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Method for purifying dihydroxynaphthalene

A technology of dihydroxynaphthalene and purification method, applied in chemical instruments and methods, preparation of organic compounds, gas treatment, etc., can solve problems such as poor economy, decreased purification ability of composition, filter blockage, etc.

Pending Publication Date: 2019-07-02
SHIN ETSU CHEM IND CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

On the other hand, although the soft particles in the composition are temporarily captured on the surface of the filter, they deform as the composition flows, and the spaces between the soft particles disappear, making it difficult to pass through the filter. The purification ability of the composition is reduced
Furthermore, if this state continues, the filter will eventually become clogged, and the filter needs to be replaced
If such filter replacement is repeated, the consumption of the filter used to produce the composition increases, resulting in poor economical efficiency.
[0011] At this time, if the hydraulic pressure difference before and after the filter is greater than 50KPa in order to ensure the liquid flow of the composition, foreign matter, especially soft particles, that must be captured by the filter will pass through the pores of the filter due to the pressure difference. , mixed into the filtrate side, filtration purification becomes insufficient
As a result, coating defects and post-etching defects increase, and the yield of semiconductor devices decreases.

Method used

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  • Method for purifying dihydroxynaphthalene
  • Method for purifying dihydroxynaphthalene
  • Method for purifying dihydroxynaphthalene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-1

[0061] 72.2g of commercially available 1,5-dihydroxynaphthalene (hereinafter referred to as 15DHN, sulfur element content 400ppm, measured by ICP-OES) was dissolved in 127.6g of propylene glycol methyl ether (hereinafter referred to as PGME) and 353.6g A mixed solvent of methyl isobutyl ketone (hereinafter referred to as MIBK). 57.2 g of neutral alumina (Tomita AD-250NS manufactured by Tomita Pharmaceutical co., Ltd., particle size 60-250 μm, pH 7.5) was added thereto, stirred at room temperature for 12 hours, and the neutral alumina was collected by filtration. , The obtained 15DHN PGME / MIBK solution was washed with ion-exchanged water, PGME was added, and concentrated to obtain 500 g of 13 wt% 15DHN-PGME solution (purification raw material 1). The sulfur element content per part of the solid content of the 15DHN solution was measured by ICP-OES, and the result was 45 ppm.

Synthetic example 1

[0094]In a 1000ml flask, mix the 13wt% 15DHN-PGME solution (purification raw material 1), 2.8g of p-toluenesulfonic acid and the PGME of 2.8g purified in the embodiment 1-1 of 500g (0.5 mole), at 80 ℃ Next, 14.3 g of 50 wt % formaldehyde aqueous solution was added with stirring. After maintaining the temperature at 80° C. and stirring for 6 hours, it was cooled to room temperature (monomer conversion rate 77%). After the obtained solution was concentrated under reduced pressure, 540 g of hexane was added to separate and precipitate the polymer component. After filtering and removing the upper filtrate, this operation was repeated to make the residual monomers less than 5%. The remaining polymer component was redissolved in 200 g of MIBK, and 200 g of ion-exchanged water was added to remove the metal ion component. 300 g of propylene glycol monomethyl ether acetate (PGMEA) was added to the MIBK solution from which metal ion components were removed, and concentrated under redu...

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Abstract

The invention provides a method for purifying dihydroxynaphthalene, which is capable of suppressing soft particle generation and obtaining dihydroxynaphthalene serving as a raw material of a resin andcomposition excellent in filterability. The method for purifying dihydroxynaphthalene includes the step of removing a sulfur content in the dihydroxynaphthalene with an adsorbent, and neutral aluminais used as the adsorbent.

Description

technical field [0001] The invention relates to a method for purifying dihydroxynaphthalene. Background technique [0002] Since dihydroxynaphthalene resins are excellent in heat resistance and moisture resistance, they are widely used as underlayer film materials, photoresist materials, and the like in the semiconductor field (Patent Document 1). [0003] Common dihydroxynaphthalene (1) is generally produced industrially by the following method. That is, dihydroxynaphthalene (1) is obtained by sulfonating naphthalene (1-1) as a starting material to obtain a sulfonic acid compound (1-2), and converting it into a hydroxyl group by alkali fusion. [0004] [chemical formula 1] [0005] [0006] In the formula, n and m are integers satisfying 0≤m≤2, 0≤n≤2, and m+n=2. [0007] In this preparation process, the sulfonic acid compound (1-2) is not completely consumed by alkali fusion, and the content of the sulfur element in the element component is the sulfonic acid compound ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C37/82C07C39/14
CPCC07C37/82C07C39/14B01D15/08B01J20/08B01D2257/30
Inventor 橘诚一郎郡大佑荻原勤北野智阿部幸雄畠山史裕小林大树
Owner SHIN ETSU CHEM IND CO LTD
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