CN106592214A - Preparation method of amphoteric ion exchange fiber - Google Patents
Preparation method of amphoteric ion exchange fiber Download PDFInfo
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- CN106592214A CN106592214A CN201611174634.4A CN201611174634A CN106592214A CN 106592214 A CN106592214 A CN 106592214A CN 201611174634 A CN201611174634 A CN 201611174634A CN 106592214 A CN106592214 A CN 106592214A
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- ion exchange
- preparation
- amphoteric ion
- exchange fibre
- aminated
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
- D06M13/325—Amines
- D06M13/332—Di- or polyamines
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/68—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof
- D06M11/70—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof with oxides of phosphorus; with hypophosphorous, phosphorous or phosphoric acids or their salts
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/26—Polymers or copolymers of unsaturated carboxylic acids or derivatives thereof
- D06M2101/28—Acrylonitrile; Methacrylonitrile
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Treatment Of Water By Ion Exchange (AREA)
Abstract
The invention discloses a preparation method of amphoteric ion exchange fiber. The method comprises steps as follows: an amination step: a proper amount of polyacrylonitrile fiber is taken and slowly added to a proper amount of organic alcohol, a proper quantity of amination reagents are added, the mixture is stirred at the specific temperature and subjected to a backflow reaction for certain time, a product is washed to be neutral with water, subjected to suction filtration and air-dried, and an aminated product is obtained; a phosphorylation step: the aminated product is taken and mixed with a proper amount of clear water and a proper quantity of aldehyde solvents, the mixture is stirred at the normal temperature, a phosphorylation agent is added, the mixture is stirred at the specific temperature and subjected to a backflow reaction for certain time, the solvents are removed after the reaction ends, a product is washed with water and hydrochloric acid sequentially and washed to be neutral finally, and the amphoteric ion exchange fiber is obtained. The specific fiber is taken as a framework, a high-selectivity adsorption material is formed through a two-step reaction of amination and phosphorylation, and the preparation method has the characteristics that the preparation method is simple, raw materials are cheap and easy to obtain, the adsorption capacity is high and the chelation capability is high.
Description
Technical field
The invention belongs to the application of modified ion exchanging fiber material, more particularly to one kind is with weak acid and weak base two
Plant characteristic and the preparation method with adsorption function and the new type amphoteric ion-exchange fibre of ion exchanging function.
Background technology
Ion-exchange fibre (IEF) is the feature adsorbing separation material of new generation after granular ion exchange resin
Material.100 μm of the most ＜ of diameter of ion-exchange fibre, or even 10 μm of ＜, with obvious kinetic advantage, it has exchange speed
Degree is fast, effective ratio area is big, and fluid resistance is little, regeneration is easy and the series of advantages such as easy to use.It can be in a variety of forms
Using, such as fiber, yarn, fabric, non-weaving cloth, thus suitable for the ion exchange process of various ways.Extensively use
In prepare electronics pure water, medicinal water, biologic product, Industrial Waste Water Treatments, the absorption of poisonous and foul gas, catalyst carrier,
The fields such as precious metal recovery, the collection of ocean rare metal, the separation and Extraction of medicine and biochemistry, develop rapidly now
One of new and high technology, application prospect is very wide.
When ion-exchange fibre is with electrolyte solution contacts, the ion on fiber can make have selection with the ion in solution
The exchange of property.Its point cation exchange fibre, anion-exchange fibre and amphoteric ion exchange fibre.Ion-exchange fibre can use
In Adsorption of Heavy Metals and pigment, it is used as new sexual function macromolecular material, the chemistry with uniqueness and physical absorption and separation property
Can, there is irreplaceable effect in some association areas, it is a kind of efficient absorption material grown up after activated carbon,
Because its surface area is big, ion-exchange speed is fast, easily regeneration, applicability extensively becomes one of technical field of environment pollution control
Study hotspot.
The structure of ion-exchange fibre is typically made up of matrix fiber and the cation exchange groups two parts being connected thereto, wherein
Matrix fiber has polyvinyl alcohol, poly- phenolic aldehyde, polyamide, polyolefin, polyacrylonitrile, polyvinyl chloride-acrylonitrile copolymer, cellulose
Deng ion-exchange group has strong acid, weak acid, highly basic, weak base, amphiprotic group etc..
Cellulose is the natural high molecular substance that nature is widely present, and is a kind of renewable resources.Plant is led to every year
Photosynthesis is crossed, hundreds of millions tons of cellulose can be produced.In recent years, with oil, the decline of coal reserves, its importance is increasingly
Significantly.Particularly since the eighties in last century, the growing interest and attention with various countries' environmental pollution forces people's handle
Notice focuses on cellulose again, and this has on the renewable resource of biodegradability, environment compatibility.Although closing
It is relatively more in the research of ion-exchange fibre, but great majority carry out graft modification based on synthetic fibers, and with fiber
Amphoteric ion exchange fibre relevant report based on element is relatively fewer.
The content of the invention
The reality such as it is difficult to reclaim in order to the heavy metal water pollution emergency disposal technology that solves to happen suddenly at present is deficient, dispose material to ask
Topic, the invention provides a kind of preparation method of new type amphoteric ion-exchange fibre；Polyacrylonitrile fibre be a class quantity it is abundant,
Wide material sources, absorption raw material cheap and easy to get, containing abundant cellulose, and high mechanical strength, chemical synthesis can be passed through
Means introduce one or more heavy metal ion (such as copper ion) on polyacrylonitrile fibre the network of very strong adsorption capacity
Group (such as carboxyl and amino) is closed, the purpose for rapidly and efficiently removing removing heavy metals is reached, and preparation method is simple, can be good at
Solve the above problems.
The purpose of the present invention can be achieved through the following technical solutions：
A kind of preparation method of amphoteric ion exchange fibre, the preparation method comprises the steps：
(1) it is aminated：Take appropriate polyacrylonitrile fibre to be slowly added in appropriate Organic Alcohol, and add quantitative amine
Base reagent, stirring and back flow reaction special time under specified temp, products in water is washed to neutrality, and suction filtration dries, and obtains amine
Base product；
(2) phosphorylation：Take aminated product and add appropriate clear water and aldehyde salt solvent, after stirring under normal temperature phosphoric acid is added
Chemical drug agent, stirring and back flow reaction special time, remove solvent under specified temp after terminating, successively with water, hydrochloric acid wash products,
Finally wash with water to neutrality, obtain product amphoteric ion exchange fibre.
Organic Alcohol described in step (1) is one or more in ethylene glycol, triethylene glycol, glycerine.
Aminated reagent described in step (1) is the one kind or many in ethylenediamine, diethylenetriamine, triethylene tetramine
Kind.
Reflux time described in step (1) is 8～12h, and specified temp is 90～100 DEG C.
Polyacrylonitrile fibre, Organic Alcohol described in step (1) is 1 with aminated reagent quality ratio:20～35:4～8.
Phosphorylation medicament described in step (2) is phosphorous acid；Described aldehyde salt solvent is in formaldehyde, acetaldehyde and propionic aldehyde
One or more.
Mixing time is 5～10min under normal temperature described in step (2)；Described reflux time is 12～15h,
Specified temp is 100～110 DEG C；Described concentration of hydrochloric acid is 1～5%.
Aminated product, phosphorylation medicament and aldehyde salt solvent mass ratio described in step (2) is 1:6～10:0.5～1.
Amphoteric ion exchange fibre described in step (2) to Adsorption of Cu 2+, Cr6+, Pb2+, adsorption rate is 95.74～
98.14%.
Described adsorption step is：Take appropriate amphoteric ion exchange fibre Jing certain density HCl or NaOH immersion activation
Afterwards, clean and load chromatographic column, heavy metal solution is adsorbed through ion-exchange fibre.
Beneficial effects of the present invention：
1) the modifying polyacrylonitrile method that the present invention is provided is simple, and easy to operate, performance is more stable, and saving is prepared into
This；
2) ion-exchange fibre that the method makes has weak acid and a big characteristic of weak base two, the scope of Adsorption of Heavy Metals it is wide and
Adsorption capacity is big, especially for the treatment effeciency height in heavy metal water pollution and with stronger stability, after process is made
While waste liquid realizes innoxious, precious metal can be also reclaimed；
3) product mechanically and chemically good stability, using method is simple, further increases using the economy of adsorbent
Property and the feature of environmental protection.
Specific embodiment
Technical scheme is further described below, but is not limited thereto, it is every to the technology of the present invention
Scheme is modified or equivalent, without deviating from the spirit and scope of technical solution of the present invention, all should be covered in the present invention
Protection domain in.
A kind of preparation method of amphoteric ion exchange fibre, the method be from polyacrylonitrile fibre as raw material, and
Group activated monomer is complexed by chemical modification, the characteristic after fiber amido phosphoric acid simultaneously with weak acid and weak base fiber is made；
The present invention, by aminated and phosphorylation two-step reaction, forms high-selectivity adsorption material with special fiber as skeleton
Material, with preparation method it is simple, raw material is cheap and easy to get, adsorption capacity is big, the characteristics of sequestering power is strong, and applied range, especially
It is directed to the treatment effeciency height of heavy metal water pollution and with stronger stability, and the waste liquid after process is made is realized innoxious
While, can also reclaim precious metal, and product mechanically and chemically good stability, using method is simple, further increases
Using the economy and the feature of environmental protection of adsorbent.
Embodiment 1：
(1) it is aminated：Polyacrylonitrile fibre 4g is taken, is slowly added in 100ml ethylene glycol and is stirred, add 5ml
Diethylenetriamine, back flow reaction 10h at 100 DEG C, after suction filtration with clean water to it is close neutrality after dry；
(2) phosphorylation：Take it is aminated after intermediate product, be added to 100ml water, 3g formalins, stirring at normal temperature 10min,
Add 8g phosphorous acid, 110 DEG C of reaction 15h remove solvent after terminating, successively with water, 3% hydrochloric acid wash products, finally with clear
It is washed to neutrality and obtains product；
(3) adsorption experiment：0.5g products are taken Jing after 2%NaOH immersion activation, is cleaned and is loaded chromatographic column, by 100mL Cu2+
Solution (the 100ppm solution being configured to by copper nitrate medicament) adsorbs through ion-exchange fibre, speed 2ml/min.
Cross the Cu of post water outlet2+Concentration is 2.13ppm, and adsorption rate is 97.87%.
Embodiment 2：
(1) it is aminated：Polyacrylonitrile fibre 4g is taken, is slowly added in 100ml ethylene glycol and is stirred, add 5ml
Ethylenediamine, back flow reaction 10h at 100 DEG C, after suction filtration with clean water to it is close neutrality after dry；
(2) phosphorylation：Take it is aminated after intermediate product, be added to 100ml water, 3g acetaldehyde liquid, stirring at normal temperature 10min,
Add 8g phosphorous acid, 110 DEG C of reaction 15h remove solvent after terminating, successively with water, 3% hydrochloric acid wash products, finally with clear
It is washed to neutrality and obtains product；
(3) adsorption experiment：0.5g products are taken Jing after 2%HCl immersion activation, is cleaned and is loaded chromatographic column, by 100mL Cr6+It is molten
Liquid (the 100ppm solution being configured to by potassium bichromate medicament) adsorbs through ion-exchange fibre, speed 2ml/min.
Cross the Cr of post water outlet6+Concentration is 3.05ppm, and adsorption rate is 96.95%.
Embodiment 3：
(1) it is aminated：Polyacrylonitrile fibre 4g is taken, is slowly added in 100ml glycerine and is stirred, add 5ml
Ethylenediamine, back flow reaction 10h at 100 DEG C, after suction filtration with clean water to it is close neutrality after dry；
(2) phosphorylation：Take it is aminated after intermediate product, be added to 100ml water, 3g acetaldehyde liquid, stirring at normal temperature 10min,
Add 8g phosphorous acid, 100 DEG C of reaction 15h remove solvent after terminating, successively with water, 3% hydrochloric acid wash products, finally with clear
It is washed to neutrality and obtains product；
(3) adsorption experiment：0.5g products are taken Jing after 2%NaOH immersion activation, is cleaned and is loaded chromatographic column, by 100mL Cu2+
Solution (the 100ppm solution being configured to by copper nitrate medicament) adsorbs through ion-exchange fibre, speed 2ml/min.
Cross the Cu of post water outlet2+Concentration is 1.86ppm, and adsorption rate is 98.14%.
Embodiment 4：
(1) it is aminated：Polyacrylonitrile fibre 4g is taken, is slowly added in 100ml glycerine and is stirred, add 5ml
Diethylenetriamine, back flow reaction 8h at 100 DEG C, after suction filtration with clean water to it is close neutrality after dry；
(2) phosphorylation：Take it is aminated after intermediate product, be added to 100ml water, 4g formalins, stirring at normal temperature 10min,
Add 8g phosphorous acid, 110 DEG C of reaction 12h remove solvent after terminating, successively with water, 3% hydrochloric acid wash products, finally with clear
It is washed to neutrality and obtains product；
(3) adsorption experiment：0.5g products are taken Jing after 2%HCl immersion activation, is cleaned and is loaded chromatographic column, by 100mL Cr6+It is molten
Liquid (the 100ppm solution being configured to by potassium bichromate medicament) adsorbs through ion-exchange fibre, speed 2ml/min.
Cross the Cr of post water outlet6+Concentration is 2.45ppm, and adsorption rate is 97.55%.
Embodiment 5：
(1) it is aminated：Polyacrylonitrile fibre 4g is taken, is slowly added in 100ml ethylene glycol and is stirred, add 5ml
Ethylenediamine, back flow reaction 10h at 100 DEG C, after suction filtration with clean water to it is close neutrality after dry；
(2) phosphorylation：Take it is aminated after intermediate product, be added to 100ml water, 3g acetaldehyde liquid, stirring at normal temperature 10min,
Add 8g phosphorous acid, 100 DEG C of reaction 12h remove solvent after terminating, successively with water, 3% hydrochloric acid wash products, finally with clear
It is washed to neutrality and obtains product；
(3) adsorption experiment：0.5g products are taken Jing after 2%NaOH immersion activation, is cleaned and is loaded chromatographic column, by 100mL Pb2+
Solution (the 100ppm solution being configured to by plumbi nitras medicament) adsorbs through ion-exchange fibre, speed 2ml/min.
Cross the Pb of post water outlet2+Concentration is 4.26ppm, and adsorption rate is 95.74%.
Embodiment 6：
(1) it is aminated：Polyacrylonitrile fibre 4g is taken, is slowly added in 100ml triethylene glycols and is stirred, add 8ml
Triethylene tetramine, back flow reaction 12h at 90 DEG C, after suction filtration with clean water to it is close neutrality after dry；
(2) phosphorylation：Take it is aminated after intermediate product, be added to 100ml water, 3g propionic aldehyde liquid, stirring at normal temperature 5min, then
Add 8g phosphorous acid, 100 DEG C of reaction 15h that solvent is removed after terminating, successively with water, 3% hydrochloric acid wash products finally use clear water
It is washed till neutrality and obtains product；
(3) adsorption experiment：0.5g products are taken Jing after 2%NaOH immersion activation, is cleaned and is loaded chromatographic column, by 100mL Cr6+
Solution (the 100ppm solution being configured to by potassium bichromate medicament) adsorbs through ion-exchange fibre, speed 2ml/min.
Cross the Cr of post water outlet6+Concentration is 2.06ppm, and adsorption rate is 97.94%.
Above content is only citing made for the present invention and explanation, and affiliated those skilled in the art are to being retouched
The specific embodiment stated is made various modifications or supplements or substituted using similar mode, without departing from invention or super
More scope defined in the claims, all should belong to protection scope of the present invention.
Claims (10)
1. a kind of preparation method of amphoteric ion exchange fibre, it is characterised in that the preparation method comprises the steps：
(1) it is aminated：Take appropriate polyacrylonitrile fibre to be slowly added in appropriate Organic Alcohol, and add quantitative aminated
Reagent, stirring and back flow reaction special time under specified temp, products in water is washed to neutrality, and suction filtration dries, and obtains aminated
Product；
(2) phosphorylation：Take aminated product and add appropriate clear water and aldehyde salt solvent, after stirring under normal temperature phosphoric acid chemical drug is added
Agent, stirring and back flow reaction special time, remove solvent, successively with water, hydrochloric acid wash products, finally under specified temp after terminating
Wash with water to neutrality, obtain product amphoteric ion exchange fibre.
2. the preparation method of a kind of amphoteric ion exchange fibre according to claim 1, it is characterised in that in step (1)
Described Organic Alcohol is one or more in ethylene glycol, triethylene glycol, glycerine.
3. the preparation method of a kind of amphoteric ion exchange fibre according to claim 1, it is characterised in that in step (1)
Described aminated reagent is one or more in ethylenediamine, diethylenetriamine, triethylene tetramine.
4. the preparation method of a kind of amphoteric ion exchange fibre according to claim 1, it is characterised in that in step (1)
Described reflux time is 8～12h, and specified temp is 90～100 DEG C.
5. the preparation method of a kind of amphoteric ion exchange fibre according to claim 1, it is characterised in that in step (1)
Described polyacrylonitrile fibre, Organic Alcohol and aminated reagent quality ratio are 1:20～35:4～8.
6. the preparation method of a kind of amphoteric ion exchange fibre according to claim 1, it is characterised in that in step (2)
Described phosphorylation medicament is phosphorous acid；Described aldehyde salt solvent is one or more in formaldehyde, acetaldehyde and propionic aldehyde.
7. the preparation method of a kind of amphoteric ion exchange fibre according to claim 1, it is characterised in that in step (2)
Mixing time is 5～10min under described normal temperature；Described reflux time is 12～15h, and specified temp is 100～110
℃；Described concentration of hydrochloric acid is 1～5%.
8. the preparation method of a kind of amphoteric ion exchange fibre according to claim 1, it is characterised in that in step (2)
Described aminated product, phosphorylation medicament and aldehyde salt solvent mass ratio are 1:6～10:0.5～1.
9. the preparation method of a kind of amphoteric ion exchange fibre according to claim 1, it is characterised in that in step (2)
Described amphoteric ion exchange fibre is to Adsorption of Cu2+、Cr6+、Pb2+, adsorption rate is 95.74～98.14%.
10. a kind of preparation method of amphoteric ion exchange fibre according to claim 9, it is characterised in that described suction
Attached step is：Appropriate amphoteric ion exchange fibre is taken Jing after certain density HCl or NaOH immersion activation, is cleaned and is loaded chromatography
Post, heavy metal solution is adsorbed through ion-exchange fibre.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114712893A (en) * | 2022-03-26 | 2022-07-08 | 昆明理工大学 | Method for recovering gold in thiosulfate solution |
| CN115770626A (en) * | 2022-11-22 | 2023-03-10 | 河南科高辐射化工科技有限公司 | Amphoteric ion exchange fiber and preparation method and application thereof |
| CN116655812A (en) * | 2023-05-23 | 2023-08-29 | 苏州博睿特环保科技有限公司 | Lead ion adsorption material in battery recovery feed liquid and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1172870A (en) * | 1997-06-18 | 1998-02-11 | 中国科学院生态环境研究中心 | Multi-dentate ion exchange chelating fibre and its synthetic method |
| CN1363426A (en) * | 2001-01-11 | 2002-08-14 | 中国科学院生态环境研究中心 | Ion exchange fibre and its synthesizing process |
| CN1563554A (en) * | 2004-03-26 | 2005-01-12 | 钢铁研究总院 | Method for preparing chelate fiber possessing reduction function |
| CN106000480A (en) * | 2016-05-24 | 2016-10-12 | 马鞍山中创环保科技有限公司 | Ion exchange fiber used for soil restoration, and preparation method thereof |
-
2016
- 2016-12-19 CN CN201611174634.4A patent/CN106592214A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1172870A (en) * | 1997-06-18 | 1998-02-11 | 中国科学院生态环境研究中心 | Multi-dentate ion exchange chelating fibre and its synthetic method |
| CN1363426A (en) * | 2001-01-11 | 2002-08-14 | 中国科学院生态环境研究中心 | Ion exchange fibre and its synthesizing process |
| CN1563554A (en) * | 2004-03-26 | 2005-01-12 | 钢铁研究总院 | Method for preparing chelate fiber possessing reduction function |
| CN106000480A (en) * | 2016-05-24 | 2016-10-12 | 马鞍山中创环保科技有限公司 | Ion exchange fiber used for soil restoration, and preparation method thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114712893A (en) * | 2022-03-26 | 2022-07-08 | 昆明理工大学 | Method for recovering gold in thiosulfate solution |
| CN115770626A (en) * | 2022-11-22 | 2023-03-10 | 河南科高辐射化工科技有限公司 | Amphoteric ion exchange fiber and preparation method and application thereof |
| CN116655812A (en) * | 2023-05-23 | 2023-08-29 | 苏州博睿特环保科技有限公司 | Lead ion adsorption material in battery recovery feed liquid and preparation method thereof |
| CN116655812B (en) * | 2023-05-23 | 2024-08-23 | 苏州博睿特环保科技有限公司 | Lead ion adsorption material in battery recovery feed liquid and preparation method thereof |
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Application publication date: 20170426 |