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A method for analyzing and detecting benzothiazole and its derivatives in the production process of dibenzothiazole disulfide

A technology of dibenzothiazole disulfide and benzothiazole, which is applied to the simultaneous analysis and detection of benzothiazole, benzothiazol-2-one, and sodium benzothiazole-2-sulfinate to achieve reliable detection means, Improve peak shape and reduce tailing effect

Active Publication Date: 2022-06-07
CHEM TECH ACAD OF SHANDONG PROVINCE
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Simultaneous determination of benzothiazole-2-sodium sulfinate (BT-2-sodium sulfinate), 2-mercaptobenzothiazole (MBT), benzothiazol-2-one (BT-2- Ketone), benzothiazole (BT) methods have not been reported in the literature

Method used

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  • A method for analyzing and detecting benzothiazole and its derivatives in the production process of dibenzothiazole disulfide
  • A method for analyzing and detecting benzothiazole and its derivatives in the production process of dibenzothiazole disulfide
  • A method for analyzing and detecting benzothiazole and its derivatives in the production process of dibenzothiazole disulfide

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Experimental program
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Effect test

Embodiment 1

[0045] Example 1 (preferred conditions)

[0046] Using Shimadzu LC 2030C high performance liquid chromatograph, Hypersil Gold C18 (250mm×4.6mm, 5μm) chromatographic column;

[0047] Flow rate: 1.0mL / min;

[0048] Detector: diode array detector;

[0049] Detection wavelength: 220nm;

[0050] Column temperature: 30℃;

[0051] Injection volume: 10 μL;

[0052] Mobile phase: use methanol and 10mmol / L ammonium acetate as mobile phase A and mobile phase B, and separate by gradient elution. The gradient elution procedure is as follows, and the chromatogram of the standard solution is shown in figure 2 , see the sample solution chromatogram image 3 , Figure 4 .

[0053]

[0054]

[0055] figure 2Among them, the retention times of BT-2-sodium sulfinate, MBT, BT-2-ketone, and BT were 4.366min, 10.572min, 11.509min, and 12.387min, respectively, and the resolutions were all >1.5, which met the baseline separation requirements. Satisfactory results were also obtained in ...

Embodiment 2

[0057] extreme conditions 1

[0058] Using Shimadzu LC 2030C high performance liquid chromatograph, Hypersil Gold (250mm×4.6mm, 5μm) chromatographic column;

[0059] Flow rate: 1.0mL / min;

[0060] Detector: diode array detector;

[0061] Detection wavelength: 215nm;

[0062] Column temperature: 20℃;

[0063] Injection volume: 5μL;

[0064] Mobile phase: use methanol and 1mmol / L ammonium acetate as mobile phase A and mobile phase B, and separate by gradient elution. The gradient elution procedure is as follows, and the chromatogram of the eluent is shown in Figure 5 .

[0065] time, min Mobile phase A (methanol) Mobile phase B (1mmol / L ammonium acetate) 0 30 70 5 30 70 7 90 10 17 90 10 20 30 70 30 30 70

[0066] Figure 5 Among them, the retention times of BT-2-sodium sulfinate, MBT, BT-2-ketone, and BT were 4.497min, 9.606min, 11.720min, and 12.288min, respectively, and the separation degree was >1.5, which met the b...

Embodiment 3

[0077] Embodiment 3 (comparative test): common C18 chromatogram

[0078] Using Shimadzu LC 2030C high performance liquid chromatograph, Inertsil OSD-SP C18 (250mm×4.6mm, 5μm) chromatographic column;

[0079] Flow rate: 1.0mL / min;

[0080] Elution mode: gradient elution;

[0081] Detector: diode array detector;

[0082] Detection wavelength: 220nm;

[0083] Column temperature: 30℃;

[0084] Injection volume: 10 μL;

[0085] Mobile phase: use methanol and 10mmol / L ammonium acetate as mobile phase A and mobile phase B, and separate by gradient elution. The gradient elution procedure is as follows, and the chromatogram of the standard solution is shown in Figure 7 .

[0086] time, min Mobile phase A (methanol) Mobile phase B (10mmol / L ammonium acetate) 0 40 60 5 40 60 7 85 15 17 85 15 20 40 60 30 40 60

[0087] Depend on Figure 7 It can be seen that on the ordinary C18 chromatographic column without end-capping treatme...

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Abstract

The invention belongs to the technical field of analysis of benzothiazole and its derivatives, and specifically discloses an analysis and detection method for benzothiazole and its derivatives in the production process of dibenzothiazole disulfide (DM). The treated high-purity silica gel C18 chromatographic column is separated, and the diode array detector is detected, and the external standard method is used to determine benzothiazole-2-sodium sulfinate, 2-mercaptobenzothiazole, The content of benzothiazole-2-ketone, benzothiazole, etc. is for the control analysis of the dibenzothiazole disulfide synthesis process, the judgment of the reaction end point, the study of the reaction mechanism, the accumulation of impurities in the process of mechanical application and the determination of the limit value, And mother liquor purification treatment, wastewater monitoring process to provide determination methods.

Description

technical field [0001] The invention relates to the technical field of analysis of benzothiazole and derivatives thereof, in particular to sodium benzothiazole-2-sulfinate (BT-2-sodium sulfinate), 2- Simultaneous analysis and detection method for mercaptobenzothiazole (MBT), benzothiazol-2-one (BT-2-one) and benzothiazole (BT). Background technique [0002] Dibenzothiazole disulfide (DM), commonly known as accelerator DM, has the characteristics of fast vulcanization, flat vulcanization curve, and easy dispersion in rubber. , cable and other rubber manufacturing industries; at the same time, it can be used as a raw material for the synthesis of pharmaceutical intermediates. Since DM is one of the most widely used vulcanization accelerators at home and abroad, the annual domestic production capacity is about 40,000 tons. At present, the synthesis method of DM mainly uses 2-mercaptobenzothiazole (MBT / M) as raw material, and is obtained by oxidation with oxidant. Commonly us...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/64
CPCG01N30/02G01N30/06G01N30/64
Inventor 王瑞菲岳涛刘启奎付永丰王艳唐晓婵
Owner CHEM TECH ACAD OF SHANDONG PROVINCE
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