CN105859981B - The method that amphoteric ion-exchange resin is prepared using thermosetting resin - Google Patents

The method that amphoteric ion-exchange resin is prepared using thermosetting resin Download PDF

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CN105859981B
CN105859981B CN201610319447.4A CN201610319447A CN105859981B CN 105859981 B CN105859981 B CN 105859981B CN 201610319447 A CN201610319447 A CN 201610319447A CN 105859981 B CN105859981 B CN 105859981B
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reaction
amphoteric ion
exchange resin
reaction system
resin
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CN105859981A (en
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张剑秋
程知萱
付凌霄
刘松杭
韩晓兵
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University of Shanghai for Science and Technology
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F283/00Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
    • C08F283/10Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polymers containing more than one epoxy radical per molecule
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J43/00Amphoteric 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
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/14Polycondensates modified by chemical after-treatment
    • C08G59/1433Polycondensates modified by chemical after-treatment with organic low-molecular-weight compounds
    • C08G59/1477Polycondensates modified by chemical after-treatment with organic low-molecular-weight compounds containing nitrogen
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/14Polycondensates modified by chemical after-treatment
    • C08G59/1494Polycondensates modified by chemical after-treatment followed by a further chemical treatment thereof
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/40Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
    • C08G59/62Alcohols or phenols

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • General Chemical & Material Sciences (AREA)
  • Treatment Of Water By Ion Exchange (AREA)
  • Manufacture Of Macromolecular Shaped Articles (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
  • Phenolic Resins Or Amino Resins (AREA)

Abstract

The invention discloses a kind of methods that amphoteric ion-exchange resin is prepared using thermosetting resin, polymer raw material is added in into paraformaldehyde, catalyst carries out chloromethyl reaction, then adds in trimethylamine and carries out amination, acrylic acid is eventually adding, ammonium persulfate carries out reaction and obtains amphoteric ion-exchange resin.Waste and old thermosetting phenolic resin, the homemade phenolic resin of epoxy resin and laboratory and epoxy resin can be prepared into amphoteric ion-exchange resin by the present invention; raw material used in the method for the present invention is cheap and easy to get; the switching performance of product disclosure satisfy that the performance requirement of commercially available amphoteric ion-exchange resin; be conducive to environmental protection, and the sustainable development of society can also be promoted.The method that the present invention prepares amphoteric ion-exchange resin using thermosetting phenolic resin, epoxy resin is simple, easily controllable, reduces the recovery processing cost of waste and old thermosetting resin, realizes the recycling of waste, the control of environmental pollution is of great significance.

Description

The method that amphoteric ion-exchange resin is prepared using thermosetting resin
Technical field
The present invention relates to a kind of preparation method of ion exchange resin, and it is related to a kind of waste thermosetting resin and recycles More particularly to a kind of preparation method of amphoteric ion-exchange resin, skill is recycled applied to polymeric scrap material for method Art field.
Background technology
The characteristics of thermosetting epoxy resin and phenolic resin are macromolecule three-dimensional polymers, they are common is that molecular structure is Crosslinked tridimensional network.Crosslinked tridimensional network has preferable mechanical property and heat resistance, but it is not molten, insoluble Characteristic make its recycling after discarded that there is very high difficulty.As can rationally being recycled to it, not only contribute to Environmental protection, and the sustainable development of society can also be promoted, but the processing method at present after recycling is preferable not enough.
Invention content
In order to solve prior art problem, it is an object of the present invention to overcome the deficiencies of the prior art, and to provide one kind The method that amphoteric ion-exchange resin is prepared using thermosetting resin, can by waste and old thermosetting phenolic resin, epoxy resin and The homemade phenolic resin in laboratory and epoxy resin are prepared into amphoteric ion-exchange resin, and the raw material used in the method for the present invention is inexpensive It being easy to get, the switching performance of product disclosure satisfy that the performance requirement of commercially available amphoteric ion-exchange resin, be conducive to environmental protection, and The sustainable development of society can also be promoted.
Purpose is created to reach foregoing invention, the present invention uses following technical proposals:
A kind of method that amphoteric ion-exchange resin is prepared using thermosetting resin, is included the following steps:
A. with any one high molecular polymer in epoxy resin and phenolic resin or arbitrary several high molecular polymer Mixture as reactant feed, according to the hybrid reaction material portion rate example chemically reacted, with reactant feed Number is the concentrated hydrochloric acid that a concentration of 38wt.% of 10 parts of reactant feeds, 0-20 parts of catalyst and 30-200ml is taken with reference to basis It is mixed and stirred for, forms pretreatment reaction system, reaction system is made to carry out reaction 4- under 50-100 DEG C of reaction temperature 9h, after reaction system to be pre-treated is cooled to room temperature, reaction terminates, and then carries out the product generated in pretreatment reaction system It is separated by filtration, so as to collect to obtain first solid product;As currently preferred technical solution, the catalyst preferably uses Anhydrous zinc chloride, and preferably according to the mixed reactant material number ratio chemically reacted, then 10 parts of paraformaldehydes is taken to make For another reaction mass, make paraformaldehyde, anhydrous zinc chloride, reactant feed and concentrated hydrochloric acid be mixed and stirred for being formed together it is pre- Reaction system is handled, chloromethyl reaction is carried out, to prepare first solid product;It is preferred that dry granularity is used as 25 ~ 40 mesh Old circuit board powder as reactant feed;
B. it the first solid matter with deionized water of gained will be washed in step a to neutrality, and refilter separation, collect To original solid material, then by the progress of original solid material, drying to constant weight;
C. using the number of reactant feed that is used in step a with reference to basis, to take 10 parts of gained in stepb Dry original solid material, and 10-60 parts of trimethylamine is measured, original solid material and trimethylamine are mixed into beaker In, 3-24h is placed in draught cupboard after then sealing beaker mouth, aminating reaction is carried out, treats after reaction, to obtain intermediate solid Product;
D. the intermediate solid product of the gained in step c is washed with deionized to neutrality, refilters separation, collect To intermediate solid material, then by the progress of intermediate solid material, drying to constant weight;
E. using the number of reactant feed used in step a as reference basis, by 10 parts of gained in step d Intermediate solid material, 0.1-1.5 part potassium peroxydisulfate, the acrylic acid of 1-15ml and 30-50ml deionized waters are mixed and stirred for End reaction system is formed, end reaction system is made to carry out reaction 8-15h under 70-80 DEG C of reaction temperature, treats end reaction After system is cooled to room temperature, reaction terminates, and is then filtered the product generated in end reaction system, so as to collect to obtain Final solid product;
F. the final solid matter with deionized water of the gained in step e is washed to neutrality, refilters separation, collected Final solid material is obtained, then final solid material is dried, obtains amphoteric ion-exchange resin.
As the further preferred technical solution of said program, in described step a, c and e, the number of each material is equal For parts by weight, the number of each material corresponds to the gravimetric value that unit of weight is g.In the step a, according to being chemically reacted Hybrid reaction material portion rate example, using the number of reactant feed as with reference to basis, preferably take 10 g reactant feed, The concentrated hydrochloric acid of the paraformaldehyde of 10g, the anhydrous zinc chloride of 10-20g and 100-200ml is mixed and stirred for, and forms pretreatment Reaction system.In the step c, using the number of reactant feed used in step a as with reference to basis, 10g is preferably taken The original solid material of the drying of gained in stepb, and the trimethylamine of 30-35g is measured, by original solid material and trimethylamine It is mixed into beaker, carries out aminating reaction.In the step e, using the number of reactant feed that is used in step a as With reference to basis, preferably by the propylene of the 10g intermediate solid material of gained, the potassium peroxydisulfate of 0.1-1.5g, 2-13ml in step d Acid and 30-50ml deionized waters carry out being mixed and stirred for forming end reaction system, are reacted end reaction system.
The present invention compared with prior art, has following obvious prominent substantive distinguishing features and remarkable advantage:
1. polymer raw material is added in paraformaldehyde by the present invention, catalyst carries out chloromethyl reaction, then adds in trimethylamine Amination is carried out, is eventually adding acrylic acid, ammonium persulfate carries out reaction and obtains amphoteric ion-exchange resin, and the present invention can will be waste and old Thermosetting phenolic resin, the homemade phenolic resin of epoxy resin and laboratory and epoxy resin are prepared into amphoteric ion-exchange resin Anion exchange resin is prepared into, raw material used is cheap and easy to get, and the switching performance of product disclosure satisfy that commercially available amphoteric ion is handed over Change the performance requirement of resin;
2. the method that the present invention prepares amphoteric ion-exchange resin using thermosetting phenolic resin, epoxy resin is simple, easily In control, the recovery processing cost of waste and old thermosetting resin is reduced, realizes the recycling of waste, the control of environmental pollution Fixture is significant.
Specific embodiment
Details are as follows for the preferred embodiment of the present invention:
Embodiment one:
In the present embodiment, a kind of method that amphoteric ion-exchange resin is prepared using thermosetting resin, including walking as follows Suddenly:
A. water-bath is warming up to 80 DEG C, using old circuit board powder as reactant feed, according to being chemically reacted Hybrid reaction material portion rate example, weigh old circuit board powder 10g, paraformaldehyde 10g, anhydrous zinc chloride 20g, and dosage Cylinder measures the concentrated hydrochloric acid of a concentration of 38wt.% of 200ml, and the material weighed and concentrated hydrochloric acid are poured into together in 500ml three-necked flasks, Pretreatment reaction system, then the hollow plug of three-necked flask beyond the Great Wall are mixed to form, then three-necked flask is placed in water-bath, in Speed stirring pretreatment reaction system at a temperature of 80 DEG C of water-bath, makes reaction system carry out reaction 8h generation first set reactions Product is treated after reaction, to close water-bath, takes out three-necked flask, the reaction system for generating first set reaction product is transferred to In 500ml beakers, three-necked flask is washed in triplicate with deionized water, and the liquid after washing is poured into beaker, it will be in beaker The reaction system containing first set reaction product filtered with sand core funnel, obtain first set reaction product, and will be just with deionized water Secondary response product is washed to neutrality, refilters separation, and collection obtains aqueous first set reaction product, then will be aqueous first anti- Product is answered to be placed in 60 DEG C of baking ovens for 24 hours, drying to constant weight, obtains dry first set reaction product;
B. the first set reaction product 10g of the drying obtained in step a is taken, and measures 30g trimethylamines, by first set reaction Product and trimethylamine are mixed into another beaker, placed in draught cupboard after then sealing beaker mouth with preservative film for 24 hours, into Row aminating reaction generates second of reaction product, treats after reaction, by the reaction containing second of reaction product in beaker System is filtered with sand core funnel, obtains second of reaction product, and washed second of reaction product to neutrality with deionized water, Separation is refiltered, collection obtains second aqueous of reaction product, then by second aqueous of reaction product in 60 DEG C of baking ovens For 24 hours, drying to constant weight for middle placement, obtains second dry of reaction product;
C. water-bath is warming up to 70 DEG C again, weighs second of reaction product 10g, 1g of the drying obtained in stepb Potassium peroxydisulfate, measure 13ml acrylic acid and 30ml deionized waters with graduated cylinder, the material weighed and the liquid measured fallen together In the three-necked flask for entering 100ml, end reaction system, then the hollow plug of three-necked flask beyond the Great Wall are mixed to form, then by three mouthfuls of burnings Bottle is placed in water-bath, and moderate-speed mixer pretreatment reaction system at a temperature of 70 DEG C of water-bath, carries out reaction system React 12h generation final reacting products;
D. by after the final reacting product cooling of gained in step c, first generation final reacting product is diluted with clear water End reaction system after dilution with sand core funnel is filtered, obtains final reacting product by end reaction system, then spend from Sub- water washs final reacting product to neutrality, refilters separation, and collection obtains aqueous final reacting product, then will be aqueous Final reacting product placed in 60 DEG C of baking ovens for 24 hours, obtain amphoteric ion-exchange resin.
Polymer raw material is added in into paraformaldehyde, catalyst carries out chloromethyl reaction, then adds in trimethylamine and carries out amination, Acrylic acid is eventually adding, ammonium persulfate carries out reaction and obtains amphoteric ion-exchange resin.The present embodiment is by waste and old thermosetting property tree Fat is prepared into anion exchange resin, and raw material used is cheap and easy to get, and the switching performance of product disclosure satisfy that commercially available amphoteric ion The performance requirement of exchanger resin.
Embodiment two:
The present embodiment and embodiment one are essentially identical, are particular in that:
In the present embodiment, a kind of method that amphoteric ion-exchange resin is prepared using thermosetting resin, including walking as follows Suddenly:
A. water-bath is warming up to 80 DEG C, using old circuit board powder as reactant feed, according to being chemically reacted Hybrid reaction material portion rate example, weigh old circuit board powder 10g, paraformaldehyde 10g, anhydrous zinc chloride 10g, and dosage Cylinder measures the concentrated hydrochloric acid of a concentration of 38wt.% of 100ml, and the material weighed and concentrated hydrochloric acid are poured into together in 500ml three-necked flasks, Pretreatment reaction system, then the hollow plug of three-necked flask beyond the Great Wall are mixed to form, then three-necked flask is placed in water-bath, in Speed stirring pretreatment reaction system at a temperature of 80 DEG C of water-bath, makes reaction system carry out reaction 8h generation first set reactions Product is treated after reaction, to close water-bath, takes out three-necked flask, the reaction system for generating first set reaction product is transferred to In 500ml beakers, three-necked flask is washed in triplicate with deionized water, and the liquid after washing is poured into beaker, it will be in beaker The reaction system containing first set reaction product filtered with sand core funnel, obtain first set reaction product, and will be just with deionized water Secondary response product is washed to neutrality, refilters separation, and collection obtains aqueous first set reaction product, then will be aqueous first anti- Product is answered to be placed in 60 DEG C of baking ovens for 24 hours, drying to constant weight, obtains dry first set reaction product;
B. the first set reaction product 10g of the drying obtained in step a is taken, and measures 35g trimethylamines, by first set reaction Product and trimethylamine are mixed into another beaker, placed in draught cupboard after then sealing beaker mouth with preservative film for 24 hours, into Row aminating reaction generates second of reaction product, treats after reaction, by the reaction containing second of reaction product in beaker System is filtered with sand core funnel, obtains second of reaction product, and washed second of reaction product to neutrality with deionized water, Separation is refiltered, collection obtains second aqueous of reaction product, then by second aqueous of reaction product in 60 DEG C of baking ovens For 24 hours, drying to constant weight for middle placement, obtains second dry of reaction product;
C. water-bath is warming up to 80 DEG C again, weigh the drying obtained in stepb second of reaction product 10g, The potassium peroxydisulfate of 0.6g measures 7ml acrylic acid and 30ml deionized waters with graduated cylinder, by the material weighed and the liquid measured together It pours into the three-necked flask of 100ml, end reaction system, then the hollow plug of three-necked flask beyond the Great Wall is mixed to form, then by three mouthfuls Flask is placed in water-bath, moderate-speed mixer pretreatment reaction system, at a temperature of 80 DEG C of water-bath, make reaction system into Row reaction 12h generation final reacting products;
D. this step is identical with embodiment one.
Embodiment three:
The present embodiment is substantially the same as in the previous example, and is particular in that:
In the present embodiment, a kind of method that amphoteric ion-exchange resin is prepared using thermosetting resin, including walking as follows Suddenly:
A. using bisphenol A type epoxy resin and isophorone diamine as first set reaction raw material, 50g bisphenol-As are weighed first Type epoxy resin and 6g isophorone diamine after stirring evenly, cure 12h at 80 DEG C, then use obtained cured product Pulverizer crushes, and the product after crushing with the sieve of 25 mesh and 40 mesh is screened, obtains the first set reaction between 25 ~ 40 mesh Raw material granular materials, is put into oven drying, water-bath is warming up to 80 DEG C, then according to the hybrid reaction chemically reacted Material number ratio weighs first set reaction raw material granular materials 10g, paraformaldehyde 10g, anhydrous zinc chloride 15g, and uses graduated cylinder The concentrated hydrochloric acid of a concentration of 38wt.% of 200ml is measured, the material weighed and concentrated hydrochloric acid are poured into together in 500ml three-necked flasks, is mixed Conjunction forms pretreatment reaction system, then the hollow plug of three-necked flask beyond the Great Wall, then three-necked flask is placed in water-bath, middling speed Pretreatment reaction system is stirred, at a temperature of 80 DEG C of water-bath, reaction system is made to carry out reaction 7h generation first set reaction productions Object is treated after reaction, to close water-bath, takes out three-necked flask, the reaction system for generating first set reaction product is transferred to 500ml In beaker, three-necked flask is washed in triplicate with deionized water, the liquid after washing is poured into beaker, by containing in beaker The reaction system of first set reaction product is filtered with sand core funnel, obtains first set reaction product, and with deionized water by first set reaction Product is washed to neutrality, refilters separation, collection obtains aqueous first set reaction product, then by aqueous first set reaction product It is placed in 60 DEG C of baking ovens for 24 hours, drying to constant weight, obtains dry first set reaction product;
B. the first set reaction product 10g of the drying obtained in step a is taken, and measures 30g trimethylamines, by first set reaction Product and trimethylamine are mixed into another beaker, placed in draught cupboard after then sealing beaker mouth with preservative film for 24 hours, into Row aminating reaction generates second of reaction product, treats after reaction, by the reaction containing second of reaction product in beaker System is filtered with sand core funnel, obtains second of reaction product, and washed second of reaction product to neutrality with deionized water, Separation is refiltered, collection obtains second aqueous of reaction product, then by second aqueous of reaction product in 60 DEG C of baking ovens For 24 hours, drying to constant weight for middle placement, obtains second dry of reaction product;
C. water-bath is warming up to 70 DEG C again, weigh the drying obtained in stepb second of reaction product 10g, The potassium peroxydisulfate of 0.1g measures 2ml acrylic acid and 30ml deionized waters with graduated cylinder, by the material weighed and the liquid measured together It pours into the three-necked flask of 100ml, end reaction system, then the hollow plug of three-necked flask beyond the Great Wall is mixed to form, then by three mouthfuls Flask is placed in water-bath, moderate-speed mixer pretreatment reaction system, at a temperature of 70 DEG C of water-bath, make reaction system into Row reaction 12h generation final reacting products;
D. this step is identical with embodiment one.
Experiment detection and analysis:
Physicochemical properties experimental analysis is carried out to amphoteric ion-exchange resin prepared by above-described embodiment, it is prepared to obtain Amphoteric ion-exchange resin specific performance parameter it is as follows:Its granular size is 40-120 mesh, and cation exchange capacity (CEC) is reachable 0.7274 mmol/g, for anion exchange capacity up to 0.7023mmol/g, maximum operation (service) temperature can reach 100 DEG C.
The embodiment of the present invention is illustrated above, but the present invention is not limited to above-described embodiments, it can also be according to this hair The purpose of bright innovation and creation makes a variety of variations, and that is done under the Spirit Essence and principle of all technical solutions according to the present invention changes Become, modification, substitute, combination or simplified, should be equivalent substitute mode, as long as meeting the goal of the invention of the present invention, as long as not Technical principle and the inventive concept of the method for amphoteric ion-exchange resin are prepared using thermosetting resin away from the present invention, is belonged to Protection scope of the present invention.

Claims (7)

  1. A kind of 1. method that amphoteric ion-exchange resin is prepared using thermosetting resin, which is characterized in that include the following steps:
    A. with the mixed of any one high molecular polymer in epoxy resin and phenolic resin or arbitrary several high molecular polymer Object is closed as reactant feed, according to the hybrid reaction material portion rate example chemically reacted, with the weight of reactant feed Part be with reference to basis, take 10 parts of reactant feeds, 0-20 parts of catalyst and 30-200ml a concentration of 38wt.% concentrated hydrochloric acid into Row is mixed and stirred for, and forms pretreatment reaction system, reaction system is made to carry out reaction 4-9h under 50-100 DEG C of reaction temperature, After reaction system to be pre-treated is cooled to room temperature, reaction terminates, and then carries out the product generated in pretreatment reaction system Filter separation, so as to collect to obtain first solid product;
    B. it the first solid matter with deionized water of gained will be washed in step a to neutrality, and refilter separation, collection obtains initial Solid material, then by the progress of original solid material, drying to constant weight;
    C. using the number of reactant feed that is used in step a with reference to basis, to take 10 parts of dryings of gained in stepb Original solid material, and 10-60 parts of trimethylamine is measured, original solid material and trimethylamine are mixed into beaker, then 3-24h is placed in draught cupboard after sealing beaker mouth, aminating reaction is carried out, treats after reaction, to obtain intermediate solid product;
    D. the intermediate solid product of the gained in step c is washed with deionized to neutrality, separation is refiltered, during collection obtains Between solid material, then by intermediate solid material carry out drying to constant weight;
    E. using the number of reactant feed used in step a as with reference to basis, the centre of 10 parts of gained in step d is consolidated Body material, 0.1-1.5 part potassium peroxydisulfate, the acrylic acid of 1-15ml and 30-50ml deionized waters carry out being mixed and stirred for being formed most End reaction system makes end reaction system carry out reaction 8-15h under 70-80 DEG C of reaction temperature, treats that end reaction system is cold But to after room temperature, reaction terminates, and is then filtered the product generated in end reaction system, finally solid so as to collect to obtain Body product;
    F. the final solid matter with deionized water of the gained in step e is washed to neutrality, refilters separation, collection obtains most Then final solid material is dried, obtains amphoteric ion-exchange resin by whole solid material.
  2. 2. the method for amphoteric ion-exchange resin is prepared using thermosetting resin according to claim 1, it is characterised in that: In the step a, the catalyst uses anhydrous zinc chloride, according to the mixed reactant material portion rate chemically reacted Example, then 10 parts of paraformaldehydes is taken to make paraformaldehyde, anhydrous zinc chloride, reactant feed and dense salt as another reaction mass Acid is mixed and stirred for forming pretreatment reaction system together, chloromethyl reaction is carried out, to prepare first solid product.
  3. 3. the method for amphoteric ion-exchange resin is prepared using thermosetting resin according to claim 2, it is characterised in that: In described step a, c and e, the number of each material is parts by weight, and the number of each material corresponds to the gravimetric value that unit of weight is g.
  4. 4. the method for amphoteric ion-exchange resin is prepared using thermosetting resin according to claim 3, it is characterised in that: In the step a, according to the hybrid reaction material portion rate example chemically reacted, using the number of reactant feed as with reference to base Plinth takes the concentrated hydrochloric acid of the reactant feed of 10g, the paraformaldehyde of 10g, the anhydrous zinc chloride of 10-20g and 100-200ml to carry out It is mixed and stirred for, forms pretreatment reaction system.
  5. 5. the method for amphoteric ion-exchange resin is prepared using thermosetting resin according to claim 3, it is characterised in that: In the step c, using the number of reactant feed that is used in step a with reference to basis, to take 10g gained in stepb Dry original solid material, and the trimethylamine of 30-35g is measured, original solid material and trimethylamine are mixed into beaker, Carry out aminating reaction.
  6. 6. the method for amphoteric ion-exchange resin is prepared using thermosetting resin according to claim 3, it is characterised in that: In the step e, using the number of reactant feed that is used in step a as with reference to basis, by 10g in step d gained Intermediate solid material, the potassium peroxydisulfate of 0.1-1.5g, the acrylic acid of 2-13ml and 30-50ml deionized waters are mixed and stirred for End reaction system is formed, is reacted end reaction system.
  7. 7. the method for amphoteric ion-exchange resin is prepared using thermosetting resin according to any one in claim 1~6, It is characterized in that:In the step a, it is the old circuit board powder of 25~40 mesh as reactant to use dry granularity Raw material.
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CN106378212B (en) * 2016-09-27 2018-11-23 南京工程学院 A kind of weak-acid cation-exchange resin and preparation method thereof containing branched structure
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101157059A (en) * 2007-08-15 2008-04-09 宁夏大学 Aporate amphion switching biology isolate medium as well as its preparing method and usage
CN101781381A (en) * 2009-12-31 2010-07-21 安徽皖东化工有限公司 Preparation method of 201*4 strong-basicity styrene series anion exchange resin

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101157059A (en) * 2007-08-15 2008-04-09 宁夏大学 Aporate amphion switching biology isolate medium as well as its preparing method and usage
CN101781381A (en) * 2009-12-31 2010-07-21 安徽皖东化工有限公司 Preparation method of 201*4 strong-basicity styrene series anion exchange resin

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
"Preparation of anion exchange resin by recycling of waste printed circuit boards";Jianqiu Zhang et al.;《RSC Advances》;20151123;106680-106687 *

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