CN103055803A - Preparation method of aluminum modified hydrotalcite fluoride-removal adsorbent - Google Patents
Preparation method of aluminum modified hydrotalcite fluoride-removal adsorbent Download PDFInfo
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- 239000003463 adsorbent Substances 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- -1 aluminum modified hydrotalcite Chemical class 0.000 title claims abstract description 10
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 9
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical class [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 claims abstract description 45
- 238000006243 chemical reaction Methods 0.000 claims abstract description 36
- 150000004645 aluminates Chemical class 0.000 claims abstract description 23
- 238000003756 stirring Methods 0.000 claims abstract description 14
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000012265 solid product Substances 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 238000001354 calcination Methods 0.000 claims abstract description 7
- QANIADJLTJYOFI-UHFFFAOYSA-K aluminum;magnesium;carbonate;hydroxide;hydrate Chemical compound O.[OH-].[Mg+2].[Al+3].[O-]C([O-])=O QANIADJLTJYOFI-UHFFFAOYSA-K 0.000 claims abstract description 5
- 229910001701 hydrotalcite Inorganic materials 0.000 claims description 19
- 229960001545 hydrotalcite Drugs 0.000 claims description 19
- 230000035484 reaction time Effects 0.000 claims description 11
- 239000004411 aluminium Substances 0.000 claims 6
- 238000004334 fluoridation Methods 0.000 claims 6
- 239000008239 natural water Substances 0.000 claims 1
- 229910052623 talc Inorganic materials 0.000 claims 1
- 235000012222 talc Nutrition 0.000 claims 1
- 239000000454 talc Substances 0.000 claims 1
- 238000005406 washing Methods 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 18
- 238000001179 sorption measurement Methods 0.000 abstract description 16
- 239000003651 drinking water Substances 0.000 abstract description 3
- 235000020188 drinking water Nutrition 0.000 abstract description 3
- 238000000926 separation method Methods 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract 1
- 238000000034 method Methods 0.000 description 20
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 10
- 239000011737 fluorine Substances 0.000 description 10
- 229910052731 fluorine Inorganic materials 0.000 description 10
- 238000006115 defluorination reaction Methods 0.000 description 8
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- 229920001661 Chitosan Polymers 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
Description
技术领域technical field
本发明涉及一种铝改性水滑石除氟吸附剂制备方法，属于水处理材料领域。The invention relates to a preparation method of an aluminum-modified hydrotalcite defluorination adsorbent, which belongs to the field of water treatment materials.
背景技术Background technique
近年来，国内外针对水中氟离子的去除出现了很多工艺，研究热点多集中在混凝沉淀法、离子交换树脂法、电化学法、膜工艺及吸附工艺等。In recent years, there have been many processes for the removal of fluoride ions in water at home and abroad, and the research hotspots are mostly concentrated on coagulation precipitation, ion exchange resin, electrochemical, membrane technology and adsorption technology.
吸附工艺是我国饮用水除氟中研究应用较多的一种方法，主要是将含氟水通过装有氟吸附剂的设备，由于氟离子在吸附剂表面固、液两相中具有不同的分配系数，从而利用固体物质对于水中氟的吸附亲和性达到除氟的效果，吸附剂则可通过再生来恢复吸附能力。吸附法主要应用于处理低浓度含氟水，也可作为含氟水的深度处理方法。可以将吸附剂填入填充柱，采用动态吸附方式，操作简便，除氟效果较为稳定，成本较低，已成为目前国内外应用最为广泛的除氟工艺。The adsorption process is a method that has been widely studied and applied in the removal of fluoride from drinking water in my country. The main method is to pass the fluorine-containing water through the equipment equipped with fluorine adsorbent, because the fluoride ions have different distributions in the solid and liquid phases on the surface of the adsorbent. coefficient, so that the adsorption affinity of solid substances for fluorine in water can be used to achieve the effect of fluorine removal, and the adsorbent can recover its adsorption capacity through regeneration. The adsorption method is mainly used to treat low-concentration fluoride-containing water, and can also be used as an advanced treatment method for fluoride-containing water. The adsorbent can be filled into the packed column, and the dynamic adsorption method is adopted. The operation is simple, the fluoride removal effect is relatively stable, and the cost is low. It has become the most widely used fluoride removal process at home and abroad.
除氟效果的好坏主要受吸附材料的制约。常用的吸附材料主要包括：含铝吸附剂（如活性氧化铝）、碳质材料（如活性碳、骨炭、碳纳米管）、生物类（如壳聚糖）、天然矿物类、以及基于这些材料所做的一些改性吸附剂，其中得到普遍肯定的是活性氧化铝除氟剂及其改性材料。但这些吸附剂存在着价格昂贵、吸附容量低或者吸附剂溶出等问题。The quality of defluoridation effect is mainly restricted by the adsorption material. Commonly used adsorption materials mainly include: aluminum-containing adsorbents (such as activated alumina), carbonaceous materials (such as activated carbon, bone charcoal, carbon nanotubes), biological (such as chitosan), natural minerals, and materials based on these Some modified adsorbents have been made, among which the activated alumina defluorination agent and its modified materials are generally affirmed. However, these adsorbents have problems such as high price, low adsorption capacity or stripping of the adsorbent.
发明内容Contents of the invention
本发明所要解决的技术问题是提供一种铝改性水滑石除氟吸附剂制备方法，克服现有除氟吸附剂价格昂贵、吸附容量低、吸附剂溶出等缺陷。The technical problem to be solved by the present invention is to provide a preparation method of an aluminum-modified hydrotalcite defluorination adsorbent, which overcomes the defects of the existing defluorination adsorbents such as high price, low adsorption capacity, and dissolution of the adsorbent.
本发明解决上述技术问题的技术方案如下：一种铝改性水滑石除氟吸附剂制备方法，包括以下步骤：The technical scheme of the present invention to solve the above-mentioned technical problems is as follows: a method for preparing an aluminum-modified hydrotalcite defluoridation adsorbent, comprising the following steps:
1）将水滑石粉末与铝酸盐或偏铝酸盐以1000:0.27～54的质量配比配制为反应体系，加热并保持反应温度在60～95℃，搅拌条件下反应，其中所述铝酸盐及偏铝酸盐以铝元素的质量计算；1) Prepare hydrotalcite powder and aluminate or metaaluminate at a mass ratio of 1000:0.27-54 as a reaction system, heat and keep the reaction temperature at 60-95°C, and react under stirring conditions, wherein the aluminum Salt and metaaluminate are calculated by the mass of aluminum element;
2）反应完毕，分离得到固体产物，水洗烘干、煅烧，即制得改性水滑石除氟吸附剂。2) After the reaction is completed, the solid product is separated, washed with water, dried, and calcined to obtain a modified hydrotalcite defluorination adsorbent.
本发明的有益效果是：采用本发明的方法制备吸附剂对氟具良好吸附效能，可实现含氟源水经处理达到饮用水标准且分离性能良好。The beneficial effect of the present invention is that: the adsorbent prepared by the method of the present invention has good adsorption performance on fluorine, and the treated fluorine-containing source water can reach the standard of drinking water and has good separation performance.
在上述技术方案的基础上，本发明还可以做如下改进。On the basis of the above technical solutions, the present invention can also be improved as follows.
进一步，所述水滑石粉末包括天然水滑石或/和人工合成水滑石。Further, the hydrotalcite powder includes natural hydrotalcite or/and synthetic hydrotalcite.
进一步，步骤1）所述搅拌条件下反应时间为1～10小时。Further, the reaction time under the stirring condition in step 1) is 1-10 hours.
进一步，步骤2）所述的煅烧为100～350℃Further, the calcination in step 2) is at 100-350°C
进一步，步骤2）所述的煅烧时间为1～5小时，Further, the calcination time in step 2) is 1 to 5 hours,
具体实施方式Detailed ways
结合以下实施例对本发明的原理和特征进行描述，所举实例只用于解释本发明，并非用于限定本发明的范围。The principles and features of the present invention are described in conjunction with the following examples, which are only used to explain the present invention, and are not intended to limit the scope of the present invention.
实施例1Example 1
本发明一种铝改性水滑石除氟吸附剂制备方法，包括以下步骤：将天然水滑石和人工合成水滑石与铝酸盐或偏铝酸盐以1000:0.27的重量配比为配制反应体系，加热并保持反应温度在60℃，搅拌条件下反应时间为1小时，其中所述铝酸盐及偏铝酸盐以铝元素的质量计算；反应完毕，分离得到固体产物，水洗烘干，在100℃煅烧4小时，即制得改性水滑石除氟吸附剂。A method for preparing an aluminum-modified hydrotalcite defluoridation adsorbent of the present invention comprises the following steps: using natural hydrotalcite and artificial synthetic hydrotalcite and aluminate or metaaluminate as a preparation reaction system in a weight ratio of 1000:0.27 , heating and keeping the reaction temperature at 60°C, the reaction time is 1 hour under stirring conditions, wherein the aluminate and metaaluminate are calculated by the mass of aluminum element; after the reaction is completed, the solid product is separated, washed with water and dried in Calcined at 100°C for 4 hours, the modified hydrotalcite defluoride adsorbent was prepared.
实施例2Example 2
本发明一种铝改性水滑石除氟吸附剂制备方法，包括以下步骤：将天然水滑石与铝酸盐或偏铝酸盐以1000:10的重量配比为配制反应体系，加热并保持反应温度在70℃，搅拌条件下反应时间为2小时，其中所述铝酸盐及偏铝酸盐以铝元素的质量计算）；反应完毕，分离得到固体产物，水洗烘干，在150℃煅烧3小时，即制得改性水滑石除氟吸附剂。A method for preparing an aluminum-modified hydrotalcite defluoridation adsorbent of the present invention comprises the following steps: using natural hydrotalcite and aluminate or metaaluminate as a preparation reaction system in a weight ratio of 1000:10, heating and maintaining the reaction The temperature is 70°C, and the reaction time is 2 hours under stirring conditions, wherein the aluminate and metaaluminate are calculated by the mass of aluminum element); after the reaction is completed, the solid product is separated, washed with water and dried, and calcined at 150°C for 3 Hours, the modified hydrotalcite defluoride adsorbent is prepared.
实施例3Example 3
本发明一种铝改性水滑石除氟吸附剂制备方法，包括以下步骤：将人工合成水滑石与铝酸盐或偏铝酸盐以1000:1的重量配比为配制反应体系，加热并保持反应温度在65℃，搅拌条件下反应时间为5小时，其中所述铝酸盐及偏铝酸盐以铝元素的质量计算；反应完毕，分离得到固体产物，水洗烘干，在250℃煅烧2小时，即制得改性水滑石除氟吸附剂。A method for preparing an aluminum-modified hydrotalcite defluoridation adsorbent of the present invention comprises the following steps: using artificially synthesized hydrotalcite and aluminate or metaaluminate as a preparation reaction system in a weight ratio of 1000:1, heating and maintaining The reaction temperature is 65°C, and the reaction time is 5 hours under stirring conditions, wherein the aluminate and metaaluminate are calculated by the mass of aluminum element; after the reaction is completed, the solid product is separated, washed with water and dried, and calcined at 250°C for 2 Hours, the modified hydrotalcite defluoride adsorbent is prepared.
实施例4Example 4
一种铝改性水滑石除氟吸附剂制备方法，包括以下步骤：将天然水滑石和人工合成水滑石与铝酸盐或偏铝酸盐以1000:30的重量配比为配制反应体系，加热并保持反应温度在80℃，搅拌条件下反应时间为7小时，其中所述铝酸盐及偏铝酸盐以铝元素的质量计算；反应完毕，分离得到固体产物，水洗烘干，在350℃煅烧1小时，即制得改性水滑石除氟吸附剂。A method for preparing an aluminum-modified hydrotalcite defluoridation adsorbent, comprising the following steps: preparing a reaction system of natural hydrotalcite and synthetic hydrotalcite and aluminate or metaaluminate in a weight ratio of 1000:30, heating And keep the reaction temperature at 80°C, and the reaction time is 7 hours under stirring conditions, wherein the aluminate and metaaluminate are calculated by the mass of aluminum element; after the reaction is completed, the solid product is separated, washed with water and dried, and heated at 350°C After calcining for 1 hour, the modified hydrotalcite defluorination adsorbent is prepared.
实施例5Example 5
本发明一种铝改性水滑石除氟吸附剂制备方法，包括以下步骤：将天然水滑石和人工合成水滑石与铝酸盐或偏铝酸盐以1000:54的重量配比为配制反应体系，加热并保持反应温度在95℃，搅拌条件下反应时间为9小时，其中所述铝酸盐及偏铝酸盐以铝元素的质量计算；反应完毕，分离得到固体产物，水洗烘干，在300℃煅烧2小时，即制得改性水滑石除氟吸附剂。A method for preparing an aluminum-modified hydrotalcite defluoridation adsorbent of the present invention comprises the following steps: using natural hydrotalcite and synthetic hydrotalcite and aluminate or metaaluminate in a weight ratio of 1000:54 as a preparation reaction system , heating and keeping the reaction temperature at 95°C, and the reaction time under stirring conditions is 9 hours, wherein the aluminate and metaaluminate are calculated by the mass of aluminum element; after the reaction is completed, the solid product is separated, washed with water and dried in Calcined at 300°C for 2 hours to obtain the modified hydrotalcite defluorination adsorbent.
实施例6Example 6
本发明一种铝改性水滑石除氟吸附剂制备方法，包括以下步骤：将天然水滑石和人工合成水滑石与铝酸盐或偏铝酸盐以1000:40的重量配比为配制反应体系，加热并保持反应温度在75℃，搅拌条件下反应时间为6小时，其中所述铝酸盐及偏铝酸盐以铝元素的质量计算；反应完毕，分离得到固体产物，水洗烘干，在200℃煅烧3小时，即制得改性水滑石除氟吸附剂。A method for preparing an aluminum-modified hydrotalcite defluoridation adsorbent of the present invention comprises the following steps: using natural hydrotalcite and artificial synthetic hydrotalcite and aluminate or metaaluminate in a weight ratio of 1000:40 as a preparation reaction system , heating and keeping the reaction temperature at 75°C, and the reaction time under stirring conditions is 6 hours, wherein the aluminate and metaaluminate are calculated by the mass of aluminum element; after the reaction is completed, the solid product is separated, washed with water and dried in Calcined at 200°C for 3 hours to obtain the modified hydrotalcite defluorination adsorbent.
实施例7Example 7
本发明一种铝改性水滑石除氟吸附剂制备方法，包括以下步骤：将天然水滑石和人工合成水滑石与铝酸盐或偏铝酸盐以1000:35的重量配比为配制反应体系，加热并保持反应温度在95℃，搅拌条件下反应时间为7.5小时，其中所述铝酸盐及偏铝酸盐以铝元素的质量计算；反应完毕，分离得到固体产物，水洗烘干，在220℃煅烧3.5小时，即制得改性水滑石除氟吸附剂。A method for preparing an aluminum-modified hydrotalcite defluoridation adsorbent of the present invention comprises the following steps: using natural hydrotalcite and artificial synthetic hydrotalcite and aluminate or metaaluminate in a weight ratio of 1000:35 as a preparation reaction system , heating and keeping the reaction temperature at 95°C, and the reaction time under stirring conditions is 7.5 hours, wherein the aluminate and metaaluminate are calculated by the mass of aluminum element; after the reaction is completed, the solid product is separated, washed with water and dried in Calcined at 220°C for 3.5 hours, the modified hydrotalcite defluoride adsorbent was prepared.
实施例8Example 8
本发明一种铝改性水滑石除氟吸附剂制备方法，包括以下步骤：将天然水滑石和人工合成水滑石与铝酸盐或偏铝酸盐以1000:45的重量配比为配制反应体系，加热并保持反应温度在95℃，搅拌条件下反应时间为8小时，其中所述铝酸盐及偏铝酸盐以铝元素的质量计算；反应完毕，分离得到固体产物，水洗烘干，在180℃煅烧4.5小时，即制得改性水滑石除氟吸附剂。A method for preparing an aluminum-modified hydrotalcite defluoridation adsorbent of the present invention comprises the following steps: using natural hydrotalcite and artificial synthetic hydrotalcite and aluminate or metaaluminate in a weight ratio of 1000:45 as a preparation reaction system , heating and keeping the reaction temperature at 95°C, and the reaction time under stirring conditions is 8 hours, wherein the aluminate and metaaluminate are calculated by the mass of aluminum element; after the reaction is completed, the solid product is separated, washed with water and dried in Calcined at 180°C for 4.5 hours, the modified hydrotalcite defluoride adsorbent was prepared.
实施例9Example 9
本发明一种铝改性水滑石除氟吸附剂制备方法，包括以下步骤：将天然水滑石和人工合成水滑石与铝酸盐或偏铝酸盐以1000:5的重量配比为配制反应体系，加热并保持反应温度在65℃，搅拌条件下反应时间为6小时，其中所述铝酸盐及偏铝酸盐以铝元素的质量计算；反应完毕，分离得到固体产物，水洗烘干，在200℃煅烧2.5小时，即制得改性水滑石除氟吸附剂。A method for preparing an aluminum-modified hydrotalcite defluoridation adsorbent of the present invention comprises the following steps: using natural hydrotalcite and artificial synthetic hydrotalcite and aluminate or metaaluminate in a weight ratio of 1000:5 as a preparation reaction system , heating and keeping the reaction temperature at 65°C, and the reaction time under stirring conditions is 6 hours, wherein the aluminate and metaaluminate are calculated by the mass of aluminum element; after the reaction is completed, the solid product is separated and washed with water and dried in Calcined at 200°C for 2.5 hours, the modified hydrotalcite defluoride adsorbent was prepared.
采用活性氧化铝及实施例1至8制备的一种铝改性水滑石除氟吸附剂制备方法制备的吸附剂吸附氟实验效果数据见表1。其中，对氟饱和吸附容量是将吸附剂在温度20℃、pH为6.5±0.1条件下对氟吸附等温线进行Langmuir吸附等温线拟合计算得到。Table 1 shows the experimental effect data of the adsorbent prepared by using activated alumina and an aluminum-modified hydrotalcite defluoridation adsorbent prepared in Examples 1 to 8. Among them, the saturated adsorption capacity for fluorine is obtained by fitting the Langmuir adsorption isotherm to the fluorine adsorption isotherm of the adsorbent at a temperature of 20°C and a pH of 6.5±0.1.
对比实施例：采用活性氧化铝吸附氟的实验效果。Comparative example: the experimental effect of using activated alumina to adsorb fluorine.
表1：活性氧化铝及实施例1至9制备的一种铝改性水滑石除氟吸附剂制备方法制备的吸附剂吸附效果比较Table 1: Comparison of adsorbent adsorption effect prepared by activated alumina and an aluminum-modified hydrotalcite defluoridation adsorbent prepared in Examples 1 to 9
结论：本发明制备的除氟吸附剂除氟效能优于目前市售吸附剂活性氧化铝。Conclusion: The fluoride removal performance of the fluorine removal adsorbent prepared by the present invention is better than that of the currently commercially available adsorbent activated alumina.
以上所述仅为本发明的较佳实施例，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。The above descriptions are only preferred embodiments of the present invention, and are not intended to limit the present invention. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principles of the present invention shall be included in the protection of the present invention. within range.
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