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1, 2-cyclohexanediamine tetraacetic acid and purification method thereof

A technology of cyclohexanediaminetetraacetic acid and purification method, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of low removal rate of metal ions, difficult removal of metal ions, and difficult purification operations, etc., Achieve the effect of low purification cost, meet mass production requirements, and easy process

Pending Publication Date: 2020-07-07
ANJI MICROELECTRONICS TECH (SHANGHAI) CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Since CDTA has a relatively high boiling point (482°C), the method of sublimation and re-sublimation using high temperature is difficult to purify, the cost is high, and the removal rate of metal ions is low.
Also affected by the higher boiling point, it is difficult to purify CDTA by vacuum distillation. In addition, it can form stable complexes with many metal ions such as sodium ions, potassium ions, magnesium ions, iron ions, etc., so as to remove CDTA. The metal ions in the

Method used

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  • 1, 2-cyclohexanediamine tetraacetic acid and purification method thereof
  • 1, 2-cyclohexanediamine tetraacetic acid and purification method thereof
  • 1, 2-cyclohexanediamine tetraacetic acid and purification method thereof

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Embodiment 1～3

[0037] A method for purifying 1,2-cyclohexanediaminetetraacetic acid (CDTA) of the present invention comprises the following steps:

[0038] Step 1, select the CDTA raw material of the manufacturer shown in Table 1, add the medium whose mass percent concentration is A, then add the alkaline pH regulator whose mass percent concentration is B to it, make it dissolve in an alkaline environment, and be formulated into CDTA alkaline solution;

[0039] Step 2, adding a slightly excess acidic pH regulator with a mass percentage concentration of C to the CDTA solution obtained in step 1 to make the solution acidic so that CDTA is completely precipitated;

[0040] Step 3, stand until layering, CDTA is completely precipitated, the upper layer liquid is poured out, and the CDTA filter cake is filtered out;

[0041] Step 4. The CDTA filter cake is placed in a vacuum drying oven with a temperature of D, and dried under reduced pressure for E hours to form a dry and pure high-purity electr...

Embodiment 4～12

[0051]Select the CDTA raw materials of the same manufacturer, use different media, alkaline pH regulators, and acidic pH regulators respectively, purify CDTA according to the purification method of the present invention, and test the concentrations of sodium ions, calcium ions, and iron ions by ICP-OES spectrometer. , the above-mentioned metal ion concentration data before and after treatment are shown in Table 4.

[0052] Table 4 Contrast data of each metal ion concentration before and after treatment by different purification methods

[0053]

[0054] As can be seen from Table 4, using the purification method of the present invention to purify the CDTA raw material of the same manufacturer, the sodium ion, calcium ion, The content of main metal ions such as iron ions is reduced to less than 1ppm, and the removal rate of sodium ions is higher than 99%, the removal rate of calcium ions is higher than 64%, and the removal rate of iron ions is higher than 94%; As a medium, i...

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Abstract

The invention provides a purification method of 1,2-cyclohexanediamine tetraacetic acid, which comprises the following steps: (1) adding a 1,2-cyclohexanediamine tetraacetic acid raw material into a medium, and adding an alkaline pH regulator into the medium to completely dissolve the 1,2-cyclohexanediamine tetraacetic acid; and (2) adding an acidic pH regulator into the 1,2-cyclohexanediamine tetraacetic acid solution obtained in the step (1) to completely precipitate 1,2-cyclohexanediamine tetraacetic acid, filtering the reaction liquid to obtain a 1,2-cyclohexanediamine tetraacetic acid filter cake, and drying the filter cake to obtain high-purity electronic-grade 1,2-cyclohexanediamine tetraacetic acid powder. The purification method disclosed by the invention is relatively low in purification cost and can meet the mass production requirement of the semiconductor high-end cleaning liquid.

Description

technical field [0001] The invention relates to the technical field of semiconductor cleaning, in particular to a 1,2-cyclohexanediaminetetraacetic acid and a purification method thereof. Background technique [0002] High-purity reagents are one of the essential raw materials for semiconductor cleaning solutions, and the purity of raw materials needs to reach electronic level. With the rapid development of the IC industry, the demand for electronic-grade reagents is getting higher and higher, and there are more and more categories. The current mainstream semiconductor process technology is 28nm, and the cutting edge has reached 7nm process. The corresponding electronic-grade reagent requirements also need to be increased accordingly, so it has gradually become one of the important factors restricting the development of integrated circuits. The production of electronic-grade reagents generally uses corresponding industrial-grade products as raw materials, and the target imp...

Claims

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Application Information

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IPC IPC(8): C07C229/16C07C227/18C07C227/40
CPCC07C227/18C07C227/40C07C2601/14C07C229/16
Inventor 肖林成刘兵
Owner ANJI MICROELECTRONICS TECH (SHANGHAI) CO LTD
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