A production method of electronic chemical resorcinol

Abstract

The production method of electronic chemical resorcin of the present invention comprises a dissolving step, a microfiltration step, an anion and cation removal step, a nanofiltration step, a flash separation step or a distillation separation step, a crystallization step and a drying step. The dissolving step is to dissolve industrial-grade resorcin to obtain a resorcin solution; the flash separation step is to separate the components of the resorcin solution through a flash tank; the distillation separation step is to separate the components of the resorcin solution through a first distillation tower and a second distillation tower; the crystallization step is to crystallize the resorcin solution after the nanofiltration step; and the drying step is to dry the resorcin product after the crystallization step. A heating step is also included. The production method of the present invention has good separation effect and strong process continuity. The bulkhead tower used can reduce the number of conventional distillation towers by half, reduce equipment, reduce energy consumption, and shorten the process; the obtained product meets the requirements of the highest electronic chemical standard SIMIC12 (G4) and above for high-purity resorcin.

Description

Technical Field

[0001] The present invention belongs to the technical field of electronic chemical preparation, and relates to high-purity electronic chemical resorcinol in the fields of semiconductors, display panels, solar energy, power batteries, medicine, chemical industry, etc., and specifically relates to a production method of electronic chemical resorcinol. Background Art

[0002] Resorcinol, also known as 1,3-benzene, is an organic compound with the chemical formula C6H6O2. Resorcinol is an important raw material for the production of synthetic resins, adhesives, dyes, medicines, ultraviolet absorbers, photographic film primers, explosives, and cosmetics.

[0003] High-purity electronic-grade resorcinol is usually purified from industrial-grade hydroquinone raw materials. For example, Chinese patent application CN 216472987 U discloses an electronic-grade catechol production device, which processes industrial-grade catechol through melt crystallization, distillation, and ion exchange to improve the purity of catechol. However, the finished particles cannot meet the requirements of SEMI C12 (G4) and SEMI C12 (G5).

[0004] The applicant's Chinese patent application CN114870420A discloses a high-purity electronic grade isopropyl alcohol production device, including: industrial grade isopropyl alcohol is subjected to microfiltration, anion and cation removal, dehydration treatment or precision distillation tower, nanofiltration, and the microfiltration and anion and cation removal cannot be dehydrated or distilled at the same time before and after; when there is no dehydration treatment and distillation before microfiltration and anion and cation removal, distillation and nanofiltration or only distillation are performed after microfiltration and anion and cation removal; when microfiltration and anion and cation removal only include anion and cation removal and the dehydration treatment or distillation before it, anion and cation removal Then nanofiltration; when microfiltration and anion and cation removal only include anion and cation removal and there is no dehydration and distillation in series before, the anion and cation removal is followed by a distillation tower and nanofiltration. The process device and physical parameters of this patent can obtain electronic-grade products of isopropanol, but due to the fact that the process parameters of different chemical products, especially different isomers of hydroquinone, have a greater impact on the purification results, the applicant has tested that it cannot be directly used for the preparation of electronic-grade products of crystalline powder chemical products. This application provides a preparation method for electronic-grade products directly used for hydroquinone.

[0005] At present, high-purity electronic-grade resorcinol is usually purified from industrial-grade resorcinol raw materials. The purity currently produced in my country can only meet the industrial grade standard, and there is no production technology that can reach the pharmaceutical grade and electronic grade G1 and above industry application standards. Summary of the invention

[0006] In view of the above problems, the present invention provides a method for producing electronic chemical resorcinol. The production method of the present invention has good separation effect and strong process continuity. The dividing wall tower used can reduce the number of conventional distillation towers by half, reduce equipment, reduce energy consumption, and shorten the process. The obtained product has high purity and low impurity content, and finally realizes the production of high-purity resorcinol that meets the highest standard SIMI C12 (G4) and above requirements of electronic chemicals from industrial-grade resorcinol.

[0007] To achieve the above-mentioned purpose of the invention, the present invention provides the following technical scheme: a method for producing electronic chemical resorcinol, the production method comprising the following steps: dissolving industrial-grade resorcinol to obtain a resorcinol solution; removing particles with a particle size of 0.2 μm or more; removing anions and cations in the resorcinol solution; removing organic impurities and solvents in the resorcinol solution; and removing particles with a particle size of 10 nm or more.

[0008] Furthermore, the preparation of the electronic chemical resorcinol also requires crystallization and drying steps.

[0009] The mass content of resorcinol in industrial-grade resorcinol raw materials is more than 98%. It is dissolved into a solution by a solvent through a stirring heater, and then enters a microfilter to remove large particles in the resorcinol solution and enters an anion and cation removal device; then enters a separator, which uses a flash tank or a conventional distillation tower or a bulkhead tower. The bulkhead tower can reduce the number of conventional distillation towers by half; the resorcinol after the separator enters a nanofiltration device, removes fine particles, and finally obtains the product through crystallization and drying. The separator can be 0-6 according to actual needs, and auxiliary equipment such as pumps and heat exchangers are common equipment.

[0010] Furthermore, a microfilter is used to remove particles with a particle size of 0.2 μm or more, wherein the microfiltration membrane is selected from a polytetrafluoroethylene membrane, a polyethersulfone membrane, a polyvinylidene fluoride membrane (PVDF), a polyimide membrane and a polyamide membrane with a pore size of 0.1-0.5 μm, and a pore size uniformity coefficient of 1.1-1.4;

[0011] The anions and cations in the resorcinol solution are removed by using an ion exchange resin and / or ion exchange fiber with a particle size of 0.3-0.6 mm, which is one or more of sulfonic acid styrene resin or fiber, carboxyl styrene resin or fiber, quaternary amino styrene resin or fiber, perfluorosulfonic acid resin or fiber, sulfonated polyethersulfone resin or fiber, and the pore size uniformity coefficient is 1.08-1.3;

[0012] Nanofiltration is used to remove particles with a particle size of more than 10nm, and the nanofiltration membrane is selected from one of polytetrafluoroethylene membrane, polyethersulfone membrane, polyvinylidene fluoride membrane (PVDF), polyimide membrane or polyamide membrane with a pore size of 10-50nm, and the pore size uniformity coefficient is 1.06-1.4.

[0013] Furthermore, the microfilter uses a polytetrafluoroethylene membrane with a pore size of 0.2 μm and a uniformity coefficient of 1.25; the ion exchange resin uses a mixed resin with a particle size of 0.6 mm, a uniformity coefficient of 1.1, and a volume ratio of sulfonic acid styrene resin and quaternary amino styrene of 2:1; the nanofilter uses a polytetrafluoroethylene membrane with a pore size of 20 nm and a uniformity coefficient of 1.2;

[0014] The microfilter uses a polyimide membrane with a pore size of 0.4μm and a uniformity coefficient of 1.15; the ion exchange resin uses a mixed resin with a particle size of 0.3mm, a uniformity coefficient of 1.3, and a volume ratio of 3:2 between perfluorosulfonic acid and quaternary aminostyrene; the nanofilter uses a polyimide membrane with a pore size of 10nm and a uniformity coefficient of 1.25.

[0015] The beneficial effects of the present invention are:

[0016] First, the process of the present invention is simple. First, industrial resorcinol is dissolved into a solution; a microfilter removes large particles (particles larger than 0.2 μm) in the resorcinol solution; then an ion exchange resin or an ion exchange fiber removes cations and anions in the resorcinol; a separator removes organic impurities and solvents in the resorcinol; a nanofilter removes tiny particle impurities (particles larger than 10 nm) in the resorcinol; a crystallizer removes organic impurities and solvents; a dryer removes solvents; and finally the product meets the electronic chemical SIMI C12 (G4) standard and above requirements. The present invention realizes the production of high-purity resorcinol that meets the electronic chemical standard requirements from industrial-grade resorcinol.

[0017] Secondly, the separator of the present invention adopts a multi-stage flash tank, a conventional distillation tower and / or a next-door distillation tower. Under the condition of meeting the same separation degree requirement, the next-door tower can greatly reduce the number of conventional distillation towers, and can reduce the original 2 distillation towers to 1, the original 4 distillation towers to 2, and the conventional 6 distillation towers to 3 distillation towers, that is, greatly reducing energy consumption and investment, and shortening the process. According to the actual raw materials and product standard requirements, the number of separators can be increased or 0-4,

[0018] Furthermore, the solvent used to dissolve the industrial-grade resorcinol is one or more of water, methanol, ethanol, n-propanol, isopropanol, acetone, methyl acetate, and ethyl acetate.

[0019] The production method removes metal impurities, non-metal impurities and organic impurities in the industrial-grade resorcinol, including gold, silicon, germanium, gallium, boron, tin, calcium, lead, iron, manganese, sulfate and other organic impurities.

[0020] The production method removes metal impurities and non-metal impurities in the industrial-grade resorcinol, and the metal impurities and non-metal impurities include at least one of the following: a first type, sodium, iron and potassium; a second type, sodium, iron, potassium, magnesium, copper, zinc, lead, arsenic, calcium, silver and silicon; a third type, sodium, iron, copper, calcium, potassium and silicon; and a fourth type, sodium, iron, copper, calcium, potassium, silicon, magnesium, manganese, zinc, lead, arsenic, aluminum, silver and cobalt. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1 It is a schematic diagram of an embodiment of the production method and production device of the electronic chemical resorcinol of the present invention.

[0022] Figure 2 It is a schematic diagram of Example 1 of the production method and production device of electronic chemical resorcinol of the present invention.

[0023] Figure 3 It is a schematic diagram of Example 2 of the production method and production device of electronic chemical resorcinol of the present invention.

[0024] Figure 4 It is a schematic diagram of Example 3 of the production method and production device of electronic chemical resorcinol of the present invention.

[0025] Figure 5 It is a schematic diagram of Example 4 of the production method and production device of electronic chemical resorcinol of the present invention.

[0026] Figure 6 It is a schematic diagram of Example 5 of the production method and production device of electronic chemical resorcinol of the present invention.

[0027] Figure 7 It is a schematic diagram of Example 6 of the production method and production device of electronic chemical resorcinol of the present invention.

[0028] Figure 8 These are several forms of the dividing wall tower, A is the middle dividing wall, B is the upper dividing wall, and C is the lower dividing wall.

[0029] Description of reference numerals:

[0030] 1 industrial grade resorcinol; 2 solvent; 3 stirring and heating mixer; 4 resorcinol solution; 5 microfilter; 6 resorcinol after microfiltration; 7 anion and cation remover; 8 resorcinol after deionization; 9 primary separator; 10 light component; 11 heavy component; 12 resorcinol after primary separation; 13 nanofilter; 14 resorcinol after nanofiltration; 15 crystallizer; 16; crystallization mother liquor; 17 resorcinol product after crystallization; 18 dryer; 19 electronic grade resorcinol product; 20 secondary separator; 21 resorcinol after secondary separation; 24 tertiary separator DETAILED DESCRIPTION

[0031] The following examples further illustrate the content of the present invention, but should not be construed as limiting the present invention. Without departing from the spirit and substance of the present invention, modifications or substitutions made to the methods, steps or conditions of the present invention all fall within the scope of the present invention.

[0032] Example

[0033] like Figure 1 As shown, the production device of electronic chemical resorcinol of the present invention includes a stirring and heating mixer, a microfilter, an anion and cation remover, a nanofilter, a separator, a crystallizer, a dryer and corresponding auxiliary equipment such as pumps and heat exchangers connected in series from feeding to discharging. The separator adopts a partition wall distillation tower, which is in the form of a middle partition wall. The method of the present invention has a short process, low energy consumption, good separation effect, strong process continuity, high product purity, low impurity content, and obtains high-purity electronic grade resorcinol that meets the electronic chemical standard SEMI C12 (G4) and above.

[0034] The industrial-grade resorcinol (1) and solvent (2) used in the present invention enter a stirring and heating mixer (3) to obtain a resorcinol solution (4), which then enters a microfilter (5) for removing particles larger than 0.2 μm (micrometer). The microfilter can be a polytetrafluoroethylene membrane, a polyethersulfone membrane, a polyvinylidene fluoride membrane (PVDF), a polyimide membrane, a polyamide membrane or other membranes of equivalent properties with a pore size of 0.1-0.5 μm.

[0035] After microfiltration, the product enters an anion and cation remover (7), which is used to remove anions and cations in resorcinol. The anion and cation remover can use ion exchange resin or ion exchange fiber, wherein the ion exchange resin uses a customized functional resin, and the ion exchange fiber uses a customized functional fiber, mainly including one or more of sulfonic acid styrene resin or fiber, carboxyl styrene resin or fiber, quaternary amino styrene resin or fiber, perfluorosulfonic acid resin or fiber, and sulfonated polyethersulfone resin or fiber;

[0036] After the anions and cations are removed, the resorcinol solution (8) enters the nanofilter (13), which is used to filter out particles larger than 10 nm (nanometers). The membrane of the nanofilter (13) can be a polytetrafluoroethylene membrane with a pore size of 10-50 nm, a polyethersulfone membrane, a polyvinylidene fluoride membrane (PVDF), a polyimide membrane, a polyamide membrane or other membranes of equivalent properties.

[0037] After nanofiltration, the product enters a separator (9). The number of separators can be increased by 0-6 according to the requirements of raw materials and product standards. The area ratio of the two sides of the distillation tower is in the range of 2:8 to 8:2. The forms of the distillation tower mainly include the middle distillation tower, the upper distillation tower and the lower distillation tower, but are not limited to the above three types. The resorcinol obtained by the separator enters a crystallizer (15). The crystallizer can be 0-3 levels according to the requirements. The crystallizer can be a suspension stirring crystallizer, a plate crystallizer or a melting crystallizer, or a combination of several of them. The product (17) obtained after crystallization passes through a dryer (18) to obtain a resorcinol product that meets the requirements of the SIMI C12 (G4) standard.

[0038] The resorcinol raw material of the present invention is industrial-grade resorcinol, with a resorcinol mass content of more than 98%, a water content of more than 500ppm, a metal ion of more than 500ppt, an anion of more than 500ppb, and more than 1000 particles larger than 0.2μm / mL. Table 1 shows the components contained in the resorcinol raw material, which does not limit the applicability of the invention. The resorcinol products produced by the production method and device of the present invention can meet the requirements of SEMI C12 (G4) and above standards.

[0039] Example 1

[0040] like Figure 2 As shown, the production device of electronic chemical resorcinol of the present invention comprises a stirring and heating mixer, a microfilter, an anion and cation remover, a flash tank, a nanofilter, a crystallizer and a dryer which are connected in series from feeding to discharging.

[0041] Resorcinol and solvent water enter the stirring and mixing heater (3) at a molar ratio of 0.32:1, are heated to 85°C and then enter the microfilter, the microfilter uses a polytetrafluoroethylene membrane with a pore size of 0.2μm and a uniformity coefficient of 1.25; the ion exchange resin uses a mixed resin with a particle size of 0.6mm, a uniformity coefficient of 1.1, and a volume ratio of sulfonic acid styrene resin and quaternary amino styrene of 2:1; the separator (9) uses a flash tank with a pressure of 100kPa and a temperature of 119°C; the nanofilter uses a polytetrafluoroethylene membrane with a pore size of 20nm and a uniformity coefficient of 1.2; the crystallizer (15) uses two-stage crystallization, which is plate crystallization and falling film crystallization, and the crystallization temperatures are 96°C and 104°C respectively; the drying conditions are 90°C, 70kPa, and 2h. A high-purity resorcinol product higher than the SEMI C12 (G4) standard is obtained, and the product indicators are shown in Table 2.

[0042] Example 2

[0043] like Figure 3 As shown, the production device of electronic chemical resorcinol of the present invention comprises a stirring and heating mixer, a microfilter, an anion and cation remover, a conventional distillation tower, a nanofilter and a crystallizer which are sequentially connected in series from feeding to discharging.

[0044] Resorcinol and solvent ethanol enter the stirring mixing heater (3) at a molar ratio of 0.5, are heated to 72°C and then enter the microfilter, the microfilter uses a polyimide membrane with a pore size of 0.4 μm and a uniformity coefficient of 1.15; the ion exchange resin uses a mixed resin with a particle size of 0.3 mm, a uniformity coefficient of 1.3, and a volume ratio of perfluorosulfonic acid and quaternary aminostyrene of 3:2; the separator (9)(20) uses two conventional distillation towers, of which the separator (9) is the first A distillation tower, the separator (20) is a second distillation tower, the top pressure of the first distillation tower is 25 kPa, the top temperature is 70.8°C, the number of theoretical plates is 12, and the reflux ratio is 1.5; the top pressure of the second distillation tower is 2 kPa, the top temperature is 163°C, the number of theoretical plates is 10, and the reflux ratio is 1.5; the nanofilter (13) uses a polyimide membrane with a pore size of 10 nm and a uniformity coefficient of 1.25; the crystallizer (15) uses a first-stage falling film crystallization, and the crystallization temperature is 97°C. A high-purity resorcinol product higher than the SEMI C12 (G4) standard is obtained, and the product indicators are shown in Table 2.

[0045] Example 3

[0046] like Figure 4 As shown, the production device of electronic chemical resorcinol of the present invention comprises a stirring and heating mixer, a microfilter, an anion and cation remover, a nanofilter, a dividing wall tower and a crystallizer connected in series from feeding to discharging. The dividing wall distillation tower is in the form of a dividing wall tower A type (middle dividing wall), a condenser and a reboiler.

[0047] Resorcinol and solvent isopropanol enter the stirring and mixing heater (3) at a molar ratio of 0.50, are heated to 55°C and then enter the microfilter, the microfilter uses a polyamide membrane with a pore size of 0.2μm and a uniformity coefficient of 1.35; the ion exchange resin uses a mixed resin with a particle size of 0.5mm, a uniformity coefficient of 1.12, and a volume ratio of sulfonate styrene resin A and quaternary amino styrene resin B of 3:1; the nanofilter (13) uses a polyvinylidene fluoride (PVDF) membrane with a pore size of 30nm and a uniformity coefficient of 1.1; the separator (9) uses a bulkhead tower A type, with a two-side area ratio of 5:5, a tower top pressure of 5kPa, a tower top temperature of 41.2°C, a theoretical plate number of 20, and a reflux ratio of 2; the crystallizer (15) uses a first-stage falling film crystallization, and the crystallization temperature is 95°C. A high-purity resorcinol product higher than the SEMI C12 (G4) standard is obtained, and the product indicators are shown in Table 3.

[0048] Example 4

[0049] like Figure 5As shown, the production device of electronic chemical resorcinol of the present invention comprises a stirring and heating mixer, a microfilter, an anion and cation remover, a nanofilter, a crystallizer and a dryer which are connected in series from feeding to discharging.

[0050] Resorcinol and solvent acetone enter the stirring and mixing heater (3) at a molar ratio of 0.45, are heated to 45°C and then enter the microfilter, which uses a polyimide membrane with a pore size of 0.1μm and a uniformity coefficient of 1.4; the ion exchange resin uses a mixed resin with a particle size of 0.6mm, a uniformity coefficient of 1.08, and a volume ratio of 3:1 between perfluorosulfonic acid and quaternary aminostyrene; the nanofilter (13) uses a polyvinylidene fluoride (PVDF) membrane with a pore size of 10nm and a uniformity coefficient of 1.25; the crystallizer (15) uses a three-stage crystallization, which is a suspended stirring crystallizer and a two-stage falling film crystallizer, and the crystallization temperatures are 15°C, 85°C, and 103°C respectively; the drying conditions are 110°C, 80kPa, and 1h. A high-purity resorcinol product higher than the SEMI C12 (G4) standard is obtained, and the product indicators are shown in Table 3.

[0051] Example 5

[0052] like Figure 6 As shown, the production device of electronic chemical resorcinol of the present invention comprises a stirring and heating mixer, an anion and cation remover, a nanofilter, a flash tank, a crystallizer and a dryer which are connected in series from feeding to discharging.

[0053] Resorcinol and solvent methyl acetate enter the stirring and mixing heater (3) at a molar ratio of 0.40, are heated to 45°C and then enter the ion exchange resin; the ion exchange resin uses a mixed resin with a particle size of 0.5 mm, a uniformity coefficient of 1.2, and a volume ratio of 3:2 of phosphate styrene and quaternary amino styrene; the nanofilter uses a polyamide membrane with a pore size of 50 nm and a uniformity coefficient of 1.06; the separator (9) uses a flash tank with a pressure of 400 kPa and a temperature of 139.5°C; the crystallizer (15) uses a first-stage falling film crystallization with a crystallization temperature of 102°C; the drying conditions are 120°C, 90 kPa, and 45 minutes. A high-purity resorcinol product higher than the SEMI C12 (G4) standard is obtained, and the product indicators are shown in Table 3.

[0054] Example 6

[0055] like Figure 7 As shown, the production device of electronic chemical resorcinol of the present invention comprises a stirring and heating mixer, an anion and cation remover, a flash tank, a nanofilter, a crystallizer and a dryer which are connected in series from feeding to discharging.

[0056] Resorcinol and solvent ethyl acetate enter the stirring and mixing heater (3) at a molar ratio of 0.55, are heated to 60°C and then enter the ion exchange resin; the ion exchange resin uses a mixed resin with a particle size of 0.4mm, a uniformity coefficient of 1.3, and a volume ratio of 3:2 of perfluorosulfonic acid resin A and quaternary aminostyrene resin B; the separator (9) uses a flash tank with a pressure of 50kPa and a temperature of 89°C; the nanofilter uses a polytetrafluoroethylene membrane with a pore size of 50nm and a uniformity coefficient of 1.07; the crystallizer (15) uses a single-stage plate crystallization with a crystallization temperature of 100°C; the drying conditions are 80°C, 50kPa, and 2h. A high-purity resorcinol product higher than the SEMI C12 (G4) standard is obtained, and the product indicators are shown in Table 3.

[0057] Comparative Example 1

[0058] The raw materials and process are the same as in Example 3. Figure 4 , the difference from Example 3 is that the particle size uniformity coefficient of the ion exchange resin used in the ion exchange remover is changed to 1.45. The product indicators are shown in Table 4. Sodium, iron and potassium cannot meet the requirements of SEMI C12 (G4); sodium, iron, potassium, magnesium, copper, zinc, lead, arsenic, calcium, silver and silicon cannot meet the requirements of SEMI C12 (G5).

[0059] Comparative Example 2

[0060] The raw materials and process are the same as those in Example 3. Figure 4 , the difference from Example 3 is that the particle size of the ion exchange resin used in the ion exchange remover is changed to 0.75 mm. The product indicators are shown in Table 4. Sodium, iron, copper, calcium, potassium and silicon cannot meet the requirements of SEMIC12 (G4); sodium, iron, copper, calcium, potassium, silicon, magnesium, manganese, zinc, lead, arsenic, aluminum, silver and cobalt cannot meet the requirements of G5.

[0061] Comparative Example 3

[0062] The raw materials and process are the same as those in Example 7. Figure 8 , which is different from Example 7 in that the nanofilter pore size uniformity coefficient is changed to 1.55, and the others are the same. Product indicators are shown in Table 4. The particles cannot meet SEMI C12 (G4) and SEMI C12 (G5).

[0063] Comparative Example 4

[0064] The raw materials and process are the same as those in Example 7. Figure 8 , which is different from Example 7 in that the pore size of the nanofilter is changed to 100 nm, and the others are the same. Product specifications are shown in Table 4. The particles cannot meet the requirements of SEMI C12 (G4) and SEMI C12 (G5).

[0065] Comparative Example 5

[0066] The feed and operating conditions of this comparative example are exactly the same as those of Example 6. Figure 7 , which is different from Example 6 in that the crystallizer is changed from three-stage to two-stage, and the product indicators are shown in Table 4. The product purity cannot meet the SEMI C12 (G4) requirements.

[0067] Comparative Example 6

[0068] The preparation process of electronic chemical resorcinol is as follows: industrial-grade resorcinol enters a melt crystallizer, and the discharge end pipe of the industrial-grade resorcinol feed pipeline is connected to the feed end of the melt crystallizer; a melt crystallization residual liquid tank and a melt crystallization finished product tank, and the feed end pipes of the melt crystallization residual liquid tank and the melt crystallization finished product tank are connected to the discharge end of the melt crystallizer; a resorcinol quartz distillation tower, the feed end of the resorcinol quartz distillation tower is connected to the discharge end pipe of the melt crystallization residual liquid tank, and the discharge end is connected to the feed end pipe of the melt crystallizer, and a resorcinol tower top condenser is arranged on the resorcinol quartz distillation tower; an ion exchange column, an ion exchange resin layer is provided in the ion exchange column, the feed end of the ion exchange column is connected to the discharge end pipe of the melt crystallization finished product tank, and the waste liquid discharge end of the ion exchange column is connected to the feed end pipe of the resorcinol quartz distillation tower; an industrial-grade resorcinol discharge pipeline, and the feed end of the industrial-grade resorcinol discharge pipeline is connected to the discharge end pipe of the ion exchange column. The product indicators are shown in Table 4. The particles cannot meet the requirements of SEMI C12 (G4) and SEMI C12 (G5).

[0069] Test Example 1

[0070] The content of the components in the electronic chemical resorcinol of Examples 1-8 and Comparative Examples 1-5 was detected by using the following instruments: PerkinElmer ICP-OES / Avio550MAX for raw material cations, Agilent ICP-MS / MS8900 for product cations, Swiss Metrohm 940 ion chromatograph for raw material and product anions, 851 Coulometric Karl Fischer water analyzer for raw material and product water content, Agilent GC-MS gas chromatograph for raw material and product organic impurities, and RION-KS-42AF for particle size analyzer. The results are shown in Tables 1-4, and the raw materials in Table 1 refer to industrial grade resorcinol.

[0071] Table 1 Industrial resorcinol raw material indicators

[0072]

[0073] Table 2 Product indicators obtained by the production method and production device of Example 1-2 of the present invention

[0074]

[0075]

[0076] Table 3 Product indicators obtained by the production method and production device of Examples 3-6 of the present invention

[0077]

[0078]

[0079] Table 4 Comparative Examples 1-5 Obtained Product Index

[0080]

[0081]

[0082] Table 5 Contents of metal impurities and non-metal impurities in the electronic chemical resorcinol

[0083]

[0084] Although the present invention has been described in detail above by general description, specific implementation methods and experiments, it is obvious to those skilled in the art that some modifications or improvements can be made to the present invention. Therefore, these modifications or improvements made without departing from the spirit of the present invention all belong to the scope of protection claimed by the present invention.

Claims

1. A method for producing electronic chemical resorcinol, comprising a dissolving step, a microfiltration step, an anion and cation removal step, a nanofiltration step, a flash separation step or a distillation separation step, a crystallization step and a drying step, characterized in that: The production method comprises any of the following steps: The first step sequentially includes a dissolution step, a microfiltration step, an anion and cation removal step, a flash separation step, a nanofiltration step, a crystallization step and a drying step; The second process sequentially includes a dissolution step, a microfiltration step, an anion and cation removal step, a rectification and separation step, a nanofiltration step, and a crystallization step; The third process sequentially includes a dissolution step, a microfiltration step, an anion and cation removal step, a nanofilter, a rectification and separation step, and a crystallization step; The fourth step sequentially includes a dissolution step, a microfiltration step, an anion and cation removal step, a nanofiltration step, a crystallization step and a drying step; The fifth step sequentially includes a dissolution step, anion and cation removal step, a nanofiltration step, a flash evaporation step, a crystallization step and a drying step; The sixth step sequentially includes a dissolution step, anion and cation removal step, a flash separation step, a nanofiltration step, a crystallization step and a drying step; The dissolving step is to dissolve industrial-grade resorcinol with a reagent to obtain a resorcinol solution, wherein the reagent is selected from one or more of water and ethanol; The flash separation step is to separate the components of the resorcinol solution through a flash tank, and the pressure of the flash separation step is 100 kPa and the temperature is 119° C.; The distillation separation step is that the resorcinol solution is separated into components by passing through a first distillation tower and a second distillation tower, wherein the first distillation tower has a top pressure of 25 kPa, a top temperature of 70.8°C, a theoretical plate number of 12, and a reflux ratio of 1.5, and the second distillation tower has a top pressure of 2 kPa, a top temperature of 163°C, a theoretical plate number of 10, and a reflux ratio of 1.5; The crystallization step is to crystallize the resorcinol solution through a crystallizer, the crystallizer adopts one or more of first-stage falling film crystallization and second-stage crystallization, the second-stage crystallization is plate crystallization and falling film crystallization in sequence, and the temperature of the crystallization step is 96-104° C.; The drying step is to dry the resorcinol product after the crystallization step at a temperature of 90° C., a pressure of 70 kPa, and a time of 2 hours; The method further comprises a heating step of heating the resorcinol solution after the dissolving step to 72-85°C.

2. The production method according to claim 1, characterized in that The microfiltration steps of the first, second, third and fourth steps remove particles with a particle size of 0.2 μm or more, and the microfiltration membrane used is selected from one of polytetrafluoroethylene membrane, polyethersulfone membrane, polyvinylidene fluoride membrane, polyimide membrane and polyamide membrane with a pore size of 0.1-0.5 μm, and the pore size uniformity coefficient is 1.1-1.4; The anion and cation removal step of each process is to remove anions and cations in the resorcinol solution by using an ion exchange resin and / or ion exchange fiber with a particle size of 0.3-0.6 mm, wherein the ion exchange resin and / or ion exchange fiber is one or more of sulfonic acid styrene resin or fiber, carboxyl styrene resin or fiber, quaternary amino styrene resin or fiber, perfluorosulfonic acid resin or fiber, sulfonated polyethersulfone resin or fiber, and the pore size uniformity coefficient is 1.08-1.3; The nanofiltration step of the first and sixth processes is to use a nanofilter to remove particles with a particle size of 10 nm or more, and the nanofilter membrane is selected from one of polytetrafluoroethylene membrane, polyethersulfone membrane, polyvinylidene fluoride membrane, polyimide membrane or polyamide membrane with a pore size of 10-50 nm, and the pore size uniformity coefficient is 1.06-1.

4.

3. The production method according to claim 2, characterized in that: The microfilter of the first process uses a polytetrafluoroethylene membrane with a pore size of 0.2 μm and a uniformity coefficient of 1.25, and the microfilter of the second process uses a polyimide membrane with a pore size of 0.4 μm and a uniformity coefficient of 1.15; The ion exchange resin in each step is a mixed resin with a particle size of 0.6 mm, a uniformity coefficient of 1.1, and a volume ratio of sulfonic acid styrene resin to quaternary amino styrene of 2:1, or a mixed resin with a particle size of 0.3 mm, a uniformity coefficient of 1.3, and a volume ratio of perfluorosulfonic acid to quaternary amino styrene of 3:2; The nanofilter in the first step uses a polytetrafluoroethylene membrane with a pore size of 20 nm and a uniformity coefficient of 1.2, and the nanofilter in the second step uses a polyimide membrane with a pore size of 10 nm and a uniformity coefficient of 1.

25.

4. The production method according to claim 3, characterized in that: The contents of various impurities in the electronic chemical resorcinol are shown in the following table:

5. The production method according to claim 1, characterized in that: The contents of various impurities in the industrial grade resorcinol are shown in the following table:

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