CN107652379A - A kind of compound cellulose - Google Patents

A kind of compound cellulose Download PDF

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Publication number
CN107652379A
CN107652379A CN201711108790.5A CN201711108790A CN107652379A CN 107652379 A CN107652379 A CN 107652379A CN 201711108790 A CN201711108790 A CN 201711108790A CN 107652379 A CN107652379 A CN 107652379A
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minutes
monomer
hydrochloric acid
soaked
stirred
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丁伟
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Chengdu Aung Biotechnology Co Ltd
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Chengdu Aung Biotechnology Co Ltd
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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
    • C08F120/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
    • C08F120/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F120/52—Amides or imides
    • C08F120/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
    • 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
    • C08F2/00—Processes of polymerisation
    • C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/26—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a solid phase from a macromolecular composition or article, e.g. leaching out
    • 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
    • C08K3/34—Silicon-containing compounds
    • C08K3/346—Clay
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2201/00—Foams characterised by the foaming process
    • C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
    • C08J2201/044—Elimination of an inorganic solid phase
    • C08J2201/0444—Salts
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
    • C08J2333/24—Homopolymers or copolymers of amides or imides

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Dispersion Chemistry (AREA)
  • Polymerisation Methods In General (AREA)
  • Medicinal Preparation (AREA)

Abstract

The invention discloses a kind of preparation method of fast temperature response nano-composite fiber element, comprise the following steps:Monomer and inorganic clay are dissolved in deionized water, stirred 30 120 minutes in an inert atmosphere;Pore former is added, is stirred 5 30 minutes in an inert atmosphere;Initiator and catalyst are added, is stirred 5 10 minutes in an inert atmosphere:Raolical polymerizable is carried out at a temperature of 0 30 DEG C 10 30 hours;Reaction product is soaked in 0.1 mol/L hydrochloric acid, was changed hydrochloric acid solution at interval of 58 hours, is continued 48 72 hours, then product is soaked in deionized water repeatedly, until removing residual hydrochloric acid, described compound cellulose is made.The beneficial effects of the invention are as follows:Not only preparation technology is simple, and the gel prepared has the faster speed of response and good mechanical property simultaneously.

Description

A kind of compound cellulose
Technical field
It is nano combined more particularly to a kind of fast temperature response the present invention relates to a kind of preparation method of compound cellulose The preparation method of cellulose.
Background technology
Intelligent fiber element is current most noticeable a kind of cellulose.The poly- isopropylacrylic acid amine of N mono- (abbreviation PN works With) cellulose be this gellike a Typical Representative.PNIPA celluloses exist volume phase transition temperature (VPTT, it is attached at 32 DEG C Closely), when environment temperature is less than VPTT, PNI is with cellulose water absorption and swelling;When environment temperature is higher than VPTT, PNI is with cellulose Acutely shrink and dehydration.Based on PN works with this thermally sensitive property of cellulose, it oneself be applied to the control of medicine and release Put, the field such as enzyme immobilizatio and cyclic absorption agent.
But traditional PNIPA celluloses exist bad mechanical property, it is frangible, can not stretch, the speed of response is slow and the transparency The shortcomings of poor, it greatly limit its application in some aspects, such as chemical sensor, artificial-muscle and chemical valve field.Pass In the PNIPA cellulosic electrodes of system often with such as N, N, one methylene bisacrylamide the phthalein amine (BIS) of the compound containing diolefin for crosslinking Agent, copolymerization is mixed with monomer by crosslinking agent, forms tridimensional network.Many studies have shown that the disadvantages mentioned above of cellulose is exactly Carried out at random with chemical crosslink reaction in radical polymerization, a large amount of crosslinking points disorder distributions it is relevant.
Nearest Haragachi etc. (MaeromoleeuleS, 2002,35:10162 1 10171, Macromol.Chem. Phys, 2005,206:1540) 1 530 one replace chemical cross-linking agent with inorganic clay, PM is prepared by in-situ polymerization intercalated The nano-composite fiber element of PA/ clays.This kind of cellulose has good mechanical property, can bend, knot, elongation at break Up to more than 1000%, but its speed of response is also slow, reaches the requirement of quick response far away.
Around the speed of response for the traditional PNIPA celluloses for improving chemical crosslinking, the method used at present mainly has following It is several:(l) micron or nano level PNIPA cellulose balls are prepared by the method for emulsion polymerization.Due to cellulose response when Between it is square directly proportional to the linear dimension of cellulose, the size for reducing cellulose will significantly improve the speed of response of cellulose; (2) comb-type structure PNIPA celluloses are prepared.Such as YoshidaR etc. (Nature, 1995,374:242) 240 1 have synthesized combed PNIPA celluloses are grafted, when the temperature increases, the hydrophobic effect being grafted on PNIPA chains produces multiple hydrophobic cores quickly, greatly Crosslinking chain aggregation is enhanced, so that the speed of response of gel greatly improves.(3) using pore former synthesis macropore and super hole PNIPA celluloses, the implementing process of this method are the simplest.Such as Liu Xiao China etc. (CN 1 328063A, CN 1328067A) Different-grain diameter CaCO is added in the polymerization3Particle, CaCO is removed through salt acid rinse after gel-forming3Particle, obtain porous The PNIPA celluloses of structure;Chen Zhaowei (Journal of Functional Polymers, 2004,17 (l):50) etc. 46 1 using silica gel as pore former system For porous PNIPA celluloses;(J.Polym.SCi, the PartA such as zhuo:Polym.Chem., 2003,41:152 1 is 159) sharp The PNIPA celluloses of quick response are prepared for by the use of polyethylene glycol as pore former;(the Journal of Polymer such as Wu Scienee, PartA:PolymerChemi stry, 1992,30:2129) 2121 1 are used as pore former system by the use of through propyl cellulose Standby macropore PNIPA celluloses.Due to adding pore former in the course of the polymerization process, make in the gel network to be formed exist be mutually communicated hole Hole structure, the absorption of solvent or is released through the convection current in hole to produce, therefore substantially increases its speed of response.
It must be noted that be all to employ N, N above by pore former synthesis quick response PN work PA celluloses are added, The chemical cross-linking agents such as one methylene bisacrylamide acid amide (BIS) formed three dimensional gell network, its poor mechanical property, low intensity, easily It is broken, it is difficult to meet the needs of practical application.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of preparation side of fast temperature response nano-composite fiber element Method, to make up the deficiencies in the prior art or defect, meet the demands of production and living.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is:A kind of fast temperature response nanometer is answered The preparation method of condensating fiber element, comprises the following steps:
(1) monomer and inorganic clay are dissolved in deionized water, the mass percent concentration of monomer is 5 one 15%, inorganic clay Quality is 10 one the 60% of monomer mass, is stirred 30 1 120 minutes in an inert atmosphere;Described monomer is the isopropyl propylene of N mono- Phthalein amine;
(2) pore former is added in above-mentioned solution, is stirred 5 one 30 minutes in an inert atmosphere;The quality of pore former is monomer matter 10 one the 70% of amount;
(3) initiator and catalyst are added, is stirred 5 one 10 minutes in an inert atmosphere;Wherein, the addition of initiator is monomer 0.5 one the 3% of quality, the addition of catalyst are 0.2 one the 4% of monomer mass;
(4) above-mentioned solution is carried out to Raolical polymerizable at a temperature of 0 one 30 DEG C 10 1 30 hours;
(5) reaction product is soaked in 0.lmol/L hydrochloric acid, changed hydrochloric acid solution at interval of 5 one 8 hours, it is small to continue 48 1 72 When, until all being removed by electron microscope observation pore former, then product is soaked in deionized water repeatedly, until removing Residual hydrochloric acid, described compound cellulose is made.
As preferable technical scheme:Described inorganic clay is the clay Laponite of synthesis, is a kind of trioctahedron Montmorillonite.
Described pore former is one kind in calcium carbonate, sodium carbonate or sodium acid carbonate.
Described initiator is Ammonium Persulfate 98.5 or potassium peroxydisulfate.
Described catalyst is N, N, N ', the tetramethylethylenediamines of N ' one or sodium hydrogensulfite.
The present invention principle be:With the isopropyl propylene phthalein amine (NIPA) of N mono- for raw material monomer, with inorganic clay Laponite Chemical cross-linking agent is substituted, with calcium carbonate etc. for pore former, fast temperature response is prepared by the method for in-situ polymerization, drilling in situ Gel.Experiment shows that clay is stripped into the lamella of nano-scale, is dispersed in gel network (see accompanying drawing 1), plays the part of The role of crosslinking agent, is formed and the traditional chemical crosslinking PA celluloses of PN 1 (CN1328063A, the CN1328067A such as Liu Xiaohua) Different physical crosslinking celluloses.This cellulose is due to PN works PA molecular chain lengths between clay layer and has good flexibility, By very big deformation can be produced during external force without destroyed, thus high tensile strength and extraordinary toughness are shown, can To stretch, bend and knot in (see accompanying drawing 2).Further, since pore former is with the addition of in polymerization, and the pore-forming after polymerizeing in gel Agent is washed out, and the pore space structure to interpenetrate is left in gel network, is advantageous to the diffusion of solvent, therefore is substantially increased solidifying The speed of response of glue.Its speed of response can be adjusted by dosage of the dosage of pore former, particle size and inorganic clay etc..
The beneficial effects of the invention are as follows:Not only preparation technology is simple, and the gel prepared has faster response simultaneously Speed and good mechanical property.
Brief description of the drawings
The TEM photos of the PNIPA/ clay nano compound celluloses of Fig. 1 fast temperature responses
The photo of Fig. 2 fast temperature response celluloses.
Embodiment
The present invention is further elaborated with reference to specific embodiment.
Embodiment 1
19 monomer NIPA, 0.1989 inorganic clay Laponite are dissolved in 8ml deionized waters, lead to nitrogen, stirring 60 minutes, Then 0.29 sodium carbonate is added, leads to nitrogen, stirring 10 minutes.Then add 0.019 Ammonium Persulfate 98.5 and 8 pL catalyst ns, N, N ', the N tetramethylethylenediamine of ' one, continue logical nitrogen 5 minutes after well mixed, then pour into a diameter of 18Inln test tube rapidly In, sealing be placed in 20 DEG C of water-baths react 20h after, reactant take out segment, be soaked in 0.lmol/L hydrochloric acid solutions, immersion 2 My god, changed hydrochloric acid solution once at interval of 8 hours.Soaked 2 days, refreshed the water periodically with deionized water again, that is, obtain elastic good contraction The fast cellulose of speed.
Using (the ColloidPolymSei such as Zhang (2005) 283:431 1 438) method disclosed in document detected, Percentage of water loss is 98.5% to the cellulose obtained in 10 minutes more than its phase transition temperature, has just reached dehydration balance within 30 minutes. Gel has good toughness, elongation at break 652%.
Embodiment 2
19 monomer NlpA, 0.339 inorganic clay Laponite are dissolved in 8ml deionized waters, lead to nitrogen, stirring 80 minutes, so After add 0.29 sodium carbonate, lead to nitrogen, stirring 10 minutes.Then add 0.029 Ammonium Persulfate 98.5 and 8 uL catalyst ns, N, N ', The tetramethylethylenediamines of N ' one, continue logical nitrogen 5 minutes after well mixed, then pour into rapidly in a diameter of 18mm test tube, be close It is sealed and placed in after reacting 20h in 20 DEG C of water-baths, reactant takes out segment, is soaked in 0.lmol/L hydrochloric acid solutions, immersion 2 days, often Change hydrochloric acid solution once within 8 hours in interval.Soaked 2 days, refreshed the water periodically with deionized water again, that is, it is fast to obtain the good contraction rate of elasticity Cellulose.
Using (the Colloid Polym such as Zhang Sci (2005) 283:431 1 438) method disclosed in document examined Survey, the cellulose obtained is more than its phase transition temperature, percentage of water loss is 93.3% in 10 minutes.Gel has good toughness, breaks Elongation is split for 585%.
Embodiment 3
1g monomers NIPA, 0.339 inorganic clay LaPonite are dissolved in 8ml deionized waters, lead to nitrogen, stirring 60 minutes, so After add 0.69 sodium carbonate, lead to nitrogen, stirring 10 minutes.Then add 0.019 potassium peroxydisulfate and 10uL catalyst ns, N, N, N One tetramethylethylenediamine, continues logical nitrogen 5 minutes after well mixed, then pour into rapidly in a diameter of 18mm test tube, seal It is placed in 20 DEG C of water-baths after reacting 20h, reactant takes out segment, is soaked in 0.lmol/L hydrochloric acid solutions, soaks 2 days, every Hydrochloric acid solution was changed every 8 hours once.Soaked 2 days, refreshed the water periodically with deionized water again, that is, it is fast to obtain elasticity good contraction rate Cellulose.
Using (the Colloid Polym such as Zhang Sci (2005) 283:431 1 438) method disclosed in document examined Survey, the cellulose obtained is more than its phase transition temperature, percentage of water loss is 97.5% in 10 minutes.Gel has good toughness, breaks Elongation is split for 623%.
Embodiment 4
19 monomer NI teams, 0.529 inorganic clay Laponite are dissolved in 8ml deionized waters, lead to nitrogen, stirring 90 minutes, so After add 0.79 sodium carbonate, lead to nitrogen, stirring 10 minutes.Then add 0.019 Ammonium Persulfate 98.5 and 8uL catalyst ns, N, N ', The tetramethylethylenediamines of N ' one, continue logical nitrogen 5 minutes after well mixed, then pour into rapidly in a diameter of 18mm test tube, be close It is sealed and placed in after reacting 25h in 20 DEG C of water-baths, reactant takes out segment, is soaked in 0.1m01/L hydrochloric acid solutions, immersion 2 days, often Change hydrochloric acid solution once within 8 hours in interval.Soaked 2 days, refreshed the water periodically with deionized water again, that is, it is fast to obtain the good contraction rate of elasticity Cellulose.
Using (the Colloid Polym such as Zhang Sci (2005) 283:431 1 438) method disclosed in document examined Survey, the cellulose obtained is more than its phase transition temperature, percentage of water loss is 92.4% in 10 minutes.Gel has good toughness, breaks Elongation is split for 524%.
Embodiment 5
0.59 monomer NIPA, 0.1 989 inorganic clay Lponite are dissolved in 5ml deionized waters, lead to nitrogen, 60 points of stirring Clock, 0.29 sodium carbonate is then added, lead to nitrogen, stirring 10 minutes.Then add 0.039 Ammonium Persulfate 98.5 and 16 pL catalyst N, N, N ', the tetramethylethylenediamines of N ' one continue logical nitrogen 5 minutes after well mixed, then pour into a diameter of 18mm examination rapidly Guan Zhong, sealing are placed in 20 DEG C of water-baths after reaction 20h, and reactant takes out segment, is soaked in 0.1mol/L hydrochloric acid solutions, are soaked 2 days, hydrochloric acid solution was changed once at interval of 8 hours.Soaked 2 days, refreshed the water periodically with deionized water again, that is, obtain elastic good contraction The fast cellulose of speed.
Using (the Colloid Polym such as Zhang Sei (2005) 283:431 1 438) method disclosed in document examined Survey, the cellulose obtained is more than its phase transition temperature, percentage of water loss is 94.6% in 10 minutes.Gel has good toughness, breaks Elongation is split for 617%.
Embodiment 6
Lg monomers NIPA, 0.339 inorganic clay LaPonite are dissolved in 8ml deionized waters, lead to nitrogen, stirring 60 minutes, so The calcium carbonate 0.29 that particle diameter is 3000 mesh is added afterwards, leads to nitrogen, stirring 10 minutes.Then add 0.019 Ammonium Persulfate 98.5 and 8 PL catalyst ns, N, N, the N tetramethylethylenediamine of ' one, continue logical nitrogen 5 minutes after well mixed, then pour into rapidly a diameter of In 18mm test tube, sealing be placed in 20 DEG C of water-baths react 20h after, reactant take out segment, it is molten to be soaked in 0.1mol/L hydrochloric acid In liquid, soak 2 days, hydrochloric acid solution was changed once at interval of 8 hours.Soaked 2 days with deionized water again, refresh the water periodically, that is, obtain The fast cellulose of the good contraction rate of elasticity.
Using (the ColloldPolyms such as Zhang.i(2005)283:431 1 438) method disclosed in document detected, Percentage of water loss is 92% to the cellulose obtained in 30 minutes more than its phase transition temperature.Gel has good toughness, extension at break Rate is 952%.
Embodiment 7
19 monomer NlpA, 0.339 inorganic clay LaPonite are dissolved in 5ml deionized waters, lead to nitrogen, stirring 60 minutes, so The calcium carbonate 0.69 that particle diameter is 3000 mesh is added afterwards, leads to nitrogen, stirring 10 minutes.Then add 0.0 19 Ammonium Persulfate 98.5s and 8 UL catalyst ns, N, N, the tetramethylethylenediamines of N mono- continue logical nitrogen 5 minutes, then poured into rapidly a diameter of after well mixed In 18mm test tube, sealing be placed in 20 DEG C of water-baths react 20h after, reactant take out segment, it is molten to be soaked in 0.1mol/L hydrochloric acid In liquid, soak 2 days, hydrochloric acid solution was changed once at interval of 8 hours.Soaked 2 days with deionized water again, refresh the water periodically, that is, obtain The fast cellulose of the good contraction rate of elasticity.
Using (the Colloid Polym such as Zhang Sei (2005) 283:431 1 438) method disclosed in document examined Survey, percentage of water loss is 94.4% to the cellulose obtained in 30 minutes more than its phase transition temperature.Gel has good toughness, breaks Elongation is split for 892%.
Embodiment 8
1 .49 monomers NlPA, 0.289 inorganic clay Laponite are dissolved in sml deionized waters, lead to nitrogen, 60 points of stirring Clock, the calcium carbonate 0.69 that particle diameter is 800 mesh is then added, lead to nitrogen, stirring 10 minutes.Then add 0.039 Ammonium Persulfate 98.5 With 12uL catalyst ns, N, N ', the tetramethylethylenediamines of N mono- continue logical nitrogen 5 minutes after well mixed, then pour into diameter rapidly For in 18Inln test tube, sealing be placed in 20 DEG C of water-baths react 20h after, reactant take out segment, be soaked in 0.lmol/L salt In acid solution, soak 2 days, hydrochloric acid solution was changed once at interval of 8 hours.Soaked 2 days, refreshed the water periodically, i.e., with deionized water again Obtain the fast cellulose of the good contraction rate of elasticity.
Using (the Colloid Polym such as Zhang Sei (2005) 283:431 1 438) method disclosed in document examined Survey, percentage of water loss is 94.5% to the cellulose obtained in 30 minutes more than its phase transition temperature, and gel has good toughness, is broken Elongation is split for 814%.
Embodiment 9
1.59 monomer N works PA, 0.6629 inorganic clay Laponite are dissolved in 8ml deionized waters, lead to nitrogen, 60 points of stirring Clock, the calcium carbonate 0.49 that particle diameter is 800 mesh is then added, lead to nitrogen, stirring 10 minutes.Then add 0.019 potassium peroxydisulfate With 8 pL catalyst ns, N, N, the tetramethylethylenediamines of N mono- continue logical nitrogen 5 minutes after well mixed, then pour into diameter rapidly For in 18mm test tube, sealing be placed in 20 DEG C of water-baths react 20h after, reactant take out segment, be soaked in 0.1mol/L hydrochloric acid In solution, soak 2 days, hydrochloric acid solution was changed once at interval of 8 hours.Soaked 2 days with deionized water again, refresh the water periodically, produce The cellulose fast to the good contraction rate of elasticity.
Using (the Colloid such as Zhang PolymS.i(2005)283:431 1 438) method disclosed in document examined Survey, the cellulose obtained is more than its phase transition temperature, percentage of water loss is 87% in 30 minutes.Elongation at break is 652%.
Embodiment 10
19 monomer NIPA, 0.5949 inorganic clay Laponite are dissolved in 8ml deionized waters, lead to nitrogen, stirring 60 minutes, Then the sodium acid carbonate 0.49 that particle diameter is 800 mesh is added, leads to nitrogen, stirring 10 minutes.Then add 0.019 Ammonium Persulfate 98.5 and 8uL catalyst ns, N, N, the N tetramethylethylenediamine of ' one, continue logical nitrogen 5 minutes after well mixed, then pour into rapidly a diameter of In 18mm test tube, sealing be placed in 20 DEG C of water-baths react 20h after, reactant take out segment, it is molten to be soaked in 0.lmol/L hydrochloric acid In liquid, soak 2 days, hydrochloric acid solution was changed once at interval of 8 hours.Soaked 2 days with deionized water again, refresh the water periodically, that is, obtain The fast cellulose of the good contraction rate of elasticity.
Using (the Colloid Polym such as Zhang Sci (2005) 283:431 1 438) method disclosed in document examined Survey, the cellulose obtained is more than its phase transition temperature, percentage of water loss is 92.5% in 10 minutes.Elongation at break is 463%.

Claims (5)

1. a kind of preparation method of fast temperature response nano-composite fiber element, it is characterised in that comprise the following steps:
(l) monomer and inorganic clay are dissolved in deionized water, the mass percent concentration of monomer is 5 one 15%, inorganic clay Quality is 10 one the 60% of monomer mass, is stirred 30 1 120 minutes in an inert atmosphere;Described monomer is the isopropyl propylene of N mono- Phthalein amine;
(2) pore former is added in above-mentioned solution, is stirred 5 one 30 minutes in an inert atmosphere;The quality of pore former is monomer matter 10 one the 70% of amount;
(3) initiator and catalyst are added, is stirred 5 one 10 minutes in an inert atmosphere;Wherein, the addition of initiator is monomer 0.5 one the 3% of quality, the addition of catalyst are 0.2 one the 4% of monomer mass;
(4) above-mentioned solution is carried out to Raolical polymerizable at a temperature of mono- 30 DEG C of O 10 1 30 hours;
(5) reaction product is soaked in 0.lmol/L hydrochloric acid, changed hydrochloric acid solution at interval of 5 one 8 hours, it is small to continue 48 1 72 When, then product is soaked in deionized water repeatedly, residual hydrochloric acid is removed, described compound cellulose is made.
2. according to the method for claim 1, it is characterised in that described inorganic clay is the clay Laponite of synthesis, It is a kind of trioctaedric smectite.
3. according to the method for claim 1, it is characterised in that described pore former is calcium carbonate, sodium carbonate or bicarbonate One kind in sodium.
4. according to the method for claim 1, it is characterised in that described initiator is Ammonium Persulfate 98.5 or potassium peroxydisulfate.
5. according to the method described in claim 1, it is characterised in that described catalyst is N, N, N ', N tetramethylethylenediamines or Asia Niter cake.
CN201711108790.5A 2017-11-11 2017-11-11 A kind of compound cellulose Pending CN107652379A (en)

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