Preparation method of high-whiteness thermosensitive color developing agent containing sulfonylurea structure

A technology containing sulfonylurea and high whiteness, which is applied in the field of preparation of heat-sensitive developer, which can solve the problem that the purity of color developer and whiteness affect the quality of thermal paper, the preparation process is cumbersome and complicated, and the heat-sensitive paper is dark. problems, to achieve the effect of preventing poor color, improving the purity of filter cake, and preventing oxidation and discoloration

Pending Publication Date: 2022-03-01
HEBEI JIANXIN CHEM IND CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Since the production process of thermal paper is to directly compound and coat the color developer, color coupler, stabilizer and other functional components on the surface of the paper base, the entire use process does not involve the color developer purification or similar purification process, so the obvious The purity and whiteness of the colorant will directly affect the quality of thermal paper; at the same time, in industrial production, since most of the sulfonylurea color developers are synthesized in a highly polar solvent, the residual solvent will cause the color d

Method used

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  • Preparation method of high-whiteness thermosensitive color developing agent containing sulfonylurea structure
  • Preparation method of high-whiteness thermosensitive color developing agent containing sulfonylurea structure

Examples

Experimental program
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Effect test

Example Embodiment

[0030] Example 1

[0031] One-step reaction: access N in the reactor 1 2 After the air was transferred, 500 L DMAC was added, stirred and stirred, adding 272.75 kg (2.50 kmol) amino phenol (MAP), dissolved at 40 ° C, slowly added 517.65 kg (2.63 kmol) of toluenesulfonyl isocyanate (PTSI), The dropwise addition of 2.5 h, 40 ° C for insulation, and the insulation is 2 hours to reach the end point.

[0032] Two-step reaction: Configuration of toluenesulfonyl chloride (PTSC): 524.42 kg (2.75 kmol) PTSC was dissolved in 525 L DMAC.

[0033] Transfer the material in the reactor 1 to N 2 In the reaction kettle 2 of the atmosphere, 10% NaOH solution 1196 kg (2.99 kmol) is pumped in the reaction kettle 2, the system pH = 10-11, and the DMAC solution of toluenesulfonyl chloride (PTSC) is slowly added drop. % NaOH is dissolved 300kg (2.25 kmol) to ensure that the system pH = 10-11, the temperature is between 40-60 ° C, the dropwise time is 1.0 h, and the insulation 1H reaches the end point o...

Example Embodiment

[0038] Example 2

[0039] One-step reaction: access N in the reactor 1 2After the air was returned, 750 L DMAC was added, stirred, and 272.75 kg (2.50 kmol) amino phenol (Map) was added, and 542.3 kg (2.75 kmol) of toluenesulfonyl isocyanate (PTSI) was slowly added dropwise. Take the dropwise time of 3.5 h, 30 ° C for insulation, and the insulation was 1.5 hours arrived at the end.

[0040] Two-step reaction: Configuration of toluenesulfonyl chloride (PTSC): 572.10 kg (3.00 kmol) PTSC was dissolved in 720l DMAC.

[0041] Transfer the material in the reactor 1 to N 2 In the atmosphere of the reaction kettle 2, a 20% NaOH solution was pumped in the reaction kettle 2, the system pH = 10-11, and the DMAC solution of toluenesulfonyl chloride (PTSC) was slowly added drop. % NaOH is 513.31kg (2.57kmol) to ensure that the system pH = 10-11, between 40-60 ° C, the dropwise time is 1.5 h, and the insulation 1H reaches the end point of the reaction.

[0042] Socket: Transfer the reactor 2 sy...

Example Embodiment

[0046] Example 3

[0047] One-step reaction: access N in the reactor 1 2 After the air was replaced, 1000 L DMAC was added, stirred, and 272.75 kg (2.50 kmol) amino phenol (MAP) was added, and 566.95 kg (2.88 kmol) of toluenesulfonyl isocyanate (PTSI) was slowly added dropwise. The dropped time was 4.0 h, and the insulation was carried out at 30 ° C, and the temperature was 1 h to the end point.

[0048] Two-step reaction: Configuration of toluenesulfonyl chloride (PTSC): 619.78 kg (3.25 kmol) PTSC was dissolved in 900l DMAC.

[0049] Transfer the material in the reactor 1 to N 2 In the reaction kettle 2, 15% Na is pumped in the reactor 2. 2 CO 3 The solution is 1060 kg (1.5 kmol), the system pH = 10-11, slowly added DMAC solution of toluenesulfonyl chloride (PTSC) while dripping 40% NaOH 280kg (2.80 kmol) to ensure the system pH = 10-11, temperature It was between 40-60 ° C, the dropwise time was 1.5 h, and the insulation 1 h reached the end of the reaction.

[0050] Socket: Tran...

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Abstract

A preparation method of a high-whiteness thermosensitive color developing agent containing a sulfonylurea structure comprises the following steps: dissolving MAP in an organic solvent, slowly dropwise adding PTSI into the organic solvent, and carrying out heat preservation to a reaction endpoint to obtain an intermediate product N-p-toluenesulfonyl-N '-(3-hydroxyphenyl) urea system; adding alkali liquor into the obtained intermediate product system for dissolving, then slowly dropwise adding an organic solution of PTSC, simultaneously dropwise adding the alkali liquor to control the pH value of the system, and carrying out heat preservation reaction to the end point to obtain a product N-p-toluenesulfonyl-N '-(3-p-toluenesulfonyloxyphenyl) urea system; adding an alcohol solvent into the prepared N-p-toluenesulfonyl-N-(3-p-toluenesulfonyloxy phenyl) urea system, neutralizing with acid, and filtering to obtain a filter cake; and carrying out post-treatment and vacuum drying on the filter cake to obtain a final product. According to the preparation method disclosed by the invention, the sulfonylurea color developing agent with high yield, high purity, whiter color and less solvent residue can be obtained, and the process operation is more suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation method of a heat-sensitive color developer, in particular to a preparation method of a high-whiteness heat-sensitive color developer containing a sulfonylurea structure. Background technique [0002] N-p-toluenesulfonyl-N'-(3-p-toluenesulfonyloxyphenyl) urea is a new type of thermosensitive chromogenic agent, which releases hydrogen ions (H + ) to make the heat-sensitive coupler color base develop color. Compared with the carcinogenic phenolic coupler, which is controversial in terms of carcinogenicity, its photostability is higher, and the image is more suitable for long-term storage. [0003] In recent years, the research on N-p-toluenesulfonyl-N'-(3-p-toluenesulfonyloxyphenyl) urea only focuses on the research on the preparation method, and there is little research on the post-treatment of the target product. [0004] Since the production process of thermal paper is to directly compound and coat the color deve...

Claims

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Application Information

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IPC IPC(8): C07C303/38C07C311/60C07C303/40C07C303/36C07C303/44
CPCC07C303/38C07C303/40C07C303/36C07C303/44C07C311/60Y02P20/55
Inventor 刘佳伟张静朱秀全王成鹏
Owner HEBEI JIANXIN CHEM IND CO LTD
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