社製)、PUROLITE A850(ピュロライト社製)等が挙げられる。 Examples of the OH-type strongly basic anion exchange resin include an acrylic-based OH-type strongly basic anion exchange resin and a styrene-based OH-type strongly basic anion exchange resin. Examples of acrylic OH-type strongly basic anion exchange resins include Amberlite (registered trademark, the same applies hereinafter) IRA958, IRA458RF (manufactured by Dow Chemical Co., Ltd.), PUROLITE (registered trademark, the same applies hereinafter) A860, A850 (Purolite). (Manufactured by the company) and the like. Among the acrylic OH-type strong basic anion exchange resins, the gel type resin is particularly advantageous because it has a large exchange capacity and the amount of sucrose solution that can be treated is large. Examples of the gel-type acrylic strongly basic anion exchange resin include Amberlite IRA458RF (manufactured by Dow Chemical Co., Ltd.) and PUROLITE A850 (manufactured by Purolite Co., Ltd.).

スチレン系のOH形強塩基性陰イオン交換樹脂としては、例えば、アンバーライト IRA900J、IRA402、IRA402BL(ダウケミカル社製)、PUROLITE A500S(ピュロライト社製)、ダイヤイオン(登録商標、以下同様) SA10A、PA308(三菱ケミカル社製)等が挙げられる。 Examples of the styrene-based OH-type strongly basic anion exchange resin include Amberlite IRA900J, IRA402, IRA402BL (manufactured by Dow Chemical Corporation), PUROLITE A500S (manufactured by Purolite Co., Ltd.), Diaion (registered trademark, the same applies hereinafter) SA10A, Examples include PA308 (manufactured by Mitsubishi Chemical Corporation).

H形弱酸性陽イオン交換樹脂としては、例えば、アンバーライト IRC76、ダウエックス(登録商標、以下同様)MAC−3(ダウケミカル社製)、PUROLITE C115E(ピュロライト社製)、ダイヤイオン WK10、WK11(三菱ケミカル社製)等が挙げられる。 Examples of the H-type weakly acidic cation exchange resin include Amberlite IRC76, Dowex (registered trademark, the same applies hereinafter) MAC-3 (manufactured by Dow Chemical Corporation), PUROLITE C115E (manufactured by Purolite), Diaion WK10, WK11 (manufactured by Purolite). Mitsubishi Chemical Corporation) and the like.

Na形またはK形陽イオン交換樹脂は、強酸性陽イオン交換樹脂であっても、弱酸性陽イオン交換樹脂であってもよい。Na形強酸性陽イオン交換樹脂としては、例えば、アンバーライト IR120B Na、IR124 Na、200CT Na、252 Na、アンバーレックス100(ダウケミカル社製)、ダイヤイオン SK1B、PK216(三菱ケミカル社製)、PUROLITE C100E(ピュロライト社製)等が挙げられる。また、公知のH形強酸性陽イオン交換樹脂をNaOHやKOH等の再生剤で再生させることによって、Na形またはK形強酸性陽イオン交換樹脂に変換したものを用いてもよい。同様に、公知のH形弱酸性陽イオン交換樹脂をNaOHやKOH等の再生剤で再生させることによって、Na形またはK形弱酸性陽イオン交換樹脂に変換したものを用いてもよい。 The Na-type or K-type cation exchange resin may be a strongly acidic cation exchange resin or a weakly acidic cation exchange resin. Examples of the Na-type strong acid cation exchange resin include Amberlite IR120B Na, IR124 Na, 200CT Na, 252 Na, Amberlex 100 (manufactured by Dow Chemical Corporation), Diaion SK1B, PK216 (manufactured by Mitsubishi Chemical Corporation), and PUROLITE. Examples include C100E (manufactured by Purolite). Alternatively, a known H-type strong acid cation exchange resin converted into a Na-type or K-type strong acid cation exchange resin by regenerating it with a regenerating agent such as NaOH or KOH may be used. Similarly, a known H-type weakly acidic cation exchange resin may be converted into a Na-type or K-type weakly acidic cation exchange resin by regenerating it with a regenerating agent such as NaOH or KOH.

結晶化工程では、イオン交換処理工程で得られたイオン交換処理液の少なくとも一部について結晶化が行われ、精製糖が得られる。結晶化は、例えば、イオン交換処理液を減圧下で40〜80℃に加熱、濃縮することによって行われる。通常は、濃縮の際に蔗糖の結晶の核を加える。 In the crystallization step, at least a part of the ion exchange treatment liquid obtained in the ion exchange treatment step is crystallized to obtain purified sugar. Crystallization is carried out, for example, by heating and concentrating the ion exchange treatment liquid at 40 to 80 ° C. under reduced pressure. Usually, sucrose crystal nuclei are added during concentration.

濃縮工程では、イオン交換処理工程で得られたイオン交換処理液の一部または全てについて濃縮され、液糖が得られる。濃縮は、例えば、イオン交換処理液を40〜80℃に加熱、濃縮することによって行われる。 In the concentration step, a part or all of the ion exchange treatment liquid obtained in the ion exchange treatment step is concentrated to obtain a liquid sugar. Concentration is performed, for example, by heating and concentrating the ion exchange treatment liquid at 40 to 80 ° C.

本実施形態に係る精製糖の製造方法により、例えば色価600I.U.以上の原料糖から、色価を30I.U.以下まで、好ましくは20I.U.以下まで低減した精製糖を得ることができる。 According to the method for producing purified sugar according to the present embodiment, for example, a color value of 600 I. U.S. From the above raw sugars, the color value was set to 30 I. U.S. To the following, preferably 20 I. U.S. Purified sugar reduced to the following can be obtained.

本実施形態に係る精製糖の製造方法および精製糖の製造装置では、ろ過手段によるろ過処理工程の前段において、酸化マグネシウム処理手段を設けて、原料糖の溶解液を酸化マグネシウムで処理してもよい。 In the method for producing purified sugar and the apparatus for producing purified sugar according to the present embodiment, a magnesium oxide treatment means may be provided in the first stage of the filtration treatment step by the filtration means, and the solution of the raw sugar may be treated with magnesium oxide. ..

図2の精製糖の製造装置3は、図1の精製糖の製造装置1の構成に加えて、ろ過装置12の前段、すなわち溶解槽10とろ過装置12との間に、原料糖の溶解液を酸化マグネシウムで処理する酸化マグネシウム処理手段として、酸化マグネシウム処理装置36をさらに備える。図2の精製糖の製造装置3において、溶解槽10の出口と酸化マグネシウム処理装置36の入口とは配管38により接続され、酸化マグネシウム処理装置36の出口とろ過装置12の入口とは配管40により接続されている。 In addition to the configuration of the purified sugar producing apparatus 1 of FIG. 1, the purified sugar producing apparatus 3 of FIG. As a magnesium oxide treatment means for treating magnesium oxide, a magnesium oxide treatment device 36 is further provided. In the purified sugar production apparatus 3 of FIG. 2, the outlet of the dissolution tank 10 and the inlet of the magnesium oxide treatment device 36 are connected by a pipe 38, and the outlet of the magnesium oxide treatment device 36 and the inlet of the filtration device 12 are connected by a pipe 40. It is connected.

図2の精製糖の製造装置3では、原料糖が溶解槽10に供給され、溶解槽10において原料糖が温水等に溶解されて溶解液が得られる(溶解工程)。原料糖の溶解液は、配管38を通して酸化マグネシウム処理装置36に供給され、酸化マグネシウム処理装置36において溶解液の酸化マグネシウム処理が行われる(酸化マグネシウム処理工程)。酸化マグネシウム処理工程で得られた酸化マグネシウム処理液は、配管40を通してろ過装置12に供給され、ろ過装置12において酸化マグネシウム処理液のろ過処理が行われる(ろ過工程)。ろ過工程の後、必要に応じて、pH調整剤により、pH6〜8の範囲に調整してもよい(pH調整工程)。pH調整剤としては、例えば、塩酸等の酸や、炭酸ナトリウム等のアルカリ剤を用いればよい。pH調整は、配管24において行われてもよいし、ろ過装置12と活性炭処理装置14との間にpH調整槽を別途設け、pH調整槽において行われてもよい。以降、図1の精製糖の製造装置1と同様にして、活性炭処理工程、イオン交換処理工程、結晶化工程、必要に応じて濃縮工程が行われる。 In the purified sugar production apparatus 3 of FIG. 2, the raw sugar is supplied to the dissolution tank 10, and the raw sugar is dissolved in warm water or the like in the dissolution tank 10 to obtain a dissolution liquid (dissolution step). The solution of the raw sugar is supplied to the magnesium oxide treatment device 36 through the pipe 38, and the magnesium oxide treatment of the solution is performed in the magnesium oxide treatment device 36 (magnesium oxide treatment step). The magnesium oxide-treated liquid obtained in the magnesium oxide treatment step is supplied to the filtration device 12 through the pipe 40, and the magnesium oxide-treated liquid is filtered in the filtration device 12 (filtration step). After the filtration step, if necessary, the pH may be adjusted to the range of 6 to 8 with a pH adjuster (pH adjustment step). As the pH adjuster, for example, an acid such as hydrochloric acid or an alkaline agent such as sodium carbonate may be used. The pH adjustment may be performed in the pipe 24, or may be performed in the pH adjustment tank by separately providing a pH adjustment tank between the filtration device 12 and the activated carbon treatment device 14. After that, in the same manner as in the refined sugar production apparatus 1 of FIG. 1, an activated carbon treatment step, an ion exchange treatment step, a crystallization step, and a concentration step if necessary are performed.

酸化マグネシウム処理を行うことにより、原料糖の品質が低い場合(例えば、色価1000I.U.以上)であっても不純物がより除去されて高品質の精製糖が得られる。原料糖の品質が高い場合(例えば、色価800I.U.未満)には、酸化マグネシウム処理は行わなくてもよい。 By performing the magnesium oxide treatment, impurities are further removed even when the quality of the raw sugar is low (for example, a color value of 1000 IU or more), and a high quality purified sugar can be obtained. When the quality of the raw sugar is high (for example, the color value is less than 800 IU), the magnesium oxide treatment may not be performed.

酸化マグネシウムとしては、粉末状の酸化マグネシウム、多孔質の酸化マグネシウム等が挙げられ、多孔質の酸化マグネシウムを用いることが好ましい。多孔質の酸化マグネシウムの比表面積は、100m/g以上であることが好ましく、120m/g以上であることがより好ましい。酸化マグネシウムの比表面積が100m/g未満であると、不純物の除去効果が低い場合がある。酸化マグネシウムの比表面積の上限は、製造できる範囲で、かつ強度が保てる範囲で高ければ高いほどよい。 Examples of magnesium oxide include powdered magnesium oxide and porous magnesium oxide, and it is preferable to use porous magnesium oxide. The specific surface area of the porous magnesium oxide is preferably 100 m 2 / g or more, and more preferably 120 m 2 / g or more. If the specific surface area of magnesium oxide is less than 100 m 2 / g, the effect of removing impurities may be low. The upper limit of the specific surface area of magnesium oxide is the higher as long as it can be produced and the strength can be maintained.

ろ過手段によるろ過工程の後段において、弱酸性陽イオン交換処理手段を設けて、ろ過工程で得られたろ過液を弱酸性陽イオン交換樹脂により処理してpH6〜8の範囲に調整してもよい(弱酸性陽イオン交換処理手段)。 In the latter stage of the filtration step by the filtration means, a weakly acidic cation exchange treatment means may be provided, and the filtrate obtained in the filtration step may be treated with a weakly acidic cation exchange resin to adjust the pH to the range of 6 to 8. (Weakly acidic cation exchange treatment means).

図3の精製糖の製造装置5は、図2の精製糖の製造装置3の構成に加えて、ろ過装置12の後段、すなわちろ過装置12と活性炭処理装置14との間に、ろ過工程で得られたろ過液を弱酸性陽イオン交換樹脂により処理してpH6〜8の範囲に調整する弱酸性陽イオン交換処理手段として、弱酸性陽イオン交換処理装置42をさらに備える。図3の精製糖の製造装置5において、ろ過装置12の出口と弱酸性陽イオン交換処理装置42の入口とは配管44により接続され、弱酸性陽イオン交換処理装置42の出口と活性炭処理装置14の入口とは配管46により接続されている。ろ過装置12と弱酸性陽イオン交換処理装置42との間にろ過液を貯留するための貯留槽、弱酸性陽イオン交換処理装置42と活性炭処理装置14との間に弱酸性陽イオン交換処理液を貯留するための貯留槽等が設けられてもよい。なお、図1の精製糖の製造装置1の構成に加えて、ろ過装置12の後段、すなわちろ過装置12と活性炭処理装置14との間に、ろ過工程で得られたろ過液を弱酸性陽イオン交換樹脂により処理してpH6〜8の範囲に調整する弱酸性陽イオン交換処理手段として、弱酸性陽イオン交換処理装置42をさらに備えてもよい。 The refined sugar production apparatus 5 of FIG. 3 is obtained in a filtration step in the latter stage of the filtration apparatus 12, that is, between the filtration apparatus 12 and the activated carbon treatment apparatus 14, in addition to the configuration of the refined sugar production apparatus 3 of FIG. A weakly acidic cation exchange treatment device 42 is further provided as a weakly acidic cation exchange treatment means for treating the obtained filtrate with a weakly acidic cation exchange resin to adjust the pH to a range of 6 to 8. In the purified sugar production apparatus 5 of FIG. 3, the outlet of the filtration apparatus 12 and the inlet of the weakly acidic cation exchange processing apparatus 42 are connected by a pipe 44, and the outlet of the weakly acidic cation exchange processing apparatus 42 and the activated charcoal processing apparatus 14 are connected. Is connected to the entrance of the pipe 46 by a pipe 46. A storage tank for storing the filtrate between the filtration device 12 and the weakly acidic cation exchange treatment device 42, and a weakly acidic cation exchange treatment liquid between the weakly acidic cation exchange treatment device 42 and the activated charcoal treatment device 14. A storage tank or the like for storing the water may be provided. In addition to the configuration of the purified sugar production device 1 in FIG. 1, a weakly acidic cation is used to transfer the filtrate obtained in the filtration step to the latter stage of the filtration device 12, that is, between the filtration device 12 and the activated carbon treatment device 14. A weakly acidic cation exchange treatment device 42 may be further provided as a weakly acidic cation exchange treatment means for treating with an exchange resin and adjusting the pH to a range of 6 to 8.

図3の精製糖の製造装置5では、原料糖が溶解槽10に供給され、溶解槽10において原料糖が温水等に溶解されて溶解液が得られる(溶解工程)。原料糖の溶解液は、配管38を通して酸化マグネシウム処理装置36に供給され、酸化マグネシウム処理装置36において溶解液の酸化マグネシウム処理が行われる(酸化マグネシウム処理工程)。酸化マグネシウム処理工程で得られた酸化マグネシウム処理液は、配管40を通してろ過装置12に供給され、ろ過装置12において酸化マグネシウム処理液のろ過処理が行われる(ろ過工程)。ろ過工程で得られたろ過液は、配管44を通して弱酸性陽イオン交換処理装置42に供給され、弱酸性陽イオン交換処理装置42においてろ過液の弱酸性陽イオン交換処理が行われる(弱酸性陽イオン交換処理工程)。弱酸性陽イオン交換処理工程で得られた弱酸性陽イオン交換処理液は、配管46を通して活性炭処理装置14に供給され、活性炭処理装置14において弱酸性陽イオン交換処理液の活性炭処理が行われる(活性炭処理工程)。以降、図1の精製糖の製造装置1と同様にして、イオン交換処理工程、結晶化工程、必要に応じて濃縮工程が行われる。 In the purified sugar manufacturing apparatus 5 of FIG. 3, the raw sugar is supplied to the dissolution tank 10, and the raw sugar is dissolved in warm water or the like in the dissolution tank 10 to obtain a dissolution liquid (dissolution step). The solution of the raw sugar is supplied to the magnesium oxide treatment device 36 through the pipe 38, and the magnesium oxide treatment of the solution is performed in the magnesium oxide treatment device 36 (magnesium oxide treatment step). The magnesium oxide-treated liquid obtained in the magnesium oxide treatment step is supplied to the filtration device 12 through the pipe 40, and the magnesium oxide-treated liquid is filtered in the filtration device 12 (filtration step). The filtrate obtained in the filtration step is supplied to the weakly acidic cation exchange treatment device 42 through the pipe 44, and the weakly acidic cation exchange treatment of the filtrate is performed in the weakly acidic cation exchange treatment device 42 (weakly acidic cations). Ion exchange processing process). The weakly acidic cation exchange treatment liquid obtained in the weakly acidic cation exchange treatment step is supplied to the activated carbon treatment apparatus 14 through the pipe 46, and the activated carbon treatment of the weakly acidic cation exchange treatment liquid is performed in the activated carbon treatment apparatus 14 ( Activated carbon treatment process). After that, the ion exchange treatment step, the crystallization step, and if necessary, the concentration step are performed in the same manner as in the purified sugar production apparatus 1 of FIG.

酸化マグネシウム処理液について弱酸性陽イオン交換処理を行うことによって、容易にpH6〜8の範囲に調整することができ、酸を加えないため、糖液中の塩濃度が増えないという利点がある。さらに糖液中のMg、Ca等の硬度成分がNa、Kと交換され、後工程における設備へのスケーリングを抑制することができる。 By performing a weakly acidic cation exchange treatment on the magnesium oxide-treated solution, the pH can be easily adjusted to the range of 6 to 8, and since no acid is added, there is an advantage that the salt concentration in the sugar solution does not increase. Further, hardness components such as Mg and Ca in the sugar solution are exchanged for Na and K, and scaling to equipment in the subsequent process can be suppressed.

弱酸性陽イオン交換樹脂としては、例えば、アンバーライト IRC76、ダウエックス(登録商標、以下同様)MAC−3(ダウケミカル社製)、PUROLITE C115E(ピュロライト社製)、ダイヤイオン WK10、WK11(三菱ケミカル社製)等のH形弱酸性陽イオン交換樹脂を用いることができる。 Examples of the weakly acidic cation exchange resin include Amberlite IRC76, Dowex (registered trademark, the same applies hereinafter) MAC-3 (manufactured by Dow Chemical Co., Ltd.), PUROLITE C115E (manufactured by Purolite Co., Ltd.), Diaion WK10, WK11 (Mitsubishi Chemical Co., Ltd.). H-type weakly acidic cation exchange resin such as (manufactured by the company) can be used.

弱酸性陽イオン交換処理装置42で用いられる弱酸性陽イオン交換樹脂の官能基の30〜60モル%が、ナトリウム形およびカリウム形のうちの少なくとも1つであることが好ましく、40〜50モル%が、ナトリウム形およびカリウム形のうちの少なくとも1つであることがより好ましい。なお、残りの官能基は、H形である。弱酸性陽イオン交換樹脂の官能基の30〜60モル%が、ナトリウム形およびカリウム形のうちの少なくとも1つであることにより、酸化マグネシウム処理液のpHを6〜8の範囲に調整しやすくなる。弱酸性陽イオン交換樹脂の官能基の30モル%未満がナトリウム形およびカリウム形のうちの少なくとも1つであると、pHが6未満となる場合があり、60モル%を超えてナトリウム形およびカリウム形のうちの少なくとも1つであると、pHが8を超える場合がある。 It is preferable that 30 to 60 mol% of the functional group of the weakly acidic cation exchange resin used in the weakly acidic cation exchange processing apparatus 42 is at least one of sodium form and potassium form, and 40 to 50 mol%. Is more preferably at least one of the sodium and potassium forms. The remaining functional groups are H-type. When 30 to 60 mol% of the functional group of the weakly acidic cation exchange resin is at least one of the sodium form and the potassium form, it becomes easy to adjust the pH of the magnesium oxide treatment solution in the range of 6 to 8. .. If less than 30 mol% of the functional groups of the weakly acidic cation exchange resin are at least one of the sodium and potassium forms, the pH can be less than 6, and more than 60 mol% of the sodium and potassium forms. At least one of the forms may have a pH greater than 8.

イオン交換処理手段によるイオン交換処理工程の後段において、第2活性炭処理手段を設けて、イオン交換処理液を活性炭で処理してもよい(第2活性炭処理工程)。第2活性炭処理工程で用いられる活性炭としては、例えば、粒状活性炭、粉状活性炭等が挙げられ、粒状活性炭を用いることが好ましい。第2活性炭処理工程では、例えば、粒状活性炭が充填された充填塔に上向流、下向流でイオン交換処理液を通液させればよい。イオン交換処理液を活性炭で処理することにより、さらに不純物を除去することができ、より色価を低減することができる。 In the latter stage of the ion exchange treatment step by the ion exchange treatment means, a second activated carbon treatment means may be provided to treat the ion exchange treatment liquid with activated carbon (second activated carbon treatment step). Examples of the activated carbon used in the second activated carbon treatment step include granular activated carbon and powdered activated carbon, and it is preferable to use granular activated carbon. In the second activated carbon treatment step, for example, the ion exchange treatment liquid may be passed through a packed bed filled with granular activated carbon by an upward flow and a downward flow. By treating the ion exchange treatment liquid with activated carbon, impurities can be further removed and the color value can be further reduced.

以下、実施例および比較例を挙げ、本発明をより具体的に詳細に説明するが、本発明は、以下の実施例に限定されるものではない。 Hereinafter, the present invention will be described in more detail with reference to Examples and Comparative Examples, but the present invention is not limited to the following Examples.

<実施例1〜3>
表1に示す品質の原料糖を用いて、図1に示す精製糖の製造装置1を用いて、精製処理を行った。
<Examples 1 to 3>
Using the raw sugars of the quality shown in Table 1, the purification treatment was carried out using the refined sugar production apparatus 1 shown in FIG.

原料糖を70℃の温水に溶解し、炭酸ナトリウムを加えて、pH7.5に調整した。珪藻土を用いてろ過処理を行い、粒状活性炭(ダイヤホープ MS−10、カルゴンカーボン社製)を充填したカラムに通液した。得られた活性炭処理液について、OH形強塩基性陰イオン交換樹脂(アンバーライトIRA458RF、ダウケミカル社製)とナトリウム(Na)形またはカリウム(K)形陽イオン交換樹脂(アンバーレックス100、ダウケミカル社製)とを複層床とした第1塔と、OH形強塩基性陰イオン交換樹脂(IRA900J、ダウケミカル社製)とH形弱酸性陽イオン交換樹脂(アンバーライトIRC76、ダウケミカル社製)とを混合充填した混床塔(第2塔)で脱塩処理した。 The raw sugar was dissolved in warm water at 70 ° C. and sodium carbonate was added to adjust the pH to 7.5. Filtration treatment was performed using diatomaceous earth, and the liquid was passed through a column packed with granular activated carbon (Diahope MS-10, manufactured by Calgon Carbon Co., Ltd.). Regarding the obtained activated carbon treatment liquid, OH type strongly basic anion exchange resin (Amberlite IRA458RF, manufactured by Dow Chemical Co., Ltd.) and sodium (Na) type or potassium (K) type cation exchange resin (Amberlex 100, Dow Chemical Co., Ltd.) OH type strongly basic anion exchange resin (IRA900J, manufactured by Dow Chemical Co., Ltd.) and H type weakly acidic cation exchange resin (Amberlite IRC76, manufactured by Dow Chemical Co., Ltd.) ) Was mixed and filled in a mixed bed tower (second tower) for desalting.

溶解液、活性炭処理入口、活性炭処理出口、イオン交換処理出口において、各液のBrix(%)、pH、導電率(μS/cm)、灰分(%)、色価(I.U.)を測定した。糖度を表すBrix(%)は、デジタル屈折計(アタゴ製、RX−5000i)を用いて測定した。pHは、pH測定装置(TOA−DKK製、HM−26S)を用いて測定した。導電率(μS/cm)は、導電率測定装置(横河電機製、SC−72)を用いて測定した。灰分(%)は、導電率の測定値からICUMSA法により算出した。色価(I.U.)は、ICUMSA法に従い、糖液の吸光度を、分光光度計(日立製作所製、U−3010)を用いて測定し、算出した。結果を表2,3,4にそれぞれ示す。 Brix (%), pH, conductivity (μS / cm), ash content (%), and color value (I.U.) of each liquid were measured at the dissolution liquid, the activated carbon treatment inlet, the activated carbon treatment outlet, and the ion exchange treatment outlet. bottom. Brix (%) representing the sugar content was measured using a digital refractometer (manufactured by Atago, RX-5000i). The pH was measured using a pH measuring device (manufactured by TOA-DKK, HM-26S). The conductivity (μS / cm) was measured using a conductivity measuring device (manufactured by Yokogawa Electric, SC-72). The ash content (%) was calculated by the ICUMSA method from the measured value of conductivity. The color value (I.U.) was calculated by measuring the absorbance of the sugar solution using a spectrophotometer (U-3010, manufactured by Hitachi, Ltd.) according to the ICUMSA method. The results are shown in Tables 2, 3 and 4, respectively.

Figure 0006942603
Figure 0006942603

Figure 0006942603
Figure 0006942603

Figure 0006942603
Figure 0006942603

Figure 0006942603
Figure 0006942603

<比較例1>
表1に示す実施例1の原料糖を用いて、従来の炭酸飽充工程を含むイオン交換樹脂による脱塩、脱色の方法で精製処理を行った。結果を表5にそれぞれ示す。
<Comparative example 1>
Using the raw sugar of Example 1 shown in Table 1, purification treatment was carried out by a method of desalting and decoloring with an ion exchange resin including a conventional carbonic acid saturation step. The results are shown in Table 5, respectively.

Figure 0006942603
Figure 0006942603

このように、実施例の方法および装置により、炭酸飽充工程の省略化が可能であり、炭酸飽充工程を含む精製方法と同等以上の品質で精製糖を得ることができた。 As described above, the method and apparatus of the examples made it possible to omit the carbonic acid saturation step, and it was possible to obtain the refined sugar with a quality equal to or higher than that of the purification method including the carbonic acid saturation step.

<参考実験1〜3>
酸化マグネシウム粉末(UC−95ST、宇部マテリアルズ株式会社製)、水酸化マグネシウム粉末(UD−650−1、宇部マテリアルズ株式会社製)、多孔質酸化マグネシウム(UCM−150、宇部マテリアルズ株式会社製)を用いて、原料糖の溶解液と接触させ、色価の低減効果を確認した(参考実験1)。
<Reference experiments 1-3>
Magnesium oxide powder (UC-95ST, manufactured by Ube Material Industries Ltd.), magnesium hydroxide powder (UD-650-1, manufactured by Ube Material Industries Ltd.), porous magnesium oxide (UCM-150, manufactured by Ube Material Industries Ltd.) ) Was used to bring it into contact with the solution of the raw sugar, and the effect of reducing the color value was confirmed (reference experiment 1).

(実験方法)
表1の実施例2の原料糖に70℃の温水を加えて溶解した溶解液を用い、添加剤をそれぞれ1000mg/L添加し、70℃で1分間撹拌後、珪藻土を用いてろ過処理を行い、炭酸ナトリウムを加えてpH7.0に調整後、色価を測定した。結果を表6に示す。
(experimental method)
Using a solution prepared by adding warm water at 70 ° C to the raw sugar of Example 2 in Table 1, 1000 mg / L of each additive was added, and the mixture was stirred at 70 ° C for 1 minute and then filtered using diatomaceous earth. , Sodium carbonate was added to adjust the pH to 7.0, and then the color value was measured. The results are shown in Table 6.

Figure 0006942603
Figure 0006942603

酸化マグネシウム粉末や多孔質酸化マグネシウムを用いることにより、原料糖の溶解液の色価を低減することができ、特に多孔質酸化マグネシウムを用いることにより、原料糖の溶解液の色価を顕著に低減することができた。 By using magnesium oxide powder or porous magnesium oxide, the color value of the solution of raw sugar can be reduced, and in particular, by using porous magnesium oxide, the color value of the solution of raw sugar is significantly reduced. We were able to.

<実施例4>
表1の実施例2の原料糖を用いて、図2に示す精製糖の製造装置3を用いて、精製処理を行った。
<Example 4>
Using the raw sugar of Example 2 in Table 1, a purification treatment was carried out using the refined sugar production apparatus 3 shown in FIG.

原料糖を70℃の温水に溶解し、多孔質酸化マグネシウム(UCM−150、宇部マテリアルズ株式会社製)を250mg/L添加し、70℃で1分間撹拌後、珪藻土を用いてろ過処理を行い、塩酸を加えて、pH7.5に調整した。粒状活性炭(ダイヤホープ MS−10)を充填したカラムに通液した。得られた活性炭処理液について、実施例2と同様にしてイオン交換樹脂により脱塩処理した。 The raw sugar is dissolved in warm water at 70 ° C., 250 mg / L of porous magnesium oxide (UCM-150, manufactured by Ube Material Industries Ltd.) is added, the mixture is stirred at 70 ° C. for 1 minute, and then filtered using diatomaceous earth. , Hydrochloric acid was added to adjust the pH to 7.5. The liquid was passed through a column packed with granular activated carbon (Diahope MS-10). The obtained activated carbon treatment liquid was desalted with an ion exchange resin in the same manner as in Example 2.

実施例2と同様にして、溶解液、酸化マグネシウム工程処理液中和後(活性炭処理入口)、活性炭処理出口、イオン交換処理出口において、Brix(%)、pH、導電率(μS/cm)、灰分(%)、色価(I.U.)を測定した。結果を表7にそれぞれ示す。 In the same manner as in Example 2, after neutralization of the solution and the magnesium oxide step treatment liquid (activated carbon treatment inlet), at the activated carbon treatment outlet and the ion exchange treatment outlet, Brix (%), pH, conductivity (μS / cm), The ash content (%) and the color value (IU) were measured. The results are shown in Table 7, respectively.

Figure 0006942603
Figure 0006942603

実施例4の結果(表7)と実施例2の結果(表3)とを比較すると、多孔質酸化マグネシウムを用いることにより、原料糖の溶解液の色価を顕著に低減することがわかった。 Comparing the results of Example 4 (Table 7) with the results of Example 2 (Table 3), it was found that the use of porous magnesium oxide significantly reduced the color value of the solution of the raw sugar. ..

<実施例5>
表1の実施例2の原料糖を用いて、図3に示す精製糖の製造装置5を用いて、精製処理を行った。
<Example 5>
Using the raw sugar of Example 2 in Table 1, a purification treatment was carried out using the refined sugar production apparatus 5 shown in FIG.

原料糖を70℃の温水に溶解し、多孔質酸化マグネシウム(UCM−150、宇部マテリアルズ株式会社製)を250mg/L添加し、70℃で1分間撹拌後、珪藻土を用いてろ過処理を行った。得られたろ過液について、水酸化ナトリウム溶液により官能基の50%をナトリウム形とした弱酸性陽イオン交換樹脂を充填したカラムに通液し、弱酸性陽イオン交換処理液を得た。得られた弱酸性陽イオン交換処理液を、粒状活性炭(ダイヤホープ MS−10)を充填したカラムに通液した。得られた活性炭処理液について、実施例2と同様にしてイオン交換樹脂により脱塩処理した。 The raw sugar is dissolved in warm water at 70 ° C., 250 mg / L of porous magnesium oxide (UCM-150, manufactured by Ube Material Industries Ltd.) is added, the mixture is stirred at 70 ° C. for 1 minute, and then filtered using diatomaceous earth. rice field. The obtained filtrate was passed through a column packed with a weakly acidic cation exchange resin having 50% of functional groups in the form of sodium with a sodium hydroxide solution to obtain a weakly acidic cation exchange treatment solution. The obtained weakly acidic cation exchange treatment liquid was passed through a column packed with granular activated carbon (Diahope MS-10). The obtained activated carbon treatment liquid was desalted with an ion exchange resin in the same manner as in Example 2.

実施例2と同様にして、溶解液、弱酸性陽イオン交換処理液(活性炭処理入口)、活性炭処理出口、イオン交換処理出口において、Brix(%)、pH、導電率(μS/cm)、灰分(%)、色価(I.U.)を測定した。結果を表8にそれぞれ示す。 Brix (%), pH, conductivity (μS / cm), ash content in the solution, the weakly acidic cation exchange treatment liquid (activated carbon treatment inlet), the activated carbon treatment outlet, and the ion exchange treatment outlet in the same manner as in Example 2. (%) And color value (IU) were measured. The results are shown in Table 8.

Figure 0006942603
Figure 0006942603

酸化マグネシウム処理液を弱酸性陽イオン交換樹脂により処理することにより、容易にpH6〜8の範囲に調整することができた。 By treating the magnesium oxide treatment liquid with a weakly acidic cation exchange resin, the pH could be easily adjusted to the range of 6 to 8.

<実施例6>
実施例5と同様にして、得られたろ過液について、水酸化ナトリウム溶液によりそれぞれ官能基の20モル%、40モル%、60モル%、80モル%をナトリウム形とした弱酸性陽イオン交換樹脂を充填したカラムに通液し、弱酸性陽イオン交換処理液を得た。得られた弱酸性陽イオン交換処理液のpHを表9にそれぞれ示す。
<Example 6>
In the same manner as in Example 5, a weakly acidic cation exchange resin in which 20 mol%, 40 mol%, 60 mol%, and 80 mol% of the functional groups were made into sodium forms of the obtained filtrate with a sodium hydroxide solution, respectively. Was passed through a column packed with a weakly acidic cation exchange treatment solution to obtain a weakly acidic cation exchange treatment solution. The pH of the obtained weakly acidic cation exchange treatment liquid is shown in Table 9, respectively.

Figure 0006942603
Figure 0006942603

このように、弱酸性陽イオン交換樹脂の官能基の30〜60モル%がナトリウム形およびカリウム形のうちの少なくとも1つであることにより、酸化マグネシウム処理液のpHを6〜8の範囲に調整しやすくなる。 As described above, the pH of the magnesium oxide treatment solution is adjusted to the range of 6 to 8 by having 30 to 60 mol% of the functional groups of the weakly acidic cation exchange resin being at least one of the sodium form and the potassium form. It will be easier to do.

1,3,5 精製糖の製造装置、10 溶解槽、12 ろ過装置、14 活性炭処理装置、16 イオン交換処理装置、18 結晶化装置、20 濃縮装置、22,24,26,28,30,32,34,38,40,44,46 配管、36 酸化マグネシウム処理装置、42 弱酸性陽イオン交換処理装置。 1,3,5 Purified sugar production equipment, 10 dissolution tanks, 12 filtration equipment, 14 activated charcoal processing equipment, 16 ion exchange processing equipment, 18 crystallization equipment, 20 concentrators, 22, 24, 26, 28, 30, 32 , 34, 38, 40, 44, 46 Piping, 36 Magnesium oxide treatment equipment, 42 Weakly acidic cation exchange treatment equipment.

Claims (8)

原料糖の溶解液をろ過処理するろ過手段と、
得られたろ過液を活性炭で処理する活性炭処理手段と、
得られた活性炭処理液を、OH形の強塩基性陰イオン交換樹脂およびH形の弱酸性陽イオン交換樹脂を含むイオン交換樹脂により脱塩処理するイオン交換処理手段と、
を備え
前記ろ過手段の前段に、前記溶解液を酸化マグネシウムで処理する酸化マグネシウム処理手段をさらに備え、
炭酸飽充を行わないことを特徴とする精製糖の製造装置。
Filtration means for filtering the solution of raw sugar and
Activated carbon treatment means for treating the obtained filtrate with activated carbon,
An ion exchange treatment means for desalting the obtained activated charcoal treatment liquid with an ion exchange resin containing an OH-type strong basic anion exchange resin and an H-type weakly acidic cation exchange resin.
Equipped with a,
A magnesium oxide treatment means for treating the solution with magnesium oxide is further provided before the filtration means.
A device for producing purified sugar, which is characterized by not performing carbonic acid saturation.
請求項に記載の精製糖の製造装置であって、
前記酸化マグネシウムは、比表面積100m/g以上の多孔質酸化マグネシウムであることを特徴とする精製糖の製造装置。
The device for producing purified sugar according to claim 1.
An apparatus for producing purified sugar, wherein the magnesium oxide is a porous magnesium oxide having a specific surface area of 100 m 2 / g or more.
請求項1または2に記載の精製糖の製造装置であって、
前記ろ過手段の後段に、得られたろ過液を弱酸性陽イオン交換樹脂により処理してpH6〜8の範囲に調整する弱酸性陽イオン交換処理手段をさらに備えることを特徴とする精製糖の製造装置。
The device for producing purified sugar according to claim 1 or 2.
The production of purified sugar is further provided with a weakly acidic cation exchange treatment means for treating the obtained filtrate with a weakly acidic cation exchange resin to adjust the pH to a range of 6 to 8 after the filtration means. Device.
請求項に記載の精製糖の製造装置であって、
前記弱酸性陽イオン交換処理手段における前記弱酸性陽イオン交換樹脂の官能基の30〜60モル%が、ナトリウム形およびカリウム形のうちの少なくとも1つであることを特徴とする精製糖の製造装置。
The device for producing purified sugar according to claim 3.
An apparatus for producing a purified sugar, wherein 30 to 60 mol% of the functional group of the weakly acidic cation exchange resin in the weakly acidic cation exchange treatment means is at least one of a sodium form and a potassium form. ..
原料糖の溶解液をろ過処理するろ過工程と、
得られたろ過液を活性炭で処理する活性炭処理工程と、
得られた活性炭処理液を、OH形の強塩基性陰イオン交換樹脂およびH形の弱酸性陽イオン交換樹脂を含むイオン交換樹脂により脱塩処理するイオン交換処理工程と、
を含み、
前記ろ過工程の前段に、前記溶解液を酸化マグネシウムで処理する酸化マグネシウム処理工程をさらに含み、
炭酸飽充工程を含まないことを特徴とする精製糖の製造方法。
A filtration process that filters the solution of the raw sugar
An activated carbon treatment step in which the obtained filtrate is treated with activated carbon,
An ion exchange treatment step of desalting the obtained activated charcoal treatment solution with an ion exchange resin containing an OH-type strong basic anion exchange resin and an H-type weakly acidic cation exchange resin.
Only including,
A magnesium oxide treatment step of treating the solution with magnesium oxide is further included before the filtration step.
A method for producing purified sugar, which does not include a carbonic acid saturation step.
請求項に記載の精製糖の製造方法であって、
前記酸化マグネシウムは、比表面積100m/g以上の多孔質酸化マグネシウムであることを特徴とする精製糖の製造方法。
The method for producing purified sugar according to claim 5.
A method for producing purified sugar, wherein the magnesium oxide is a porous magnesium oxide having a specific surface area of 100 m 2 / g or more.
請求項5または6に記載の精製糖の製造方法であって、
前記ろ過工程の後段に、得られたろ過液を弱酸性陽イオン交換樹脂により処理してpH6〜8の範囲に調整する弱酸性陽イオン交換処理工程をさらに含むことを特徴とする精製糖の製造方法。
The method for producing a purified sugar according to claim 5 or 6.
The production of purified sugar further comprises a weakly acidic cation exchange treatment step of treating the obtained filtrate with a weakly acidic cation exchange resin to adjust the pH to a range of 6 to 8 after the filtration step. Method.
請求項に記載の精製糖の製造方法であって、
前記弱酸性陽イオン交換処理工程における前記弱酸性陽イオン交換樹脂の官能基の30〜60モル%が、ナトリウム形およびカリウム形のうちの少なくとも1つであることを特徴とする精製糖の製造方法。
The method for producing purified sugar according to claim 7.
A method for producing a purified sugar, wherein 30 to 60 mol% of the functional group of the weakly acidic cation exchange resin in the weakly acidic cation exchange treatment step is at least one of a sodium form and a potassium form. ..
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