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CN-121990881-A - Production method of electronic grade catechol

CN121990881ACN 121990881 ACN121990881 ACN 121990881ACN-121990881-A

Abstract

The invention relates to a production method of electronic grade catechol, which comprises the steps of stirring, heating and mixing industrial grade catechol from outside a boundary area with a solvent to prepare catechol solution, and then sequentially carrying out procedures of microfiltration, ion removal, nanofiltration, crystallization and drying to obtain a high-purity catechol product meeting SEMI C12 standards and above. Compared with the prior art, the method has the advantages of short flow, low energy consumption, good separation effect, strong process continuity, high purity and low impurity content, and can meet the production of high-purity catechol with the requirements of G4 above.

Inventors

  • HOU JINGWEI
  • YU YANG
  • WU LIPING
  • HUANG XUDONG
  • XU PENG
  • SONG ZIHANG
  • YE HAIBO

Assignees

  • 中石油(上海)新材料研究院有限公司
  • 中国石油天然气股份有限公司

Dates

Publication Date
20260508
Application Date
20241105

Claims (10)

  1. 1. The production process of electronic grade catechol features that industrial grade catechol from outside boundary area and solvent are mixed through stirring and heating to prepare catechol solution, and the catechol solution is further micro filtered, ion eliminated, nano filtered, crystallized and dried to obtain high purity catechol product meeting SEMIC standard and beyond.
  2. 2. The method for producing electronic grade catechol according to claim 1, wherein the solvent is one or a combination of several of water, methanol, ethanol, n-propanol, isopropanol, acetone, methyl acetate and ethyl acetate, and the molar ratio of the solvent to catechol is 0.32-0.62:1.
  3. 3. The method for producing electronic grade catechol according to claim 1, wherein the microfiltration process is performed in a microfilter to remove particles having a particle diameter of 0.2 μm or more.
  4. 4. The method for producing electronic grade catechol according to claim 1, wherein the ion removal process is to remove anions and cations in catechol by ion exchange resin or ion exchange fiber in an anion and cation remover.
  5. 5. The method for producing electronic grade catechol according to claim 4, wherein the ion exchange resin is one or more of sulfonic styrene resin, carboxyl styrene resin, quaternary amine styrene resin, perfluorinated sulfonic acid resin and sulfonated polyether sulfone resin, and the particle size of the ion exchange resin is 0.3-0.6 mm; The ion exchange fiber is one or more of sulfostyrene fiber, carboxyl styrene fiber, quaternary amine styrene fiber, perfluorinated sulfonic acid fiber and sulfonated polyether sulfone fiber.
  6. 6. The method for producing electronic grade catechol according to claim 1, wherein the nanofiltration step is performed in a nanofiltration membrane, and particles of 10nm or more are filtered out.
  7. 7. The method for producing electronic grade catechol of claim 6, wherein the nanofiltration membrane is a polytetrafluoroethylene membrane, a polyethersulfone membrane, a polyvinylidene fluoride membrane, a polyimide membrane or a polyamide membrane with a pore size of 10-50 nm.
  8. 8. The method for producing electronic grade catechol according to claim 1, characterized in that the crystallization process is performed in a crystallizer, the crystallizer is at least one grade, and the crystallization temperature of each grade is 10-100 ℃.
  9. 9. The method for producing electronic grade catechol of claim 1, wherein the drying temperature is 70-110 ℃.
  10. 10. An apparatus for producing electronic grade catechol for use in the implementation of a production process according to any of the claims 1 to 9, characterized in that said apparatus comprises, connected in sequence: a stirring and heating mixer for preparing the catechol solution; a micro filter for performing a micro filtering process; An anion and cation remover for performing an ion removal process; A nanofiltration device for performing a nanofiltration process; a crystallizer for performing a crystallization process; And a dryer for performing a drying process.

Description

Production method of electronic grade catechol Technical Field The invention belongs to the technical field of electronic grade catechol production, and relates to a production method of electronic grade catechol. Background With the rapid development of the technology in the fields of semiconductors, batteries and medicines, the requirements on high-purity chemical reagents are increasing. The purity and cleanliness of the alloy have great influence on the yield, the electrical performance and the reliability. High purity catechol has been widely used as an important electronic chemical in the fields of power batteries, medicine and semiconductors. As integrated circuit processing dimensions enter the nanoera, higher requirements are put on catechol matched with the integrated circuit processing dimensions, and the integrated circuit processing dimensions are required to meet SEMI C12 standards formulated by international semiconductor equipment and material organizations, wherein the metal cation content is less than 100 ppt. There are few domestic studies on high-quality and high-purity reagents, and the data which can be retrieved are mostly in the aspect of basic technology and patent report. The international high-purity reagent process route belongs to industry confidentiality, and some basic technologies also apply for patent protection. Chinese patent application CN202310337953.6 provides a method for producing catechol as an electronic chemical product, which includes a dissolution step, a microfiltration step, an anion and cation removal step, a flash separation step or a rectification separation step, a nanofiltration step, a crystallization step and a drying step. Although catechol satisfying the requirements of the electronic chemical G4 and above can be obtained in this patent, the whole steps are complicated, and the energy consumption of the flash evaporation or rectification separation step is high, and there are side reactions. Disclosure of Invention The invention aims to provide a production method of electronic grade catechol, which has the advantages of short flow, low energy consumption, good separation effect, strong process continuity, high purity, low impurity content and the like. The aim of the invention can be achieved by the following technical scheme: In one aspect, the invention provides a method for producing electronic grade catechol, which comprises the steps of stirring, heating and mixing industrial grade catechol from outside a boundary area with a solvent to prepare a catechol solution, and then sequentially carrying out microfiltration, ion removal, nanofiltration, crystallization and drying procedures to obtain a high-purity catechol product meeting SEMIC (G4) standards and above. Further, the solvent is one or a combination of more of water, methanol, ethanol, n-propanol, isopropanol, acetone, methyl acetate and ethyl acetate, and the feeding mole ratio of the solvent to catechol is 0.32-0.62:1. Further, the microfiltration step is performed in a microfilter to remove particles having a particle diameter of 0.2 μm or more. Further, the ion removal procedure is to remove anions and cations in catechol in an anion and cation remover through ion exchange resin or ion exchange fiber. Further, the ion exchange resin is one or more of sulfonic styrene resin, carboxyl styrene resin, quaternary amine styrene resin, perfluorinated sulfonic acid resin and sulfonated polyether sulfone resin; The ion exchange fiber is one or more of sulfostyrene fiber, carboxyl styrene fiber, quaternary amine styrene fiber, perfluorinated sulfonic acid fiber and sulfonated polyether sulfone fiber. Further, the nanofiltration step is performed in a nanofiltration membrane, and particles of 10nm or more are filtered off. Furthermore, the nanofiltration membrane is a polytetrafluoroethylene membrane, a polyethersulfone membrane, a polyvinylidene fluoride membrane, a polyimide membrane or a polyamide membrane with the aperture of 10-50 nm. Further, the crystallization step is performed in a crystallizer at a crystallization temperature of 10 to 100 ℃. The crystallizer is at least one stage, preferably two or more stages. Further, the drying temperature is 70-110 ℃. In another aspect, the present invention provides a production apparatus for electronic grade catechol for carrying out the production method as described above, the production apparatus comprising, in succession: a stirring and heating mixer for preparing the catechol solution; a micro filter for performing a micro filtering process; An anion and cation remover for performing an ion removal process; A nanofiltration device for performing a nanofiltration process; a crystallizer for performing a crystallization process; And a dryer for performing a drying process. Although catechol products meeting the requirements of the electronic chemical G4 and above can be obtained in the prior art such as CN202310337953.6, the whole process is com