CN109775747B - Preparation method of high-purity anhydrous indium trichloride - Google Patents
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- PSCMQHVBLHHWTO-UHFFFAOYSA-K indium(iii) chloride Chemical compound Cl[In](Cl)Cl PSCMQHVBLHHWTO-UHFFFAOYSA-K 0.000 title claims abstract description 105
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 42
- 229910052738 indium Inorganic materials 0.000 claims abstract description 34
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 32
- 239000003960 organic solvent Substances 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 14
- 238000009835 boiling Methods 0.000 claims abstract description 8
- 239000000126 substance Substances 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 239000011261 inert gas Substances 0.000 claims abstract description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 15
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 15
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 11
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 6
- 238000004821 distillation Methods 0.000 claims description 3
- 239000003350 kerosene Substances 0.000 claims description 3
- 239000000047 product Substances 0.000 abstract description 17
- 239000012535 impurity Substances 0.000 abstract description 12
- 239000004065 semiconductor Substances 0.000 abstract description 3
- 239000006227 byproduct Substances 0.000 abstract description 2
- 238000002474 experimental method Methods 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract 1
- 230000018044 dehydration Effects 0.000 description 7
- 238000006297 dehydration reaction Methods 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 238000005660 chlorination reaction Methods 0.000 description 6
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 5
- 239000012298 atmosphere Substances 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 239000000460 chlorine Substances 0.000 description 5
- 238000001514 detection method Methods 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 238000000746 purification Methods 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 229910021617 Indium monochloride Inorganic materials 0.000 description 4
- 229910052801 chlorine Inorganic materials 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 4
- APHGZSBLRQFRCA-UHFFFAOYSA-M indium(1+);chloride Chemical compound [In]Cl APHGZSBLRQFRCA-UHFFFAOYSA-M 0.000 description 4
- 238000009616 inductively coupled plasma Methods 0.000 description 4
- 239000002932 luster Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 238000012797 qualification Methods 0.000 description 4
- 238000010992 reflux Methods 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 238000001704 evaporation Methods 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000005416 organic matter Substances 0.000 description 3
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 239000012300 argon atmosphere Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 229910003437 indium oxide Inorganic materials 0.000 description 2
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000011112 process operation Methods 0.000 description 2
- 238000007086 side reaction Methods 0.000 description 2
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 2
- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- 229910021618 Indium dichloride Inorganic materials 0.000 description 1
- DHKHKXVYLBGOIT-UHFFFAOYSA-N acetaldehyde Diethyl Acetal Natural products CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 description 1
- 125000002777 acetyl group Chemical class [H]C([H])([H])C(*)=O 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- RPMLLLKOEWHKLT-UHFFFAOYSA-N butan-1-ol;heptane Chemical compound CCCCO.CCCCCCC RPMLLLKOEWHKLT-UHFFFAOYSA-N 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- NHYCGSASNAIGLD-UHFFFAOYSA-N chlorine monoxide Inorganic materials Cl[O] NHYCGSASNAIGLD-UHFFFAOYSA-N 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- VOWMQUBVXQZOCU-UHFFFAOYSA-L dichloroindium Chemical compound Cl[In]Cl VOWMQUBVXQZOCU-UHFFFAOYSA-L 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- -1 indium series compounds Chemical class 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000003495 polar organic solvent Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 150000004685 tetrahydrates Chemical class 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
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Abstract
The invention discloses a preparation method of high-purity anhydrous indium trichloride, which is characterized in that under the protection of inert gas, refined indium and hydrochloric acid are used as raw materials, an organic solvent is dropwise added into the reaction raw materials while stirring, and the dropwise adding speed is 12-30 mL/min, so that a complex of the organic solvent and the indium trichloride is prepared; after the reaction is finished, distilling to remove low boiling point substances, and then decomposing a complex of an organic solvent and indium trichloride to prepare high-purity anhydrous indium trichloride; experiments prove that the purity of the anhydrous indium trichloride obtained by the method can reach more than 99.999 percent, and the requirement of the raw material of a semiconductor is met; the method has the advantages of simple process flow, less by-products, high product preparation efficiency, high product purity and low impurity content, and is suitable for industrial production and market popularization and application.
Description
Technical Field
The invention relates to the technical field of rare metal fine chemical engineering, in particular to a method for preparing high-purity anhydrous indium trichloride.
Background
The high-purity anhydrous indium trichloride is a main raw material for preparing a laminated cell cathode conductive adhesive, an ITO thin film and a III-V group semiconductor material, can also be used as a catalyst for acetal and ketal reaction, is also a basic raw material for synthesizing organic indium series compounds, and has wide application in the aspects of organic synthesis, solar materials and electronic industry. At present, the preparation method of indium trichloride mainly comprises a direct chlorination method of metal indium, an oxide chlorination method, a gradual heating chlorination method, an organic solvent dehydration method and the like. However, the indium trichloride sample prepared by the methods usually contains crystal water or an organic solvent and cannot be directly applied; the water or organic solvent is difficult to be completely removed by directly heating and raising the temperature, and meanwhile, new impurities are introduced due to decomposition or other side reactions caused by high temperature in the heating process, so that the product purification process and technology need to be further researched, and the high-purity anhydrous indium trichloride product is obtained.
The direct chlorination method of indium is characterized in that indium is used as a raw material, metal indium is directly introduced with chlorine under the condition of vacuum pumping or inert gas atmosphere, and a high-purity indium trichloride product is prepared by slow heating.
The oxide chlorination method is to chlorinate indium oxide as a raw material to prepare the indium-containing oxide; the oxidation method for preparing high-purity indium trichloride can use chlorine, mixed gas of chlorine and carbon monoxide, carbon tetrachloride or thionyl chloride and indium oxide to react together. When the reaction kettle is heated to a certain temperature, the reaction starts, and indium trichloride generated by the reaction is sublimated.
The gradual heating chlorination method is that metal indium is used as a raw material and heated for a long time at the temperature of 150-. The above three methods require good control of the flow and temperature of the chlorine; when the introduced chlorine gas flow is weak, intermediate products of indium monochloride and indium dichloride appear, and the purity of the obtained product is not high. If the introduced chlorine is excessive and the heating temperature is too high, the indium will burn and generate vaporous indium trichloride, which will cause raw material waste and environmental pollution.
The organic solvent dehydration method is based on InCl3·4H2H in O2O can be replaced by a polar organic solvent with oxygen and nitrogen donors, and organic solvents such as amine, formamide and kerosene are adopted to remove crystal water in crystal chloride to prepare high-purity anhydrous indium trichloride. However, the method is difficult to obtain a sample with high purity because the processes involved in the reactions are complex, the reaction time is long, the requirements on experimental conditions are high, the reagents are expensive, organic reagent pollution exists and the like. Meanwhile, the first step of the organic solvent dehydration method requires preparation of InCl3·4H2And O. At a certain temperature, indium chloride can be crystallized from an aqueous solution in the form of tetrahydrate. If the crystallization process contacts with the air for a long time, there will be insoluble InOCl impurity in the crystallization, if there is trace amount of oxygen to exist in indium trichloride heating sublimation purification process moreover, all can cause to have minute quantity of oxygen complex oxide in final product, become contaminated impurity, can influence the quality of high-purity indium trichloride product.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of high-purity anhydrous indium trichloride, which comprises the steps of taking refined indium and hydrochloric acid as raw materials under the protection of inert gas, dropwise adding an organic solvent into the reaction raw materials while stirring, wherein the dropwise adding speed is 12-30 mL/min, and preparing a complex of the organic solvent and the indium trichloride; after the reaction is finished, distilling to remove low boiling point substances, and then decomposing the complex of the organic solvent and the indium trichloride to prepare the high-purity anhydrous indium trichloride.
The method of the invention prepares InCl in inert atmosphere3·4H2O, dehydration and purification are completed in one step, the problem of dehydration of crystal water in the indium trichloride product is solved, impurity removal is performed by using inert gas flow (inert gas or argon-hydrogen mixed gas), the formation of byproducts is reduced, the product preparation efficiency is improved, and the method has the advantages of high product purity, low impurity content, simple process operation and the like.
In the method, the indium content of the refined indium is more than 99.995 percent, and the hydrochloric acid is analytically pure hydrochloric acid with the mass concentration of 36 to 38 percent.
The molar ratio of the refined indium to the hydrochloric acid is 1: 4-10.
The molar ratio of the organic solvent to the indium is 25-35: 1.
The organic solvent is polar organic matter containing oxygen and nitrogen donors or azeotropic matter, such as one or two of dimethyl formamide, n-butanol, n-heptane, kerosene and toluene.
The distillation temperature is 60-110 ℃.
The decomplexing temperature is 120-300 ℃.
Compared with the prior art, the invention has the following advantages:
(1) adopts a one-step synthesis method to synthesize InCl in an inert atmosphere3·4H2O, dehydration and purification are completed in one step, the technical problems of dehydration, purification and the like in the preparation of the high-purity anhydrous indium trichloride are solved, and the process has the advantages of short flow, no generation of three wastes, high product purity, simple process operation and the like;
(2) because the organic solvent adopted in the invention is a polar organic matter containing oxygen and nitrogen donors, the water can be effectively separated, and the solvent is easy to recover, so that the chemical stability is better, namely, the side reaction is minimum, the reaction product can not act with the solvent, the solvent and the product are easy to separate, and the solvent has low toxicity, no pollution and low price; not only provides good reaction environment, but also reduces the boiling point of the complex of the organic matter and the indium trichloride, thereby being convenient for distinguishing impurities and purifying when the impurities are removed by distillation; experiments prove that the purity of the high-purity anhydrous indium trichloride obtained by the method can reach more than 99.999 percent, and the high-purity anhydrous indium trichloride can completely meet the requirements of being used as a semiconductor raw material.
Drawings
Figure 1 is a product XRD survey.
Detailed Description
The present invention will be described in further detail with reference to the following examples, but the scope of the present invention is not limited to the above-mentioned descriptions.
Example 1:
under argon atmosphere, putting refined indium (with indium content of 99.995%) and hydrochloric acid (analytically pure hydrochloric acid with mass concentration of 36%) into a reaction kettle for dissolution, wherein the molar ratio of the refined indium to the hydrochloric acid is 1:4, and then dropwise adding n-butanol at the speed of 15mL/min under the stirring condition, wherein the molar ratio of the n-butanol to the indium is 25: 1; after reacting for 2h, refluxing for 6h at 65 ℃ to evaporate low boiling point substances, and then raising the temperature to 160 ℃ to decompound the complex of the n-butyl alcohol and the indium trichloride to prepare white fluffy flake anhydrous indium trichloride with metallic luster, wherein the yield is 97%; the XRD detection result of the anhydrous indium trichloride is shown in figure 1, and the characteristic peak is calibrated: by comparing with standard PDF card, the characteristic peak of the sample and the InCl marked with blue vertical line3The characteristic peaks of the standard map are basically consistent, and the main component of the prepared sample is determined to be InCl3. The purity of the product is analyzed by an Inductively Coupled Plasma (ICP) method, a third-party detection mechanism with professional qualification is responsible for testing, and the obtained results are shown in the following table:
TABLE 1 content of impurity element in Anhydrous indium trichloride (unit: ppm)
Example 2:
under argon atmosphere, putting refined indium (with indium content of 99.995%) and hydrochloric acid (analytically pure hydrochloric acid with mass concentration of 38%) into a reaction kettle for dissolution, wherein the molar ratio of the refined indium to the hydrochloric acid is 1:7, and then dropwise adding n-butanol-n-heptane (with the volume ratio of 1:1) at the speed of 20mL/min under stirring, wherein the molar ratio of an organic solvent to indium is 30: 1; after reacting for 2h, refluxing for 6h at 80 ℃, evaporating low boiling point substances, then raising the temperature to 200 ℃, and decomposing the complex of the organic solvent and the indium trichloride to obtain white fluffy flake anhydrous indium trichloride with metallic luster, wherein the yield is 95%.
The purity of the product is analyzed by an Inductively Coupled Plasma (ICP) method, a third-party detection mechanism with professional qualification is responsible for testing, and the obtained results are shown in the following table:
TABLE 2 content of impurity element in anhydrous indium trichloride (unit: ppm)
Example 3:
under the mixed atmosphere of argon and hydrogen, putting refined indium (the indium content is 99.995%) and hydrochloric acid (analytically pure hydrochloric acid with the mass concentration of 36%) into a reaction kettle for dissolution, wherein the molar ratio of the refined indium to the hydrochloric acid is 1:10, and then dropwise adding dimethylformamide at the speed of 30mL/min under the stirring condition, wherein the molar ratio of the dimethylformamide to the indium is 35: 1; after reacting for 2h, refluxing for 6h at 100 ℃, evaporating low boiling point substances, and then raising the temperature to 300 ℃ to decompound the complex of dimethylformamide and indium trichloride to prepare white fluffy flake anhydrous indium trichloride with metallic luster, wherein the yield is 97%.
The purity of the product is analyzed by an Inductively Coupled Plasma (ICP) method, a third-party detection mechanism with professional qualification is responsible for testing, and the obtained results are shown in the following table:
TABLE 3 content of impurity element in anhydrous indium trichloride (unit: ppm)
Example 4:
under the mixed atmosphere of argon and hydrogen, refined indium (with the indium content being 99.995%) and hydrochloric acid (analytically pure hydrochloric acid with the mass concentration being 37%) are put into a reaction kettle for dissolution, the molar ratio of the refined indium to the hydrochloric acid is 1:6, then toluene is added dropwise at the speed of 15mL/min under the stirring condition, and the molar ratio of the toluene to the indium is 32: 1; after reacting for 2h, refluxing for 6h at 110 ℃, evaporating low boiling point substances, raising the temperature to 250 ℃ to decomplex the complex of toluene and indium trichloride, and obtaining white fluffy flake anhydrous indium trichloride with metallic luster, wherein the yield is 94%.
The purity of the product is analyzed by an Inductively Coupled Plasma (ICP) method, a third-party detection mechanism with professional qualification is responsible for testing, and the obtained results are shown in the following table:
TABLE 4 content of impurity element in Anhydrous indium trichloride (unit: ppm)
Claims (5)
1. A preparation method of high-purity anhydrous indium trichloride is characterized by comprising the following steps: under the protection of inert gas, taking refined indium and hydrochloric acid as raw materials, dropwise adding an organic solvent into the reaction raw materials while stirring, wherein the dropwise adding speed is 12-30 mL/min, and preparing a complex of the organic solvent and indium trichloride; after the reaction is finished, distilling to remove low boiling point substances, and then decomposing a complex of an organic solvent and indium trichloride to prepare high-purity anhydrous indium trichloride;
the organic solvent is one or two of dimethylformamide, n-butanol, n-heptane, kerosene and toluene at any ratio;
the decomplexing temperature is 120-300 ℃.
2. The method for preparing high-purity anhydrous indium trichloride as claimed in claim 1, wherein: the indium content of the refined indium is more than 99.995%, and the hydrochloric acid is analytically pure hydrochloric acid with the mass concentration of 36-38%.
3. The method for preparing high-purity anhydrous indium trichloride as claimed in claim 1, wherein: the mol ratio of the refined indium to the hydrochloric acid is 1: 4-10.
4. The method for preparing high-purity anhydrous indium trichloride as claimed in claim 1, wherein: the molar ratio of the organic solvent to the indium is 25-35: 1.
5. The method for preparing high-purity anhydrous indium trichloride as claimed in claim 1, wherein: the distillation temperature is 60-110 ℃.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101254942A (en) * | 2008-04-07 | 2008-09-03 | 昆明理工大学 | Method for preparing high-purity anhydrous indium trichloride |
| CN104310487A (en) * | 2014-09-30 | 2015-01-28 | 江西西林科股份有限公司 | Method for preparing anhydrous manganese chloride under anhydrous reaction conditions |
| JP2018016822A (en) * | 2016-07-25 | 2018-02-01 | 住友金属鉱山株式会社 | Production method of high purity indium |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101254942A (en) * | 2008-04-07 | 2008-09-03 | 昆明理工大学 | Method for preparing high-purity anhydrous indium trichloride |
| CN104310487A (en) * | 2014-09-30 | 2015-01-28 | 江西西林科股份有限公司 | Method for preparing anhydrous manganese chloride under anhydrous reaction conditions |
| JP2018016822A (en) * | 2016-07-25 | 2018-02-01 | 住友金属鉱山株式会社 | Production method of high purity indium |
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