CN116333192A - Amphoteric ion exchange resin special for EDI technology and synthesis method thereof - Google Patents
Amphoteric ion exchange resin special for EDI technology and synthesis method thereof Download PDFInfo
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- CN116333192A CN116333192A CN202310364540.7A CN202310364540A CN116333192A CN 116333192 A CN116333192 A CN 116333192A CN 202310364540 A CN202310364540 A CN 202310364540A CN 116333192 A CN116333192 A CN 116333192A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/44—Preparation of metal salts or ammonium salts
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J43/00—Amphoteric ion-exchange, i.e. using ion-exchangers having cationic and anionic groups; Use of material as amphoteric ion-exchangers; Treatment of material for improving their amphoteric ion-exchange properties
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/469—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis
- C02F1/4693—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis electrodialysis
- C02F1/4695—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis electrodialysis electrodeionisation
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/18—Introducing halogen atoms or halogen-containing groups
- C08F8/24—Haloalkylation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/30—Introducing nitrogen atoms or nitrogen-containing groups
- C08F8/32—Introducing nitrogen atoms or nitrogen-containing groups by reaction with amines
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/34—Introducing sulfur atoms or sulfur-containing groups
- C08F8/36—Sulfonation; Sulfation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/02—Non-contaminated water, e.g. for industrial water supply
- C02F2103/04—Non-contaminated water, e.g. for industrial water supply for obtaining ultra-pure water
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/124—Water desalination
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Abstract
The invention relates to the technical field of ion exchange resins, and discloses a special amphoteric ion exchange resin for EDI technology, which comprises the following components: the material comprises the following raw materials in parts by weight: the material comprises the following raw materials in parts by weight: 1 part of crosslinked polystyrene chloromethylation ball, 2-2.5 parts of chloromethyl ether, 0.4-0.6 part of anhydrous ferric trichloride, 0.5-0.6 part of dichloroethane, 8-10 parts of 98% concentrated sulfuric acid, 2.9-3.5 parts of methanol and 2-3 parts of 30% trimethylamine. A preparation method of a special amphoteric ion exchange resin for EDI technology comprises the following steps: through chloromethylation, acid functional group reaction and alkaline functional group reaction, the resin contains acid functional groups and alkaline functional groups simultaneously, has larger specific surface area and high exchange speed, and can replace cation and anion exchange resins in various prior EDI and MFEDI technologies; the problems of high voltage, resin damage and low regeneration efficiency in the regeneration process are solved, and the purposes of improving the regeneration efficiency of the resin, prolonging the service life, saving energy and reducing consumption are further achieved.
Description
Technical Field
The invention relates to the technical field of ion exchange resins, in particular to a special amphoteric ion exchange resin for EDI technology and a synthesis method thereof.
Background
The ion exchange resin is a polymer compound having a network structure and being insoluble, and having a functional group (an active group for exchanging ions). Typically spherical particles. The full name of the ion exchange resin consists of a classification name, a framework (or gene) name, and a basic name. The pore structure is divided into gel type and macroporous type, so that the macroporous type resin with a physical pore structure is added before the full name. The classification is acidic, and should be preceded by a "cation" and the classification is basic, and should be preceded by a "yin". Such as: macroporous strong acid styrene cation exchange resin. Ion exchange resins can also be classified into styrene-based resins and acrylic-based resins according to the kind of the matrix. The type of chemically active groups in the resin determines the main properties and class of the resin. First, the cationic resins and the anionic resins are classified into two main classes, which can be ion-exchanged with cations and anions in solution, respectively. Cationic resins are classified into strong acid and weak acid, and anionic resins are classified into strong base and weak base.
Electroplating is one of the global heavy pollution industries at present, according to incomplete statistics, the annual discharged electroplating wastewater in the electroplating industry in China has 40 hundred million m < 3 >, the water quality of the electroplating wastewater is complex, the components are not easy to control, a large number of heavy metal ions and chelates thereof are contained, and some of the electroplating wastewater belongs to cancerogenic, teratogenic and mutagenic extremely toxic substances and has extremely great harm to human beings. The existing EDI technology uses cation and anion exchange resins with different specific gravity and granularity in the same membrane stack, and the problems of uneven mixing and layering of the cation and anion exchange resins exist in practical application, so that the quality of effluent water is affected, the resins are damaged, and the regeneration efficiency is low.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the special amphoteric ion exchange resin for the EDI technology and the synthesis method thereof, which have the advantages of improving the adsorption capacity of heavy metals, reducing the harm to the environment and the like, and solve the problems raised by the background technology.
In order to achieve the above purpose, the present invention provides the following technical solutions: the amphoteric ion exchange resin special for the EDI technology is characterized by comprising the following raw materials in parts by weight: 1 part of crosslinked polystyrene chloromethylation ball, 2-2.5 parts of chloromethyl ether, 0.4-0.6 part of anhydrous ferric trichloride, 0.5-0.6 part of dichloroethane, 8-10 parts of 98% concentrated sulfuric acid, 2.9-3.5 parts of methanol and 2-3 parts of 30% trimethylamine.
The special amphoteric ion exchange resin for EDI technology as set forth in claim 1, comprising the following raw materials in parts by weight: 1 part of crosslinked polystyrene chloromethylation ball, 2-2.3 parts of chloromethyl ether, 0.4-0.5 part of anhydrous ferric trichloride, 0.5-0.55 part of dichloroethane, 8-9 parts of 98% concentrated sulfuric acid, 2.9-3.0 parts of methanol and 2-2.5 parts of 30% trimethylamine.
The special amphoteric ion exchange resin for EDI technology as set forth in claim 1, comprising the following raw materials in parts by weight: 1 part of crosslinked polystyrene chloromethylation ball, 2 parts of chloromethyl ether, 0.4 part of anhydrous ferric trichloride, 0.5 part of dichloroethane, 8-9 parts of 98% concentrated sulfuric acid, 2.9-3.0 parts of methanol and 2 parts of 30% trimethylamine.
The invention provides a preparation method of the special amphoteric ion exchange resin for EDI technology, which comprises the following steps:
1) Chloromethylation: and (3) sequentially adding 1 part of crosslinked polystyrene chloromethylation balls and 2-2.5 parts of chloromethyl ether into a reactor, expanding under stirring, stopping stirring, adding 0.4-0.6 part of anhydrous ferric trichloride, stabilizing for 1-2h, heating to 48 ℃, reacting for 8-10h, controlling the chlorine content to be more than or equal to 14.5%, and washing with anisole and methanol, washing, filtering and drying.
2) Acid functional group reaction: 1 part of chloromethylation dry ball obtained in the step (1), 0.5-0.6 part of dichloroethane and 8-10 parts of 98% concentrated sulfuric acid, stirring, heating to 54 ℃, expanding for 0.5h, heating to 85 ℃ within 1.5h, not preserving heat, continuously heating to 140 ℃ within 4 hours, continuously heating to open, not allowing the dichloroethane to reflux, continuously preserving heat for 2 hours at 140 ℃, sampling and analyzing, controlling the exchange amount to be more than or equal to 2.5mmol/g (dry), then cooling to 50 ℃, diluting the obtained resin, adding sodium hydroxide to convert into sodium form, filtering and washing.
3) Basic functional group reaction: 1 part of the sulfonated spheres obtained in the step (2), 2.9-3.5 parts of methanol, 2-3 parts of 30% trimethylamine, wherein the time for dropwise adding the trimethylamine is 8-12h, the speed for dropwise adding the trimethylamine is 80-180kg/h, the temperature in the whole process of dropwise adding the trimethylamine is controlled to be not higher than 40 ℃, the dropwise adding of the trimethylamine is completed, the alkali is dropwise added for about 1h, the temperature is raised to 42 ℃ after stabilizing, the temperature is kept for 6 h, sampling analysis is carried out after the temperature is kept for 6 h, the exchange amount is controlled to be more than or equal to 2.0mmol/g (dry), the mother liquor is pumped, washed and fed, hydrochloric acid is dropwise added to adjust the pH to be 2, the feeding is stabilized for 2h, the cooling is carried out to the room temperature, and the obtained resin is diluted, filtered and washed with pure water to be clean to obtain the average particle amphoteric ion exchange resin.
Preferably: the functionalizing agent in the step 2 has two amino groups, preferably any one of tryptophan, asparagine, glutamine, lysine, arginine or histidine.
Preferably: the mass ratio of chloromethylation dry balls, dichloroethane, 98% concentrated sulfuric acid and sulfonated balls in the step 2 is 1-1.5:4-6:0.2-0.6:1-2.5.
Compared with the prior art, the invention provides the special amphoteric ion exchange resin for the EDI technology and the synthesis method thereof, and has the following beneficial effects:
according to the amphoteric ion exchange resin special for the EDI technology and the synthesis method thereof, through the innovation of the technology, the resin simultaneously contains an acidic functional group and an alkaline functional group, has larger specific surface area and high exchange speed, can replace cation and anion exchange resins in various existing EDI and MFEDI technologies, and solves the problems of uneven mixing and layering of the cation and anion exchange resins with different specific gravities and particle sizes in the same membrane stack in the existing EDI technology in practical application, thereby influencing the quality of effluent; the problems of high voltage, resin damage and low regeneration efficiency in the regeneration process are solved, and the purposes of improving the regeneration efficiency of the resin, prolonging the service life, saving energy and reducing consumption are further achieved. The prepared particle-uniform amphoteric ion exchange resin has good desalting and regenerating properties, and can be used for preparing pure water and ultrapure water in the fields of nuclear industry, electric power, petrochemical industry, hydrometallurgy, biological medicine and the like.
Description of the embodiments
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Embodiment one: the amphoteric ion exchange resin special for the EDI technology is characterized by comprising the following raw materials in parts by weight: 1 part of crosslinked polystyrene chloromethylation ball, 2 parts of chloromethyl ether, 0.4 part of anhydrous ferric trichloride, 0.5 part of dichloroethane, 8 parts of 98% concentrated sulfuric acid, 3 parts of methanol and 2 parts of 30% trimethylamine.
A preparation method of a special amphoteric ion exchange resin for EDI technology comprises the following steps:
step one: chloromethylation: sequentially adding 1 part of crosslinked polystyrene chloromethylation balls and 2 parts of chloromethyl ether into a reactor, expanding under stirring, stopping stirring, adding 0.4 part of anhydrous ferric trichloride, stabilizing for 1-2h, heating to 48 ℃, reacting for 8-10h, controlling chlorine content to be more than or equal to 14.5%, and cleaning with anisole and methanol, washing with water, filtering and drying.
Step two: acid functional group reaction: 1 part of chloromethylation dry ball obtained in the step (1), 0.5 part of dichloroethane, 8 parts of 98% concentrated sulfuric acid, stirring, heating to 54 ℃, expanding for 0.5h, heating to 85 ℃ in 1.5h, keeping the temperature, continuously heating to 140 ℃ and continuously heating for less than 4 hours, carrying out open heating, keeping the temperature of the dichloroethane for 2 hours, sampling and analyzing, controlling the exchange amount to be more than or equal to 2.5mmol/g (dry), then cooling to 50 ℃, diluting the obtained resin, adding sodium hydroxide to convert the resin into sodium type, filtering and washing, and functionalizing the amino acid with two amino groups, preferably any one of tryptophan, asparagine, glutamine, lysine, arginine or histidine, wherein the mass ratio of chloromethylation dry ball, dichloroethane, 98% concentrated sulfuric acid and sulfonated ball is (1-1.5): 4-6:0.2-0.6:1-2.5.
Step three: basic functional group reaction: 1 part of the sulfonated ball obtained in the step (2), 3 parts of methanol, 2 parts of 30% trimethylamine, wherein the dropwise adding time is 8-12h, the dropwise adding speed is 80-180kg/h, the temperature in the whole process of dropwise adding is controlled to be not higher than 40 ℃, the dropwise adding is finished, the alkali is dropwise added for about 1h, the temperature is raised to 42 ℃ after the dropwise adding is finished, the sample analysis is carried out after the temperature is kept for 6 hours, the exchange amount is controlled to be more than or equal to 2.0mmol/g (dry), the mother liquor is pumped, the washing and the blanking are carried out, the hydrochloric acid is dropwise added to adjust the pH to be 2, the stabilizing is carried out for 2 hours, the blanking is carried out, the cooling is carried out to the room temperature, and the obtained resin is diluted, filtered, washed with pure water and washed cleanly in sequence, thereby obtaining the average particle amphoteric ion exchange resin.
The amphoteric ion exchange resin prepared in the method has a relatively general adsorption capacity for heavy metals, and finally has relatively more residual heavy metals.
Examples
The amphoteric ion exchange resin special for the EDI technology is characterized by comprising the following raw materials in parts by weight: 1 part of crosslinked polystyrene chloromethylation ball, 2.5 parts of chloromethyl ether, 0.5 part of anhydrous ferric trichloride, 0.5 part of dichloroethane, 9 parts of 98% concentrated sulfuric acid, 3.5 parts of methanol and 2 parts of 30% trimethylamine.
A preparation method of a special amphoteric ion exchange resin for EDI technology comprises the following steps:
step one: chloromethylation: and (3) sequentially adding 1 part of crosslinked polystyrene chloromethylation balls and 2.5 parts of chloromethyl ether into a reactor, expanding under stirring, stopping stirring, adding 0.5 part of anhydrous ferric trichloride, stabilizing for 1-2h, heating to 48 ℃, reacting for 8-10h, controlling chlorine content to be more than or equal to 14.5%, and cleaning with chloromethyl ether and methanol, washing with water, filtering and drying.
Step two: acid functional group reaction: 1 part of chloromethylation dry ball obtained in the step (1), 0.5 part of dichloroethane, 9 parts of 98% concentrated sulfuric acid, stirring, heating to 54 ℃, expanding for 0.5h, heating to 85 ℃ in 1.5h, keeping the temperature, continuously heating to 140 ℃ and continuously heating for less than 4 hours, carrying out open heating, keeping the temperature of the dichloroethane for 2 hours, sampling and analyzing, controlling the exchange amount to be more than or equal to 2.5mmol/g (dry), then cooling to 50 ℃, diluting the obtained resin, adding sodium hydroxide to convert the resin into sodium type, filtering and washing, and functionalizing the amino acid with two amino groups, preferably any one of tryptophan, asparagine, glutamine, lysine, arginine or histidine, wherein the mass ratio of chloromethylation dry ball, dichloroethane, 98% concentrated sulfuric acid and sulfonated ball is (1-1.5): 4-6:0.2-0.6:1-2.5.
Step three: basic functional group reaction: 1 part of the sulfonated ball obtained in the step (2), 3.5 parts of methanol and 2 parts of 30% trimethylamine, wherein the time for dropwise adding the trimethylamine is 8-12 hours, the speed for dropwise adding the trimethylamine is 80-180 kg/hour, the temperature in the whole process of dropwise adding the trimethylamine is controlled to be not higher than 40 ℃, the dropwise adding of the trimethylamine is completed, the alkali is then dropwise added for about 1 hour, the temperature is raised to 42 ℃ after the dropwise adding of the alkali is completed, the sample analysis is carried out after the temperature is kept for 6 hours, the exchange capacity is controlled to be more than or equal to 2.0mmol/g (dry), the mother liquor is pumped, the washing and the blanking are carried out, the hydrochloric acid is dropwise added to adjust the pH to be 2, the stabilizing is carried out for 2 hours, the blanking is carried out, the cooling to the room temperature is carried out, and the obtained resin is diluted, filtered and washed with pure water to be clean to obtain the average particle amphoteric ion exchange resin.
The amphoteric ion exchange resin prepared by the method has strong adsorption capacity to heavy metals and relatively less residual heavy metals finally.
Examples
The amphoteric ion exchange resin special for the EDI technology is characterized by comprising the following raw materials in parts by weight: 1 part of crosslinked polystyrene chloromethylation ball, 2.5 parts of chloromethyl ether, 0.6 part of anhydrous ferric trichloride, 0.6 part of dichloroethane, 10 parts of 98% concentrated sulfuric acid, 3.8 parts of methanol and 3 parts of 30% trimethylamine.
A preparation method of a special amphoteric ion exchange resin for EDI technology comprises the following steps:
step one: chloromethylation: and (3) sequentially adding 1 part of crosslinked polystyrene chloromethylation balls and 2.5 parts of chloromethyl ether into a reactor, expanding under stirring, stopping stirring, adding 0.6 part of anhydrous ferric trichloride, stabilizing for 1-2h, heating to 48 ℃, reacting for 8-10h, controlling chlorine content to be more than or equal to 14.5%, and cleaning with chloromethyl ether and methanol, washing with water, filtering and drying.
Step two: acid functional group reaction: 1 part of chloromethylation dry ball obtained in the step (1), 0.6 part of dichloroethane, 10 parts of 98% concentrated sulfuric acid, stirring, heating to 54 ℃, expanding for 0.5h, heating to 85 ℃ in 1.5h, keeping the temperature, continuously heating to 140 ℃ and continuously heating for less than 4 hours, carrying out open heating, keeping the temperature of the dichloroethane for 2 hours, sampling and analyzing, controlling the exchange amount to be more than or equal to 2.5mmol/g (dry), then cooling to 50 ℃, diluting the obtained resin, adding sodium hydroxide to convert the resin into sodium type, filtering and washing, and functionalizing the amino acid with two amino groups, preferably any one of tryptophan, asparagine, glutamine, lysine, arginine or histidine, wherein the mass ratio of chloromethylation dry ball, dichloroethane, 98% concentrated sulfuric acid and sulfonated ball is (1-1.5): 4-6:0.2-0.6:1-2.5.
Step three: basic functional group reaction: 1 part of the sulfonated ball obtained in the step (2), 3.8 parts of methanol and 3 parts of 30% trimethylamine, wherein the time for dropwise adding the trimethylamine is 8-12 hours, the speed for dropwise adding the trimethylamine is 80-180kg/h, the temperature in the whole process of dropwise adding the trimethylamine is controlled to be not higher than 40 ℃, the dropwise adding of the trimethylamine is completed, the alkali is then dropwise added for about 1 hour, the temperature is raised to 42 ℃ after the dropwise adding of the alkali is completed, the sample analysis is carried out after the temperature is kept for 6 hours, the exchange capacity is controlled to be more than or equal to 2.0mmol/g (dry), the mother liquor is pumped, the washing and the blanking are carried out, the hydrochloric acid is dropwise added to adjust the pH to be 2, the stabilizing is carried out for 2 hours, the blanking is carried out, the cooling to the room temperature is carried out, and the obtained resin is diluted, filtered and washed with pure water to be clean to obtain the average particle amphoteric ion exchange resin.
The amphoteric ion exchange resin prepared by the method has strong adsorption capacity to heavy metals and almost no residual heavy metals.
Judgment standard: when the ratio of the chlorine balls is larger, the residual heavy metals in the finally treated polluted water are less.
The beneficial effects of the invention are as follows: according to the amphoteric ion exchange resin special for the EDI technology and the synthesis method thereof, through the innovation of the technology, the resin simultaneously contains an acidic functional group and an alkaline functional group, has larger specific surface area and high exchange speed, can replace cation and anion exchange resins in various existing EDI and MFEDI technologies, and solves the problems of uneven mixing and layering of the cation and anion exchange resins with different specific gravities and particle sizes in the same membrane stack in the existing EDI technology in practical application, thereby influencing the quality of effluent; the problems of high voltage, resin damage and low regeneration efficiency in the regeneration process are solved, and the purposes of improving the regeneration efficiency of the resin, prolonging the service life, saving energy and reducing consumption are further achieved. The prepared particle-uniform amphoteric ion exchange resin has good desalting and regenerating properties, and can be used for preparing pure water and ultrapure water in the fields of nuclear industry, electric power, petrochemical industry, hydrometallurgy, biological medicine and the like.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (6)
1. The amphoteric ion exchange resin special for the EDI technology is characterized by comprising the following raw materials in parts by weight: 1 part of crosslinked polystyrene chloromethylation ball, 2-2.5 parts of chloromethyl ether, 0.4-0.6 part of anhydrous ferric trichloride, 0.5-0.6 part of dichloroethane, 8-10 parts of 98% concentrated sulfuric acid, 2.9-3.5 parts of methanol and 2-3 parts of 30% trimethylamine.
2. The special amphoteric ion exchange resin for EDI technology as set forth in claim 1, which is characterized by comprising the following raw materials in parts by weight: 1 part of crosslinked polystyrene chloromethylation ball, 2-2.3 parts of chloromethyl ether, 0.4-0.5 part of anhydrous ferric trichloride, 0.5-0.55 part of dichloroethane, 8-9 parts of 98% concentrated sulfuric acid, 2.9-3.0 parts of methanol and 2-2.5 parts of 30% trimethylamine.
3. The special amphoteric ion exchange resin for EDI technology as set forth in claim 1, which is characterized by comprising the following raw materials in parts by weight: 1 part of crosslinked polystyrene chloromethylation ball, 2 parts of chloromethyl ether, 0.4 part of anhydrous ferric trichloride, 0.5 part of dichloroethane, 8-9 parts of 98% concentrated sulfuric acid, 2.9-3.0 parts of methanol and 2 parts of 30% trimethylamine.
4. The preparation method of the amphoteric ion exchange resin special for the EDI technology is characterized by comprising the following steps of:
1) Chloromethylation: sequentially adding 1 part of crosslinked polystyrene chloromethylation balls and 2-2.5 parts of chloromethyl ether into a reactor, expanding under stirring, stopping stirring, adding 0.4-0.6 part of anhydrous ferric trichloride, stabilizing for 1-2h, heating to 48 ℃, reacting for 8-10h, controlling chlorine content to be more than or equal to 14.5%, and washing with anisole and methanol, washing with water, filtering and drying;
2) Acid functional group reaction: stirring 1 part of chloromethylation dry ball obtained in the step (1), 0.5-0.6 part of dichloroethane and 8-10 parts of 98% concentrated sulfuric acid, heating to 54 ℃, expanding for 0.5h, heating to 85 ℃ within 1.5h, not preserving heat, continuously heating to 140 ℃ for 4 hours, continuously heating to open, not allowing the dichloroethane to reflux, continuously preserving heat for 2 hours at 140 ℃, sampling and analyzing, controlling the exchange amount to be more than or equal to 2.5mmol/g (dry), then cooling to 50 ℃, diluting the obtained resin, adding sodium hydroxide to convert into sodium form, filtering and washing;
3) Basic functional group reaction: 1 part of the sulfonated spheres obtained in the step (2), 2.9-3.5 parts of methanol, 2-3 parts of 30% trimethylamine, wherein the time for dropwise adding the trimethylamine is 8-12h, the speed for dropwise adding the trimethylamine is 80-180kg/h, the temperature in the whole process of dropwise adding the trimethylamine is controlled to be not higher than 40 ℃, the dropwise adding of the trimethylamine is completed, the alkali is dropwise added for about 1h, the temperature is raised to 42 ℃ after stabilizing, the temperature is kept for 6 h, sampling analysis is carried out after the temperature is kept for 6 h, the exchange amount is controlled to be more than or equal to 2.0mmol/g (dry), the mother liquor is pumped, washed and fed, hydrochloric acid is dropwise added to adjust the pH to be 2, the feeding is stabilized for 2h, the cooling is carried out to the room temperature, and the obtained resin is diluted, filtered and washed with pure water to be clean to obtain the average particle amphoteric ion exchange resin.
5. The EDI technology-specific amphoteric ion exchange resin according to claim 4, wherein the functionalizing agent in the step 2 has two amino acids, preferably any one of tryptophan, asparagine, glutamine, lysine, arginine or histidine.
6. The EDI technology-specific amphoteric ion exchange resin according to claim 4, wherein: the mass ratio of chloromethylation dry balls, dichloroethane, 98% concentrated sulfuric acid and sulfonated balls in the step 2 is 1-1.5:4-6:0.2-0.6:1-2.5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310364540.7A CN116333192A (en) | 2023-04-07 | 2023-04-07 | Amphoteric ion exchange resin special for EDI technology and synthesis method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310364540.7A CN116333192A (en) | 2023-04-07 | 2023-04-07 | Amphoteric ion exchange resin special for EDI technology and synthesis method thereof |
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| CN116333192A true CN116333192A (en) | 2023-06-27 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202310364540.7A Pending CN116333192A (en) | 2023-04-07 | 2023-04-07 | Amphoteric ion exchange resin special for EDI technology and synthesis method thereof |
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2023
- 2023-04-07 CN CN202310364540.7A patent/CN116333192A/en active Pending
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