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Preparing method of electric grade acetonitrile

An electronic grade, acetonitrile technology, applied in the purification/separation of carboxylic acid nitrile, organic chemistry, etc., can solve the problems that the purification technology of electronic grade reagents is in the laboratory stage, and the electronic grade reagents rely on imports, etc., and achieve a wide range of market application prospects and operation Simple, low energy consumption effect

Inactive Publication Date: 2017-01-11
NAT INST OF METROLOGY CHINA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, foreign countries have proficiently mastered the purification process of electronic grade reagents, have a complete standard system, and have already mass-produced; while domestic electronic grade reagent purification technology is still in the laboratory stage, there is no relevant standard as a basis, and domestic electronic grade reagents mainly rely on import

Method used

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  • Preparing method of electric grade acetonitrile
  • Preparing method of electric grade acetonitrile
  • Preparing method of electric grade acetonitrile

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] The preparation of embodiment 1 electronic grade acetonitrile product

[0054] (1) Oxidative distillation

[0055]Put 1L of industrial acetonitrile raw material (Nanjing Nanshi Chemical Reagent Co., Ltd.) and 1g of potassium permanganate into a 2L round bottom flask, turn on the condensing device, and turn on the heating device when the temperature of the condensate reaches 0°C to 4°C. 220V, after more than 2 hours of total reflux, remove the light components with a reflux ratio of 20:1, and then obtain a crude product with a reflux ratio of 1:1.

[0056] (2) Adsorption

[0057] Add iron oxyphosphate metal ion adsorbent microspheres (Ningbo Subokoneng Environmental Protection Technology Co., Ltd.) at 5% of the amount of acetonitrile raw material to the above crude product, stir at 50° C. for 2 h, and take the supernatant.

[0058] (3) filter

[0059] The above-mentioned supernatant is subjected to membrane filtration, and an organic membrane with a pore size of 0.22 ...

Embodiment 2

[0060] Embodiment 2 gas chromatography-hydrogen flame ionization detector (GC-FID) detection

[0061] GC-FID detection conditions:

[0062] The instrument model in this experiment: Agilent 6890;

[0063] Chromatographic column model: HP-5 capillary column (Agilent company, length 30m, inner diameter 0.53mm, film thickness 3μm);

[0064] Carrier gas: high-purity nitrogen (0.4MPa) and high-purity hydrogen (0.3MPa);

[0065] Carrier gas column flow rate: 1mL min-1;

[0066] Inlet temperature: 250°C; FID detector temperature: 280°C;

[0067] Injection method: 50:1 split injection;

[0068] Injection volume: 1μL;

[0069] Heating program: initial temperature of 40°C, keep for 5min, then raise the temperature to 120°C at 10°C·min-1, keep for 5min, then raise the temperature to 250°C at 15°C·min-1, and hold for 5min.

[0070] The detection result of the electronic grade acetonitrile obtained through the preparation method purification of the embodiment of the present invention ...

Embodiment 3

[0073] Example 3 Trace metal ion content inductively coupled plasma (ICP-MS) detection

[0074] The instrument model in this experiment: Agilent 7500

[0075] Detection method: direct sample injection, cooling air flow: 10L min -1 , Auxiliary gas consumption: 1L min -1 , injection volume: 1mL min -1 .

[0076] The ICP-MS detection results of electronic-grade acetonitrile and technical-grade acetonitrile purified by the preparation method of Example 1 of the present invention are shown in Table 2:

[0077] Table 2 Product trace metal ion content test results

[0078]

[0079] As can be seen from Table 2, the metal ion content of industrial-grade acetonitrile raw materials is higher than the qualified index of electronic-grade acetonitrile when the ICP-MS detection is carried out, and the metal ion content of acetonitrile obtained through the purification of the preparation method of Example 1 of the present invention meets the electronic-grade acetonitrile standard.

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Abstract

The invention relates to a preparing method of an electric grade acetonitrile. The method comprises the steps of removing metal cation with ferrous phosphate metal ion adsorbent after acetonitrile raw material is oxidized and rectified, and removing dust particles with a filtering membrane. The purity of the obtained product (GC-FID) is 99.99% or above, water content (w / %) is 0.05 or below, metal ion content is 10 microgramme.L<-1> or below, particles of dust particles (0.5micrometer or above) is 25 pieces / mL or below. The electric grade acetonitrile is simple in operation, safe and environment-friendly, and has low energy consumption and good application prospect.

Description

technical field [0001] The invention relates to the field of high-purity chemical reagents, in particular to a method for purifying electronic-grade acetonitrile for electronic chemical products. Background technique [0002] The molecular formula of acetonitrile is CH 3 CN, with a relative molecular mass of 41.05, is a colorless and transparent liquid at normal temperature and pressure. The melting point is -45.7°C, the boiling point is 81.1°C, the relative density is 0.79, the relative vapor density is 1.42, the flash point is 2°C, the ignition temperature is 524°C, and it is flammable. Acetonitrile is extremely volatile, miscible with water, soluble in most organic solvents such as alcohol, and is a polar solvent with a high insulation coefficient. It has excellent solvent properties and can dissolve various organic, inorganic and gaseous substances. It can occur typical nitrile reactions and is used to prepare many nitrogen-containing compounds. It is an important org...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/34C07C255/03
CPCC07C253/34C07C255/03
Inventor 全灿韩强杜然戴新华
Owner NAT INST OF METROLOGY CHINA
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