WO2021002601A1 - Méthode de décomposition par catalyseur au charbon actif pour éliminer le peroxyde d'hydrogène dans des déchets d'acide sulfurique - Google Patents

Méthode de décomposition par catalyseur au charbon actif pour éliminer le peroxyde d'hydrogène dans des déchets d'acide sulfurique Download PDF

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WO2021002601A1
WO2021002601A1 PCT/KR2020/007315 KR2020007315W WO2021002601A1 WO 2021002601 A1 WO2021002601 A1 WO 2021002601A1 KR 2020007315 W KR2020007315 W KR 2020007315W WO 2021002601 A1 WO2021002601 A1 WO 2021002601A1
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hydrogen peroxide
sulfuric acid
activated carbon
decomposition
tank
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PCT/KR2020/007315
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English (en)
Korean (ko)
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정영남
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정영남
에스제이기술 주식회사
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B17/00—Sulfur; Compounds thereof
    • C01B17/69—Sulfur trioxide; Sulfuric acid
    • C01B17/90—Separation; Purification
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/74—Iron group metals
    • B01J23/745—Iron
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J35/61—Surface area
    • B01J35/617—500-1000 m2/g
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J35/61—Surface area
    • B01J35/618—Surface area more than 1000 m2/g
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02—Impregnation, coating or precipitation
    • B01J37/0201—Impregnation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/08—Heat treatment

Definitions

  • the present invention relates to an activated carbon catalytic decomposition method for removing hydrogen peroxide in spent sulfuric acid, and more particularly, to purify sulfuric acid by decomposing hydrogen peroxide contained in the spent sulfuric acid generated in the wafer cleaning process during semiconductor manufacturing through an activated carbon catalyst. It's about how.
  • hydrogen peroxide (H 2 O 2 ) is a kind of oxidizing agent that is commonly used. It is always used with sulfuric acid (H 2 SO 4 ) and can be used as a photoresist removal solution or etchant. Sulfate waste acid accounts for more than 30-40%.
  • Heat decomposition Hydrogen peroxide heated to a high temperature of 140°C or higher rapidly decomposes to release oxygen gas. The most problematic drawback of this method is the risk of exothermic reactions at high temperatures.
  • Nitric acid decomposition Oxygen gas is released by adding nitric acid (HNO 3 ) to a sulfuric acid solution containing hydrogen peroxide to generate a decomposition reaction. In this method, since a high exothermic temperature is accompanied during the decomposition reaction, sulfuric acid gas may be released, and an additional process of removing nitric acid used as a catalyst for the reaction is required.
  • HNO 3 nitric acid
  • the inventors of the present invention were studying a method for removing hydrogen peroxide in spent sulfuric acid in order to overcome the above problems, and simply adding existing activated carbon or nitric acid to decompose hydrogen peroxide (Korean Patent Laid-Open Patent No. 10-2018-0051250
  • the present invention was completed by confirming that the heating temperature is lower and the hydrogen peroxide decomposition time is shortened if the step of stepwise inputting the activated carbon content is different than that of Korean Patent No. 10-1641959).
  • activated carbon impregnated with iron oxide than conventional activated carbon, it was confirmed that the hydrogen peroxide decomposition time was shortened, thereby completing the present invention.
  • Patent Document 1 Korean Patent Registration No. 10-1641959 (Name of the invention: Method for removing hydrogen peroxide from sulfuric acid-hydrogen peroxide solution and its treatment agent, Applicant: Trussval Technology Company, Limited, registration date: 2016.07.18.)
  • Patent Document 2 Korean Laid-Open Patent No. 10-2018-0051250 (Name of the invention: hydrogen peroxide decomposition catalyst and its manufacturing method, hydrogen peroxide decomposition apparatus and method using the catalyst, Applicant: Korea Institute of Science and Technology, Publication Date: May 2018. 16.)
  • Patent Document 3 Korean Patent Registration No. 10-1237919 (Name of the invention: Recycling device for waste sulfuric acid contaminated with hydrogen peroxide, Applicant: Kwang-min So, Registration date: February 21, 2013)
  • An object of the present invention is to provide an activated carbon catalytic decomposition method for removing hydrogen peroxide in spent sulfuric acid, and more particularly, hydrogen peroxide contained in the spent sulfuric acid generated in the wafer cleaning process during the semiconductor manufacturing process is decomposed through an activated carbon catalyst to decompose sulfuric acid. It is to provide a way to purify.
  • Another object of the present invention is to impregnate activated carbon with an iron salt to promote hydrogen peroxide decomposition reaction. Also, by dividing activated carbon, the hydrogen peroxide decomposition time is shorter than that of shortening, and the reaction temperature is lowered to stably decompose hydrogen peroxide in sulfuric acid waste acid to purify sulfuric acid. To provide a way to do it.
  • the present invention comprises the steps of (first step) collecting waste sulfuric acid generated in the semiconductor industry;
  • the method of removing hydrogen peroxide comprising: transferring sulfuric acid, which has been decomposed of hydrogen peroxide in the third step, to a sulfuric acid storage tank through a filtration device in a retention type decomposition tank.
  • One or two or more retention-type decomposition tanks in the second step may be installed to continuously remove hydrogen peroxide.
  • the activated carbon of the third step may be one having a granular form having a specific surface area of 500 to 3000 m 2 /g.
  • the activated carbon of the third step may be impregnated with an iron salt solution and subjected to heat treatment to use activated carbon impregnated with iron oxide.
  • the step of decomposing hydrogen peroxide in the spent sulfuric acid in the third step may be to maintain an exothermic temperature of 30° C. or less during hydrogen peroxide decomposition.
  • Spent sulfuric acid containing hydrogen peroxide in the first step is a solution containing hydrogen peroxide in sulfuric acid among by-products generated in the semiconductor production process, and generally 50 to 70% by weight of sulfuric acid, 1 to 10% by weight of hydrogen peroxide, and 20 to 40% by weight of water It may be to include.
  • the retention-type cracking tank includes an acid-resistant material tank including a filtering device capable of filtering the activated carbon catalyst, an acid-resistant steel and concrete tank, and a batch-type cracking tank using one cracking tank and two or more cracking tanks.
  • a continuous cracking tank can be used. Most preferably, it is recommended to use a continuous cracking tank in which three cracking tanks are connected. At this time, different amounts of activated carbon may be added to each of the cracking tanks connected in the continuous cracking tank.
  • 0.5 to 1 parts by weight, 1 to 2 parts by weight, and 2 to 5 parts by weight of activated carbon based on 100 parts by weight of spent sulfuric acid may be added to each decomposition tank to sequentially decompose hydrogen peroxide in the spent sulfuric acid.
  • the spent sulfuric acid is introduced from a decomposition tank in which less activated carbon is added, and hydrogen peroxide is decomposed and removed sequentially.
  • the spent sulfuric acid has a residence time of 2 to 5 hours in each of the cracking tanks. If the residence time is less than 2 hours, hydrogen peroxide cannot be sufficiently decomposed, which is not preferable. If the residence time is more than 5 hours, the operating time of the facility is lengthened and production efficiency is lowered, which is not economical.
  • the retention-type decomposition method for removing hydrogen peroxide in the spent sulfuric acid is economically excellent because the equipment, installation and operation costs of the decomposition tank are very low, and sulfuric acid from which hydrogen peroxide has been removed can be provided to be recycled to various industries. It is an eco-friendly way to recycle to resources.
  • activated carbon having a specific surface area of 500 to 3,000 m 2 /g, more preferably 1,000 to 2,000 m 2 /g. If the specific surface area of activated carbon is less than 500m2/g, hydrogen peroxide decomposition reaction does not occur well or decomposition may take a long time, which is not preferable. If the specific surface area of the activated carbon exceeds 3,000m2/g, hydrogen peroxide decomposition reaction occurs too actively. It is difficult to control and is economically unfavorable because it is expensive.
  • activated carbon impregnated with iron oxide may be used. More specifically, activated carbon having a specific surface area of 500 to 3,000 m 2 /g may be added to an ethanol solution containing an iron salt so that the ethanol solution containing the iron salt may be impregnated with the activated carbon.
  • Activated carbon may be mixed and impregnated with 150 to 300 parts by weight of an ethanol solution based on 100 parts by weight, and the ethanol solution may contain any one or more of iron nitrate, iron chloride, iron hydroxide and iron sulfate, and 100 parts by weight of the ethanol solution It is preferable to contain 0.01 to 2 parts by weight based on parts. Most preferably, 0.01 to 2 parts by weight of iron trinitrate is included. If the iron salt is less than 0.01 parts by weight, the iron salt applied to the surface may not be sufficient, and if it is more than 2 parts by weight, the concentration of the iron salt is too high, which is not economically preferable.
  • the ethanol solution containing the iron salt is impregnated with the activated carbon by a method of applying vibration in an ultrasonic cleaner.
  • the ethanol solution may be removed by separating activated carbon from the ethanol solution containing the iron salt and washing with water.
  • the method of removing the ethanol solution is preferably washed 1 to 3 times with water. Iron salts that are not sufficiently washed with water and not impregnated adhere to the activated carbon, and thus remain unimpregnated and adhered during the hydrogen peroxide decomposition step in the spent sulfuric acid may contaminate sulfuric acid, which is undesirable.
  • the activated carbon from which the ethanol solution has been removed may be heat-treated at 300 to 500° C. to impregnate the surface of the activated carbon with iron oxide. If the heat treatment temperature is less than 300°C, oxidation of iron may not be sufficient, and if it exceeds 500°C, heating energy may be wasted.
  • the type of iron oxide after the heat treatment may vary depending on the type of iron salt in the ethanol solution containing the iron salt, but it is preferable that iron oxide which can be used for the hydrogen peroxide decomposition reaction is impregnated, and trivalent iron oxide is impregnated.
  • the impregnating material may be impregnated with not only pure iron oxide, but also other elements capable of increasing the efficiency of the hydrogen peroxide decomposition reaction.
  • the activated carbon impregnated with iron oxide according to the present invention may exhibit an effect in decomposing and removing hydrogen peroxide in waste sulfuric acid.
  • the present invention relates to an activated carbon catalytic decomposition method for removing hydrogen peroxide in spent sulfuric acid, and has a lower risk than a method of removing by heating or simply adding nitric acid to remove hydrogen peroxide. It has a stable effect in treating sulfuric acid waste of
  • 1 is a flow chart of purifying sulfuric acid by a method of removing hydrogen peroxide in waste sulfuric acid by a retention-type continuous decomposition tank.
  • 2 is a graph measuring the amount of oxygen gas generated after hydrogen peroxide decomposition when activated carbon is added to waste sulfuric acid.
  • the spent sulfuric acid of the present invention used sulfuric acid containing hydrogen peroxide generated in the semiconductor industry, and more specifically, 60% by weight of sulfuric acid, 5% by weight of hydrogen peroxide, and 35% by weight of water were used.
  • activated carbon was prepared with a specific surface area of at least 950 m 2 /g or more of a coal-based 8 ⁇ 30 mesh size.
  • Activated carbon was prepared by impregnating the activated carbon prepared in Example 1 with iron oxide.
  • the activated carbon prepared in Example 1 was first etched and oxidized in an acid solution.
  • As an acid solution 95% (v/v) sulfuric acid and 70% (v/v) nitric acid were prepared in a ratio of 3:1, and activated carbon was immersed in the prepared acid solution at 25° C. for 24 hours. After that, the acid solution-treated activated carbon was repeatedly washed with distilled water to adjust the pH to neutral.
  • the process of impregnating the neutralized activated carbon with iron oxide proceeded as follows.
  • Tri(III) iron nitrate (Fe(NO 3 ) 3 ⁇ 9H 2 O) was added to ethanol to prepare a 3% by weight iron salt solution. Thereafter, the activated carbon was added to the iron salt solution, and the iron salt solution was placed in an ultrasonic cleaner to vibrate for 10 minutes so that the iron salt solution was impregnated with the activated carbon. Thereafter, the activated carbon impregnated with the iron salt solution was heat-treated at 100° C. for 1 hour to remove ethanol, and then heat-treated at 400° C. for 4 hours to oxidize the iron salt to prepare activated carbon impregnated with iron oxide.
  • the decomposition completion time of hydrogen peroxide decreases as the amount of activated carbon increases, and in Experimental Example 1-5, it can be seen that the decomposition completion time is 4 hours.
  • the decomposition completion time was 20 hours and the number of bubbles generated was maintained for 11 hours or less. Therefore, it was confirmed that the decomposition time was faster as the input amount of activated carbon increased.
  • a retention-type decomposition tank made of a tank made of acid-resistant material was prepared, and activated carbon 1g, 2g, 3g, 4g, 5g each was added to the retention-type decomposition tank, respectively, and 100 g of spent sulfuric acid collected in Example 1 was prepared. After pouring into each retention type decomposition tank, the temperature change over time was measured and shown in Table 2 below.
  • the retention type decomposition tank includes a filtration device capable of filtering activated carbon and is made of an acid-resistant tank, and is a continuous type that can continuously supply and discharge sulfuric acid waste by connecting three retention type decomposition tanks.
  • a digestion tank was used.
  • the three retention-type decomposition tanks were divided into a decomposition tank (1), a decomposition tank (2), and a decomposition tank (3).
  • the amount of activated carbon in each decomposition tank was 1 g in the decomposition tank 1, 2 g in the decomposition tank 2, and 4 g in the decomposition tank 3 each. Thereafter, 100 g of the spent sulfuric acid collected in Example 1 was poured into the decomposition tank 1, and after the hydrogen peroxide decomposition reaction for 4 hours, the activated carbon was filtered, and the spent sulfuric acid in the decomposition tank 1 was moved to the next decomposition tank 2, followed by hydrogen peroxide. The decomposition reaction proceeded. After an additional 4 hours reaction in the decomposition tank 2, it was moved to the decomposition tank 3 into which 4 g of activated carbon was added to proceed with the hydrogen peroxide decomposition reaction.
  • Hydrogen peroxide decomposition reactions in spent sulfuric acid were carried out stepwise in decomposition tanks with different amounts of activated carbon, and decomposition times and temperature changes were measured in the same manner as in Experimental Examples 1 and 2, and are shown in Tables 3 and 4 below.
  • Decomposition tank (1) in which 1g of activated carbon was added
  • Decomposition tank (2) containing 2 g of activated carbon
  • Decomposition tank (3) containing 4 g of activated carbon
  • Initial input 7 1 hours 8 2 hours 8 3 hours 8 4 hours Move to the disassembly tank (2) ⁇ 10 5 hours 9 6 hours 8 7 hours 4 8 hours Move to the disassembly tank (3) ⁇ 8 9 hours 2 10 hours 0
  • the hydrogen peroxide decomposition time was not shortened compared to Experimental Examples 1-4 and 1-5, but sulfuric acid contamination and sulfuric acid gas by activated carbon generated in Experimental Examples 1-4 and 1-5 did not occur in Experimental Example 3, and , It can be seen that the exothermic temperature is also 30°C or less, confirming that hydrogen peroxide is decomposed in a stable state, and is a method of more effectively removing hydrogen peroxide in the spent sulfuric acid.
  • Decomposition tank (1) in which 1g of activated carbon impregnated with iron oxide was added
  • Decomposition tank (2) in which 2g of activated carbon impregnated with iron oxide was added
  • Decomposition tank (3) containing 4 g of activated carbon impregnated with iron oxide

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  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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  • Inorganic Chemistry (AREA)
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Abstract

La présente invention concerne une méthode de décomposition par catalyseur au charbon actif de type à rétention pour éliminer le peroxyde d'hydrogène dans des déchets d'acide sulfurique. Plus spécifiquement, la présente invention concerne une méthode de raffinage d'acide sulfurique par décomposition du peroxyde d'hydrogène dans des déchets d'acide sulfurique, qui est généré pendant le nettoyage de tranche dans un procédé de fabrication de semi-conducteur, au moyen d'un catalyseur au charbon actif. L'industrie des semi-conducteurs en Corée se développe et croît au niveau mondial. Par rapport à cette dernière, des déchets d'acide sulfurique comprenant inévitablement du peroxyde d'hydrogène sont générés. Les technologies de recyclage autres que l'élimination par une méthode de neutralisation du calcium ou la préparation de sulfate de fer et d'un agent de traitement de l'eau sont actuellement insuffisantes. La présente invention permet de préparer et d'utiliser un acide sulfurique mince en tant que ressource industrielle au moyen d'une méthode de raffinage par élimination d'impuretés de déchets d'acide sulfurique, et permet ainsi de grands avantages de prévention de pollution environnementale et de réduction de coût économique pour l'industrie.
PCT/KR2020/007315 2019-07-03 2020-06-05 Méthode de décomposition par catalyseur au charbon actif pour éliminer le peroxyde d'hydrogène dans des déchets d'acide sulfurique WO2021002601A1 (fr)

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CN116253421A (zh) * 2022-11-29 2023-06-13 嘉兴沃特泰科环保科技股份有限公司 一种水处理用双氧水去除剂、制备方法和应用

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KR102047212B1 (ko) * 2019-07-03 2019-11-20 정영남 황산폐산 내의 과산화수소를 제거하기 위한 활성탄 촉매 분해방법
NL2028174B1 (en) 2021-05-07 2022-11-24 Kuijpers Kunststoftechniek B V Apparatus for neutralizing acid solution
KR102630759B1 (ko) * 2021-07-27 2024-01-30 주식회사 프로그린테크 폐황산 용액에 포함된 프탈라이드 유도체 제거 방법

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CN116253421B (zh) * 2022-11-29 2024-05-28 嘉兴沃特泰科环保科技股份有限公司 一种水处理用双氧水去除剂、制备方法和应用

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