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Method for directly analyzing content of 1,5-naphthalene diisocyanate by normal-phase high performance liquid chromatography

A high-performance liquid chromatography and naphthalene diisocyanate technology, applied in the field of direct analysis of 1,5-naphthalene diisocyanate, can solve problems such as harsh analysis conditions, achieve fast analysis speed, increase product yield, and accurate analysis results Effect

Inactive Publication Date: 2014-09-24
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] These existing instrumental analysis methods all need derivatization pretreatment, and the content of isocyanate cannot be directly measured. Therefore, ensuring that the derivatization reaction is complete and no side reactions occur during the derivatization process is the premise and condition for accurate analysis results. Analytical conditions are very harsh

Method used

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  • Method for directly analyzing content of 1,5-naphthalene diisocyanate by normal-phase high performance liquid chromatography
  • Method for directly analyzing content of 1,5-naphthalene diisocyanate by normal-phase high performance liquid chromatography
  • Method for directly analyzing content of 1,5-naphthalene diisocyanate by normal-phase high performance liquid chromatography

Examples

Experimental program
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Embodiment 1

[0032] Direct Quantitative Analysis of 1,5-Naphthalene Diisocyanate by Normal Phase High Performance Liquid Chromatography

[0033] 1.1 Chromatographic separation and detection conditions

[0034] Chromatographic column: Agilent ZORBAX CN, 5μm, 4.6×250mm

[0035] Mobile phase: n-hexane-dichloromethane-acetonitrile (volume ratio 70:20:10)

[0036] Flow rate: 1.0mL / min

[0037] Column temperature: 25°C

[0038] Detection wavelength of UV detector: 325nm

[0039] Injection volume: 20μL

[0040] 1.2 Preparation of standard solution and sample solution

[0041] Accurately weigh about 0.02g (accurate to 0.0001g) of 1,5-naphthalene diisocyanate standard sample into a 25mL brown volumetric flask, add dimethyl carbonate to dissolve and constant volume, and obtain standard sample 1 (original standard sample); Take 7mL of the original standard sample into a 10mL volumetric flask, add dimethyl carbonate to volume to obtain standard sample 2; take 5mL of the original standard sample ...

Embodiment 2

[0050] Intermediate Control Analysis Method for Synthesis of 1,5-Naphthalene Diisocyanate Reaction Solution Using 1,5-Naphthalene Diamine and Solid Phosgene as Raw Materials

[0051] Chromatographic separation and detection conditions are the same as in Example 1.

[0052] Accurately weigh about 0.01g (accurate to 0.0001g) of 1,5-naphthalenediamine in a 100mL brown volumetric flask, add dimethyl carbonate to make up to the mark. Analysis spectrum see image 3 .

[0053] Accurately weigh about 0.1g (accurate to 0.0001g) of 1,5-naphthalene diamine and solid phosgene as raw materials to synthesize the reaction solution of 1,5-naphthalene diisocyanate into a 100mL brown volumetric flask, add dimethyl carbonate to dissolve And constant volume, get the sample to be analyzed. For the analytical spectrum, see Figure 4 .

[0054] Under the selected chromatographic conditions, use the external standard method to qualitatively determine whether there are raw materials and products ...

Embodiment 3

[0056] Intermediate Control Analysis Method for Synthesis of 1,5-Naphthalene Diisocyanate Reaction Solution Using 1,5-Naphthalene Diamine and Solid Phosgene as Raw Materials

[0057] Except columns for Agilent ZORBAX NH 2 , 5 μm, 4.6 * 250mm, outside, others are all the same as embodiment 1.

[0058] Inject and analyze the reaction solution sample prepared in Example 2. Analysis spectrum see Figure 5 .

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Abstract

The invention discloses a method for directly analyzing content of 1,5-naphthalene diisocyanate by normal-phase high performance liquid chromatography. According to chromatography conditions, polar CN or NH2 bonded stationary phase is employed as a stationary phase and an n-hexane-dichloromethane-acetonitrile system with a water content being less than 0.05% or an n-hexane-ethyl acetate-acetonitrile system with a water content being less than 0.05% is employed as a mobile phase. The invention has following technical effects that the method can be directly applied in quantitative analysis of a 1,5-naphthalene diisocyanate product and has characteristics that the method is accurate in analysis result and quick in analysis speed and a sample is free of pre-treatment. Intermediate control analysis can be carried out for tracing a reaction progress of a reaction liquid in a reaction of synthesizing 1,5-naphthalene diisocyanate with 1,5-naphthalenediamine and bis(trichloromethyl)carbonate being raw materials. The method provides a basis for optimizing technological conditions in synthesis of 1,5-naphthalene diisocyanate and has important guiding significances in increase of product yield and economical benefit of enterprises.

Description

technical field [0001] The invention relates to an analysis method for directly analyzing 1,5-naphthalene diisocyanate. Background technique [0002] At present, the synthesis of 1,5-naphthalene diisocyanate mainly takes 1,5-naphthalene diamine and bis(trichloromethyl) carbonate as the solid phosgene method of raw materials, and the main reaction formula is as follows: [0003] [0004] Since 1,5-naphthalene diisocyanate is very sensitive to water, alcohols, amines, etc., it cannot be directly injected and analyzed by reversed-phase liquid chromatography, let alone intermediate control analysis of its production process to understand the reaction process, guide and optimize production process conditions. Therefore, it is of great significance to invent a method that can directly, quickly and accurately measure the content of 1,5-naphthalene diisocyanate. [0005] At present, the determination of isocyanate by liquid chromatography is mainly derivatized with alcohols or ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/50G01N30/36
Inventor 段正康曾航日王良芥艾秋红
Owner XIANGTAN UNIV