A kind of jasmonal intermediate synthesis reaction post-processing method
A technology of synthesis reaction and post-processing, which is applied in the field of post-processing of jasmonal intermediate synthesis reaction, can solve problems such as difficulty in stirring, and achieve the effects of reducing side reactions, shortening length and facilitating installation.
Active Publication Date: 2018-09-21
福建仁宏医药化工有限公司
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[0011] The purpose of the present invention is to provide a technical solution for the post-processing method of the synthetic reaction of jasminal intermediate in view of the deficiencies in the prior art. more difficult questions
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[0032] like figure 1 Shown, be a kind of jasmonal intermediate synthetic reaction post-processing method of the present invention, comprise the steps:
[0033]1) First, add an auger 3 at the discharge port 7 below the bottom valve of the reactor 1, so that the feed port 8 of the auger 3 is aligned with the discharge port 7 of the reactor 1, and the feed port 8 is in line with the discharge port 7 of the reactor 1. The distance between the feed openings 7 is less than 5cm, and then the water analysis kettle 2 is set at the outlet end of the auger 3, and the water analysis kettle 2 is located 10-20 cm below the outlet end of the auger 3, and the auger 3 is made of acid-resistant material. It can effectively prevent concentrated sulfuric acid from corroding the inner wall of the auger 3 and the screw delivery rod 9, thereby affecting the normal operation of the auger 3. The auger 3 is equivalent to a continuous pipeline reactor with a stirring function and a heating function. By...
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The invention discloses an after-treatment method for heliotropin intermediate synthesis reaction. According to the after-treatment method, after pentamethyleneamine is dropwise added, a solid product is gradually generated in reaction mixed liquid and gradually becomes viscous, a bottom valve of a reaction kettle is switched on, materials are added into a packing auger, a motor is started, a hot water inlet / outlet of a jacket is opened, the materials are stirred by the packing auger and heated by hot water in the jacket, and the reaction is accelerated during the forward feeding of the materials and is finished when the materials are fed to an outlet of the packing auger; and the materials deviated from the packing auger enter an elutriation kettle, are continuously stirred for 15 minutes, are discharged and are centrifuged, a mother solution is neutralized, and the obtained filter residue is the reaction product 3,4-dioxymethylene mandelic acid. The after-treatment method has the beneficial effects that the structure is simple; by additionally arranging the packing auger, a continuous pipeline reactor is formed; and by regulating the rotation speed and the temperature of the hot water, the reaction mixture fed to the outlet of the packing auger just approaches or reaches a reaction endpoint, so that the problem that the stirring is difficult in the later period of the reaction is solved, and the large-scale industrial production can be smoothly realized by virtue of a process in which pentamethyleneamine and glyoxylic acid are utilized as main raw materials.
Description
technical field [0001] The invention relates to a post-treatment method for the synthetic reaction of a jasmonal intermediate. Background technique [0002] Jasmonal is also known as piperonal, heliopine, heliopine, pepper formaldehyde, oxidized piperonal, etc. Its chemical name is 3,4-methylenedioxybenzaldehyde, and its English name is: piperonal, helitropine, 3,4 -methylenedioxybenzaldehyde, whose structure is as follows: [0003] [0004] The molecular formula is: C 8 h 6 o 3 [0005] Molecular weight: 150.13 [0006] C: 64.00%, H: 4.03%, O: 31.97% [0007] The appearance of jasmonal is white shiny crystal, with a melting point of 37°C and a boiling point of 263°C; insoluble in water and glycerin, easily soluble in ethanol, ether, benzyl benzoate, diethyl phthalate, soluble in propylene glycol, in olive oil. Jasmonal is easy to change color under heat and light, and is stable in dilute acid and dilute alkali. [0008] Jasmonal is a very important intermediate ...
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IPC IPC(8): C07D317/60
CPCC07D317/60
Inventor 樊彬王国洪刘志铭黄京波林振洪朱次成
Owner 福建仁宏医药化工有限公司