CN105419732B - A kind of preparation method of ternary nitric acid fuse salt phase-change heat-storage material - Google Patents
A kind of preparation method of ternary nitric acid fuse salt phase-change heat-storage material Download PDFInfo
- Publication number
- CN105419732B CN105419732B CN201510908061.2A CN201510908061A CN105419732B CN 105419732 B CN105419732 B CN 105419732B CN 201510908061 A CN201510908061 A CN 201510908061A CN 105419732 B CN105419732 B CN 105419732B
- Authority
- CN
- China
- Prior art keywords
- nitric acid
- storage material
- fuse salt
- change heat
- salt phase
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 150000003839 salts Chemical class 0.000 title claims abstract description 77
- 238000005338 heat storage Methods 0.000 title claims abstract description 68
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 229910017604 nitric acid Inorganic materials 0.000 title claims abstract description 61
- 239000011232 storage material Substances 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims abstract description 124
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims abstract description 120
- 239000000843 powder Substances 0.000 claims abstract description 90
- 235000010333 potassium nitrate Nutrition 0.000 claims abstract description 62
- 239000004323 potassium nitrate Substances 0.000 claims abstract description 62
- 235000010344 sodium nitrate Nutrition 0.000 claims abstract description 60
- 239000004317 sodium nitrate Substances 0.000 claims abstract description 60
- CFYGEIAZMVFFDE-UHFFFAOYSA-N neodymium(3+);trinitrate Chemical compound [Nd+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O CFYGEIAZMVFFDE-UHFFFAOYSA-N 0.000 claims abstract description 58
- 238000000034 method Methods 0.000 claims abstract description 10
- 238000012545 processing Methods 0.000 claims abstract description 5
- 238000000498 ball milling Methods 0.000 claims description 30
- 238000001035 drying Methods 0.000 claims description 27
- 239000004570 mortar (masonry) Substances 0.000 claims description 26
- 238000010438 heat treatment Methods 0.000 claims description 18
- 239000011148 porous material Substances 0.000 claims description 15
- 239000000919 ceramic Substances 0.000 claims description 13
- 238000000227 grinding Methods 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 9
- 238000001291 vacuum drying Methods 0.000 claims description 9
- 150000002500 ions Chemical class 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 238000003701 mechanical milling Methods 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 3
- 239000004519 grease Substances 0.000 claims description 3
- 239000000155 melt Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- -1 salt neodymium nitrate Chemical class 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 3
- 230000008901 benefit Effects 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 229910002651 NO3 Inorganic materials 0.000 description 4
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 4
- 238000007580 dry-mixing Methods 0.000 description 3
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 235000002639 sodium chloride Nutrition 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- GTTYPHLDORACJW-UHFFFAOYSA-N nitric acid;sodium Chemical compound [Na].O[N+]([O-])=O GTTYPHLDORACJW-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000001938 differential scanning calorimetry curve Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 238000007500 overflow downdraw method Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
Landscapes
- Seasonings (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The preparation method of ternary nitric acid fuse salt phase-change heat-storage material disclosed by the invention, method particularly includes: 1) weigh sodium nitrate, potassium nitrate and neodymium nitrate, sodium nitrate, potassium nitrate, neodymium nitrate are crushed with mechanical crushing method, obtain sodium nitrate powder, potassium nitrate powder, neodymium nitrate powder；2) sodium nitrate powder, potassium nitrate powder, neodymium nitrate powder are mixed to obtain ternary nitric acid fuse salt phase-change heat-storage material precast body；3) first ternary nitric acid fuse salt phase-change heat-storage material precast body is melted, is then successively dried, ball mill crushing processing, obtains ternary nitric acid fuse salt phase-change heat-storage material.The preparation method of ternary nitric acid fuse salt phase-change heat-storage material of the present invention solve the problems, such as existing fuse salt phase-change heat-storage material during the preparation process it is existing it is at high cost, the production cycle is long and complex process, the ternary nitric acid fuse salt phase-change heat-storage material prepared have the advantages that use temperature range is wide, heat storage capacity is high, corrosivity is low and good fluidity.
Description
Technical field
The invention belongs to phase-change heat-storage material preparation method technical fields, and in particular to a kind of ternary nitric acid fuse salt phase transformation
The preparation method of heat accumulating.
Technical background
Solar energy is by earth rotation, intensity of illumination power, alternation of day and night, climatic season variation, geographical location difference
It influences, haves the defects that discontinuous and unstable, heat-storage technology can effectively get up intermittent heat storage, while need
Heat is released again when wanting, makes up shortage of heat, realizes the effect of " peak load shifting ".
Heat accumulating can be temporary unused industrial exhaust heat or unstable, discontinuous warm as the core of heat-storage technology
Amount (such as: solar energy, underground heat) is stored in medium appropriate, stable by certain method, continuous again when needed
Ground releases, and can reduce energy consumption in this way, reduce pollution, while be able to satisfy the strategy of sustainable development.
Fuse salt phase-change heat-storage material has nearly test in 30 years and applicating history in external solar energy thermal-power-generating field, but
It is domestic to put into operation not yet using mixed melting salt as heat absorption and the solar energy thermal-power-generating power station of heat-storage medium.
Nowadays, home and abroad solar energy thermal-power-generating fuse salt heat accumulating research and development trend is: polynary fused salt is blended
The fused salt that heat storage capacity is high, fusing point is suitable, corrosivity is small and thermal stability is good is made.It can be seen that preparing a kind of items
The excellent fuse salt phase-change heat-storage material of energy is the emphasis researched and developed in recent years.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation method of ternary nitric acid fuse salt phase-change heat-storage material, the preparation sides
Method has the characteristics that preparation cost is low and simple process, and the material prepared has that fusing point is suitable, heat storage capacity is big and thermostabilization
The good feature of property.
The technical scheme adopted by the invention is that a kind of preparation method of ternary nitric acid fuse salt phase-change heat-storage material, tool
Body follows the steps below to implement:
Step 1 weighs sodium nitrate, potassium nitrate, neodymium nitrate respectively, then by weighed sodium nitrate, potassium nitrate and neodymium nitrate
It is broken with mechanical crushing method, respectively obtain sodium nitrate powder, potassium nitrate powder, neodymium nitrate powder；
Step 2 mixes the sodium nitrate powder obtained through step 1, potassium nitrate powder, neodymium nitrate powder, obtains
Ternary nitric acid fuse salt phase-change heat-storage material precast body；
Step 3 first melts the ternary nitric acid fuse salt phase-change heat-storage material precast body obtained through step 2, then
It is successively dried, ball mill crushing processing, finally obtains ternary nitric acid fuse salt phase-change heat-storage material.
The features of the present invention also characterized in that:
Step 1.1 is that 50~60:40~50:1~5 distinguishes weighed sodium nitrate, potassium nitrate, neodymium nitrate according to mass ratio；
Sodium nitrate weighed in step 1.1 is put into mortar by step 1.2, using Mechanical Crushing mode grind 35min~
45min sifts out after the completion of to be ground, and the average pore size of sieve is 1mm~2mm, obtains sodium nitrate powder；
Potassium nitrate weighed in step 1.1 is put into mortar, 35min~45min is ground using Mechanical Crushing mode, to
It sifts out after the completion of grinding, the average pore size of sieve is 1mm~2mm, obtains potassium nitrate powder；
Neodymium nitrate weighed in step 1.1 is put into mortar, 35min~45min is ground using Mechanical Crushing mode, to
It sifts out after the completion of grinding, the average pore size of sieve is 1mm~2mm, obtains neodymium nitrate powder；
Step 1.3, the sodium nitrate powder by through step 1.2 Mechanical Crushing, potassium nitrate powder and neodymium nitrate powder are respectively only
Vertical placement is dried in a vacuum drying oven.
The purity of the sodium nitrate, potassium nitrate and the salt neodymium nitrate that use in step 1 is all larger than 99%, and foreign ion summation is less than
1%.
In step 1.2, first to use distilled water, dehydrated alcohol, acetone washing mortar respectively before using mortar, be ground with removal
Grease and spot in alms bowl.
In step 1.3, the condition of drying process are as follows: drying temperature be 80 DEG C~120 DEG C, drying time be 12h~
24h。
Step 3 is specifically implemented according to the following steps:
The ternary nitric acid fuse salt phase-change heat-storage material precast body obtained through step 2 is placed in crucible by step 3.1,
Then the crucible is put into program-controlled cabinet-type electric furnace and is heated, taken after crucible natural cooling after the completion of heat treatment
Out；
Step 3.2 will be dried in a vacuum drying oven through step 3.1 treated crucible placement, be mixed
Close object；
Step 3.3 takes abrading-ball, will mix after the mixture that step 3.2 obtains with abrading-ball according to ratio of grinding media to material for 8~12:1
It closes, is then fitted into ball mill together and carries out ball-milling treatment, allow sodium nitrate powder, potassium nitrate powder and nitric acid in mechanical milling process
Neodymium powder obtains full and uniform mixing, stops ball milling after after Ball-milling Time, obtains ternary nitric acid fuse salt phase-change thermal storage material
Material.
In step 3.1, the condition of heat treatment are as follows: heating temperature be 340 DEG C~360 DEG C, heating time be 1.5h~
2.5h。
In step 3.2, it is dried condition are as follows: drying time is 100 DEG C~120 DEG C, and drying time is 12h~for 24 hours.
In step 3.3, the ball-milling treatment time is 25min~35min, and ball-milling medium is air.
Crucible is ceramic crucible.
The beneficial effects of the present invention are:
(1) it is closed using the ternary nitric acid fuse salt phase-change heat-storage material that preparation method of the invention is prepared with fusing point
The advantage suitable, heat storage capacity is big and thermal stability is good can be used as heat accumulating for solar energy thermal-power-generating and other related accumulation of heats
Field.
(2) in the preparation method of ternary nitric acid fuse salt phase-change heat-storage material of the present invention, used raw material has nitric acid
Sodium, potassium nitrate, neodymium nitrate, raw material are easy to get, and low in raw material price, so that preparation cost is low.
(3) preparation method of ternary nitric acid fuse salt phase-change heat-storage material of the present invention is very simple, easy to accomplish, is suitble to big
Batch production.
Detailed description of the invention
Fig. 1 is the differential scanning for the ternary nitric acid fuse salt phase-change heat-storage material prepared using preparation method of the invention
Calorimeter analyzes (i.e. DSC) curve；
Fig. 2 is the thermal weight loss point for the ternary nitric acid fuse salt phase-change heat-storage material prepared using preparation method of the invention
Analyse (TG) curve.
Specific embodiment
The following describes the present invention in detail with reference to the accompanying drawings and specific embodiments.
The preparation method of ternary nitric acid fuse salt phase-change heat-storage material of the present invention, is specifically implemented according to the following steps:
Step 1 weighs sodium nitrate, potassium nitrate, neodymium nitrate respectively, then uses weighed sodium nitrate, potassium nitrate, neodymium nitrate
Mechanical crushing method is broken, respectively obtains sodium nitrate powder, potassium nitrate powder, neodymium nitrate powder, is specifically implemented according to the following steps:
Step 1.1 is that 50~60:40~50:1~5 distinguishes weighed sodium nitrate, potassium nitrate, neodymium nitrate according to mass ratio；
The mass ratio between sodium nitrate, potassium nitrate, neodymium nitrate further can be optimized for 52~54:43~45:1~5；
Wherein, the purity of sodium nitrate, potassium nitrate and neodymium nitrate is all larger than 99%, and foreign ion summation is less than 1%；
Sodium nitrate weighed in step 1.1 is put into mortar by step 1.2, using Mechanical Crushing mode grind 35min~
45min sifts out after the completion of to be ground, and the average pore size of sieve is 1mm~2mm, obtains sodium nitrate powder；
Potassium nitrate weighed in step 1.1 is put into mortar, 35min~45min is ground using Mechanical Crushing mode, to
It sifts out after the completion of grinding, the average pore size of sieve is 1mm~2mm, obtains potassium nitrate powder；
Neodymium nitrate weighed in step 1.1 is put into mortar, 35min~45min is ground using Mechanical Crushing mode, to
It sifts out after the completion of grinding, the average pore size of sieve is 1mm~2mm, obtains neodymium nitrate powder；
Distilled water, dehydrated alcohol, acetone washing mortar are used, respectively first before using mortar to remove the grease in mortar
And spot；
Step 1.3, the sodium nitrate powder by through step 1.2 Mechanical Crushing, potassium nitrate powder and neodymium nitrate powder are respectively only
Vertical placement is dried in a vacuum drying oven, the condition of drying process are as follows: drying temperature is 80 DEG C~120 DEG C, is done
The dry time is 12h~for 24 hours.
Step 2 mixes the sodium nitrate powder obtained through step 1, potassium nitrate powder, neodymium nitrate powder, obtains
Ternary nitric acid fuse salt phase-change heat-storage material precast body.
Step 3 first melts the ternary nitric acid fuse salt phase-change heat-storage material precast body obtained through step 2, then
It is successively dried, ball mill crushing processing, finally obtains ternary nitric acid fuse salt phase-change heat-storage material, specifically according to the following steps
Implement:
The ternary nitric acid fuse salt phase-change heat-storage material precast body obtained through step 2 is placed in crucible by step 3.1,
Then the crucible is put into program-controlled cabinet-type electric furnace and is heated, heat the condition of temperature processing are as follows: heating temperature is 340 DEG C
~360 DEG C, heating time is 1.5h~2.5h, after the completion of heat treatment, is taken out after ceramic crucible natural cooling；
Step 3.2 will be dried in a vacuum drying oven through step 3.1 treated ceramic crucible placement, do
The dry time is 100 DEG C~120 DEG C, drying time is 12h~for 24 hours, obtains mixture；
Step 3.3 takes abrading-ball, will mix after the mixture that step 3.2 obtains with abrading-ball according to ratio of grinding media to material for 8~12:1
It closes, is then fitted into ball mill together and carries out ball-milling treatment, the ball-milling treatment time is 25min~35min, and ball-milling medium is sky
Gas allows sodium nitrate powder, potassium nitrate powder and neodymium nitrate powder to obtain full and uniform mixing, when ball milling in mechanical milling process
Between stop ball milling after, obtain ternary nitric acid fuse salt phase-change heat-storage material.
Using above-mentioned heating condition, the nitric acid sodium powder in ternary nitric acid fuse salt phase-change heat-storage material precast body can guarantee
End, potassium nitrate powder and neodymium nitrate powder can melt completely, and will not decompose or can send out, so that three kinds of fused salts are abundant
Mixing reaches eutectic state；It to be sealed against saving after preparing ternary nitric acid fuse salt phase-change heat-storage material, in use
Powder type presence can be ground into according to the needs of actual industrial production.
Embodiment 1
Sodium nitrate, potassium nitrate, neodymium nitrate are weighed respectively in mass ratio for 54:45:1；Wherein, sodium nitrate, potassium nitrate and salt
The purity of neodymium nitrate is all larger than 99%, and foreign ion summation is less than 1%；Weighed sodium nitrate is put into mortar, using machinery
Lapping mode grinds 35min, sifts out (average pore size of sieve is 1mm) after the completion of to be ground, obtains sodium nitrate powder；It will claim
The potassium nitrate taken is put into mortar, grind 35min using mechanical lapping mode, and sifting out after the completion of to be ground, (sieve is averaged
Aperture is 1mm), obtain potassium nitrate powder；Weighed neodymium nitrate is put into mortar, 35min is ground using mechanical lapping mode,
It sifts out (average pore size of sieve is 1mm) after the completion of to be ground, obtains neodymium nitrate powder；By sodium nitrate powder, potassium nitrate powder
End and the neodymium nitrate powder vacuum oven independent that is placed in are dry, and in the drying process: drying temperature is 100 DEG C, is done
The dry time is 12h；
Sodium nitrate powder, potassium nitrate powder, neodymium nitrate powder are uniformly mixed, ternary nitric acid fuse salt phase-change thermal storage is obtained
Prefabricated body；
Obtained ternary nitric acid fuse salt phase-change heat-storage material precast body is placed in ceramic crucible, then by the ceramics
Crucible is put into program-controlled cabinet-type electric furnace and heats, and heating temperature is 340 DEG C, heating time 1.5h；To ceramic crucible natural cooling
After take out；It puts and dries in a vacuum drying oven, drying time is 100 DEG C, drying time 23h；Abrading-ball is taken, by dry mixing
Fused salt and abrading-ball are that 9:1 is mixed according to ratio of grinding media to material, are then fitted into ball mill together and carry out ball-milling treatment, and the ball-milling treatment time is
25min, ball-milling medium are air, and sodium nitrate powder, potassium nitrate powder and neodymium nitrate powder obtain sufficiently in mechanical milling process
Even mixing stops ball milling after after Ball-milling Time, obtains ternary nitric acid fuse salt phase-change heat-storage material.
Embodiment 2
Sodium nitrate, potassium nitrate, neodymium nitrate are weighed respectively in mass ratio for 53:44:3；Wherein, sodium nitrate, potassium nitrate and salt
The purity of neodymium nitrate is all larger than 99%, and foreign ion summation is less than 1%；Weighed sodium nitrate is put into mortar, using machinery
Lapping mode grinds 40min, sifts out (average pore size of sieve is 2mm) after the completion of grinding, obtains sodium nitrate powder；It will weigh
Potassium nitrate be put into mortar, 40min is ground using mechanical lapping mode, (the average hole of sieve of sifting out after the completion of to be ground
Diameter is 2mm), obtain potassium nitrate powder；Weighed neodymium nitrate is put into mortar, 40min is ground using mechanical lapping mode, to
It sifts out (average pore size of sieve is 2mm) after the completion of grinding, obtains neodymium nitrate powder；By sodium nitrate powder, potassium nitrate powder
And the independent vacuum oven that is placed in of neodymium nitrate powder is dry, in the drying process: drying temperature is 110 DEG C, drying time
For for 24 hours；
Sodium nitrate powder, potassium nitrate powder, neodymium nitrate powder are uniformly mixed, ternary nitric acid fuse salt phase-change thermal storage is obtained
Prefabricated body；
Obtained ternary nitric acid fuse salt phase-change heat-storage material precast body is placed in ceramic crucible, then by the ceramics
Crucible is put into program-controlled cabinet-type electric furnace and heats, and heating temperature is 350 DEG C, heating time 2h；After ceramic crucible natural cooling
It takes out；It puts and dries in a vacuum drying oven, drying time is 110 DEG C, drying time is for 24 hours；Abrading-ball is taken, dry mixing is melted
Salt and abrading-ball are that 10:1 is mixed according to ratio of grinding media to material, are then fitted into ball mill together and carry out ball-milling treatment, and the ball-milling treatment time is
30min, ball-milling medium are air, and sodium nitrate powder, potassium nitrate powder and neodymium nitrate powder obtain sufficiently in mechanical milling process
Even mixing stops ball milling after after Ball-milling Time, obtains ternary nitric acid fuse salt phase-change heat-storage material.
Embodiment 3
Sodium nitrate, potassium nitrate, neodymium nitrate are weighed respectively in mass ratio for 52:43:5；Wherein, sodium nitrate, potassium nitrate and salt
The purity of neodymium nitrate is all larger than 99%, and foreign ion summation is less than 1%；Weighed sodium nitrate is put into mortar, using machinery
Lapping mode grinds 45min, sifts out (average pore size of sieve is 1.5mm) after the completion of to be ground, obtains sodium nitrate powder；It will
Weighed potassium nitrate is put into mortar, grinds 45min using mechanical lapping mode, sift out after the completion of to be ground (sieve it is flat
Equal aperture is 1.5mm), obtain potassium nitrate powder；Weighed neodymium nitrate is put into mortar, is ground using mechanical lapping mode
45min sifts out (average pore size of sieve is 1.5mm) after the completion of to be ground, obtains neodymium nitrate powder；By sodium nitrate powder,
Potassium nitrate powder and the neodymium nitrate powder vacuum oven independent that is placed in are dry, and in the drying process: drying temperature is
120 DEG C, drying time 18h；
Sodium nitrate powder, potassium nitrate powder, neodymium nitrate powder are uniformly mixed, ternary nitric acid fuse salt phase-change thermal storage is obtained
Prefabricated body；
Obtained ternary nitric acid fuse salt phase-change heat-storage material precast body is placed in ceramic crucible, then by the ceramics
Crucible is put into program-controlled cabinet-type electric furnace and heats, and heating temperature is 360 DEG C, heating time 2.5h；To ceramic crucible natural cooling
After take out；It puts and dries in a vacuum drying oven, drying time is 120 DEG C, drying time 18h；Abrading-ball is taken, by dry mixing
Fused salt is that 12:1 is mixed according to ratio of grinding media to material with abrading-ball, is then fitted into ball mill together and carries out ball-milling treatment, the ball-milling treatment time
For 35min, ball-milling medium is air, and sodium nitrate powder, potassium nitrate powder and neodymium nitrate powder obtain sufficiently in mechanical milling process
Uniform mixing, stops ball milling after after Ball-milling Time, obtains ternary nitric acid fuse salt phase-change heat-storage material.
The preparation method of ternary nitric acid fuse salt phase-change heat-storage material of the present invention is on the basis of two end number mixing nitric acid fused salt
On, by the addition of the third fused salt, ternary mixed nitrate fuse salt (that is: ternary nitric acid fuse salt phase-change heat-storage material is made
Precast body)；Wherein binary molten nitrate salt heat accumulating is made of sodium nitrate and potassium nitrate, sodium nitrate and potassium nitrate it is optimal
Mass ratio is 55:45, and the purity of sodium nitrate, potassium nitrate is greater than 99%, and foreign ion summation is less than 1%；It is molten in binary nitric acid
On the basis of melting salt, rare earth nitrades neodymium nitrate is added, ternary mixed nitrate fuse salt is made (i.e.: by static fusion method
Ternary nitric acid fuse salt phase-change heat-storage material precast body), wherein the purity of neodymium nitrate is greater than 99%, and foreign ion summation is less than
1%.
The ternary nitric acid fuse salt phase obtained using the preparation method of ternary nitric acid fuse salt phase-change heat-storage material of the present invention
Change heat storage material adds ternary mixed nitrate fuse salt (that is: the ternary after neodymium nitrate it can be seen from table 1, table 2, Fig. 1, Fig. 2
Nitric acid fuse salt phase-change heat-storage material precast body) it is remarkably reinforced compared with binary nitrate and sodium nitrate, potassium nitrate heat storage capacity, fusing point
Reduction increases its scope of application, has good thermal stability within smaller 550 DEG C of corrosivity.
1 fuse salt DSC curve peak integration of table obtains heat storage capacity (mW/mg)
2 fuse salt items physical and chemical performance of table
The preparation method of ternary nitric acid fuse salt phase-change heat-storage material of the present invention, with preparation cost is low and simple process
Feature, the material prepared have the characteristics that fusing point is suitable, heat storage capacity is big, thermal stability is good.
Claims (8)
1. a kind of preparation method of ternary nitric acid fuse salt phase-change heat-storage material, which is characterized in that specifically real according to the following steps
It applies:
Step 1 weighs sodium nitrate, potassium nitrate, neodymium nitrate respectively, then by sodium nitrate, potassium nitrate, neodymium nitrate mechanical crushing method
It is broken, respectively obtain sodium nitrate powder, potassium nitrate powder, neodymium nitrate powder；
Step 2 mixes the sodium nitrate powder obtained through step 1, potassium nitrate powder, neodymium nitrate powder, obtains ternary
Nitric acid fuse salt phase-change heat-storage material precast body；
Step 3 first melts the ternary nitric acid fuse salt phase-change heat-storage material precast body obtained through step 2, then successively
It is dried, ball mill crushing processing, finally obtains ternary nitric acid fuse salt phase-change heat-storage material, specific steps are as follows:
The ternary nitric acid fuse salt phase-change heat-storage material precast body obtained through step 2 is placed in crucible by step 3.1, then
The crucible is put into program-controlled cabinet-type electric furnace and is heated, is taken out after crucible natural cooling after the completion of heat treatment；Add
The condition of heat treatment is: heating temperature is 340 DEG C~360 DEG C, and heating time is 1.5h~2.5h,
Step 3.2 will be dried in a vacuum drying oven through step 3.1 treated crucible placement, obtain mixture；
Step 3.3 takes abrading-ball, will mix after the mixture that step 3.2 obtains with abrading-ball according to ratio of grinding media to material for 8~12:1, so
It is fitted into ball mill together afterwards and carries out ball-milling treatment, allow sodium nitrate powder, potassium nitrate powder and neodymium nitrate powder in mechanical milling process
End obtains full and uniform mixing, stops ball milling after after Ball-milling Time, obtains ternary nitric acid fuse salt phase-change heat-storage material.
2. a kind of preparation method of ternary nitric acid fuse salt phase-change heat-storage material according to claim 1, which is characterized in that
The step 1 is specifically implemented according to the following steps:
Step 1.1 is that 50~60:40~50:1~5 distinguishes weighed sodium nitrate, potassium nitrate, neodymium nitrate according to mass ratio；
Sodium nitrate weighed in step 1.1 is put into mortar by step 1.2, using Mechanical Crushing mode grind 35min~
45min sifts out after the completion of grinding, and the average pore size of sieve is 1mm~2mm, obtains sodium nitrate powder；
Potassium nitrate weighed in step 1.1 is put into mortar, 35min~45min is ground using Mechanical Crushing mode, has been ground
It sifts out after, the average pore size of sieve is 1mm~2mm, obtains potassium nitrate powder；
Neodymium nitrate weighed in step 1.1 is put into mortar, 35min~45min is ground using Mechanical Crushing mode, has been ground
It sifts out after, the average pore size of sieve is 1mm~2mm, obtains neodymium nitrate powder；
Step 1.3, the sodium nitrate powder by through step 1.2 Mechanical Crushing, potassium nitrate powder and neodymium nitrate powder are independent
Placement is dried in a vacuum drying oven.
3. a kind of preparation method of ternary nitric acid fuse salt phase-change heat-storage material according to claim 1 or 2, feature exist
In the purity of the sodium nitrate, potassium nitrate and the salt neodymium nitrate that use in the step 1 is all larger than 99%, and foreign ion summation is less than
1%.
4. a kind of preparation method of ternary nitric acid fuse salt phase-change heat-storage material according to claim 2, which is characterized in that
In the step 1.2, distilled water, dehydrated alcohol, acetone washing mortar are used, respectively first before using mortar to remove in mortar
Grease and spot.
5. a kind of preparation method of ternary nitric acid fuse salt phase-change heat-storage material according to claim 2, which is characterized in that
In the step 1.3, the condition of drying process are as follows: drying temperature is 80 DEG C~120 DEG C, and drying time is 12h~for 24 hours.
6. a kind of preparation method of ternary nitric acid fuse salt phase-change heat-storage material according to claim 1, which is characterized in that
In the step 3.2, it is dried condition are as follows: drying time is 100 DEG C~120 DEG C, and drying time is 12h~for 24 hours.
7. a kind of preparation method of ternary nitric acid fuse salt phase-change heat-storage material according to claim 1, which is characterized in that
In the step 3.3, the ball-milling treatment time is 25min~35min, and ball-milling medium is air.
8. a kind of preparation method of ternary nitric acid fuse salt phase-change heat-storage material according to claim 1, which is characterized in that
The crucible is ceramic crucible.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510908061.2A CN105419732B (en) | 2015-12-09 | 2015-12-09 | A kind of preparation method of ternary nitric acid fuse salt phase-change heat-storage material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510908061.2A CN105419732B (en) | 2015-12-09 | 2015-12-09 | A kind of preparation method of ternary nitric acid fuse salt phase-change heat-storage material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105419732A CN105419732A (en) | 2016-03-23 |
| CN105419732B true CN105419732B (en) | 2019-03-08 |
Family
ID=55498285
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510908061.2A Active CN105419732B (en) | 2015-12-09 | 2015-12-09 | A kind of preparation method of ternary nitric acid fuse salt phase-change heat-storage material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105419732B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105838339B (en) * | 2016-05-26 | 2019-03-15 | 中国科学院上海应用物理研究所 | A kind of nitric acid fused salt of highly endothermic efficiency and the preparation method and application thereof |
| CN106590546A (en) * | 2016-12-13 | 2017-04-26 | 上海铂拓能源科技有限公司 | Ternary mixed molten salt heat storage material and preparation method thereof |
| CN107418520B (en) * | 2017-05-24 | 2020-06-09 | 中南大学 | Phase-change energy storage medium and preparation method and application thereof |
| CN110172332B (en) * | 2019-04-25 | 2020-11-17 | 武汉理工大学 | NaNO with high specific heat capacity3Phase-change heat storage material and preparation method thereof |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102533226A (en) * | 2011-12-15 | 2012-07-04 | 中山大学 | Nitrate molten salt heat transferring and reserving medium and preparation method and application thereof |
| CN102585779A (en) * | 2011-11-18 | 2012-07-18 | 牟邦志 | Preparation method of high-purity heat-conduction energy storage molten salt |
| CN103459547A (en) * | 2011-02-11 | 2013-12-18 | 艾尼股份公司 | Mixture of inorganic nitrate salts |
| CN103911119A (en) * | 2013-02-01 | 2014-07-09 | 深圳市爱能森科技有限公司 | Heat-transfer heat-accumulation medium prepared by combining quartz sand and ternary molten nitrate salt and preparation method thereof |
| CN103923612A (en) * | 2013-12-26 | 2014-07-16 | 深圳市爱能森科技有限公司 | Quartz sand compound binary molten nitrate salt heat transfer and storage medium and its preparation method |
| CN103992775A (en) * | 2014-06-11 | 2014-08-20 | 武汉理工大学 | Heat transferring and storing material with low smelting point and preparation method thereof |
| CN104109508A (en) * | 2014-06-30 | 2014-10-22 | 中国科学院青海盐湖研究所 | Nitrate-system molten salt heat storage material and preparation method thereof |
| CN104293304A (en) * | 2014-09-18 | 2015-01-21 | 孙希干 | Solar heat accumulation type vacuum heat pipe, heat accumulation phase change material and preparation technology of heat accumulation phase change material |
| CN104403642A (en) * | 2014-10-13 | 2015-03-11 | 赵家春 | Fused salt used for solar energy photo-thermal electricity generating and preparation method thereof |
| CN104559942A (en) * | 2015-02-03 | 2015-04-29 | 王军涛 | Mixed molten salt heat storage and heat transfer material and preparation method thereof |
| CN104610927A (en) * | 2015-02-03 | 2015-05-13 | 王军涛 | Low-melting-point mixed fused salt heat storage and heat transfer material and preparation method thereof |
-
2015
- 2015-12-09 CN CN201510908061.2A patent/CN105419732B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103459547A (en) * | 2011-02-11 | 2013-12-18 | 艾尼股份公司 | Mixture of inorganic nitrate salts |
| CN102585779A (en) * | 2011-11-18 | 2012-07-18 | 牟邦志 | Preparation method of high-purity heat-conduction energy storage molten salt |
| CN102533226A (en) * | 2011-12-15 | 2012-07-04 | 中山大学 | Nitrate molten salt heat transferring and reserving medium and preparation method and application thereof |
| CN103911119A (en) * | 2013-02-01 | 2014-07-09 | 深圳市爱能森科技有限公司 | Heat-transfer heat-accumulation medium prepared by combining quartz sand and ternary molten nitrate salt and preparation method thereof |
| CN103923612A (en) * | 2013-12-26 | 2014-07-16 | 深圳市爱能森科技有限公司 | Quartz sand compound binary molten nitrate salt heat transfer and storage medium and its preparation method |
| CN103992775A (en) * | 2014-06-11 | 2014-08-20 | 武汉理工大学 | Heat transferring and storing material with low smelting point and preparation method thereof |
| CN104109508A (en) * | 2014-06-30 | 2014-10-22 | 中国科学院青海盐湖研究所 | Nitrate-system molten salt heat storage material and preparation method thereof |
| CN104293304A (en) * | 2014-09-18 | 2015-01-21 | 孙希干 | Solar heat accumulation type vacuum heat pipe, heat accumulation phase change material and preparation technology of heat accumulation phase change material |
| CN104403642A (en) * | 2014-10-13 | 2015-03-11 | 赵家春 | Fused salt used for solar energy photo-thermal electricity generating and preparation method thereof |
| CN104559942A (en) * | 2015-02-03 | 2015-04-29 | 王军涛 | Mixed molten salt heat storage and heat transfer material and preparation method thereof |
| CN104610927A (en) * | 2015-02-03 | 2015-05-13 | 王军涛 | Low-melting-point mixed fused salt heat storage and heat transfer material and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 《熔融盐高储热材料的研究进展》;赵倩等;《无机盐工业》;20141130;第46卷(第11期);第5-8页 * |
| 《高温熔盐相变蓄热材料》;崔海亭等;《太阳能》;20030131(第1期);第27-28页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105419732A (en) | 2016-03-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105419732B (en) | A kind of preparation method of ternary nitric acid fuse salt phase-change heat-storage material | |
| CN102531550B (en) | Poly fatty acid shape-stabilized phase change material and preparation method thereof | |
| CN104559936B (en) | A kind of medium temperature phase change heat storage material and preparation method thereof | |
| CN106118610B (en) | Polyethylene glycol/graphene sizing phase-change material preparation method | |
| CN104497988A (en) | Kaolin phase-change composite energy storage material and preparation method thereof | |
| CN106848237A (en) | A kind of preparation method of the sodium ion positive electrode of height ratio capacity | |
| CN105577034B (en) | The preparation method of multistage coupling high temperature sensible heat latent heat phase-change accumulation energy temperature difference electricity generation device | |
| CN104388055A (en) | Novel composite type organic-substance phase-change heat storage material and preparation method thereof | |
| CN104164219A (en) | Shape-stabilized phase-change energy storage material and preparation method thereof | |
| CN105838331B (en) | A kind of diatomite base composite phase-change heat accumulation ball, preparation method and purposes | |
| CN110862805A (en) | Constant-temperature phase-change energy storage material and preparation method thereof | |
| CN108285777A (en) | A kind of production method of ternary fused salt mixt medium temperature phase-changing energy storage material | |
| CN109021931A (en) | A kind of phase-change heat-storage material preparation method using unorganic glass as heat-storage medium | |
| CN104388054A (en) | Novel composite organic heat storage material and preparation method thereof | |
| CN103897668B (en) | A kind of high temperature heat transfer material based on carbonate and preparation method thereof | |
| CN109181655A (en) | The formula and preparation method of a kind of hot enhanced physical properties of iron ore for high temperature heat accumulation | |
| CN105154022A (en) | Metal substrate highly heat-conducting heat storage material and preparation method therefor | |
| CN104193179A (en) | Nanoscale glass powder for silicon solar cell front-side silver paste and preparation method thereof | |
| CN104164218A (en) | Heat storage material and preparation method thereof | |
| CN108675822A (en) | A kind of heat accumulation ceramic based material and preparation method thereof | |
| CN103965838A (en) | High-temperature phase-change heat storage material and preparation method thereof | |
| CN105621987B (en) | A kind of preparation method of high-temperature phase-change energy-storing concrete | |
| CN106905929A (en) | A kind of solid heat storage material and preparation method and application | |
| CN105154019A (en) | Inorganic finalized phase change heat storage material and preparation method therefor | |
| CN110372211A (en) | One kind positive silver glass powder used for solar batteries and preparation method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20210401 Address after: 113000 No.36, Shendong 5th Road, Shenfu New District, Fushun City, Liaoning Province Patentee after: LIAONING ZEAL SCIENCE AND TECHNOLOGY Co.,Ltd. Address before: 710048 No. 19 Jinhua South Road, Shaanxi, Xi'an Patentee before: XI'AN POLYTECHNIC University |