CN100335416C - Method for preparing rutile type nanometer Ti02 in low temperature using carboxylic acid as finishing agent - Google Patents
Method for preparing rutile type nanometer Ti02 in low temperature using carboxylic acid as finishing agent Download PDFInfo
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- CN100335416C CN100335416C CNB200510038935XA CN200510038935A CN100335416C CN 100335416 C CN100335416 C CN 100335416C CN B200510038935X A CNB200510038935X A CN B200510038935XA CN 200510038935 A CN200510038935 A CN 200510038935A CN 100335416 C CN100335416 C CN 100335416C
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 23
- 150000001732 carboxylic acid derivatives Chemical class 0.000 title 1
- 239000003795 chemical substances by application Substances 0.000 title 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000012153 distilled water Substances 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims abstract description 14
- 239000000243 solution Substances 0.000 claims abstract description 12
- 239000007864 aqueous solution Substances 0.000 claims abstract description 10
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000706 filtrate Substances 0.000 claims abstract description 10
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 claims abstract description 10
- 230000007062 hydrolysis Effects 0.000 claims abstract description 10
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 10
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000003607 modifier Substances 0.000 claims abstract description 10
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 10
- 239000010935 stainless steel Substances 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 239000000725 suspension Substances 0.000 claims abstract description 10
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 8
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims abstract description 7
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims abstract description 7
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims abstract description 5
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims abstract description 5
- 239000005639 Lauric acid Substances 0.000 claims abstract description 5
- 150000001735 carboxylic acids Chemical class 0.000 claims abstract description 5
- 235000019253 formic acid Nutrition 0.000 claims abstract description 5
- 229940074391 gallic acid Drugs 0.000 claims abstract description 5
- 235000004515 gallic acid Nutrition 0.000 claims abstract description 5
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 claims abstract description 3
- 239000005711 Benzoic acid Substances 0.000 claims abstract 2
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims abstract 2
- 235000010233 benzoic acid Nutrition 0.000 claims abstract 2
- 239000002244 precipitate Substances 0.000 claims abstract 2
- 235000002906 tartaric acid Nutrition 0.000 claims abstract 2
- 239000011975 tartaric acid Substances 0.000 claims abstract 2
- 230000032683 aging Effects 0.000 claims description 25
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 6
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims 1
- 239000005977 Ethylene Substances 0.000 claims 1
- 239000012895 dilution Substances 0.000 claims 1
- 238000010790 dilution Methods 0.000 claims 1
- -1 polytetrafluoroethylene Polymers 0.000 claims 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims 1
- 239000004810 polytetrafluoroethylene Substances 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 13
- 239000002245 particle Substances 0.000 abstract description 9
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 abstract description 8
- 235000011187 glycerol Nutrition 0.000 abstract description 4
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 3
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 abstract description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 19
- 239000000047 product Substances 0.000 description 14
- 239000004809 Teflon Substances 0.000 description 8
- 229920006362 Teflon® Polymers 0.000 description 8
- 239000003513 alkali Substances 0.000 description 8
- 239000012065 filter cake Substances 0.000 description 8
- 238000000089 atomic force micrograph Methods 0.000 description 7
- 239000011248 coating agent Substances 0.000 description 7
- 238000000576 coating method Methods 0.000 description 7
- 230000001186 cumulative effect Effects 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 229940013688 formic acid Drugs 0.000 description 3
- 229960005150 glycerol Drugs 0.000 description 3
- 229940033355 lauric acid Drugs 0.000 description 3
- 229940095064 tartrate Drugs 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000001384 succinic acid Substances 0.000 description 2
- 229960005137 succinic acid Drugs 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 150000003608 titanium Chemical class 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 229910000348 titanium sulfate Inorganic materials 0.000 description 1
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Abstract
本发明涉及一种制备金红石型纳米二氧化钛的方法，特指以四氯化钛为原料、添加羧酸、水热合成法制备金红石型纳米二氧化钛的方法，其特征在于：将四氯化钛溶液加入到稀盐酸中稀释，然后逐滴加入碱性水溶液，直到pH值在7以上，加入碱液以后，一边搅拌，一边加入含羟基、羧基的有机物修饰剂，修饰剂为甘油、丁二酸、甲酸、酒石酸、没食子酸、月桂酸、苯甲酸中的一种，在40-80℃老化0.5-3h；用蒸馏水洗涤沉淀至滤液的电导率小于20mS/m；加入硝酸或盐酸和蒸馏水，使得溶液pH在0.7以下，然后在室温下老化1-3小时，将老化后的悬浮液放入聚四氟乙烯衬里的不锈钢水解釜中，在120-220℃反应10-18h后得到金红石型纳米二氧化钛。用此方法制备的金红石型纳米二氧化钛，颗粒粒径小，颗粒粒径大小在15nm～70nm之间。本方法具有反应条件温和、反应易于控制、成本低、工艺和流程简便的优点。The invention relates to a method for preparing rutile nano-titanium dioxide, in particular to a method for preparing rutile nano-titanium dioxide by using titanium tetrachloride as a raw material, adding carboxylic acid, and hydrothermal synthesis, which is characterized in that: titanium tetrachloride solution is added Dilute in dilute hydrochloric acid, and then add alkaline aqueous solution drop by drop until the pH value is above 7. After adding the lye, while stirring, add organic modifiers containing hydroxyl and carboxyl groups. The modifiers are glycerin, succinic acid, formic acid , tartaric acid, gallic acid, lauric acid, benzoic acid, aged at 40-80°C for 0.5-3h; wash the precipitate with distilled water until the conductivity of the filtrate is less than 20mS/m; add nitric acid or hydrochloric acid and distilled water to make the pH of the solution Below 0.7, then aged at room temperature for 1-3 hours, put the aged suspension into a polytetrafluoroethylene-lined stainless steel hydrolysis kettle, and react at 120-220°C for 10-18 hours to obtain rutile nano-titanium dioxide. The rutile nano-titanium dioxide prepared by the method has a small particle size, and the particle size is between 15nm and 70nm. The method has the advantages of mild reaction conditions, easy control of the reaction, low cost, and simple technique and process.
Description
Technical field
The present invention relates to a kind of method for preparing rutile type nano titanic oxide, refer in particular to the carboxylic acid and prepare rutile type nano TiO for modifier low temperature
2Method
Background technology
Nano titanium oxide is widely used in various fields, for example environmental purification, opto-electronic conversion, anti-atomizing, clean surfaces, pigment, makeup and photochemical catalysis etc.The method that many synthesis of nano titanium dioxide are arranged, for example titanium tetrachloride flame oxidation method, anti-glue crystallization process, supercritical CO
2Crystallization process, light assisting sol-gel method, polymer template method, hydrothermal synthesis method.These methods use pure titanium salt, titanium tetrachloride and titanium sulfate etc. as initial reactant usually.The physicochemical property of the nano titanium oxide that different building-up processes is prepared are also different.The shortcoming of these methods is need calcine down at high temperature (1173K-1273K) to obtain nano titanium oxide, consumes a large amount of energy, the aggravation environmental pollution, and the titanium dioxide granule that makes is thick, and size distribution is inhomogeneous.
Summary of the invention
The objective of the invention is to propose a kind of be raw material with the titanium tetrachloride, be the method that modifier, hydrothermal synthesis method prepare rutile type nano titanic oxide by adding the carboxylic acid organism, to overcome above-mentioned drawback.
Its preparation method is as follows:
Titanium tetrachloride solution joined in the dilute hydrochloric acid dilute, dropwise add alkaline aqueous solution then, up to the pH value more than 7, add after the alkali lye, stir on one side, the organism modifier that adds on one side hydroxyl, carboxyl, modifier are a kind of in glycerine, Succinic Acid, formic acid, tartrate, gallic acid, lauric acid, the phenylformic acid, at 40-80 ℃ of aging 0.5-3h; Be precipitated to the specific conductivity of filtrate less than 20mS/m with distilled water wash; Filter cake after handling as stated above is divided into three parts, gets a copy of it and add nitric acid or hydrochloric acid and distilled water, make that pH is below 0.7; At room temperature aging 1-3 hour then.Suspension after aging is put into the stainless steel hydrolysis still of teflon lined, behind 120-220 ℃ of reaction 10-18h, obtain rutile type nano titanic oxide.
With the rutile type nano titanic oxide of this method preparation, grain diameter is little, and the grain diameter size is between 15nm～70nm.Present method has that reaction conditions gentleness, reaction are easy to control, cost is low, the advantage of technology and simple flow.
Description of drawings
Fig. 1: glycerine is the atomic force micrograph of the rutile type nano titanic oxide product of coating materials
Fig. 2: Succinic Acid is the atomic force micrograph of the rutile type nano titanic oxide product of coating materials
Fig. 3: formic acid is the atomic force micrograph of the rutile type nano titanic oxide product of coating materials
Fig. 4: tartrate is the atomic force micrograph of the rutile type nano titanic oxide product of coating materials
Fig. 5: gallic acid is the atomic force micrograph of the rutile type nano titanic oxide product of coating materials
Fig. 6: lauric acid is the atomic force micrograph of the rutile type nano titanic oxide product of coating materials
Fig. 7: phenylformic acid is the atomic force micrograph of the rutile type nano titanic oxide product of coating materials
Embodiment
The present invention will be further described below in conjunction with concrete embodiment.
Example 1
As scheme A1, and measure the 68ml titanium tetrachloride solution, join in the dilute hydrochloric acid that 204ml concentration is 0.5mol/L and dilute, dropwise add the Na of 2.1M/L then
2CO
3The aqueous solution equals 7 up to pH.Add after the alkali lye, stir on one side, add 2.3g glycerine on one side.At 40 ℃ of aging 0.5h.The specific conductivity that is precipitated to filtrate with distilled water wash is that the filter cake after 18mS/m. will handle as stated above is divided into three parts, gets a copy of it and adds nitric acid (60%) and distilled water up to cumulative volume 200ml, and pH is 0.7.At room temperature aging 1 hour then.Suspension after aging is put into the stainless steel hydrolysis still of teflon lined, behind 120 ℃ of reaction 10h., obtain rutile type nano titanic oxide.Product is through the atomic force microscope analysis, and particle diameter is in the 20-55 nanometer, median size 36 nanometers.
Example 2
As scheme A2, and measure the 68ml titanium tetrachloride solution, join in the dilute hydrochloric acid that 204ml concentration is 0.5mol/l and dilute, dropwise add the NaOH aqueous solution of 1.5M/L then, equal 9 up to pH.Add after the alkali lye, stir on one side, add the 4.425g Succinic Acid on one side.At 60 ℃ of aging 1.5h.The specific conductivity that is precipitated to filtrate with distilled water wash is that the filter cake after 17mS/m. will handle as stated above is divided into three parts, gets a copy of it and adds hydrochloric acid (36%) and distilled water up to cumulative volume 200ml, and pH is 0.5.At room temperature aging 3 hours then.Suspension after aging is put into the stainless steel hydrolysis still of teflon lined, behind 200 ℃ of reaction 12h., obtain rutile type nano titanic oxide.Product is through the atomic force microscope analysis, and particle diameter is in the 35-65 nanometer, median size 49 nanometers.
Example 3
As scheme A3, and measure the 68ml titanium tetrachloride solution, join in the dilute hydrochloric acid that 204ml concentration is 0.5mol/l and dilute, dropwise add the NH of 2.0M/L then
3The OH aqueous solution equals 10 up to pH.Add after the alkali lye, stir on one side, add 3.45g formic acid on one side.At 60 ℃ of aging 2h.The specific conductivity that is precipitated to filtrate with distilled water wash is that the filter cake after 15mS/m. will handle as stated above is divided into three parts, gets a copy of it and adds nitric acid (60%) and distilled water up to cumulative volume 200ml, and pH is 0.4.At room temperature aging 2 hours then.Suspension after aging is put into the stainless steel hydrolysis still of teflon lined, behind 210 ℃ of reaction 13h., obtain rutile type nano titanic oxide.Product is through the atomic force microscope analysis, and particle diameter is in the 25-55 nanometer, median size 35 nanometers.
Example 4
As scheme A4, and measure the 68ml titanium tetrachloride solution, join in the dilute hydrochloric acid that 204ml concentration is 0.5mol/l and dilute, dropwise add the Na of 2.1M/L then
2CO
3The aqueous solution equals 12 up to pH.Add after the alkali lye, stir on one side, add 2.81g tartrate on one side.At 80 ℃ of aging 2h.The specific conductivity that is precipitated to filtrate with distilled water wash is that the filter cake after 19mS/m. will handle as stated above is divided into three parts, gets a copy of it and adds nitric acid (60%) and distilled water up to cumulative volume 200ml, and pH is 0.2.At room temperature aging 1 hour then.Suspension after aging is put into the stainless steel hydrolysis still of teflon lined, behind 150 ℃ of reaction 15h., obtain rutile type nano titanic oxide.Product is through the atomic force microscope analysis, and particle diameter is in the 35-60 nanometer, median size 46 nanometers.
Example 5
As scheme A5, and measure the 68ml titanium tetrachloride solution, join in the dilute hydrochloric acid that 204ml concentration is 0.5mol/l and dilute, dropwise add the Na of 2.1M/L then
2CO
3The aqueous solution equals 13 up to pH.Add after the alkali lye, stir on one side, add the 3.19g gallic acid on one side.At 60 ℃ of aging 2.5h.The specific conductivity that is precipitated to filtrate with distilled water wash is that the filter cake after 16mS/m. will handle as stated above is divided into three parts, gets a copy of it and adds nitric acid (60%) and distilled water up to cumulative volume 200ml, and pH is 0.1.At room temperature aging 3 hours then.Suspension after aging is put into the stainless steel hydrolysis still of teflon lined, behind 220 ℃ of reaction 16h., obtain rutile type nano titanic oxide.Product is through the atomic force microscope analysis, and particle diameter is in the 10-40 nanometer, median size 20 nanometers.
Example 6
As scheme A6, and measure the 68ml titanium tetrachloride solution, join in the dilute hydrochloric acid that 204ml concentration is 0.5mol/l and dilute, dropwise add the Na of 2.1M/L then
2CO
3The aqueous solution equals 10 up to pH.Add after the alkali lye, stir on one side, add the 15g lauric acid on one side.At 60 ℃ of aging 3h.The specific conductivity that is precipitated to filtrate with distilled water wash is that the filter cake after 18mS/m. will handle as stated above is divided into three parts, gets a copy of it and adds hydrochloric acid (36%) and distilled water up to cumulative volume 200ml, and pH is 0.6.At room temperature aging 3 hours then.Suspension after aging is put into the stainless steel hydrolysis still of teflon lined, behind 130 ℃ of reaction 17h., obtain rutile type nano titanic oxide.Product is through the atomic force microscope analysis, and particle diameter is in the 20-45 nanometer, median size 31 nanometers.
Example 7
As scheme A7, and measure the 68ml titanium tetrachloride solution, join in the dilute hydrochloric acid that 204ml concentration is 0.5mol/l and dilute, dropwise add the Na of 2.1M/L then
2CO
3The aqueous solution equals 10 up to pH.Add after the alkali lye, stir on one side, add the 9.15g phenylformic acid on one side.At 80 ℃ of aging 1h.The specific conductivity that is precipitated to filtrate with distilled water wash is that the filter cake after 17mS/m. will handle as stated above is divided into three parts, gets a copy of it and adds nitric acid (60%) and distilled water up to cumulative volume 200ml, and pH is 0.1.At room temperature aging 3 hours then.Suspension after aging is put into the stainless steel hydrolysis still of teflon lined, behind 160 ℃ of reaction 18h., obtain rutile type nano titanic oxide.Product is through the atomic force microscope analysis, and particle diameter is in the 15-40 nanometer, median size 26 nanometers.
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN100537433C (en) * | 2006-04-30 | 2009-09-09 | 中国科学院合肥物质科学研究院 | Preparation method of rutile titanium dioxide nanopowder |
| CN101148538B (en) * | 2006-09-23 | 2010-08-11 | 宁波荣山新型材料有限公司 | Method for preparing nano titanium dioxide modified polyurethane material and products thereof |
| CN101456583B (en) * | 2007-12-12 | 2011-05-25 | 中国科学院理化技术研究所 | Synthetic method for preparing rutile type nano titanium dioxide sol or powder at low temperature |
| CN101823766B (en) * | 2010-05-17 | 2012-01-18 | 山东理工大学 | Preparation method of hafnium oxide powder with nano-porous structure |
| EP2607318B1 (en) * | 2010-08-17 | 2017-12-06 | Sakai Chemical Industry Co., Ltd. | Method for producing dispersion of rutile-type titanium oxide particles |
| CN102383180B (en) * | 2011-10-24 | 2013-11-27 | 中山大学 | A kind of synthesis method of titanium dioxide single crystal rutile nanowire array thin film |
| CN106315670A (en) * | 2015-11-10 | 2017-01-11 | 河南大学 | Dispersible wedge nano titanium dioxide, and preparation method and application thereof |
| CN106345396A (en) * | 2016-11-07 | 2017-01-25 | 苏州寰泰环境工程技术有限公司 | Preparation method of nano TiO2 adsorbent for purifying oily substance in water |
| CN118059951B (en) * | 2024-04-11 | 2024-09-10 | 内蒙古工业大学 | Polycarboxylic acid carbide modified carbon-doped oxygen-defect TiO2Is prepared by the preparation method of (2) |
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| WO1999036362A1 (en) * | 1998-01-13 | 1999-07-22 | Metallgesellschaft Aktiengesellschaft | METHOD FOR PRODUCING TiO2 ACCORDING TO THE SULFATE METHOD |
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| WO1999036362A1 (en) * | 1998-01-13 | 1999-07-22 | Metallgesellschaft Aktiengesellschaft | METHOD FOR PRODUCING TiO2 ACCORDING TO THE SULFATE METHOD |
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