CN106947244A - A kind of preparation method of nylon gel body - Google Patents
A kind of preparation method of nylon gel body Download PDFInfo
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- CN106947244A CN106947244A CN201710265997.7A CN201710265997A CN106947244A CN 106947244 A CN106947244 A CN 106947244A CN 201710265997 A CN201710265997 A CN 201710265997A CN 106947244 A CN106947244 A CN 106947244A
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- nylon
- gel body
- electroresponse
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/16—Halogen-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/16—Halogen-containing compounds
- C08K2003/162—Calcium, strontium or barium halides, e.g. calcium, strontium or barium chloride
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/16—Halogen-containing compounds
- C08K2003/166—Magnesium halide, e.g. magnesium chloride
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/16—Halogen-containing compounds
- C08K2003/168—Zinc halides
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention discloses a kind of preparation method of nylon gel body.The preparation method of intelligent gel body with electroresponse, comprises the following steps：By metal salt M+X‑With the sealing stirring mixing of 2 chlorethanols, nylon colloidal sol is obtained after adding nylon dissolving；Wherein, M+For Li+、K+、Ca2+、Zn2+、Mg2+、Ga3+In any one；X‑For Cl‑、Br‑、I‑、SCN‑In any one；By the nylon colloidal sol heated sealed, ultrasonically treated, sealing and standing is that can obtain nylon gel body at room temperature.The present invention have chosen a variety of nylon materials, be dissolved in M+X‑With in the mixed solution of 2 chlorethanols, the nylon gel body of reusable edible is obtained after heating stirring ultrasound, it shows the electrical response characteristics of sensitivity under electric field action, has widened the application of nylon gel body.
Description
Technical field
The invention belongs to intelligent gel body field, and in particular to a kind of preparation of the intelligent gel body with sensitive electroresponse
Method.
Background technology
Contain amide group on nylon molecules main chain, it is polar group, it is intermolecular to there is strong hydrogen bond action, molecule
Chain arranged regular, so nylon crystallinity is high, mechanical performance and excellent shock resistance, metal salt can occur with amide group
Hydrogen bond between complex reaction, saboteur, can effectively control the crystallinity of nylon.Nylon is polar polymer, Zhi Nengrong
In some highly polar solvents of Xie Yu, but the solvent of some low poles and the mixed solution of inorganic salts can also dissolve nylon, lead to
Polymer intelligent gelinite can be prepared by crossing this solvent, available for weaving, the research of nylon aggregation state change and phase-change material.
In addition, the current research to temperature sensitive intelligent gelinite and pH sensitiveness intelligent gel bodies is more concentrated, and to electricity
The research for responding intelligent gel body is less.It is not only cumbersome by changing temperature or pH value of solution for intelligent gel body, and
And the stimuli responsive speed of gelinite is slow.
Preparing the method for gel mainly has two kinds, and one kind is to prepare gel by micro-crystallization and hydrogen bond formation crosslinking points, separately
One kind is to prepare gel by coordinate bond formation crosslinking points.Crosslinking agent glutaraldehyde is added to prepare in gelatin by Liu's root et al. to coagulate
Glue.Liu Wei et al. is with 2- acrylamide-2-methyl propane sulfonics (AMPS) and diethylaminoethyl base ethyl ester (DEAEM) formation
Ion complex, novel ion is prepared for by free radicals copolymerization reaction and is crosslinked polyampholyte (ICPA), and is obtained
ICPA gels.Gelinite prepared by both the above method contains ionogen, destroys three-dimensional netted under electric field action
Structure, shows as Volume Changes i.e. electroresponse.And few people prepare gel using introducing ion salt by coordination mode, so
Obtained gelinite can show obvious phase in version under electric field action and quickly make electroresponse.
Under electric field action, directional migration occurs for the counter ion counterionsl gegenions in gelinite, causes osmotic pressure and polyelectrolyte to ionize
The change of state, causes the change of network structure inside gelinite, can be by the changes pair of the properties such as own vol, phase or mechanics
Electrical field stimulation makes the response of sensitivity.By the exploration to such gel material, a kind of intelligence with sensitive electroresponse is prepared
Energy gelinite, has huge researching value in the intelligent gel body such as micromechanics and sensor field.
The content of the invention
Present invention aims at provide a kind of preparation method of the intelligent gel body with sensitive electroresponse, and technique mistake
Journey is simple, easily prepared.
To reach that above-mentioned purpose is as follows using technical scheme：
Intelligent gel body with electroresponse, it is dispersed in nylon colloidal sol to have metal salt M+X-, ultrasonically treated rear standing
Obtain the intelligent gel body with electroresponse；Wherein, M+For Li+、K+、Ca2+、Zn2+、Mg2+、Ga3+In any one；X-For Cl-、
Br-、I-、SCN-In any one.
The preparation method of intelligent gel body with electroresponse, comprises the following steps：
1) by metal salt M+X-With ethylene chlorhydrin sealing stirring mixing, nylon colloidal sol is obtained after adding nylon dissolving；Wherein, M+For Li+、K+、Ca2+、Zn2+、Mg2+、Ga3+In any one；X-For Cl-、Br-、I-、SCN-In any one；
2) ultrasonically treated by the nylon colloidal sol heated sealed, sealing and standing is that can obtain nylon gel body at room temperature.
By such scheme, also including metal salt M+X-With the pretreatment of nylon；By metal salt M+X-Smash and vacuum adds
Heated drying；By nylon vacuum heat drying.
By such scheme, the nylon is nylon 6, nylon66 fiber, nylon 7, nylon 9, nylon 11, nylon 12, nylon 13, Buddhist nun
One kind in dragon 610, nylon 612, nylon 1010.
By such scheme, each component is as follows by mass percentage in step 1：
Metal salt M+X-, 0.83~3.2wt%；Ethylene chlorhydrin, 64.8~90.1wt%, nylon, 8.9~32.7wt%.
By such scheme, step 2 is heated to temperature for 40~60 DEG C.
By such scheme, step 2 sonification power is 300~600W, and the time is 3~4h.
By such scheme, 8~12h of sealing and standing obtains gelinite to step 2 at room temperature.
It is ultrasonically treated also including gained nylon gel body is reheated by such scheme, realize gel turning to colloidal sol
Become；Sealing and standing realizes colloidal sol to the transformation of gel at room temperature again；The sonification power is 300~600W, and the time is 3
~4h.
Easily hydrogen bond is formed between amide group in nylon molecules chain and cause the increase of nylon crystallinity, due to metal ion
M+Easily with amide group formation coordinate bond, hydrogen bond structure, therefore metal salt M are destroyed+X-Addition can effectively reduce nylon
Crystallinity.Ethylene chlorhydrin can play a part of being swelled as a kind of poor solvent of nylon to it, effectively increase and gold
Belong to ion M+Contact area, heating ultrasonication under can promote metal ions M+Movement so that metal ions M+It is scattered
Uniformly, so as to improve the probability of ligand complex so that metal ions M+More easily form many with amide group ligand complex
Ligand structure, forms cross-linked structure in whole system, so as to form a kind of physical gel.
Nylon gel body prepared by the present invention is under electric field action, and the counter ion counterionsl gegenions of the charged group in gelinite occur to determine
To migration, cause the change of osmotic pressure and polyelectrolyte ionized state, cause the change of network structure inside gelinite, can pass through
The response of sensitivity is made in the change of the properties such as own vol, phase or mechanics to electrical field stimulation.The present invention is by this kind of gelinite
The intelligent gel body for the electroresponse that the exploration of material is obtained, can realize quick response, in microcomputer under the application and regulation and control of electric field
The intelligent gel body such as tool and sensor field has huge researching value.
The present invention compared with prior art, has the following advantages that：
The present invention has obtained a kind of novel dissolvent (i.e. M for dissolving nylon+X-With the mixed solution of ethylene chlorhydrin), metal salt M+X-Addition effectively promote the dissolving of nylon, and the control to nylon crystallinity can be realized, nylon state of aggregation control skill
Art is more perfect.
The present invention have chosen a variety of nylon materials, be dissolved in M+X-With in the mixed solution of ethylene chlorhydrin, by heating stirring
The nylon gel body of reusable edible is obtained after ultrasound, the object that the technology of extending is used has stronger for nylon material
Universality.
The nylon gel body that the present invention is obtained shows the electrical response characteristics of sensitivity under electric field action, has widened nylon and has coagulated
The application of colloid.
Embodiment
To make those skilled in the art more fully understand technical scheme, the present invention is made further in detail below
Description.But present disclosure is not limited solely to the following examples.
Embodiment 1
A kind of novel nylon gelinite, is prepared via a method which to obtain：
(1) 0.3g metal salts CaCl is weighed first2, smashed in mortar；3g nylon 6 is weighed, after processing
CaCl2With nylon 6, in 100 DEG C of dry 12h in vacuum drying chamber.
(2) 10mL ethylene chlorhydrins are measured, the CaCl that will be dried in step (1)2Dissolve wherein, and sealing stirs
Obtain mixed solution.
(3) nylon 6 dried in step (1) is dissolved in the mixed solution in step (2), and heated sealed is to 40
DEG C, solution is transferred in homemade mould (4cm × 4cm × 1.5cm), room by the ultrasound 3h in power is 600W ultrasonic device
Warm sealing and standing 8h, you can obtain the gelinite of nylon 6.
(4) gel seal obtained in step (3) is heated to 40 DEG C, the ultrasound in power is 600W ultrasonic device
3h, can be achieved the transformation of gel-sol, sealing and standing 8h can obtain gelinite at room temperature by colloidal sol.
Embodiment 2
A kind of novel nylon gelinite, is prepared via a method which to obtain：
(1) 0.4g metal salt LiBr are weighed first, are smashed in mortar；5g nylon66 fibers are weighed, after processing
LiBr and nylon66 fiber, in 100 DEG C of dry 12h in vacuum drying chamber.
(2) 20mL ethylene chlorhydrins are measured, by the LiBr dissolvings dried in step (1) wherein, and sealing stirs
To mixed solution.
(3) nylon66 fiber dried in step (1) is dissolved in the mixed solution in step (2), and heated sealed is to 50
DEG C, solution is transferred in homemade mould (4cm × 4cm × 1.5cm) by the ultrasound 3.5h in power is 500W ultrasonic device,
Room-temperature seal stands 10h, you can obtain nylon66 fiber gelinite.
(4) gel seal obtained in step (3) is heated to 50 DEG C, the ultrasound in power is 500W ultrasonic device
3.5h, can be achieved the transformation of gel-sol, sealing and standing 10h can obtain gelinite at room temperature by colloidal sol.
Embodiment 3
A kind of novel nylon gelinite, is prepared via a method which to obtain：
(1) 0.5g metal salts MgCl is weighed first2, smashed in mortar；6g nylon 9s are weighed, after processing
MgCl2With nylon 9, in 100 DEG C of dry 12h in vacuum drying chamber.
(2) 25mL ethylene chlorhydrins are measured, the MgCl that will be dried in step (1)2Dissolve wherein, and sealing stirs
Obtain mixed solution.
(3) nylon 9 dried in step (1) is dissolved in the mixed solution in step (2), and heated sealed is to 60
DEG C, solution is transferred in homemade mould (4cm × 4cm × 1.5cm), room by the ultrasound 4h in power is 300W ultrasonic device
Warm sealing and standing 12h, you can obtain nylon gel body.
(4) gel seal obtained in step (3) is heated to 60 DEG C, the ultrasound in power is 300W ultrasonic device
4h, can be achieved the transformation of gel-sol, sealing and standing 12h can obtain gelinite at room temperature by colloidal sol.
Embodiment 4
A kind of novel nylon gelinite, is prepared via a method which to obtain：
(1) 0.3g metal salts GaCl is weighed first3, smashed in mortar；6g nylon 612s are weighed, after processing
GaCl3With nylon 612, in 100 DEG C of dry 12h in vacuum drying chamber.
(2) 25mL ethylene chlorhydrins are measured, the GaCl that will be dried in step (1)3Dissolve wherein, and sealing stirs
Obtain mixed solution.
(3) nylon 612 dried in step (1) is dissolved in the mixed solution in step (2), and heated sealed is to 40
DEG C, solution is transferred in homemade mould (4cm × 4cm × 1.5cm), room by the ultrasound 4h in power is 400W ultrasonic device
Warm sealing and standing 11h, you can obtain nylon gel body.
(4) gel seal obtained in step (3) is heated to 40 DEG C, the ultrasound in power is 400W ultrasonic device
4h, can be achieved the transformation of gel-sol, sealing and standing 11h can obtain gelinite at room temperature by colloidal sol.
Embodiment 5
A kind of novel nylon gelinite, is prepared via a method which to obtain：
(1) 0.5g metal salts ZnI is weighed first2, smashed in mortar；4g nylon is weighed, by the ZnCl after processing2
With nylon 1010, in 100 DEG C of dry 12h in vacuum drying chamber.
(2) 15mL ethylene chlorhydrins are measured, the ZnI that will be dried in step (1)2Dissolve wherein, and sealing stirs
To mixed solution.
(3) nylon dried in step (1) is dissolved in the mixed solution in step (2), and heated sealed is to 60 DEG C,
The ultrasound 4h in power is 300W ultrasonic device, solution is transferred in homemade mould (4cm × 4cm × 1.5cm), room temperature is close
Envelope stands 12h, you can obtain nylon gel body.
(4) gel seal obtained in step (3) is heated to 60 DEG C, the ultrasound in power is 300W ultrasonic device
4h, can be achieved the transformation of gel-sol, sealing and standing 8h can obtain gelinite at room temperature by colloidal sol.
Embodiment 6
A kind of novel nylon gelinite, is prepared via a method which to obtain：
(1) 0.5g metal salt KSCN are weighed first, are smashed in mortar；4g NYLON610s are weighed, after processing
KSCN and NYLON610, in 100 DEG C of dry 12h in vacuum drying chamber.
(2) 25mL ethylene chlorhydrins are measured, by the KSCN dissolvings dried in step (1) wherein, and sealing stirs
To mixed solution.
(3) nylon dried in step (1) is dissolved in the mixed solution in step (2), and heated sealed is to 50 DEG C,
The ultrasound 4h in power is 400W ultrasonic device, solution is transferred in homemade mould (4cm × 4cm × 1.5cm), room temperature is close
Envelope stands 10h, you can obtain nylon gel body.
(4) gel seal obtained in step (3) is heated to 50 DEG C, the ultrasound in power is 400W ultrasonic device
4h, can be achieved the transformation of gel-sol, sealing and standing 10h can obtain gelinite at room temperature by colloidal sol.
Claims (9)
1. the intelligent gel body with electroresponse, it is characterised in that dispersed in nylon colloidal sol to have at metal salt M+X-, ultrasound
Stood after reason and obtain the intelligent gel body with electroresponse；Wherein, M+For Li+、K+、Ca2+、Zn2+、Mg2+、Ga3+In any one；
X-For Cl-、Br-、I-、SCN-In any one.
2. the preparation method of the intelligent gel body with electroresponse described in claim 1, it is characterised in that comprise the following steps：
1) by metal salt M+X-With ethylene chlorhydrin sealing stirring mixing, nylon colloidal sol is obtained after adding nylon dissolving；
2) ultrasonically treated by the nylon colloidal sol heated sealed, sealing and standing is that can obtain nylon gel body at room temperature.
3. there is the preparation method of the intelligent gel body of electroresponse as claimed in claim 1, it is characterised in that also including metal
Salt M+X-With the pretreatment of nylon；By metal salt M+X-Smash and vacuum and heating drying；By nylon vacuum heat drying.
4. the preparation method of the intelligent gel body with electroresponse as claimed in claim 1, it is characterised in that the nylon is
One in nylon 6, nylon66 fiber, nylon 7, nylon 9, nylon 11, nylon 12, nylon 13, NYLON610, nylon 612, nylon 1010
Kind.
5. there is the preparation method of the intelligent gel body of electroresponse as claimed in claim 1, it is characterised in that each group in step 1
Divide as follows by mass percentage：
Metal salt M+X-, 0.83~3.2wt%；Ethylene chlorhydrin, 64.8~90.1wt%, nylon, 8.9~32.7wt%.
6. there is the preparation method of the intelligent gel body of electroresponse as claimed in claim 1, it is characterised in that step 2 is heated to
Temperature is 40~60 DEG C.
7. there is the preparation method of the intelligent gel body of electroresponse as claimed in claim 1, it is characterised in that at step 2 ultrasound
Reason power is 300~600W, and the time is 3~4h.
8. there is the preparation method of the intelligent gel body of electroresponse as claimed in claim 1, it is characterised in that step 2 is at room temperature
8~12h of sealing and standing obtains gelinite.
9. the preparation method of the intelligent gel body with electroresponse as claimed in claim 1, it is characterised in that also including by institute
Nylon gel body is obtained to reheat, it is ultrasonically treated, realize gel to the transformation of colloidal sol；Sealing and standing realizes colloidal sol at room temperature again
To the transformation of gel；The sonification power is 300~600W, and the time is 3~4h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710265997.7A CN106947244B (en) | 2017-04-21 | 2017-04-21 | A kind of preparation method of nylon gel body |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710265997.7A CN106947244B (en) | 2017-04-21 | 2017-04-21 | A kind of preparation method of nylon gel body |
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| CN106947244A true CN106947244A (en) | 2017-07-14 |
| CN106947244B CN106947244B (en) | 2019-06-28 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107501594A (en) * | 2017-08-23 | 2017-12-22 | 成都新柯力化工科技有限公司 | A kind of method with gel state nylon blown foams |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102807761A (en) * | 2011-06-02 | 2012-12-05 | 张晓� | Gel and manufacturing process thereof |
| WO2014095427A1 (en) * | 2012-12-20 | 2014-06-26 | L'oreal | Water-insoluble cyclodextrin polycondensate; uses as a capturing agent |
| CN105601955A (en) * | 2016-02-03 | 2016-05-25 | 合肥工业大学 | Electric-stimulation fluorescence-response aquagel |
-
2017
- 2017-04-21 CN CN201710265997.7A patent/CN106947244B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102807761A (en) * | 2011-06-02 | 2012-12-05 | 张晓� | Gel and manufacturing process thereof |
| WO2014095427A1 (en) * | 2012-12-20 | 2014-06-26 | L'oreal | Water-insoluble cyclodextrin polycondensate; uses as a capturing agent |
| CN105601955A (en) * | 2016-02-03 | 2016-05-25 | 合肥工业大学 | Electric-stimulation fluorescence-response aquagel |
Non-Patent Citations (1)
| Title |
|---|
| 马前: "智能聚合物凝胶的研究进展", 《广东化工》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107501594A (en) * | 2017-08-23 | 2017-12-22 | 成都新柯力化工科技有限公司 | A kind of method with gel state nylon blown foams |
| CN107501594B (en) * | 2017-08-23 | 2021-05-25 | 长沙争明新材料有限公司 | Method for foaming foamed plastic by using gel state nylon |
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| CN106947244B (en) | 2019-06-28 |
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