CN106675527A - Nanocellulose composite hydrogel based phase change material as well as preparation method and application thereof - Google Patents
Nanocellulose composite hydrogel based phase change material as well as preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a nanocellulose composite hydrogel based phase change material as well as a preparation method and an application thereof. The material comprises, in parts by weight, 1-10 parts of a nanocellulose composite hydrogel base material, 85-98 parts of a phase-change main energy storage agent and 1-5 parts of a nucleating agent. The nanocellulose composite hydrogel based phase change material does not have supercooling or phase separation phenomenon and has good recycling property and long service life. The preparation method of the nanocellulose composite hydrogel based phase change material adopts a simple process, and the phase change material with stable performance is synthesized by sufficiently utilizing bond energy among all components.
Description
Technical field
The invention belongs to field of packaging material, it is related to a kind of packaging material suitable for cold chain transportation, specially one
Plant nano-cellulose composite aquogel based phase-change material and its preparation method and application.
Background technology
As the cold chain transportation of continuous progress scientific and technological in recent years, fruit-vegetable food and pharmaceutical products has obtained preferably sending out
Exhibition.In transportation, to make product keep at a certain temperature, just having to take special measure, phase-change material without
It is suspected to be best selection.Phase-change material can be such that product maintains within a certain period of time under certain cryogenic conditions, so as to extend product
Shelf life, reduce loss rate of the product in transportation.Phase-change material need to have suitable phase transition temperature, and larger phase transformation is dived
Heat, longer service life etc. are meeting use requirement.
At present, conventional phase-change material is broadly divided into inorganic phase-changing material, organic phase change material and composite phase-change material
Three kinds of material.Wherein, inorganic phase-changing material is based on crystalline hydrate salt, with raw material sources are extensive, cheap, latent heat of phase change is big
Advantage, but generally existing is supercool and phenomenon of phase separation；Organic phase change material mainly have paraffin, organic salt, polyalcohols and
Fatty acid etc., there's almost no supercool and phenomenon of phase separation, but its heat conductivity is poor, cause phase-change material in phase transition process
Middle cold-storage/accumulation of heat speed is low, and service efficiency is not high；Composite phase-change material be people to improve the performance of single phase-change material and
A kind of novel phase-change material of invention, it combines the advantage of single phase-change material, has single phase-change material not have feature again,
Make phase-change material that there is better performance, meet use requirement.
Nano-cellulose, is the nano material with certain draw ratio of a diameter of nano-scale.Due to nano-cellulose
The mechanical property and architectural feature of itself, is used frequently as the mechanics enhancing phase for being macromolecular material.Because it has height hydrophilic
The advantages of property, high-specific surface area, high intensity, in recent years, favored by people.But nano-grade matter is easily reunited, institute
Should prevent in the preparation process of composite and eliminate the impact of the reunion to composite property of nano-cellulose.
In recent years, going deep into nano materials research, people attempt research and nano-cellulose are added to phase transformation material
Improving the performance of phase-change material in material.
The content of the invention
The technical problem of solution：In in order to overcome prior art phase-change material supercool and be separated, reusing not
The shorter defect of good, service life, obtains a kind of with low cost, safe and reliable, almost no supercool and phenomenon of phase separation, repetition
Usability is preferable, the longer phase-change material of service life, the invention provides a kind of nano-cellulose compound water congealing gum base phase transformation
Material and its preparation method and application.
Technical scheme：A kind of nano-cellulose composite aquogel based phase-change material, by weight, the material includes receiving
1~10 part of rice cellulose compound water congealing gum base materials, 85~98 parts of the main energy storage agent of phase transformation, 1~5 part of nucleator；Wherein nanofiber
Plain compound water congealing gum base materials include nano-cellulose, Carboxymethyl cellulose sodium, aqueous slkali, monomer, initiator, cross-linking agent, extraction
Agent, deionized water, the ratio of each component is 0.5~5mg:1~5g:5~30mL:6~7.2g:0.05~0.15g:40~60mg:
200~250mL:90~100mL.
Preferably, the aqueous slkali is the sodium hydroxide solution that molar concentration is 0.5~2mol/L, monomer be acrylic acid and
Acrylamide, acrylic acid is 2~6 with the weight ratio of acrylamide:1, initiator is Ammonium persulfate., and cross-linking agent is N, N '-methylene
Base bisacrylamide, extractant is acetone.
Preferably, the main energy storage agent of the phase transformation is Sodium Chloride, ammonium chloride, calcium chloride, the chlorination of mass concentration 5%~15%
At least one in potassium solution.
Preferably, the nucleator is at least one in sodium tetraborate, kieselguhr, barium fluoride.
The preparation method of nano-cellulose composite aquogel based phase-change material, comprises the steps of：
(1) nano-cellulose compound water congealing gum base materials are prepared
A, Carboxymethyl cellulose sodium powder is scattered in deionized water, and under 50~60 DEG C of water bath conditions, uses nitrogen
Air in purging discharge system；
B, into system initiator is added, 30~40 DEG C are down to after being sufficiently stirred for, add monomer, nano-cellulose and crosslinking
Agent, system is warming up to 65~75 DEG C, fully reacts in nitrogen atmosphere；
C, the product after step b polyreaction is moved in room temperature environment, stood to abundant gelation；
Deca aqueous slkali in d, the gel obtained to step c, with excessive deionized water wash after abundant deprotonation, extremely
The pH value of cleaning mixture is 6~8；
Under e, room temperature, using extractant process Jing step d process after gel, take its precipitate be placed in baking oven be dried extremely
Constant weight, crushes, sieves, and collects the gel of 60~100 mesh；
(2) nano-cellulose composite aquogel based phase-change material is prepared
The nano-cellulose compound water congealing gum base materials that step (1) is prepared are sufficiently stirred for mixing with the main energy storage agent of phase transformation
It is even, nucleator is added, stir prepared.
Preferably, aqueous slkali and the mixed proportion of gel are 5~30mL in step d:80~100g.
The nano-cellulose composite aquogel based phase-change material is in fruit-vegetable food or the packaging of pharmaceutical products cold chain transportation
Application in material.
The principle of nano-cellulose composite aquogel based phase-change material of the present invention work is：Nano-cellulose table
There are substantial amounts of active group, such as-OH ,-COOH in face, appropriate nano-cellulose is added to into cellulose as Nano filling and is connect
In the hydrogel of branch acrylic acid and acrylamide, nano-cellulose can form hydrogen with the macromolecule in cellulose aquagel system
Key is acted on, so as to play a part of to build gel three-dimensional network structure.This three-dimensional net structure can make the crystal point of bulk
Little system is divided into, so as to prevent sedimentation of the main energy storage agent of chloride inorganic salt in phase transition process, so as to improve phase point
From phenomenon, according to heterogeneous nucleation mechanism, nucleator is added in phase-change material, effectively improve the supercool existing of phase-change material
As.
Nano-cellulose compound water congealing gum base materials are used as a kind of polyelectrolyte, the long chain macromolecule with ionogen.
When nano-cellulose composite aquogel substrate applications, in phase-change material, these ionogens can make nano-cellulose and master
Energy storage agent and nucleator well it is compatible together, and due to the Interaction Force of electronics, phase-change material is followed through heat
After ring, good performance is still kept, reusing is good.
Nano-cellulose has high intensity, using nano-cellulose composite aquogel as phase-change material base material, it is high
The performance of intensity causes the base material of phase-change material to be not easily susceptible to pressure and cave in, so as to extend the service life of base material, and then
Extend the life-span of phase-change material.
Beneficial effect：(1) nano-cellulose composite aquogel based phase-change material of the present invention is existing without supercool and phase separation
As reusing is good, long service life；(2) preparation of nano-cellulose composite aquogel based phase-change material of the present invention
Method, process is simple makes full use of the bond energy between each component, the stable phase-change material of synthesis performance.
Specific embodiment
Following examples further illustrate present disclosure, but should not be construed as limiting the invention.Without departing substantially from
In the case of spirit of the invention and essence, the modification made to the inventive method, step or condition and replacement belong to the present invention
Scope.If not specializing, the conventional meanses that technological means used are well known to those skilled in the art in embodiment.
Embodiment 1
A kind of nano-cellulose composite aquogel based phase-change material, by weight, the material includes nano-cellulose
1 part of compound water congealing gum base materials, 98 parts of the main energy storage agent of phase transformation, 1 part of nucleator；Wherein nano-cellulose compound water congealing gum base materials include
Nano-cellulose 2.5mg, Carboxymethyl cellulose sodium 1g, aqueous slkali 12mL, monomer 7.2g, initiator 0.15g, cross-linking agent 50mg,
Extractant 200mL, deionized water 100mL.
The aqueous slkali is the sodium hydroxide solution of 1mol/L, and monomer is 6g acrylic acid and 1.2g acrylamides, initiator
For Ammonium persulfate., cross-linking agent is N, and N '-methylene-bisacrylamide, extractant is acetone.
The main energy storage agent of the phase transformation for mass concentration 15% Sodium Chloride.
The nucleator is kieselguhr.
The preparation method of nano-cellulose composite aquogel based phase-change material, comprises the steps of：
(1) nano-cellulose compound water congealing gum base materials are prepared
A, Carboxymethyl cellulose sodium powder is scattered in 100mL deionized waters, and under 60 DEG C of water bath conditions, uses nitrogen
Air in 30 minutes discharge systems of purging；
B, into system initiator is added, be sufficiently stirred for being down to 40 DEG C after producing to free radical within 5 minutes, added monomer, receive
Rice cellulose and cross-linking agent, system is warming up to 70 DEG C, fully reacts 2 hours in nitrogen atmosphere；
C, the product after step b polyreaction is moved in room temperature environment, stand 24 hours to abundant gelation；
The enough aqueous slkalis of Deca in d, the gel obtained to step c, with excessive deionization washing after abundant deprotonation
Wash, the pH value to cleaning mixture is 6；
Under e, room temperature, using gel of the extractant process Jing after the process of step d, take its precipitate and be placed in baking oven 70 DEG C and do
It is dry to crush, sieve to constant weight, collect the gel of 60~100 mesh；
(2) nano-cellulose composite aquogel based phase-change material is prepared
The nano-cellulose compound water congealing gum base materials that step (1) is prepared are sufficiently stirred for mixing with the main energy storage agent of phase transformation
It is even, nucleator is added, stir prepared.
The nano-cellulose composite aquogel based phase-change material is used for into fruit-vegetable food or pharmaceutical products cold chain transportation
In packaging material, the phase transition temperature of the phase-change material is -9.0 DEG C, and latent heat of phase change is 172.7J/g.
Embodiment 2
A kind of nano-cellulose composite aquogel based phase-change material, by weight, the material includes nano-cellulose
3 parts of compound water congealing gum base materials, 88 parts of the main energy storage agent of phase transformation, 5 parts of nucleator；Wherein nano-cellulose compound water congealing gum base materials include
Nano-cellulose 5mg, Carboxymethyl cellulose sodium 1g, aqueous slkali 18mL, monomer 7g, initiator 0.15g, cross-linking agent 45mg, extraction
Agent 200mL, deionized water 90mL.
The aqueous slkali is the sodium hydroxide solution of 1mol/L, and monomer is 6g acrylic acid and 1g acrylamides, and initiator is
Ammonium persulfate., cross-linking agent is N, and N '-methylene-bisacrylamide, extractant is acetone.
The main energy storage agent of the phase transformation for mass concentration 5% potassium chloride.
The nucleator is sodium tetraborate.
The preparation method of nano-cellulose composite aquogel based phase-change material, comprises the steps of：
(1) nano-cellulose compound water congealing gum base materials are prepared
A, Carboxymethyl cellulose sodium powder is scattered in 100mL deionized waters, and under 60 DEG C of water bath conditions, uses nitrogen
Air in 30 minutes discharge systems of purging；
B, into system initiator is added, be sufficiently stirred for being down to 35 DEG C after producing to free radical within 5 minutes, added monomer, receive
Rice cellulose and cross-linking agent, system is warming up to 70 DEG C, fully reacts 2 hours in nitrogen atmosphere；
C, the product after step b polyreaction is moved in room temperature environment, stand 24 hours to abundant gelation；
The enough aqueous slkalis of Deca in d, the gel obtained to step c, with excessive deionization washing after abundant deprotonation
Wash, the pH value to cleaning mixture is 7；
Under e, room temperature, using gel of the extractant process Jing after the process of step d, take its precipitate and be placed in baking oven 70 DEG C and do
It is dry to crush, sieve to constant weight, collect the gel of 60~100 mesh；
(2) nano-cellulose composite aquogel based phase-change material is prepared
The nano-cellulose compound water congealing gum base materials that step (1) is prepared are sufficiently stirred for mixing with the main energy storage agent of phase transformation
It is even, nucleator is added, stir prepared.
The nano-cellulose composite aquogel based phase-change material is used for into fruit-vegetable food or pharmaceutical products cold chain transportation
In packaging material, the phase transition temperature of the phase-change material is -3.8 DEG C, and latent heat of phase change is 149.6J/g.
Embodiment 3
A kind of nano-cellulose composite aquogel based phase-change material, by weight, the material includes nano-cellulose
10 parts of compound water congealing gum base materials, 90 parts of the main energy storage agent of phase transformation, 3 parts of nucleator；Wherein nano-cellulose compound water congealing gum base materials bag
Include nano-cellulose 1mg, Carboxymethyl cellulose sodium 3g, aqueous slkali 25mL, monomer 6g, initiator 0.13g, cross-linking agent 55mg, extraction
Take agent 250mL, deionized water 98mL.
The aqueous slkali is the sodium hydroxide solution of 1.5mol/L, and monomer is 4g acrylic acid and 2g acrylamides, initiator
For Ammonium persulfate., cross-linking agent is N, and N '-methylene-bisacrylamide, extractant is acetone.
The main energy storage agent of the phase transformation presses 7 for the ammonium chloride and 5% Sodium Chloride of mass concentration 10%:2 mixing are obtained.
The nucleator is barium fluoride.
The preparation method of nano-cellulose composite aquogel based phase-change material, comprises the steps of：
(1) nano-cellulose compound water congealing gum base materials are prepared
A, Carboxymethyl cellulose sodium powder is scattered in 100mL deionized waters, and under 55 DEG C of water bath conditions, uses nitrogen
Air in 30 minutes discharge systems of purging；
B, into system initiator is added, be sufficiently stirred for being down to 40 DEG C after producing to free radical within 5 minutes, added monomer, receive
Rice cellulose and cross-linking agent, system is warming up to 70 DEG C, fully reacts 2 hours in nitrogen atmosphere；
C, the product after step b polyreaction is moved in room temperature environment, stand 24 hours to abundant gelation；
The enough aqueous slkalis of Deca in d, the gel obtained to step c, with excessive deionization washing after abundant deprotonation
Wash, the pH value to cleaning mixture is 7；
Under e, room temperature, using gel of the extractant process Jing after the process of step d, take its precipitate and be placed in baking oven 70 DEG C and do
It is dry to crush, sieve to constant weight, collect the gel of 60~100 mesh；
(2) nano-cellulose composite aquogel based phase-change material is prepared
The nano-cellulose compound water congealing gum base materials that step (1) is prepared are sufficiently stirred for mixing with the main energy storage agent of phase transformation
It is even, nucleator is added, stir prepared.
The nano-cellulose composite aquogel based phase-change material is used for into fruit-vegetable food or pharmaceutical products cold chain transportation
In packaging material, the phase transition temperature of the phase-change material is -6.1 DEG C, and latent heat of phase change is 146.5J/g.
Embodiment 4
A kind of nano-cellulose composite aquogel based phase-change material, by weight, the material includes nano-cellulose
5 parts of compound water congealing gum base materials, 95 parts of the main energy storage agent of phase transformation, 1 part of nucleator；Wherein nano-cellulose compound water congealing gum base materials include
Nano-cellulose 0.5mg, Carboxymethyl cellulose sodium 5g, aqueous slkali 28mL, monomer 7.2g, initiator 0.15g, cross-linking agent 50mg,
Extractant 230mL, deionized water 93mL.
The aqueous slkali is the sodium hydroxide solution of 1mol/L, and monomer is 6g acrylic acid and 1.2g acrylamides, initiator
For Ammonium persulfate., cross-linking agent is N, and N '-methylene-bisacrylamide, extractant is acetone.
The main energy storage agent of the phase transformation for mass concentration 15% ammonium chloride.
The nucleator is kieselguhr.
The preparation method of nano-cellulose composite aquogel based phase-change material, comprises the steps of：
(1) nano-cellulose compound water congealing gum base materials are prepared
A, Carboxymethyl cellulose sodium powder is scattered in 100mL deionized waters, and under 60 DEG C of water bath conditions, uses nitrogen
Air in 30 minutes discharge systems of purging；
B, into system initiator is added, be sufficiently stirred for being down to 40 DEG C after producing to free radical within 5 minutes, added monomer, receive
Rice cellulose and cross-linking agent, system is warming up to 68 DEG C, fully reacts 2 hours in nitrogen atmosphere；
C, the product after step b polyreaction is moved in room temperature environment, stand 24 hours to abundant gelation；
The enough aqueous slkalis of Deca in d, the gel obtained to step c, with excessive deionization washing after abundant deprotonation
Wash, the pH value to cleaning mixture is 8；
Under e, room temperature, using gel of the extractant process Jing after the process of step d, take its precipitate and be placed in baking oven 70 DEG C and do
It is dry to crush, sieve to constant weight, collect the gel of 60~100 mesh；
(2) nano-cellulose composite aquogel based phase-change material is prepared
The nano-cellulose compound water congealing gum base materials that step (1) is prepared are sufficiently stirred for mixing with the main energy storage agent of phase transformation
It is even, nucleator is added, stir prepared.
The nano-cellulose composite aquogel based phase-change material is used for into fruit-vegetable food or pharmaceutical products cold chain transportation
In packaging material, the phase transition temperature of gained phase-change material is -7.4 DEG C, and latent heat of phase change is 148.9J/g.
Embodiment 5
A kind of nano-cellulose composite aquogel based phase-change material, by weight, the material includes nano-cellulose
7 parts of compound water congealing gum base materials, 85 parts of the main energy storage agent of phase transformation, 2 parts of nucleator；Wherein nano-cellulose compound water congealing gum base materials include
Nano-cellulose 4mg, Carboxymethyl cellulose sodium 1g, aqueous slkali 12mL, monomer 6.5g, initiator 0.15g, cross-linking agent 40mg, extraction
Take agent 200mL, deionized water 100mL.
The aqueous slkali is the sodium hydroxide solution of 2mol/L, and monomer is 4.5g acrylic acid and 2g acrylamides, initiator
For Ammonium persulfate., cross-linking agent is N, and N '-methylene-bisacrylamide, extractant is acetone.
The main energy storage agent of the phase transformation for mass concentration 15% ammonium chloride.
It is 1 that the nucleator is mass ratio:1 kieselguhr and sodium tetraborate.
The preparation method of nano-cellulose composite aquogel based phase-change material, comprises the steps of：
(1) nano-cellulose compound water congealing gum base materials are prepared
A, Carboxymethyl cellulose sodium powder is scattered in 100mL deionized waters, and under 58 DEG C of water bath conditions, uses nitrogen
Air in 30 minutes discharge systems of purging；
B, into system initiator is added, be sufficiently stirred for being down to 35 DEG C after producing to free radical within 5 minutes, added monomer, receive
Rice cellulose and cross-linking agent, system is warming up to 70 DEG C, fully reacts 2 hours in nitrogen atmosphere；
C, the product after step b polyreaction is moved in room temperature environment, stand 24 hours to abundant gelation；
The enough aqueous slkalis of Deca in d, the gel obtained to step c, with excessive deionization washing after abundant deprotonation
Wash, the pH value to cleaning mixture is 8；
Under e, room temperature, using gel of the extractant process Jing after the process of step d, take its precipitate and be placed in baking oven 70 DEG C and do
It is dry to crush, sieve to constant weight, collect the gel of 60~100 mesh；
(2) nano-cellulose composite aquogel based phase-change material is prepared
The nano-cellulose compound water congealing gum base materials that step (1) is prepared are sufficiently stirred for mixing with the main energy storage agent of phase transformation
It is even, nucleator is added, stir prepared.
The nano-cellulose composite aquogel based phase-change material is used for into fruit-vegetable food or pharmaceutical products cold chain transportation
In packaging material, the phase transition temperature of gained phase-change material is -7.9 DEG C, and latent heat of phase change is 153.6/g.
Claims (7)
1. a kind of nano-cellulose composite aquogel based phase-change material, it is characterised in that by weight, the material includes receiving
1~10 part of rice cellulose compound water congealing gum base materials, 85~98 parts of the main energy storage agent of phase transformation, 1~5 part of nucleator；Wherein nanofiber
Plain compound water congealing gum base materials include nano-cellulose, Carboxymethyl cellulose sodium, aqueous slkali, monomer, initiator, cross-linking agent, extraction
Agent, deionized water, the ratio of each component is 0.5~5mg:1~5g:5~30mL:6~7.2g:0.05~0.15g:40~60mg:
200~250mL:90~100mL.
2. a kind of nano-cellulose composite aquogel based phase-change material according to claim 1, it is characterised in that the alkali
Solution is the sodium hydroxide solution that molar concentration is 0.5~2mol/L, and monomer is acrylic acid and acrylamide, acrylic acid and propylene
The weight ratio of amide is 2~6:1, initiator is Ammonium persulfate., and cross-linking agent is N, N '-methylene-bisacrylamide, and extractant is
Acetone.
3. a kind of nano-cellulose composite aquogel based phase-change material according to claim 1, it is characterised in that the phase
Become main energy storage agent at least one in Sodium Chloride, ammonium chloride, calcium chloride, the Klorvess Liquid of mass concentration 5%~15%.
4. a kind of nano-cellulose composite aquogel based phase-change material according to claim 1, it is characterised in that it is described into
Core agent is at least one in sodium tetraborate, kieselguhr, barium fluoride.
5. the preparation method of the arbitrary nano-cellulose composite aquogel based phase-change material of Claims 1 to 4, its feature exists
In comprising the steps of：
(1) nano-cellulose compound water congealing gum base materials are prepared
A, Carboxymethyl cellulose sodium powder is scattered in deionized water, and under 50~60 DEG C of water bath conditions, is purged with nitrogen
Air in discharge system；
B, into system initiator is added, 30~40 DEG C is down to after being sufficiently stirred for, add monomer, nano-cellulose and cross-linking agent,
System is warming up to 65~75 DEG C, fully reacts in nitrogen atmosphere；
C, the product after step b polyreaction is moved in room temperature environment, stood to abundant gelation；
Deca aqueous slkali in d, the gel obtained to step c, with excessive deionized water wash after abundant deprotonation, to washing
The pH value of liquid is 6~8；
Under e, room temperature, using extractant process Jing step d process after gel, take its precipitate be placed in baking oven be dried to perseverance
Weight, crushes, sieves, and collects the gel of 60~100 mesh；
(2) nano-cellulose composite aquogel based phase-change material is prepared
The nano-cellulose compound water congealing gum base materials that step (1) is prepared are sufficiently stirred for mixing with the main energy storage agent of phase transformation, plus
Enter nucleator, stir prepared.
6. the preparation method of nano-cellulose composite aquogel based phase-change material according to claim 5, it is characterised in that
Aqueous slkali and the mixed proportion of gel are 5~30mL in step d:80~100g.
7. the arbitrary nano-cellulose composite aquogel based phase-change material of Claims 1 to 4 is in fruit-vegetable food or pharmaceutical products
Application in the packaging material of cold chain transportation.
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| CN109943291A (en) * | 2019-04-04 | 2019-06-28 | 江南大学 | A kind of high thermal conductivity selfreparing gel based phase-change material and preparation method thereof |
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| CN111613828A (en) * | 2020-06-04 | 2020-09-01 | 武汉理工大学 | Batch preparation method of micro energy storage devices on flexible film substrate |
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| WO2024060036A1 (en) * | 2022-09-20 | 2024-03-28 | 纯钧新材料(深圳)有限公司 | Phase change material having phase change temperature of 2-8°c and preparation method therefor |
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