Search

CN-122016695-A - Method and device for detecting inorganic carbon in titanium tetrachloride

CN122016695ACN 122016695 ACN122016695 ACN 122016695ACN-122016695-A

Abstract

The invention discloses a method and a device for detecting inorganic carbon in titanium tetrachloride, wherein the method comprises the following steps of S1, taking a titanium tetrachloride sample, removing light components through rectification to separate organic carbon, concentrating inorganic carbon to obtain tower kettle concentrated solution, S2, weighing 0.1-1 g of tower kettle concentrated solution, burning in an oxygen-enriched environment at 1300-1500 ℃, detecting CO 2 by using an NDIR detector, S3, calculating the inorganic carbon content in the tower kettle concentrated solution according to a carbon content standard curve, and converting the inorganic carbon content in the titanium tetrachloride sample by combining a concentration factor. According to the invention, physical concentration of inorganic carbon is realized by evaporating the main solvent, the difficult problem of detecting trace inorganic carbon is solved, high-efficiency separation of organic carbon and inorganic carbon can be realized, and most of titanium tetrachloride main bodies can be evaporated and separated, so that inorganic carbon is highly concentrated in a small amount of residual liquid, thereby coupling carbon-sulfur analysis, realizing accurate and high-sensitivity detection of trace inorganic carbon, and the detection limit can reach ppb level.

Inventors

  • CHEN YONGJIE
  • ZHANG JIANBO
  • QIN ZHIFENG
  • WANG KUI

Assignees

  • 成都先进金属材料产业技术研究院股份有限公司

Dates

Publication Date
20260512
Application Date
20260410

Claims (10)

  1. 1. The method for detecting the inorganic carbon in the titanium tetrachloride is characterized by comprising the following steps of: S1, taking a titanium tetrachloride sample, removing light components by rectification, separating organic carbon and concentrating inorganic carbon to obtain tower kettle concentrated solution; S2, sampling the tower kettle concentrated solution and accurately quantifying inorganic carbon by adopting a carbon-sulfur analyzer.
  2. 2. The method for detecting inorganic carbon in titanium tetrachloride according to claim 1, wherein the distillation light component removal is performed by a distillation light component removal tower, which is a packed tower.
  3. 3. The method for detecting inorganic carbon in titanium tetrachloride according to claim 2, wherein the filler in the filler tower comprises one or more of a stainless steel theta ring filler with an external dimension of 2-15 mm, a triangular spiral filler with an external dimension of 2-15 mm, a quartz spring filler with an external dimension of 2-15 mm and a filler with an external dimension of 2-15 mm pfa.
  4. 4. The method for detecting inorganic carbon in titanium tetrachloride according to claim 2, wherein the material of the inner wall of the rectifying and light component removing tower comprises at least one of 316L stainless steel, titanium metal, hastelloy and quartz glass.
  5. 5. The method for detecting inorganic carbon in titanium tetrachloride according to claim 2, wherein the theoretical plate number of the rectifying and light component removing tower is 30 to 70.
  6. 6. The method for detecting inorganic carbon in titanium tetrachloride according to claim 1, wherein the rectifying and light component removing control tower bottom temperature is within a range of 120-150 ℃ and tower top temperature is controlled within a range of 60-120 ℃.
  7. 7. The method for detecting inorganic carbon in titanium tetrachloride according to claim 1, wherein the rectification and light component removal control reflux ratio is within a range of 10-40.
  8. 8. The method for detecting inorganic carbon in titanium tetrachloride according to claim 1, wherein step S2 comprises: establishing a carbon content standard curve by using the carbon-sulfur analyzer; weighing 0.1-1 g of the tower kettle concentrated solution, burning in an oxygen-enriched environment at 1300-1500 ℃, and detecting the concentration of CO 2 by using an NDIR detector of the carbon-sulfur analyzer; and calculating the inorganic carbon content in the tower kettle concentrated solution according to the carbon content standard curve and the concentration of CO 2 detected by the NDIR detector, and then combining a concentration factor to calculate the inorganic carbon content in the titanium tetrachloride sample.
  9. 9. The method for detecting inorganic carbon in titanium tetrachloride according to claim 1, wherein the concentration factor is a ratio of the mass of the titanium tetrachloride sample to the mass of the tower bottom concentrate.
  10. 10. A device for detecting inorganic carbon in titanium tetrachloride, which is used for carrying out the detection method according to any one of claims 1 to 9, and comprises a rectification light component removal tower and a carbon sulfur analyzer, wherein the rectification light component removal tower is provided with a rectification inlet, a rectification waste gas outlet and a rectification liquid outlet, the rectification waste gas outlet is arranged at the top of the rectification light component removal tower, and the rectification liquid outlet is arranged at the bottom of the rectification light component removal tower.

Description

Method and device for detecting inorganic carbon in titanium tetrachloride Technical Field The invention relates to the technical field of chemical analysis, in particular to a method and a device for detecting inorganic carbon in titanium tetrachloride. Background Titanium tetrachloride (TiCl 4) is a key precursor for the production of titanium sponge, titanium dioxide and semiconductor thin film materials, the purity of which directly affects the properties of the final product. Elemental carbon is one of the common impurities in titanium tetrachloride, and exists mainly in the form of organic carbon (e.g., CCl 3COCl、COCl2, etc.) and inorganic carbon (e.g., fine carbon powder, certain carbon chlorides, etc.). Wherein, inorganic carbon impurities are more difficult to remove in the subsequent process due to chemical inertness, particle characteristics and the like, and have great harm to the electrical property, uniformity and yield of the product. Currently, the detection of carbon content in titanium tetrachloride has focused on total or organic carbon. For example, chinese patent publication No. CN116046600a discloses a method for detecting carbon content in titanium tetrachloride by hydrolyzing, neutralizing, filtering a titanium tetrachloride sample to obtain a neutralized slag, and then detecting the carbon content in the neutralized slag using a carbon-sulfur instrument to calculate the total organic content. Although the method is relatively simple to operate, the method has obvious defects that 1) the method aims at detecting the total organic matter content, does not distinguish organic carbon from inorganic carbon (such as carbon powder, carbon chloride and the like), but inorganic carbon in titanium tetrachloride is more harmful to high-end application of semiconductors and the like, and needs to be independently and accurately monitored, and 2) the hydrolysis and neutralization methods can cause partial loss or conversion of volatile or soluble inorganic carbon to influence the detection accuracy. Chinese patent publication No. CN120685414a discloses a method for preparing and detecting total carbon content test solution in titanium tetrachloride, and total carbon is detected by hydrolysis, evaporating to dryness, dissolution in hydrofluoric acid, ICP-MS/OES. The method also cannot distinguish between organic and inorganic carbon. In addition, the pretreatment process involves the use of hydrofluoric acid, the danger is high, and the high-temperature evaporation and the strong acid environment can cause the loss or interference of part of inorganic carbon in a form, so that the process is relatively complex. The existing detection means has obvious defects in the aspect of accurately quantifying the inorganic carbon content, and is difficult to provide timely and accurate data support for inorganic carbon impurities in the production process. The unstable control of C element in fine TiCl 4 of the climbing steel sponge titanium production line becomes a key bottleneck for restricting the quality improvement of products, and the development of a method capable of accurately detecting the inorganic carbon content is urgent. In view of this, improvements should be made over the prior art. Disclosure of Invention The invention mainly aims to provide a method for detecting inorganic carbon in titanium tetrachloride, which realizes physical concentration of inorganic carbon by evaporating a main solvent, solves the difficult problem of detecting trace inorganic carbon, can realize efficient separation of organic carbon and inorganic carbon, and can enable inorganic carbon to be highly concentrated in a small amount of residual liquid by evaporating and separating most of titanium tetrachloride main bodies, thereby coupling carbon-sulfur analysis, realizing accurate and high-sensitivity detection of trace inorganic carbon, and the detection limit can reach ppb level. According to one aspect of the present invention, there is provided a method for detecting inorganic carbon in titanium tetrachloride, comprising the steps of: S1, taking a titanium tetrachloride sample, removing light components by rectification to separate organic carbon, and concentrating inorganic carbon to obtain tower kettle concentrated solution; S2, weighing 0.1-1 g of tower kettle concentrate, burning in an oxygen-enriched environment at 1300-1500 ℃, and detecting CO 2 by using an NDIR detector; S3, calculating the inorganic carbon content in the tower kettle concentrated solution according to a carbon content standard curve, and converting the inorganic carbon content in the titanium tetrachloride sample by combining a concentration factor. According to one embodiment of the invention, the rectifying and light component removal is performed by a rectifying and light component removal tower, and the rectifying and light component removal tower is a packed tower. According to one embodiment of the invention, the packing in the pa