CN113526470A - Continuous preparation method of ultra-clean high-purity hydrogen peroxide - Google Patents
Continuous preparation method of ultra-clean high-purity hydrogen peroxide Download PDFInfo
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- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 title claims abstract description 271
- 238000002360 preparation method Methods 0.000 title claims abstract description 49
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 120
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 claims abstract description 80
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical group C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000000178 monomer Substances 0.000 claims abstract description 40
- 239000003960 organic solvent Substances 0.000 claims abstract description 40
- 238000000746 purification Methods 0.000 claims abstract description 29
- 238000005086 pumping Methods 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 25
- 239000000945 filler Substances 0.000 claims abstract description 23
- 238000001914 filtration Methods 0.000 claims abstract description 22
- 239000011347 resin Substances 0.000 claims abstract description 19
- 229920005989 resin Polymers 0.000 claims abstract description 19
- 238000001704 evaporation Methods 0.000 claims abstract description 17
- 239000003463 adsorbent Substances 0.000 claims abstract description 14
- 238000005349 anion exchange Methods 0.000 claims abstract description 9
- 238000005341 cation exchange Methods 0.000 claims abstract description 9
- 238000007334 copolymerization reaction Methods 0.000 claims abstract description 9
- 230000008020 evaporation Effects 0.000 claims abstract description 9
- 239000012766 organic filler Substances 0.000 claims abstract description 9
- 239000000725 suspension Substances 0.000 claims abstract description 9
- 239000002826 coolant Substances 0.000 claims description 38
- 239000003381 stabilizer Substances 0.000 claims description 38
- 238000002156 mixing Methods 0.000 claims description 30
- 230000000274 adsorptive effect Effects 0.000 claims description 29
- 238000011403 purification operation Methods 0.000 claims description 20
- 239000007788 liquid Substances 0.000 claims description 18
- 239000011159 matrix material Substances 0.000 claims description 16
- 238000001223 reverse osmosis Methods 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 16
- 239000012530 fluid Substances 0.000 claims description 14
- 238000001179 sorption measurement Methods 0.000 claims description 14
- 238000003860 storage Methods 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 12
- 238000005374 membrane filtration Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims description 7
- 239000001257 hydrogen Substances 0.000 claims description 7
- 238000004821 distillation Methods 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- 238000010924 continuous production Methods 0.000 claims 7
- 230000000694 effects Effects 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 description 11
- 239000012466 permeate Substances 0.000 description 7
- 238000009826 distribution Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000012840 feeding operation Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
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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
- C01B15/00—Peroxides; Peroxyhydrates; Peroxyacids or salts thereof; Superoxides; Ozonides
- C01B15/01—Hydrogen peroxide
- C01B15/013—Separation; Purification; Concentration
- C01B15/0135—Purification by solid ion-exchangers or solid chelating agents
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B15/00—Peroxides; Peroxyhydrates; Peroxyacids or salts thereof; Superoxides; Ozonides
- C01B15/01—Hydrogen peroxide
- C01B15/013—Separation; Purification; Concentration
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses a continuous preparation method of ultra-clean high-purity hydrogen peroxide, which comprises the following operation steps: selecting a certain amount of industrial-grade hydrogen peroxide, selecting a certain amount of styrene monomer, divinylbenzene monomer, toluene organic solvent and filler, preparing the styrene monomer, the divinylbenzene monomer, the toluene organic solvent and the filler into a porous resin adsorbent body by a suspension copolymerization method, enabling the industrial-grade hydrogen peroxide to sequentially pass through the porous resin adsorbent body, a cation exchange column and an anion exchange column at a flow rate of 280-460L/H, and then performing circulating filtration by using a 0.1 micron filter element to obtain primary purified hydrogen peroxide. The continuous preparation method of the ultra-clean high-purity hydrogen peroxide can be used for feeding in a pumping mode, is convenient to control the feeding amount, can be used for continuous preparation operation, improves the preparation efficiency, improves the purity of hydrogen dioxide by performing constant-temperature evaporation and purification treatment under the low-temperature condition, and has more excellent use effect.
Description
Technical Field
The invention relates to the field of hydrogen peroxide preparation, and particularly relates to a continuous preparation method of ultra-clean high-purity hydrogen peroxide.
Background
The continuous preparation method of the ultra-clean high-purity hydrogen peroxide is a method for continuously preparing the hydrogen peroxide, and can use a hydrogen peroxide solution when medical disinfection is carried out, the hydrogen peroxide solution is widely applied to military, chemical engineering and medical treatment, impurities need to be decomposed when the hydrogen peroxide solution is prepared, the purity of the hydrogen peroxide solution is improved, and along with the continuous development of science and technology, the requirements of people on the manufacturing process of the continuous preparation method of the ultra-clean high-purity hydrogen peroxide are higher and higher.
In the prior art, patent with publication number CN201811216055.0 discloses an electrochemical device for preparing hydrogen peroxide and its application, the device is composed of a cathode chamber, an anode chamber, a cathode and an anode; the side part of the cathode chamber is communicated with the side part of the anode chamber; an air distribution chamber is arranged in the cathode chamber below the cathode, and the top surface of the air distribution chamber is a porous plate; the bottom surface of the cathode is arranged towards the central line of the top surface of the gas distribution chamber; the cathode is made of graphene-doped carbon foam or carbon nitride-doped carbon foam, and the existing continuous preparation method of the ultra-clean high-purity hydrogen peroxide has certain defects in use.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a continuous preparation method of ultra-clean high-purity hydrogen peroxide, which can be used for feeding operation in a pumping mode, is convenient to control the feeding amount, can be used for continuous preparation operation, improves the preparation efficiency, improves the purity of hydrogen dioxide by carrying out constant-temperature evaporation and purification treatment under the low-temperature condition, has more excellent use effect and can effectively solve the problems in the background technology.
(II) technical scheme
In order to achieve the purpose, the invention adopts the technical scheme that: a continuous preparation method of ultra-clean high-purity hydrogen peroxide comprises the following operation steps:
s1: preparation of materials: selecting a certain amount of industrial-grade hydrogen peroxide which is an oxide of another hydrogen except water, has strong oxidizability and weak acidity, selecting a certain amount of styrene monomer, divinylbenzene monomer, toluene organic solvent and filler, and preparing the styrene monomer, the divinylbenzene monomer, the toluene organic solvent and the filler into a porous resin adsorbent body by a suspension copolymerization method;
s2: preparation of a hydrogen peroxide purification solution: preparing hydrogen peroxide purification solution, including back-penetrating fluid, cooling agent, environment-friendly stabilizer, distilled solution and adsorptive solution, using the back-penetrating fluid as matrix, mixing and stirring the cooling agent, environment-friendly stabilizer, distilled solution and adsorptive solution;
s3: purifying industrial grade hydrogen peroxide: enabling industrial-grade hydrogen peroxide to sequentially pass through a porous resin adsorption material body, a cation exchange column and an anion exchange column at a flow rate of 280-460L/H, and then performing circulating filtration by using a 0.1-micron filter element to obtain primary purified hydrogen peroxide;
s4: mixing and filtering: continuously pumping the primary purified industrial-grade hydrogen peroxide, namely secondary industrial-grade hydrogen peroxide, into a specified container, adding a divinylbenzene monomer, a styrene monomer and a toluene organic solvent, mixing, performing filtration at low temperature by adopting a membrane filtration method, and generating a hydrogen oxide solution with high purity;
s5: and (3) distillation and purification: introducing a hydrogen peroxide solution with high purity into a specified container, adding a hydrogen peroxide purification solution prepared by mixing and stirring a reverse osmosis liquid serving as a matrix, a cooling agent, an environment-friendly stabilizer, a distilled solution and an adsorptive solution, continuously pumping, distilling under a low-temperature condition and evaporating at a constant temperature, and performing purification operation;
s6: preparation and storage: and after the purification operation is finished, continuously pumping the purified high-purity hydrogen peroxide solution into a solution storage, performing concentration operation, further performing purification operation, and finishing the preparation of the ultra-clean high-purity hydrogen peroxide.
As a preferred technical solution, the step S1 includes the following raw materials: the industrial-grade hydrogen peroxide accounts for 36-48%, the styrene monomer accounts for 14-25%, the divinylbenzene monomer accounts for 10-19%, the toluene organic solvent accounts for 10-18%, and the filler accounts for 6-18%.
As a preferred technical solution, the content of the technical grade hydrogen peroxide is 42%, the content of the styrene monomer is 18%, the content of the divinylbenzene monomer is 15%, the content of the toluene organic solvent is 15%, and the content of the filler is 10%.
As a preferred technical solution, the content of the technical grade hydrogen peroxide is 44%, the content of the styrene monomer is 16%, the content of the divinylbenzene monomer is 17%, the content of the toluene organic solvent is 14%, and the content of the filler is 9%.
As a preferable technical scheme, the portion of the reverse osmosis liquid is 38-51%, the portion of the cooling agent is 10-16%, the portion of the environmental protection stabilizer is 12-22%, the portion of the distilled solution is 10-18%, and the portion of the adsorption solution is 8-16%.
As a preferred technical solution, the portion of the anti-permeate liquid is 44%, the portion of the coolant is 16%, the portion of the environmental protection stabilizer is 15%, the portion of the distilled solution is 14%, and the portion of the adsorptive solution is 11%.
As a preferred technical solution, the portion of the anti-permeate liquid is 46%, the portion of the coolant is 14%, the portion of the environmental protection stabilizer is 17%, the portion of the distilled solution is 13%, and the portion of the adsorptive solution is 10%.
As a preferable technical scheme, the step S5 is implemented with constant temperature evaporation operation under the temperature condition of 2-15 ℃ for 15-25 min.
(III) advantageous effects
Compared with the prior art, the invention provides a continuous preparation method of ultra-clean high-purity hydrogen peroxide, which has the following beneficial effects: the continuous preparation method of the ultra-clean high-purity hydrogen peroxide can be used for feeding operation in a pumping mode, is convenient to control the feeding amount, can be used for continuous preparation operation, improves the preparation efficiency, can be used for constant-temperature evaporation purification treatment under the low-temperature condition, improves the purity of hydrogen dioxide, has more excellent using effect, selects a certain amount of industrial grade hydrogen peroxide, selects another hydrogen oxide except water, has strong oxidability and weak acidity, selects a certain amount of styrene monomer, divinylbenzene monomer, toluene organic solvent and filler, prepares the styrene monomer, the divinylbenzene monomer, the toluene organic solvent and the filler into a porous resin adsorbent body by a suspension copolymerization method, prepares a hydrogen peroxide purification solution, and comprises a reverse osmosis liquid, a cooling agent, an environment-friendly stabilizer, a distilled solution and an adsorptive solution, mixing and stirring a reverse osmosis liquid serving as a matrix, a cooling agent, an environment-friendly stabilizer, a distilled solution and an adsorptive solution, enabling industrial-grade hydrogen peroxide to sequentially pass through a porous resin adsorption body, a cation exchange column and an anion exchange column at a flow rate of 280-460L/H, circularly filtering by using a 0.1 micron filter element to obtain primary purified hydrogen peroxide, continuously pumping the primary purified industrial-grade hydrogen peroxide, namely secondary industrial-grade hydrogen peroxide into a specified container, adding a divinylbenzene monomer, a styrene monomer and a toluene organic solvent for mixing, filtering under a low temperature condition by adopting a membrane filtration method to generate a hydrogen oxide solution with higher purity, introducing the hydrogen peroxide solution with higher purity into the specified container, adding the hydrogen peroxide purified solution prepared by mixing and stirring the cooling agent, the environment-friendly stabilizer, the distilled solution and the adsorptive solution by taking the reverse osmosis liquid as the matrix, continuous pumping, distilling and constant-temperature evaporating under the low-temperature condition, purifying, continuously pumping the purified high-purity hydrogen peroxide solution into a solution storage device after the purification operation is finished, concentrating, further purifying, and preparing the ultra-clean high-purity hydrogen peroxide.
Detailed Description
The first embodiment is as follows:
a continuous preparation method of ultra-clean high-purity hydrogen peroxide comprises the following operation steps:
s1: preparation of materials: selecting a certain amount of industrial-grade hydrogen peroxide which is an oxide of another hydrogen except water, has strong oxidizability and weak acidity, selecting a certain amount of styrene monomer, divinylbenzene monomer, toluene organic solvent and filler, and preparing the styrene monomer, the divinylbenzene monomer, the toluene organic solvent and the filler into a porous resin adsorbent body by a suspension copolymerization method;
s2: preparation of a hydrogen peroxide purification solution: preparing hydrogen peroxide purification solution, including back-penetrating fluid, cooling agent, environment-friendly stabilizer, distilled solution and adsorptive solution, using the back-penetrating fluid as matrix, mixing and stirring the cooling agent, environment-friendly stabilizer, distilled solution and adsorptive solution;
s3: purifying industrial grade hydrogen peroxide: enabling industrial-grade hydrogen peroxide to sequentially pass through a porous resin adsorption material body, a cation exchange column and an anion exchange column at a flow rate of 280-460L/H, and then performing circulating filtration by using a 0.1-micron filter element to obtain primary purified hydrogen peroxide;
s4: mixing and filtering: continuously pumping the primary purified industrial-grade hydrogen peroxide, namely secondary industrial-grade hydrogen peroxide, into a specified container, adding a divinylbenzene monomer, a styrene monomer and a toluene organic solvent, mixing, performing filtration at low temperature by adopting a membrane filtration method, and generating a hydrogen oxide solution with high purity;
s5: and (3) distillation and purification: introducing a hydrogen peroxide solution with high purity into a specified container, adding a hydrogen peroxide purification solution prepared by mixing and stirring a reverse osmosis liquid serving as a matrix, a cooling agent, an environment-friendly stabilizer, a distilled solution and an adsorptive solution, continuously pumping, distilling under a low-temperature condition and evaporating at a constant temperature, and performing purification operation;
s6: preparation and storage: and after the purification operation is finished, continuously pumping the purified high-purity hydrogen peroxide solution into a solution storage, performing concentration operation, further performing purification operation, and finishing the preparation of the ultra-clean high-purity hydrogen peroxide.
The step S1 includes the following portions of raw materials: the content of industrial grade hydrogen peroxide is 36-48%, the content of styrene monomer is 14-25%, the content of divinylbenzene monomer is 10-19%, the content of toluene organic solvent is 10-18%, and the content of filler is 6-18%.
The content of technical grade hydrogen peroxide is 44%, the content of styrene monomer is 16%, the content of divinylbenzene monomer is 17%, the content of toluene organic solvent is 14%, and the content of filler is 9%.
The portion of the reverse osmosis liquid is 38-51%, the portion of the coolant is 10-16%, the portion of the environmental protection stabilizer is 12-22%, the portion of the distilled solution is 10-18%, and the portion of the adsorptive solution is 8-16%.
The proportion of the anti-permeate is 46%, the proportion of the coolant is 14%, the proportion of the environmental protection stabilizer is 17%, the proportion of the distilled solution is 13%, and the proportion of the adsorption solution is 10%.
In the step S5, constant temperature evaporation operation is carried out at the temperature of 4 ℃ for 15 min.
Example two:
on the basis of the first embodiment, the continuous preparation method of the ultra-clean high-purity hydrogen peroxide comprises the following operation steps:
s1: preparation of materials: selecting a certain amount of industrial-grade hydrogen peroxide which is an oxide of another hydrogen except water, has strong oxidizability and weak acidity, selecting a certain amount of styrene monomer, divinylbenzene monomer, toluene organic solvent and filler, and preparing the styrene monomer, the divinylbenzene monomer, the toluene organic solvent and the filler into a porous resin adsorbent body by a suspension copolymerization method;
s2: preparation of a hydrogen peroxide purification solution: preparing hydrogen peroxide purification solution, including back-penetrating fluid, cooling agent, environment-friendly stabilizer, distilled solution and adsorptive solution, using the back-penetrating fluid as matrix, mixing and stirring the cooling agent, environment-friendly stabilizer, distilled solution and adsorptive solution;
s3: purifying industrial grade hydrogen peroxide: enabling industrial-grade hydrogen peroxide to sequentially pass through a porous resin adsorption material body, a cation exchange column and an anion exchange column at a flow rate of 280-460L/H, and then performing circulating filtration by using a 0.1-micron filter element to obtain primary purified hydrogen peroxide;
s4: mixing and filtering: continuously pumping the primary purified industrial-grade hydrogen peroxide, namely secondary industrial-grade hydrogen peroxide, into a specified container, adding a divinylbenzene monomer, a styrene monomer and a toluene organic solvent, mixing, performing filtration at low temperature by adopting a membrane filtration method, and generating a hydrogen oxide solution with high purity;
s5: and (3) distillation and purification: introducing a hydrogen peroxide solution with high purity into a specified container, adding a hydrogen peroxide purification solution prepared by mixing and stirring a reverse osmosis liquid serving as a matrix, a cooling agent, an environment-friendly stabilizer, a distilled solution and an adsorptive solution, continuously pumping, distilling under a low-temperature condition and evaporating at a constant temperature, and performing purification operation;
s6: preparation and storage: and after the purification operation is finished, continuously pumping the purified high-purity hydrogen peroxide solution into a solution storage, performing concentration operation, further performing purification operation, and finishing the preparation of the ultra-clean high-purity hydrogen peroxide.
The step S1 includes the following portions of raw materials: the content of industrial grade hydrogen peroxide is 36-48%, the content of styrene monomer is 14-25%, the content of divinylbenzene monomer is 10-19%, the content of toluene organic solvent is 10-18%, and the content of filler is 6-18%.
The content of industrial-grade hydrogen peroxide is 42%, the content of styrene monomer is 18%, the content of divinylbenzene monomer is 15%, the content of toluene organic solvent is 15%, and the content of filler is 10%.
The portion of the reverse osmosis liquid is 38-51%, the portion of the coolant is 10-16%, the portion of the environmental protection stabilizer is 12-22%, the portion of the distilled solution is 10-18%, and the portion of the adsorptive solution is 8-16%.
The proportion of the anti-permeate is 44%, the proportion of the coolant is 16%, the proportion of the environmental protection stabilizer is 15%, the proportion of the distilled solution is 14%, and the proportion of the adsorption solution is 11%.
In the step S5, constant temperature evaporation operation is carried out at the temperature of 6 ℃ for 18 min.
Example three:
on the basis of the second embodiment, the continuous preparation method of the ultra-clean high-purity hydrogen peroxide comprises the following operation steps:
s1: preparation of materials: selecting a certain amount of industrial-grade hydrogen peroxide which is an oxide of another hydrogen except water, has strong oxidizability and weak acidity, selecting a certain amount of styrene monomer, divinylbenzene monomer, toluene organic solvent and filler, and preparing the styrene monomer, the divinylbenzene monomer, the toluene organic solvent and the filler into a porous resin adsorbent body by a suspension copolymerization method;
s2: preparation of a hydrogen peroxide purification solution: preparing hydrogen peroxide purification solution, including back-penetrating fluid, cooling agent, environment-friendly stabilizer, distilled solution and adsorptive solution, using the back-penetrating fluid as matrix, mixing and stirring the cooling agent, environment-friendly stabilizer, distilled solution and adsorptive solution;
s3: purifying industrial grade hydrogen peroxide: enabling industrial-grade hydrogen peroxide to sequentially pass through a porous resin adsorption material body, a cation exchange column and an anion exchange column at a flow rate of 280-460L/H, and then performing circulating filtration by using a 0.1-micron filter element to obtain primary purified hydrogen peroxide;
s4: mixing and filtering: continuously pumping the primary purified industrial-grade hydrogen peroxide, namely secondary industrial-grade hydrogen peroxide, into a specified container, adding a divinylbenzene monomer, a styrene monomer and a toluene organic solvent, mixing, performing filtration at low temperature by adopting a membrane filtration method, and generating a hydrogen oxide solution with high purity;
s5: and (3) distillation and purification: introducing a hydrogen peroxide solution with high purity into a specified container, adding a hydrogen peroxide purification solution prepared by mixing and stirring a reverse osmosis liquid serving as a matrix, a cooling agent, an environment-friendly stabilizer, a distilled solution and an adsorptive solution, continuously pumping, distilling under a low-temperature condition and evaporating at a constant temperature, and performing purification operation;
s6: preparation and storage: and after the purification operation is finished, continuously pumping the purified high-purity hydrogen peroxide solution into a solution storage, performing concentration operation, further performing purification operation, and finishing the preparation of the ultra-clean high-purity hydrogen peroxide.
The step S1 includes the following portions of raw materials: the content of industrial grade hydrogen peroxide is 36-48%, the content of styrene monomer is 14-25%, the content of divinylbenzene monomer is 10-19%, the content of toluene organic solvent is 10-18%, and the content of filler is 6-18%.
The content of technical grade hydrogen peroxide is 44%, the content of styrene monomer is 16%, the content of divinylbenzene monomer is 17%, the content of toluene organic solvent is 14%, and the content of filler is 9%.
The portion of the reverse osmosis liquid is 38-51%, the portion of the coolant is 10-16%, the portion of the environmental protection stabilizer is 12-22%, the portion of the distilled solution is 10-18%, and the portion of the adsorptive solution is 8-16%.
The proportion of the anti-permeate is 44%, the proportion of the coolant is 16%, the proportion of the environmental protection stabilizer is 15%, the proportion of the distilled solution is 14%, and the proportion of the adsorption solution is 11%.
In the step S5, constant temperature evaporation operation is carried out at the temperature of 8 ℃ for 20 min.
Example four:
on the basis of the third embodiment, the continuous preparation method of the ultra-clean high-purity hydrogen peroxide comprises the following operation steps:
s1: preparation of materials: selecting a certain amount of industrial-grade hydrogen peroxide which is an oxide of another hydrogen except water, has strong oxidizability and weak acidity, selecting a certain amount of styrene monomer, divinylbenzene monomer, toluene organic solvent and filler, and preparing the styrene monomer, the divinylbenzene monomer, the toluene organic solvent and the filler into a porous resin adsorbent body by a suspension copolymerization method;
s2: preparation of a hydrogen peroxide purification solution: preparing hydrogen peroxide purification solution, including back-penetrating fluid, cooling agent, environment-friendly stabilizer, distilled solution and adsorptive solution, using the back-penetrating fluid as matrix, mixing and stirring the cooling agent, environment-friendly stabilizer, distilled solution and adsorptive solution;
s3: purifying industrial grade hydrogen peroxide: enabling industrial-grade hydrogen peroxide to sequentially pass through a porous resin adsorption material body, a cation exchange column and an anion exchange column at a flow rate of 280-460L/H, and then performing circulating filtration by using a 0.1-micron filter element to obtain primary purified hydrogen peroxide;
s4: mixing and filtering: continuously pumping the primary purified industrial-grade hydrogen peroxide, namely secondary industrial-grade hydrogen peroxide, into a specified container, adding a divinylbenzene monomer, a styrene monomer and a toluene organic solvent, mixing, performing filtration at low temperature by adopting a membrane filtration method, and generating a hydrogen oxide solution with high purity;
s5: and (3) distillation and purification: introducing a hydrogen peroxide solution with high purity into a specified container, adding a hydrogen peroxide purification solution prepared by mixing and stirring a reverse osmosis liquid serving as a matrix, a cooling agent, an environment-friendly stabilizer, a distilled solution and an adsorptive solution, continuously pumping, distilling under a low-temperature condition and evaporating at a constant temperature, and performing purification operation;
s6: preparation and storage: and after the purification operation is finished, continuously pumping the purified high-purity hydrogen peroxide solution into a solution storage, performing concentration operation, further performing purification operation, and finishing the preparation of the ultra-clean high-purity hydrogen peroxide.
The step S1 includes the following portions of raw materials: the content of industrial grade hydrogen peroxide is 36-48%, the content of styrene monomer is 14-25%, the content of divinylbenzene monomer is 10-19%, the content of toluene organic solvent is 10-18%, and the content of filler is 6-18%.
The content of industrial-grade hydrogen peroxide is 42%, the content of styrene monomer is 18%, the content of divinylbenzene monomer is 15%, the content of toluene organic solvent is 15%, and the content of filler is 10%.
The portion of the reverse osmosis liquid is 38-51%, the portion of the coolant is 10-16%, the portion of the environmental protection stabilizer is 12-22%, the portion of the distilled solution is 10-18%, and the portion of the adsorptive solution is 8-16%.
The proportion of the anti-permeate is 46%, the proportion of the coolant is 14%, the proportion of the environmental protection stabilizer is 17%, the proportion of the distilled solution is 13%, and the proportion of the adsorption solution is 10%.
In the step S5, constant temperature evaporation operation is carried out at the temperature of 12 ℃ for 24 min.
The working principle is as follows: selecting a certain amount of industrial-grade hydrogen peroxide which is an oxide of another hydrogen except water and has strong oxidizability and weak acidity, selecting a certain amount of styrene monomer, divinylbenzene monomer, toluene organic solvent and filler, preparing the styrene monomer, the divinylbenzene monomer, the toluene organic solvent and the filler into a porous resin adsorbent body by a suspension copolymerization method, preparing a hydrogen peroxide purification solution by mixing and stirring the porous resin adsorbent body, the coolant, the environment-friendly stabilizer, the distilled solution and the adsorbent solution, taking the permeate as a matrix, the coolant, the environment-friendly stabilizer, the distilled solution and the adsorbent solution, and enabling the industrial-grade hydrogen peroxide to sequentially pass through the porous resin adsorbent body, the cation exchange column and the anion exchange column at a flow rate of 280-460L/H and then to be circularly filtered by a 0.1 micron filter element, obtaining primary purified hydrogen peroxide, continuously pumping the primary purified industrial grade hydrogen peroxide, namely secondary industrial grade hydrogen peroxide, into a specified container, adding divinylbenzene monomer, styrene monomer and toluene organic solvent for mixing, filtering at low temperature by membrane filtration method to obtain hydrogen peroxide solution with high purity, introducing the hydrogen peroxide solution into a designated container, adding purified hydrogen peroxide solution prepared by mixing and stirring anti-penetrating fluid as matrix, coolant, environment-friendly stabilizer, distilled solution and adsorptive solution, continuously pumping, distilling and evaporating at constant temperature at low temperature, purifying, continuously pumping the purified high-purity hydrogen peroxide solution into a solution storage, and (5) performing concentration operation, and further performing purification operation to complete the preparation of the ultra-clean high-purity hydrogen peroxide.
It is noted that, herein, relational terms such as first and second (a, b, etc.) and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed.
Claims (8)
1. A continuous preparation method of ultra-clean high-purity hydrogen peroxide is characterized by comprising the following steps: the method comprises the following operation steps:
s1: preparation of materials: selecting a certain amount of industrial-grade hydrogen peroxide which is an oxide of another hydrogen except water, has strong oxidizability and weak acidity, selecting a certain amount of styrene monomer, divinylbenzene monomer, toluene organic solvent and filler, and preparing the styrene monomer, the divinylbenzene monomer, the toluene organic solvent and the filler into a porous resin adsorbent body by a suspension copolymerization method;
s2: preparation of a hydrogen peroxide purification solution: preparing hydrogen peroxide purification solution, including back-penetrating fluid, cooling agent, environment-friendly stabilizer, distilled solution and adsorptive solution, using the back-penetrating fluid as matrix, mixing and stirring the cooling agent, environment-friendly stabilizer, distilled solution and adsorptive solution;
s3: purifying industrial grade hydrogen peroxide: enabling industrial-grade hydrogen peroxide to sequentially pass through a porous resin adsorption material body, a cation exchange column and an anion exchange column at a flow rate of 280-460L/H, and then performing circulating filtration by using a 0.1-micron filter element to obtain primary purified hydrogen peroxide;
s4: mixing and filtering: continuously pumping the primary purified industrial-grade hydrogen peroxide, namely secondary industrial-grade hydrogen peroxide, into a specified container, adding a divinylbenzene monomer, a styrene monomer and a toluene organic solvent, mixing, performing filtration at low temperature by adopting a membrane filtration method, and generating a hydrogen oxide solution with high purity;
s5: and (3) distillation and purification: introducing a hydrogen peroxide solution with high purity into a specified container, adding a hydrogen peroxide purification solution prepared by mixing and stirring a reverse osmosis liquid serving as a matrix, a cooling agent, an environment-friendly stabilizer, a distilled solution and an adsorptive solution, continuously pumping, distilling under a low-temperature condition and evaporating at a constant temperature, and performing purification operation;
s6: preparation and storage: and after the purification operation is finished, continuously pumping the purified high-purity hydrogen peroxide solution into a solution storage, performing concentration operation, further performing purification operation, and finishing the preparation of the ultra-clean high-purity hydrogen peroxide.
2. The continuous process for preparing ultra-clean high-purity hydrogen peroxide according to claim 1, characterized in that: the step S1 includes the following raw materials: the industrial-grade hydrogen peroxide accounts for 36-48%, the styrene monomer accounts for 14-25%, the divinylbenzene monomer accounts for 10-19%, the toluene organic solvent accounts for 10-18%, and the filler accounts for 6-18%.
3. The continuous process for preparing ultra-clean high-purity hydrogen peroxide according to claim 2, characterized in that: the industrial-grade hydrogen peroxide accounts for 42%, the styrene monomer accounts for 18%, the divinylbenzene monomer accounts for 15%, the toluene organic solvent accounts for 15%, and the filler accounts for 10%.
4. The continuous process for preparing ultra-clean high-purity hydrogen peroxide according to claim 2, characterized in that: the industrial grade hydrogen peroxide accounts for 44%, the styrene monomer accounts for 16%, the divinylbenzene monomer accounts for 17%, the toluene organic solvent accounts for 14%, and the filler accounts for 9%.
5. The continuous process for preparing ultra-clean high-purity hydrogen peroxide according to claim 1, characterized in that: the anti-penetrating fluid accounts for 38-51%, the coolant accounts for 10-16%, the environment-friendly stabilizer accounts for 12-22%, the distilled solution accounts for 10-18%, and the adsorptive solution accounts for 8-16%.
6. The continuous process for preparing ultra-clean high-purity hydrogen peroxide according to claim 5, wherein: the portion of the reverse osmosis liquid is 44%, the portion of the coolant is 16%, the portion of the environment-friendly stabilizer is 15%, the portion of the distilled solution is 14%, and the portion of the adsorption solution is 11%.
7. The continuous process for preparing ultra-clean high-purity hydrogen peroxide according to claim 5, wherein: the portion of the reverse osmosis liquid is 46%, the portion of the coolant is 14%, the portion of the environment-friendly stabilizer is 17%, the portion of the distilled solution is 13%, and the portion of the adsorption solution is 10%.
8. The continuous process for preparing ultra-clean high-purity hydrogen peroxide according to claim 1, characterized in that: in the step S5, constant-temperature evaporation operation is carried out at the temperature of 2-15 ℃ for 15-25 min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113912109A (en) * | 2021-11-23 | 2022-01-11 | 成都先进金属材料产业技术研究院股份有限公司 | Preparation method of nano titanium dioxide porous material |
| CN115072668A (en) * | 2022-08-11 | 2022-09-20 | 江苏瑞兆科电子材料有限公司 | Hydrogen peroxide purification method and hydrogen peroxide preparation method |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1104995A (en) * | 1993-09-13 | 1995-07-12 | 三菱瓦斯化学株式会社 | Method for enrichment and purification of aqueous hydrogen peroxide solution |
| CN1919724A (en) * | 2006-08-18 | 2007-02-28 | 上海华谊微电子化学品有限公司 | Process for preparation of ultrapure hydrogen peroxide |
| CN101239704A (en) * | 2008-03-14 | 2008-08-13 | 华南理工大学 | Method for purifying hydrogen peroxide solution |
| CN102701158A (en) * | 2012-06-21 | 2012-10-03 | 苏州晶瑞化学有限公司 | Continuous preparation method for high-purity hydrogen peroxide |
| US20210009417A1 (en) * | 2020-08-31 | 2021-01-14 | Beijing University Of Chemical Technology | Production device and production method of electronic grade hydrogen peroxide aqueous solution |
| CN112830457A (en) * | 2020-12-31 | 2021-05-25 | 安瑞森(宁夏)电子材料有限公司 | Novel purification process of hydrogen peroxide |
-
2021
- 2021-08-09 CN CN202110906158.5A patent/CN113526470A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1104995A (en) * | 1993-09-13 | 1995-07-12 | 三菱瓦斯化学株式会社 | Method for enrichment and purification of aqueous hydrogen peroxide solution |
| CN1919724A (en) * | 2006-08-18 | 2007-02-28 | 上海华谊微电子化学品有限公司 | Process for preparation of ultrapure hydrogen peroxide |
| CN101239704A (en) * | 2008-03-14 | 2008-08-13 | 华南理工大学 | Method for purifying hydrogen peroxide solution |
| CN102701158A (en) * | 2012-06-21 | 2012-10-03 | 苏州晶瑞化学有限公司 | Continuous preparation method for high-purity hydrogen peroxide |
| US20210009417A1 (en) * | 2020-08-31 | 2021-01-14 | Beijing University Of Chemical Technology | Production device and production method of electronic grade hydrogen peroxide aqueous solution |
| CN112830457A (en) * | 2020-12-31 | 2021-05-25 | 安瑞森(宁夏)电子材料有限公司 | Novel purification process of hydrogen peroxide |
Non-Patent Citations (1)
| Title |
|---|
| 于剑昆: "电子工业用超高纯过氧化氢的制备工艺", 《化学推进剂与高分子材料》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113912109A (en) * | 2021-11-23 | 2022-01-11 | 成都先进金属材料产业技术研究院股份有限公司 | Preparation method of nano titanium dioxide porous material |
| CN115072668A (en) * | 2022-08-11 | 2022-09-20 | 江苏瑞兆科电子材料有限公司 | Hydrogen peroxide purification method and hydrogen peroxide preparation method |
| CN115072668B (en) * | 2022-08-11 | 2022-12-20 | 江苏瑞兆科电子材料有限公司 | Hydrogen peroxide purification method and hydrogen peroxide preparation method |
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