CN103911119A - Heat-transfer heat-accumulation medium prepared by combining quartz sand and ternary molten nitrate salt and preparation method thereof - Google Patents
Heat-transfer heat-accumulation medium prepared by combining quartz sand and ternary molten nitrate salt and preparation method thereof Download PDFInfo
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- CN103911119A CN103911119A CN201310040070.5A CN201310040070A CN103911119A CN 103911119 A CN103911119 A CN 103911119A CN 201310040070 A CN201310040070 A CN 201310040070A CN 103911119 A CN103911119 A CN 103911119A
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Abstract
The invention discloses a heat-transfer heat-accumulation medium prepared by combining quartz sand and a ternary molten nitrate salt and a preparation method thereof, and belongs to the field of solar energy photo-thermal electricity generation. The heat-transfer heat-accumulation medium is composed of a ternary molten nitrate salt system and quartz sand. The invention also provides a preparation method of the heat-transfer heat-accumulation medium. The heat-transfer heat-accumulation medium basically does not change the freezing point of the ternary molten nitrate salt, also the upper limit operating temperature of the ternary molten nitrate salt is improved and is up to 750 DEG C. The heat-transfer heat-accumulation medium is good in thermal stability, high in thermal conductivity, low in cost and extremely suitable for solar energy thermal power electricity generation systems and solar energy photo-thermal electricity-generation heat-accumulation heat-transfer systems.
Description
Technical field
The present invention relates to the heat-accumulating heat-transfer complex media for solar light-heat power-generation, particularly relate to the compound ternary nitric acid of a kind of quartz sand Molten Salt Heat Transfer heat storage medium and preparation method thereof.
Background technology
In industrial accumulation of energy and solar light-heat power-generation technology, the heat-accumulating heat-transfer medium using at present mainly contains air, water, thermal oil, melting salt, sodium and aluminum metal etc.Fused salt is because having use temperature scope widely, low-steam pressure, low viscosity, satisfactory stability, many characteristics such as low cost have become the heat transfer heat storage medium that has much potentiality in solar light-heat power-generation technology, become current application more, comparatively ripe heat transfer heat storage medium.
The outstanding advantages of nitric acid molten salt system be that raw material sources are extensive, cheap, corrodibility is little and generally 500 ℃ below can thermolysis, therefore, compared with other fused salts, nitric acid fused salt has very large advantage.At present, the heat transfer heat storage medium that the power station of external solar light-heat power-generation is used is mainly binary nitrate system (40%KNO
3-60%NaNO3) and ternary nitrate system (KNO
3-NaNO
3-NaNO
2).The fusing point of ternary nitrate system is lower, more satisfactory, but upper limit working temperature is on the low side, and solution heat is less, thermal conductivity is lower.
In order to address the above problem, Chinese patent application 00111406.9 discloses a kind of LiNO3-KNO
3-NaNO
3-NaNO
2system, its operating temperature range is 250 ℃-550 ℃, the upper limit working temperature of this individual system is than ternary nitrate system KNO
3-NaNO
3-NaNO
2height, but its lower limit working temperature is also enhanced, and while causing obnubilation, maintenance cost increases, and adding of LiNO3 its corrodibility is increased, cost up.
U.S. Pat 007588694B1 discloses a kind of LiNO
3-KNO
3-NaNO
3-Ca(NO
3)
2system, its fusing point is lower than 100 ℃, and upper limit use temperature is higher than 500 ℃, but adding of LiNO3 increased the corrodibility of fused salt and cost.
Molecular chain structure, crystal shape and the lattice variations rule of quartz sand uniqueness, make it have high temperature resistant, anti-oxidant, thermal expansivity is little, high-insulation, unique many characteristics such as physics, chemistry such as corrosion-resistant, in many high-tech products, bring into play more and more important effect, be often used as the raw material of manufacturing glass, refractory materials, smelting duriron, flux for metallurgy, ceramic grinding material, casting.
So far, do not see quartz sand is joined in ternary nitric acid fused salt as the report of the heat transfer heat storage medium in industrial accumulation of energy and solar energy high temperature thermal utilization field.
Summary of the invention
The object of the present invention is to provide the compound ternary nitric acid of a kind of quartz sand Molten Salt Heat Transfer heat storage medium and preparation method, low to improve ternary nitric acid fused salt SC service ceiling temperature.The present invention adopts the raw material of quartz sand as heat-accumulating heat-transfer medium, not only can improve the upper limit use temperature of melting salt, gained composite fused salt has the zero pour (being the fusing point that adopts differential scanning instrument to measure under normal pressure) that is less than 100 ℃ simultaneously, the maintenance cost while reducing obnubilation; Quartz sand is cheap in addition, can also significantly reduce the industrial cost of heat storage medium.
For achieving the above object, technical scheme of the present invention is as follows:
The compound ternary nitric acid of a kind of quartz sand Molten Salt Heat Transfer heat storage medium, is characterized in that: described heat transfer heat storage medium is in ternary nitric acid molten salt system, to add quartz sand to be composited.
Described ternary nitric acid molten salt system accounts for 50 ~ 99% of heat transfer heat storage medium gross weight, and described quartz sand accounts for 1 ~ 50% of heat transfer heat storage medium gross weight.
Described ternary nitric acid molten salt system accounts for 50 ~ 90% of heat transfer heat storage medium gross weight, and described quartz sand accounts for 10 ~ 50% of heat transfer heat storage medium gross weight.
Described ternary nitric acid molten salt system and components by weight percent thereof are as follows: KNO
3-NaNO
3-NaNO
2system: wherein saltpetre: 40-80 part; SODIUMNITRATE: 5-15 part; Sodium Nitrite: 10-50 part.
Described ternary nitric acid molten salt system and components by weight percent thereof are as follows: KNO
3-NaNO
3-Ca (NO
3)
2system: wherein saltpetre: 5-40 part; SODIUMNITRATE: 5-25 part; Nitrocalcite: 10-70 part.
The purposes of above-mentioned arbitrary heat transfer heat storage medium in industrial accumulation of energy or solar light-heat power-generation.
The preparation method of above-mentioned arbitrary heat transfer heat storage medium, its step is as follows:
(1) composition ternary nitric acid molten salt system, puts into reactor, and heated and stirred makes the complete melting of solid, is then incubated 0.5-1h,
(2) under agitation condition, quartz sand is distributed in high-temperature fusion salt, continues to stir 1-2h, mixture agglutination state,
(3) cooling, packing.
The temperature that heated and stirred makes solid become melting to adopt is completely the above 50-100 ℃ of transformation temperature of described ternary nitric acid fused salt.
The present invention selects the matrix material of quartz sand as nitric acid fused salt first, and quartz sand is a kind of silicate minerals of hard, wear-resisting, stable chemical performance, and its main component is SiO
2, in mineral, often contain a small amount of impurity component as Fe
2o
3, Al
3o
2, CaO, MgO, NaO etc.Approximately 1723 ℃ of fusing points, approximately 2230 ℃ of boiling points, have higher fire performance.The common quartz sand that adopts dioxide-containing silica to be greater than 75% for quartz sand of the present invention.Experiment showed, and in ternary nitric acid molten salt system, add quartz sand to prepare the heat transfer heat storage medium of gained, industrial cost is low, very micro-to hold over system corrodibility, and also has following advantage and positively effect compared with former ternary nitric acid molten salt system:
1. the heat transfer property of the existing nitric acid fused salt of composite fused salt heat transfer heat storage medium that prepared by the present invention, improved thermostability and and upper limit use temperature, the zero pour of fused salt does not change substantially.
2. the latent heat of phase change of the Molten Salt Heat Transfer heat storage medium that prepared by the present invention increases, and energy storage density is high, has reduced the requirement to hold over system size and energy, and capacity usage ratio is high, good energy-conserving effect.
In the preferred embodiments of the invention, quartz sand accounts for 1 ~ 50%, and quartz sand content is higher, reduces costs more obvious; The ceiling temperature that can guarantee ternary nitric acid fused salt within the scope of this improves, and can guarantee that again fusing point does not raise, and the heat transfer of the more thin more system of the quartz sand particle degree of introducing is more even.
Embodiment
Describe the present invention below in conjunction with specific embodiment.
Experiment material:
Common quartz sand (dioxide-containing silica is greater than 75%), 100 orders are purchased from Shandong Hong Tai quartz sand factory.
Saltpetre, SODIUMNITRATE, Sodium Nitrite, the general chemical article of nitrocalcite company can buy.
Ternary nitrate system formulation is as table 1.
Ternary nitric acid molten salt system formula in the each embodiment of table 1.
Embodiment 1 ~ 4. ternary nitrate system KNO
3-NaNO
3-NaNO
2in add quartz sand to prepare heat-accumulating heat-transfer medium
Step 1. is pressed the material of the listed formula preparation composition ternary nitric acid molten salt system of table 1, puts into reactor, and heated and stirred makes the complete melting of solid, is then incubated 0.5-1h, and Heating temperature is the above 50-100 ℃ of fused salt transformation temperature.
Under step 2. agitation condition, quartz sand is distributed in the ternary nitric acid molten salt system of melting, continues to stir 1-2h, it is gluey that mixture is.
Step 3. is cooling, packing.
The quartz sand (specification is 100 orders) adding carries out in following ratio gradient:
First group: quartz sand accounts for 1% in the four kinds of compound ternary nitric acid of quartz sand Molten Salt Heat Transfer heat storage mediums, obtains 1st ~ 4 products.
Second group: quartz sand accounts for 10% in the four kinds of compound ternary nitric acid of quartz sand Molten Salt Heat Transfer heat storage mediums, obtains 5th ~ 8 products.
The 3rd group: quartz sand accounts for 25% in the four kinds of compound ternary nitric acid of quartz sand Molten Salt Heat Transfer heat storage mediums, obtains 9th ~ 12 products.
The 4th group: quartz sand accounts for 40% in the four kinds of compound ternary nitric acid of quartz sand Molten Salt Heat Transfer heat storage mediums, obtains 13rd ~ 16 products.
The 5th group: quartz sand accounts for 50% in the four kinds of compound ternary nitric acid of quartz sand Molten Salt Heat Transfer heat storage mediums, obtains 17th ~ 20 products.
The test of step 4. latent heat of phase change and fusing point test.
Adopt general differential scanning instrument DSC to carry out (under normal pressure, scanning).
Test result demonstration, compared with the control, latent heat of phase change all obviously increases; 1st ~ 3 set product fusing points are substantially constant, and the fusing point of the 4th group and the 5th set product increases a little.
Step 5: heat stability testing.
Carry out heat stability testing to preparing 20 kinds of heat transfer heat storage mediums and contrasting ternary nitric acid fused salt.
Test adopts weighting method to carry out: 20 kinds of melting salts of embodiment 1 ~ 4 gained are respectively charged in the crucible of nickel system, put into temperature controlling stove and heat, start to test from normal temperature, take out at set intervals experiment crucible analytical balance and weigh.If in a certain temperature section, the weight of sample no longer reduces, then improves the temperature of temperature controlling stove.And then take out at set intervals experiment crucible and weigh, after another stable state, continue again to heat up.
The equilibrium temperature boundary of contrast ternary nitric acid system is 500 ℃, heats 100 hours at 500 ℃, and rate of loss can reach 25%, heats 30 hours, and rate of loss reaches 10%.
5 of embodiment 1 ~ 4 gained groups of 20 kinds of heat transfer heat storage mediums are carried out to heat stability testing,
Rate of loss statistics at table 2.600 ℃
Rate of loss statistics at table 3.700 ℃
| Time (hour) | 30 | 100 |
[0054]?
| Product group number | ? | ? |
| First group | 15~20% | 25~30% |
| Second group | 12~15% | 20~23% |
| The 3rd group | 10~13% | 18~20% |
| The 4th group | 8~12% | 15~18% |
| The 5th group | 9~12% | 15~18% |
Embodiment 5 ~ 7 ternary nitrate system KNO
3-NaNO
3-Ca(NO
3) in add quartz sand to prepare heat-accumulating heat-transfer medium
Prepare the compound ternary nitric acid of quartz sand fused salt by the listed formula of table 1, method is with the method for embodiment 1 ~ 4 step 1.
The quartz sand adding is undertaken by gradient:
First group: quartz sand accounts for 1% in the three kinds of compound ternary nitric acid of quartz sand Molten Salt Heat Transfer heat storage mediums, obtains 17th ~ 19 products.
Second group: quartz sand accounts for 30% in the four kinds of compound ternary nitric acid of quartz sand Molten Salt Heat Transfer heat storage mediums, obtains 20th ~ 22 products.
The 3rd group: quartz sand accounts for 50% in the four kinds of compound ternary nitric acid of quartz sand Molten Salt Heat Transfer heat storage mediums, obtains 23rd ~ 25 products
The test of step 3. latent heat of phase change and fusing point test.
Adopt general differential scanning instrument DSC to carry out (under normal pressure, scanning).
Test result demonstration, latent heat of phase change all obviously increases; (118 ℃, the zero pour of 3 kinds of contrast ternary systems, 173 ℃, 131 ℃ compared with the control.), first group and second group of fusing point substantially constant, the 3rd group of fusing point increases.
Step 4: heat stability testing
Carry out heat stability testing to preparing 20 kinds of heat transfer heat storage mediums and contrasting ternary nitric acid fused salt.
Test adopts weighting method to carry out: 9 kinds of melting salts of embodiment 5 ~ 7 gained are respectively charged in the crucible of nickel system, put into temperature controlling stove and heat, start to test from normal temperature, take out at set intervals experiment crucible analytical balance and weigh.If in a certain temperature section, the weight of sample no longer reduces, then improves the temperature of temperature controlling stove.And then take out at set intervals experiment crucible and weigh, after another stable state, continue again to heat up.
The equilibrium temperature boundary of contrast ternary nitric acid system is 550 ℃, heats 30 hours at 550 ℃, and rate of loss approximately 3%, while heating 50 hours, rate of loss is approximately 8%;
3 of embodiment 5 ~ 7 gained groups of 9 kinds of heat transfer heat storage mediums are carried out to heat stability testing,
Rate of loss statistics at table 4.650 ℃
Rate of loss statistics at table 5.750 ℃
Can find out, product of the present invention, illustrates with suitable to impinging upon the rate of loss of 550 ℃ the rate of loss of 750 ℃, and product of the present invention has better thermostability, can be at 750 ℃ the stable operation long period.
Claims (8)
1. the compound ternary nitric acid of a quartz sand Molten Salt Heat Transfer heat storage medium, is characterized in that: described heat transfer heat storage medium is in ternary nitric acid molten salt system, to add quartz sand to be composited.
2. heat transfer heat storage medium according to claim 1, is characterized in that: described ternary nitric acid molten salt system accounts for 50 ~ 99% of heat transfer heat storage medium gross weight, and described quartz sand accounts for 1 ~ 50% of heat transfer heat storage medium gross weight.
3. heat transfer heat storage medium according to claim 2, is characterized in that: described ternary nitric acid molten salt system accounts for 50 ~ 90% of heat transfer heat storage medium gross weight, and described quartz sand accounts for 10 ~ 50% of heat transfer heat storage medium gross weight.
4. heat transfer heat storage medium according to claim 1, is characterized in that: described ternary nitric acid molten salt system and components by weight percent thereof are as follows: KNO
3-NaNO
3-NaNO
2system: wherein saltpetre: 40-80 part; SODIUMNITRATE: 5-15 part; Sodium Nitrite: 10-50 part.
5. heat transfer heat storage medium according to claim 1, is characterized in that: described ternary nitric acid molten salt system and components by weight percent thereof are as follows: KNO
3-NaNO
3-Ca (NO
3)
2system: wherein saltpetre: 5-40 part; SODIUMNITRATE: 5-25 part; Nitrocalcite: 10-70 part.
6. the purposes of the arbitrary heat transfer heat storage medium of claim 1 ~ 5 in industrial accumulation of energy or solar light-heat power-generation.
7. the preparation method of the arbitrary heat transfer heat storage medium of claim 1 ~ 5, its step is as follows:
(1) composition ternary nitric acid molten salt system, puts into reactor, and heated and stirred makes the complete melting of solid, is then incubated 0.5-1h,
(2) under agitation condition, quartz sand is distributed in high-temperature fusion salt, continues to stir 1-2h, mixture agglutination state,
(3) cooling, packing.
8. preparation method according to claim 7, the temperature that described heated and stirred makes solid become melting to adopt is completely the above 50-100 ℃ of transformation temperature of described ternary nitric acid fused salt.
Priority Applications (6)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310040070.5A CN103911119B (en) | 2013-02-01 | 2013-02-01 | Quartz sand complex ternary nitric acid Molten Salt Heat Transfer heat storage medium and preparation method thereof |
| PCT/CN2014/070970 WO2014117663A1 (en) | 2013-02-01 | 2014-01-21 | Quartz sand/graphite composite molten salt heat transfer and heat storage medium and preparation method thereof |
| US14/765,295 US10865335B2 (en) | 2013-02-01 | 2014-01-21 | Quartz sand/graphite composite molten salt heat transfer and heat storage medium and preparation method thereof |
| ES14745627T ES2848832T3 (en) | 2013-02-01 | 2014-01-21 | Molten salt heat transfer and heat storage medium composed of quartz sand |
| EP14745627.1A EP2952551B1 (en) | 2013-02-01 | 2014-01-21 | Quartz sand composite molten salt heat transfer and heat storage medium |
| PT147456271T PT2952551T (en) | 2013-02-01 | 2014-01-21 | Quartz sand/graphite composite molten salt heat transfer and heat storage medium and preparation method thereof |
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|---|---|---|---|
| CN201310040070.5A CN103911119B (en) | 2013-02-01 | 2013-02-01 | Quartz sand complex ternary nitric acid Molten Salt Heat Transfer heat storage medium and preparation method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105131911A (en) * | 2015-09-21 | 2015-12-09 | 上海交通大学 | Phase-change heat storage medium as well as preparation and application thereof |
| CN105154029A (en) * | 2015-10-11 | 2015-12-16 | 郑叶芳 | Nanometer aluminium nitride modified fused salt and preparation method thereof |
| CN105255454A (en) * | 2015-10-11 | 2016-01-20 | 郑叶芳 | Ternary nitrate/hydrotalcite composite heat storage material and preparing method thereof |
| CN105419732A (en) * | 2015-12-09 | 2016-03-23 | 西安工程大学 | Method for preparing ternary nitric acid molten salt phase change heat storage material |
| CN106433565A (en) * | 2016-09-09 | 2017-02-22 | 青海盐湖工业股份有限公司 | Mixed molten salt and preparation method thereof |
| CN109777369A (en) * | 2019-03-22 | 2019-05-21 | 中国科学院过程工程研究所 | A kind of two-part micropackaging thermal energy storage material and preparation method thereof and purposes |
| WO2019105448A1 (en) * | 2017-11-30 | 2019-06-06 | 深圳市爱能森科技有限公司 | Low melting point molten salt heat transfer and heat storage medium, preparation method therefor and use thereof |
| CN110137051A (en) * | 2019-04-29 | 2019-08-16 | 广东中贝能源科技有限公司 | A kind of arc quenching material composition improving fuse energy density |
| CN113175686A (en) * | 2021-05-08 | 2021-07-27 | 中煤科工集团重庆研究院有限公司 | Preheating method of molten salt heat storage system based on gas heat storage oxidation |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105131911A (en) * | 2015-09-21 | 2015-12-09 | 上海交通大学 | Phase-change heat storage medium as well as preparation and application thereof |
| CN105154029A (en) * | 2015-10-11 | 2015-12-16 | 郑叶芳 | Nanometer aluminium nitride modified fused salt and preparation method thereof |
| CN105255454A (en) * | 2015-10-11 | 2016-01-20 | 郑叶芳 | Ternary nitrate/hydrotalcite composite heat storage material and preparing method thereof |
| CN105419732A (en) * | 2015-12-09 | 2016-03-23 | 西安工程大学 | Method for preparing ternary nitric acid molten salt phase change heat storage material |
| CN105419732B (en) * | 2015-12-09 | 2019-03-08 | 西安工程大学 | A kind of preparation method of ternary nitric acid fuse salt phase-change heat-storage material |
| CN106433565A (en) * | 2016-09-09 | 2017-02-22 | 青海盐湖工业股份有限公司 | Mixed molten salt and preparation method thereof |
| WO2019105448A1 (en) * | 2017-11-30 | 2019-06-06 | 深圳市爱能森科技有限公司 | Low melting point molten salt heat transfer and heat storage medium, preparation method therefor and use thereof |
| CN109777369A (en) * | 2019-03-22 | 2019-05-21 | 中国科学院过程工程研究所 | A kind of two-part micropackaging thermal energy storage material and preparation method thereof and purposes |
| CN109777369B (en) * | 2019-03-22 | 2020-09-08 | 中国科学院过程工程研究所 | Two-section type micro-packaging composite heat storage material and preparation method and application thereof |
| CN110137051A (en) * | 2019-04-29 | 2019-08-16 | 广东中贝能源科技有限公司 | A kind of arc quenching material composition improving fuse energy density |
| CN113175686A (en) * | 2021-05-08 | 2021-07-27 | 中煤科工集团重庆研究院有限公司 | Preheating method of molten salt heat storage system based on gas heat storage oxidation |
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Address after: Room 1901, building 2, Hualing international building, 722 Beiyi Road, Dongying District, Dongying City, Shandong Province 257000 Patentee after: Shandong ainengsen New Material Technology Co.,Ltd. Address before: 817000 No. 20, Ulan Dong Road, Haixi Mongol and Tibetan Autonomous Prefecture, Delingha, Qinghai Patentee before: QINGHAI ENESOON NEW MATERIAL TECHNOLOGY Co.,Ltd. |