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
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[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 of t
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 syste
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: Transfe
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