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Method for determination of 2-isopropyl thioxanthone reaction intermediate content

A technology of isopropylthioxanthone and a determination method, which is applied in the field of chemistry, can solve the problems of no public detection method, irritating ammonia smell, and difficulty in controlling the input amount, and achieves stable and reliable results, analysis time period, quality Guaranteed effect

Active Publication Date: 2016-01-13
SHANDONG JIURI CHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

U.S. Patent US2003229233 discloses the detection of 2-chlorothiobenzoyl chloride by using HPLC to detect the reaction derivatives of 2-chlorothiobenzoyl chloride and ammonia gas. The detailed detection method is not disclosed, and the smell of ammonia gas is more irritating. Intake is difficult to control
[0005] So far, the detailed analysis and detection method of this intermediate has not been recorded in the literature, but the analysis and detection of this intermediate plays an important role in reaction control and yield improvement, and also directly affects the quality of the final product photoinitiator ITX. Therefore, it is very necessary to establish a fast, accurate, good separation effect, stable and effective analysis and detection method for quality control of this intermediate.

Method used

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  • Method for determination of 2-isopropyl thioxanthone reaction intermediate content
  • Method for determination of 2-isopropyl thioxanthone reaction intermediate content
  • Method for determination of 2-isopropyl thioxanthone reaction intermediate content

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Embodiment 1

[0023] Example 1 : Sample preparation

[0024] Wash the 10ml vials and syringes, dry them in an oven at 110°C for 2 hours, take them out immediately before use, plug them with rubber stoppers, and keep them cool for later use. Use a syringe to take the reaction intermediate 2-thiochlorobenzoyl chloride solution, which contains about 0.15g of acid chloride per 1ml, 0.73mmol in a vial, and then take 0.5ml of anhydrous n-butylamine (0.36g, 5mmol) In the vial, the syringe was drawn repeatedly 3 times, placed in an ultrasonic oscillator under normal pressure to react for 0.5 h, and the resulting reaction mixture was added to methanol until it was completely dissolved.

Embodiment 2

[0026] Instruments and conditions: Agilent 1200 liquid chromatography system, the chromatographic column adopts octadecylsilane bonded silica gel column; the ultraviolet detection wavelength is 254nm, methanol is the mobile phase, and the flow rate is 1.0ml / min.

[0027] Experimental procedure: take 50ul of the sample solution prepared in Example 1 and add it to the sample tube, add 3ml of methanol to the sample tube, shake it fully, filter out insoluble impurities, then take 10ul of the sample solution and carry out liquid chromatography analysis according to the above conditions, Record the chromatogram, see the attached results figure 1 .

[0028] attached figure 1 It shows that under this chromatographic condition, it can be completely separated, and the retention time of 2-butyl-1,2-benzisothiazolin-3-one, an intermediate derivative of 2-chlorothiobenzoyl chloride, is 3.04min.

Embodiment 3

[0030] Get another batch of reaction intermediate 2-thiochlorobenzoyl chloride solution, analyze according to the mode of embodiment 1 and example 2, the results are shown in the attached figure 2 .

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Abstract

The invention provides a method for determination of 2-isopropyl thioxanthone reaction intermediate content, and the method is used for quality control of 2-isopropyl thioxanthone. The method uses a chromatographic column using octadecylsilane bonded silica as a filler and uses methanol as a mobile phase to conduct HPLC analysis and detection at the flow rate of 0.7-1.1 ml / min and detection wavelength of 254 + / - 2 nm. The analysis detection method of the invention converts a reaction intermediate 2-chlorothio benzoyl chloride and n-butylamine into n-butyl-1,2-isothiazolin-3-ketone, and realizes indirect quality control of 2-isopropyl thioxanthone through derivative detection; and the method has the advantages of good repeatability, short analysis time, simple operation, and stable and reliable results.

Description

technical field [0001] The present invention relates to a method for determining the content of a 2-isopropylthioxanthone reaction intermediate, in particular to a 2-isopropylthioxanthone reaction intermediate 2-chlorothiobenzoyl chloride content The assay method belongs to the field of chemical technology. Background technique [0002] 2-Isopropylthioxanthone, referred to as photoinitiated ITX, is a high-efficiency free radical type II photoinitiator with an absorption wavelength of 258~382nm. It is suitable for photocurable materials composed of unsaturated polyester and acrylic monomers. , can be used for colorless or colored UV curing inks, wooden furniture, decorative paints and adhesives, etc. It can act as a sensitizer when used together with a cationic photoinitiator, and can also be used as a photosensitizer to enhance the curing performance of photoinitiator 907. Photoinitiated ITX-chlorothiobenzoyl chloride preparation process is as follows: [0003] [0004...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 吴吉蒋雷韩时操凌爱祥周海兵敖文亮张齐毛桂红罗想
Owner SHANDONG JIURI CHEM TECH CO LTD