CN221388094U - High-value utilization system of waste quartz crucible - Google Patents
High-value utilization system of waste quartz crucible Download PDFInfo
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- CN221388094U CN221388094U CN202323264807.XU CN202323264807U CN221388094U CN 221388094 U CN221388094 U CN 221388094U CN 202323264807 U CN202323264807 U CN 202323264807U CN 221388094 U CN221388094 U CN 221388094U
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- 239000002699 waste material Substances 0.000 title claims abstract description 95
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 85
- 239000010453 quartz Substances 0.000 title claims abstract description 73
- 238000005406 washing Methods 0.000 claims abstract description 150
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 101
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims abstract description 101
- 239000007788 liquid Substances 0.000 claims abstract description 69
- 238000006243 chemical reaction Methods 0.000 claims abstract description 59
- 238000000926 separation method Methods 0.000 claims abstract description 41
- 239000004115 Sodium Silicate Substances 0.000 claims abstract description 36
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229910052911 sodium silicate Inorganic materials 0.000 claims abstract description 36
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 120
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 72
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 60
- 239000002994 raw material Substances 0.000 claims description 47
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- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 36
- 238000002156 mixing Methods 0.000 claims description 25
- 239000000843 powder Substances 0.000 claims description 23
- 238000001816 cooling Methods 0.000 claims description 21
- 229910052751 metal Inorganic materials 0.000 claims description 20
- 239000002184 metal Substances 0.000 claims description 20
- 238000000746 purification Methods 0.000 claims description 9
- 239000000047 product Substances 0.000 abstract description 40
- 239000006227 byproduct Substances 0.000 abstract description 8
- 238000011084 recovery Methods 0.000 abstract description 6
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- 238000001035 drying Methods 0.000 description 17
- 238000010586 diagram Methods 0.000 description 16
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- 238000004519 manufacturing process Methods 0.000 description 6
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- 229910021645 metal ion Inorganic materials 0.000 description 5
- 239000000377 silicon dioxide Substances 0.000 description 5
- 239000008139 complexing agent Substances 0.000 description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 239000012043 crude product Substances 0.000 description 3
- 239000006148 magnetic separator Substances 0.000 description 3
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- 229910052710 silicon Inorganic materials 0.000 description 3
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- 238000003786 synthesis reaction Methods 0.000 description 3
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 2
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000001099 ammonium carbonate Substances 0.000 description 2
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- 239000000126 substance Substances 0.000 description 2
- RAEOEMDZDMCHJA-UHFFFAOYSA-N 2-[2-[bis(carboxymethyl)amino]ethyl-[2-[2-[bis(carboxymethyl)amino]ethyl-(carboxymethyl)amino]ethyl]amino]acetic acid Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(=O)O)CCN(CCN(CC(O)=O)CC(O)=O)CC(O)=O RAEOEMDZDMCHJA-UHFFFAOYSA-N 0.000 description 1
- RNMCCPMYXUKHAZ-UHFFFAOYSA-N 2-[3,3-diamino-1,2,2-tris(carboxymethyl)cyclohexyl]acetic acid Chemical compound NC1(N)CCCC(CC(O)=O)(CC(O)=O)C1(CC(O)=O)CC(O)=O RNMCCPMYXUKHAZ-UHFFFAOYSA-N 0.000 description 1
- BDDLHHRCDSJVKV-UHFFFAOYSA-N 7028-40-2 Chemical compound CC(O)=O.CC(O)=O.CC(O)=O.CC(O)=O BDDLHHRCDSJVKV-UHFFFAOYSA-N 0.000 description 1
- FCKYPQBAHLOOJQ-UHFFFAOYSA-N Cyclohexane-1,2-diaminetetraacetic acid Chemical compound OC(=O)CN(CC(O)=O)C1CCCCC1N(CC(O)=O)CC(O)=O FCKYPQBAHLOOJQ-UHFFFAOYSA-N 0.000 description 1
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 1
- QPCDCPDFJACHGM-UHFFFAOYSA-N N,N-bis{2-[bis(carboxymethyl)amino]ethyl}glycine Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(=O)O)CCN(CC(O)=O)CC(O)=O QPCDCPDFJACHGM-UHFFFAOYSA-N 0.000 description 1
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 1
- RUSUZAGBORAKPY-UHFFFAOYSA-N acetic acid;n'-[2-(2-aminoethylamino)ethyl]ethane-1,2-diamine Chemical compound CC(O)=O.CC(O)=O.CC(O)=O.CC(O)=O.CC(O)=O.CC(O)=O.NCCNCCNCCN RUSUZAGBORAKPY-UHFFFAOYSA-N 0.000 description 1
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- 239000004964 aerogel Substances 0.000 description 1
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- 239000003795 chemical substances by application Substances 0.000 description 1
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- -1 diisopropylamino Chemical group 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000005350 fused silica glass Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000012943 hotmelt Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000007885 magnetic separation Methods 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
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- 235000006408 oxalic acid Nutrition 0.000 description 1
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- 229920005591 polysilicon Polymers 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
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- 239000011975 tartaric acid Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
Landscapes
- Silicon Compounds (AREA)
Abstract
The utility model provides a high-value utilization system of a waste quartz crucible, which comprises the following components: a separation device, a silicon nitride washing device, a crucible washing device and a waste liquid purifying device; the separating device is used for separating the waste quartz crucible to obtain a crude silicon nitride product and a crucible body, and is provided with a waste quartz crucible inlet, a crude silicon nitride product outlet and a crucible body outlet; wherein, the outlet of the crude silicon nitride is communicated with the inlet of the silicon nitride washing device, and the outlet of the crucible body is communicated with the inlet of the crucible body of the crucible washing device; the waste liquid outlet of the silicon nitride washing device and the waste liquid outlet of the crucible washing device are respectively communicated with the waste liquid inlet of the waste liquid purifying device; the high-value utilization system can utilize the waste quartz crucible in a high-value mode, the purified crucible body is separated, sodium silicate is obtained through reaction, meanwhile, silicon nitride is recovered as a byproduct, the economic value is improved, waste liquid is purified, and the recovery process is environment-friendly.
Description
Technical Field
The utility model belongs to the technical field of recycling of waste crucibles in polysilicon crystal pulling, and particularly relates to a high-value utilization system of waste quartz crucibles.
Background
The quartz crucible has strong heat resistance, low thermal expansion coefficient and stable physicochemical property, and becomes an indispensable product in the process of pulling polycrystalline silicon into single crystals in the photovoltaic or semiconductor industry. In the single crystal pulling process, the quartz crucible is used for containing molten silicon at 1450-1550 ℃, so that phenomena such as crystallization can occur after long-time use, the quality of the single crystal is affected, and the quartz crucible after crystallization cannot be used continuously and can only be scrapped. Generally, the service life of the quartz crucible is generally 200-500 hours, along with the rapid development of the photovoltaic and semiconductor industries, a large number of waste quartz crucibles are generated, and the quartz crucible contains Ba, B, fe, ni, cr and other impurities, so that in the production process, a high-purity silicon nitride layer is required to be coated on the inner surface of the quartz crucible, and how to recycle a large number of waste quartz crucibles becomes a focus of attention of the industry.
At present, the main way of recycling the waste quartz crucible is to recycle the silicon dioxide component to be fused quartz, sodium silicate and the like, and the sodium silicate is used as an important silicon-based chemical product, has wide downstream application, and can be used for producing new chemical materials with high added value such as aerogel, precipitated white carbon black, molecular sieve and the like. Therefore, the recovery of the waste quartz crucible to produce sodium silicate and the recovery of silicon nitride are main ideas for the high-value utilization of the waste quartz crucible, but in the prior art, the equipment for recovering the quartz crucible is generally high in energy consumption and cost, and the prepared sodium silicate is low in modulus and purity and the silicon nitride is low in purity.
Disclosure of utility model
The utility model provides a high-value utilization system of a waste quartz crucible, which aims to solve the problems that equipment for recycling the quartz crucible in the prior art is high in energy consumption, the purity of recycled silicon nitride is low, and the modulus and purity of the prepared sodium silicate are low.
The utility model provides a high-value utilization system of a waste quartz crucible, which comprises the following components: a separation device, a silicon nitride washing device, a crucible washing device and a waste liquid purifying device; the separating device is used for separating the waste quartz crucible to obtain a crude silicon nitride product and a crucible body, and is provided with a waste quartz crucible inlet, a crude silicon nitride product outlet and a crucible body outlet;
The outlet of the crude silicon nitride product is communicated with the inlet of the silicon nitride washing device, and the outlet of the crucible body is communicated with the inlet of the crucible body of the crucible washing device; the waste liquid outlet of the silicon nitride washing device and the waste liquid outlet of the crucible washing device are respectively communicated with the waste liquid inlet of the waste liquid purifying device.
Further, the reaction device is used for obtaining sodium silicate by taking the quartz crucible body as a raw material for reaction;
the outlet of the crucible washing device is communicated with the inlet of the reaction device.
Further, the silicon nitride washing device comprises a first washing unit and a second washing unit; the inlet of the first washing unit is the inlet of the silicon nitride washing device, the silicon nitride outlet of the first washing unit is communicated with the silicon nitride inlet of the second washing unit, and the waste liquid outlet of the first washing unit is the waste liquid outlet of the silicon nitride washing device.
Further, the purifying liquid outlet of the waste liquid purifying device is respectively communicated with the washing liquid inlet of the silicon nitride washing device and the washing liquid inlet of the crucible washing device.
Further, the device also comprises a pot body pretreatment device; the outlet of the crucible washing device is communicated with the inlet of the reaction device body through the pot pretreatment device.
Further, the pot pretreatment device comprises a crushing unit and a metal separation unit;
The crushing inlet of the crushing unit is communicated with the body outlet of the crucible washing device, the powder outlet of the crushing unit is communicated with the separation inlet of the metal separation unit, and the separation outlet of the metal separation unit is communicated with the body inlet of the reaction device.
Further, the pot pretreatment device also comprises a raw material mixing unit, and the separation outlet is communicated with the inlet of the body of the reaction device through the raw material mixing unit;
The raw material mixing unit comprises a quartz powder inlet, a sodium carbonate inlet and a mixed raw material outlet, the separation outlet is communicated with the quartz powder inlet, and the mixed raw material outlet is communicated with the body inlet of the reaction device.
Further, the device also comprises a sodium carbonate generating device;
The reaction device comprises a sodium silicate outlet and a carbon dioxide outlet, and the carbon dioxide outlet is communicated with a carbon dioxide inlet of the sodium carbonate generating device and is used for providing raw materials for generating sodium carbonate;
And a sodium carbonate outlet of the sodium carbonate generating device is communicated with a sodium carbonate inlet of the raw material mixing unit.
Further, the device also comprises a cooling device, and the carbon dioxide outlet is communicated with the carbon dioxide inlet of the sodium carbonate generating device through the cooling device.
Further, the separating device is a layer stripping machine.
The high-value utilization system of the waste quartz crucible provided by the utility model can realize high-value utilization of the waste quartz crucible, separate the purified crucible body, recover silicon nitride as a byproduct, improve the economic value, purify waste liquid and realize environment-friendly recovery process.
Drawings
FIG. 1 is a schematic diagram of a first high-value utilization system according to the present utility model;
FIG. 2 is a schematic diagram of a second high-value utilization system according to the present utility model;
FIG. 3 is a schematic diagram of a third high-value utilization system according to the present utility model;
FIG. 4 is a schematic diagram of a fourth high-value utilization system according to the present utility model;
FIG. 5 is a schematic diagram of a fifth high-value utilization system according to the present utility model;
FIG. 6 is a schematic diagram of a sixth high-value utilization system according to the present utility model;
FIG. 7 is a schematic diagram of a seventh high-value utilization system according to the present utility model;
fig. 8 is a schematic diagram of an eighth high-value utilization system according to the present utility model.
Reference numerals illustrate:
1: a separation device;
2: a silicon nitride washing device;
3: a crucible washing device;
4: a waste liquid purifying device;
5: a reaction device;
6: a pot pretreatment device;
7: sodium carbonate generating device;
8: a cooling device;
21: a first washing unit;
22: a second washing unit;
61: a pulverizing unit;
62: a metal separation unit;
63: and a raw material mixing unit.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the present utility model more apparent, the technical solutions in the embodiments of the present utility model will be clearly and completely described in the following in conjunction with the embodiments of the present utility model, and it is apparent that the described embodiments are some embodiments of the present utility model, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the utility model without making any inventive effort, are intended to be within the scope of the utility model.
Embodiments of the present utility model are described in detail below, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to like or similar elements or elements having like or similar functions throughout. The embodiments described below by referring to the drawings are exemplary only for explaining the present utility model and are not to be construed as limiting the present utility model.
In the description of the present utility model, it should be understood that the terms "upper," "lower," "front," "rear," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like indicate or are based on the orientation or positional relationship shown in the drawings, merely to facilitate description of the utility model and to simplify the description, and do not indicate or imply that the devices or elements referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus should not be construed as limiting the utility model. In the description of the present utility model, the meaning of "a plurality" is two or more, unless specifically stated otherwise.
The terms "first," "second," "third," "fourth" and the like in the description and in the claims and in the above drawings, if any, are used for distinguishing between similar objects and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used may be interchanged where appropriate such that the embodiments of the application described herein may be implemented, for example, in sequences other than those illustrated or otherwise described herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
In the description of the present utility model, it should be noted that, unless explicitly stated and limited otherwise, the terms "mounted," "connected," and "coupled" are to be construed broadly, and may be fixedly connected, or may be connected via an intermediary, or may be in communication with each other within two elements or in an interaction relationship between two elements, for example. The specific meaning of the above terms in the present utility model can be understood by those of ordinary skill in the art according to the specific circumstances.
Fig. 1 is a schematic diagram of a first high-value utilization system provided by the present utility model, and as shown in fig. 1, the present utility model provides a high-value utilization system for a waste quartz crucible, including: a separation device 1, a silicon nitride washing device 2, a crucible washing device 3 and a waste liquid purifying device 4; the separating device 1 is used for separating the waste quartz crucible to obtain a crude silicon nitride product and a crucible body, and the separating device 1 is provided with a waste quartz crucible inlet, a crude silicon nitride product outlet and a crucible body outlet;
Wherein, the outlet of the crude silicon nitride is communicated with the inlet of the silicon nitride washing device 2, and the outlet of the crucible body is communicated with the inlet of the crucible body of the crucible washing device 3; the waste liquid outlet of the silicon nitride washing device 2 and the waste liquid outlet of the crucible washing device 3 are respectively communicated with the waste liquid inlet of the waste liquid purifying device 4.
In the production process of the quartz crucible, the quartz crucible contains Ba, B, fe, ni, cr and other impurities, the inner surface of the quartz crucible needs to be coated with a high-purity silicon nitride layer, and the silicon nitride layer is used as a release agent, so that a crystal silicon ingot can be easily released from the quartz crucible.
The utility model is not limited by the connection mode among the units, and can ensure that the materials can smoothly circulate. In one embodiment, the units are connected using piping.
The utility model is not limited in the expression form of each unit, wherein the separation unit 1 is used for stripping the waste quartz crucible to separate the crude silicon nitride product and the crucible body, so that the crude silicon nitride product and the crucible body are separated and recycled in the follow-up process, the removal of silicon nitride impurities in the waste quartz crucible is facilitated, and meanwhile, the recycling of silicon nitride improves the economic value. The separation unit 1 is provided with a waste quartz crucible inlet, a silicon nitride crude product outlet and a crucible body outlet, the waste quartz crucible enters the separation unit through the waste quartz crucible inlet, after separation and delamination treatment, the obtained silicon nitride crude product leaves the separation unit 1 through the silicon nitride crude product outlet, and the obtained crucible body leaves the separation unit 1 through the crucible body outlet.
The silicon nitride washing device 2 is used for washing a crude silicon nitride product to remove residual silicon dioxide, metal ions and other impurities to obtain a high-purity silicon nitride product, and preferably the washing treatment comprises acid washing, water washing and drying treatment, wherein the acid is at least one of nitric acid and hydrochloric acid, and the volume ratio of the crude silicon nitride product to the acid is 1: (1.5 to 6), the washing treatment time is 120 to 180 minutes, preferably 150 minutes. The crude silicon nitride enters the silicon nitride washing device 2 through the inlet of the silicon nitride washing device 2, residual silicon dioxide and other impurities are removed in the crude silicon nitride, and the crude silicon nitride leaves the silicon nitride washing device 2 through the outlet of the silicon nitride product to output the silicon nitride product; wherein the waste liquid generated after the washing treatment leaves the silicon nitride washing device 2 through a waste liquid outlet of the silicon nitride washing device 2.
The crucible washing device 3 is used for performing washing impurity removal treatment on the crucible body to remove impurities such as metal ions, preferably, the washing impurity removal treatment comprises acid washing, water washing and drying treatment, wherein acid is at least one of nitric acid and hydrochloric acid, and the volume ratio of the crucible body to the acid is 1: (1.5 to 6), the washing treatment time is 120 to 180 minutes, preferably 150 minutes. The crucible body enters the crucible washing device 3 through a crucible body inlet of the crucible washing device 3, and leaves the crucible washing device 3 through a body outlet of the crucible washing device 3 after the impurities are washed and removed in the crucible body inlet; in a specific embodiment, the crucible cleaning apparatus 3 comprises a cleaning tank.
The waste liquid purifying device 4 is used for purifying the waste liquid in the silicon nitride washing device 2 and the crucible washing device 3 to obtain a purified liquid, and meets the requirement of green production, preferably, metal ion impurities contained in waste quartz crucibles such as Ba, fe, cr and the like are subjected to complex sedimentation through complexing agents to achieve the effect of purifying and separating treatment, wherein the complexing agents are at least one of tartaric acid, citric acid, oxalic acid, triethylenetetramine hexaacetic acid TTHA, diisopropylamino tetraacetic acid DTPA, cyclohexanediamine tetraacetic acid CDTA and ethylenediamine tetraacetic acid EDTA, and the volume ratio of the complexing agents to the acid waste liquid is 1:4-10; waste liquid in the silicon nitride washing device 2 and the crucible washing device 3 respectively leave through waste liquid outlets thereof, and enter the waste liquid purifying device 4 through a waste liquid inlet of the waste liquid purifying device 4 for purifying treatment; in one embodiment, the waste liquid purification device 4 comprises an acid purification tank.
The utility model provides a high-value utilization system of a waste quartz crucible, which can utilize the waste quartz crucible in a high-value manner, separate a purified crucible body, recover silicon nitride as a byproduct, improve the economic value, purify waste liquid and realize the environment-friendly recovery process.
FIG. 2 is a schematic diagram of a second high-value utilization system provided by the utility model, further comprising a reaction device 5, wherein the reaction device 5 is used for sodium silicate obtained by reacting a quartz crucible body as a raw material; the outlet of the crucible washing device 3 is communicated with the inlet of the reaction device 5.
The reaction device 5 is used for adding the purified crucible body into required raw materials to perform melting reaction, and can realize the functions of forming, cooling, packaging and the like of the hot-melt sodium silicate, so that a massive solid, namely a sodium silicate product, is obtained. The crucible body enters the reaction device 5 through a body inlet of the reaction device 5, and sodium silicate products obtained by reaction leave the reaction device 5 through a sodium silicate outlet and are output; in one embodiment, the reaction device 5 includes a melt synthesis furnace and a molding press.
The high-value utilization system provided by the utility model can realize high-value utilization of the waste quartz crucible, prepare sodium silicate products through compression cooling after melt reaction, and simultaneously recover silicon nitride as a byproduct, thereby improving the economic value, and discharging the waste liquid after purification, and the process is environment-friendly. Fig. 3 is a schematic diagram of a third high-value utilization system provided by the present utility model, where as shown in the drawing, the silicon nitride washing device 2 includes a first washing unit 21 and a second washing unit 22; the inlet of the first washing unit 21 is the inlet of the silicon nitride washing device 2, the silicon nitride outlet of the first washing unit 21 is communicated with the silicon nitride inlet of the second washing unit 22, and the waste liquid outlet of the first washing unit 21 is the waste liquid outlet of the silicon nitride washing device.
It can be understood that after the washing treatment of the first washing unit 21, the crude silicon nitride may have residual silicon dioxide and metal ion impurities not removed, and then the second washing unit 22 is used to remove the residual impurities, thereby obtaining high-purity silicon nitride. Preferably, in the first washing unit 21, acid washing and water washing treatment are performed, wherein the acid is at least one of nitric acid and hydrochloric acid, and the volume ratio of the crude silicon nitride to the acid is 1: (1.5-6), the washing treatment time is 120-180 minutes, preferably 150 minutes; in the second washing unit 22, a secondary acid washing, a secondary water washing and a drying treatment are performed, wherein the acid used for the secondary acid washing is a mixture of H 2O、H2O2、H2SO4 and HF, and the mass composition of the acid is H 2O：H2O2：H2SO4: HF=100:0.1-10:1-50:0.2-0.6, the treatment temperature is 20-70 ℃, and the volume ratio of the crude silicon nitride to the acid is 1: (2-5), controlling the time to be 20-60 minutes; the volume ratio of water used for the water washing treatment is 1: (5-50), washing until the pH of the washing liquid is neutral, and drying for 0.5-3 hours. The crude silicon nitride enters the first washing unit 21 through an inlet of the first washing unit 21, after the impurities are primarily removed through washing treatment, the crude silicon nitride leaves the first washing unit 21 through a silicon nitride outlet of the first washing unit 21, enters the second washing unit 22 through a silicon nitride inlet of the second washing unit 22, is subjected to secondary washing treatment, and leaves the second washing unit 22 through a silicon nitride product outlet of the second washing unit 22 after the residual impurities are removed; in a specific embodiment, the first washing unit 21 includes a first washing tank, and the second washing unit 22 includes a second washing tank.
The high-value utilization system provided by the utility model can realize high-value utilization of the waste quartz crucible, obtain a high-purity silicon nitride product, prepare a sodium silicate product, purify waste liquid and discharge the waste liquid, and is energy-saving and environment-friendly.
Further, the cleaning liquid outlet of the waste liquid cleaning device 4 is respectively communicated with the cleaning liquid inlet of the silicon nitride cleaning device 2 and the cleaning liquid inlet of the crucible cleaning device 3.
It can be understood that the cost can be reduced by recycling the purified liquid treated by the waste liquid purifying device 4, and the full utilization of resources can be realized; the purified purification liquid leaves the waste liquid purification device 4 through a purification liquid outlet of the waste liquid purification device 4, and enters the silicon nitride washing device 2 and the crucible washing device 3 through a washing liquid inlet of the silicon nitride washing device 2 and a washing liquid inlet of the crucible washing device 3 respectively.
The high-value utilization system provided by the utility model can realize high-value utilization of the waste quartz crucible, prepare sodium silicate products with few impurities, simultaneously recycle silicon nitride as a byproduct, and recycle acid liquor, thereby improving economic value and meeting the requirements of green production. FIG. 4 is a schematic diagram of a fourth high-value utilization system according to the present utility model, and as shown in the figure, the high-value utilization system further includes a boiler pretreatment device 6; the outlet of the crucible washing device 3 is communicated with the inlet of the reaction device 5 through a pot pretreatment device 6.
The pot body pretreatment device 6 is used for pretreating the purified crucible body, so that the crucible body is changed into a raw material which is more beneficial to preparing sodium silicate, the reaction in the reaction device 5 is more beneficial to being carried out, and the purity of the product is improved. The purified crucible body enters the pot body pretreatment device 6 through the inlet of the pot body pretreatment device 6, leaves the pot body pretreatment device 6 through the outlet of the pot body pretreatment device 6 after being pretreated, and enters the reaction device 5 through the body inlet of the reaction device 5.
The high-value utilization system provided by the utility model can prepare sodium silicate products with high purity and few impurities by utilizing the pot body pretreatment device, and can recycle silicon nitride as a byproduct.
Fig. 5 is a schematic diagram of a fifth high-value utilization system provided by the present utility model, and further, the pot pretreatment device 6 includes a crushing unit 61 and a metal separation unit 62; the pulverizing inlet of the pulverizing unit 61 is communicated with the body outlet of the crucible washing apparatus 3, the powder outlet of the pulverizing unit 61 is communicated with the separation inlet of the metal separation unit 62, and the separation outlet of the metal separation unit 62 is communicated with the body inlet of the reaction apparatus 5.
Wherein, the crushing unit 61 is used for crushing the purified crucible body, so that the crucible body is more beneficial to the reaction production of sodium silicate products, when the high-value utilization system provided by the utility model is used for recycling the waste quartz crucible, the purified crucible body is crushed to 50-70 meshes, the particles are larger, the product modulus can be improved, the equipment is prevented from being blocked by superfine powder, the process consumption is reduced, and the cost is reduced; in a specific embodiment, the pulverizing unit 61 includes at least one of a crusher and a superfine crusher.
The metal separation unit 62 is used for removing metal impurities introduced in the crushing process, and further improving the purity of the product; in one embodiment, the metal separation unit 62 comprises a magnetic separator, and the magnetic separation treatment time is 10-20 min, and the magnetic field strength is 1.2-1.6T, so that Fe impurities in the quartz powder can be effectively removed.
Specifically, the crucible body after passing through enters the pulverizing unit 61 through the pulverizing inlet of the pulverizing unit 61, after the pulverizing treatment is performed therein, the obtained quartz powder leaves the pulverizing unit 61 through the powder outlet, then enters the metal separating unit 62 through the separating inlet, after removing the metal impurities therein, leaves the metal separating unit 62 through the separating outlet, and then enters the reaction apparatus 5 through the body inlet of the reaction apparatus 5.
According to the high-value utilization system provided by the utility model, the purified crucible is crushed by the crushing unit, and then the metal impurities introduced in the crushing process are removed by the metal separation unit, so that the impurities of sodium silicate products are further reduced, and meanwhile, the silicon nitride is recovered as a byproduct, so that the cost is reduced.
FIG. 6 is a schematic diagram of a sixth high-value utilization system provided by the present utility model, where the boiler pretreatment device 6 further includes a raw material mixing unit 63, and the separation outlet is communicated with the inlet of the reaction device 5 through the raw material mixing unit 63; wherein the raw material mixing unit 63 includes a quartz powder inlet, a sodium carbonate inlet, and a mixed raw material outlet, the separation outlet is communicated with the quartz powder inlet, and the mixed raw material outlet is communicated with the body inlet of the reaction device 5.
The raw material mixing unit 63 is used for mixing sodium carbonate and quartz powder, and can further regulate and control the modulus and quality of the prepared sodium silicate product; in one embodiment, the raw material mixing unit 63 includes a solid mixer, the molar ratio of the quartz powder to the sodium carbonate is 2.8-3.5:1, the reaction temperature is 1400-1500 ℃, and the reaction time is 30-120 min. Specifically, the quartz powder subjected to impurity removal enters the raw material mixing unit 63 through the quartz powder inlet, the solid sodium carbonate enters the raw material mixing unit 63 through the sodium carbonate inlet, the solid sodium carbonate and the raw material are mixed, the mixed raw material leaves the raw material mixing unit 63 through the mixed raw material outlet, and then enters the reaction device 5 through the body inlet of the reaction device 5.
According to the high-value utilization system provided by the utility model, the specific amount of sodium carbonate is added into the raw material mixing unit to be mixed with the quartz powder obtained by the preamble device, so that the modulus of sodium silicate can be further improved, and the quality of sodium silicate products can be improved.
Fig. 7 is a schematic diagram of a seventh high-value utilization system provided by the present utility model, and preferably further includes a sodium carbonate generating device 7; the reaction device 5 comprises a sodium silicate outlet and a carbon dioxide outlet, and the carbon dioxide outlet is communicated with a carbon dioxide inlet of the sodium carbonate generating device 7 and is used for providing raw materials for generating sodium carbonate; the sodium carbonate outlet of the sodium carbonate generating means 7 communicates with the sodium carbonate inlet of the raw material mixing unit 63.
The sodium carbonate generating device 7 is used for generating sodium carbonate solid by utilizing the carbon dioxide produced by the reaction of the reaction device 5, so that the high-efficiency utilization of raw materials is realized, and the cost is reduced; in a specific embodiment, the sodium carbonate generating device 7 comprises an absorption tower and a crystallization drying tank, preferably, the lower section of the absorption tower is provided with a carbon dioxide inlet, the upper section of the absorption tower is provided with a sodium hydroxide solution inlet, the carbon dioxide gas and the sodium hydroxide solution are in countercurrent full contact under the action of gravity to generate sodium carbonate solution, the bottom of the absorption tower is provided with a sodium carbonate solution outlet, and the sodium carbonate solution is evaporated, crystallized and dried by the crystallization drying tank to obtain sodium carbonate solid; wherein the concentration of the sodium hydroxide solution is 10-45%, the reaction temperature is 5-50 ℃, and the evaporation, crystallization and drying treatment can be realized by at least one of mechanical stirring and air flow stirring.
Specifically, sodium silicate products and carbon dioxide gas are obtained by reaction in the reaction device 5, wherein the sodium silicate products leave the reaction device 5 through a sodium silicate outlet, the carbon dioxide gas leaves the reaction device 5 through a carbon dioxide outlet, then enters the sodium carbonate generating device 7 through a carbon dioxide inlet to generate sodium carbonate solids therein, then leaves the sodium carbonate generating device 7 through a sodium carbonate outlet, and enters the raw material mixing unit 63 through a sodium carbonate inlet of the raw material mixing unit 63 to provide raw materials for mixing, so that raw material recycling is realized.
According to the high-value utilization system provided by the utility model, the sodium carbonate generating device is utilized, carbon dioxide generated by the reaction device can be recycled and used, sodium hydroxide is used for generating sodium carbonate solution, and then the ammonium carbonate solid is obtained after evaporation, crystallization and drying, so that raw materials are provided for generating sodium silicate, the cost is further reduced, and the economic value is improved.
Fig. 8 is a schematic diagram of an eighth high-value utilization system provided by the present utility model, preferably, the high-value utilization system further includes a cooling device 8, and the carbon dioxide outlet is communicated with the carbon dioxide inlet of the sodium carbonate generating device 7 through the cooling device 8.
The cooling device 8 is used for cooling the carbon dioxide gas generated in the reaction device 5 and improving the rate of producing sodium carbonate; in a specific embodiment, the cooling device 8 comprises a cooler. Specifically, the hot carbon dioxide gas enters the cooling device 8 through the inlet of the cooling device 8, after being cooled therein, leaves the cooling device 8 through the outlet of the cooling device 8, and then enters the sodium carbonate generating device 7 through the carbon dioxide inlet of the sodium carbonate generating device 7.
Further, the sodium carbonate generating device 7 is further provided with a carbon dioxide outlet, and it can be understood that part of carbon dioxide in the sodium carbonate generating device 7 is not absorbed, so that the carbon dioxide leaves the sodium carbonate generating device 7 as residual carbon dioxide, the residual carbon dioxide is led into the inlet of the cooling device 8 again for cooling treatment, and the residual carbon dioxide reenters the sodium carbonate generating device 7 to participate in producing sodium carbonate solid, so that further utilization of carbon dioxide is realized.
The high-value utilization system provided by the utility model can further improve the efficiency of the ammonium carbonate generating device and further reduce the cost by utilizing the cooling device.
In one embodiment, the separating apparatus 1 is a delamination machine. The silicon nitride layer of the waste quartz crucible can be stripped and separated efficiently, so that the subsequent separation and recycling are facilitated, and the high-purity silicon nitride and sodium silicate products are produced.
In another embodiment, the first washing unit 21 is a washing tank, the second washing unit 22 is a washing and drying tank, the crucible washing device 3 is a washing and drying tank, the waste liquid purifying device 4 is an acid purifying tank, the reaction device 5 is a melting synthesis furnace and a profiling machine, the pulverizing unit 61 is at least one of a roll mill and a ball mill, the metal separating unit 62 is a magnetic separator, the raw material mixing unit 63 is at least one of a stirred tank and a double-screw mixer, the sodium carbonate generating device 7 is a packed tower and a crystallization and drying tank, and the cooling device 8 is a cooler.
Specifically, the waste quartz crucible enters a layer stripping machine, and a silicon nitride layer is separated to obtain a crude silicon nitride product and a crucible body; and (3) after the crude silicon nitride is washed in a washing tank and washed with water, the crude silicon nitride enters a second washing and drying tank, and residual silicon dioxide is removed after secondary washing, washing and drying, so that the high-purity silicon nitride is obtained. And (3) carrying out acid washing, water washing and drying on the crucible body in a washing and drying tank to obtain the purified crucible body. The acid waste liquid in the washing tank enters an acid purifying tank, metal ion impurities such as Ba, fe, cr and the like are subjected to complexing sedimentation separation by using a complexing agent, and the purified acid is recycled;
Crushing the purified crucible body by a crusher to obtain quartz powder with the mesh number of 50-70 meshes. The quartz powder enters a magnetic separator to remove Fe impurities introduced in the crushing process, the quartz powder after the impurities are removed enters a solid mixer after being metered, sodium carbonate powder from a crystallization drying tank enters the solid mixer after being metered, and the sodium carbonate and the quartz powder are uniformly mixed to obtain a reaction mixed raw material;
The reaction mixed raw materials enter a melting synthesis furnace, high-temperature reaction is carried out to generate a high-temperature melting solid high-modulus sodium silicate product, the high-temperature melting solid high-modulus sodium silicate product flows out of a furnace mouth to a molding press, and a massive solid is obtained after cooling, namely the high-modulus sodium silicate product; carbon dioxide generated in the reaction process enters a cooler, enters the lower section of a packing tower after being cooled, and is introduced with sodium hydroxide solution for absorption in the upper section, so that sodium carbonate aqueous solution is obtained in the tower kettle; the unabsorbed carbon dioxide enters a packing tower after being cooled by a cooler again; the sodium carbonate aqueous solution is treated for 0.5 to 3 hours at the temperature of between 90 and 150 ℃ in a crystallization drying tank, evaporated and crystallized to obtain sodium carbonate solid which is taken as a raw material to continuously enter a reaction system.
Preferably, the temperature of the separation device 1 is controlled to be 0-60 ℃ and the pressure is controlled to be 150-300Kpa;
The temperature of the silicon nitride washing device 2 is 15-30 ℃ and the pressure is 150-300Kpa;
the temperature of the crucible washing device 3 is 15-30 ℃ and the pressure is 150-300Kpa;
The temperature of the waste liquid purifying device 4 is 15-30 ℃ and the pressure is 150-300Kpa;
The temperature of the reaction device 5 is 1400-1500 ℃ and the pressure is 102-150Kpa;
the temperature of the boiler body pretreatment device 6 is 15-30 ℃ and the pressure is 150-300Kpa;
the temperature of the sodium carbonate generating device 7 is 5-50 ℃ and the pressure is 102-150Kpa;
the temperature of the cooling device 8 is 5-50 ℃ and the pressure is 102-1102Kpa;
the temperature of the first washing unit 21 is 15-30 deg.c and the pressure is 150-300Kpa;
the temperature of the second washing unit 22 is 15-30 deg.c and the pressure is 150-300Kpa;
The temperature of the pulverizing unit 61 is 0-60deg.C, and the pressure is 150-300Kpa;
the temperature of the metal separation unit 62 is 15-30 ℃ and the pressure is 150-300Kpa;
The temperature of the raw material mixing unit 63 is 0-60 deg.c and the pressure is 150-300Kpa.
The high-value utilization system provided by the utility model realizes recovery treatment of the waste quartz crucible, generates high-purity silicon nitride and high-purity manuscript modulus sodium silicate products, can recycle carbon dioxide generated by the system, further reduces the cost, improves the economic value, and is environment-friendly in the production process.
The utility model provides a high-value utilization system of a waste quartz crucible, which can utilize the waste quartz crucible in a high-value manner, prepare a sodium silicate product with high purity, few impurities and high modulus, simultaneously recycle silicon nitride as a byproduct, recycle acid liquor, improve economic value and realize environment-friendly process.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present utility model, and not for limiting the same; although the utility model has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the utility model.
Claims (10)
1. A high value utilization system of a waste quartz crucible, comprising: a separation device, a silicon nitride washing device, a crucible washing device and a waste liquid purifying device; the separating device is used for separating the waste quartz crucible to obtain a crude silicon nitride product and a crucible body, and is provided with a waste quartz crucible inlet, a crude silicon nitride product outlet and a crucible body outlet;
The outlet of the crude silicon nitride product is communicated with the inlet of the silicon nitride washing device, and the outlet of the crucible body is communicated with the inlet of the crucible body of the crucible washing device; the waste liquid outlet of the silicon nitride washing device and the waste liquid outlet of the crucible washing device are respectively communicated with the waste liquid inlet of the waste liquid purifying device.
2. The high value utilization system according to claim 1, further comprising a reaction device for sodium silicate obtained by reacting a quartz crucible body as a raw material;
the outlet of the crucible washing device is communicated with the inlet of the reaction device.
3. The high value utilization system of claim 1, wherein the silicon nitride washing device comprises a first washing unit and a second washing unit; the inlet of the first washing unit is the inlet of the silicon nitride washing device, the silicon nitride outlet of the first washing unit is communicated with the silicon nitride inlet of the second washing unit, and the waste liquid outlet of the first washing unit is the waste liquid outlet of the silicon nitride washing device.
4. The high value utilization system according to any one of claims 1 to 3, wherein the purification liquid outlet of the waste liquid purification device is respectively communicated with the washing liquid inlet of the silicon nitride washing device and the washing liquid inlet of the crucible washing device.
5. The high value utilization system according to claim 2, further comprising a pot pretreatment device; the outlet of the crucible washing device is communicated with the inlet of the reaction device body through the pot pretreatment device.
6. The high value utility system of claim 5, wherein the pot pretreatment device comprises a crushing unit and a metal separation unit;
The crushing inlet of the crushing unit is communicated with the body outlet of the crucible washing device, the powder outlet of the crushing unit is communicated with the separation inlet of the metal separation unit, and the separation outlet of the metal separation unit is communicated with the body inlet of the reaction device.
7. The high value utilization system according to claim 6, wherein the pot pretreatment device further comprises a raw material mixing unit, and the separation outlet is communicated with the inlet of the body of the reaction device through the raw material mixing unit;
The raw material mixing unit comprises a quartz powder inlet, a sodium carbonate inlet and a mixed raw material outlet, the separation outlet is communicated with the quartz powder inlet, and the mixed raw material outlet is communicated with the body inlet of the reaction device.
8. The high value utility system of claim 7, further comprising a sodium carbonate generating device;
The reaction device comprises a sodium silicate outlet and a carbon dioxide outlet, and the carbon dioxide outlet is communicated with a carbon dioxide inlet of the sodium carbonate generating device and is used for providing raw materials for generating sodium carbonate;
And a sodium carbonate outlet of the sodium carbonate generating device is communicated with a sodium carbonate inlet of the raw material mixing unit.
9. The high value utilization system of claim 8, further comprising a cooling device through which the carbon dioxide outlet communicates with a carbon dioxide inlet of the sodium carbonate generating device.
10. The high value utility system of claim 4, wherein the separation device is a stripping machine.
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