WO2017162037A1 - 去除甘蔗糖蜜中钙镁离子的方法 - Google Patents

去除甘蔗糖蜜中钙镁离子的方法 Download PDF

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WO2017162037A1
WO2017162037A1 PCT/CN2017/076144 CN2017076144W WO2017162037A1 WO 2017162037 A1 WO2017162037 A1 WO 2017162037A1 CN 2017076144 W CN2017076144 W CN 2017076144W WO 2017162037 A1 WO2017162037 A1 WO 2017162037A1
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cane molasses
fluoride
sugar cane
magnesium ions
calcium
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PCT/CN2017/076144
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French (fr)
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邹传军
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邹传军
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Priority claimed from CN201610177090.0A external-priority patent/CN105779661A/zh
Priority claimed from CN201610177003.1A external-priority patent/CN105776471A/zh
Priority claimed from CN201610179579.1A external-priority patent/CN105854350B/zh
Application filed by 邹传军 filed Critical 邹传军
Publication of WO2017162037A1 publication Critical patent/WO2017162037A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C13—SUGAR INDUSTRY
    • C13B—PRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
    • C13B20/00—Purification of sugar juices
    • C—CHEMISTRY; METALLURGY
    • C13—SUGAR INDUSTRY
    • C13B—PRODUCTION OF SUCROSE; APPARATUS SPECIALLY ADAPTED THEREFOR
    • C13B50/00—Sugar products, e.g. powdered, lump or liquid sugar; Working-up of sugar

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  • the invention relates to the field of cane molasses, in particular to a method for removing calcium and magnesium ions from cane molasses.
  • Sugar cane molasses is a by-product of sucrose crystallization.
  • the main components that can be used include 25%-35% sucrose and 13-23% reducing sugar, which are important raw materials for the fermentation industry.
  • Sugar cane molasses also contains a large amount of inorganic matter, and sulfuric acid ash is about 10%, which contains 1-2% of calcium and magnesium ions, which has many adverse effects on the production process.
  • sulfuric acid ash is about 10%, which contains 1-2% of calcium and magnesium ions, which has many adverse effects on the production process.
  • the presence of calcium ions It affects the crystallization of glutamic acid.
  • calcium and magnesium ions are easily scaled, which affects the evaporation and concentration of alcohol waste liquid.
  • the scale of the evaporator is serious, which affects the concentration of pigment. Therefore, the removal of calcium and magnesium ions is of great significance for the deep processing of sugar cane molasses.
  • Ion exchange method the material passes through the cation resin, the calcium and magnesium ions are exchanged by sodium ion, and the resin is saturated and then regenerated with sodium chloride solution.
  • the calcium and magnesium ion concentration of the sugar cane molasses is too high, the cation resin can only be treated 2 ⁇ With 5 times the volume of the material, the resin is quickly saturated and the regeneration is frequent. Therefore, the method has high production cost, does not meet the requirements of large-scale production, and has no actual production value.
  • Soda ash method that is, adding soda ash to the material to form a precipitate of calcium carbonate and magnesium carbonate to achieve the purpose of softening, and the decalcified magnesium ion of the beet molasses adopts this method.
  • the pH of the sugar cane molasses is about 4.5, containing a large amount of organic acid, it is necessary to consume a large amount of soda ash to completely precipitate calcium and magnesium; in the process of sinking, the pH of the sugar cane molasses is increased a lot. , leading to many side reactions, this method has no industrial value.
  • the object of the present invention is to provide a method for removing calcium and magnesium ions from cane molasses, which utilizes fluoride to remove calcium and magnesium ions from cane molasses, which is economical and simple, and meets industrial production requirements.
  • the present invention provides a method for removing calcium and magnesium ions in cane molasses, comprising the following steps:
  • the sugar cane molasses is diluted with pure water to obtain an aqueous solution of sugar cane molasses with a mass fraction of 55-60%; the sugar cane molasses with a mass fraction of 55-60% is selected to reduce the volume of the material and facilitate operation;
  • step 3 heating all the sugar cane molasses aqueous solution in step 1) from room temperature to 80-90 ° C, and slowly adding all the fluoride suspension or solution in step 2) to the sugar cane molasses aqueous solution, stirring while stirring, stirring and keeping warm 1 ⁇ 3h; obtaining stable precipitation of calcium fluoride and magnesium fluoride, and then filtering or centrifuging to remove the precipitate, thereby obtaining sugar cane molasses containing no calcium and magnesium ions.
  • the sugar cane molasses aqueous solution having a temperature of 80 to 90 ° C is selected to promote the precipitation of magnesium fluoride, and at the same time, it can also function as a molasses sterilization.
  • the fluoride is any one of sodium fluoride, potassium fluoride, and ammonium fluoride.
  • the weight ratio of the fluoride to the dry weight of the cane molasses is 2.0 to 5.0:100, and the ratio is adjusted according to the change in the salt composition of the cane molasses.
  • the weight ratio of sodium fluoride to sugar cane molasses is 2.0-3.5:100, and the ratio is adjusted according to the salt composition of the sugar cane molasses.
  • the weight ratio of sodium fluoride to hot water is 1:4 to 7, and the temperature of the hot water is 90 °C.
  • the rate of heating the aqueous solution of the cane molasses is 3 to 5 ° C / s.
  • the aqueous solution of the sugar cane molasses has a temperature of 90 °C.
  • the invention adopts fluoride to remove calcium and magnesium ions in sugar cane molasses, and has a removal rate of 100%, a small amount of fluoride and a low cost, and is suitable for industrial production.
  • the invention adopts fluoride to fully precipitate calcium and magnesium ions, and obtains sugar cane molasses which does not contain calcium and magnesium ions, and the solution thereof
  • the adverse effects of calcium and magnesium ions during the use of sugar cane molasses are overcome, and the disadvantages of high cost of using sodium carbonate and sodium sulfite are overcome, which is economically feasible.
  • step 1) The whole aqueous solution of cane molasses in step 1) is heated from room temperature to 90 ° C at a rate of 3 ° C / s, and then all the fluoride suspension is slowly added to the aqueous solution of cane molasses, stirred while stirring, and kept for 2 h. Filtration with a vacuum drum filter removes calcium fluoride, magnesium fluoride and other precipitates, and the filtrate is sugar cane molasses 1 which does not contain calcium and magnesium ions.
  • the total content of calcium and magnesium ions in the sugar cane molasses 1 was 0 ppm as determined by the above method.
  • step 1) The whole aqueous solution of cane molasses in step 1) is heated from room temperature to 90 ° C at a rate of 5 ° C / s, and then all the fluoride suspension is slowly added to the aqueous solution of cane molasses, stirred while stirring, and kept for 2 h. Separation by centrifugation and removal of the precipitate, the supernatant is sugar cane molasses 2 which does not contain calcium and magnesium ions.
  • the total content of calcium and magnesium ions in the sugar cane molasses 2 was 0 ppm as determined by the above method.
  • step 3 The whole aqueous solution of cane molasses in step 1) is heated from room temperature to 85 ° C at a rate of 5 ° C / s, and then all the fluoride suspension is slowly added to the aqueous solution of cane molasses, stirred while stirring, and kept for 1 h. The precipitate was removed by a plate and frame filter, and the filtrate was sugar cane molasses 3 which did not contain calcium and magnesium ions.
  • the total content of calcium and magnesium ions in the sugar cane molasses 3 was 0 ppm as determined by the above method.
  • step 1) The aqueous solution of the sugar cane molasses in step 1) is heated from room temperature to 90 ° C at a rate of 3 ° C / s, and then the entire fluoride suspension is slowly added to the aqueous solution of cane molasses, while stirring, stirring and holding for 2 h; The precipitate was removed using a plate and frame filter, and the filtrate was sugar cane molasses 4 which did not contain calcium and magnesium ions.
  • the total content of calcium and magnesium ions in the sugar cane molasses 4 was 0 ppm as determined by the above method.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Processing Of Solid Wastes (AREA)
  • Saccharide Compounds (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Removal Of Specific Substances (AREA)

Abstract

去除甘蔗糖蜜中钙镁离子的方法，包括：将甘蔗糖蜜稀释得到水溶液，将氟化物加入热水中制成悬浊液或溶液，将甘蔗糖蜜水溶液加热后加入氟化物悬浊液或溶液，得到氟化钙、氟化镁沉淀，过滤或离心沉降，除去沉淀物，得到不含钙镁离子的甘蔗糖蜜。

Description

去除甘蔗糖蜜中钙镁离子的方法 技术领域
本发明涉及甘蔗糖蜜领域，具体地指一种去除甘蔗糖蜜中钙镁离子的方法。
背景技术
甘蔗糖蜜是蔗糖结晶后的副产物，主要可以利用的成分包括25％-35％的蔗糖，13～23％还原糖，是发酵工业的重要原料。甘蔗糖蜜还含有大量的无机物，硫酸灰分大约10％，其中含有1-2％的钙、镁离子，对生产过程产生了很多不利影响，比如，在糖蜜味精的生产中，钙离子的存在，影响谷氨酸的结晶，在糖蜜酒精的生产中，钙镁离子容易结垢，影响酒精废液的蒸发浓缩，在糖蜜焦糖色素的生产过程中，蒸发器结垢严重，影响色素的浓缩。因此，去除钙镁离子，对甘蔗糖蜜的深加工，具有非常重要的意义。
目前，除钙镁离子的常用方法有如下三种：
1)离子交换法，物料通过阳树脂，钙镁离子被钠离子交换，树脂饱和后，用氯化钠溶液再生，但是，由于甘蔗糖蜜的钙镁离子浓度过高，阳树脂只能处理2～5倍体积的物料，树脂很快饱和，再生频繁,因此该方法生产成本高，不符合大规模生产要求，没有实际生产价值。
2)纯碱法，即在物料中加入纯碱，形成碳酸钙、碳酸镁的沉淀，达到软化的目的，甜菜糖蜜的脱钙镁离子就是采用这种方法。然而在甘蔗糖蜜的处理中，由于甘蔗糖蜜的pH值在4.5左右，含有大量的有机酸，需要消耗大量的纯碱，才能将钙镁完全沉淀；在沉沉的过程中，甘蔗糖蜜的pH值提高很多，导致很多副反应，这种方法，没有工业价值。其它常用的除钙镁的化学品，包括硫酸钠、亚硫酸钠、草酸钠等，用于甘蔗糖蜜除钙镁，也存在效果不好或者用量太大的问题，没有工业生产价值。
3)常用的脱盐设备—电渗析，由于甘蔗糖蜜含有大量的钙镁离子和硫酸根离子，在电渗析膜的表面会形成硫酸钙的沉淀，造成很难清洗的污染，使得电渗析设备无法运行，达不到甘蔗糖蜜脱盐的目的。
由上可知，上述三种方法均无法适用于工业化大生产，迫切需要一种适用于工业化生产，且经济适用的去除甘蔗糖蜜中钙镁离子的方法。
发明内容
本发明的目的是提供了一种去除甘蔗糖蜜中钙镁离子的方法，该方法利用氟化物去除甘蔗糖蜜中钙镁离子，该方法即经济、又简单,符合工业化生产要求。
为解决上述技术问题，本发明提供的一种去除甘蔗糖蜜中钙镁离子的方法，包括以下步骤：
1)将甘蔗糖蜜用纯水稀释，得到质量分数为55～60％的甘蔗糖蜜水溶液；选择质量分数为55～60％的甘蔗糖蜜是为了减少物料的体积，便于操作；
2)称取氟化物并将氟化物缓慢加入温度为80～90℃的热水中，边加边搅拌溶解，得到氟化物悬浊液或溶液，
3)将步骤1)中全部的甘蔗糖蜜水溶液从室温加热至80～90℃，再向甘蔗糖蜜水溶液中缓慢加入步骤2)中全部的氟化物悬浊液或溶液，边加边搅拌，搅拌保温1～3h；得到氟化钙、氟化镁的稳定沉淀，然后过滤或离心沉降，除去沉淀物，即得到不含有钙镁离子的甘蔗糖蜜。
选择温度为80～90℃的甘蔗糖蜜水溶液是为了促进氟化镁的沉淀，同时，也可以起到糖蜜灭菌的作用。
进一步地，所述步骤2)中，氟化物为氟化钠、氟化钾、氟化铵中任意一种。
再进一步地，所述步骤2)中，氟化物与甘蔗糖蜜干重的重量比为2.0～5.0:100，该比例随甘蔗糖蜜的盐分组成变化而调整。
再进一步地，所述步骤2)中，氟化钠与甘蔗糖蜜干重的重量比为2.0-3.5∶100，该比例随甘蔗糖蜜的盐分组成变化而调整。
再进一步地，其特征在于：所述步骤2)中，氟化钠与热水的重量比为1∶4～7，所述热水的温度为90℃。
再进一步地，所述步骤3)中，甘蔗糖蜜水溶液加热的速率为3～5℃/s。
再进一步地，甘蔗糖蜜水溶液温度为90℃。
本发明的有益效果在于：
1)本发明采用氟化物去除甘蔗糖蜜中钙镁离子的效果好，去除率可以达到100％，氟化物用量少，成本低，适合工业化生产。
2)本发明采用氟化物使钙镁离子充分沉淀，得到不含有钙镁离子的甘蔗糖蜜，其解 决了甘蔗糖蜜的使用过程中钙镁离子带来的不利影响，克服了使用碳酸钠和亚硫酸钠成本高的缺陷，经济上具有可行性。
具体实施方式
为了更好地解释本发明，以下结合具体实施例进一步阐明本发明的主要内容，但本发明的内容不仅仅局限于以下实施例。
实施例1
1)称取1公斤的甘蔗糖蜜，其质量分数为82％，采用EDTA法检测甘蔗糖蜜中钙和镁离子总含量为9800ppm，加纯水稀释得到质量分数为60％的甘蔗糖蜜水溶液；
2)将22克氟化钠，缓慢加入到100克纯水中，边加边搅拌，加热到90℃，即得到氟化钠悬浊液；
3)将步骤1)中全部的甘蔗糖蜜水溶液按速率3℃/s从室温进行加热至90℃，再向甘蔗糖蜜水溶液中缓慢加入全部的氟化物悬浊液，边加边搅拌，搅拌保温2h；用真空转鼓过滤机过滤，除去氟化钙、氟化镁以及其它的沉淀物，过滤液即为不含有钙镁离子的甘蔗糖蜜1。
经上述方法检测，甘蔗糖蜜1中钙、镁离子总含量为0ppm。
实施例2
1)称取1公斤的甘蔗糖蜜，其质量分数为82％，采用EDTA法检测甘蔗糖蜜中钙和镁离子总含量为10500ppm，加纯水稀释得到质量分数为55％的甘蔗糖蜜水溶液；
2)将23克氟化钠，缓慢加入到100克纯水中，边加边搅拌，加热到90℃，即得到氟化钠悬浊液；
3)将步骤1)中全部的甘蔗糖蜜水溶液按速率5℃/s从室温进行加热至90℃，再向甘蔗糖蜜水溶液中缓慢加入全部的氟化物悬浊液，边加边搅拌，搅拌保温2h；用离心机沉降分离，除去沉淀物，上清液即为不含有钙镁离子的甘蔗糖蜜2。
经上述方法检测，甘蔗糖蜜2中钙、镁离子总含量为0ppm。
实施例3
1)称取1公斤的甘蔗糖蜜，其质量分数为82％，采用EDTA法检测甘蔗糖蜜中钙和镁离子总含量为11500ppm，加纯水稀释得到质量分数为58％的甘蔗糖蜜水溶液；
2)将24克氟化钠，缓慢加入到100克纯水中，边加边搅拌，加热到85℃，搅拌保温1h，即得到氟化钠悬浮液；
3)将步骤1)中全部的甘蔗糖蜜水溶液按速率5℃/s从室温进行加热至85℃，再向甘蔗糖蜜水溶液中缓慢加入全部的氟化物悬浊液，边加边搅拌，搅拌保温1h；用板框过滤机除去沉淀物，过滤液即为不含有钙镁离子的甘蔗糖蜜3。
经上述方法检测，甘蔗糖蜜3中钙、镁离子总含量为0ppm。
实施例4
1)称取1公斤的甘蔗糖蜜，其质量分数为82％，采用EDTA法检测甘蔗糖蜜中钙和镁离子总含量为10100ppm，加纯水稀释得到质量分数为59％的甘蔗糖蜜水溶液；
2)将42克氟化钾，缓慢加入到150克纯水中，边加边搅拌，加热到90℃，即得到氟化钾溶液；
3)将步骤1)中全部的甘蔗糖蜜水溶液按速率3℃/s从室温进行加热至90℃，再向甘蔗糖蜜水溶液中缓慢加入全部氟化物悬浊液，边加边搅拌，搅拌保温2h；使用板框过滤机除去沉淀物，过滤液即为不含有钙镁离子的甘蔗糖蜜4。
经上述方法检测，甘蔗糖蜜4中钙、镁离子总含量为0ppm。
其它未详细说明的部分均为现有技术。尽管上述实施例对本发明做出了详尽的描述，但它仅仅是本发明一部分实施例，而不是全部实施例，人们还可以根据本实施例在不经创造性前提下获得其他实施例，这些实施例都属于本发明保护范围。

Claims (7)

  1. 一种去除甘蔗糖蜜中钙镁离子的方法，其特征在于：包括以下步骤：
    1)将甘蔗糖蜜用纯水稀释，得到质量分数为55～60％的甘蔗糖蜜水溶液；
    2)称取氟化物并将氟化物缓慢加入温度为80～90℃的热水中，边加边搅拌溶解，得到氟化物悬浊液或溶液，
    3)将步骤1)中全部的甘蔗糖蜜水溶液从室温加热至80～90℃，再向步骤1)中甘蔗糖蜜水溶液中缓慢加入步骤2)中全部的氟化物悬浊液或溶液，边加边搅拌，搅拌保温1～3h；得到氟化钙、氟化镁的稳定沉淀，然后过滤或离心沉降，除去沉淀物，即得到不含有钙镁离子的甘蔗糖蜜。
  2. 根据权利要求1所述去除甘蔗糖蜜中钙镁离子的方法，其特征在于：所述步骤2)中，氟化物为氟化钠、氟化钾、氟化铵中任意一种。
  3. 根据权利要求2所述去除甘蔗糖蜜中钙镁离子的方法，其特征在于：所述步骤2)中，氟化物与甘蔗糖蜜干重的重量比为2～5∶100。
  4. 根据权利要求3所述去除甘蔗糖蜜中钙镁离子的方法，其特征在于：所述步骤2)中，氟化钠与甘蔗糖蜜干重的重量比为2～3.5∶100。
  5. 根据权利要求2～4中任意一项所述去除甘蔗糖蜜中钙镁离子的方法，其特征在于：所述步骤2)中，氟化钠与热水的重量比为1∶4～7，所述热水的温度为90℃。
  6. 根据权利要求1或2所述去除甘蔗糖蜜中钙镁离子的方法，其特征在于：所述步骤3)中，甘蔗糖蜜水溶液加热的速率为3～5℃/s。
  7. 根据权利要6所述去除甘蔗糖蜜中钙镁离子的方法，其特征在于：所述步骤3)中，甘蔗糖蜜水溶液温度为90℃。
PCT/CN2017/076144 2016-03-25 2017-03-09 去除甘蔗糖蜜中钙镁离子的方法 WO2017162037A1 (zh)

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Application Number Priority Date Filing Date Title
CN201610177003.1 2016-03-25
CN201610177090.0 2016-03-25
CN201610177090.0A CN105779661A (zh) 2016-03-25 2016-03-25 去除甘蔗糖蜜中钙镁离子的方法
CN201610179579.1 2016-03-25
CN201610177003.1A CN105776471A (zh) 2016-03-25 2016-03-25 植物深加工产品中除钙镁离子的方法
CN201610179579.1A CN105854350B (zh) 2016-03-25 2016-03-25 分离甘蔗糖蜜各组份的方法

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