CN115196642B - Purification method of silicon dioxide - Google Patents
Purification method of silicon dioxide Download PDFInfo
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- CN115196642B CN115196642B CN202210782044.9A CN202210782044A CN115196642B CN 115196642 B CN115196642 B CN 115196642B CN 202210782044 A CN202210782044 A CN 202210782044A CN 115196642 B CN115196642 B CN 115196642B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
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- C—CHEMISTRY; METALLURGY
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- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses a purification method of silicon dioxide, which comprises the following steps: s1: mixing quartz particles with carbon nanotubes, sintering and oxidizing under inert atmosphere to obtain a primary sintering product, and screening the primary sintering product to obtain a plurality of first purified products with different purity levels; s2: carrying out acid washing treatment on the first purified product which does not meet the purity grade requirement to obtain a plurality of second purified products with different purity grades; s3: mixing the second purified product which does not meet the purity grade requirement with a carbon nano tube, sintering and oxidizing under inert atmosphere to obtain a re-sintered product, and screening the re-sintered product to obtain a plurality of third purified products with different purity grades; s4: and sequentially and circularly carrying out the operations corresponding to the S2 and the S3 on the third purified product which does not meet the purity grade requirement until the obtained purified product meets the purity grade requirement of silicon dioxide.
Description
Technical Field
The invention relates to the technical field of material purification, in particular to a purification method of silicon dioxide.
Background
RNA/DNA sequencing is an important tool for pathological research, and the particulate materials commonly used in the existing RNA/DNA sequencing process are: crosslinked polystyrene, organic hydrogels, resins and silica (glass, silica gel), wherein silica is a relatively low cost, high throughput and high reliability material and the purity of silica also has a significant impact on sequencing results, there is a strong need to provide a lower cost and higher purity purification method for silica.
On the other hand, with the development of quantum physics, quantum computers are gradually put into folk use, and their wide application will be a major revolution in human history. Because the quantum computer depends on a plurality of photon transmission data, any photon loss can cause data distortion, the primary photon loss is an impurity on a physical level, in order to ensure higher data transmission efficiency, a silicon dioxide material for transmitting data is required to have extremely high purity, and in order to ensure that the manufacturing cost of the quantum computer is in a range which can be born folk, the highest purification purity is required to reach 99.999999 percent so as to realize a microwave photon entangled state storage mechanism and the like as core components required by the quantum medical CT. In addition, when the material for transmitting data of the quantum computer is provided, the principle of no waste is maintained, and if the low-purity silicon dioxide can be simultaneously screened out during screening of the high-purity silicon dioxide, the low-purity silicon dioxide can be used as a mask plate in the semiconductor industry, used as a heat insulation bearing material such as an electronic packaging material and a submarine buoyancy material in the microelectronics industry and the transportation industry, used as a high-resistance coating in the building industry, used as an antibacterial material and the like.
The current high purity silica purification technology is limited by the quartz material and graphene costs of raw materials, the high-grade sinters costs, the high electric quantity costs and the high grinding (diamond) costs, resulting in very high costs for manufacturing quantum computers, and simultaneously, a great deal of waste is easily caused to waste materials in the purification process, resulting in further improvement of the purification costs.
Disclosure of Invention
The main purpose of the invention is to provide a purification method of silicon dioxide, which aims at reducing the purification cost of the silicon dioxide and solving the problem of difficult purification of the high-purity silicon dioxide.
In order to achieve the above object, the purification method of silica provided by the present invention comprises the following steps:
s1: mixing quartz particles with carbon nanotubes and sintering in a sintering device under inert atmosphere to melt and evaporate metal impurities in the quartz particles, oxidizing the metal impurities in the sintering device by oxidizing gas, discharging the oxidized metal impurities from the sintering device to obtain primary sintering products of the quartz particles, and screening the primary sintering products to obtain first purified products with various different purity levels;
s2: if the first purified product comprises a first purified product which does not meet the purity grade requirement, carrying out acid washing treatment on the first purified product which does not meet the purity grade requirement to obtain a plurality of second purified products with different purity grades;
S3: if the second purified product comprises a second purified product which does not meet the purity grade requirement, mixing the second purified product which does not meet the purity grade requirement with carbon nano tubes, sintering in a sintering device under inert atmosphere to enable metal impurities in the second purified product which does not meet the purity grade requirement to be melted and evaporated, oxidizing the metal impurities in the sintering device by oxidizing gas, discharging the oxidized metal impurities from the sintering device to obtain a re-sintered product of quartz particles, and screening the re-sintered product to obtain a plurality of third purified products with different purity grades;
s4: and if the third purified product comprises a third purified product which does not meet the purity grade requirement, sequentially and circularly carrying out the operations corresponding to the S2 and the S3 on the third purified product which does not meet the purity grade requirement until the obtained purified product meets the purity grade requirement of the silicon dioxide.
In an embodiment, the sintering process in the operation corresponding to S1 and S3 includes a heating stage and a heat preservation stage located after the heating stage, the sintering temperature of the heat preservation stage is 700-2200 ℃, and the sintering temperature of the heat preservation stage in the operation corresponding to S3 is greater than the sintering temperature of the heat preservation stage in S1;
In the step S4, as the number of cycles of the operation corresponding to the step S3 increases, the sintering temperature of the heat preservation stage in the operation corresponding to the step S3 gradually increases.
In one embodiment, the sintering temperature in the heating stage is uniformly increased within 2-12 h, and inert gas is introduced into the sintering device in the heating stage; and/or the heat preservation period of the heat preservation stage is 0.5-2 h, and oxidizing gas is introduced into the sintering device in the heat preservation stage.
In one embodiment, the particle size of the quartz particles is not less than 800 mesh; and/or the carbon nanotubes have a diameter of not more than 20nm and a length of not more than 1um.
In one embodiment, in S1, the weight ratio of the quartz particles to the carbon nanotubes is d 1 The d is 1 Not less than 10; in the operation corresponding to S3, the weight ratio of the second purified product to the carbon nano tube is d 2 ；
In the step S4, as the number of cycles of the operation corresponding to the step S3 increases, the weight ratio of the third purified product to the carbon nanotubes gradually increases, and the weight ratio of the third purified product to the carbon nanotubes is d 3 The d is 3 Not more than 100, said d 1 D, said d 2 D, said d 3 Gradually increasing.
In one embodiment, the specific steps of the oxidation process in the operation corresponding to S1 and/or S3 include: and in the initial stage of the heat preservation stage, starting to introduce oxidizing gas into the sintering device, and gradually increasing the mole fraction of the oxidizing gas in the sintering device along with the extension of the heat preservation time, wherein the mole fraction of the oxidizing gas in the sintering device is 1% -99%.
In one embodiment, the oxidizing gas comprises oxygen and chlorine, wherein the molar ratio of oxygen to chlorine is (2.5-3.5): 1.
in an embodiment, during the pickling process corresponding to the operation S3, one or more acids selected from hydrochloric acid, sulfuric acid, nitric acid, oxalic acid, formic acid, and citric acid are selected for washing.
In one embodiment, the pickling process includes a plurality of washing and purifying processes, wherein the washing and purifying processes are respectively performed by selecting inorganic acid and organic acid according to the operation sequence of the washing and purifying processes; and/or the cycle number of the operation corresponding to the S3 is 10-55, and the combination of the acids selected in the pickling process of the operation corresponding to the S3 in the previous nine cycles is not repeated.
In one embodiment, in the step S1, the sieving treatment is performed using a gradient sieving device, and/or in the operation corresponding to the step S3, the sieving treatment is performed using a gradient sieving device;
the gradient screening device comprises a centrifugal bowl and a classification groove, wherein the centrifugal bowl is arranged in the classification groove and is rotatable relative to the classification groove, a centrifugal cavity for accommodating a primary sintering product or a secondary sintering product is formed in the centrifugal bowl, a plurality of screening holes which are arranged up and down are formed in the side wall of the centrifugal bowl, the size of the screening holes is sequentially reduced from top to bottom, and a plurality of gradient strips which are sequentially arranged from inside to outside by taking the centrifugal bowl as a center are formed at the bottom of the classification groove.
According to the technical scheme, the purification cost is reduced by mixing the carbon nano tube with quartz particles and sintering and oxidizing the mixture; in addition, the purification cost is further reduced while ensuring the high purity purification effect by using the multi-purity gradient purification method instead of the general co-purity gradient purification method. In the technical scheme of the invention, the cheap carbon nano tube is adopted to replace expensive graphene used in the conventional extraction method, so that the raw material cost is reduced, and the hollow tubular structure of the carbon nano tube can improve the sintering treatment effect and the oxidation treatment effect in the purification step, thereby accelerating the purification progress and reducing the waste of raw materials; the purification products in different steps are subjected to screening treatment according to different purity grades, and the screened purification products which do not meet the purity grade requirement are further purified and recycled, so that on one hand, the problem that raw materials, electric quantity and equipment consumption are increased due to repeated purification of the purification products with qualified purity grade is avoided, and on the other hand, under the whole purification system of the technical scheme of the invention, the purification products with unqualified purity grade can be repeatedly purified, so that the raw material purity grade requirement of the quartz particles is not particularly high (unlike the conventional purification method, natural quartz is required to be selected, and in the invention, the quartz particles can be artificial quartz with relatively low price), and the overall purity of the finally purified silicon dioxide can reach higher purity grade. The purification method of the silicon dioxide has the advantages of simple process, strong feasibility, low purification cost and high purification efficiency, and the purity of the silicon dioxide purified by the purification method can reach 99.999999 percent, so that the method can be widely applied to the fields of RNA/DNA sequencing, quantum computers and other industries.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to the structures shown in these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic illustration of a process flow in one embodiment of a method for purifying silica according to the present invention;
FIG. 2 is a schematic diagram showing the structure of a gradient sifter in an embodiment of the method for purifying silica according to the present invention;
FIG. 3 is a schematic structural diagram of a triaxial weight loss wheel in an embodiment of the silica purification method according to the present invention.
Reference numerals illustrate:
| reference numerals | Name of the name | Reference numerals | Name of the name |
| 100 | Gradient screening device | 110 | Centrifugal bowl |
| 111 | Centrifugal cavity | 113 | Screen mesh |
| 130 | Sorting tank | 131 | Gradient band |
| 200 | Triaxial weightlessness wheel | 210 | Fixing seat |
| 220 | First fixing rod | 230 | Second fixing rod |
| 240 | Third fixingRod | 250 | Washing pot |
The achievement of the objects, functional features and advantages of the present invention will be further described with reference to the accompanying drawings, in conjunction with the embodiments.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
It should be noted that, if directional indications (such as up, down, left, right, front, and rear … …) are included in the embodiments of the present invention, the directional indications are merely used to explain the relative positional relationship, movement conditions, etc. between the components in a specific posture (as shown in the drawings), and if the specific posture is changed, the directional indications are correspondingly changed. In addition, if there is a description of "first", "second", etc. in the embodiments of the present invention, the description of "first", "second", etc. is for descriptive purposes only and is not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include at least one such feature. In addition, if the meaning of "and/or" is presented throughout this document, it is intended to include three schemes in parallel, taking "a and/or B" as an example, including a scheme, or B scheme, or a scheme where a and B meet simultaneously. In addition, the technical solutions of the embodiments may be combined with each other, but it is necessary to base that the technical solutions can be realized by those skilled in the art, and when the technical solutions are contradictory or cannot be realized, the combination of the technical solutions should be considered to be absent and not within the scope of protection claimed in the present invention.
The terms "comprising," "including," "containing," "having," or other variations thereof herein are intended to cover a non-closed inclusion, without distinguishing between them. The term "comprising" means that other steps and ingredients may be added that do not affect the end result. The term "comprising" also includes the terms "consisting essentially of …" and "consisting essentially of …". The compositions and methods/processes of the present application comprise, consist of, and consist essentially of the essential elements and limitations described herein, as well as additional or optional ingredients, components, steps, or limitations of any of the embodiments described herein.
All numbers or expressions referring to amounts of components, process conditions, etc. used in the specification and claims are to be understood as modified in all instances by "about". All ranges directed to the same component or property are inclusive of the endpoints, which endpoints are independently combinable. Because these ranges are continuous, they include every value between the minimum and maximum values. It should also be understood that any numerical range recited herein is intended to include all sub-ranges within that range. As used herein, "weight ratio" and "mass ratio" are used interchangeably.
The invention provides a purification method of silicon dioxide.
In the embodiment of the invention, the purification method of the silicon dioxide comprises the following steps:
s1: mixing quartz particles with carbon nanotubes, sintering and oxidizing under inert atmosphere to obtain a primary sintering product, and screening the primary sintering product to obtain a plurality of first purified products with different purity levels;
in the step S1, the quartz particles may be artificial quartz or natural quartz, and a large amount of metal impurities exist in the quartz particles as raw materials before sintering and oxidation treatment, and the metal impurities in the quartz particles can be melted and evaporated by high-temperature sintering, and then the evaporated metal gas is oxidized into metal oxide, and then the metal oxide is discharged from the sintering device, thereby achieving the purpose of purifying the quartz particles. The purpose of sintering and oxidizing the corresponding operations in the subsequent steps is similar to that of sintering and oxidizing in S1, and will not be described in detail.
S2: if the plurality of first purified products comprise first purified products which do not meet the purity grade requirement, carrying out acid washing treatment on the first purified products which do not meet the purity grade requirement to obtain a plurality of second purified products with different purity grades;
In the sintering and oxidizing process of S1, the metal impurities on the outer layer of the quartz particles are mainly removed, and in order to remove the metal impurities on the inner layer of the quartz particles together, in S2, the first purified product which does not meet the purity grade requirement is subjected to acid washing treatment, so that the purpose of purifying the first purified product which does not meet the purity grade requirement is achieved. The purpose of the pickling treatment of the corresponding operation in the subsequent step is similar to that of the pickling treatment in S2, and will not be described in detail.
S3: if the second purified products do not meet the purity grade requirement, mixing the second purified products which do not meet the purity grade requirement with the carbon nano tube, sintering and oxidizing under inert atmosphere to obtain a re-sintered product, and screening the re-sintered product to obtain a plurality of third purified products with different purity grades;
s4: and if the plurality of third purified products comprise third purified products which do not meet the purity grade requirement, sequentially and circularly carrying out the operations corresponding to the S2 and the S3 on the third purified products which do not meet the purity grade requirement until the obtained purified products meet the purity grade requirement of the silicon dioxide.
It should be noted that, if the purity levels of the purified products of the plurality of different purity levels obtained in the step S1 meet the purity requirement of the required silica, the operations in the step S2, the step S3 and the step S4 are not required; if the purity levels of the purified products of the plurality of different purity levels obtained in the step S2 meet the purity requirements of the required silicon dioxide, the operations in the step S3 and the step S4 are not required; if the purity levels of the purified products of the plurality of different purity levels obtained in the step S3 meet the purity requirement of the required silica, the operation in the step S4 is not required; in addition, in the step S4, after the operation corresponding to the first recycling step S2 of the third purified product not meeting the purity level requirement, when the purity levels of the obtained purified products with different purity levels meet the purity requirement of the required silica, the operation corresponding to the subsequent recycling step S3 is not required. According to the actual purity requirement of the silicon dioxide and the change of the purification efficiency, the required steps of the silicon dioxide purification method can be S1, S1-S2-S3-S2 or S1-S2-S3, or the steps of S1, S2, S3, S2, and S2 can be sequentially repeated until the obtained purified product meets the purity level requirement of the silicon dioxide, and the steps are not repeated herein.
According to the technical scheme, the purification cost is reduced by mixing the carbon nano tube with quartz particles and sintering and oxidizing the mixture; in addition, the purification cost is further reduced while ensuring the high purity purification effect by using the multi-purity gradient purification method instead of the general co-purity gradient purification method. In the technical scheme of the invention, the cheap carbon nano tube is adopted to replace expensive graphene used in the conventional extraction method, so that the raw material cost is reduced, and the hollow tubular structure of the carbon nano tube can improve the sintering treatment effect and the oxidation treatment effect in the purification step, thereby accelerating the purification progress and reducing the waste of raw materials; the purification products in different steps are subjected to screening treatment according to different purity grades, and the screened purification products which do not meet the purity grade requirement are further purified and recycled, so that on one hand, the problem that raw materials, electric quantity and equipment consumption are increased due to repeated purification of the purification products with qualified purity grade is avoided, and on the other hand, under the whole purification system of the technical scheme of the invention, the purification products with unqualified purity grade can be repeatedly purified, so that the raw material purity grade requirement of the quartz particles is not particularly high (unlike the conventional purification method, natural quartz is required to be selected, and in the invention, the quartz particles can be artificial quartz with relatively low price), and the overall purity of the finally purified silicon dioxide can reach higher purity grade. The purification method of the silicon dioxide has the advantages of simple process, strong feasibility, low purification cost and high purification efficiency, and the purity of the silicon dioxide purified by the purification method can reach 99.999999 percent, so that the method can be widely applied to the fields of RNA/DNA sequencing, quantum computers and other industries.
According to the purification method of silica of the present invention, in order to further improve purification efficiency, the quartz particles may be ground before being mixed with the carbon nanotubes, so as to increase the total surface area of the quartz particles; similarly, in order to further enhance the purification efficiency, the first purified product which does not meet the purity grade requirement and the third purified product which does not meet the purity grade requirement to be subjected to acid washing need to be subjected to grinding treatment before the acid washing treatment operation is performed.
According to the purification method of silicon dioxide, the sintering process in the operation corresponding to the S1 and the S3 comprises a heating stage and a heat preservation stage positioned after the heating stage, wherein the sintering temperature of the heat preservation stage is 700-2200 ℃, namely the sintering temperature of the heat preservation stage can be 700 ℃, 100 ℃, 1500 ℃ or any value between the two, most of metal impurities can be melted by controlling the sintering temperature of the heat preservation stage to be not lower than 700 ℃, and the sintering temperature of the heat preservation stage is controlled to be not higher than 2200 ℃, so that the electric charge cost and the cost of a sintering device are saved.
The sintering temperature of the heat preservation stage in the operation corresponding to the step S3 is higher than that of the heat preservation stage in the step S1; in the step S4, as the number of cycles of the operation corresponding to the step S3 increases, the sintering temperature of the heat preservation stage in the operation corresponding to the step S3 gradually increases; on one hand, by uniformly increasing the sintering temperature of the heat preservation stage along with the increase of the cycle times, different metals, particularly high-melting-point metal impurities, can be sufficiently melted and evaporated; on the other hand, the purpose of saving the electric charge can be achieved on the premise of ensuring the purification effect. For example, if the purification steps of the silica are in sequence: and (3) sintering treatment is sequentially performed in the whole purification step, wherein the sintering temperatures in the previous and subsequent 3 times of sintering treatment are inconsistent and gradually increased according to the sintering sequence.
It should be noted that, since the quartz particles are melted to be liquid when the sintering temperature is higher than 1700 ℃, and the silicon compound in the quartz particles is easily reduced to elemental silicon by the carbon nanotubes, when the sintering temperature is higher than 1700 ℃, the sintered product at this temperature needs to be successively ground and oxidized before being subjected to the sieving treatment in order to ensure the purification effect, and in this process, the cooled bulk sintered product is ground to be fine particles meeting the requirements, and then the elemental silicon in the sintered product is oxidized to be silicon dioxide by the oxidizing treatment.
According to the purification method of the silicon dioxide, preferably, the sintering temperature in the heating stage is uniformly increased within 2-12 h, and the higher the sintering temperature in the heating stage is, the longer the heating period is needed; introducing inert gas into the sintering device in the heating stage to enable the quartz particles to be sintered and oxidized in inert atmosphere; the heat preservation period of the heat preservation stage is 0.5-2 h, the higher the sintering temperature of the heat preservation stage is, the longer the heat preservation period is needed, meanwhile, oxidizing gas is introduced into the sintering device in the heat preservation stage, the mole fraction of the oxidizing gas in the sintering device is gradually increased along with the extension of the heat preservation time, and the change range of the mole fraction of the oxidizing gas in the sintering device is 1% -99%; by introducing oxidizing gas into the sintering device, on the one hand, metal impurity gas can be removed by oxidation, and on the other hand, silicon compounds with low valence state can be oxidized into silicon dioxide with high valence state; on the one hand, the molar fraction of the oxidizing gas in the sintering device is gradually changed from low to high so as to ensure the safety of the purification process from unexpected explosion, and the concentration of evaporated metal impurities is slowly increased along with the increase of the time, so that a large amount of oxidizing gas is not required to be introduced at one time.
Furthermore, in order to maintain the purity of the oxidizing gas in the sintering device, a negative pressure cycle is required to continuously pump out the gas containing other oxidation products in the sintering device while introducing new oxidizing gas into the sintering device, so as to avoid the occurrence of the condition that the purification effect is not up to standard due to incomplete oxidation of evaporated metal impurities.
According to the purification method of silica of the present invention, the oxidizing gas introduced into the sintering vessel during the heat-retaining stage may be one or more selected from the group consisting of air, oxygen and chlorine, preferably, the oxidizing gas includes oxygen and chlorine, wherein the molar ratio of the oxygen to the chlorine is (2.5 to 3.5): 1, i.e. the molar ratio of said oxygen to said chlorine may be 2.5: 1. 3: 1. 3.5:1 or any value therebetween, more preferably, the molar ratio of said oxygen to said chlorine is 3:1, at which the vast majority of metal impurities can be fully oxidized and removed.
It should be noted that, when the sintering temperature is higher than 1700 ℃, the composition of the oxidizing gas introduced during the oxidation treatment performed before the sintering product at the temperature is subjected to the sieving treatment may also refer to the composition of the oxidizing gas, and of course, due to a certain difference between the reducibility of the elemental silicon and the reducibility of the metal impurities, the proportion of each component may be appropriately adjusted by a person skilled in the art, which is not described herein.
According to the method for purifying silicon dioxide of the invention, the inert gas is selected from one or more of helium, neon, argon, krypton and xenon, and in one embodiment, the inert gas is selected from argon. The inert gas is used for fully filling the space in the sintering device in the heating stage, and the inert gas is required to be filled to ensure that any other gas cannot be mixed, and the inert gas is not easy to react with most substances, so that metal impurities cannot be oxidized when the metal impurities exist in the quartz in a solid state form in the sintering treatment process. If the metal oxide is formed in the quartz material due to the careless mixing of the active gas during the sintering process, the purification is failed because the metal oxide forms an oxide film once formed on the surface of the quartz particles, so that the melted metal impurities in the quartz particles cannot be evaporated into the inert gas and are sealed in the quartz particles, and the generated metal oxide is very hard and is difficult to be removed by a grinding physical method later; if it is to be removed, expensive high-quality diamond is required, thereby increasing the cost of purification, and discarding quartz particles having a metal oxide film formed on the surface and taking the raw material again for de-novo purification results in waste of raw material, thereby increasing the cost of raw material.
According to the purification method of the silica of the present invention, in order to obtain a better purification effect, the particle size of the quartz particles is not less than 800 mesh; and/or the carbon nanotubes have a diameter of not more than 20nm and a length of not more than 1um.
According to the purification method of the silicon dioxide of the invention, in the S1, the weight ratio of the quartz particles to the carbon nano tubes is d 1 The d is 1 Not less than 10; in the operation corresponding to S3, the weight ratio of the second purified product to the carbon nano tube is d 2 The method comprises the steps of carrying out a first treatment on the surface of the In the step S4, as the number of cycles of the operation corresponding to the step S3 increases, the weight ratio of the third purified product to the carbon nanotubes gradually increases, and the weight ratio of the third purified product to the carbon nanotubes is d 3 The d is 3 Not more than 100, said d 1 D, said d 2 D, said d 3 Gradually increasing. For example, if the purification steps of the silica are in sequence: S1-S2-S3-S2 operation-S3 operation-S2 operation, and 3 sintering steps are performed in sequence in the whole purification stepThe weight ratio of the object to be purified to the carbon nano tube in the previous and subsequent sintering treatment processes is inconsistent and the size of the object to be purified is gradually increased according to the sintering sequence, for example: 10:1 to 50:1 to 100:1. since the pre-purified product which has been partially purified in the previous stage is used in the subsequent purification process and a certain amount of impurities are also present in the carbon nanotubes, it is necessary to control the amount of the carbon nanotubes in the subsequent purification process in order to prevent the occurrence of the decrease in purity of the silica which has undergone the subsequent purification.
According to the purification method of the silicon dioxide, in the pickling treatment process of the operation corresponding to the step S3, one or more acids selected from hydrochloric acid, sulfuric acid, nitric acid, oxalic acid, formic acid or citric acid can be selected for washing.
Further, the pickling treatment process comprises a plurality of washing and purifying processes, and the washing and purifying processes are respectively carried out by selecting different acids for washing; preferably, one of the pickling treatments comprises 2 washing and purifying processes, in which case the above six acids can in principle form 6x5x4x3x2 = 720 permutations, but the random permutation is not necessarily good; more preferably, the washing and purifying process is performed by selecting inorganic acid and organic acid according to the operation sequence. In an embodiment, the pickling process includes a first washing and a second washing sequentially performed, wherein an inorganic acid, that is, one or more of hydrochloric acid, sulfuric acid, or nitric acid, is selected in the first washing, and an organic acid, that is, one or more of oxalic acid, formic acid, or citric acid, is selected in the second washing, and in this case, the six acids may form a 3×3=9 permutation and combination in principle.
According to the purification method of silica of the present invention, the acid selected during the pickling treatment of the operation corresponding to S3 in different cyclic operations is not exactly the same. In order to achieve better purification effect, the number of cycles of the operation corresponding to S3 is 10-55, the combination of the acids selected in the pickling process of the operation corresponding to S3 in the previous 9 cycles is not repeated, the combination of the acids used in the 10 th cycle is the combination of the acids used in the previous 2 nd cycle, and so on, and at most 10+9+8+7+6+5+4+3+2+1=55 cycles can be formed.
According to the purification method of silica of the present invention, in the S1, the primary sintered product is separated by using a gradient sifter 100 to obtain a first purified product of various purity levels. In an embodiment, the gradient sifter 100 includes a centrifuge bowl 110 and a classification groove 130, the centrifuge bowl 110 is conical, the classification groove 130 is flat and cylindrical, and the centrifuge bowl 110 is disposed in the classification groove 130 and rotatable relative to the classification groove 130; the centrifugal bowl 110 is provided with a centrifugal cavity 111 for accommodating the primary sintered product, the upper surface of the centrifugal bowl 110 is provided with an accent for communicating the centrifugal cavity 111 with the outside, the side wall of the centrifugal bowl 110 is provided with a plurality of screen holes 113 which are arranged up and down, the pore sizes of the screen holes 113 are sequentially reduced from top to bottom, and the bottom of the classifying groove 130 is provided with a plurality of gradient belts 131 which are sequentially arranged from inside to outside by taking the centrifugal bowl 110 as a center. When the primary sintered product is sieved, the primary sintered product is firstly put into the centrifugal bowl 110 for centrifugation, the mass of primary sintered product particles with higher purity is smaller and is easier to approach the lower end part of the centrifugal bowl 110, the mass of primary sintered product particles with lower purity is larger and is easier to approach the upper end part of the centrifugal bowl 110, the primary sintered product particles near the lower end of the centrifugal bowl 110 leave the centrifugal cavity 111 from the sieve holes 113 on the side wall of the lower end of the centrifugal bowl 110 and enter the corresponding gradient zones 131 in the classifying groove 130, and the primary sintered product particles near the upper end of the centrifugal bowl 110 leave the centrifugal cavity 111 from the sieve holes 113 on the side wall of the upper end of the centrifugal bowl 110 and enter the corresponding gradient zones 131 in the classifying groove 130. By adopting the gradient sifter 110, not only the primary sintered products can be sifted successfully to obtain the first purified products with various purity grades, but also the purification efficiency of the pickling treatment and sintering treatment in the subsequent steps is higher because some liquid products in the primary sintered products can pull out micron-sized filiform products after centrifugal operation. The separation of the purified product at various stages in the subsequent steps may also be performed as described above and will not be described in detail herein.
According to the purification method of silicon dioxide of the invention, in the S1, a plurality of the first purification products which do not meet the purity grade requirement can be mixed together for acid washing treatment; the plurality of first purified products which do not meet the purity grade requirements can be subjected to acid washing treatment separately according to the purity grade division, and in this case, the plurality of first purified products which do not meet the purity grade requirements can be subjected to acid washing treatment simultaneously or sequentially; the latter has a higher purification efficiency and can save more costs than the former. The pickling treatment process of the subsequent steps is the same and is not repeated.
Further, the pickling treatment is a resuspension pickling, and in the pickling process, the acid liquid in the washing device completely coats the sintered product in the corresponding stage, so that the metal impurities which are not removed in the inner layer of the sintered product in the corresponding stage can be fully contacted with the acid liquid and removed in the cleaning process, and the purification purity is further improved.
In an embodiment, the washing device is a triaxial weightless wheel 200, the triaxial weightless wheel 200 includes a fixed seat 210, a first fixed rod 220, a second fixed rod 230, a third fixed rod 240, and a washing pot 250, the first fixed rod 220 is vertically disposed and the lower end of the first fixed rod is connected with the fixed seat 210, the first fixed rod 220 can move back and forth relative to the fixed seat 210, one end of the second fixed rod 230 is rotatably connected with the upper end of the first fixed rod 220, the second fixed rod 230 can rotate by 360 ° left and right relative to the first fixed rod 220, the other end of the second fixed rod 230 is rotatably connected with one end of the third fixed rod 240, the third fixed rod 240 can rotate by 360 ° up and down relative to the second fixed rod 230, the other end of the third fixed rod 240 is connected with the washing pot 250, the washing pot 250 is used for containing acidic liquid for washing and products of corresponding phases, the number of the third fixed rod 240 and the washing pot 250 can be equal to a plurality of independent fixed rods 240 and a plurality of the third fixed rod 240. In an embodiment, the number of the third fixing bars 240 is 6, the number of the washing pans 250 is 6, and the 6 washing pans 250 are respectively marked as a No. 1 pan, a No. 2 pan, a No. 3 pan, a No. 4 pan, a No. 5 pan, and a No. 6 pan; in this embodiment, the tri-axial weightless wheel 200 may wash the pre-purified products of the quartz particles of 6 purity levels at the same time, thereby accelerating the purification progress, or may divide the pre-purified products of the quartz particles of the same purity level into a plurality of parts to be washed in different numbered pots, respectively, thereby further improving the purification efficiency.
The technical features of the present invention provided in the technical solutions will be further and fully described in the following with reference to the specific embodiments, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The examples are not to be construed as limiting the specific techniques or conditions described in the literature in this field or as per the specifications of the product. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
In this example, the purity requirement of the purified silica is not less than 99.999999%; for this reason, we choose to perform 10 sintering treatments and 10 pickling treatments, and select 800-mesh quartz particles, and use carbon nanotubes with a diameter of 19 nm and a length of 0.9 μm.
(1) Firstly, grinding quartz particles, wherein the weight ratio of the quartz particles to the carbon nano tubes is 10:1, then placing the mixed product into a sintering device, pumping out the air in the sintering device and introducing argon to replace filling. The first sintering is carried out at 700 ℃, and after the temperature is slowly raised to 700 ℃ for 2 hours, the heat preservation process is started. And (3) starting the heat preservation process, slowly introducing oxidizing gas (n (oxygen): n (chlorine) =3:1) from 1% concentration, continuously circularly pumping out and filtering the internal gas, keeping the heat for 0.5h, finally introducing the oxidizing gas with 99% concentration before cooling, and starting cooling after the last filtering, and simultaneously feeding the mixture into a gradient filter.
Grinding the cooled sintered product which does not meet the purity grade requirement, and then carrying out acid washing treatment, wherein the acid washing treatment process comprises 2 washing and purifying processes, hydrochloric acid is selected for the first time, oxalic acid is selected for the second time, and washing is carried out after the completion of the first washing and purifying process.
(2) Mixing the cleaned product which does not meet the purity grade requirement with carbon nano tubes in a ratio of 20:1, putting the mixed product into a sintering device, pumping out air in the sintering device, and introducing argon to replace filling. And sintering at 850 ℃ in the second sintering treatment, and slowly heating to 850 ℃ in 3.1h, and then starting the heat preservation process. And (3) starting the heat preservation process, slowly introducing oxidizing gas (n (oxygen): n (chlorine) =3:1) from 1% concentration, continuously circularly pumping out and filtering the internal gas, keeping the heat for 0.65h, finally introducing the oxidizing gas with 99% concentration before cooling, and starting cooling after the last filtering, and simultaneously feeding the mixture into a gradient filter.
Grinding the cooled sintered product which does not meet the purity grade requirement, and then carrying out acid washing treatment, wherein the acid washing treatment process comprises 2 washing and purifying processes, the first washing and selecting sulfuric acid, the second washing and selecting oxalic acid, and cleaning is carried out after the completion of the washing.
(3) Mixing the cleaned product which does not meet the purity grade requirement with carbon nano tubes in a ratio of 30:1, putting the mixed product into a sintering device, pumping out air in the sintering device, and introducing argon to replace filling. And sintering at 1000 ℃ for the third sintering treatment, and after the temperature is slowly raised to 1000 ℃ for 4.2 hours, starting the heat preservation process. And (3) starting the heat preservation process, slowly introducing oxidizing gas (n (oxygen): n (chlorine) =3:1) from 1% concentration, continuously circularly pumping out and filtering the internal gas, keeping the heat for 0.8h, finally introducing the oxidizing gas with 99% concentration before cooling, and starting cooling after the last filtering, and simultaneously feeding the mixture into a gradient filter.
Grinding the cooled sintered product which does not meet the purity grade requirement, and then carrying out acid washing treatment, wherein the acid washing treatment process comprises 2 washing and purifying processes, nitric acid is selected for the first time, oxalic acid is selected for the second time, and washing is carried out after the completion of the first washing and purifying process.
(4) Mixing the cleaned product which does not meet the purity grade requirement with carbon nano tubes in a ratio of 40:1, putting the mixed product into a sintering device, pumping out air in the sintering device, and introducing argon to replace filling. The fourth sintering treatment is carried out by selecting 1150 ℃ for sintering, and after the temperature is slowly raised to 1150 ℃ for 5.3 hours, the heat preservation process is started. And (3) starting the heat preservation process, slowly introducing oxidizing gas (n (oxygen): n (chlorine) =3:1) from 1% concentration, continuously circularly pumping out and filtering the internal gas, keeping the heat for 0.95h, finally introducing the oxidizing gas with 99% concentration before cooling, and starting cooling after the last filtering, and simultaneously feeding the mixture into a gradient filter.
Grinding the cooled sintered product which does not meet the purity grade requirement, and then carrying out acid washing treatment, wherein the acid washing treatment process comprises 2 washing and purifying processes, hydrochloric acid is selected for the first time, formic acid is selected for the second time, and washing is carried out after the completion of the second washing.
(5) Mixing the cleaned product which does not meet the purity grade requirement with carbon nano tubes at a ratio of 50:1, putting the mixed product into a sintering device, pumping out air in the sintering device, and introducing argon to replace filling. The fifth sintering is carried out at 1300 ℃, and after the temperature is slowly raised to 1300 ℃ for 6.4 hours, the heat preservation process is started. And (3) starting the heat preservation process, slowly introducing oxidizing gas (n (oxygen): n (chlorine) =3:1) from 1% concentration, continuously circularly pumping out and filtering the internal gas, keeping the heat for 1.1h, finally introducing the oxidizing gas with 99% concentration before cooling, and starting cooling after the last filtering, and simultaneously feeding the mixture into a gradient filter.
Grinding the cooled sintered product which does not meet the purity grade requirement, and then carrying out acid washing treatment, wherein the acid washing treatment process comprises 2 washing and purifying processes, the first washing and selecting sulfuric acid, the second washing and selecting formic acid, and cleaning is carried out after the completion of the washing.
(6) Mixing the cleaned product which does not meet the purity grade requirement with the carbon nano tube to obtain a mixture of the carbon nano tube and the carbon nano tube with the purity grade of 60:1, putting the mixed product into a sintering device, pumping out air in the sintering device, and introducing argon to replace filling. The sixth sintering is carried out at 1450 ℃, and after the temperature is slowly raised to 1450 ℃ for 7.5 hours, the heat preservation process is started. And (3) starting the heat preservation process, slowly introducing oxidizing gas (n (oxygen): n (chlorine) =3:1) from 1% concentration, continuously circularly pumping out and filtering the internal gas, keeping the heat for 1.25h, finally introducing the oxidizing gas with 99% concentration before cooling, and starting cooling after the last filtering, and simultaneously feeding the mixture into a gradient filter.
Grinding the cooled sintered product which does not meet the purity grade requirement, and then carrying out acid washing treatment, wherein the acid washing treatment process comprises 2 washing and purifying processes, nitric acid is selected for the first time, formic acid is selected for the second time, and cleaning is carried out after the completion of the first washing and purifying process.
(7) Mixing the cleaned product which does not meet the purity grade requirement with carbon nano tubes at a ratio of 70:1, putting the mixed product into a sintering device, pumping out air in the sintering device, and introducing argon to replace filling. And sintering at 1600 ℃ for the seventh sintering, and after the temperature is slowly increased to 1600 ℃ for 8.6 hours, starting the heat preservation process. And (3) starting the heat preservation process, slowly introducing oxidizing gas (n (oxygen): n (chlorine) =3:1) from 1% concentration, continuously circularly pumping out and filtering the internal gas, keeping the heat for 1.4 hours, finally introducing the oxidizing gas with 99% concentration before cooling, and starting cooling after the last filtering, and simultaneously feeding the mixture into a gradient filter.
Grinding the cooled sintered product which does not meet the purity grade requirement, and then carrying out acid washing treatment, wherein the acid washing treatment process comprises 2 washing and purifying processes, hydrochloric acid is selected for the first time, citric acid is selected for the second time, and washing is carried out after the completion of the second washing.
(8) Mixing the cleaned product which does not meet the purity grade requirement with carbon nano tubes in a ratio of 80:1, putting the mixed product into a sintering device, pumping out air in the sintering device, and introducing argon to replace filling. The eighth sintering is carried out at 1750 ℃, and after the temperature is slowly raised to 1750 ℃ for 9.7 hours, the heat preservation process is started. And (3) starting the heat preservation process, slowly introducing oxidizing gas (n (oxygen): n (chlorine) =3:1) from 1% concentration, continuously circularly extracting and filtering the internal gas, keeping the heat for 1.55h, finally introducing the oxidizing gas with 99% concentration before cooling, starting cooling after the last filtering, sequentially grinding and oxidizing the sintered product, and then sending the sintered product into a gradient filter.
Grinding the cooled sintered product which does not meet the purity grade requirement, and then carrying out acid washing treatment, wherein the acid washing treatment process comprises 2 washing and purifying processes, the first washing and selecting sulfuric acid, the second washing and selecting citric acid, and cleaning after the completion.
(9) Mixing the cleaned product which does not meet the purity grade requirement with the carbon nano tube at 90:1, putting the mixed product into a sintering device, pumping out air in the sintering device, and introducing argon to replace filling. And the ninth sintering is carried out at 2050 ℃, and the heat preservation process is started after the temperature is slowly increased to 2050 ℃ for 10.8 hours. And (3) starting the heat preservation process, slowly introducing oxidizing gas (n (oxygen): n (chlorine) =3:1) from 1% concentration, continuously circularly extracting and filtering the internal gas, keeping the heat for 1.85 hours, finally introducing the oxidizing gas with 99% concentration before cooling, starting cooling after the last filtering, sequentially grinding and oxidizing the sintered product, and then sending the sintered product into a gradient filter.
Grinding the cooled sintered product which does not meet the purity grade requirement, and then carrying out acid washing treatment, wherein the acid washing treatment process comprises 2 washing and purifying processes, nitric acid is selected for the first time, citric acid is selected for the second time, and cleaning is carried out after the completion of the second washing.
(10) Mixing the cleaned product which does not meet the purity grade requirement with the carbon nano tube to obtain a mixture of 100:1, putting the mixed product into a sintering device, pumping out air in the sintering device, and introducing argon to replace filling. Sintering at 2200 ℃ for the tenth sintering, slowly heating to 2200 ℃ for 12 hours, and then starting the heat preservation process. And (3) starting the heat preservation process, slowly introducing oxidizing gas (n (oxygen): n (chlorine) =3:1) from 1% concentration, continuously circularly pumping out and filtering the internal gas, keeping the heat for 2 hours, finally introducing the oxidizing gas with the concentration of 99% before cooling, starting cooling after the last filtering, sequentially grinding and oxidizing the sintered product, and then sending the sintered product into a gradient filter.
Grinding the cooled sintered product which does not meet the purity grade requirement, and then carrying out acid washing treatment, wherein the acid washing treatment process comprises 2 washing and purifying processes, sulfuric acid is selected by first washing, oxalic acid is selected by second washing, and the silicon dioxide with the overall purity of not less than 99.999999% is obtained by washing after the completion of the second washing.
The foregoing examples are illustrative only and serve to explain some features of the method of the invention. The appended claims are intended to claim the broadest possible scope and the embodiments presented herein are merely illustrative of selected implementations based on combinations of all possible embodiments. It is, therefore, not the intention of the applicant that the appended claims be limited by the choice of examples illustrating the features of the invention. Some numerical ranges used in the claims also include sub-ranges within which variations in these ranges should also be construed as being covered by the appended claims where possible.
Claims (10)
1. A method for purifying silica, comprising the steps of:
s1: mixing quartz particles with carbon nanotubes and sintering in a sintering device under inert atmosphere to melt and evaporate metal impurities in the quartz particles, oxidizing the metal impurities in the sintering device by oxidizing gas, discharging the oxidized metal impurities from the sintering device to obtain primary sintering products of the quartz particles, and screening the primary sintering products to obtain first purified products with various different purity levels;
S2: if the first purified product comprises a first purified product which does not meet the purity grade requirement, carrying out acid washing treatment on the first purified product which does not meet the purity grade requirement to obtain a plurality of second purified products with different purity grades;
s3: if the second purified product comprises a second purified product which does not meet the purity grade requirement, mixing the second purified product which does not meet the purity grade requirement with carbon nano tubes, sintering in a sintering device under inert atmosphere to enable metal impurities in the second purified product which does not meet the purity grade requirement to be melted and evaporated, oxidizing the metal impurities in the sintering device by oxidizing gas, discharging the oxidized metal impurities from the sintering device to obtain a re-sintered product of quartz particles, and screening the re-sintered product to obtain a plurality of third purified products with different purity grades;
s4: and if the third purified product comprises a third purified product which does not meet the purity grade requirement, sequentially and circularly carrying out the operations corresponding to the S2 and the S3 on the third purified product which does not meet the purity grade requirement until the obtained purified product meets the purity grade requirement of the silicon dioxide.
2. The purification method according to claim 1, wherein the sintering process in the operation corresponding to S1 and S3 includes a temperature raising stage and a heat preservation stage located after the temperature raising stage, the sintering temperature of the heat preservation stage is 700 to 2200 ℃, and the sintering temperature of the heat preservation stage in the operation corresponding to S3 is greater than the sintering temperature of the heat preservation stage in S1;
in the step S4, as the number of cycles of the operation corresponding to the step S3 increases, the sintering temperature of the heat preservation stage in the operation corresponding to the step S3 gradually increases.
3. The purification method according to claim 2, wherein the sintering temperature in the temperature rising stage is increased uniformly within 2 to 12 hours, and inert gas is introduced into the sintering device in the temperature rising stage; and/or the heat preservation period of the heat preservation stage is 0.5-2 h, and oxidizing gas is introduced into the sintering device in the heat preservation stage.
4. The purification method according to claim 1, wherein the particle size of the quartz particles is not less than 800 mesh; and/or the carbon nanotubes have a diameter of not more than 20nm and a length of not more than 1um.
5. The method of purifying as recited in claim 4, wherein in S1, the weight ratio of the quartz particles to the carbon nanotubes is d 1 The d is 1 Not less than 10; in the operation corresponding to S3, the weight ratio of the second purified product to the carbon nano tube is d 2 ；
In the step S4, as the number of cycles of the operation corresponding to the step S3 increases, the weight ratio of the third purified product to the carbon nanotubes gradually increases, and the weight ratio of the third purified product to the carbon nanotubes is d 3 The d is 3 Not more than 100, said d 1 D, said d 2 D, said d 3 Gradually increasing.
6. The purification method according to claim 2, wherein the specific steps of the oxidation treatment process in the operation corresponding to S1 and/or S3 include: and in the initial stage of the heat preservation stage, starting to introduce oxidizing gas into the sintering device, and gradually increasing the mole fraction of the oxidizing gas in the sintering device along with the extension of the heat preservation time, wherein the mole fraction of the oxidizing gas in the sintering device is changed within the range of 1% -99%.
7. The purification method of claim 6, wherein the oxidizing gas comprises oxygen and chlorine, and wherein the molar ratio of oxygen to chlorine is (2.5-3.5): 1.
8. the method according to claim 1, wherein the acid washing treatment performed in the operation corresponding to S3 is performed by washing with one or more acids selected from the group consisting of hydrochloric acid, sulfuric acid, nitric acid, oxalic acid, formic acid and citric acid.
9. The purification method according to claim 8, wherein the acid washing treatment process comprises a plurality of washing purification processes, wherein the washing purification processes are respectively performed by selecting an inorganic acid and an organic acid in order of operation; and/or the cycle number of the operation corresponding to the S3 is 10-55, and the combination of the acids selected in the pickling process of the operation corresponding to the S3 in the previous nine cycles is not repeated.
10. The purification method according to any one of claims 1 to 9, wherein in the S1, the sieving treatment is performed using a gradient sieve, and/or wherein in the operation corresponding to the S3, the sieving treatment is performed using a gradient sieve;
the gradient screening device comprises a centrifugal bowl and a classification groove, wherein the centrifugal bowl is arranged in the classification groove and is rotatable relative to the classification groove, a centrifugal cavity for accommodating a primary sintering product or a secondary sintering product is formed in the centrifugal bowl, a plurality of screening holes which are arranged up and down are formed in the side wall of the centrifugal bowl, the size of the screening holes is sequentially reduced from top to bottom, and a plurality of gradient strips which are sequentially arranged from inside to outside by taking the centrifugal bowl as a center are formed at the bottom of the classification groove.
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