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CN-121990880-A - Production method of electronic grade hydroquinone

CN121990880ACN 121990880 ACN121990880 ACN 121990880ACN-121990880-A

Abstract

The invention relates to a production method of electronic grade hydroquinone, sending industrial grade hydroquinone from outside of a boundary area and solvent into a stirring and heating mixer for stirring and mixing, after obtaining hydroquinone solution, sending into a microfilter to remove particles above 0.2 mu m, then sending into an ion remover to remove anions and cations in hydroquinone, then sending into a nanofiltration filter to remove particles above 10nm, finally sending into a crystallizer for crystallization treatment, and drying the obtained crystallized product to obtain the high-purity hydroquinone product meeting SEMI C12 standard 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 hydroquinone with the requirements of G4.

Inventors

  • HOU JINGWEI
  • XU PENG
  • WU LIPING
  • HUANG XUDONG
  • SONG ZIHANG
  • YU YANG
  • 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 hydroquinone features that industrial grade hydroquinone and solvent from outside boundary area are mixed in a stirring and heating mixer to obtain hydroquinone solution, the hydroquinone solution is first eliminated in a microfilter to 0.2 micron or more, the ion eliminating device to eliminate negative and positive ions from hydroquinone, the nano filter to eliminate 10nm or more of grains, the crystallizer to crystallize, and the crystallized product is dried to obtain high purity hydroquinone product meeting SEMI C12 standard or above.
  2. 2. The method for producing electronic grade hydroquinone 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 the hydroquinone is 1-15:1.
  3. 3. The method according to claim 1, wherein the micro filtration membrane used in the micro filter is one of polytetrafluoroethylene membrane, polyethersulfone membrane, polyvinylidene fluoride membrane, polyimide membrane, and polyamide membrane having a pore size of 0.1 to 0.5 μm.
  4. 4. The method for producing electronic grade hydroquinone according to claim 1, wherein the ion remover adopts ion exchange resin or ion exchange fiber for ion removal treatment.
  5. 5. The method for producing electronic grade hydroquinone 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, 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.
  6. 6. The method for producing electronic grade hydroquinone according to claim 1, wherein the nanofiltration membrane used in the nanofiltration 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.
  7. 7. The process for the production of electronic grade hydroquinone according to claim 1, characterized in that the crystallizer is provided with 2 or more stages, each stage having a crystallization temperature of 20-170 ℃.
  8. 8. The process for producing electronic grade hydroquinone as claimed in claim 1, wherein the crystallizer is a suspension stirring crystallizer, a plate crystallizer or a melt crystallizer.
  9. 9. The process for producing electronic grade hydroquinone as claimed in claim 1, wherein the dryer temperature is not more than 180 ℃.
  10. 10. A production plant for electronic grade hydroquinone for carrying out the production method according to any one of claims 1 to 9, characterized in that it comprises, connected in succession: A stirring and heating mixer for preparing the hydroquinone 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 hydroquinone Technical Field The invention belongs to the technical field of electronic grade hydroquinone, and relates to a production method of electronic grade hydroquinone by using industrial grade hydroquinone as a raw material. Background With the rapid development of technologies in the fields of semiconductors, power batteries, medicines and chemical industry, 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 hydroquinone has been widely used as an important electronic chemical in the fields of power batteries, medicine, semiconductor lithography, and the like. Along with the processing size of integrated circuits entering the nanometer age, the service life requirement of power batteries is higher and higher, the life health is stricter and stricter to medical standards, and higher requirements are put on high-purity hydroquinone matched with the power batteries, so that the SEMI C12 standard formulated by international semiconductor equipment and material organization is required to be met, and the metal cation content is less than 100ppt. 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. For example, chinese patent application CN202310338042.5 provides a method for producing hydroquinone as an electronic chemical, which comprises 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 hydroquinone meeting the requirements of electronic chemicals G4 and above can be obtained in the patent, the whole steps are complex, the energy consumption of the steps of flash evaporation or rectification separation is high, and side reactions exist. Disclosure of Invention The invention aims to provide a production method of electronic grade hydroquinone, 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 production method of electronic grade hydroquinone, which comprises the steps of sending industrial grade hydroquinone from outside a boundary area and a solvent into a stirring and heating mixer for stirring and mixing to obtain hydroquinone solution, sending the hydroquinone solution into a microfilter to remove particles with the particle size of more than 0.2 mu m, sending the hydroquinone solution into an ion remover to remove anions and cations in the hydroquinone, sending the hydroquinone solution into a nanofiltration device to filter out particles with the particle size of more than 10nm, sending the hydroquinone solution into a crystallizer to carry out crystallization treatment, and drying the obtained crystallized product to obtain a high-purity hydroquinone product meeting SEMI C12 standard 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 molar ratio of the solvent to hydroquinone is 1-15:1, and can be 1:1,5:1,10:1,15:1 and other ratio values. Further, the micro-filtration membrane used in the micro-filter is one of polytetrafluoroethylene membrane, polyethersulfone membrane, polyvinylidene fluoride membrane, polyimide membrane and polyamide membrane with pore diameter of 0.1-0.5 μm. Further, the ion remover adopts ion exchange resin or ion exchange fiber to carry out ion removal treatment. 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. Furthermore, the nanofiltration membrane used in the nanofiltration is a polytetrafluoroethylene membrane, a polyethersulfone membrane, a polyvinylidene fluoride membrane, a polyimide membrane or a polyamide membrane with the pore diameter of 10-50 nm. Further, the crystallizer is provided with 2 stages or more, and the crystallization temperature of each stage is 20-170 ℃. Further, the crystallizer is a suspension stirring crystallizer, a plate-type crystallizer or a melting crystallizer. Further, the temperature of the dryer is not more than 180 ℃. In another aspect, the