CN204841649U - A retort for preparing fluoride fused salt - Google Patents
A retort for preparing fluoride fused salt Download PDFInfo
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- CN204841649U CN204841649U CN201520614732.XU CN201520614732U CN204841649U CN 204841649 U CN204841649 U CN 204841649U CN 201520614732 U CN201520614732 U CN 201520614732U CN 204841649 U CN204841649 U CN 204841649U
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- retort
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Abstract
The utility model discloses a retort for preparing fluoride fused salt, the retort includes one a jar of body and a crucible, jar body is including a top cap, one jar of wall and a base, the top cap jar wall with the base encloses to close and forms a closed chamber, the crucible is located in the closed chamber, and paste and locate on the internal face of jar wall, the crucible is made by carbon - carbon composites, the below of base still is equipped with a flange and a bayonet lock, flange with the bayonet lock be used for with the base detachably be fixed in the bottom of jar wall, the retort still includes an insulating washer, the insulating washer be used for with the crucible seal in the below of top cap. The retort has the preparation of characteristics such as high temperature resistant, corrosion -resistant, that the seal is good, specially adapted high -purity fluoride fused salt, the retort has realized jar the body to be connected with dismantling of crucible, can change the crucible extremely conveniently, greatly reduced the use cost of equipment.
Description
Technical field
The utility model relates to a kind of chemical industry equipment, particularly a kind of retort for the preparation of fluoride molten salt.
Background technology
The stable supply of the energy and resource is the necessary basis ensureing China's long-term sustainable development, and nuclear energy is that a kind of energy density is high, clean, the energy of low-carbon (LC), is the important means ensureing national energy security, promote energy-saving and emission-reduction.Thorium base MSR nuclear power system (TMSR) is one of global forth generation nuclear reactor technology, be using thorium uranium as nuclear fuel, fused salt is as the advanced high temperature nuclear reactor of cooling agent, at guarantee national energy security, promote energy-saving and emission-reduction, promote in economic development significant, be also there is international influence, country needs world's frontier science and technology of plugging a gap badly.
High-temperature fluorination thing fused salt is with the performance of its excellence, as large in the operating temperature of broadness, thermal capacity, good fluidity, the hot operation etc. that can realize under normal pressure, both act as reactor coolant, is again the supporting electrolyte of nuclear fuel, is one of critical material of thorium base MSR.The character such as hot physical property, corrosivity, neutronics of high-temperature fluorination thing fused salt not only affects the efficiency of reactor, more closely bound up with its safe operation.Therefore very strict requirement is had to entering to pile fused salt, as under high temperature, the corrosivity of cooling agent villiaumite alloy material depends on the oxidative impurities content such as water, oxygen, sulphur to a great extent, MSR uses harsh requirement to be very large challenge concerning the technique such as preparation, purifying of fused salt.
Due to the metal impurities ion and the oxo-anions that make the corrosion of structural material fused salt in turn introduce other, exacerbate the complexity of fused salt removal of impurities system further, greatly have impact on degree and the effect of Impurity removal.And fluoride molten salt almost cannot be avoided the corrosion of plant constructional material in the preparation process of fluoride molten salt, it is the extremely crucial technical barrier in fused salt purification and impurity removal aspect.
Such as U.S.'s Oak Ridge laboratory (ORNL) sixties in last century adopts Ni-based material crucible to carry out the preparation of fluoride molten salt, and the corrosion of fused salt alloy material is comparatively serious, prepares in the process of fused salt to reduce generating a large amount of metal impurities.Although this technique is follow-up have employed high temperature filtration measure, because the corrosivity of fused salt is strong, and Ni, Cr, Fe powder that reduction reaction produces is very thin, large, the weak effect of filter operation difficulty under 600 DEG C of hot conditions.Impurity content still very high (the bibliography JamesH.Shaffer such as the fused salt product nickel content of gained and oxygen, Preparationandhandlingofsaltmixturesforthemoltensaltreac torexperiment, ORNL-4616, P28).Fused salt Preparation equipment simultaneously disclosed in Chinese patent CN204275955U adopts pure nickel matter crucible, also can produce larger corrosion to pollute fused salt in actual production process.In the manufacture practice of current fluoride molten salt, still do not find comparatively suitable crucible material to avoid the corrosion of fused salt and strong corrosive medium completely, be a difficult problem that solution is needed in current fluoride molten salt preparation development badly.
Generally speaking, existing high-temperature fluorination thing fused salt Preparation equipment, what its crucible generally adopted is the materials such as graphite, 316 stainless steels, pure nickel, all than being easier to the attack being subjected to high temperature strong corrosion medium, introduce a large amount of corrosion contaminating impurity fused salts on the one hand, exacerbate the complexity of fused salt removal of impurities system, greatly have impact on degree and the effect of Impurity removal, the outward appearance cleanliness factor of fused salt is poor, and the life simultaneously due to the effect crucible of corrosion is also all shorter; Existing fused salt Preparation equipment is generally that crucible and tank body are welded as a whole completely on the other hand, and cannot carry out dismounting and change to it when crucible is scrapped, tank body cannot recycle, and together can only scrap with crucible, and the replacing maintenance cost of equipment is higher.
Utility model content
The technical problems to be solved in the utility model be in order to overcome prior art high-temperature fluorination thing fused salt Preparation equipment easily reduces fused salt cleanliness factor, pot life is short, and crucible and tank body Integral design and the defect that when crucible is scrapped, replacement cost is high, and provide a kind of retort for the preparation of fluoride molten salt.The retort that the utility model provides integrates charging process, fused salt melting operation, fused salt cleaning procedure, sampling operation, fused salt transfering process, there is high temperature resistant, dielectric corrosion, the good leak tightness etc. of being able to bear strong corrosion distinguishing feature, utilization ratio is high, is specially adapted to the preparation of high-purity fluoride molten salt; Described retort achieves removably connecting of tank body and crucible, can change crucible extremely easily, greatly reduce the use cost of equipment; Described retort can bear the operating pressure of-0.5Mpa ~ 0.5Mpa, and principle of differential pressure can be utilized to carry out discharging transfer operation.
The utility model solves above-mentioned technical problem by following technical proposals:
The utility model provides a kind of retort for the preparation of fluoride molten salt, described retort comprises a tank body and a crucible, described tank body comprises a top cover, one tank skin and a base, described top cover, described tank skin and described base enclose formation one airtight chamber, described crucible is located in described airtight chamber, and be attached on the internal face of described tank skin, described crucible is made up of carbon-carbon composite, the below of described base is also provided with an adpting flange and a bayonet lock, described adpting flange and described bayonet lock are used for the bottom described base being removably fixed on described tank skin, described retort also comprises an insulating washer, described insulating washer is used for the below of described sealed crucible in described top cover.
Preferably, an elastic buffering pad is also provided with between the bottom of described crucible and described base.
Preferably, described retort also comprises a feeding device, a Material and article holding frame, a sampler, an air inlet pipe and an escape pipe, described feeding device, described sampler, described air inlet pipe and described escape pipe all wear described top cover, and stretching in described crucible, described Material and article holding frame is fixedly arranged on the top of described top cover by 4 feets.
Wherein, the charging aperture of described feeding device and described escape pipe all stretch in the headroom of described crucible, the sample tap of described sampler stretches in the middle hypomere space of described crucible, described air inlet pipe stretches in the bottom space of described crucible, and the internal diameter of described air inlet pipe and described escape pipe is 10-15mm.
Wherein, described feeding device is a reinforced hopper, described reinforced hopper has a charge door, the upper end of described charge door is internal diameter is the cylindric of 30-35cm, the taper of to be cone bottom diameter be in the lower end of described charge door 30-35cm, the lower end of described charge door is also connected with a blanking pipe by a valve, and the material of described reinforced hopper is pure nickel.
Preferably, described tank body and described crucible are cylindrical.
Preferably, described tank skin comprises insulation cortex, an insulating materials heat-insulation layer and the resistive heater layer arranged from outside to inside, and described resistive heater layer is wound around and is arranged in the outside wall surface of described crucible.
Wherein, described insulation cortex is made up of SUS314 stainless steel material, and described insulating materials heat-insulation layer is made up of asbestos, alumina silicate needle punched blanket or polycrystalline alumina fiber.
Preferably, described insulating washer is made up of high purity graphite.The insulating washer adopting high purity graphite to make has high temperature resistant, corrosion resistant advantage.
Preferably, the bottom of described tank skin is also provided with at least two castors, for the movement of described retort.
Preferably, described retort also comprises one first thermocouple temperature measuring apparatus and one second thermocouple temperature measuring apparatus, and described first thermocouple is located in the epimere space of described crucible, and described second thermocouple is located in the hypomere space of described crucible.
Positive progressive effect of the present utility model is:
(1) retort that the utility model provides integrates charging process, fused salt melting operation, fused salt cleaning procedure, sampling operation, fused salt transfering process, there is high temperature resistant, dielectric corrosion, the good leak tightness etc. of being able to bear strong corrosion distinguishing feature, utilization ratio is high, is specially adapted to the preparation of high-purity fluoride molten salt; The fluoride molten salt product utilizing this equipment to prepare is pure white, puts down without the need to fused salt impurity content being made to be reduced to reactor quality water through process means such as special contaminant filters, can meet the instructions for use of MSR completely;
(2) crucible adopts carbon-carbon composite, solve the problem of the high temperature corrosion dielectric corrosion alloy material always perplexed in fluoride molten salt preparation process, substantially prolongs the service life of equipment, and achieve removably connecting of tank body and crucible, crucible can be changed extremely easily, greatly reduce the use cost of equipment;
(3) described retort can bear the operating pressure of-0.5Mpa ~ 0.5Mpa, operable pressure limit is wide in range, and principle of differential pressure can be utilized to carry out discharging transfer operation, achieve high temperature highly corrosive fused salt and shift in completely airtight environment, security is good.
Accompanying drawing explanation
Fig. 1 is the structural representation of the retort of the utility model embodiment 1.
Detailed description of the invention
Lift preferred embodiment below, and come by reference to the accompanying drawings clearlyer intactly the utility model to be described.
Embodiment 1
The structural representation of the retort for the preparation of fluoride molten salt that the present embodiment provides as shown in Figure 1.Described retort comprises a tank body and a crucible 7, described tank body comprises a top cover 2, one tank skin 3 and a base 1, described top cover 2, described tank skin 3 and described base 1 enclose formation one airtight chamber, described crucible 7 is located in described airtight chamber, and be attached on the internal face of described tank skin 3, described crucible 7 is made up of carbon-carbon composite, the below of described base 1 is also provided with adpting flange 17 and a bayonet lock 16, described adpting flange 17 and described bayonet lock 16 are for being removably fixed on the bottom of described tank skin 3 by described base 1, described retort also comprises an insulating washer 15, described insulating washer 15 is for being sealed in the below of described top cover 2 by described crucible 7.An elastic buffering pad 8 is also provided with between the bottom of described crucible 7 and described base 1.
Described retort also comprises feeding device 12, Material and article holding frame 13, sampler 11, air inlet pipe 10 and an escape pipe 14, described feeding device 12, described sampler 11, described air inlet pipe 10 and described escape pipe 14 all wear described top cover 2, and stretching in described crucible 7, described Material and article holding frame 13 is fixedly arranged on the top of described top cover 2 by 4 feets.Wherein, the charging aperture of described feeding device 12 and described escape pipe 14 all stretch in the headroom of described crucible 7, the sample tap of described sampler 11 stretches in the middle hypomere space of described crucible 7, described air inlet pipe 10 stretches in the bottom space of described crucible 7, and described air inlet pipe 10 is for passing into the gases such as hydrogen fluoride, hydrogen, argon gas.The internal diameter of described air inlet pipe 10 and described escape pipe 14 is 10-15mm.Wherein, described feeding device 12 is a reinforced hopper, described reinforced hopper has a charge door, the upper end of described charge door is internal diameter is the cylindric of 30-35cm, the taper of to be cone bottom diameter be in the lower end of described charge door 30-35cm, the lower end of described charge door is also connected with a blanking pipe by a valve, and the material of described reinforced hopper is pure nickel.
Described tank body and described crucible 7 are cylindrical.Described tank skin 3 comprises insulation cortex 9, insulating materials heat-insulation layer 6 and the resistive heater layer 5 arranged from outside to inside, and described resistive heater layer 5 is wound around and is arranged in the outside wall surface of described crucible 7.Wherein, described insulation cortex 9 is made up of SUS314 stainless steel material, and described insulating materials heat-insulation layer 6 is made up of asbestos, alumina silicate needle punched blanket or polycrystalline alumina fiber.
Described insulating washer 15 is made up of high purity graphite.The bottom of described tank skin 3 is also provided with at least two castors 4, for the movement of described retort.Described retort also comprises one first thermocouple temperature measuring apparatus and one second thermocouple temperature measuring apparatus, and described first thermocouple is located in the epimere space of described crucible 7, and described second thermocouple is located in the hypomere space of described crucible 7.
Effect example 1
The retort utilizing embodiment 1 to provide carries out the preparation of high-purity fluoride molten salt, and operating procedure is as follows:
(1) airtight test: the air-tightness of each gas piping of close inspection, valve and Pressure gauge part, is filled with the argon gas of 0.2Mpa pressure in advance, keeps 0.5h, sees whether its pressure occurs change, if pressure remains unchanged, then the air-tightness of proof system is good.
(2) raw material takes: accurately take the LiF2.413Kg after vacuum drying respectively, NaF0.964Kg, KF4.876Kg, fully mix, and must carry out airtight simultaneously, avoids material to expose in atmosphere, in order to avoid suck more moisture content as far as possible.
(3) feeding operation: after using absolute ethyl alcohol to be cleaned up by reinforced hopper, then fluoride molten salt is carefully added in retort by reinforced hopper, avoid airborne dust to cause loss of material as far as possible, and then cause material proportion to change.
(4) vaccum dewatering: open vacuum pump evacuation 2 hours, pays close attention to vacuum situation of change.
(5) intensification melting: set heating schedule: be raised to 200 DEG C in 0.5 hour, is heated to 300 DEG C in 1 hour, within 1 hour, is heated to 470 DEG C, within 2 hours, is heated to 600 DEG C of meltings.
(6) pass into hydrogen/hydrogen fluoride impurity and purification: first in tank body, pass into hydrogen, then pass into the moisture in high-pure anhydrous hydrogen fluoride removal fused salt, the generation of control oxide, reduces the oxygen content of fused salt, passes into H
2/ HF mist, after 48 ~ 72 hours, closes HF, and the alloy material being fluorinated hydrogen-type corrosion is reduced into metal simple-substance and stays in tank body by continuation logical hydrogen again, reduces the corrosion of equipment.Last applying argon gas again drives hydrogen remaining in tank body and hydrogen fluoride.
(7) fused salt transfer: in advance about 40min opens pipeline and is heated to 600 DEG C, controls pipeline valve well, is transferred in storage tank by fused salt.In storage tank, pass into about 0.2Mpa pressure argon gas after having shifted again carry out pressurize cooling.Be cooled to after normal temperature until temperature of molten salt and take off storage tank, the fused salt in storage tank is shifted rapidly the sampling of placement glove box and analyze.
(8) testing result is analyzed: every quality index of gained fused salt is as follows:
1. fusing point: 456 ~ 458 DEG C.
2. oxygen content: 80 ~ 100ppm.
3. each metal impurities ion concentration: all lower than below 5ppm.
4. each anion-content: chlorion, phosphate radical, nitrate anion plasma are all lower than below 25ppm, and sulfate radical is lower than detectability.
The retort that embodiment 1 provides adopts the liner of crucible as this equipment of carbon-carbon composite, crucible and tank body do not do soldering, and use high-temperature corrosion resistance insulating washer to seal, fabulous seal ensure that fused salt melt in fused salt preparation process, the high temperature corrosive mediums such as hydrogen fluoride only react in crucible, and high temperature corrosion medium is extremely small to the corrosion of carbon-to-carbon composite crucible, after the manufacture of tens of batches of fused salts, crucible is not almost corroded, metal impurities ion concentration <5ppm in the fused salt of preparation, be different from completely when using nickel matter crucible for smelting and introduce metal impurities ion because of corrosion, there will not be a large amount of nickel powder of fused salt surface flotation, fused salt product color is poor, the situation of inner inclusion black nickel spot, the fused salt product adopting carbon-to-carbon composite crucible to prepare is pure white, be reduced to reactor quality water without the need to can make fused salt impurity content through process means such as special contaminant filters to put down, the complete instructions for use that can meet MSR, the result that fused salt metal impurities prepared by the carbon-to-carbon composite crucible that table 1 provides for use Ni crucible and embodiment 1 compare.
The impurity of fused salt metal prepared by the retort showing 1Ni crucible and embodiment 1 compares
Less corrosiveness substantially prolongs the service life of crucible simultaneously, in addition because crucible is combined with the activity of tank body, only adpting flange and bayonet lock need be removed and can realize being separated completely of crucible and tank body, very convenient scrapping and replacing in crucible, avoid occurring the at present normal tank body that occurs and crucible is welded cannot dismantle the situation of together scrapping, achieve the utilization again of tank body, thus reduce the replacing maintenance cost of equipment significantly.
Claims (11)
1. the retort for the preparation of fluoride molten salt, described retort comprises a tank body and a crucible, it is characterized in that, described tank body comprises a top cover, one tank skin and a base, described top cover, described tank skin and described base enclose formation one airtight chamber, described crucible is located in described airtight chamber, and be attached on the internal face of described tank skin, described crucible is made up of carbon-carbon composite, the below of described base is also provided with an adpting flange and a bayonet lock, described adpting flange and described bayonet lock are used for the bottom described base being removably fixed on described tank skin, described retort also comprises an insulating washer, described insulating washer is used for the below of described sealed crucible in described top cover.
2. retort as claimed in claim 1, is characterized in that, be also provided with an elastic buffering pad between the bottom of described crucible and described base.
3. retort as claimed in claim 1, it is characterized in that, described retort also comprises a feeding device, a Material and article holding frame, a sampler, an air inlet pipe and an escape pipe, described feeding device, described sampler, described air inlet pipe and described escape pipe all wear described top cover, and stretching in described crucible, described Material and article holding frame is fixedly arranged on the top of described top cover by 4 feets.
4. retort as claimed in claim 3, it is characterized in that, the charging aperture of described feeding device and described escape pipe all stretch in the headroom of described crucible, the sample tap of described sampler stretches in the middle hypomere space of described crucible, described air inlet pipe stretches in the bottom space of described crucible, and the internal diameter of described air inlet pipe and described escape pipe is 10-15mm.
5. the retort as described in claim 3 or 4, it is characterized in that, described feeding device is a reinforced hopper, described reinforced hopper has a charge door, the upper end of described charge door is internal diameter is the cylindric of 30-35cm, the taper of to be cone bottom diameter be in the lower end of described charge door 30-35cm, the lower end of described charge door is also connected with a blanking pipe by a valve, and the material of described reinforced hopper is pure nickel.
6. retort as claimed in claim 1, it is characterized in that, described tank body and described crucible are cylindrical.
7. retort as claimed in claim 1, is characterized in that, described tank skin comprises insulation cortex, an insulating materials heat-insulation layer and the resistive heater layer arranged from outside to inside, and described resistive heater layer is wound around and is arranged in the outside wall surface of described crucible.
8. retort as claimed in claim 7, it is characterized in that, described insulation cortex is made up of SUS314 stainless steel material, and described insulating materials heat-insulation layer is made up of asbestos, alumina silicate needle punched blanket or polycrystalline alumina fiber.
9. retort as claimed in claim 1, it is characterized in that, described insulating washer is made up of high purity graphite.
10. retort as claimed in claim 1, it is characterized in that, the bottom of described tank skin is also provided with at least two castors, for the movement of described retort.
11. retort as claimed in claim 1, it is characterized in that, described retort also comprises one first thermocouple temperature measuring apparatus and one second thermocouple temperature measuring apparatus, and described first thermocouple is located in the epimere space of described crucible, and described second thermocouple is located in the hypomere space of described crucible.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201520614732.XU CN204841649U (en) | 2015-08-14 | 2015-08-14 | A retort for preparing fluoride fused salt |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201520614732.XU CN204841649U (en) | 2015-08-14 | 2015-08-14 | A retort for preparing fluoride fused salt |
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| CN204841649U true CN204841649U (en) | 2015-12-09 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107189766A (en) * | 2017-06-08 | 2017-09-22 | 中国科学院上海应用物理研究所 | Prepared by a kind of inert environments fused salt, the apparatus and method of transhipment |
| CN110671517A (en) * | 2019-09-30 | 2020-01-10 | 中国科学院上海应用物理研究所 | Molten salt cut-off device, and use method and application thereof |
| CN113332787A (en) * | 2021-08-05 | 2021-09-03 | 天津包钢稀土研究院有限责任公司 | Filtration purification device of tombarthite chloride fused salt |
-
2015
- 2015-08-14 CN CN201520614732.XU patent/CN204841649U/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107189766A (en) * | 2017-06-08 | 2017-09-22 | 中国科学院上海应用物理研究所 | Prepared by a kind of inert environments fused salt, the apparatus and method of transhipment |
| CN110671517A (en) * | 2019-09-30 | 2020-01-10 | 中国科学院上海应用物理研究所 | Molten salt cut-off device, and use method and application thereof |
| CN113332787A (en) * | 2021-08-05 | 2021-09-03 | 天津包钢稀土研究院有限责任公司 | Filtration purification device of tombarthite chloride fused salt |
| CN113332787B (en) * | 2021-08-05 | 2021-10-29 | 天津包钢稀土研究院有限责任公司 | Filtration purification device of tombarthite chloride fused salt |
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Granted publication date: 20151209 Termination date: 20180814 |