CN101780401A - Preparation method of zirconium phosphate intercalation material for adsorbing phenol - Google Patents
Preparation method of zirconium phosphate intercalation material for adsorbing phenol Download PDFInfo
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- CN101780401A CN101780401A CN200910234362A CN200910234362A CN101780401A CN 101780401 A CN101780401 A CN 101780401A CN 200910234362 A CN200910234362 A CN 200910234362A CN 200910234362 A CN200910234362 A CN 200910234362A CN 101780401 A CN101780401 A CN 101780401A
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- 229910000166 zirconium phosphate Inorganic materials 0.000 title claims abstract description 30
- LEHFSLREWWMLPU-UHFFFAOYSA-B zirconium(4+);tetraphosphate Chemical compound [Zr+4].[Zr+4].[Zr+4].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LEHFSLREWWMLPU-UHFFFAOYSA-B 0.000 title claims abstract description 19
- 230000002687 intercalation Effects 0.000 title claims abstract description 17
- 238000009830 intercalation Methods 0.000 title claims abstract description 17
- 239000000463 material Substances 0.000 title claims abstract description 13
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 title abstract description 46
- 238000002360 preparation method Methods 0.000 title abstract description 3
- 239000007864 aqueous solution Substances 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 150000004982 aromatic amines Chemical class 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 8
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 3
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 14
- 239000007787 solid Substances 0.000 claims description 9
- 150000001412 amines Chemical class 0.000 claims 3
- 238000001179 sorption measurement Methods 0.000 abstract description 10
- -1 aliphatic amine Amines Chemical class 0.000 abstract description 4
- 229920002994 synthetic fiber Polymers 0.000 abstract description 2
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 description 14
- 239000002131 composite material Substances 0.000 description 12
- 239000002351 wastewater Substances 0.000 description 12
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 8
- 150000002989 phenols Chemical class 0.000 description 8
- 239000003463 adsorbent Substances 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 239000012153 distilled water Substances 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000011229 interlayer Substances 0.000 description 3
- IOQPZZOEVPZRBK-UHFFFAOYSA-N octan-1-amine Chemical compound CCCCCCCCN IOQPZZOEVPZRBK-UHFFFAOYSA-N 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
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- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 238000006065 biodegradation reaction Methods 0.000 description 1
- 238000010170 biological method Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
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- 210000003169 central nervous system Anatomy 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
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- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明一种磷酸锆插层材料的制备方法，按照下述步骤进行，在重量百分比1～30％脂肪胺或芳香胺水溶液中加入α-磷酸锆，其中α-磷酸锆与脂肪胺或芳香胺水溶液的固液比以质量与体积比计为1∶40～1∶100，搅拌反应1～4小时，经去离子水洗涤，干燥后形成脂肪胺或芳香胺的插层材料，其中所述脂肪胺为C4～C8的脂肪胺。本发明与现有技术相比具有下列优点：苯酚吸附材料合成材料易得，合成路线简便。吸附苯酚速率快，20分钟即可以达到吸附平衡。
The preparation method of a zirconium phosphate intercalation material of the present invention is carried out according to the following steps, adding α-zirconium phosphate to an aqueous solution of 1 to 30% by weight of aliphatic amine or aromatic amine, wherein α-zirconium phosphate and aliphatic amine or aromatic amine The solid-to-liquid ratio of the aqueous solution is 1:40 to 1:100 in terms of mass and volume ratio, stirred and reacted for 1 to 4 hours, washed with deionized water, and dried to form an intercalation material of aliphatic amine or aromatic amine, wherein the aliphatic amine Amines are C 4 -C 8 aliphatic amines. Compared with the prior art, the present invention has the following advantages: the synthetic material of the phenol adsorption material is easy to obtain, and the synthetic route is simple and convenient. The adsorption rate of phenol is fast, and the adsorption equilibrium can be reached within 20 minutes.
Description
技术领域technical field
本发明涉及一种吸附苯酚的磷酸锆插层材料的制备方法The invention relates to a preparation method of a zirconium phosphate intercalation material that adsorbs phenol
背景技术Background technique
苯酚类主要来自炼焦、炼油、制造煤气、酚、绝缘材料、药品和纸张等生产过程中排出的废物。低浓度苯酚能使蛋白变性，高浓度的苯酚能使蛋白沉淀。对皮肤、粘膜有强烈的腐蚀作用，也可抑制中枢神经系统或损害肝、肾功能。含苯酚废水一旦排出，便会挥发进入大气或渗入地下，污染大气、地下水和农作物。酚类化合物的稳定性强，自然降解时间漫长，将会对土壤和地下水造成永久性破环。按中国《生活饮用水卫生标准》规定饮用水中挥发性酚类不得超过0.002毫克/升；《工业企业设计卫生标准》规定，地面水中挥发性酚类的最高容许浓度为0.01毫克/升；规定含挥发性酚废水最高容许排放浓度为0.5毫克/升。Phenols mainly come from coking, oil refining, manufacturing gas, phenol, insulating materials, pharmaceuticals, and paper wastes. Low concentrations of phenol can denature proteins, while high concentrations of phenol can precipitate proteins. It has a strong corrosive effect on the skin and mucous membranes, and can also inhibit the central nervous system or damage the liver and kidney functions. Once phenol-containing wastewater is discharged, it will volatilize into the atmosphere or seep into the ground, polluting the atmosphere, groundwater and crops. Phenolic compounds are highly stable and take a long time to naturally degrade, which will cause permanent damage to soil and groundwater. According to China's "Drinking Water Hygienic Standards", the volatile phenols in drinking water shall not exceed 0.002 mg/L; the "Industrial Enterprise Design Hygienic Standards" stipulates that the maximum allowable concentration of volatile phenols in surface water is 0.01 mg/L; The maximum allowable discharge concentration of wastewater containing volatile phenols is 0.5 mg/L.
目前工业上对含酚废水主要有下列处理方法：蒸馏气提法，主要根据挥发性酚类化合物与水蒸气形成共沸化合物，利用酚在两相中的浓度差将酚水分离，从而使水得以净化。适合高浓度的含酚废水，去除率在80％～85％，处理完后含少量残酚的废水需再输入电化学电解设备进一步脱酚处理。该方法成本较高。光催化降解法，利用氧化钛光催化剂在紫外光的照射下对水的苯酚进行光催化降解处理，例如专利200610069447.X将纳米二氧化钛粉体固定于活性炭纤维表面，在紫外光照下，可将水溶液中苯酚污染物消除，专利200710037911.1制备了TiO2多孔微管，可以高效降解水体中苯酚为水和二氧化碳。生物法降解法，利用生物菌对水中的苯酚进行降解去除，例如专利01113915.3采用生物工程菌去除或降解酚含量很高的工业废水，专利200710056322.8使苯酚废水通过生物膜电极反应器处理浓度为100～300mg·L-1的苯酚废水。一般而言，生物法比较适合于低浓度含酚废水的处理，高浓度高毒性含酚废水对微生物的繁殖生长有较强的抑止和毒害作用。目前应用较为广泛的去处水中苯酚的方法是吸附法，吸附法利用一些多孔吸附剂较高的比表面积表现出的较强吸附性能将废水中的酚类物质吸附。常用的吸附剂主要有活性炭、大孔吸附树脂及有机合成吸附剂等，例如发明专利200510037861.8将硝基化大孔树脂用于含酚废水的处理，可以使废水含酚量降低到0.5ppm的排放标准。专利85108327用活性炭作为苯酚吸附剂，使酚处理后的含量＜0.5mg/L，而专利200310109698.2则将金属催化剂负载在活性炭上，在吸附苯酚的同时进行催化降解。At present, there are mainly the following treatment methods for phenol-containing wastewater in industry: Distillation and gas stripping, mainly based on the formation of azeotropic compounds between volatile phenolic compounds and water vapor, and the separation of phenol and water by using the concentration difference of phenol in the two phases, so that the water be purified. It is suitable for high-concentration phenol-containing wastewater, and the removal rate is 80% to 85%. After treatment, the wastewater containing a small amount of residual phenol needs to be input into electrochemical electrolysis equipment for further dephenolization treatment. This method is costly. Photocatalytic degradation method, using titanium oxide photocatalyst to photocatalytically degrade phenol in water under the irradiation of ultraviolet light, such as patent 200610069447. In the elimination of phenol pollutants, the patent 200710037911.1 prepared TiO 2 porous microtubes, which can efficiently degrade phenol in water into water and carbon dioxide. Biodegradation method, using biological bacteria to degrade and remove phenol in water, for example, patent 01113915.3 uses bioengineering bacteria to remove or degrade industrial wastewater with high phenol content, and patent 200710056322.8 makes phenol wastewater pass through a biofilm electrode reactor to treat the concentration of 100~ 300mg·L -1 phenol wastewater. Generally speaking, the biological method is more suitable for the treatment of low-concentration phenol-containing wastewater, and high-concentration and highly toxic phenol-containing wastewater has a strong inhibitory and toxic effect on the reproduction and growth of microorganisms. At present, the widely used method for removing phenol in water is the adsorption method. The adsorption method uses the strong adsorption performance of some porous adsorbents with high specific surface area to adsorb the phenolic substances in the wastewater. Commonly used adsorbents mainly include activated carbon, macroporous adsorbent resin and organic synthetic adsorbent, etc. For example, in the invention patent 200510037861.8, the nitrated macroporous resin is used for the treatment of phenol-containing wastewater, which can reduce the phenol content of wastewater to 0.5ppm. standard. Patent 85108327 uses activated carbon as a phenol adsorbent to make the content of phenol less than 0.5mg/L after treatment, while patent 200310109698.2 loads a metal catalyst on activated carbon to degrade phenol while adsorbing it.
在上述诸多的苯酚处理方法中，吸附法以可再生性及成本低的优势，一直是研究者关注的热点。α-磷酸锆，Zr(HPO4)2·H2O(简称α-ZrP)具有纳米级层间距，其基本结构规整，同一平面上的原子之间以牢固的共价键结合，相邻层与层之间存在范德华力。由于层与层之间弱的作用力，这使得层间距具有可调性，通过插入数量不同、种类各异的客体，使层间距增大，形成的插层化合物可应用在异相催化、特异吸附剂等众多领域。利用直接插层技术或胶体化插层技术将丁胺，辛胺等脂肪胺或苯胺等芳香族胺插入到α-磷酸锆的层间，可以快速吸附水溶液中的苯酚化合物，是一种有发展前途的苯酚类化合物吸附材料。Among the many phenol treatment methods mentioned above, the adsorption method has always been the focus of researchers because of its advantages of reproducibility and low cost. α-zirconium phosphate, Zr(HPO 4 ) 2 ·H 2 O (abbreviated as α-ZrP) has a nanoscale layer spacing, its basic structure is regular, atoms on the same plane are bonded by strong covalent bonds, and adjacent layers There are van der Waals forces between the layers. Due to the weak force between layers, this makes the interlayer spacing adjustable. By inserting different numbers and types of guests, the interlayer spacing is increased, and the intercalation compounds formed can be used in heterogeneous catalysis, specific Adsorbents and many other fields. Using direct intercalation technology or colloidal intercalation technology to insert aliphatic amines such as butylamine and octylamine or aromatic amines such as aniline into the interlayer of α-zirconium phosphate can quickly adsorb phenol compounds in aqueous solution. Promising adsorbent materials for phenolic compounds.
发明内容Contents of the invention
本发明目的是为了克服上述现有技术中的不足，提供一种吸附苯酚的磷酸锆插层材料的制备方法。The object of the present invention is to provide a method for preparing a zirconium phosphate intercalation material that adsorbs phenol in order to overcome the above-mentioned deficiencies in the prior art.
本发明采用的技术方案如下：The technical scheme that the present invention adopts is as follows:
一种磷酸锆插层材料的制备方法，在重量百分比1～30％脂肪胺(C4～C8)或芳香胺水溶液中加入α-磷酸锆，固液比为1∶40～1∶100(质量与体积比)，搅拌反应1～4小时，经去离子水洗涤，干燥后形成脂肪胺或芳香胺插层材料，该脂肪胺或芳香胺插层磷酸锆材料可以有效吸附水溶液中苯酚。A method for preparing a zirconium phosphate intercalation material, comprising adding α-zirconium phosphate to an aqueous solution of 1 to 30% by weight of aliphatic amine (C 4 to C 8 ) or aromatic amine, with a solid-to-liquid ratio of 1:40 to 1:100 ( mass to volume ratio), stirred and reacted for 1 to 4 hours, washed with deionized water, and dried to form an aliphatic amine or aromatic amine intercalation material, which can effectively adsorb phenol in aqueous solution.
由于上述技术方案运用，本发明与现有技术相比具有下列优点：Due to the use of the above-mentioned technical solutions, the present invention has the following advantages compared with the prior art:
1、苯酚吸附材料合成材料易得，合成路线简便。1. Phenol adsorption material The synthetic material is easy to obtain, and the synthetic route is simple.
2、吸附苯酚速率快，20分钟即可以达到吸附平衡。2. The adsorption rate of phenol is fast, and the adsorption equilibrium can be reached within 20 minutes.
附图说明Description of drawings
附图1为本发明实施例一制备的丁胺插层的磷酸锆复合材料的XRD图谱(纵坐标为衍射强度，横坐标为扫描2θ角)Accompanying drawing 1 is the XRD pattern of the zirconium phosphate composite material of the butylamine intercalation prepared by the embodiment of the present invention (the ordinate is the diffraction intensity, and the abscissa is the scanning 2θ angle)
附图2为本发明实施例三制备的苯胺插层的磷酸锆复合材料的XRD图谱(纵坐标为衍射强度，横坐标为扫描2θ角)Accompanying drawing 2 is the XRD pattern of the zirconium phosphate composite material of the aniline intercalation prepared by the embodiment of the present invention three (the ordinate is the diffraction intensity, and the abscissa is the scanning 2θ angle)
具体实施方式Detailed ways
下面结合附图及实施例对本发明作进一步描述：The present invention will be further described below in conjunction with accompanying drawing and embodiment:
实施例一：称取α-磷酸锆约2g放入到100ml烧杯中，加入重量百分比为6％的丁胺水溶液80ml，常温下搅拌反应4小时，过滤，蒸馏水充分洗涤3次，液固分离，室温干燥24小时，得到丁胺插层的磷酸锆复合材料。Example 1: Weigh about 2 g of α-zirconium phosphate and put it into a 100 ml beaker, add 80 ml of 6% butylamine aqueous solution, stir and react at room temperature for 4 hours, filter, fully wash with distilled water 3 times, separate liquid and solid, Dry at room temperature for 24 hours to obtain a zirconium phosphate composite material intercalated with butylamine.
称取按上述条件制备的磷酸锆复合材料1.5g，放入到100ml苯酚浓度为1000ppm的水溶液中，在震荡器中常温震荡15分种，液固分离后，利用紫外光度仪在270nm测定水溶液中苯酚浓度，结果表明水溶液中苯酚浓度小于5ppm。Weigh 1.5g of the zirconium phosphate composite material prepared according to the above conditions, put it into 100ml of an aqueous solution with a phenol concentration of 1000ppm, shake it in an oscillator at room temperature for 15 minutes, and after liquid-solid separation, use a UV photometer to measure the concentration of the aqueous solution at 270nm. Phenol concentration, the results show that the phenol concentration in the aqueous solution is less than 5ppm.
附图1为本发明实施例一制备的丁胺插层的磷酸锆复合材料的XRD图谱(纵坐标为衍射强度，横坐标为扫描2θ角)；Accompanying drawing 1 is the XRD spectrum of the zirconium phosphate composite material of the butylamine intercalation prepared by the embodiment of the present invention (the ordinate is the diffraction intensity, and the abscissa is the scanning 2θ angle);
实施例二：称取α-磷酸锆约2g放入到100ml烧杯中，加入重量百分比为8％的辛胺水溶液80ml，常温下搅拌反应4小时，过滤，蒸馏水充分洗涤3次，液固分离，室温干燥24小时，得到辛胺插层的磷酸锆复合材料。Embodiment 2: Weigh about 2 g of α-zirconium phosphate and put it into a 100 ml beaker, add 80 ml of 8% octylamine aqueous solution by weight percentage, stir and react at room temperature for 4 hours, filter, fully wash with distilled water 3 times, separate liquid and solid, Dry at room temperature for 24 hours to obtain a zirconium phosphate composite material intercalated with octylamine.
称取按上述条件制备的磷酸锆复合材料1g，放入到100ml苯酚浓度为1000ppm的水溶液中，在震荡器中常温震荡20分种，液固分离后，利用紫外光度仪在270nm测定水溶液中苯酚浓度，结果表明水溶液中苯酚浓度小于5ppm。Weigh 1g of the zirconium phosphate composite material prepared according to the above conditions, put it into 100ml of an aqueous solution with a phenol concentration of 1000ppm, shake it in an oscillator at room temperature for 20 minutes, and after liquid-solid separation, use a UV photometer to measure the phenol in the aqueous solution at 270nm. Concentration, the results show that the concentration of phenol in the aqueous solution is less than 5ppm.
实施例三：称取α-磷酸锆约2g放入到100ml烧杯中，加入重量百分比为10％的苯胺水溶液80ml，常温下搅拌反应4小时，过滤，蒸馏水充分洗涤3次，液固分离，室温干燥24小时，得到苯胺插层的磷酸锆复合材料。Example 3: Weigh about 2g of α-zirconium phosphate and put it into a 100ml beaker, add 80ml of aniline aqueous solution with a weight percentage of 10%, stir and react at room temperature for 4 hours, filter, fully wash with distilled water 3 times, separate liquid and solid, and store at room temperature After drying for 24 hours, an aniline-intercalated zirconium phosphate composite material was obtained.
称取按上述条件制备的磷酸锆复合材料1.5g，放入到100ml苯酚浓度为1000ppm的水溶液中，在震荡器中常温震荡20分种，液固分离后，利用紫外光度仪在270nm测定水溶液中苯酚浓度，结果表明水溶液中苯酚浓度小于5ppm。Weigh 1.5g of the zirconium phosphate composite material prepared according to the above conditions, put it into 100ml of an aqueous solution with a phenol concentration of 1000ppm, shake it in an oscillator at room temperature for 20 minutes, and after the liquid and solid are separated, use a UV photometer to measure the concentration in the aqueous solution at 270nm. Phenol concentration, the results show that the phenol concentration in the aqueous solution is less than 5ppm.
附图2为本发明实施例三制备的苯胺插层的磷酸锆复合材料的XRD图谱(纵坐标为衍射强度，横坐标为扫描2θ角)Accompanying drawing 2 is the XRD pattern of the zirconium phosphate composite material of the aniline intercalation prepared by the embodiment of the present invention three (the ordinate is the diffraction intensity, and the abscissa is the scanning 2θ angle)
实施例四：称取α-磷酸锆约2g放入到250ml烧杯中，加入重量百分比为20％的丁胺水溶液200ml，常温下搅拌反应3小时，过滤，蒸馏水充分洗涤3次，液固分离，室温干燥24小时，得到丁胺插层的磷酸锆复合材料。Embodiment 4: Weigh about 2 g of α-zirconium phosphate and put it into a 250 ml beaker, add 200 ml of butylamine aqueous solution with a weight percentage of 20%, stir and react at room temperature for 3 hours, filter, fully wash with distilled water 3 times, separate liquid and solid, Dry at room temperature for 24 hours to obtain a zirconium phosphate composite material intercalated with butylamine.
称取按上述条件制备的磷酸锆复合材料1.5g，放入到100ml苯酚浓度为1000ppm的水溶液中，在震荡器中常温震荡15分种，液固分离后，利用紫外光度仪在270nm测定水溶液中苯酚浓度，结果表明水溶液中苯酚浓度小于5ppm。Weigh 1.5g of the zirconium phosphate composite material prepared according to the above conditions, put it into 100ml of an aqueous solution with a phenol concentration of 1000ppm, shake it in an oscillator at room temperature for 15 minutes, and after liquid-solid separation, use a UV photometer to measure the concentration of the aqueous solution at 270nm. Phenol concentration, the results show that the phenol concentration in the aqueous solution is less than 5ppm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI550024B (en) * | 2015-01-09 | 2016-09-21 | 中原大學 | Method of producing polyaniline zorcornia nanocomposite and uses thereof |
| CN109134971B (en) * | 2018-08-30 | 2020-08-07 | 西南石油大学 | A kind of anti-aging nitrile rubber composite material based on functional zirconium phosphate modification and preparation method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI550024B (en) * | 2015-01-09 | 2016-09-21 | 中原大學 | Method of producing polyaniline zorcornia nanocomposite and uses thereof |
| CN109134971B (en) * | 2018-08-30 | 2020-08-07 | 西南石油大学 | A kind of anti-aging nitrile rubber composite material based on functional zirconium phosphate modification and preparation method |
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