LCD 제조공정의 혼합폐산으로부터 일인산암모늄 제조 기술

이하영; 이상길; 박성국; 김주한; 김주엽; 김준영; Ha-young Lee; Sang-gil Lee; Sung-Kook Park; Ju-han Kim; Ju-yup Kim; Jun-young Kim

Clean Technology, Vol.15, No.4, 253-257, December, 2009

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LCD 제조공정의 혼합폐산으로부터 일인산암모늄 제조 기술

Manufacture Technology of Monoammonium phosphate from LCD Waste Acid

이하영, 이상길, 박성국^†, 김주한¹, 김주엽¹, 김준영¹

포항산업과학연구원 환경연구실, 790-330 경북 포항시 남구 효자동 산32
¹(주)엔아이티, 573-882 전라북도 군산시 소룡동 1662

Ha-young Lee, Sang-gil Lee, Sung-Kook Park^†, Ju-han Kim¹, Ju-yup Kim¹, and Jun-young Kim¹

Environment Research Department, Research Institute of Industrial Science & Technology, 32 Hyoja-dong, Nam-gu, Pohang, Kyungbuk 790-330, Korea
¹NIT Co., Ltd., 1662 Soryong-dong, Gunsan, Jeonbuk 573-882, Korea

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초록

LCD 제조공정에서 배출되는 질산과 초산, 인산, 그리고 Al과 같은 금속이온을 함유한 폐에칭액으로부터 진공증발과 확산투석을 이용하여 고순도 인산을 회수하여 인산암모늄을 제조하고자 하였다. 진공증발을 이용하여 질산과 초산을 제거하였다. 진공도가 -650 mmHg인 경우에는 온도 413 K 이상에서 완전 분리되었고, 진공도가 -700 mmHg인 경우에는 온도 393 K 이상의 영역에서 완전히 분리되었다. 그리고 진공도 -730 mmHg의 경우는 온도 383 K 이상에서도 완전 분리가 가능하였다. 99%의 질산과 초산을 제거하였으며, 확산투석을 이용하여 약 97.5% 이상의 Al을 제거하였다. 이렇게 얻어진 고순도 인산과 수산화암모늄을 이용하여 일인산암모늄을 제조하는 공정에서 급격한 발열반응을 제어하고 안정된 적정조건을 도출하기 위하여 수산화암모늄의 농도, 적정 몰비, pH, 온도 등의 반응인자를 조절하여 회수율 약 90%의 일인산암모늄을 제조하였다.

The waste solution discharged form the LCD(Liquid Crystal Display) manufacturing process contains phosphoric acid, nitric acid, acetic acid and metal ions such Al and other impurities. In this study, vacuum evaporation and diffusion dialysis was developed to commercialize an efficient system for recovering the high-purity phosphoric acid and manufacturing monoammonium phosphate. By vacuum evaporation, almost 99% of nitric and acetic acid was removed. Also, by diffusion dialysis, about 97.5% of Al was removed. Monoammonium phosphate was manufactured from purified phosphoric acid and ammonium hydroxide. In order to get the optimum manufacturing condition, the molar ratio of ammonium hydroxide and phosphoric acid, pH and temperature was controlled. Using this optimum condition, we obtained the recovery rate of monoammonium phosphate of about 90%.

Keywords:Nitric acid;Acetic acid;Phosphoric acid;Vacuum evaporation;Diffusion dialysis;Monoammonium phosphate

[References]

National Institute of Environmental Research, Ministry of Environment, "The designation waste occurrences and process present situation," National Institute of Environmental Research (2008)
Kwon KS, Kang KH, Kim MK, "Method and Apparatus for Separatin Acetic Acid and Nitric Salts," Korean Patent No. 100550829 B1 (2006)
Yoon CJ, Park BK, Choi SJ, "Method for Preparing Sodium Nitrate Using Waste Nitric Acid" Korean Patent No. 10008603 B1 (2003)
Park SK, Roh YM, Lee SG, Kim JY, Shin CH, Kim JY, Ahn JW, J. Korean Inst. of Resour. Recycl., 15, 26 (2006)
Lee HS, Shin CH, Kim JY, Kim JY, Ahn JW, J. Korean Inst. of Resour. Recycl., 14, 18 (2005)
Park SK, Lee SG, Korean Patent No. 1020070068204 A (2007)

[1] National Institute of Environmental Research, Ministry of Environment, "The designation waste occurrences and process present situation," National Institute of Environmental Research (2008)

[2] Kwon KS, Kang KH, Kim MK, "Method and Apparatus for Separatin Acetic Acid and Nitric Salts," Korean Patent No. 100550829 B1 (2006)

[3] Yoon CJ, Park BK, Choi SJ, "Method for Preparing Sodium Nitrate Using Waste Nitric Acid" Korean Patent No. 10008603 B1 (2003)

[4] Park SK, Roh YM, Lee SG, Kim JY, Shin CH, Kim JY, Ahn JW, J. Korean Inst. of Resour. Recycl., 15, 26 (2006)

[5] Lee HS, Shin CH, Kim JY, Kim JY, Ahn JW, J. Korean Inst. of Resour. Recycl., 14, 18 (2005)

[6] Park SK, Lee SG, Korean Patent No. 1020070068204 A (2007)