CN110305470A - A kind of solid solid/phase-change accumulation energy composite modified nylon material with prepare raw material and its preparation method and application - Google Patents
A kind of solid solid/phase-change accumulation energy composite modified nylon material with prepare raw material and its preparation method and application Download PDFInfo
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- CN110305470A CN110305470A CN201910590395.8A CN201910590395A CN110305470A CN 110305470 A CN110305470 A CN 110305470A CN 201910590395 A CN201910590395 A CN 201910590395A CN 110305470 A CN110305470 A CN 110305470A
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- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
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- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/02—Materials undergoing a change of physical state when used
- C09K5/06—Materials undergoing a change of physical state when used the change of state being from liquid to solid or vice versa
- C09K5/063—Materials absorbing or liberating heat during crystallisation; Heat storage materials
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Abstract
The invention belongs to phase-changing energy storage material fields, solid to disclose a kind of solid/phase-change accumulation energy composite modified nylon material and prepare raw material and its preparation method and application.Gu the raw material for preparing of the solid/phase-change accumulation energy composite modified nylon material contains nylon resin, phase-change material, compatilizer, coupling agent and processing aid, the phase-change material is vanadium dioxide and content is not less than 10wt%.The present invention uses phase-change material of the vanadium dioxide as nylon resin, the phase transition temperature of the phase-change material is 68 DEG C, the crystal habit of vanadium dioxide can change at this temperature, it is changed into the monoclinic form of low temperature from the cubic rutile crystal type of high temperature, volume resistivity is mutated 4~6 orders of magnitude, it absorbs or releases energy, the adjusting to temperature can be achieved, thus obtained composite modified nylon material has thermoplasticity, easy processing, it is easy to control, the feature that enthalpy of phase change is high and thermal coefficient is high, it can apply in building energy conservation, intelligent temperature control film, temperature-sensitive element material, the fields such as luminous energy thermal energy.
Description
Technical field
The invention belongs to phase-changing energy storage material fields, and in particular to Gu a kind of solid/phase-change accumulation energy composite modified nylon material
With prepare raw material and its preparation method and application.
Background technique
Phase-changing energy storage material refers in certain temperature range, using material phase itself or structure change, to environment from
It is dynamic to absorb or discharge latent heat, to reach a substance of Regulate Environment temperature.Phase-changing energy storage material can be divided into according to property
Inorganic phase-changing material, four class of organic phase change material, polymeric phase change material and composite phase-change material, can be divided into according to phase transformation mode
Solid-liquid phase change material, four class of solid-solid phase change material, solid-gas reaction material and liquid-gas phase transition material.Solid-gas reaction material and liquid gas phase
Become material because on the turn with the presence of gas, uncontrollable in use, practical application is less；Solid-liquid phase change material exists because of liquid
Need to be packaged the processing such as absorption, liquid easily loses when phase transition；And solid-solid phase change material uses with processing and stablizes, is easily-controllable
System, the advantages that performance is good and easily molded become the important directions that phase-changing energy storage material is researched and developed, can be widely applied to building energy conservation,
The fields such as solar energy, thermal energy.
CN103773317A discloses a kind of multilayer carbon nanotube composite phase-change energy storage material comprising organic phase-change material
Material, multi-layer nano carbon pipe and tungsten doping nano vanadium dioxide powder, the content of the multilayer carbon nanotube are 5~20wt%,
The content of the tungsten doping nano vanadium dioxide powder is 1~10wt%；The organic phase change material is molecular weight 200~6000
PEG and/or C12~C16Fatty acid, the minimum latent heat of phase change of the composite phase-change energy storage material is 100~120J/g, thermally conductive
Coefficient is 0.25~0.35W/mK.Wherein, the fine structure of carbon nanotube and tungsten doping nano vanadium dioxide powder is to phase transformation material
Material plays fixed, coating function, plays a protective role to the thermal property of phase-change material.
Summary of the invention
Gu the present invention is intended to provide a kind of solid/phase-change accumulation energy composite modified nylon material with high enthalpy of phase change and thermal coefficient
Expect and prepare raw material and its preparation method and application.
It is received as described above, CN103773317A is disclosed including organic phase change material, multi-layer nano carbon pipe and witch culture
The multilayer carbon nanotube composite phase-change energy storage material of rice hypovanadic oxide powder.Wherein, the carbon nanotube and tungsten doping nano two
Vanadium oxide powder role is to play the role of fixed, cladding and protective effect to phase-change material, and risen phase-change accumulation energy
Practical is the PEG and/or C of molecular weight 200~600012~C16Fatty acid.The present inventor sends out after further investigation
Existing, vanadium dioxide itself can be used as the phase-change material of nylon resin, and the phase transition temperature of the phase-change material is 68 DEG C, in this temperature
The crystal habit of lower vanadium dioxide can change, and be changed into the monoclinic form of low temperature, body from the cubic rutile crystal type of high temperature
Product resistivity is mutated 4~6 orders of magnitude, absorbs or releases energy, it can be achieved that adjusting to temperature, is equipped with using vanadium dioxide
Compatilizer, coupling agent and processing aid are modified nylon resin, and gained modified nylon materials have enthalpy of phase change high and thermally conductive
The high feature of coefficient.Based on this, the present invention is completed.
Specifically, Gu preparing raw material the present invention provides a kind of solid/phase-change accumulation energy composite modified nylon material, wherein
Gu the raw material for preparing of the solid/phase-change accumulation energy composite modified nylon material contains nylon resin, phase-change material, compatilizer, coupling
Agent and processing aid, the phase-change material are not less than 10wt% for the content of vanadium dioxide and the phase-change material.
Further, Gu on the basis of the total weight for preparing raw material of the solid/phase-change accumulation energy composite modified nylon material,
The content of the nylon resin is 50~85wt%, and the content of the phase-change material is 10~40wt%, and the compatilizer contains
Amount is 2~15wt%, and the content of the coupling agent is 0.1~1wt%, and the content of the processing aid is 0.1~1wt%.
Further, Gu on the basis of the total weight for preparing raw material of the solid/phase-change accumulation energy composite modified nylon material,
The content of the nylon resin is 58~84wt%, and the content of the phase-change material is 10~30wt%, and the compatilizer contains
Amount is 5~10wt%, and the content of the coupling agent is 0.5~1wt%, and the content of the processing aid is 0.5~1wt%.
Further, the relative viscosity of the nylon resin is 2.0~2.4.
Further, the moisture content of the nylon resin is 0.2wt% or less.
Further, the compatilizer is that maleic anhydride is grafted POE.
Further, the grafting rate of maleic anhydride is 0.8~1.2wt% in the maleic anhydride grafting POE.
Further, the coupling agent is silane coupling agent.
Further, the processing aid is antioxidant and/or lubricant；The antioxidant be Hinered phenols antioxidant and
The compound or amine antioxidants of phosphite ester antioxidant and the compound of phosphite ester antioxidant.
Further, the lubricant in E wax, calcium stearate, silicone master batch and pentaerythritol stearate extremely
Few one kind.
Gu the present invention also provides by the above-mentioned solid/phase-change accumulation energy composite modified nylon material for preparing raw material and being prepared.
Gu the present invention also provides the preparation methods of the solid/phase-change accumulation energy composite modified nylon material, wherein this method
It include: that the nylon resin, phase-change material, compatilizer, coupling agent and processing aid are placed in double screw extruder to melt
Gu melting extrusion, tie rod, cooling and pelletizing to get the solid/phase-change accumulation energy composite modified nylon material.
Further, the draw ratio of the double screw extruder be (38~48): 1, extruder temperature range be 220~
260 DEG C, screw speed is 250~600rpm.
It is answered Gu the present invention also provides the solid/phase-change accumulation energy composite modified nylon materials as phase-changing energy storage material
With.
The present invention uses phase-change material of the vanadium dioxide as nylon resin, and is equipped with compatilizer, coupling agent and processing and helps
Agent is modified nylon resin, thus obtained modified nylon materials have thermoplasticity, easy processing, easy to control, enthalpy of phase change is high
And the feature that thermal coefficient is high, it can apply in fields such as building energy conservation, intelligent temperature control film, temperature-sensitive element material, luminous energy thermal energy,
Great prospects for commercial application.
Specific embodiment
Gu the raw material for preparing of solid/phase-change accumulation energy composite modified nylon material provided by the invention contains nylon resin, phase transformation
Material, compatilizer, coupling agent and processing aid are preferably grouped as by above several groups.Wherein, the content of the nylon resin is excellent
It is selected as 50~85wt%, more preferably 58~84wt%.The phase-change material is vanadium dioxide and content is not less than 10wt%, excellent
It is selected as 10~40wt%, more preferably 10~30wt%.The content of the compatilizer is preferably 2~15wt%, more preferably 5~
10wt%.The content of the coupling agent is preferably 0.1~1wt%, more preferably 0.5~1wt%.The content of the processing aid
Preferably 0.1~1wt%, more preferably 0.5~1wt%.
In the present invention, the specific example of the nylon resin includes but is not limited to nylon66 fiber, nylon 6, nylon 612 and Buddhist nun
At least one of dragon 12, particularly preferably nylon 6 (PA6).The relative viscosity of the nylon resin is preferably 2.0~2.4.?
In the present invention, the test temperature of the relative viscosity is 40 DEG C ± 0.1 DEG C, and reference medium is that the sulfuric acid of 96 ± 0.15wt% is water-soluble
Liquid.In addition, the moisture content of the nylon resin is preferably 0.2wt% or less.
In the present invention, the compatilizer can be the existing various substances that each component can be promoted to dissolve each other, especially excellent
It is selected as maleic anhydride grafting POE.Wherein, the grafting rate of maleic anhydride is preferably 0.8~1.2wt%.In the present invention, term
" grafting rate " refers to that the weight of maleic anhydride accounts for the percentage composition of maleic anhydride grafting POE total weight.
In the present invention, the coupling agent role is the interface company for improving phase-change material and nylon resin matrix
It connects, makes material that there is better mechanical performance.The coupling agent is preferably silane coupling agent, can specifically be selected from γ-aminopropyl
Triethoxysilane, 3- (methacryloxypropyl) propyl trimethoxy silicane and isopropyl three (dodecyl benzenesulfonyl) metatitanic acid
At least one of ester.
In the present invention, the processing aid for example can be antioxidant and/or lubricant.Wherein, the antioxidant is excellent
It is selected as the compound or amine antioxidants and phosphite ester antioxidant of Hinered phenols antioxidant and phosphite ester antioxidant
Compound.In the Hinered phenols antioxidant and the compound of phosphite ester antioxidant, the Hinered phenols antioxidant
Weight ratio with phosphite ester antioxidant is preferably (0.5~2): 1.In the amine antioxidants and phosphite ester antioxidant
Compound in, the weight ratio of the amine antioxidants and phosphite ester antioxidant is preferably (0.5~2): 1.The lubrication
The specific example of agent includes but is not limited to: at least one of E wax, calcium stearate, silicone master batch and pentaerythritol stearate.
Gu the present invention also provides by the above-mentioned solid/phase-change accumulation energy composite modified nylon material for preparing raw material and being prepared.
Gu the present invention also provides the preparation methods of the solid/phase-change accumulation energy composite modified nylon material, wherein this method
It include: that the nylon resin, phase-change material, compatilizer, coupling agent and processing aid are placed in double screw extruder to melt
Gu melting extrusion, tie rod, cooling and pelletizing to get the solid/phase-change accumulation energy composite modified nylon material.Wherein, by each component
Before being placed in double screw extruder, first each component can also be pre-mixed.The premixing can be mixed with hand operated mixing,
Mechanical mixture can also be carried out using existing various mixing apparatus.The condition of the premixing so that more than several component shapes
At uniform system.In the pre-mixing process, above several components can be mixed with random order, for example, can incite somebody to action
Above several components are added in mixing vessel one by one in any order to be mixed, can also be by appointing in above several components
Two kinds of meaning adds other components after mixing and continuess to mix uniformly.In addition, the draw ratio of the double screw extruder can be with
For (38~48): 1, extruder temperature may range from 220~260 DEG C, and screw speed can be 250~600rpm.
A kind of specific embodiment according to the present invention, Gu the preparation of the solid/phase-change accumulation energy composite modified nylon material
Method the following steps are included:
S1, the nylon resin is dried into 80~90 DEG C of dehumidifying device 4~6h, moisture content control is existed
0.2wt% is hereinafter, obtain dry nylon resin；
S2, the phase-change material, compatilizer, coupling agent and processing aid are uniformly mixed, add step S1 later and obtains
To drying nylon resin continues to mix uniformly, obtain premix；
S3, progress fusion plastification in double screw extruder is sent into the premix, mediates kneading, most squeezed afterwards through head
Gu out, tie rod, cooling and pelletizing are to get the solid/phase-change accumulation energy composite modified nylon material.
It is answered Gu the present invention also provides the solid/phase-change accumulation energy composite modified nylon materials as phase-changing energy storage material
With.
The embodiment of the present invention is described below in detail, the examples of the embodiments are intended to be used to explain the present invention, and cannot
It is interpreted as limitation of the present invention.In the examples where no specific technique or condition is specified, described according to the literature in the art
Technology or conditions or carried out according to product description.Reagents or instruments used without specified manufacturer is that can lead to
Cross the conventional products of commercially available acquisition.
Examples 1 to 4
Gu Examples 1 to 4 is used to illustrate the preparation side of solid/phase-change accumulation energy composite modified nylon material provided by the invention
Method, specifically includes the following steps:
S1, by nylon resin (PA6, in the sulfuric acid that temperature is 40 DEG C ± 0.1 DEG C, reference medium is 96 ± 0.15wt%
Relative viscosity under aqueous conditions is 2.5) the dry 5h in 85 DEG C of dehumidifying device, and moisture content control is existed
0.2wt% is hereinafter, obtain dry nylon resin；
S2, by phase-change material (vanadium dioxide), compatilizer, (maleic anhydride is grafted POE, is purchased from Foshan City South Sea Bai Chen high score
Sub- new material Co., Ltd, model PC-28, grafting rate are 0.8~1.2wt%), coupling agent (gamma-aminopropyl-triethoxy silicon
Alkane), the antioxidant compound of weight ratio 1:2 (1010 and 168 according to) and lubricant (silicone master batch) be uniformly mixed, be added later
The drying nylon resin that step S1 is obtained continuess to mix uniformly, obtains premix；
S3, the premix for obtaining step S2, which are sent into double screw extruder, to be carried out fusion plastification, mediates kneading, is most passed through afterwards
Gu head extrusion, tie rod, cooling and pelletizing are to get the solid/phase-change accumulation energy composite modified nylon material.The twin-screw extrusion
The draw ratio of machine is 44:1, and extruder temperature is set as 220~260 DEG C, and screw speed is set as 250rpm.Wherein, each raw material
Dosage it is as shown in table 1, Gu gained it is solid/performance of phase-change accumulation energy composite modified nylon material is as shown in table 2.
Comparative example 1
Gu solid/phase-change accumulation energy composite modified nylon material is prepared according to the method for embodiment 1, unlike, by phase transformation material
Material is substituted using the PA6 resin of identical weight part, remaining condition is same as Example 1, Gu obtain reference it is solid/phase-change accumulation energy is compound
Modified nylon materials.Wherein, the dosage of each raw material is as shown in table 1, Gu gained reference consolidates/phase-change accumulation energy composite modified nylon material
Performance it is as shown in table 2.
Comparative example 2
Gu solid/phase-change accumulation energy composite modified nylon material is prepared according to the method for embodiment 1, unlike, phase-change material
Dosage not within the scope of the invention, remaining condition is same as Example 1, Gu obtain reference it is solid/phase-change accumulation energy is composite modified
Nylon material.Wherein, the dosage of each raw material is as shown in table 1, Gu gained reference it is solid/property of phase-change accumulation energy composite modified nylon material
It can be as shown in table 2.
The dosage (wt%) of each raw material of table 1
| Project | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Comparative example 1 | Comparative example 2 |
| PA6 resin | 83 | 78 | 68 | 63 | 93 | 84 |
| Phase-change material | 10 | 15 | 25 | 30 | 0 | 9 |
| Compatilizer | 5 | 5 | 5 | 5 | 5 | 5 |
| Coupling agent | 1 | 1 | 1 | 1 | 1 | 1 |
| Antioxidant | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 |
| Lubricant | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 |
Table 2
It can be seen that from the comparison of embodiment 1 and comparative example 1 after phase-change material vanadium dioxide is added into formula, no
The enthalpy of phase change of material can be only greatlyd improve, and the thermal coefficient of gained composite material is also obviously improved.From embodiment 1
Comparison with comparative example 2 can be seen that when the content for the phase-change material being added into formula is lower than 10wt%, gained composite wood
The enthalpy of phase change and thermal coefficient of material are relatively not added with phase-change material and do not significantly improve.It can from the result of Examples 1 to 4
Out, when the dosage of each component within the scope of the invention when, the enthalpy of phase change and thermal coefficient of gained composite material are with phase transformation
The increase of material additional amount and improve, and when enthalpy of phase change and thermal coefficient are relatively not added with phase-change material, is significantly improved.
Although the embodiments of the present invention has been shown and described above, it is to be understood that above-described embodiment is example
Property, it is not considered as limiting the invention, those skilled in the art are not departing from the principle of the present invention and objective
In the case where can make changes, modifications, alterations, and variations to the above described embodiments within the scope of the invention.
Claims (10)
1. Gu a kind of solid/phase-change accumulation energy composite modified nylon material prepares raw material, which is characterized in that the solid/solid phase becomes storage
The raw material for preparing of energy composite modified nylon material contains nylon resin, phase-change material, compatilizer, coupling agent and processing aid, institute
Stating phase-change material is the content of vanadium dioxide and the phase-change material not less than 10wt%.
2. Gu solid/phase-change accumulation energy composite modified nylon material according to claim 1 prepares raw material, which is characterized in that
Gu the nylon resin contains on the basis of the total weight for preparing raw material of the solid/phase-change accumulation energy composite modified nylon material
Amount is 50~85wt%, and the content of the phase-change material is 10~40wt%, and the content of the compatilizer is 2~15wt%, institute
The content for stating coupling agent is 0.1~1wt%, and the content of the processing aid is 0.1~1wt%；Preferably, Gu with it is described it is solid/
On the basis of the total weight for preparing raw material of phase-change accumulation energy composite modified nylon material, the content of the nylon resin is 58~
84wt%, the content of the phase-change material are 10~30wt%, and the content of the compatilizer is 5~10wt%, the coupling agent
Content be 0.5~1wt%, the content of the processing aid is 0.5~1wt%.
3. Gu feature exists solid/phase-change accumulation energy composite modified nylon material according to claim 1 or 2 prepares raw material
In the relative viscosity of the nylon resin is 2.0~2.4；The moisture content of the nylon resin is 0.2wt% or less.
4. Gu feature exists solid/phase-change accumulation energy composite modified nylon material according to claim 1 or 2 prepares raw material
In the compatilizer is that maleic anhydride is grafted POE；In the maleic anhydride grafting POE grafting rate of maleic anhydride be 0.8~
1.2wt%.
5. Gu feature exists solid/phase-change accumulation energy composite modified nylon material according to claim 1 or 2 prepares raw material
In the coupling agent is silane coupling agent.
6. Gu feature exists solid/phase-change accumulation energy composite modified nylon material according to claim 1 or 2 prepares raw material
In the processing aid is antioxidant and/or lubricant；The antioxidant is Hinered phenols antioxidant and phosphorous acid esters antioxygen
The compound or amine antioxidants of agent and the compound of phosphite ester antioxidant；The lubricant is selected from E wax, stearic acid
At least one of calcium, silicone master batch and pentaerythritol stearate.
7. Gu prepare solid/composite modified Buddhist nun of phase-change accumulation energy that raw material is prepared as described in any one of claim 1~6
Imperial material.
8. Gu the preparation method of solid/phase-change accumulation energy composite modified nylon material as claimed in claim 7, which is characterized in that the party
Method includes: that the nylon resin, phase-change material, compatilizer, coupling agent and processing aid are placed in double screw extruder to carry out
Gu melting extrusion, tie rod, cooling and pelletizing are to get the solid/phase-change accumulation energy composite modified nylon material.
9. Gu the preparation method of solid/phase-change accumulation energy composite modified nylon material according to claim 8, which is characterized in that
The draw ratio of the double screw extruder is (38~48): 1, extruder temperature range is 220~260 DEG C, screw speed 250
~600rpm.
10. Gu solid/application of the phase-change accumulation energy composite modified nylon material as phase-changing energy storage material as claimed in claim 7.
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| CN114806158A (en) * | 2022-05-09 | 2022-07-29 | 厦门金沐实业有限公司 | Modified nylon composite material and preparation method thereof |
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