CN115260771B - Mining high-flexibility phase-change cold storage material and preparation method thereof - Google Patents
Mining high-flexibility phase-change cold storage material and preparation method thereof Download PDFInfo
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- CN115260771B CN115260771B CN202210746865.7A CN202210746865A CN115260771B CN 115260771 B CN115260771 B CN 115260771B CN 202210746865 A CN202210746865 A CN 202210746865A CN 115260771 B CN115260771 B CN 115260771B
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L87/00—Compositions of unspecified macromolecular compounds, obtained otherwise than by polymerisation reactions only involving unsaturated carbon-to-carbon bonds
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- 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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention relates to a mining high-flexibility phase-change cold storage material and a preparation method thereof, and belongs to the technical field of phase-change cold storage material preparation. Dissolving polyethylene glycol in DMF, adding 4, 4-diphenylmethane diisocyanate, and adding hydroxypropyl methylcellulose to obtain cellulose-polyethylene glycol oligomer; dispersing cellulose-polyethylene glycol oligomer in water, and adding a silane coupling agent KH550 to react to obtain silane-terminated cellulose-polyethylene glycol oligomer; and adding silicon rubber and glycerin into the inorganic filler composite silane end capped cellulose-polyethylene glycol oligomer, and uniformly mixing to obtain a finished product. According to the invention, the cellulose-polyethylene glycol oligomer is formed, the silicon-containing functional compound is used for end sealing, the regulation and control on the performance of the cellulose-polyethylene glycol graft are realized, the cellulose-polyethylene glycol graft with excellent comprehensive performance is designed, the material strength is increased through inorganic nano particles, and the high-flexibility silicon rubber is introduced to improve the flexibility of the material.
Description
Technical Field
The invention belongs to the technical field of phase change cold storage material preparation, and particularly relates to a mining high-flexibility phase change cold storage material and a preparation method thereof.
Background
The energy is the material basis of economic development, along with the continuous promotion of the industrialization progress, the coal consumption is continuously increased, underground shallow coal mine resources face to be exhausted, and meanwhile, the mechanized and automatic technology of the new generation of large-mining-height coal mine exploitation equipment is continuously improved, and the depth of mine exploitation is also increased. However, with the increase of the depth of the mine, high-temperature heat damage is easily caused by the over-high temperature of geological geothermal and underground rock, and the exploitation experience of deep coal mines in some major mining countries in the world shows that when the exploitation depth reaches 1000m, the temperature of raw rock can reach 60 ℃ at most, and the heat emitted during the operation of mechanical and electromechanical equipment, the heat generated by air compression, the heat dissipation of human bodies of coal workers and other comprehensive factors are added, so that the severe degree of the underground operation environment is extremely harmful to the life safety of the workers, and therefore, the mine high-temperature heat damage becomes a sixth natural disaster after coal mine gas, water burst, fire disaster and powder sitting on a roof.
In order to ensure the physical and psychological health and the safe production of coal mine workers, the traditional protection modes comprise mechanical refrigeration, mechanical ice making, heat pipe cooling, air compression refrigeration and the like, but the traditional protection modes also have the defects of high energy consumption, poor effect, complex implementation and the like. With the progress of material science and technology and the upgrade of intelligent manufacturing technology, the realization of human body cooling by wearable individual protection mode gradually becomes the emerging direction of current research, so a phase change cold storage material with good strength, toughness and thermal stability and high heat absorption and energy storage efficiency is needed.
Disclosure of Invention
The invention aims to provide a mining high-flexibility phase-change cold storage material and a preparation method thereof, and solves the problems of large energy consumption, poor effect, complex implementation and the like of the traditional protection modes including mechanical refrigeration, mechanical ice making, heat pipe cooling, air compression refrigeration and the like in the prior art.
The aim of the invention can be achieved by the following technical scheme:
a preparation method of a mining high-flexibility phase change cold storage material comprises the following steps:
s1, dissolving polyethylene glycol in DMF, adding 4, 4-diphenylmethane diisocyanate, stirring at 80-100 ℃ under nitrogen atmosphere, keeping the reaction for 1-5h, adding hydroxypropyl methylcellulose after the reaction is finished, keeping the temperature for continuous reaction for 5-10h, and drying in an oven for 48h to obtain a cellulose-polyethylene glycol oligomer;
s2, ultrasonically dispersing the cellulose-polyethylene glycol oligomer in deionized water, adding a silane coupling agent KH550, reacting for 1-3 hours at 30-50 ℃, and adding absolute ethyl alcohol after the reaction is finished to stably obtain a silane-terminated cellulose-polyethylene glycol oligomer;
s3, adding inorganic filler into absolute ethyl alcohol, carrying out ultrasonic mixing to obtain a dispersion liquid, adding silane-terminated cellulose-polyethylene glycol oligomer into the suspension liquid, carrying out ultrasonic mixing uniformly, and filtering to obtain an inorganic filler composite silane-terminated cellulose-polyethylene glycol oligomer;
s4, mixing the inorganic filler composite silane end capped cellulose-polyethylene glycol oligomer and the silicon rubber, adding a proper amount of glycerol, and uniformly mixing to obtain a finished product.
As a preferable technical scheme of the invention:
in the step S1, the dosage ratio of the polyethylene glycol, the DMF, the 4, 4-diphenylmethane diisocyanate and the hydroxypropyl methylcellulose is 8-10g:100-200mL:2.5-4g:0.5-0.7g.
In the step S2, the dosage ratio of the cellulose-polyethylene glycol oligomer, the deionized water and the silane coupling agent KH550 is 1-5g:300-400mL:30-50mL.
In the step S3, the dosage ratio of the inorganic filler to the silane-terminated cellulose-polyethylene glycol oligomer is 0.1-0.5g:3-6g.
In the step S4, the dosage ratio of the inorganic filler composite silane end capped cellulose-polyethylene glycol oligomer, the silicon rubber and the glycerol is 5-10g:1-5g:0.5-1mL.
The inorganic filler is prepared from the following components in percentage by mass: 1-2, wherein the particle size of the silicon dioxide is 10-50 mu m, and the particle size of the hollow glass beads is 2-10 mu m.
The molecular weight of the polyethylene glycol is 1000-6000.
Compared with the prior art, the invention has the beneficial effects that:
1) The invention utilizes the advantage of strong designability of grafted polymer molecules, selects hydroxypropyl methyl cellulose as a molecular skeleton, forms cellulose-polyethylene glycol oligomer by grafting serial functionalized polyethylene glycol, and carries out end sealing by a silicon-containing functional compound, adjusts the proportion of a soft segment and a hard segment to realize the regulation and control of the performance of the cellulose-polyethylene glycol graft, realizes the controllable distribution of functional structural units on the hydroxypropyl methyl cellulose main chain, and synthesizes the cellulose-polyethylene glycol graft with specific structure and excellent comprehensive performance.
2) The invention adopts SiO 2 And inorganic fillers such as hollow glass beads and the like are compounded with cellulose-polyethylene glycol phase change composite materials capped by silicon-containing functional compounds, and organic-inorganic hybridization crosslinking between the silicon-containing functional compounds and the inorganic fillers is utilized to jointly construct a multi-crosslinking network structure with crosslinking between hard segments and soft segments of a multifunctional structure, so that the strength, toughness and thermal stability of the material are improved.
3) According to the technical scheme, the high-flexibility silicone rubber and the cellulose-polyethylene glycol oligomer are mixed and compounded, physical crosslinking effects such as molecular chain entanglement are utilized, the acting force and crosslinking density of a two-phase interface are improved, meanwhile, the proportion of a molecular chain structure, the molecular weight and two components is regulated, the phase state structure of the two phases is regulated and controlled, the interfacial adhesion between the two phases is improved, the flexibility of the material is improved, and meanwhile, the heat absorption and energy storage efficiency of the material is guaranteed to the greatest extent.
4) The mining high-flexibility phase-change cold storage material prepared by the invention has larger phase-change latent heat and proper phase-change temperature, can not harden after freezing, can keep proper softness, can increase human comfort when being applied to cooling clothes, and improves use comfort. Meanwhile, the preparation method is simple and is beneficial to large-scale production.
Drawings
Fig. 1 is a schematic structural diagram of a mining high-flexibility phase change cold storage material prepared by the method.
Figures 2, 3 and 4 are DSC curves of three mining high-flexibility phase-change cold-storage materials prepared in examples 1, 2 and 3 respectively.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Referring to FIG. 1, siO 2 And the hollow glass beads are compounded with the cellulose-polyethylene glycol phase-change composite material capped by the silicon-containing functional compound, and the organic-inorganic hybrid crosslinking between the silicon-containing functional compound and the inorganic filler is utilized to jointly construct a multi-crosslinking network structure with the crosslinking between the hard segment and the soft segment of the multifunctional structure, so that the strength, the toughness and the thermal stability of the material are improved.
Example 1
The preparation method of the mining high-flexibility phase-change cold storage material comprises the following steps:
s1, 8g of polyethylene glycol 1000 is dissolved in 100mL of DMF, 2.5g of 4, 4-diphenylmethane diisocyanate is added, stirring is carried out at 90 ℃ under nitrogen atmosphere, reaction is kept for 3h, 0.5g of hydroxypropyl methylcellulose is added after the reaction is finished, heat preservation is carried out for continuous reaction for 7h, and then the mixture is placed in an oven for drying for 48h, thus obtaining the cellulose-polyethylene glycol oligomer.
S2, ultrasonically dispersing 1g of cellulose-polyethylene glycol oligomer in 300mL of deionized water, adding 30mL of silane coupling agent KH550, reacting for 3h at 50 ℃, and adding absolute ethyl alcohol after the reaction is finished to stably obtain the silane-terminated cellulose-polyethylene glycol oligomer.
S3, adding 0.1g of inorganic filler (silicon dioxide and hollow glass beads with the mass ratio of 1:1, the particle size of the silicon dioxide being 10 mu m, the particle size of the hollow glass beads being 2 mu m) into 50mL of absolute ethyl alcohol, ultrasonically mixing for 30min to obtain a dispersion liquid, adding 3g of silane end capped cellulose-polyethylene glycol oligomer into the suspension liquid, ultrasonically mixing uniformly, and filtering to obtain the inorganic filler composite silane end capped cellulose-polyethylene glycol oligomer.
S4, mixing 5g of inorganic filler composite silane end capped cellulose-polyethylene glycol oligomer with 3g of silicone rubber, adding 1mL of glycerol, and uniformly mixing to obtain a finished product.
After fully cooling at room temperature, the result is shown in figure 2, the phase change latent heat is larger (258J/g), the initial melting temperature (phase change temperature) is-4.1 ℃, and the cold storage agent material with better performance is obtained.
Example 2
The preparation method of the mining high-flexibility phase-change cold storage material comprises the following steps:
s1, 9g of polyethylene glycol 4000 is dissolved in 150mL of DMF, 3g of 4, 4-diphenylmethane diisocyanate is added, stirring is carried out at 95 ℃ under nitrogen atmosphere, reaction is kept for 4 hours, 0.65g of hydroxypropyl methylcellulose is added after the reaction is finished, the reaction is kept for 8 hours, and the mixture is dried in an oven for 48 hours to obtain the cellulose-polyethylene glycol oligomer.
S2, ultrasonically dispersing 3g of cellulose-polyethylene glycol oligomer in 350mL of deionized water, adding 45mL of silane coupling agent KH550, reacting for 2h at 45 ℃, and adding absolute ethyl alcohol after the reaction is finished to stably obtain the silane-terminated cellulose-polyethylene glycol oligomer.
S3, adding 0.3g of inorganic filler (silicon dioxide and hollow glass beads with the mass ratio of 1:1.5, the particle size of the silicon dioxide being 30 mu m, the particle size of the hollow glass beads being 6 mu m) into 50mL of absolute ethyl alcohol, ultrasonically mixing for 30min to obtain dispersion liquid, adding 4.5g of silane-terminated cellulose-polyethylene glycol oligomer into the suspension liquid, ultrasonically mixing uniformly, and filtering to obtain the inorganic filler composite silane-terminated cellulose-polyethylene glycol oligomer.
S4, mixing 8g of inorganic filler composite silane end capped cellulose-polyethylene glycol oligomer with 5g of silicone rubber, adding 1mL of glycerol, and uniformly mixing to obtain a finished product.
After cooling sufficiently at room temperature, the result is shown in figure 3, the phase change latent heat is larger (249.6J/g), the initial melting temperature (phase change temperature) is-5.1 ℃, and the cold storage agent material with better performance is obtained.
Example 3
The preparation method of the mining high-flexibility phase-change cold storage material comprises the following steps:
s1, dissolving 10g of polyethylene glycol 6000 in 200mL of DMF, adding 4g of 4, 4-diphenylmethane diisocyanate, stirring at 80 ℃ under nitrogen atmosphere, keeping the reaction for 2h, adding 0.7g of hydroxypropyl methylcellulose after the reaction is finished, keeping the temperature for continuous reaction for 10h, and drying in an oven for 48h to obtain the cellulose-polyethylene glycol oligomer.
S2, dispersing 5g of cellulose-polyethylene glycol oligomer in 400mL of deionized water by ultrasonic, adding 50mL of silane coupling agent KH550, reacting for 2h at 35 ℃, and adding absolute ethyl alcohol after the reaction is finished to stably obtain the silane-terminated cellulose-polyethylene glycol oligomer.
S3, adding 0.45g of inorganic filler (silicon dioxide and hollow glass beads with the mass ratio of 1:2, the particle size of the silicon dioxide being 50 mu m, the particle size of the hollow glass beads being 8 mu m) into 60mL of absolute ethyl alcohol, ultrasonically mixing for 30min to obtain a dispersion liquid, adding 6g of silane end capped cellulose-polyethylene glycol oligomer into the suspension liquid, ultrasonically mixing uniformly, and filtering to obtain the inorganic filler composite silane end capped cellulose-polyethylene glycol oligomer.
S4, mixing 10g of inorganic filler composite silane end capped cellulose-polyethylene glycol oligomer with 2g of silicone rubber, adding 1mL of glycerol, and uniformly mixing to obtain a finished product.
After cooling sufficiently at room temperature, the result is shown in FIG. 4, the latent heat of phase change is larger (280.6J/g), the initial melting temperature (phase change temperature) is-1.5 ℃, and the cold storage agent material with better performance is obtained.
The foregoing is merely illustrative and explanatory of the principles of the invention, as various modifications and additions may be made to the specific embodiments described, or similar thereto, by those skilled in the art, without departing from the principles of the invention or beyond the scope of the appended claims.
Claims (5)
1. The preparation method of the mining high-flexibility phase-change cold storage material is characterized by comprising the following steps of:
s1, dissolving polyethylene glycol in DMF, adding 4, 4-diphenylmethane diisocyanate, stirring at 80-100 ℃ under nitrogen atmosphere, keeping the reaction for 1-5h, adding hydroxypropyl methylcellulose after the reaction is finished, keeping the temperature for continuous reaction for 5-10h, and drying in an oven to obtain a cellulose-polyethylene glycol oligomer;
s2, ultrasonically dispersing the cellulose-polyethylene glycol oligomer in deionized water, adding a silane coupling agent KH550, reacting for 1-3 hours at 30-50 ℃, and adding absolute ethyl alcohol after the reaction is finished to stably obtain a silane-terminated cellulose-polyethylene glycol oligomer;
s3, adding inorganic filler into absolute ethyl alcohol, carrying out ultrasonic mixing to obtain dispersion liquid, and adding silane end capped cellulose-polyethylene glycol oligomer into the suspension liquid, wherein the dosage ratio of the inorganic filler to the silane end capped cellulose-polyethylene glycol oligomer is 0.1-0.5g:3-6g, after ultrasonic mixing, filtering to obtain inorganic filler composite silane end capped cellulose-polyethylene glycol oligomer;
wherein the inorganic filler is prepared from the following components in percentage by mass: 1-2, wherein the particle size of the silicon dioxide is 10-50 mu m, and the particle size of the hollow glass beads is 2-10 mu m;
s4, mixing the inorganic filler composite silane end-capped cellulose-polyethylene glycol oligomer with the silicon rubber, and adding glycerol, wherein the dosage ratio of the inorganic filler composite silane end-capped cellulose-polyethylene glycol oligomer to the silicon rubber to the glycerol is 5-10g:1-5g: and (3) 0.5-1mL, and uniformly mixing to obtain a finished product.
2. The method according to claim 1, wherein in the step S1, the ratio of the polyethylene glycol, DMF, 4-diphenylmethane diisocyanate and hydroxypropyl methylcellulose is 8-10g:100-200mL:2.5-4g:0.5-0.7g.
3. The preparation method according to claim 1, wherein in step S2, the dosage ratio of the cellulose-polyethylene glycol oligomer, deionized water and the silane coupling agent KH550 is 1 to 5g:300-400mL:30-50mL.
4. The method of claim 1, wherein the polyethylene glycol has a molecular weight of 1000 to 6000.
5. A mining highly flexible phase change cold storage material made by the method of any one of claims 1-4.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106084179A (en) * | 2016-06-08 | 2016-11-09 | 东莞市吉鑫高分子科技有限公司 | A kind of high-strength thermoplastic polyurethane solid-solid phase change energy storage material and preparation method thereof |
| CN106811179A (en) * | 2017-01-03 | 2017-06-09 | 温州大学 | The preparation method of polyethylene glycol/silicon dioxide composite phase-change energy storage material |
| CN110804301A (en) * | 2019-12-11 | 2020-02-18 | 桂林电子科技大学 | Polyethylene glycol/hydroxypropyl cellulose carbon nanotube composite solid-solid phase change material and preparation method thereof |
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| US8852488B2 (en) * | 2004-04-12 | 2014-10-07 | Mohini M. Sain | Manufacturing process for high performance short ligno-cellulosic fibre—thermoplastic composite materials |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106084179A (en) * | 2016-06-08 | 2016-11-09 | 东莞市吉鑫高分子科技有限公司 | A kind of high-strength thermoplastic polyurethane solid-solid phase change energy storage material and preparation method thereof |
| CN106811179A (en) * | 2017-01-03 | 2017-06-09 | 温州大学 | The preparation method of polyethylene glycol/silicon dioxide composite phase-change energy storage material |
| CN110804301A (en) * | 2019-12-11 | 2020-02-18 | 桂林电子科技大学 | Polyethylene glycol/hydroxypropyl cellulose carbon nanotube composite solid-solid phase change material and preparation method thereof |
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