CN102002342A - Method for preparing waste acrylic fiber and fatty acid combined phase change material - Google Patents

Method for preparing waste acrylic fiber and fatty acid combined phase change material Download PDF

Info

Publication number
CN102002342A
CN102002342A CN2010102970019A CN201010297001A CN102002342A CN 102002342 A CN102002342 A CN 102002342A CN 2010102970019 A CN2010102970019 A CN 2010102970019A CN 201010297001 A CN201010297001 A CN 201010297001A CN 102002342 A CN102002342 A CN 102002342A
Authority
CN
China
Prior art keywords
change material
phase change
waste silk
lipid acid
acrylic fibres
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN2010102970019A
Other languages
Chinese (zh)
Other versions
CN102002342B (en
Inventor
郭静
相恒学
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Dalian Polytechnic University
Original Assignee
Dalian Polytechnic University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Dalian Polytechnic University filed Critical Dalian Polytechnic University
Priority to CN 201010297001 priority Critical patent/CN102002342B/en
Publication of CN102002342A publication Critical patent/CN102002342A/en
Application granted granted Critical
Publication of CN102002342B publication Critical patent/CN102002342B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Landscapes

  • Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

The invention relates to a method for preparing a waste acrylic fiber and fatty acid combined phase change material, which comprises: preparing uniform polymer solution by stirring waste acrylic fibers and fatty acid in a solvent; and allowing the polymer solution to precipitate in a precipitator quickly. Macro molecules of polyacrylonitrile and molecules of fatty acid are agglomerated together through the intermolecular forces, so that the phase change material does not seeps out even the outside temperature reaches 100 DEG C. The amorphous phase change material prepared by the method has the advantages that: the enthalpy value and thermal stability are high; the preparation method is simple; the cost is low; the solvent can be recycled; and the like. The method realizes waste fiber recycling, reduces environmental pollution and provides a new energy-saving material for the society. The invention is a new project with low cost, high profit and sufficient resources, and has a bright development prospect.

Description

The preparation method of a kind of acrylic fibres waste silk and the compound phase change material of lipid acid
Technical field
The invention belongs to the phase-changing energy storage material technical field, be specifically related to a kind of preparation method who utilizes acrylic fibres waste silk and the compound shaping phase-change material of lipid acid.
Background technology
Phase-changing energy storage material is to utilize heat absorption and the exothermic effect of material in phase transition process, carries out the material of thermal energy storage and temperature adjusting.Phase change material has approximately constant temperature in phase transition process; system temperature such as can control at advantage; obtained utilizing preferably in the fields such as insulation of recycling, clothes bed clothes and the building construction of sun power utilization, used heat and waste heat, and at alleviating energy crisis, improve aspect such as energy utilization rate and brought into play important effect.
Acrylic fibers because of structural reason can not be by heat fusing granulation again regeneration, can not reclaim monomer with the method for thermo-cracking, but have active cyano group in its molecular structure (C ≡ N), can utilize cyano group to transform, acrylic fibers are reclaimed and are utilized.Existing report obtains polyacrylic acid or sodium polyacrylate with waste and old acrylic fibers hydrolysis, is used to prepare High hydrophilous resin, ion-exchange fiber, drilling well additive etc., but the rarely seen report of using it for the preparation phase change material.
In phase-changing energy storage material, lipid acid has advantages such as higher enthalpy of phase change, no surfusion, corrodibility be little.But be difficult to satisfy in the practical application the demand of different transformation temperatures at the lipid acid of one-component, often seek binary lipid acid compound system.Because lipid acid has phase mixcibility preferably, several lipid acid can be carried out consolute and handle, form binary or polybasic eutectic system, to reduce the fusing point of material, obtain the phase change material of temperature of fusion a wider range, superior performance, make it to obtain better application.Though document report employing binary lipid acid is direct and inorganic particulate is compound to obtain phase change material, there are serious problems such as phase change material seepage in this phase change material.
Summary of the invention
For addressing the above problem, the invention provides a kind of preparation method who utilizes acrylic fibres waste silk and the compound shaping phase-change material of lipid acid, this method is a kind of recovery and utilization technology of acrylic fibres waste silk cheaply; Gu a kind of novel solid-energy storage material can be provided again.The phase change material phase transition process form stable of the present invention's preparation,, polyacrylonitrile macromole and fatty acid molecule are agglomerated together by Intermolecular Forces, even outside temperature reaches 100 ℃, phase change material can not ooze out yet.Except that the characteristics that possess common shaping phase-change material, also have higher enthalpy, heat-insulating property preferably.Therefore it can be used as a kind of new phase change material and is applied in accumulation of heat and energy-saving field widely.
The present invention can be achieved by the following technical programs:
The first step, under 60~90 ℃, press certain mass than with acrylic fibres waste silk, lipid acid, N, dinethylformamide joins in the reactor, stirring and refluxing 10~40min obtains uniform oyster white polymers soln; Wherein said acrylic fibres waste silk, lipid acid and N, the mass ratio of dinethylformamide are 1: 1~4: 4~25, and lipid acid is stearic acid or stearic acid and lauric mixture, and stearic acid and lauric mass ratio are 1: 2~5.02 in the mixture.
Second step, the polymers soln of the first step gained is injected precipitation agent, occur white precipitate in the solution, white precipitate is separated after drying, be the compound phase change material of acrylic fibres waste silk and lipid acid; Wherein said precipitation agent is the aqueous solution of water or polyvinyl alcohol, and the massfraction of the aqueous solution of polyvinyl alcohol is 15~25%.
The present invention can also be by the certain mass ratio with acrylic fibres waste silk, inorganic particulate, lipid acid, N, dinethylformamide joins in the reactor, stirring and refluxing 10~40min, obtain uniform oyster white polymers soln, wherein used inorganic particulate is any one of polynite or molecular sieve, its consumption be in the reactor raw material total mass 0.829%~3.57%; Polymers soln is injected the aqueous solution of polyvinyl alcohol, occur white precipitate in the solution,, be the compound phase change material of inoganic particle modified acrylic fibres waste silk and lipid acid the precipitate and separate after drying.
Compare with other disclosed setting phase change energy storage material and preparation method, the present invention has following advantage:
1, the propping material of shaping phase-change material of the present invention is selected acrylic fibres waste silk, not only solve acrylic fibres waste silk and recycled a difficult problem, realized the resource recycling, reduced environmental pollution, and acrylic fibres waste silk has reduced very big cost directly by the dissolution with solvents utilization than recycling by hydrolysis.
2, the enthalpy of phase change of the prepared shaping phase-change material of the present invention is higher, reaches 170J/g.
3, the prepared shaping phase-change material of the present invention has good morphological stability and thermostability, even still can keep solid-form Gu temperature reaches 110 ℃.Its reason be acrylic fibres waste silk, lipid acid in the blend process, produced the certain physical effect between the polymer macromolecular chain and existed, as only there being quite weak model ylid bloom action power between hydrocarbon chain, have stronger hydrogen bond etc. between the polar group.After temperature surpasses the fusing point of lipid acid,, can from composite phase-change material, not ooze out because lipid acid is subjected to the constraint of Intermolecular Forces yet.
4, preparation technology of the present invention is simple, the raw material acrylic fibres waste silk that adopts not only price is low, and directly by the dissolution with solvents utilization, recycle by hydrolysis method with it and to compare, reduced very big cost.
Description of drawings
The infrared spectrogram of Fig. 1, stearic acid, lauric acid, acrylic fibres waste silk and composite phase-change material.
The stereoscan photograph of Fig. 2, gained composite phase-change material of the present invention.
The composite phase-change material DSC heating curve of Fig. 3, gained of the present invention.
The DSC temperature lowering curve of the composite phase-change material of Fig. 4, gained of the present invention.
Cooling curve under the composite phase-change material thermal cycling of Fig. 5, gained of the present invention.
The thermogravimetric curve of the composite phase-change material of Fig. 6, gained of the present invention.
Embodiment
Embodiment 1:
With acrylic fibres waste silk 2g, lauric acid 6.67g, stearic acid 1.33g, N, dinethylformamide (DMF) 25g adds in the there-necked flask, after for some time, obtains uniform oyster white polymers soln in 90 ℃ of stirring and refluxing.Polymers soln is injected water, white precipitate occurs, be the compound phase change material of acrylic fibres waste silk and lipid acid after the drying.
Above-mentioned shaping phase-change material and preparation raw material thereof are carried out the analysis of infrared spectra (see figure 1), this spectrogram of inventing prepared phase change material be not three kinds of raw materials simply adding and, and the disappearance at Partial Feature peak and the generation of new characteristic peak are arranged, although illustrate between isonomic lipid acid stearic acid and the lauric acid, can not produce chemical reaction between acrylic fibers (PAN) and the binary lipid acid, there is the certain physical effect to exist between the three of back but mix, as only there being quite weak model ylid bloom action power between hydrocarbon chain, there is stronger hydrogen bond etc. between the polar group.And pass through the scanning electron microscope (see figure 2) and should invent each uniform component distribution in the prepared phase change material as can be seen, there is not phenomenon of phase separation, the phase variant is by in the firm skeleton propping material that is fixed on PAN.
By differential scanning research (seeing Fig. 3, Fig. 4), the melting enthalpy of the phase change material that this invention is prepared is 152.42J/g, crystallization enthalpy is 135.80J/g, and the DSC thermal cycling is found out after eliminating thermal history, the DSC cyclic curve of phase change material overlaps substantially, shows this phase change material good thermal stability.And the cooling curve (see figure 5) demonstration that should invent prepared phase change material, phase change material platform occurs at 29 ℃, and the platform time can be near 1060s.The cooling curve of this phase change material heating for multiple times shows that this material has good insulation stability simultaneously, and with the increase of times of thermal cycle, heat insulation effect does not weaken.The cooling curve (see figure 6) of the phase change material that this invention is prepared shows that the thermal weight loss scope of phase change material degraded is 180 ℃~500 ℃, and locates to occur two very big degradation rate districts at 252 ℃ with 346 ℃, and this composition with phase change material is relevant.Thermogravimetric curve shows that the prepared phase change material of this invention uses in being lower than 180 ℃ environment stable.
Embodiment 2:
With acrylic fibres waste silk 5g, lauric acid 3.33g, stearic acid 1.67g, N, dinethylformamide (DMF) 25g adds in the there-necked flask, after for some time, obtains uniform oyster white polymers soln in 60 ℃ of stirring and refluxing.With polymers soln implantation quality mark is in 15% polyvinyl alcohol water solution, white precipitate occurs,
Be the compound phase change material of acrylic fibres waste silk and lipid acid after the drying.
Embodiment 3:
The preparation of acrylic fibres waste silk and stearic acid composite phase-change material: with acrylic fibres waste silk 4g, stearic acid 6g, N, dinethylformamide (DMF) 25g adds in the there-necked flask, after for some time, obtains uniform oyster white polymers soln in 60 ℃ of stirring and refluxing.Polymers soln is injected water, white precipitate occurs, be the compound phase change material of acrylic fibres waste silk and lipid acid after the drying.
Embodiment 4:
With acrylic fibres waste silk 2g, stearic acid 8g, N, dinethylformamide (DMF) 25g adds in the there-necked flask, after for some time, obtains uniform oyster white polymers soln in 90 ℃ of stirring and refluxing.It is 25% polyvinyl alcohol water solution that polymers soln is injected the implantation quality mark, white precipitate occurs, is the compound phase change material of acrylic fibres waste silk and lipid acid after the drying.
Embodiment 5:
With acrylic fibres waste silk 3.75g, organo montmorillonite 1.25g, lauric acid 3.33g, stearic acid 1.67g,, N, dinethylformamide (DMF) 25g adds in the there-necked flask, after for some time, obtains uniform oyster white polymers soln in 90 ℃ of stirring and refluxing.Polymers soln is injected water, white precipitate occurs, be imvite modified acrylic fibres waste silk/compound phase change material of binary lipid acid after the drying.
Embodiment 6:
With acrylic fibres waste silk 1.71g, organo montmorillonite 0.29g, lauric acid 5.33g, stearic acid 2.67g, N, dinethylformamide (DMF) 25g adds in the there-necked flask, after for some time, obtains uniform oyster white polymers soln in 60 ℃ of stirring and refluxing.With polymers soln implantation quality mark is in 15% polyvinyl alcohol water solution, white precipitate occurs, is imvite modified acrylic fibres waste silk/compound phase change material of binary lipid acid after the drying.
Embodiment 7:
With acrylic fibres waste silk 3.75g, molecular sieve 1.25g, lauric acid 3.33g, stearic acid 1.67g, N, dinethylformamide (DMF) 25g adds in the there-necked flask, after for some time, obtains uniform oyster white polymers soln in 90 ℃ of stirring and refluxing.Polymers soln is injected water, white precipitate occurs, be molecular sieve modified acrylic fibres waste silk/compound phase change material of binary lipid acid after the drying.
Embodiment 8:
With acrylic fibres waste silk 1.71g, molecular sieve 0.29g, lauric acid 5.33g, stearic acid 2.67g, N, dinethylformamide (DMF) 25g adds in the there-necked flask, after for some time, obtains uniform oyster white polymers soln in 60 ℃ of stirring and refluxing.With polymers soln implantation quality mark is in 25% polyvinyl alcohol water solution, white precipitate occurs, is molecular sieve modified acrylic fibres waste silk/compound phase change material of binary lipid acid after the drying.

Claims (7)

1. the preparation method of acrylic fibres waste silk and the compound phase change material of lipid acid is characterized in that the concrete operations step is as follows:
The first step, with acrylic fibres waste silk, lipid acid, N, dinethylformamide joins in the reactor, stirring and refluxing obtains uniform oyster white polymers soln;
Second step, polymers soln is injected precipitation agent, occur white precipitate in the solution, will precipitate after the drying promptly.
2. the preparation method of a kind of acrylic fibres waste silk according to claim 1 and the compound phase change material of lipid acid is characterized in that acrylic fibres waste silk in the first step, lipid acid, N, and the temperature of reaction of dinethylformamide is 60~90 ℃, and the reaction times is 10~40 minutes.
3. the preparation method of a kind of acrylic fibres waste silk according to claim 1 and the compound phase change material of lipid acid, the mass ratio that it is characterized in that joining the raw material in the reactor is an acrylic fibres waste silk: lipid acid: N, dinethylformamide=1: 1~4: 4~25.
4. the preparation method of a kind of acrylic fibres waste silk according to claim 1 and the compound phase change material of lipid acid, it is characterized in that the lipid acid described in the first step is stearic acid or stearic acid and lauric mixture, stearic acid and lauric mass ratio are 1: 2~5.02 in the mixture.
5. the preparation method of a kind of acrylic fibres waste silk according to claim 1 and the compound phase change material of lipid acid, it is characterized in that described acrylic fibres waste silk the preparation composite phase-change material in as the skeleton propping material.
6. the preparation method of a kind of acrylic fibres waste silk according to claim 1 and the compound phase change material of lipid acid is characterized in that the precipitation agent described in second step is the aqueous solution of water or polyvinyl alcohol, and wherein the aqueous solution massfraction of polyvinyl alcohol is 15~25%.
7. the preparation method of a kind of acrylic fibres waste silk according to claim 1 and the compound phase change material of lipid acid is characterized in that the concrete operations step is as follows:
The first step, with acrylic fibres waste silk, inorganic particulate, lipid acid, N, dinethylformamide joins in the reactor, stirring and refluxing obtains uniform oyster white polymers soln;
Second step, polymers soln is injected the aqueous solution of polyvinyl alcohol, occur white precipitate in the solution, will precipitate after the drying promptly;
Wherein used inorganic particulate is polynite or molecular sieve, its consumption be in the reactor raw material total mass 0.829%~3.57%.
CN 201010297001 2010-09-26 2010-09-26 Method for preparing waste acrylic fiber and fatty acid combined phase change material Expired - Fee Related CN102002342B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 201010297001 CN102002342B (en) 2010-09-26 2010-09-26 Method for preparing waste acrylic fiber and fatty acid combined phase change material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN 201010297001 CN102002342B (en) 2010-09-26 2010-09-26 Method for preparing waste acrylic fiber and fatty acid combined phase change material

Publications (2)

Publication Number Publication Date
CN102002342A true CN102002342A (en) 2011-04-06
CN102002342B CN102002342B (en) 2013-05-08

Family

ID=43810044

Family Applications (1)

Application Number Title Priority Date Filing Date
CN 201010297001 Expired - Fee Related CN102002342B (en) 2010-09-26 2010-09-26 Method for preparing waste acrylic fiber and fatty acid combined phase change material

Country Status (1)

Country Link
CN (1) CN102002342B (en)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1465648A (en) * 2002-06-17 2004-01-07 中国人民解放军第二军医大学 Phase change energy storage composite material and preparation process thereof
CN1493720A (en) * 2003-07-02 2004-05-05 东华大学 Phase change composite spinning solution and its preparation and application
CN1850937A (en) * 2005-04-22 2006-10-25 财团法人纺织产业综合研究所 High temperature-resistant polymer phase-transition material
CN1908258A (en) * 2006-08-10 2007-02-07 中国科学院广州化学研究所 Phase-change energy-storage ultra-fine composite fiber and preparation method and application thereof
US20080292560A1 (en) * 2007-01-12 2008-11-27 Dov Tamarkin Silicone in glycol pharmaceutical and cosmetic compositions with accommodating agent

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1465648A (en) * 2002-06-17 2004-01-07 中国人民解放军第二军医大学 Phase change energy storage composite material and preparation process thereof
CN1493720A (en) * 2003-07-02 2004-05-05 东华大学 Phase change composite spinning solution and its preparation and application
CN1850937A (en) * 2005-04-22 2006-10-25 财团法人纺织产业综合研究所 High temperature-resistant polymer phase-transition material
CN1908258A (en) * 2006-08-10 2007-02-07 中国科学院广州化学研究所 Phase-change energy-storage ultra-fine composite fiber and preparation method and application thereof
US20080292560A1 (en) * 2007-01-12 2008-11-27 Dov Tamarkin Silicone in glycol pharmaceutical and cosmetic compositions with accommodating agent

Also Published As

Publication number Publication date
CN102002342B (en) 2013-05-08

Similar Documents

Publication Publication Date Title
CN102153528B (en) Method for preparing furfural, polyether polyalcohol, phenolic resin and nanometer silicon dioxide from straw
CN102604599A (en) Inorganic phase change energy storage material
CN103980863B (en) A kind of side chain liquid crystalline polymer composite shape-setting phase-change material and preparation method thereof
CN102992703A (en) Phase-change thermal-storage intelligent temperature-control wall material and preparation method thereof
CN102070908A (en) Straw ethanol fermentation residue-containing modified asphalt composite material for waterproof coiled material and preparation method thereof
CN102659377A (en) Thermal preservation energy saving composite phase change energy storage gypsum board prepared by using phosphorous gypsum and preparation method thereof
CN110453562B (en) Method for improving self-healing of cold-mix asphalt mixture based on nano carbon fiber
CN103131395A (en) Paraffin-graphite foam composite shape-stabilized phase change material and preparation method thereof
CN101225237B (en) Method for preparing modified asphalt by using waste plastics
CN105152674A (en) Preparation method of pantograph slide plate made of graphene modified carbon/carbon composite material
CN102888211A (en) Composite shape-stabilized phase change material and preparation method thereof
CN106634850A (en) Heat-conducting composite solid-solid phase-change material and preparation method therefor
CN103146351B (en) Shaped phase-change material with high heat-conducting property and preparation method thereof
Li et al. Synthesis of microencapsulated stearic acid with amorphous TiO2 as shape-stabilized PCMs for thermal energy storage
CN102285774A (en) Asphalt pavement warm mixing regenerator and preparation method and using method thereof
CN104877641A (en) Method for low-cost quick preparation of paraffin/graphite phase-change composite material
CN102703035A (en) Road phase-change temperature regulator and preparation method thereof
CN102614917B (en) Preparation method of composite carbon base solid acid catalyst
CN101979728B (en) Method for preparing phase change fibers by utilizing acrylic waste silk
Sun et al. Composites with a novel core–shell structural expanded perlite/polyethylene glycol composite PCM as novel green energy storage composites for building energy conservation
CN101121875A (en) Phase-change energy-storage composite material and preparation method thereof
CN101851336B (en) Method for preparing shape-stabilized phase change material by using acrylic fiber waste silks
CN102002342B (en) Method for preparing waste acrylic fiber and fatty acid combined phase change material
CN103044934A (en) Preparation method of composite modified asphalt
CN104448850A (en) Preparation method of novel modified asphalt

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
EE01 Entry into force of recordation of patent licensing contract

Application publication date: 20110406

Assignee: Liaoyang Yilong composite material fine chemical factory

Assignor: Dalian Polytechnic University

Contract record no.: 2013210000063

Denomination of invention: Method for preparing waste acrylic fiber and fatty acid combined phase change material

Granted publication date: 20130508

License type: Common License

Record date: 20130627

LICC Enforcement, change and cancellation of record of contracts on the licence for exploitation of a patent or utility model
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20130508

Termination date: 20160926

CF01 Termination of patent right due to non-payment of annual fee