CN108841361A - A kind of preparation method of rancid object sizing heat-storing material - Google Patents
A kind of preparation method of rancid object sizing heat-storing material Download PDFInfo
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- 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
- C09K5/063—Materials absorbing or liberating heat during crystallisation; Heat storage materials
Abstract
The present invention relates to a kind of preparation methods of rancid object sizing heat-storing material, belong to heat-storing material preparation technical field.The present invention is made in heat-storing material first that biomass grease and carbon nano-fiber mixing is rancid, biomass hydrolysis spoiled by rancid oil or fat is generated into abundant fatty acid and free property ester group using microorganism under the air-proof condition of high temperature and humidity, it is polymerized by monomer methyl acrylate, it is a kind of rigid, hard colourless transparent material, it can guarantee that matrix does not deform or melts when fatty acid melts, play the role of matrix protection, to reach styling, on the other hand, the free property ester group of rancid generation can be introduced in carbon nano-fiber surface under the action of microorganism, the carbon nano-fiber of high-termal conductivity is introduced into composite setting heat-storing material, also the thermal coefficient of composite setting heat-storing material can be promoted, rancid object sizing heat-storing material produced by the present invention is not easy to reveal, and thermal coefficient is high, it has broad application prospects.
Description
Technical field
The present invention relates to a kind of preparation methods of rancid object sizing heat-storing material, belong to heat-storing material preparation technical field.
Background technique
Heat-storing material is exactly a kind of new chemical material that can store thermal energy.Object phase transformation occurs in it within specified temperatures
Change, and along with absorbing or releasing heat, can be used to the temperature for controlling ambient enviroment, or to store thermal energy.It heat or
Cooling capacity stores, it is released again when needed, to improve the utilization rate of the energy.
The course of work of heat-storing material includes two stages：First is that the storage stage of heat, i.e., extra dynamic in peak period
Power, industrial exhaust heat waste heat or solar energy etc. are stored by heat-storing material；Second is that the release stage of heat, i.e., lead to when in use
It crosses heat-storing material and releases heat, for heating, heat supply etc..Heat storage and release step cycle carry out, so that it may utilize storage
Hot material solves the incoordination of thermal energy over time and space, reaches high efficiency of energy and utilizes and energy-efficient purpose.
Divide by heat storage type, heat-storing material can be divided into four classes：Sensible heat heat-storing material, phase change heat storage material, heat chemistry
Heat-storing material and adsorptive heat-storage material.Sensible heat heat-storing material is the storage that heat is carried out using the change procedure of substance self-temperature
It deposits, since direct contact heat transfer or fluid inherently heat storage medium can be used, thus storage, exothermic process are relatively
It simply, is early stage to apply more heat-storing material.Sensible heat heat storage technology the most also compares into all heat-storing materials
It is ripe.Phase change heat storage material is using substance in phase transformation（Such as solidification/fusing, condensation/vaporization, solidification/distillation）What process occurred
The heat of transformation carries out the storage and utilization of heat.Compared with sensible heat heat-storing material, phase change heat storage material thermal storage density is high, Neng Goutong
It crosses phase transformation and releases amount of heat at a constant temperature.Heat chemistry heat-storing material is mostly using metal hydride and amic to sting inverse chemistry anti-
Accumulation of heat should be carried out, thermal response speed is fast when having catalyst, temperature height and far from equilibrium state.It is external to be carried out too using this reaction
Sun can store the experimental study of heat power generation, but need emphasis to consider the tightness of storage container and system, and generate gas to material
Corrosion the problems such as.When absorption refers to fluid phase with being in contact with porous solid particle, suction of the solid particle to adsorbate
Or withhold process.Because of the heterogencity on adsorbent solids surface, the conversion effet of energy is generated along with adsorption process, referred to as
Heat of adsorption.For heat-storing material common at present since chemical reaction leads to accumulation of heat material volume change, expansion or shrinkage is unformed, holds
Easily leakage, there is also the low defects of thermal coefficient.Therefore, a kind of rancid object sizing storage for being not easy to reveal and thermal coefficient is high is invented
Hot material has positive effect to heat-storing material preparation technical field.
Summary of the invention
Present invention mainly solves the technical issues of, for common heat-storing material at present since chemical reaction leads to accumulation of heat material
Volume change, expansion or shrinkage is unformed, is easy leakage, and there is also the low defects of thermal coefficient, and it is fixed to provide a kind of rancid object
The preparation method of type heat-storing material.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that：
A kind of preparation method of rancid object sizing heat-storing material, it is characterised in that specifically preparation step is：
（1）It weighs leaf fat and is put into 20~30min of crushing in tissue pulverizer, be put into iron pan after crushed material and water are mixed,
Infusion after infusion, uses screen filtration, isolated filtrate while hot；
（2）It is poured into stainless steel pallet after above-mentioned filtrate and carbon nano-fiber are mixed, and stainless steel pallet is moved into closed temperature
In room, rancid processing 5~7 days are stood, rancid product is obtained, it is spare；
（3）Methyl methacrylate is added into separatory funnel, is washed with the sodium hydroxide solution that mass fraction is 5% to washing
Liquid is in colourless, then is washed with deionized to neutrality, is dried over anhydrous sodium sulfate air-distillation after 5~7 days, and collect 98~
100 DEG C of fraction obtains refining methacylic acid methyl esters；
（4）It is fitted into round-bottomed flask after above-mentioned refining methacylic acid methyl esters and azodiisobutyronitrile are mixed, is placed on shaking table
Upper oscillation, which is mixed to azodiisobutyronitrile, to be completely dissolved, then round-bottomed flask is moved into water-bath, is heated to 80~90 DEG C,
20~30min is stirred with the revolving speed of 200~300r/min with blender, obtains covering liquid；
（5）Spare rancid product is heated to 50~60 DEG C, obtains melting rancid product, then rancid product will be melted and fallen
Enter in above-mentioned covering liquid, is stirred to react 15~20min at 50~60 DEG C and obtains performed polymer；
（6）Above-mentioned performed polymer is poured into mold, then mold is placed in the thermostatic water bath that temperature is 65~70 DEG C, standing 2~
3h is being heated to 90~100 DEG C, continue stand polymerization 1~2h, stand polymerization after cooled to room temperature, demoulding,
Up to rancid object sizing heat-storing material.
Step（1）Described in crushed material and water mass ratio be 5:1, the temperature of infusion is 100~105 DEG C, infusion
Time is 1~2h.
Step（2）Described in filtrate and carbon nano-fiber mass ratio be 10:1, the temperature in closed greenhouse is 35~45
DEG C, relative air humidity is 60~70%.
Step（4）Described in refining methacylic acid methyl esters and azodiisobutyronitrile mass ratio be 500:1.
Step（5）Described in the rancid product of melting and the mass ratio of covering liquid be 1:2.
The beneficial effects of the invention are as follows：
The invention firstly uses biomass leaf fats as raw material, biomass grease is obtained after high temperature infusion, by bio-oil
Rouge and carbon nano-fiber with high-termal conductivity are blended, and are placed on rancid in the greenhouse of high temperature, high humidity and sealing, obtain rancid production
Object, then select polymethyl methacrylate as fatty acid amorphous matrix, pass through the bulk polymerization of methyl methacrylate monomer
Reaction by rancid product package, is fixed in the base, and rancid object sizing heat-storing material is prepared, and accumulation of heat material is made in the present invention
It is first that biomass grease and carbon nano-fiber mixing is rancid in material, it will be given birth under the air-proof condition of high temperature and humidity using microorganism
Substance hydrolysis spoiled by rancid oil or fat generates abundant fatty acid and free property ester group, and the fatty acid on the one hand generated is a kind of non-convention
The phase change heat storage material thought, and fatty acid and methyl methacrylate are all oiliness organic matter, and the two has good miscible
Property and compatibility, are easily formed homogeneous, isotropic composite material, polymethyl methacrylate is commonly called as organic glass, by list
Body methyl acrylate is polymerized, and is a kind of rigid, hard colourless transparent material, the softening point of polymethyl methacrylate and point
Solve temperature be respectively 100 DEG C and 360 DEG C or so, be above the fusing point of fatty acid, it is ensured that fatty acid melt when matrix not
It deforms or melts, play the role of matrix protection, thus reach styling, on the other hand, the free property of rancid generation
Ester group can be introduced in carbon nano-fiber surface under the action of microorganism, to increase the oleophylic of carbon nano-fiber
Property, so that modified Nano carbon fibers peacekeeping oiliness Coated with Organic Matter matrix polymethyl methacrylate compatibility improves, Xiang Fu
The carbon nano-fiber for introducing high-termal conductivity in sizing heat-storing material is closed, the thermal coefficient of composite setting heat-storing material can be also promoted,
Rancid object sizing heat-storing material produced by the present invention is not easy to reveal, and thermal coefficient is high, has broad application prospects.
Specific embodiment
It weighs leaf fat and is put into 20~30min of crushing in tissue pulverizer, be in mass ratio 5 by crushed material and water:1 mixing
After be put into iron pan, be heated to 100~105 DEG C, keep the temperature 1~2h of infusion, after infusion, use screen filtration while hot, point
From obtaining filtrate；It is in mass ratio 10 by above-mentioned filtrate and carbon nano-fiber:It is poured into stainless steel pallet after 1 mixing, and will not
It is 35~45 DEG C that the steel tray that becomes rusty, which moves into temperature, in the closed greenhouse that relative air humidity is 60~70%, stands rancid processing 5~7
It, obtains rancid product, spare；Methyl methacrylate is added into separatory funnel, the sodium hydroxide for being 5% with mass fraction
It is in colourless that solution, which is washed to cleaning solution, then is washed with deionized to neutrality, and normal pressure steams after being dried over anhydrous sodium sulfate 5~7 days
It evaporates, and collects 98~100 DEG C of fraction, obtain refining methacylic acid methyl esters；It is in mass ratio 500:1 by above-mentioned purification methyl
It is fitted into round-bottomed flask after methyl acrylate and azodiisobutyronitrile mixing, is placed on oscillation on shaking table and mixes to two isobutyl of azo
Nitrile is completely dissolved, then round-bottomed flask is moved into water-bath, 80~90 DEG C is heated to, with blender with 200~300r/
The revolving speed of min is stirred 20~30min, obtains covering liquid；Spare rancid product is heated to 50~60 DEG C, is obtained
Rancid product is melted, then is in mass ratio 1:2, which will melt rancid product, pours into above-mentioned covering liquid, stirs at 50~60 DEG C anti-
15~20min is answered to obtain performed polymer；Above-mentioned performed polymer is poured into mold, then mold is placed in the constant temperature that temperature is 65~70 DEG C
In sink, 2~3h is stood, is being heated to 90~100 DEG C, continued to stand 1~2h of polymerization, stand naturally cold after polymerizeing
But to room temperature, demoulding is to get rancid object sizing heat-storing material.
Example 1
It weighs leaf fat and is put into tissue pulverizer and crush 20min, be in mass ratio 5 by crushed material and water:Iron is put into after 1 mixing
In pot, 100 DEG C are heated to, keeps the temperature infusion 1h, after infusion, uses screen filtration, isolated filtrate while hot；It will be above-mentioned
Filtrate and carbon nano-fiber are 10 in mass ratio:It is poured into stainless steel pallet after 1 mixing, and is by stainless steel pallet immigration temperature
35 DEG C, relative air humidity is in 60% closed greenhouse, the rancid processing of standing 5 days obtains rancid product, spare；It is leaked to liquid separation
Methyl methacrylate is added in bucket, it is in colourless for being washed with the sodium hydroxide solution that mass fraction is 5% to cleaning solution, then is spent
Ion water washing is dried over anhydrous sodium sulfate air-distillation after 5 days to neutrality, and collects 98 DEG C of fraction, obtains purification methyl
Methyl acrylate；It is in mass ratio 500:1 will above-mentioned refining methacylic acid methyl esters and azodiisobutyronitrile mix after be packed into circle
It in the flask of bottom, is placed on shaking table oscillation and mixes to azodiisobutyronitrile and be completely dissolved, then round-bottomed flask is moved into water-bath,
80 DEG C are heated to, 20min is stirred with the revolving speed of 200r/min with blender, obtains covering liquid；It will be spare rancid
Product is heated to 50 DEG C, obtains melting rancid product, then be in mass ratio 1:2, which will melt rancid product, pours into above-mentioned cladding
In liquid, 15min is stirred to react at 50 DEG C and obtains performed polymer；Above-mentioned performed polymer is poured into mold, then mold is placed in temperature
To stand 2h, being heated to 90 DEG C in 65 DEG C of thermostatic water baths, continues to stand polymerization 1h, stand natural after polymerizeing
It is cooled to room temperature, demoulding is to get rancid object sizing heat-storing material.
Example 2
It weighs leaf fat and is put into tissue pulverizer and crush 25min, be in mass ratio 5 by crushed material and water:Iron is put into after 1 mixing
In pot, 102 DEG C are heated to, keeps the temperature infusion 1.5h, after infusion, uses screen filtration, isolated filtrate while hot；It will be upper
It states filtrate and carbon nano-fiber is 10 in mass ratio:It is poured into stainless steel pallet after 1 mixing, and stainless steel pallet is moved into temperature
It is 40 DEG C, in the closed greenhouse that relative air humidity is 65%, stands rancid processing 6 days, obtain rancid product, it is spare；To liquid separation
Methyl methacrylate is added in funnel, it is in colourless for being washed with the sodium hydroxide solution that mass fraction is 5% to cleaning solution, then is used
Deionized water is washed to neutrality, and air-distillation after 6 days is dried over anhydrous sodium sulfate, and collects 99 DEG C of fraction, obtains purification first
Base methyl acrylate；It is in mass ratio 500:1 will be packed into after above-mentioned refining methacylic acid methyl esters and azodiisobutyronitrile mixing
It in round-bottomed flask, is placed on shaking table oscillation and mixes to azodiisobutyronitrile and be completely dissolved, then round-bottomed flask is moved into water-bath
In, 85 DEG C are heated to, 25min is stirred with the revolving speed of 250r/min with blender, obtains covering liquid；By spare acid
It loses product and is heated to 55 DEG C, obtain melting rancid product, then be in mass ratio 1:2, which will melt rancid product, pours into above-mentioned packet
In covering liquid, 17min is stirred to react at 55 DEG C and obtains performed polymer；Above-mentioned performed polymer is poured into mold, then mold is placed in temperature
Degree continues to stand polymerization 1.5h, stands polymerization knot to stand 2.5, being heated to 95 DEG C in 65~70 DEG C of thermostatic water bath
Cooled to room temperature after beam, demoulding is to get rancid object sizing heat-storing material.
Example 3
It weighs leaf fat and is put into tissue pulverizer and crush 30min, be in mass ratio 5 by crushed material and water:Iron is put into after 1 mixing
In pot, 105 DEG C are heated to, keeps the temperature infusion 2h, after infusion, uses screen filtration, isolated filtrate while hot；It will be above-mentioned
Filtrate and carbon nano-fiber are 10 in mass ratio:It is poured into stainless steel pallet after 1 mixing, and is by stainless steel pallet immigration temperature
45 DEG C, relative air humidity is in 70% closed greenhouse, the rancid processing of standing 7 days obtains rancid product, spare；It is leaked to liquid separation
Methyl methacrylate is added in bucket, it is in colourless for being washed with the sodium hydroxide solution that mass fraction is 5% to cleaning solution, then is spent
Ion water washing is dried over anhydrous sodium sulfate air-distillation after 7 days to neutrality, and collects 100 DEG C of fraction, obtains purification methyl
Methyl acrylate；It is in mass ratio 500:1 will above-mentioned refining methacylic acid methyl esters and azodiisobutyronitrile mix after be packed into circle
It in the flask of bottom, is placed on shaking table oscillation and mixes to azodiisobutyronitrile and be completely dissolved, then round-bottomed flask is moved into water-bath,
90 DEG C are heated to, 30min is stirred with the revolving speed of 300r/min with blender, obtains covering liquid；It will be spare rancid
Product is heated to 60 DEG C, obtains melting rancid product, then be in mass ratio 1:2, which will melt rancid product, pours into above-mentioned cladding
In liquid, 20min is stirred to react at 60 DEG C and obtains performed polymer；Above-mentioned performed polymer is poured into mold, then mold is placed in temperature
To stand 3h, being heated to 100 DEG C in 70 DEG C of thermostatic water baths, continues to stand polymerization 2h, stand natural after polymerizeing
It is cooled to room temperature, demoulding is to get rancid object sizing heat-storing material.
Comparative example
Rancid object sizing produced by the present invention is stored as a comparison case with the rancid object sizing heat-storing material of Shanghai company production
Rancid object sizing heat-storing material in hot material and comparative example carries out performance detection, and testing result is as shown in table 1：
Test method：
Thermal storage density test is detected using heat storage coefficient tester；
Thermal conductivity test is detected using conductometer；
Volume change and sizing test：Heat-storing material in example 1~3 and comparative example is passed through under the conditions of 450 DEG C of temperature
Whether after the test of 200 solidification thaw cycles and 500 solidification thaw cycles are tested, it is damaged to observe each heat-storing material appearance, and
Measure rate of mass reduction.
1 heat-storing material performance measurement result of table
According to there is some strength after the rancid object sizing heat-storing material sizing produced by the present invention of data among the above, it is not easy to send out
Raw deformation, under the conditions of 450 DEG C of temperature after 200 solidification thaw cycle tests and 500 solidification thaw cycle tests,
For appearance without breakage, rate of mass reduction is lower than 1.4%, is not susceptible to leak, and thermal storage density is high, and thermal conductivity is good, can be used in solar energy,
The application fields such as industrial afterheat recovery, have broad application prospects.
Claims (5)
1. a kind of preparation method of rancid object sizing heat-storing material, it is characterised in that specifically preparation step is：
（1）It weighs leaf fat and is put into 20~30min of crushing in tissue pulverizer, be put into iron pan after crushed material and water are mixed,
Infusion after infusion, uses screen filtration, isolated filtrate while hot；
（2）It is poured into stainless steel pallet after above-mentioned filtrate and carbon nano-fiber are mixed, and stainless steel pallet is moved into closed temperature
In room, rancid processing 5~7 days are stood, rancid product is obtained, it is spare；
（3）Methyl methacrylate is added into separatory funnel, is washed with the sodium hydroxide solution that mass fraction is 5% to washing
Liquid is in colourless, then is washed with deionized to neutrality, is dried over anhydrous sodium sulfate air-distillation after 5~7 days, and collect 98~
100 DEG C of fraction obtains refining methacylic acid methyl esters；
（4）It is fitted into round-bottomed flask after above-mentioned refining methacylic acid methyl esters and azodiisobutyronitrile are mixed, is placed on shaking table
Upper oscillation, which is mixed to azodiisobutyronitrile, to be completely dissolved, then round-bottomed flask is moved into water-bath, is heated to 80~90 DEG C,
20~30min is stirred with the revolving speed of 200~300r/min with blender, obtains covering liquid；
（5）Spare rancid product is heated to 50~60 DEG C, obtains melting rancid product, then rancid product will be melted and fallen
Enter in above-mentioned covering liquid, is stirred to react 15~20min at 50~60 DEG C and obtains performed polymer；
（6）Above-mentioned performed polymer is poured into mold, then mold is placed in the thermostatic water bath that temperature is 65~70 DEG C, standing 2~
3h is being heated to 90~100 DEG C, continue stand polymerization 1~2h, stand polymerization after cooled to room temperature, demoulding,
Up to rancid object sizing heat-storing material.
2. a kind of preparation method of rancid object sizing heat-storing material according to claim 1, it is characterised in that：Step
（1）Described in crushed material and water mass ratio be 5:1, the temperature of infusion is 100~105 DEG C, and the time of infusion is 1~2h.
3. a kind of preparation method of rancid object sizing heat-storing material according to claim 1, it is characterised in that：Step
（2）Described in filtrate and carbon nano-fiber mass ratio be 10:1, the temperature in closed greenhouse is 35~45 DEG C, and air is relatively wet
Degree is 60~70%.
4. a kind of preparation method of rancid object sizing heat-storing material according to claim 1, it is characterised in that：Step
（4）Described in refining methacylic acid methyl esters and azodiisobutyronitrile mass ratio be 500:1.
5. a kind of preparation method of rancid object sizing heat-storing material according to claim 1, it is characterised in that：Step
（5）Described in the rancid product of melting and the mass ratio of covering liquid be 1:2.
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Cited By (1)
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Application publication date: 20181120 |