CN102585779B - Preparation method of high-purity heat-conduction energy storage molten salt - Google Patents
Preparation method of high-purity heat-conduction energy storage molten salt Download PDFInfo
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- CN102585779B CN102585779B CN201110385115.3A CN201110385115A CN102585779B CN 102585779 B CN102585779 B CN 102585779B CN 201110385115 A CN201110385115 A CN 201110385115A CN 102585779 B CN102585779 B CN 102585779B
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Abstract
The invention discloses a preparation method of a high-purity heat-conduction energy storage molten salt, which comprises the following steps that: a single-product salt meeting national standards is selected, and is purified, and then the single-product salt is physically and uniformly mixed to obtain the molten salt. According to the preparation method, the content of a corrosive medium is reduced, the corrosivity on various metal material molten salt devices is greatly reduced, so that the life cycle of the molten salt devices is prolonged by 15 to 20 years; the washed solution is crystallized by concentration to be prepared into a high-quality fertilizer or cement additive which can not pollute the environment; the purity of the molten salt is greatly improved, and the service life of the molten salt is prolonged to 15 years or more; and the required cost is lower, and the benefits are great.
Description
Technical field
The present invention relates to a kind of preparation method of salt, specifically, relate to a kind of preparation method of high-purity heat-conduction energy storage molten salt.
Background technology
At present, in preparing high-purity heat-conduction energy storage molten salt field, the preparation of fused salt generally adopts the method for electrolysis, and this preparation method has shortcomings:
(1) cost is high, and investment is large, and income is low;
(2) the various corrosive medium index severe overweights of fused salt, as chlorion 1000ppm, vitriol 1000ppm, water-insoluble 2000ppm, calcium contents 100ppm, Mg content 200ppm, iron level 100ppm, the corrosive medium of these severe overweights causes equipment to be corroded in a short time, has shortened the work-ing life of equipment and the work-ing life of fused salt itself;
(3) in fused salt use procedure, various metallic substance fused salt equipment is had to stronger corrodibility, greatly shortened the life cycle of metallic substance fused salt equipment;
(4) because the impurity of fused salt is high, purity is low, causes equipment corrosion or fouling, the thermal conductivity of fused salt and heat transfer efficiency is reduced, Melting point elevation.Therefore the work-ing life of fused salt generally about 3 years,
(5) because fused salt is often changed, life cycle is short, and institute is so that cost improves, and environmental pollution is serious.
Summary of the invention
The technical problem to be solved in the present invention is to overcome above-mentioned defect, provide that a kind of cost is low, income is high and the preparation method to the little high-purity heat-conduction energy storage molten salt of equipment corrosion, the fused salt making by this preparation method has higher purity, thermal conductivity and heat transfer efficiency, and itself has heat accumulation fused salt, cause the heat storage capacity of fused salt high.
For addressing the above problem, the technical solution adopted in the present invention is:
A preparation method for high-purity heat-conduction energy storage molten salt, is characterized in that: described preparation method comprises the following steps:
A. choose respectively the single salt of savoring being up to state standards;
B. single purification of savoring salt;
C. single salt of savoring is obtained to fused salt after physical mixed is even.
As a kind of improvement:
Described single purification number of times of savoring salt is twice.
As further improvement:
Single salt of savoring in described steps A is: saltpetre, SODIUMNITRATE and Sodium Nitrite.
As further improvement:
Described single purification of savoring salt comprises the following steps:
A) dissolve, single salt of savoring is dissolved to the single product salts solution of formation; Single product salts solution is passed through to pressure filter press filtration
B) recrystallization, carries out cooling rear recrystallization by the single product salts solution after press filtration;
C) washing, the single salt of savoring with pure water after to recrystallization washs;
D) heating for dissolving, puts into electric heating reacting kettle by the single salt of savoring after washing, adds pure water post-heating to dissolve;
E) crystallization, is placed in water cooler crystallisation by cooling by the single product salts solution in electric heating reacting kettle;
F) dehydration, passes through centrifuge dewatering by the single salt of savoring after crystallization;
G) washing, washs the single salt of savoring after dewatering with pure water;
H) washing is dry, and after washing, single salt of savoring is again by centrifuge dewatering, then dry, obtains highly purified single salt of savoring.
Single product in salt after purification, the purity of saltpetre is 99.8%, higher than 99.4% before purifying; The purity of Sodium Nitrite is 99.3%, higher than 98.5% before purifying; The purity of SODIUMNITRATE is 99.7%, higher than 99.3% before purifying.
And single content of savoring chlorion CL and water-insoluble in salt also reduces greatly, design parameter as shown in Table 1.
Table one
As can be seen from Table I single after twice purification savor salt at the content of chlorion CL, water-insoluble apparently higher than before purifying, refining effect is remarkable.
As further improving:
The weight ratio of described nitric acid Potassium, SODIUMNITRATE and Sodium Nitrite is 53: 7: 40.
As further improving:
The weight ratio of described nitric acid Potassium, SODIUMNITRATE and Sodium Nitrite is 2: 1: 1.
As further improving:
Single salt of savoring in described steps A is: saltpetre and Sodium Nitrite.
The weight ratio of described nitric acid Potassium and Sodium Nitrite is 1: 1.
Owing to having adopted technique scheme, the preparation method described in the present invention has following advantages:
(1) reduced the content of corrosive medium, greatly reduced the corrodibility to various metallic substance fused salt equipment, made the life cycle of fused salt equipment extend for 15～20 anniversaries;
(2) solution after washing, by after condensing crystal, can be made fertilizer or cement additire, can be to environment;
(3) purity of fused salt is greatly improved, and extends to the work-ing life of fused salt more than 15 years;
(4) required cost is lower, and income is large.
In addition, the fused salt making by this preparation method has that purity is high, thermal conductivity and the high feature of heat transfer efficiency, and the fused salt making by this preparation method has thermal storage performance and heat dispersion faster, improves the heat storage capacity of fused salt.Concrete detected result as shown in Table 2.
Table two
| Fusing point ℃ | 142-146 | Cr content ppm≤ | 10 |
| Cl content ppm≤ | 100 | Ni content ppm≤ | 10 |
| Sulphur content ppm≤ | 60 | Ca content ppm≤ | 10 |
| Carbonate ppm≤ | 80 | Mg content ppm≤ | 10 |
| Sodium oxide ppm≤ | 100 | Iron level ppm≤ | 15 |
| Carbon content ppm≤ | 80 | Water-insoluble ppm≤ | 10 |
| OH-content ppm≤ | 100 | Moisture %≤ | 0.1 |
Known by table two, according to preparation method of the present invention, aspect the content of reduction corrosive medium, effect is remarkable.
Below in conjunction with embodiment, the present invention will be further described.
Embodiment
Embodiment 1: a kind of preparation method of high-purity heat-conduction energy storage molten salt, choose respectively the single salt of savoring being up to state standards: 530 kilograms, saltpetre, 400 kilograms of 70 kilograms of SODIUMNITRATE and Sodium Nitrites, after dissolving respectively, form single product salts solution, by pressure filter press filtration, again single product salts solution is carried out to cooling rear recrystallization, single salt of savoring with pure water after to recrystallization washs, again the single salt of savoring after washing is put into electric heating reacting kettle, add pure water post-heating, single product salts solution in electric heating reacting kettle is placed in to water cooler crystallisation by cooling, single salt of savoring after crystallization is passed through to centrifuge dewatering, with pure water, the single salt of savoring after dewatering is washed again, after washing, single salt of savoring passes through centrifuge dewatering again, then dry, obtain highly purified single salt of savoring.
By three kinds of highly purified single salt nitric acid Potassium, SODIUMNITRATE, Sodium Nitrites savored, be to weigh at 53: 7: 40 to put into three-dimensional mixer and mix and form the about 800kg of highly purified fused salt by weight again.
Embodiment 2: a kind of preparation method of high-purity heat-conduction energy storage molten salt, choose respectively the single salt of savoring being up to state standards: 500 kilograms, saltpetre, 250 kilograms of 250 kilograms of SODIUMNITRATE and Sodium Nitrites, after dissolving respectively, form single product salts solution, by pressure filter press filtration, again single product salts solution is carried out to cooling rear recrystallization, single salt of savoring with pure water after to recrystallization washs, again the single salt of savoring after washing is put into electric heating reacting kettle, add pure water post-heating, single product salts solution in electric heating reacting kettle is placed in to water cooler crystallisation by cooling, single salt of savoring after crystallization is passed through to centrifuge dewatering, with pure water, the single salt of savoring after dewatering is washed again, after washing, single salt of savoring passes through centrifuge dewatering again, then dry, obtain highly purified single salt of savoring.
By three kinds of highly purified single salt nitric acid Potassium, SODIUMNITRATE and Sodium Nitrites savored, be to put into three-dimensional mixer at 2: 1: 1 to mix the highly purified fused salt 780kg of formation by weight again.
Embodiment 3: a kind of preparation method of high-purity heat-conduction energy storage molten salt, choose respectively the single salt of savoring being up to state standards: each 500 kilograms of saltpetre and Sodium Nitrites, after dissolving respectively, form single product salts solution, by pressure filter press filtration, again single product salts solution is carried out to cooling rear recrystallization, single salt of savoring with pure water after to recrystallization washs, again the single salt of savoring after washing is put into electric heating reacting kettle, add pure water post-heating, single product salts solution in electric heating reacting kettle is placed in to water cooler crystallisation by cooling, single salt of savoring after crystallization is passed through to centrifuge dewatering, with pure water, the single salt of savoring after dewatering is washed again, after washing, single salt of savoring passes through centrifuge dewatering again, then dry, obtain highly purified single salt of savoring.
By two kinds of highly purified single salt nitric acid Potassium and Sodium Nitrites savored, be to put into three-dimensional mixer at 1: 1 to mix and form highly purified fused salt 750kg by weight again.
In above-mentioned steps, electric heating reacting kettle, water cooler, whizzer, pressure filter and three-dimensional mixer are commercially available prod.Wherein, three-dimensional mixer utilizes unique three-dimensional oscillating, translation rotation and rock and roll principle, produce one powerful ALT pulse campaign, continuously promote to carry out mixture, the vicissitudinous energy gradient of eddy current tool of its generation, has good mixing effect, mixing time is short, and mixture homogeneity reaches 99.5% with first-class advantage.
Three-dimensional mixer is that Jiangyin City Shuan Chengyaohua mechanical means company limited produces, model SC-1500;
Electric heating reacting kettle is that Laizhou Hong Feng chemical produces, model 5000L;
Pressure filter is that Shanghai great Zhang filter plant company limited produces, model 800;
Water cooler is that Jiangyan City Jin Xin heat exchanger factory manufactures, model GLC series;
Whizzer is that Taizhou City Bao Jin Machinery Manufacturing Co., Ltd. produces, model SME301-1200.
Claims (1)
1. a preparation method for high-purity heat-conduction energy storage molten salt, is characterized in that: described preparation method comprises the following steps:
A. choose respectively the single salt of savoring being up to state standards;
B. single purification of savoring salt;
C. single product after salt mixes obtained to fused salt;
In described step B, single purification of savoring salt comprises the following steps:
A) dissolve, single salt of savoring is dissolved to the single product salts solution of formation;
B) recrystallization, carries out cooling rear recrystallization by the single product salts solution after dissolving;
C) washing, the single salt of savoring with pure water after to recrystallization washs;
D) heating for dissolving, puts into electric heating reacting kettle by the single salt of savoring after washing, adds pure water post-heating to dissolve;
E) crystallization, is placed in water cooler crystallisation by cooling by the single product salts solution in electric heating reacting kettle;
F) dehydration, passes through centrifuge dewatering by the single salt of savoring after crystallization;
G) washing, washs the single salt of savoring after dewatering with pure water;
H) washing is dry, and after washing, single salt of savoring is again by centrifuge dewatering, then dry, obtains highly purified single salt of savoring.
2. the preparation method of a kind of high-purity heat-conduction energy storage molten salt according to claim 1, is characterized in that: described single purification number of times of savoring salt is twice.
3. the preparation method of a kind of high-purity heat-conduction energy storage molten salt according to claim 1 and 2, is characterized in that: the single salt of savoring in described steps A is: saltpetre, SODIUMNITRATE and Sodium Nitrite.
4. the preparation method of a kind of high-purity heat-conduction energy storage molten salt according to claim 3, is characterized in that: the weight ratio of described nitric acid Potassium, SODIUMNITRATE and Sodium Nitrite is 53: 7: 40.
5. the preparation method of a kind of high-purity heat-conduction energy storage molten salt according to claim 3, is characterized in that: the weight ratio of described nitric acid Potassium, SODIUMNITRATE and Sodium Nitrite is 2: 1: 1.
6. the preparation method of a kind of high-purity heat-conduction energy storage molten salt according to claim 1 and 2, is characterized in that: described single salt of savoring is: saltpetre and Sodium Nitrite.
7. the preparation method of a kind of high-purity heat-conduction energy storage molten salt according to claim 6, is characterized in that: the weight ratio of described nitric acid Potassium and Sodium Nitrite is 1: 1.
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| MA20150382A1 (en) * | 2012-08-17 | 2015-10-30 | Basf Se | Process for improving nitrate salt compositions during their use as a heat transfer medium or heat accumulator |
| CN103105085A (en) * | 2013-02-01 | 2013-05-15 | 北京工业大学 | Automobile tail gas waste heat recovery fused salt heat transfer and heat storage heat exchanger |
| CN103923612B (en) * | 2013-12-26 | 2017-10-27 | 深圳市爱能森科技有限公司 | Quartz sand is combined binary nitric acid Molten Salt Heat Transfer heat storage medium and preparation method thereof |
| CN103204522A (en) * | 2013-04-09 | 2013-07-17 | 牟邦志 | Preparation method of high-purity mass potassium nitrate |
| CN103911124B (en) * | 2013-12-26 | 2016-11-23 | 深圳市爱能森科技有限公司 | Waterglass complex ternary nitric acid Molten Salt Heat Transfer heat storage medium and preparation method and application |
| CN105115336A (en) * | 2015-09-07 | 2015-12-02 | 河北艺能锅炉有限责任公司 | Molten salt thermal storage heater |
| 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 |
| CN108851193B (en) * | 2018-05-29 | 2021-08-10 | 江苏中烟工业有限责任公司 | Preparation method of heating non-combustible core material |
| CN111849427A (en) * | 2020-09-07 | 2020-10-30 | 新疆硝石钾肥有限公司 | Mixed salt production system of sodium nitrate and potassium nitrate |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1146972A (en) * | 1995-06-08 | 1997-04-09 | 蔺向阳 | Process for preparing potassium nitrate and sodium nitrate |
| CN1184077A (en) * | 1996-12-06 | 1998-06-10 | 陈淑奇 | Ion exchange process for producing potassium nitrate |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1146972A (en) * | 1995-06-08 | 1997-04-09 | 蔺向阳 | Process for preparing potassium nitrate and sodium nitrate |
| CN1184077A (en) * | 1996-12-06 | 1998-06-10 | 陈淑奇 | Ion exchange process for producing potassium nitrate |
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Denomination of invention: A Preparation Method of High Purity Heat Conductive Energy Storage Molten Salt Effective date of registration: 20230316 Granted publication date: 20140205 Pledgee: Postal Savings Bank of China Limited by Share Ltd. Weifang branch Pledgor: WEIFANG CHANGSHENG NITRATE CO.,LTD. Registration number: Y2023980034891 |
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