Preparation method of Schiff base and application thereof

A Schiff base and wastewater technology, applied in the field of analytical chemistry, can solve problems such as damage to human health, pollution of agricultural and aquatic products, and threats to human health, and achieve the effects of wide detection range, high sensitivity, and fast detection speed

Inactive Publication Date: 2015-05-20
昆明理工大学驾驶培训有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

On the one hand, it causes heavy metal poisoning through direct drinking and damages human health; on the other hand, it indirectly pollutes agricultural and aquatic products and poses a threat to human health through the food chain.

Method used

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  • Preparation method of Schiff base and application thereof
  • Preparation method of Schiff base and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Embodiment 1: Determination of chromium content in industrial waste water, concrete steps are as follows:

[0021] (1) Preparation of Schiff's base: Dissolve 0.03mol (3.24g) of o-phenylenediamine in 30mL of anhydrous methanol, drop into 30mL of 0.07mol (8.79g) from the constant pressure funnel at a rate of 30 drops / min The methanol solution of salicylaldehyde was stirred for 20 minutes under the protection of nitrogen, and the system turned into a yellow transparent solution; after the dropwise addition, the reaction was refluxed for 4 hours, cooled to room temperature and then distilled to obtain an orange-red solid, which was filtered, washed with methanol, and recrystallized with acetone , to obtain orange-red Schiff base flaky crystals, vacuum-dried to obtain 20.9g, and the yield was 62.5%. 1H-NMR (500 MHz, CDCl3): 8.29 (s, 2H), 7.30 (t, J=7.5 Hz, 2H), 7.15 (d, J=7.5 Hz, 2H), 6.99 (d, J=7.5 Hz, 2H), 6.88 (t, J=7.5 Hz, 2H), 3.97 (s,4H); 13C-NMR (125 MHz, CDCl 3 ):...

Embodiment 2

[0024] Embodiment 2: Determination of chromium in domestic waste water, concrete operations are as follows:

[0025] (1) Same as step (1) of Example 1;

[0026] (2) Preparation of Cr(Ⅲ) standard color scale: put 1 mL of Cr(Ⅲ) standard solutions with concentrations of 0.0, 0.1, 1, 5, and 10 μg / mL into graduated centrifuge tubes, and dilute to 10 mL with distilled water , add 1.0 mL of the 50 μg / mL Schiff base solution prepared in step (1), adjust the pH to 5.5 with acetic acid-sodium acetate buffer solution, and make the Cr(Ⅲ) in the standard solution form a complex with the Schiff base; add Nonionic surfactant Tergitol TMN-6 0.2mL and Na 2 SO 4 0.4g, vortex mixed for 3 minutes to obtain a cloudy emulsion; then placed in a constant temperature water bath at 50°C, heated for 15 minutes, centrifuged at 4000r / min for 10 minutes to separate the phases, took out the water phase with a syringe, and obtained the surface active substance at the bottom of the centrifuge tube The sta...

Embodiment 3

[0028] Embodiment 3: Determination of chromium in mineral waste water

[0029] (1) Same as step (1) in Example 1;

[0030] (2) Preparation of Cr(Ⅲ) standard color scale: put 1 mL of Cr(Ⅲ) standard solutions with concentrations of 0.0, 0.1, 1, 5, and 10 μg / mL into graduated centrifuge tubes, and dilute to 10 mL with distilled water , add 0.5mL of the 500μg / mL Schiff base solution prepared in step (1), adjust the pH to 4.0 with acetic acid-sodium acetate buffer solution, and make the Cr(Ⅲ) in the standard solution form a complex with the Schiff base; add Non-ionic surfactant NP-7 0.4mL and NaCl 0.3g, vortex mixed for 3min to obtain a cloudy emulsion; then placed in a constant temperature water bath at 40°C, heated for 20min, centrifuged at 5000r / min for 5min to separate the phases, and Take out the water phase with the syringe, and obtain the standard color scale of the surfactant-rich phase from light yellow to dark yellow series at the bottom of the centrifuge tube;

[0031]...

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PUM

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Abstract

The invention discloses a preparation method of Schiff base and an application thereof in detecting trace chromium in environmental wastewater. The chromium in the environmental wastewater is reduced to Cr(III) which reacts with Schiff base to form a complex; the Cr(III)-Schiff base complex in the sample is separated and enriched by CPE (cloud point extraction) using a nonionic surfactant / salt to form a yellow complex; and the trace chromium in the sample is detected by comparing the enrichment phase enriched on the surfactant with the standard chromium content, wherein the detection limit is 0.1mug / mL. The method disclosed by the invention has the advantages of simplicity in operation, high detection sensitivity, no use of organic solvent, environmental protection, short detection time and the like, is a simple, quick and accurate analysis method and has wide application prospect.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to a method for preparing a Schiff base and a method for detecting chromium content thereof. The method is used for detecting trace amounts of chromium in a sample. Background technique [0002] Heavy metal ions have serious toxicological effects on living organisms. On the one hand, it causes heavy metal poisoning through direct drinking and damages human health; on the other hand, it indirectly pollutes agricultural and aquatic products, posing a threat to human health through the food chain. At present, the most attention is lead, mercury, chromium, cadmium and so on. Chromium is an essential trace element for the human body, and hexavalent chromium is poisonous. Chromium compounds have obvious local irritation and corrosion effects at high concentrations, and are common carcinogens at low concentrations. [0003] Chromium is harmful to human health. With the wo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C251/24C07C249/02G01N21/78
Inventor 杨亚玲孟丽芬李英堂
Owner 昆明理工大学驾驶培训有限公司
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