CN104592945A - Flame-retardant organic phase-change material and preparation method thereof - Google Patents
Flame-retardant organic phase-change material and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- 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
- C09K5/066—Cooling mixtures; De-icing compositions
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09K21/00—Fireproofing materials
- C09K21/06—Organic materials
- C09K21/12—Organic materials containing phosphorus
Abstract
The invention discloses a flame-retardant organic phase-change material and a preparation method thereof. The preparation method for the flame-retardant organic phase-change material comprises the following steps: uniformly mixing a specific silicon-containing organic compound with low-carbon alcohol; then dropwise adding the obtained mixture into a mixture of an organic phase-change material and an organic solvent; adding ammonia water and carrying out uniform mixing under stirring; and successively carrying out cooling, rotary evaporation, washing and vacuum drying so as to obtain the flame-retardant organic phase-change material. The flame-retardant organic phase-change material prepared by using the method has good compatibility, high flame retardant property and thermal conductivity and long life cycle.
Description
Technical field
The present invention relates to organic phase change material technical field, particularly a kind of flame retardant type organic phase change material and preparation method thereof.
Background technology
Phase change material (Phase change materials, PCMs), can the heat of absorbing environmental when there is phase-state change, and releases heat when needed, thus reaches the object controlling ambient temperature.Phase change material is as energy storage carrier, an energy-intensive difficult problem can be alleviated, be widely used in, in air-conditioning cold, the automatic constant-temperature of intelligent building of storage and the energy storage of Application of Solar Energy and switching technology, in fields such as insulation garment, cold compress health care, instrument heat radiations, also there is potential application prospect and market.
Paraffin is the organic phase change material of good properties, and its potential heat value is high, chemical stability good, almost without crossing cold-peace phenomenon of phase separation; But as organic phase change material, also there is the shortcomings such as inflammable, thermal conductivity is low in paraffin.
CN101397489A discloses a kind of flame-retardant shaping organic phase change material and preparation method thereof.The method be by account for total paraffin of system mass percent 50% ~ 60%, the expansion type flame retardant of 15% ~ 20% and 1% ~ 10% metal-powder mix after, join in the high density polyethylene(HDPE) of the melting accounting for total system mass percent 15% ~ 20%, gained mixture, through granulation, shaping, obtains flame-retardant shaping organic phase change material.Due to the synergy of expansion type flame retardant and metal-powder, improve flame retardant resistance and the thermal conductivity of organic phase change material to a certain extent.But, the flame-retardant composition added mainly mineral-type materials, poor with paraffin phase capacitive, and whole complex process, cost is higher, is unfavorable for large-scale promotion.
The disclosed organic phase change energy storage material based on the encapsulation of inorganic materials shell of CN102827585A and CN101880521A, it is encapsulated by the outside inorganic silicon dioxide sheating material of paraffin organic phase change energy storage material, its preparation process is by the organic phase change energy storage material paraffin wax emulsion uniform stirring of preparation, then obtained presoma solution of inorganic silicon dioxide sol-gel is dropwise joined in above-mentioned paraffin wax emulsion by dropping funnel, organic paraffin wax phase change energy storage material of obtained inorganic silicon dioxide encapsulation.The silicon source that wherein CN102827585A adopts is methyl triethyl silicane, and the silicon source that CN101880521A adopts is tetraethoxy.Prepared by the method is microcapsule, owing to adopting silicon-dioxide to be cyst material, has certain flame retardant effect, and can prevent the loss of core paraffin and leak; But silicon-dioxide belongs to high heat capacity type fire retardant material, simple its flame retardant effect that relies on is limited, and the paraffin heat-transfer effect be encapsulated in shell is not good, has a strong impact on its effect as phase-changing energy storage material.In addition, paraffin energy storage material and the organic parent compatibility of passing through its encapsulation are poor, and silicon-dioxide is more crisp, and namely toughness is not enough, and life-time service easily ftractures.
Summary of the invention
In view of the deficiencies in the prior art, the invention provides a kind of flame retardant type organic phase change material and preparation method thereof.The method preparation technology is simple, the flame retardant type organic phase change material compatibility of gained is good, flame retardant properties and thermal conductivity higher, life cycle is longer.
The preparation method of flame retardant type organic phase change material of the present invention, comprises the steps:
(1) organic phase change material and organic solvent are mixed, wherein the mass ratio of organic phase change material and organic solvent is 1:5 ~ 25;
(2) mixed with low-carbon alcohol by silicon-containing organic compound, described silicon-containing organic compound is triethoxysilicane phosphamide, and wherein the mass ratio of silicon-containing organic compound and low-carbon alcohol is 1:5 ~ 30;
(3) mixture of step (2) gained is dropwise added in the mixture of step (1) gained, after mixing, then add ammoniacal liquor, stir; Wherein the add-on of each material is by following ratio control: the mass ratio of silicon-containing organic compound and organic phase change material is 1 ~ 5:1, and the mass ratio of silicon-containing organic compound and ammonia is 1:0.5 ~ 4;
(4) after the solution of step (3) gained is cooled to room temperature, through rotary evaporation process, to products obtained therefrom washing, then through vacuum-drying, flame retardant type organic phase change material is obtained.
In step (1), described organic phase change material can be selected from paraffin, higher fatty acid and ester class thereof one or more, preferred paraffin, the transformation temperature of described organic phase change material is 25 DEG C ~ 58 DEG C.Organic solvent used can be selected from sherwood oil, Skellysolve A, octane one or more, wherein sherwood oil is selected from the sherwood oil that boiling range is 60 DEG C ~ 90 DEG C.
In step (1), the organic phase change material stated and the mixing temperature of organic solvent are 60 DEG C ~ 90 DEG C.
In low-carbon alcohol described in step (2), carbon number is 1 ~ 4, is selected from one or more in methyl alcohol, ethanol, propyl alcohol, butanols.
The mixture of step (2) gained dropwise adds in the mixture of step (1) gained and preferably adds while stirring, make it mix evenly.
Triethoxysilicane phosphamide described in step (2) can adopt ordinary method to synthesize.Preferably adopt in the present invention and prepare with the following method: the dehydrated alcohol and the mixing of triethoxyl silane monomer that by mass ratio are 5 ~ 10:1, add Glacial acetic acid, wherein the add-on of Glacial acetic acid and the mass ratio of triethoxyl silane add-on are 0.1 ~ 2:1.Then at 40 DEG C ~ 60 DEG C, dropwise add water under agitation condition, wherein the add-on of water and the mass ratio of triethoxyl silane are 0.1 ~ 1:1, and being stirred to reactant is colloidal sol shape.Poly-phosphamide (molecular weight 1000 ~ 5000) is added again in this system, the mass ratio of poly-phosphamide and triethoxyl silane is 0.5 ~ 1.5:1, violent stirring is to being uniformly dispersed, and then this mixture is at dry 2h ~ 5h under 80 DEG C ~ 120 DEG C conditions, obtains triethoxysilicane phosphamide.
In step (3), the total Water of the hierarchy of control and the mass ratio of silicon-containing organic compound are 1 ~ 5:1, can add water as required, preferably add water before ammoniacal liquor adds.
In step (3), the temperature controlling reaction system is 60 DEG C ~ 90 DEG C, and the mass concentration of described ammoniacal liquor is 25% ~ 28%.
Rotary evaporation described in step (4), speed range is 150 ~ 300 rpm, and vacuum drying condition is as follows: vacuum tightness is 50 ~ 300Pa, and drying temperature is 10 ~ 50 DEG C, and time of drying is 5 ~ 70h.
Flame retardant type organic phase change material of the present invention is prepared by the invention described above method.Interweaved by the spatial cuboids lattice of such as Fig. 1 and become tridimensional network, organic phase change material is immobilized in above-mentioned reticulated structure.
The flame retardant type organic phase change material that the inventive method provides, concrete advantage is as follows:
(1) the triethoxysilicane phosphamide of the present invention's employing, both there is organo-functional group feature, easily be combined with paraffin phase, there is again Inorganic functional groups's feature, make this phase change material can be simultaneously mutually affine with inorganic and organic two class fertile materials, the remarkable compatibility improving organic phase change material, improves its life cycle;
(2) the silicious sesquioxane hybrid material that is nitrogenous, phosphoric generated after the triethoxysilicane phosphamide hydrolysis that the present invention adopts is reticulated structure, on the one hand can immobilized molten state paraffin well, prevent it from coming off, can increase toughness again, another aspect Inorganic functional groups wherein can improve the thermal conductivity of organic phase change material;
(3) flame retardant effect of organic phase change material that prepared by the inventive method is better than adopting expansion type flame retardant and metal-powder based flame retardant to prepare organic phase change material, this is because the silsesquioxane material of generation after the hydrolysis of triethoxysilicane phosphamide can form fine and close carbon-coating on organic phase change material surface at the initial stage on fire, stop flame to extend internally further, significantly improve the flame retardant properties of organic phase change material.
(4) the inventive method technique is simple, workable, is beneficial to large-scale promotion and uses.
Accompanying drawing explanation
Fig. 1 is that the triethoxysilicane phosphamide hydrolysis generation that the present invention uses is nitrogenous, the mechanism figure of the silicious sesquioxane hybrid material of phosphoric;
Fig. 2 is sedimentation of coke scanning electron microscope (SEM) figure that comparative example 3 products obtained therefrom L of the present invention obtains sample after 600 DEG C of burnings;
Fig. 3 is sedimentation of coke scanning electron microscope (SEM) figure that the embodiment of the present invention 3 products obtained therefrom C obtains sample after 600 DEG C of burnings.
Embodiment
Below in conjunction with embodiment, the present invention will be further described.In the present invention, wt% is massfraction.
Be can clearly be seen that by Fig. 1, triethoxysilicane phosphamide is the persursor material containing organo units and inorganic unit, above-mentioned composition is still remained in silicious sesquioxane after hydrolysis, particularly containing ignition-proof elements such as phosphorus, nitrogen, silicon, the cubes-reticulated structure of silicious sesquioxane is that molten state organic phase change material provides abundant storage space in addition.
Embodiment 1
Be dehydrated alcohol and the mixing of triethoxyl silane monomer of 8:1 by mass ratio, add Glacial acetic acid, wherein the add-on of Glacial acetic acid and the mass ratio of triethoxyl silane add-on are 1:1.Then at 50 DEG C, dropwise add water under agitation condition, wherein the add-on of water and the mass ratio of triethoxyl silane are 0.5:1, and being stirred to reactant is colloidal sol shape.In this system, add poly-phosphamide (molecular weight is 2500) again, the mass ratio of poly-phosphamide and triethoxyl silane is 1:1, and violent stirring is to being uniformly dispersed, and then this mixture is at 100 DEG C of dry 4h, obtains triethoxysilicane phosphamide.
In polytetrafluoroethylene beaker, add 20g paraffin and 100g sherwood oil (boiling range is 60 DEG C ~ 90 DEG C), the transformation temperature of paraffin and latent heat of phase change value are 58 DEG C and 165kJ/kg respectively, stir at 60 DEG C, obtain mixture A.Separately get glass beaker, add 20g triethoxysilicane phosphamide and 200g dehydrated alcohol, stirring at room temperature is even, obtains mixture B.Controlling temperature of reaction system is 60 DEG C, and continuously stirring, mixture B is dropwise added in mixture A, then add 40g deionized water, stir, then in above-mentioned system, add 80g ammoniacal liquor (mass concentration of ammoniacal liquor is 25%), stir.
Be cooled to after room temperature until said mixture, through rotary evaporation process, after product washing, be transferred in vacuum drying oven, keep vacuum tightness 100Pa, dry 48h at 35 DEG C, obtain flame retardant type organic phase change material A.
Embodiment 2
The synthetic method of triethoxysilicane phosphamide is with embodiment 1.
In embodiment 1, the quality of triethoxysilicane phosphamide and dehydrated alcohol is increased to 40g and 400g respectively, deionized water and ammoniacal liquor add-on are adjusted to 80g and 160g respectively, and other working method and material form constant, obtain flame retardant type organic phase change material B.
Embodiment 3
The synthetic method of triethoxysilicane phosphamide is with embodiment 1.
In embodiment 1, the temperature controlling reaction system is 75 DEG C, and other working method and material form constant, obtain flame retardant type organic phase change material C.
Embodiment 4
The synthetic method of triethoxysilicane phosphamide is with embodiment 1.
In embodiment 1, the temperature controlling reaction system is 90 DEG C, and other working method and material form constant, obtain flame retardant type organic phase change material D.
Embodiment 5
The synthetic method of triethoxysilicane phosphamide is with embodiment 1.
In embodiment 3, the add-on of deionized water is increased to 80g, and other working method and material form constant, obtain flame retardant type organic phase change material E.
Embodiment 6
The synthetic method of triethoxysilicane phosphamide is with embodiment 1.
In embodiment 1, take 10g paraffin and 200g sherwood oil, other working method and material form constant, obtain flame retardant type organic phase change material F.
Embodiment 7
The synthetic method of triethoxysilicane phosphamide is with embodiment 1.
In embodiment 1, ammoniacal liquor add-on brings up to 240g, and other working method and material form constant, obtain flame retardant type organic phase change material G.
Embodiment 8
The synthetic method of triethoxysilicane phosphamide is with embodiment 1.
In embodiment 1, take 20g triethoxysilicane phosphamide and 400g dehydrated alcohol, other working method and material form constant, obtain flame retardant type organic phase change material H.
Embodiment 9
The synthetic method of triethoxysilicane phosphamide is with embodiment 1.
In embodiment 1, take 50g triethoxysilicane phosphamide and 500g dehydrated alcohol, deionized water add-on is increased to 100g, and ammoniacal liquor add-on is 200g, and other working method and material form constant, obtain flame retardant type organic phase change material I.
Comparative example 1
According to the method that CN102827585A describes, get 10 grams of paraffin organic phase change energy storage materials, 120 ml distilled waters and 2.5 grams of sodium lauryl sulphate and stir this mixing, prepare paraffin wax emulsion.Take 20 grams of Union carbide A-162s, 20 grams of dehydrated alcohols and 30 grams of distilled water again to join respectively in another beaker, and in beaker, instill a little hydrochloric acid the pH value of this mixture is adjusted to 2 ~ 3, prepare presoma solution of inorganic silicon dioxide sol-gel.By the above-mentioned paraffin wax emulsion uniform stirring under the rotating speed of 300 revs/min preparing gained, and ammonia soln is instilled in beaker, milk sap pH value is transferred to 10, again presoma silicon dioxide gel dropwise is joined in above-mentioned paraffin wax emulsion, stir this mixing solutions 120 minutes, its temperature controls at 75 DEG C.The organic phase change energy storage material of inorganic materials shell micropackaging is obtained with this mixing solutions of filter paper filtering, by this composite phase-change energy storage material in vacuum drying oven dry 23 hours, the temperature of loft drier controls at 55 DEG C, obtains organic paraffin wax phase change energy storage material J of inorganic silicon dioxide shell encapsulation.
Comparative example 2
According to the method that CN101397489A describes, opening rubber mixing machine is warmed up to 180 DEG C, the high density polyethylene(HDPE) making to account for total system mass percent 19% is all after rolling melting, again by the paraffin accounting for total system mass percent 60% mixed, 10% ammonium polyphosphate, the tetramethylolmethane of 5%, the trimeric cyanamide of 5% and 1% iron powder join gradually in high density polyethylene(HDPE), melt blending 10 minutes again after adding, take out mixture, shaping, obtain flame-retardant shaping phase-change material K.
Comparative example 3
According to the method that CN101880521A describes, get 10g paraffin organic phase change material, 100ml distilled water and 0.2g sodium lauryl sulphate, blending and stirring at 70 DEG C, obtains paraffin wax emulsion.Take 40g tetraethoxy, 40g dehydrated alcohol and 80g distilled water, add in other beaker, its pH value is adjusted to about 2.5, blending and stirring at 50 DEG C, obtain silicon dioxide gel solution.Silicon dioxide gel dropwise is joined in paraffin wax emulsion, the final organic paraffin phase change material L obtaining inorganic silicon dioxide encapsulation.
In addition, in order to further illustrate the difference of flame retardant type organic phase change material prepared by the present invention and existing flame retardant type organic phase change material, listing table 1 and comparing.In table 1, limiting oxygen index(LOI) is for measuring the burning capacity of product, and limiting oxygen index(LOI) height represents that product is nonflammable, otherwise easily burns.According to GB GB 2406-80, limiting oxygen index(LOI) <22 belongs to inflammable material, and limiting oxygen index(LOI) >27 belongs to nonflammable material.Thermal release peak value is according to pyrolysis and combustion flowing calorimetric determination, and namely product heats up from room temperature, to 600 DEG C, and the Thermal release maximum that period occurs.Thermal release peak value is higher, illustrates at combustion processes product thermal discharge many, and namely disaster hidden-trouble is large, and flame retardant effect is bad; Otherwise disaster hidden-trouble is little, flame retardant effect is good.
The contrast of table 1 each halogen-free flame-retardant organic phase change material physicochemical property
As seen from Table 1, flame retardant type organic phase change material prepared by the present invention, in latent heat of phase change value and flame retardant properties, is all obviously better than existing flame retardant type organic phase change material.By adjustment preparation technology, higher flame retardant properties can be obtained.Composition graphs 3 can be found out, product prepared by the present invention, and after 600 DEG C of perfect combustion, the carbon-coating of Surface Creation covers evenly, does not have obvious gap, namely prevents the further extension of flame; And can find out at comparative example 3 composition graphs 2, after perfect combustion, there is gap in carbon-coating, and flame extends internally, and flame retardant properties is obviously not as good as product of the present invention.
In addition, in the test process to above-mentioned flame retardant type organic phase change material life cycle, find because the simple silicon-dioxide that uses is as cyst material, its toughness is poor, namely there is the phenomenon of latent heat of phase change value deep fades through the times of about 6 months, illustrate that the paraffin solution wherein encapsulated has leakage phenomenon; And it is melting in process mutually with organic basis material, there is the phenomenon of obvious layering and difficult mixing.Flame retardant type organic phase change material prepared by the present invention was through the continuous heat absorption-heat release test of 3 years, and obvious decline does not occur its latent heat of phase change value, and namely paraffin solution does not leak, and its with the mixing process of all types of body material in show well.
Claims (13)
1. a preparation method for flame retardant type organic phase change material, comprises the steps:
(1) organic phase change material and organic solvent are mixed, wherein the mass ratio of organic phase change material and organic solvent is 1:5 ~ 25;
(2) mixed with low-carbon alcohol by silicon-containing organic compound, described silicon-containing organic compound is triethoxysilicane phosphamide, and wherein the mass ratio of silicon-containing organic compound and low-carbon alcohol is 1:5 ~ 30;
(3) mixture of step (2) gained is dropwise added in the mixture of step (1) gained, after mixing, then add ammoniacal liquor, stir; Wherein the add-on of each material is by following ratio control: the mass ratio of silicon-containing organic compound and organic phase change material is 1 ~ 5:1, and the mass ratio of silicon-containing organic compound and ammonia is 1:0.5 ~ 4;
(4) after the solution of step (3) gained is cooled to room temperature, through rotary evaporation process, to products obtained therefrom washing, then through vacuum-drying, flame retardant type organic phase change material is obtained.
2. in accordance with the method for claim 1, it is characterized in that in step (1), described organic phase change material be selected from paraffin, higher fatty acid and ester class thereof one or more, the transformation temperature of organic phase change material is 25 DEG C ~ 58 DEG C.
3. in accordance with the method for claim 1, it is characterized in that the organic phase change material described in step (1) is paraffin, the transformation temperature of organic phase change material is 25 DEG C ~ 58 DEG C.
4. in accordance with the method for claim 1, it is characterized in that organic solvent used in step (1) is selected from sherwood oil, Skellysolve A, octane one or more, wherein sherwood oil is selected from the sherwood oil that boiling range is 60 DEG C ~ 90 DEG C.
5. in accordance with the method for claim 1, it is characterized in that in step (1), the mixing temperature of organic phase change material and organic solvent is 60 DEG C ~ 90 DEG C.
6. in accordance with the method for claim 1, it is characterized in that in step (2), triethoxysilicane phosphamide synthetic method is as follows: the dehydrated alcohol and the mixing of triethoxyl silane monomer that by mass ratio are 5 ~ 10:1, add Glacial acetic acid, wherein the add-on of Glacial acetic acid and the mass ratio of triethoxyl silane add-on are 0.1 ~ 2:1;
Then at 40 DEG C ~ 60 DEG C, dropwise add water under agitation condition, wherein the add-on of water and the mass ratio of triethoxyl silane are 0.1 ~ 1:1, and being stirred to reactant is colloidal sol shape;
The poly-phosphamide that molecular weight is 1000 ~ 5000 is added again in this system, the mass ratio of poly-phosphamide and triethoxyl silane is 0.5 ~ 1.5:1, violent stirring is to being uniformly dispersed, and then this mixture dry 2h ~ 5h under 80 DEG C ~ 120 DEG C conditions, obtains triethoxysilicane phosphamide.
7. in accordance with the method for claim 1, it is characterized in that in the low-carbon alcohol described in step (2), carbon number is 1 ~ 4.
8., according to the arbitrary described method of claim 1 ~ 5, it is characterized in that in step (3), the temperature controlling reaction system is 60 DEG C ~ 90 DEG C.
9. in accordance with the method for claim 1, it is characterized in that in step (3), the mass concentration of described ammoniacal liquor is 25% ~ 28%.
10. in accordance with the method for claim 1, it is characterized in that, in step (3), before ammoniacal liquor adds, adding water.
11. according to the method described in claim 1,9 or 10, it is characterized in that in step (3), the mass ratio 1 ~ 5:1 of the total Water in the hierarchy of control and silicon-containing organic compound.
12. in accordance with the method for claim 1, it is characterized in that the rotary evaporation described in step (4), and rotating speed is for being 150 ~ 300 rpm, and vacuum drying condition is as follows: vacuum tightness is 50 ~ 300Pa, and drying temperature is 10 ~ 50 DEG C, and time of drying is 5 ~ 70h.
13. 1 kinds of flame retardant type organic phase change materials, is characterized in that adopting the arbitrary described method of claim 1 ~ 12 to prepare.
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| CN105969315A (en) * | 2016-04-22 | 2016-09-28 | 江苏楚汉新能源科技有限公司 | Phase change thermal conducting material for lithium ion battery and preparation method thereof |
| CN106810761A (en) * | 2016-12-22 | 2017-06-09 | 阜阳市三郁包装材料有限公司 | Modified polypropylene flame redardant foamed board of a kind of hydridization polytetrafluoroethylene (PTFE) silica aerogel and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105220314A (en) * | 2015-11-13 | 2016-01-06 | 深圳市名仕度服饰有限公司 | A kind of resistance to 320 ~ 340 DEG C of fire-resistance cloths and preparation method thereof |
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| CN105969315A (en) * | 2016-04-22 | 2016-09-28 | 江苏楚汉新能源科技有限公司 | Phase change thermal conducting material for lithium ion battery and preparation method thereof |
| CN106810761A (en) * | 2016-12-22 | 2017-06-09 | 阜阳市三郁包装材料有限公司 | Modified polypropylene flame redardant foamed board of a kind of hydridization polytetrafluoroethylene (PTFE) silica aerogel and preparation method thereof |
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Application publication date: 20150506 |