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WO2014042431A1 - Procédé de régénération d'un agent de polissage contenant de l'oxyde de cérium usé - Google Patents

Procédé de régénération d'un agent de polissage contenant de l'oxyde de cérium usé Download PDF

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Publication number
WO2014042431A1
WO2014042431A1 PCT/KR2013/008222 KR2013008222W WO2014042431A1 WO 2014042431 A1 WO2014042431 A1 WO 2014042431A1 KR 2013008222 W KR2013008222 W KR 2013008222W WO 2014042431 A1 WO2014042431 A1 WO 2014042431A1
Authority
WO
WIPO (PCT)
Prior art keywords
ceria
abrasive
containing waste
waste
waste sludge
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/KR2013/008222
Other languages
English (en)
Korean (ko)
Inventor
곽익순
조승범
노준석
김종필
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
LG Chem Ltd
Original Assignee
LG Chem Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by LG Chem Ltd filed Critical LG Chem Ltd
Priority to CN201380047554.0A priority Critical patent/CN104619462B/zh
Priority to JP2015531851A priority patent/JP5940224B2/ja
Priority claimed from KR1020130108820A external-priority patent/KR101539419B1/ko
Publication of WO2014042431A1 publication Critical patent/WO2014042431A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B57/00—Devices for feeding, applying, grading or recovering grinding, polishing or lapping agents

Definitions

  • the present invention relates to a regeneration method of ceria-containing waste abrasive. More specifically, the present invention is to effectively remove the impurities contained in the ceria-containing waste abrasive material, while improving the efficiency of the regeneration process including a washing process, and of the ceria-containing waste abrasive material that can suppress the re-formation of the ceria-containing abrasive during the washing process It relates to a reproduction method.
  • TV CRT tubes and TFT-LCD glass substrates used as liquid crystal panels are produced with poor surface flatness and roughness during the production process. Therefore, using original glass as a TV CRT tube or liquid crystal panel glass substrate is a problem. It is difficult.
  • the TFT-LCD glass panel used as a liquid crystal panel has been examined in various ways to improve the brightness, viewing angle, and contrast of the product. It is known to receive.
  • companies producing glass substrates are making efforts to improve the surface of glass substrates, and various glass substrate abrasives are used.
  • an abrasive containing ceria (Ce0 2 ) is widely used as a general abrasive.
  • Such ceria-containing abrasives are disposed of as waste sludge due to a decrease in polishing efficiency after a certain time of glass polishing process. This is because, after a certain time of polishing, the polishing efficiency of the abrasive decreases and agglomeration between the abrasive grains occurs, resulting in a high possibility of scratches.
  • impurities derived from the polishing pad generated during polishing are introduced into the abrasive slurry to further increase the possibility of scratches.
  • a solvent solution containing hydrofluoric acid or hydrogen fluoride compounds is used to dissolve impurities derived from glass substrates such as silica contained in ceria-containing waste sludge, and After separating such impurities from the waste sludge, a method of regenerating the waste sludge and the waste abrasive material through a drying and calcining process is mainly used.
  • the present invention can effectively remove the impurities contained in the ceria-containing waste abrasive material, and can efficiently regenerate the regeneration process including the washing process, and can suppress the reagglomeration of the ceria-containing abrasive during the washing process.
  • the present invention comprises the steps of mixing a ceria (Ce0 2 ) -containing waste sludge and a solvent solution containing a fluorine-based compound to selectively dissolve the silica (Si0 2 ) -containing impurities contained in the waste sludge; Washing the ceria-containing waste sludge while passing through a cross-flow fliltration system to selectively remove the silica (SiO 2 ) -containing impurities; And drying and firing the washed ceria-containing waste sludge.
  • a method for regenerating waste ceria-containing waste abrasive according to an embodiment of the present invention will be described in detail.
  • ceria (CeO 2 ) containing waste sludge, and a solvent solution containing a fluorine-based compound by mixing, selectively dissolving the silica (Si0 2 ) containing impurities contained in the waste sludge; Washing the ceria-containing waste sludge through a cross-flow fliltration system to selectively remove the silica (Si0 2 ) -containing impurities; And drying and firing the washed ceria-containing waste sludge.
  • the ceria-containing waste sludge derived from the waste abrasive is dissolved in a predetermined solution of a solvent to dissolve impurities derived from a glass substrate, and the like.
  • the waste abrasive containing ceria can be regenerated into regenerated abrasives.
  • the waste sludge treated with the solvent solution is washed while passing through a cross-flow fliltration system to remove the waste sludge and the solvent solution.
  • the impurities dissolved in the solid-liquid separation, and these impurities are removed.
  • the cross-flow filtration system used at this time includes a predetermined filter in the system,
  • the system refers to a system for filtering a target solution while continuously passing the target solution in a direction perpendicular to the filter through the upper space of the filter. That is, in such a cross flow filtration system, while the target solution passes through the system, impurities in the target solution may be caught by the filter while being continuously contacted with the lower filter, thereby filtering and removing the target solution.
  • the cleaning process may be performed while continuously passing the waste sludge treated with the solubilizer solution through the cross flow filtration system. Therefore, the regeneration method of one embodiment may continuously process the cleaning and regeneration process.
  • the waste sludge treated with the solvent solution continuously passes through the cross-flow filtration system, and the impurities dissolved in the solvent solution are filtered, solid-liquid separated and removed, the impurities are removed and washed efficiently. The yield of the whole regeneration process can be further improved.
  • the recycled abrasive obtained by the method of one embodiment can exhibit a desired polishing rate without fear of scratching by the large particles, and greatly reduces the need for additional redispersing, grinding or classifying processes for removing the large particles.
  • the regeneration method of one embodiment can efficiently remove the impurities contained in the ceria-containing waste abrasive material, and can efficiently regenerate the regeneration process including the cleaning process, and aggregate the ceria-containing abrasive during the cleaning process and generate large particles. Etc. can be suppressed.
  • FIG. 1 is a view schematically illustrating an example of a method for regenerating waste ceria-containing waste abrasive according to one embodiment
  • FIG. 2 is a cross-flow filtration used in a method of regenerating waste-containing abrasion containing ceria according to one embodiment. It is a figure which shows the basic principle and structure of a system typically.
  • the ceria-containing waste abrasive material and the waste sludge derived therefrom which is the object of the regeneration method of one embodiment, may be derived from a ceria-containing abrasive material used for polishing a glass substrate in a TFT-LCD manufacturing process.
  • the ceria-containing waste sludge or the like contains silica (Si0 2 ) and alumina (Al 2 0 3 ) derived from a glass substrate as main impurities.
  • the waste sludge and the waste abrasive material may include, as impurities, various polishing pads that have undergone polishing, various organic substances derived from back pads used to support the glass substrate to be polished, and the like (Fe), chromium (Cr). Or other metallic component-containing impurities such as nickel (Ni).
  • ceria (Ce0 2 ) -containing waste sludge and a dissolving agent solution containing a fluorine-based compound are mixed to selectively select silica (SiO 2 ) -containing impurities contained in the waste sludge. Melting process can proceed. At this time, the solubilizer solution without substantially dissolved in the ceria to be reproduced as the abrasive material from the waste sludge (e. G., About 0.01 by weight of the ceria content in the waste sludge 0 /.
  • the glass contained in the waste sludge and waste abrasive Substrate-derived impurities such as silica (Si0 2 ), alumina (Al 2 0 3 ), and the like, are selectively dissolved to allow the silica (Si0 2 ) -containing impurities to be nearly black to nearly 100% through subsequent cleaning steps. Can be removed completely As a result, it is possible to increase the removal rate of impurities, to suppress the loss of ceria together with the silica-containing impurities, and to greatly increase the regeneration rate of ceria.
  • the solubilizer solution comprises a hydrofluoric acid or hydrogen fluoride compound and a strong base of sodium or potassium hydroxide, or (a) a predetermined fluorine-based compound of NaHF 2 , (NH 4 ) HF 2 or KHF 2 , or (b) a combination of a predetermined fluorine salt of NaF, (NH 4 ) F or KF with a non-fluoric acid such as sulfuric acid, nitric acid or hydrochloric acid.
  • non-fluoric acid refers to hydrochloric acid, sulfuric acid, or nitric acid which does not contain fluorine in its chemical structure, and acids containing hydrofluoric acid, hydrogen fluoride compounds, and other fluorine may be excluded from the category of "non-fluoric acid.” Can be. Unless otherwise specified, “non-fluoric acid” is used in the above meaning.
  • the hydrofluoric acid or hydrogen fluoride compound is mainly used as a glass etching solution, and may also selectively dissolve impurities such as silica or alumina derived from the glass substrate.
  • the strong base can also selectively dissolve impurities such as silica derived from a glass substrate.
  • Fluorine compounds such as KHF 2 , or (b) fluorine salts such as NaF, (NH 4 ) F or KF, and a mixture of non-fluoric acid, have an ionization and dissociation state similar to the above-mentioned hydrofluoric acid when dissolved in a solvent solution. Accordingly, the glass substrate-derived impurities contained in the waste sludge and the waste abrasive material, for example, silica (Si0 2 ) and alumina (Al 2 0 3 ), etc., are selectively dissolved to completely or close to 100%. It can be almost completely removed.
  • solubilizer solution does not substantially dissolve ceria to be regenerated from the waste sludge as an abrasive, and such ceria can By suppressing the loss with impurities, the regeneration rate of ceria can be greatly increased.
  • the glass substrate-derived impurities contained in the waste sludge for example, silica and alumina, are treated. It can be selectively dissolved by the solvent solution and separated from the waste sludge.
  • the concentration of the fluorine compound, fluorine salt, non-fluoric acid acid or strong base including the hydrofluoric acid or hydrogen fluoride compound in the solubilizer solution can be appropriately adjusted.
  • compounds such as hydrofluoric acid, hydrogen fluoride compounds and other NaHF 2 and fluorine salts such as NaF may be used.
  • the fluorine-containing compound is included at a concentration of about 0.01 to 20M, or about 0.1 to 15M, or about 1 to 10M in the solvent solution.
  • the non-fluoric acid-based acid or strong base which may be included together with the hydrofluoric acid, hydrogen fluoride compound, or fluorine salt may be included at a concentration of about 0.01 to 20M, or about 0.1 to 15M, or about 1 to 10M in the solvent solution. If the concentration of each component in the solvent solution is too low, the removal efficiency of the impurities may be lowered, and if the concentration is too high, the amount of the raw material may be unnecessarily increased.
  • waste sludge after dissolving the ceria-containing waste sludge, in particular, the silica-containing impurities contained therein in a predetermined solvent solution, such waste sludge may be washed to selectively remove the silica-containing impurities from the waste sludge by solid-liquid separation.
  • the solvent solution does not substantially dissolve ceria to be regenerated from the waste sludge, it is possible to selectively remove and remove only the silica-containing impurities selectively dissolved in the solvent solution through the washing while lowering the loss rate thereof.
  • the washing process proceeds while continuously passing the waste sludge treated with the solvent solution through a cross-flow fliltration system.
  • the cross flow filtration system includes a predetermined filter in the system, and the filtration and solid-liquid separation proceed as the waste sludge-containing solution continuously passes in a direction perpendicular to the filter through the upper space of the filter.
  • the waste sludge-containing solution is continuously contacted with the lower filter while passing through the system, and liquid impurities (eg, silica or alumina, etc.) dissolved in the solvent solution are discharged to the filter and filtered.
  • Solid liquor can be separated and removed and the remaining waste sludge containing high concentrated solution can be withdrawn from the system without exiting through the filter.
  • the above-described process may be repeated while the highly concentrated solution is circulated and passed again through the cross-flow filtration system and the filter a plurality of times, for example, about 2 to 10 times.
  • the above-described cleaning process can be continuously processed to proceed more efficiently.
  • the waste sludge-containing solution continuously passes through the system and contacts the lower filter with a large surface area, impurities dissolved in the solvent solution are filtered, solid-liquid separated and removed, thereby removing and washing impurities.
  • Efficiency and the yield of the whole regeneration process can be improved more.
  • coarse grains of abrasive grains, formation of macroparticles, and the like can be suppressed during the cleaning process.
  • the cross-flow fliltration system is a ceramic material such as alumina or zirconia having a filter eye for filtering particles having a particle diameter of about 5 or less and black or about 0.002 to 5 It may include a filter.
  • a filter By the use of such a filter, the abrasive particles in the waste sludge can be filtered and lost by the filter to suppress the reduction of the regeneration yield, and more effectively to remove impurities dissolved in the solvent solution. While completely removable, the life of the filter can be improved.
  • the cross flow filtration system can remove the powder on the surface of the filter through a back pulse to the filter, thereby reducing the accumulation of powder on the filter or shortening the life of the filter, and cleaning and regeneration.
  • the overall process can be made more efficient.
  • the washing process may be performed by adding a separate washing liquid such as deionized water, water, or other aqueous solvent to the filtration system.
  • a separate washing liquid such as deionized water, water, or other aqueous solvent
  • the washing liquid may have a pH of 1 to 1. 4 or a solvent adjusted to pH 10-14.
  • an acid or a base may be appropriately dissolved in the water or deionized water and used as a washing liquid, and the impurities may be more completely removed through the above-described washing process.
  • the flux to be used in the sintering process to be described later may be added to the waste sludge to be recycled.
  • the washed ceria-containing waste sludge may be dried.
  • this drying step the above-mentioned dissolving agent solution treatment step, and to dry and remove the moisture in the cleaning process from the waste sludge with the impurities have been removed, and this waste sludge drying process conducted from about 1 weight 0/0 or less, Or dry to have a moisture content of about 0 to 1 weight 0 /.
  • This drying process may proceed with an oven dryer or compact disc dreyer.
  • the CD dryer is a type of disk type dryer in which the waste sludge is dried on a rotating disk that is heat-supplied.
  • the CD dryer is used to remove the grains between the abrasive particles (for example, ceria particles) during the drying process. Can be suppressed Therefore, it is possible to suppress the generation of macroparticles and to suppress the occurrence of scratches when using the recycled ceria-containing abrasive. Therefore, the said CD dryer can be used more suitably in a drying process. This is expected because the drying in the CD dryer can uniformly transfer heat to the waste sludge with high efficiency.
  • the drying step is carried out in an oven dryer for about 1 to 30 seconds with a silver of about 100 to 200 ° C, or on a CD dryer rotated at about 1 to 10 rpm, black to about 5 to 10 rpm, about 100 to 200 It can proceed for about 1 to 30 seconds at a temperature of ° C. If the rotation speed of the CD dryer is too low, or the drying time is too long, there is an increased risk of scratches caused by the generation of coarse particles, and conversely, if the rotation speed is too fast or the drying time is too short, However, the drying process may not be effective.
  • the recycled ceria-containing regenerated abrasive may have an appropriate average particle size of about 0.5 to 3.0, and the formation of large particles of about 6.0 GPa or more is suppressed, thereby reducing the possibility of scratches. rather, the drying proceeds efficiently the moisture content can be readily obtained the up to about 1 weight 0 / playback abrasive.
  • the dried waste sludge About 800 to 1200 ° C, black may proceed to about 800 to 1000 ° C, or 800 to 900 ° C.
  • the surface characteristics and crystal properties of the ceria-containing abrasive contained in the waste sludge can be restored, thereby increasing the polishing rate of the recycled abrasive and also removing impurities such as various organic substances derived from the pad.
  • the force is about 1 to 3.0 weight 0 /., Or about 1 to 2.0 weight 0 /., Black is about 1 to 1.5 weight 0 /.
  • the particle size distribution and the crystal size of the recycled abrasive are appropriately adjusted to the crystal sizes of about 0.5 to 3.0 and about 60 to 90 nm, respectively, The production of particles can be suppressed, the polishing rate of the regenerated abrasive can be adjusted well and the occurrence of scratches due to the generation of the large particles can be suppressed.
  • the flux is ammonium salt such as ammonium fluoride, ammonium chloride or ammonium sulfate; Alkali metal salts or alkaline earth metal salts such as sodium chloride, sodium fluoride, sodium hydroxide, potassium chloride, sodium borate or barium chloride; Metal oxides such as boron oxide; Metal oxygen acids, such as boric acid, can also be used, and 2 or more types selected from these can also be used together.
  • the surface characteristics or crystal characteristics of the recycled abrasive may be adjusted to a desirable range.
  • the flux may be wet mixed by being introduced in a previously cleaned washing step, or dry mixed immediately before the firing process, and may be wet mixed in the washing step as appropriate.
  • the firing step may be performed for about 1 to 4 hours at the above-mentioned temperature.
  • a ceria-containing regenerated abrasive having a crystal size of about 60 to 90 nm and an average particle size of about 0.5 to 3.0 / zm and suppressing the formation of large particles can be obtained. If the crystal size or the average particle size is too small, the polishing of the regenerated abrasive may not be possible. If the crystal size or the average particle size is too large, scratches may occur in the polishing process using the regenerated abrasive or after the firing process. Grinding and classification processes that proceed as needed may be unnecessarily inefficient.
  • the grinding process may be performed using a jet-mill Get-mill, etc.
  • the classification process may be performed by using a wind classifier such as a cyclone, a dry classifier, a dipole or a tripole tip. Proceed with a sieve for supply or classification.
  • impurities derived from the glass substrates are substantially completely and effectively removed, the entire regeneration process including the cleaning process is continuously processed and the efficiency is improved, the formation of coarse particles of ceria-containing abrasives during the cleaning process, generation of large particles, and the like. This can be suppressed.
  • a ceria-containing regenerated abrasive which exhibits excellent properties with excellent efficiency and yield and is suppressed from producing large particles can be obtained.
  • Such ceria-containing regenerated abrasives can be used alone or in combination with new abrasives to be recycled for polishing of glass substrates for LCDs, etc., which can greatly contribute to the economics and yield of the process.
  • the cleaning process and the regeneration process including the same can be efficiently performed in a continuous process, and the size and size of the ceria-containing abrasive material of the cleaning process is increased.
  • a method for regenerating ceria-containing waste abrasive materials which can suppress the production of particles and the like.
  • FIG. 1 is a view schematically showing an example of a method for regenerating waste ceria-containing waste abrasive according to one embodiment for each step.
  • FIG. 2 is a view schematically showing the basic principle and configuration of the cross-flow filtration system used in the method for regenerating waste ceria-containing waste abrasive of one embodiment.
  • 3 to 5 after the progress to the cleaning process in Examples 1 to 3, It is a graph which measured the particle size distribution of the obtained recycled abrasive.
  • FIG. 6 to 8 are graphs in which particle size distributions of the recycled abrasives obtained are measured after advancing to the washing step in Comparative Examples 1 to 3.
  • FIG. 6 to 8 are graphs in which particle size distributions of the recycled abrasives obtained are measured after advancing to the washing step in Comparative Examples 1 to 3.
  • Example 2 Regeneration of ceria-containing waste abrasive
  • Example 3 Regeneration of ceria-containing waste abrasive A recycled abrasive of Comparative Example 3 was obtained in the same manner as in Comparative Example 2, except that 4 kg of NH 4 F and hydrogen peroxide were used instead of NaHF 2 . After the cleaning process, it was confirmed that the ion conductivity (IC) value was dropped from 30mS / cm to 1500yS / cm, but the residual content of silica was 0.2 weight 0 /.
  • IC ion conductivity

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Grinding-Machine Dressing And Accessory Apparatuses (AREA)

Abstract

La présente invention concerne un procédé de régénération d'un agent de polissage contenant de l'oxyde de cérium usé, le procédé permettant au processus de régénération, comprenant un processus de nettoyage, d'être efficace et supprimant la re-coagulation de l'agent de polissage contenant de l'oxyde de cérium au cours du processus de nettoyage, tout en éliminant efficacement les impuretés contenues dans l'agent de polissage contenues dans l'agent de polissage contenant de l'oxyde de cérium usé. Le procédé de régénération de l'agent de polissage contenant de l'oxyde de cérium usé comprend les étapes consistant à : mélanger de la boue contenant de l'oxyde de cérium (CeO2) usé et un solvant contenant un composé de fluor, et à dissoudre sélectivement les impuretés contenant de la silice (SiO2) contenues dans la boue usée ; à nettoyer la boue contenant de l'oxyde de cérium usé en la faisant passer dans un système de filtration à écoulement transversal et à rejeter sélectivement les impuretés contenant de la silice (SiO2) ; et à sécher et à fritter la boue contenant de l'oxyde de cérium usé épurée.
PCT/KR2013/008222 2012-09-14 2013-09-11 Procédé de régénération d'un agent de polissage contenant de l'oxyde de cérium usé Ceased WO2014042431A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
CN201380047554.0A CN104619462B (zh) 2012-09-14 2013-09-11 含氧化铈废磨料的再生方法
JP2015531851A JP5940224B2 (ja) 2012-09-14 2013-09-11 セリア含有廃研磨材の再生方法

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
KR10-2012-0102369 2012-09-14
KR20120102369 2012-09-14
KR1020130108820A KR101539419B1 (ko) 2012-09-14 2013-09-11 세리아 함유 폐연마재의 재생 방법
KR10-2013-0108820 2013-09-11

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105419645A (zh) * 2014-09-16 2016-03-23 旭硝子株式会社 抛光浆料的再生方法、基板的制造方法
CN114084974A (zh) * 2021-11-23 2022-02-25 上海赛奥分离技术工程有限公司 一种玻璃研磨液的处理方法

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JP2011502054A (ja) * 2007-10-30 2011-01-20 ポール・コーポレーション 使用済み研磨スラリーを処理するための方法
KR101051207B1 (ko) * 2011-02-09 2011-07-21 윤종훈 희토류 금속 산화물을 기반으로 하는 ｌｃｄ 및 ｐｄｐ 유리패널용 재생 무기 연마재 및 이를 제조하기 위한 무기 연마재 폐슬러지 재생 방법
JP2011189503A (ja) * 2010-03-12 2011-09-29 Lg Chem Ltd 酸化セリウム研磨材のリサイクル方法
KR20110132458A (ko) * 2009-03-25 2011-12-07 어플라이드 머티어리얼스, 인코포레이티드 화학기계적 폴리싱 슬러리의 소요지 재생 시스템
KR20120021478A (ko) * 2010-08-03 2012-03-09 주식회사 랜코 세리아계 연마재의 재생방법

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Publication number Priority date Publication date Assignee Title
JP2011502054A (ja) * 2007-10-30 2011-01-20 ポール・コーポレーション 使用済み研磨スラリーを処理するための方法
KR20110132458A (ko) * 2009-03-25 2011-12-07 어플라이드 머티어리얼스, 인코포레이티드 화학기계적 폴리싱 슬러리의 소요지 재생 시스템
JP2011189503A (ja) * 2010-03-12 2011-09-29 Lg Chem Ltd 酸化セリウム研磨材のリサイクル方法
KR20120021478A (ko) * 2010-08-03 2012-03-09 주식회사 랜코 세리아계 연마재의 재생방법
KR101051207B1 (ko) * 2011-02-09 2011-07-21 윤종훈 희토류 금속 산화물을 기반으로 하는 ｌｃｄ 및 ｐｄｐ 유리패널용 재생 무기 연마재 및 이를 제조하기 위한 무기 연마재 폐슬러지 재생 방법

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105419645A (zh) * 2014-09-16 2016-03-23 旭硝子株式会社 抛光浆料的再生方法、基板的制造方法
CN114084974A (zh) * 2021-11-23 2022-02-25 上海赛奥分离技术工程有限公司 一种玻璃研磨液的处理方法

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