WO2012024911A1 - 一种饮用水除氟滤料的再生方法 - Google Patents

一种饮用水除氟滤料的再生方法 Download PDF

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WO2012024911A1
WO2012024911A1 PCT/CN2011/070799 CN2011070799W WO2012024911A1 WO 2012024911 A1 WO2012024911 A1 WO 2012024911A1 CN 2011070799 W CN2011070799 W CN 2011070799W WO 2012024911 A1 WO2012024911 A1 WO 2012024911A1
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regeneration
filter material
hydroxyapatite
treatment
regeneration treatment
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French (fr)
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刘泽山
冯莉
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JIANGSU YONGGUAN WATER AND WASTEWATER EQUIPMENT CO Ltd
China University of Mining and Technology CUMT
China University of Mining and Technology Beijing CUMTB
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JIANGSU YONGGUAN WATER AND WASTEWATER EQUIPMENT CO Ltd
China University of Mining and Technology CUMT
China University of Mining and Technology Beijing CUMTB
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Publication of WO2012024911A1 publication Critical patent/WO2012024911A1/zh
Priority to ZA2012/04090A priority Critical patent/ZA201204090B/en
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    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
    • B01J20/048—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium containing phosphorus, e.g. phosphates, apatites, hydroxyapatites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/34—Regenerating or reactivating
    • B01J20/3433—Regenerating or reactivating of sorbents or filter aids other than those covered by B01J20/3408 - B01J20/3425
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/34—Regenerating or reactivating
    • B01J20/3483—Regenerating or reactivating by thermal treatment not covered by groups B01J20/3441 - B01J20/3475, e.g. by heating or cooling
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/50—Aspects relating to the use of sorbent or filter aid materials
    • B01J2220/56—Use in the form of a bed
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C02F2101/12—Halogens or halogen-containing compounds
    • C02F2101/14—Fluorine or fluorine-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2303/00—Specific treatment goals
    • C02F2303/16—Regeneration of sorbents, filters

Definitions

  • the invention relates to a drinking water treatment technology, in particular to a method for regenerating a drinking water defluoridation filter material for granular hydroxyapatite.
  • Fluorosis caused by drinking high-fluorine water is a worldwide endemic disease. It causes fluorosis in the light, and causes fluorosis in the severe cases, causing osteoporosis, bone deformation, and even paralysis. China is one of the countries with the most serious fluorosis in the world. Except for Shanghai, it is distributed in all provinces of the country, mainly in rural and desert areas with relatively backward economy. At present, the population of sick villages with high fluoride water poisoning is as high as 81.41 million. The National Eleventh Five-Year Plan for Rural Drinking Water Safety Project decided to basically solve the drinking water safety problem of more than 300 million rural people by 2015.
  • the general fluorine removal technology at home and abroad mainly adopts the adsorption method, and the regeneration problem of the adsorbent is one of the key factors affecting whether the adsorbent material can be used for the fluorine removal filter.
  • Hydroxyapatite (HAP) is gradually recognized and accepted as a fluoride removal filter for drinking water.
  • the traditional regeneration method is mainly 0.25%. ⁇ 1%
  • the NaOH solution is used as a regenerant, and is neutralized with hydrochloric acid or sulfuric acid solution after regeneration.
  • the regeneration efficiency of the method is low, and the device has a corrosive effect, which affects the promotion and application of the hydroxyapatite defluoridation agent.
  • the coating regeneration method needs to return the HAP saturated with fluoride ions back to a solution consisting of a certain concentration of Ca2+ and H2PO3-, and adjust the pH of the solution to about 3, and re-react on the surface to form a new layer of hydroxyphosphorus. Graystone to restore its ability to remove fluorine. For the vast rural areas, this kind of operation is relatively complicated, and the reaction conditions are not easy to control, which makes it difficult to guarantee the regeneration efficiency.
  • the object of the present invention is to provide a method for regenerating a drinking water defluoridation filter material, which realizes high efficiency of regeneration of hydroxyapatite filter material by coupling of thermal regeneration and mechanical wear, no need to replace filter material, convenient use, and simple method. Fast.
  • the regeneration method of the present invention is as follows: a, using thermal regeneration treatment: the hydroxyapatite granular filter material saturated with fluoride ions is heated in water for a period of time, and can be reused until it is again saturated with fluoride ions; b. Re-recycling the granular hydroxyapatite filter material saturated with fluoride ions again; c, repeat step b, perform multiple thermal regeneration treatment until the regeneration rate of hydroxyapatite is less than 20%; d.
  • Mechanical wear regeneration treatment the hydroxyapatite granular filter material saturated with fluoride ions with a regeneration rate of less than 20% is used in the fluorine removal device, and the fluoroapatite is worn away by the water flow to remove the hydroxyapatite.
  • the outer layer reveals a fresh surface, restores the fluorine removal ability of the hydroxyapatite, and replenishes the new filter material corresponding to the corresponding amount of wear; e, then use the thermal regeneration treatment method, repeat steps c and d, recycle the thermal regeneration treatment multiple times, mechanical wear regeneration once, can achieve the reuse of the fluorine removal filter; through thermal regeneration treatment and mechanical wear regeneration The treatment is used alternately to maximize the filter regeneration efficiency and cycle times.
  • the filter material is heated in water at a temperature of 50 to 100 ° for a duration of 0.5 to 5 hours; and the number of repeated use of the thermal regeneration treatment is about 5 times.
  • the regeneration method of the present invention achieves the maximum of regeneration efficiency and repeated use by alternately treating the thermal regeneration treatment and mechanical wear of the hydroxyapatite granular filter material saturated with fluoride ions, thereby realizing the hydroxyapatite filter material.
  • the regeneration is highly efficient. After repeated heat regeneration treatment, the mechanical wear treatment is used when the regeneration rate is low, so that the fresh surface of the hydroxyapatite pellet is exposed, the fluorine removal ability is restored, and the new material is added according to the wear amount to ensure the fluorine removal ability, instead of Wait until the filter material is completely effective after removing the fluorine performance.
  • the main advantages are: 1.
  • the regeneration efficiency of the fluorine removal filter is high: the single regeneration efficiency is greater than 50% to 80%; 2.
  • the fluorine removal filter material is continuously updated during the operation, and the fluorine removal performance is stable for a long time. 3.
  • the regeneration method is simple and easy.
  • thermal regeneration treatment is adopted: by using a heating method to provide energy for removing the fluorine-containing filter material to obtain energy of the hydroxyapatite saturated with fluorine ions, the fluorine ions on the surface of the hydroxyapatite migrate to the inside, and the surface The active position is vacated and the fluorine removal ability is restored; By loading the container for removing the fluorine filter, the granular filter material saturated with fluoride ions is heated to 95° in water for 0.5 hour, and then can be used continuously;
  • Q is the regeneration defluoridation capacity mg/g
  • Co is the concentration of fluoride ion in the raw water mg/L
  • C is the concentration of fluoride ion in the water after saturation adsorption of the regenerated defluorinated filter material, mg/L
  • V is the water sample volume L
  • m is the mass g of the fluorine-containing granular filter.
  • the granular hydroxyapatite filter material saturated with fluoride ions is heated to 95° for 0.5 hours, and can be used continuously.
  • the regeneration rate at this time can be measured by the same method as above. %;
  • step c repeat the process of step b, after 5 times of thermal regeneration, mechanical wear regeneration treatment is required, and the measured regeneration rate is reduced to 19%;
  • the second embodiment is basically the same as the first embodiment, the same parts are omitted, and the different parts are as follows:
  • the granular filter material saturated with fluoride ions is heated to 50 ° in water, and can continue to be used after 5 hours, at which time the measured regeneration rate is 55%;
  • the granular hydroxyapatite filter material saturated with fluoride ions is heated to 50°, and can be used continuously after 5 hours, and the measured regeneration rate is 45%;
  • step c repeat the process of step b, after 5 times of thermal regeneration, mechanical wear regeneration treatment is required, and the measured regeneration rate is reduced to 18%;
  • the method of the thermal regeneration treatment is repeated, and the steps c and d are repeated, and after the thermal regeneration treatment is cycled for about 5 times, the mechanical abrasion is regenerated once, and the recycling of the fluorine-removing filter material can be realized.
  • the third embodiment is basically the same as the first embodiment, the same parts are omitted, and the different parts are as follows:
  • the granular filter material saturated with fluoride ions is heated to 70 ° in water, and can continue to be used after 3 hours, at which time the measured regeneration rate is 65%;
  • the granular hydroxyapatite filter material saturated with fluoride ions is heated to 70° for 3 hours, and the measured regeneration rate is 55%;
  • step c repeat the process of step c, after 5 times of thermal regeneration, mechanical wear regeneration treatment is required, and the measured regeneration rate is reduced to 19%;
  • the method of the thermal regeneration treatment is repeated, and the steps c and d are repeated, and after the thermal regeneration treatment is cycled for about 5 times, the mechanical abrasion is regenerated once, and the recycling of the fluorine-removing filter material can be realized.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Thermal Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Water Treatment By Sorption (AREA)

Description

一种饮用水除氟滤料的再生方法 技术领域
本发明涉及一种饮用水处理技术，尤其适用于粒状羟基磷灰石的饮用水除氟滤料的再生方法。
背景技术
饮用高氟水造成的氟中毒是涉及世界范围的地方病，轻者引起氟斑牙，重者会引起氟骨症，造成骨质疏松、骨变形，甚至瘫痪，丧失劳动能力。中国是世界上氟中毒最严重的国家之一，除上海市外，遍布全国各省，主要分布在经济相对落后的农村和牧区，目前因高氟水源中毒的病村人口高达8141万。《全国农村饮水安全工程“十一五”规划》决定到2015年基本解决3亿多农村人口的饮水安全问题。
目前，国内外通用除氟技术主要采用吸附法，而吸附剂的再生问题是影响吸附材料能否用于除氟滤料的关键因素之一。羟基磷灰石（HAP）作为饮用水除氟滤料正在逐渐被人们所认识和接受，其传统的再生方法主要是用0.25％ ～1％ 的NaOH溶液作为再生剂，再生后用盐酸或硫酸溶液中和，该法再生效率低，对设备有腐蚀作用，影响了羟基磷灰石降氟剂的推广和应用。应波，李新云，丛正茂在“饮水降氟材料—羟基磷灰石的再生方法的研究” （卫生研究, 2002, 31(02): 83-84）一文中报道了羟基磷灰石的NaOH再生法与表面涂层再生法的再生效果比较，结果表明，用表面涂层再生法对饱和的羟基磷灰石进行再生处理，其再生效率可达46 ％－64 ％，与传统的NaOH再生法相比，再生效率提高了2倍以上。但涂层再生法需要将已被氟离子饱和的HAP放回到由一定浓度Ca2+和H2PO3-组成的溶液中，并调整溶液pH值为3左右，在其表面重新反应生成一层新的羟基磷灰石，以恢复其除氟能力。对于广大农村地区来说，这种操作相对复杂，反应条件不易控制，从而容易造成再生效率难以保证。
由于除氟滤料的使用寿命都较短，在除氟滤料不能再生时，需要整体更换滤料，更换过程非常麻烦，是导致很多除氟设备不能长期使用的一个重要原因。
 技术问题
本发明的目的是提供一种饮用水除氟滤料的再生方法，通过热再生和机械磨损的耦合，实现羟基磷灰石滤料再生高效率、滤料无需更换、使用方便、方法简单易行、快捷。
技术解决方案
本发明的再生方法如下：
a、采用热再生处理：对已被氟离子饱和的羟基磷灰石粒状滤料在水中加热，持续一段时间，即可重新使用至再次被氟离子饱和；
b、对再次被氟离子饱和的粒状羟基磷灰石滤料再次进行热再生处理；
c、重复步骤b，进行多次热再生处理，直至羟基磷灰石的再生率低于20%；
d、采用机械磨损再生处理：使再生率低于20%的被氟离子饱和的羟基磷灰石粒状滤料在除氟装置内，通过水流使得除氟滤料运动磨损，磨去羟基磷灰石的外层，露出新鲜表面，恢复羟基磷灰石的除氟能力，补充相应磨损量的新滤料即可重新使用；
e、之后再使用热再生处理的方法，重复步骤c和d，循环使用热再生处理多次，机械磨损再生1次，即可实现除氟滤料的重复利用；通过热再生处理与机械磨损再生处理交替使用，达到滤料再生效率和循环使用次数的最大化。
所述滤料在水中加热的温度为50～100°，持续时间为0.5～5小时；所述重复使用热再生处理的次数约为5次。
 有益效果
本发明的再生方法，通过对被氟离子饱和的羟基磷灰石粒状滤料的热再生处理和机械磨损的交替处理，达到再生效率和重复使用次数的极大化，实现羟基磷灰石滤料的再生高效率。经过多次热再生处理后，再生率较低时采用机械磨损处理，从而使得羟基磷灰石小球的新鲜表面暴露，除氟能力得以恢复，并根据磨损量添加新料，保证除氟能力，而不是等到滤料除氟性能实效后全部更新。主要优点在于：
1、除氟滤料再生效率高：单次再生效率大于50%～80%；
2、除氟滤料在运行过程中不断更新，除氟性能长期稳定。
3、再生方法简单易行。
 本发明的实施方式
实施例一、
a、首先采用热再生处理：利用加热的方式，提供除氟滤料以能量，使已被氟离子饱和的羟基磷灰石获得能量后，羟基磷灰石表面的氟离子向内部迁移，表面的活性位置空出来，除氟能力得以恢复； 通过装放除氟滤料的容器，对已被氟离子饱和的粒状滤料在水中加热至95°，持续0.5h后，即可继续使用；
依据是：假如在容器中放入一定质量（m）的再生除氟粒状滤料，向内加入含氟水，含氟水的体积(v)为将再生除氟滤料完全浸泡为准，然后振荡容器，使再生除氟滤料达到吸附氟离子饱和后，采用氟离子电极测试水中含氟离子的浓度（按照GB7484-87水质-氟化物的测定方法-离子选择电极法），利用公式Q=V*(C0-C)/m计算出再生除氟容量，用再生除氟容量除以再生前的除氟滤料的除氟容量，得出再生率为50%；
式中Q为再生除氟容量mg/g，Co为原水中氟离子的浓度mg/L，C为再生除氟滤料饱和吸附之后水中氟离子的浓度mg/L，V为水样体积L，m为除氟粒状滤料的质量g。
b、使用一段时间后，将再次被氟离子饱和的粒状羟基磷灰石滤料加热至95°，持续0.5h后即可继续使用，用上述同样的方法可测出此时的再生率为40%；
c、重复步骤b的过程，热再生5次后，需进行机械磨损再生处理，此时测出的再生率降到19%；
d、机械磨损再生处理：通过水流使得除氟滤料在除氟装置内运动，造成已被氟离子饱和的粒状羟基磷灰石的机械磨损；从而使得羟基磷灰石小球的新鲜表面暴露，除氟能力得以恢复；用与步骤b同样的方法测定此时再生率达80%；将磨损后的粒状滤料过滤、洗涤，然后将滤液蒸发、称重，得到粒状滤料的磨损量，一般一次磨损量约为投药量的10%，补充相应磨损量的新滤料；
e、之后再使用热再生处理的方法，重复步骤c和d，循环使用热再生处理约5次后，机械磨损再生1次，即可实现除氟滤料的重复利用；通过热再生处理与机械磨损再生处理交替使用，达到滤料再生效率和循环使用次数的最大化。
实施例二、与实施例一基本相同，相同部分略，不同部分如下：
a、首先采用热再生处理：对已被氟离子饱和的粒状滤料在水中加热至50°，持续5h后即可继续使用，此时测出的再生率为55%；
b、使用一段时间后，将再次被氟离子饱和的粒状羟基磷灰石滤料加热至50°，持续5h后即可继续使用，此时测出的再生率为45%；
c、重复步骤b的过程，热再生5次后，需进行机械磨损再生处理，此时测出的再生率降到18%；
d、机械磨损再生处理：测定此时再生率达80%；磨损量约为投药量的10%，补充相应磨损量的新滤料；
e、之后再使用热再生处理的方法，重复步骤c和d，循环使用热再生处理约5次后，机械磨损再生1次，即可实现除氟滤料的重复利用。
实施例三、与实施例一基本相同，相同部分略，不同部分如下：
a、首先采用热再生处理：对已被氟离子饱和的粒状滤料在水中加热至70°，持续3h后即可继续使用，此时测出的再生率为65%；
b、使用一段时间后，将再次被氟离子饱和的粒状羟基磷灰石滤料加热至70°，持续3h，此时测出的再生率为55%；
c、重复步骤c的过程，热再生5次后，需进行机械磨损再生处理，此时测出的再生率降到19%；
d、机械磨损再生处理：测定此时再生率达80%；磨损量约为投药量的10%，补充相应磨损量的新滤料；
e、之后再使用热再生处理的方法，重复步骤c和d，循环使用热再生处理约5次后，机械磨损再生1次，即可实现除氟滤料的重复利用。

Claims (3)

  1. 一种饮用水除氟滤料的再生方法，其特征在于：
    a、采用热再生处理：对已被氟离子饱和的羟基磷灰石粒状滤料在水中加热，持续一段时间，即可重新使用至再次被氟离子饱和；
    b、对再次被氟离子饱和的粒状羟基磷灰石滤料再次进行热再生处理；
    c、重复步骤b，进行多次热再生处理，直至羟基磷灰石的再生率低于20%；
    d、采用机械磨损再生处理：使再生率低于20%的被氟离子饱和的羟基磷灰石粒状滤料在除氟装置内，通过水流使得除氟滤料运动磨损，磨去羟基磷灰石的外层，露出新鲜表面，恢复羟基磷灰石的除氟能力，补充相应磨损量的新滤料即可重新使用；
    e、之后再使用热再生处理的方法，重复步骤c和d，循环使用热再生处理多次，机械磨损再生1次，即可实现除氟滤料的重复利用；通过热再生处理与机械磨损再生处理交替使用，达到滤料再生效率和循环使用次数的最大化。
  2. 根据权利要求1所述的一种饮用水除氟滤料的再生方法，其特征在于：所述滤料在水中加热的温度为50～100°，持续时间为0.5～5小时。
  3. 根据权利要求1所述的一种饮用水除氟滤料的再生方法，其特征在于：所述重复使用热再生处理的次数约为5次。
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CN102728333B (zh) * 2012-07-09 2014-08-13 河海大学 一种除氟用球状羟基磷灰石再生装置
CN107324459B (zh) * 2017-07-31 2019-10-01 武汉理工大学 一种鱼骨炭除氟电极的制作方法
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