阅读说明：本技术 惰性气体纯化材料的制备方法 (Preparation method of inert gas purification material ) 是由 付泽华 周锐 张军社 邓浩 李侨 谢志宴 于 2018-07-27 设计创作，主要内容包括：本发明公开的惰性气体纯化材料的制备方法,用于对惰性气体除杂,包括步骤：氧化物制备,所述氧化物制备包括选取适量的氧化物,所述氧化物为过渡金属氧化物或过渡金属氧化物矿石；催化剂溶液配制,配制适量的催化剂溶液,所述催化剂溶液为稀有金属盐溶液；基体配制,将所述适量的催化剂溶液与所述适量的氧化物混合、干燥,然后在500-1000℃条件下煅烧,煅烧时间为10-14h,即得所述惰性气体纯化材料。本发明惰性气体纯化材料的制备方法,其工艺控制简单、制备效率高；原料选取容易,制备成本低；制备的惰性气体纯化材料可循环多次使用,使用寿命长。(The invention discloses a preparation method of an inert gas purification material, which is used for removing impurities from inert gas and comprises the following steps: preparing an oxide, wherein the oxide preparation comprises selecting a proper amount of oxide, and the oxide is a transition metal oxide or a transition metal oxide ore; preparing a catalyst solution, namely preparing a proper amount of catalyst solution, wherein the catalyst solution is a rare metal salt solution; and (2) preparing a matrix, namely mixing the proper amount of catalyst solution and the proper amount of oxide, drying, and then calcining at the temperature of 500-1000 ℃ for 10-14h to obtain the inert gas purification material. The preparation method of the inert gas purification material has the advantages of simple process control and high preparation efficiency; the raw materials are easy to select, and the preparation cost is low; the prepared inert gas purification material can be recycled for multiple times and has long service life.)

1. The preparation method of the inert gas purification material is used for removing impurities from inert gas, and is characterized by comprising the following steps of:

preparing an oxide: the preparation of the oxide comprises selecting a proper amount of oxide, wherein the oxide is transition metal oxide or transition metal oxide ore;

preparing a catalyst solution: preparing a proper amount of catalyst solution, wherein the catalyst solution is a rare metal salt solution;

preparing a matrix: and mixing the appropriate amount of catalyst solution and the appropriate amount of oxide, drying, and calcining at the temperature of 500-1000 ℃ for 10-14h to obtain the inert gas purification material.

2. The preparation of an inert gas purification material according to claim 1, wherein the transition metal oxide is at least one or more of copper oxide, iron oxide, magnesium oxide, titanium oxide, or manganese oxide; the oxide ore is at least one or more of iron ore, copper ore or manganese ore.

3. The preparation of an inert gas purification material according to claim 2, characterized in that the rare metal salt solution is at least one or more of ruthenium salt solution, palladium salt solution, platinum salt solution.

4. The method as claimed in claim 3, wherein the step of preparing the oxide further comprises pulverizing and sieving the selected oxide to obtain oxide particles of 250-2000 μm.

5. The method of claim 4, wherein the step of preparing the oxide further comprises the steps of washing and drying the selected oxide or the oxide particles.

6. The method according to claim 5, wherein the matrix preparation step comprises preparing a mixture comprising the catalyst solution and the dried oxide or oxide particles by incipient wetness impregnation.

7. The method of claim 6, wherein after preparing the mixture, the matrix formulating step further comprises drying the mixture and oven drying to remove moisture to form a precursor.

8. The method as claimed in claim 7, wherein the step of preparing the matrix further comprises calcining the precursor at 500-1000 ℃ for 10-14h, and introducing a proper amount of gas during the calcining.

9. The method of claim 7 or 8, wherein in the step of preparing the oxide, if the selected oxide is in a powder form, the step of preparing the matrix further comprises preparing a suitable amount of a binder, and mixing the binder with the calcined precursor to increase the viscosity of the calcined precursor.

10. The preparation of an inert gas purification material according to claim 9, wherein the powdered oxide has an average particle size of 10-100 um.

11. The method for preparing an inert gas purification material as claimed in claim 9, wherein the step of preparing the matrix comprises mixing the calcined precursor with a binder, and the step of granulating the powder formed into uniform particles having a particle size of 250 μm and 2000 μm.

12. The method of claim 11, wherein the matrix preparation step, after powder granulation, further comprises drying and sieving the uniform granules to remove moisture and particulate powder that does not meet the particle size requirements.

13. The method as claimed in claim 12, wherein the step of preparing the matrix comprises calcining the dried and sieved uniform particles at 1000 ℃ for 10-14h, and introducing a proper amount of gas during the calcining.

Technical Field

The invention belongs to the technical field of preparation of monocrystalline silicon materials, and particularly relates to a preparation method of an inert gas purification material.

Background

In the process of growing monocrystalline silicon, polycrystalline silicon and other crystals, inert gas needs to be introduced into the furnace to stabilize the furnace pressure, and impurities such as volatile matters and oxides are taken away, so that the stability of crystal growth and the product quality are improved. The existing inert gas for crystal growth, such as argon, is mostly disposable. The purity of the used inert gas is reduced by collecting the impurities such as carbon monoxide and hydrocarbon from equipment such as a czochralski crystal growing furnace and a polycrystal ingot furnace. In order to improve the purity of the recovered gas, a reactor is required to remove or oxidize impurities in the inert gas, and the reactor is filled with a gas purification material.

The preparation of the gas purification material requires the use of a catalyst. Chinese patents with application date of 2016, 11 and 24, application number of 201611042389.1, publication number of 2018, 6 and 1, and publication number of CN108097244A disclose a preparation method of a supported ruthenium catalyst, which mainly comprises heating a ruthenium-containing precursor to 450-1200 ℃ to form volatile ruthenium species; and (3) transferring the volatile ruthenium species to a carrier material preheated to 450-1200 ℃ by using a carrier gas for adsorption and deposition, wherein the deposition time is 0.5-48 hours, and cooling to obtain the supported ruthenium catalyst. The carrier material can be transition metal oxides such as alumina, copper oxide, iron oxide and the like, or composite oxides such as magnesium aluminate spinel, hydrotalcite and the like. According to the method, a catalyst precursor is heated to form volatile matters, the volatile matters are deposited on a carrier material to prepare the supported catalyst, and the catalyst is prepared in a vapor deposition mode, so that the problems of low preparation efficiency, complex process control and the like exist.

There is therefore a need for a process for producing an inert gas purification material, which is capable of producing a gas purification material for removing impurities from an inert gas; meanwhile, the requirements of high preparation efficiency and low process complexity are required to be met, and the purification cost of the inert gas in the actual production process can be reduced.

Disclosure of Invention

The invention aims to provide a preparation method of an inert gas purification material, the prepared purification material is used for removing impurities from inert gas, and the preparation method has the advantages of simple process, convenient raw material selection and low preparation cost.

The technical scheme adopted by the invention is as follows: the preparation method of the inert gas purification material is used for removing impurities from inert gas and comprises the following steps:

preparing an oxide: the preparation of the oxide comprises selecting a proper amount of oxide, wherein the oxide is transition metal oxide or transition metal oxide ore;

preparing a catalyst solution: preparing a proper amount of catalyst solution, wherein the catalyst solution is a rare metal salt solution;

preparing a matrix: and mixing the appropriate amount of catalyst solution and the appropriate amount of oxide, drying, and calcining at the temperature of 500-1000 ℃ for 10-14h to obtain the inert gas purification material.

Preferably, the transition metal oxide is at least one or more of copper oxide, iron oxide, magnesium oxide, titanium oxide or manganese oxide; the oxide ore is at least one or more of iron ore, copper ore or manganese ore.

Preferably, the rare metal salt solution is at least one or more of ruthenium salt solution, palladium salt solution and platinum salt solution.

Further, the oxide preparation step also comprises the steps of crushing and screening the selected oxide to obtain oxide particles of 250-2000 μm; washing and drying the selected oxide or the oxide particles.

Illustratively, the matrix preparation step includes preparing a mixture including the catalyst solution and the dried oxide or oxide particles by an incipient wetness impregnation method; then drying the mixture, and drying to remove moisture to form a precursor; and finally, calcining the precursor at the temperature of 500-1000 ℃, wherein the calcining time is 10-14h, and a proper amount of gas, such as argon, nitrogen or air, is introduced during calcining.

Preferably, in the oxide preparation step, if the selected oxide is in a powder form, the average particle size of the selected oxide is 10-100um, and the base body preparation step further comprises the step of preparing a proper amount of a binder, mixing the binder with the calcined precursor, and increasing the viscosity of the calcined precursor; then, mixing the calcined precursor with an adhesive, and then performing powder granulation to form uniform particles with the particle size of 250-2000 mu m; then, drying and screening the uniform particles, and removing moisture and particle powder which does not meet the requirement of the particle size; and finally, calcining the dried and screened uniform particles at the temperature of 500-1000 ℃ for 10-14h, and introducing a proper amount of gas such as argon, nitrogen or air during calcination.

The invention has the beneficial effects that: the preparation method of the inert gas purification material has simple process and high preparation efficiency; the raw materials are easy to select, and the preparation cost is low; the prepared inert gas purification material can be recycled for multiple times and has long service life.

Drawings

FIG. 1 is a flow chart of a process for preparing an inert gas purification material for breaking and sampling;

FIG. 2 is a flow chart of the process for preparing the inert gas purification material for forming and sampling.

Detailed Description

The preparation method of the inert gas purification material provided by the invention is used for removing impurities from the inert gas, and the inert gas can be inert gas for growing monocrystalline silicon, such as argon, and can also be other inert gases. The method specifically comprises the following steps:

preparing an oxide: the preparation of the oxide comprises selecting a proper amount of oxide, wherein the oxide is transition metal oxide or transition metal oxide ore; preferably, the transition metal oxide is at least one or more of copper oxide, iron oxide, magnesium oxide, titanium oxide or manganese oxide; the oxide ore is at least one or more of iron ore, copper ore or manganese ore.

In the oxide preparation step, the method can also comprise the steps of crushing and screening the selected oxide to obtain oxide particles of 250-2000 mu m; the selected oxide or oxide particles are washed and dried.

Preparing a catalyst solution: preparing a proper amount of catalyst solution which is rare metal salt solution; the rare metal salt solution is at least one or more of ruthenium salt solution, palladium salt solution and platinum salt solution.

Preparing a matrix: mixing a proper amount of catalyst solution and a proper amount of oxide, drying, and calcining at the temperature of 500-1000 ℃ for 10-14h to obtain the inert gas purification material.

In the matrix preparation step, a mixture containing a catalyst solution and dried oxides or oxide particles may be prepared by an incipient wetness impregnation method; then drying the mixture, and drying to remove moisture to form a precursor; and finally, calcining the precursor at the temperature of 500-1000 ℃ for 10-14h, and introducing a proper amount of gas such as argon, nitrogen or air during calcination. The incipient wetness impregnation method is a method in which a catalyst is dissolved in water to prepare a catalyst solution, the volume of the solution is made to be equal to the saturated water absorption capacity of an oxide carrier, and then the catalyst solution is added dropwise to the oxide carrier and mixed uniformly.

Preferably, in the oxide preparation step, if the selected oxide is in a powder form, and the average particle size of the selected oxide is 10-100um, the matrix preparation step further comprises the step of preparing a proper amount of adhesive, and mixing the adhesive with the calcined precursor to increase the viscosity of the calcined precursor; then, mixing the calcined precursor with an adhesive, and then performing powder granulation to form uniform particles with the particle size of 250-2000 mu m; then, drying and screening the uniform particles, and removing moisture and particle powder which does not meet the particle size requirement; and finally, calcining the dried and screened uniform particles at the temperature of 500-1000 ℃, wherein the calcining time is 10-14h, and a proper amount of gas, such as argon, nitrogen or air, is introduced during calcining.

The invention is described in detail below with reference to the figures and specific embodiments. The figures are simplified schematic diagrams illustrating only the basic method steps of the invention in a schematic way, and therefore only show the constituents relevant to the invention.