Reaction kettle for preparing aldehyde by hydrolyzing fluorine-containing aromatic hydrocarbon cross benzyl chloride

Abstract

The reaction kettle comprises a reaction kettle body made of a glass lining material, a kettle cover made of a glass lining material and a stirrer system, a polytetrafluoroethylene coating is arranged on the surface of the side, in contact with materials, of the kettle cover, a polytetrafluoroethylene winding short section is arranged on the inner side of the reaction kettle body, and the kettle cover is connected with the stirrer system through a pipeline. And the length of the polytetrafluoroethylene winding short section is 1 / 2 of the height of the reaction kettle body. Aiming at the problems of the conventional hydroformylation hydrolysis kettle, the problem of corrosion is solved by adding the polytetrafluoroethylene coating on the part, which does not need heating or heat exchange, of the kettle cover in contact with a material, and the problem of corrosion is solved by adding the polytetrafluoroethylene winding short section on the part, which needs heating or heat exchange, of the reaction kettle body in contact with a liquid material. The reaction kettle body is prevented from being in contact with a gas-phase material with strong corrosivity and strong oxidizing property, and the corrosion resistance is remarkably improved, so that the service life of the reaction kettle is prolonged, the product quality is improved, and material polymerization accidents are reduced.

Description

TECHNICAL FIELD

[0001] The utility model belongs to the technical field of chemical equipment relates to the reaction kettle especially under the aldehyde hydrolysis reaction of fluorine-containing aromatic hydrocarbon fork chlorobenzyl hydrolysis preparation aldehyde's reaction kettle suitable for high corrosive environment. BACKGROUND

[0002] 2-chloro-6-fluorobenzaldehyde is the key intermediate of human antibiotic sodium flucloxacillin, and there are two production routes, the first route is to take 3-chloro-2-methyl aniline as raw material, through diazo reaction and fluorination reaction, 2-chloro-6-fluorotoluene is prepared, then through photochlorination reaction, rectification and hydrolysis process route, the second route is to take toluene as raw material, through chlorination reaction and rectification, 2,6-dichlorotoluene is prepared, then through fluorination reaction and rectification, 2-chloro-6-fluorotoluene is obtained, and finally through photochlorination reaction, rectification and hydrolysis process route.

[0003] The two process routes have their own advantages, but since the drug has strict control requirements for impurities, the related impurities in the second production route are difficult to control, and the conversion efficiency is also very low, which has no actual industrial value, and at present, the first production route is used for production at home and abroad.

[0004] 2,6-dichlorobenzaldehyde is a key raw material for synthesizing dieloxaeillinsodium, and dieloxaeillinsodium is a semi-synthetic beta-lactam penicillin, mainly used for staphylococcus infection resistant to penicillin, including septicemia, endocarditis, bone osteomyelitis, respiratory tract infection and wound infection, etc. Compared with penicillin G, the antibacterial effect on pneumococcus is 1 / 3 of penicillin G, and the antibacterial effect on other gram-positive bacteria not producing penicillinase is 1 / 15-1 / 3. The antibacterial effect on drug-resistant bacteria is 100 times stronger than that of penicillin G. The Staphylococcus aureus resistant to oxacillin or cloxacillin is sensitive to the product.

[0005] The production process route and production device of 2,6-dichlorobenzaldehyde are basically the same as those of 2-chloro-6-fluorobenzaldehyde, taking 2,6-dichlorotoluene as raw material, through chlorination, degassing and rectification, 2,6-dichlorobenzaldehyde is obtained, and then through catalytic hydrolysis, 2,6-dichlorobenzaldehyde is obtained.

[0006] In the catalytic hydrolysis process, due to high-temperature hydrolysis under high-concentration sulfuric acid or a mixed system of sulfuric acid and Lewis acid, the material in the system has strong oxidizing property and acidity, and side reactions are prone to occur in the hydrolysis process, fluoride ions are separated to form hydrogen fluoride which has strong corrosiveness to enamel, and the reaction kettle for preparing aldehyde by hydrolysis is often seriously corroded in less than 3 months in production, especially the manhole, gas phase pipe, raw material dropping port and stirring machine mounting port on the kettle cover are easily corroded and perforated, causing the equipment to be scrapped, and the polymerization of the material is prone to cause production accidents, which is dangerous. Content of the utility model

[0007] In order to solve the above problems, the utility model provides a reaction kettle for preparing aldehyde by hydrolysis of fluorine-containing aromatic hydrocarbon chlorobenzyl, the reaction kettle has the characteristics of simple and reasonable structure, low cost and long service life, does not affect the function of the original equipment, prolongs the service life of the reaction kettle, improves the product quality and reduces the occurrence of polymerization accidents.

[0008] In order to achieve the above object, the utility model adopts the following technical scheme:

[0009] The utility model provides a reaction kettle for preparing aldehyde by hydrolysis of fluorine-containing aromatic hydrocarbon chlorobenzyl, including the reaction kettle body made of enamel material, the kettle cover and the stirrer system made of enamel material, one side surface of the kettle cover in contact with the material is provided with a polytetrafluoroethylene coating, the inner side of the reaction kettle body is provided with a polytetrafluoroethylene winding short section, and the length of the polytetrafluoroethylene winding short section is 1 / 2 of the height of the reaction kettle body.

[0010] As a preferred scheme of the utility model, the kettle cover is provided with a thermometer mounting port, a manhole, a first flange, a gas phase pipe port, a nitrogen replacement port, a raw material dropping port, a bursting disc mounting port, a pressure gauge mounting port and a stirring machine mounting port; the reaction kettle body is provided with a second flange, a jacket cooling water outlet, a steam condensate water outlet, a discharge port, a jacket cooling water inlet and a jacket steam inlet.

[0011] As a preferred scheme of the utility model, the polytetrafluoroethylene winding short section is inserted into the reaction kettle body from top to bottom, the end of the polytetrafluoroethylene winding short section overlaps the second flange, and is fixed and sealed through a Haifu.

[0012] As a preferred scheme of the utility model, the stirrer system includes a stirring paddle, a stirring shaft made of enamel material, a stirring machine frame and a driving motor, and the upper half of the shaft surface of the stirring shaft is provided with a polytetrafluoroethylene coating.

[0013] As a preferred scheme of the utility model, a flange gasket is arranged between the first flange and the second flange.

[0014] As a preferred scheme of the utility model, the thermometer installation port is equipped with a thermometer insertion tube made of glass lining material.

[0015] As a preferred scheme of the utility model, the thermometer insertion tube penetrates into the reaction kettle body from the thermometer installation port, and the upper part of the thermometer insertion tube, which is not in contact with the material, is provided with a polytetrafluoroethylene coating.

[0016] As a preferred scheme of the utility model, the raw material drop adding port is equipped with a second polytetrafluoroethylene winding short section, and the gas phase pipe port is equipped with a third polytetrafluoroethylene winding short section.

[0017] Compared with the prior art, the utility model has the following beneficial effects:

[0018] 1. The utility model is aimed at the problems existing in the conventional aldehyde hydrolysis kettle, and the polytetrafluoroethylene coating is added to the kettle cover and the material contact part which does not need to be heated or heat exchanged to solve the corrosion problem.

[0019] 2. The utility model adds the polytetrafluoroethylene winding short section to the reaction kettle body which does not contact with the liquid material, thereby preventing the reaction kettle body from contacting with the gas phase material which has strong corrosion and strong oxidation, significantly improving the corrosion resistance, thereby prolonging the service life of the reaction kettle, improving the product quality, and reducing the occurrence of material polymerization accidents.

[0020] 3. The polytetrafluoroethylene winding short section of the utility model separates the gas phase corrosion medium from the kettle body, reduces the erosion of hydrogen fluoride to the glass lining, has reasonable structure design, prolongs the service life of the equipment to more than 12 months, and reduces the maintenance cost and the production accident risk. DRAWINGS

[0021] In order to more clearly illustrate the technical scheme in the embodiments of the present application or the prior art, the drawings needed to be used in the embodiment or the prior art description will be briefly introduced as follows. Obviously, the drawings in the following description are only some embodiments of the present application, and other drawings can be obtained by those skilled in the art without creative labor.

[0022] Figure 1 It is a structural schematic view of the utility model.

[0023] Figure 2 It is a top view of the kettle cover of the utility model.

[0024] Figure 3 It is a schematic view of the polytetrafluoroethylene winding short section of the utility model.

[0025] Figure 4 It is a front view of the kettle cover of the utility model.

[0026] In the figure: 1. kettle cover; 2. reaction figure body; 3. stirring shaft; 4. stirring paddle; 5. polytetrafluoroethylene coating coating; 6. driving motor; 7. polytetrafluoroethylene winding short section; 8. stirring frame; 9. thermometer installation mouth; 10. thermometer insertion tube; 11. manhole mouth; 12. harrow; 13-1. first flange; 13-2. second flange; 14. flange gasket; 15. jacket cooling water outlet; 16. steam condensate outlet; 17. discharge port; 18. jacket cooling water inlet; 19. jacket steam inlet; 20. nitrogen replacement mouth; 21. raw material drop adding mouth; 22. bursting disc installation mouth; 23. pressure gauge installation mouth; 24. stirrer installation mouth; 25. second polytetrafluoroethylene winding short section; 26. third polytetrafluoroethylene winding short section; 27. gas phase pipe mouth. DETAILED DESCRIPTION

[0027] In order to further understand the content of the present application, the present application will be described in detail in combination with the drawings and examples.

[0028] The present application will be further described in detail below with reference to the accompanying drawings and embodiments. It is understood that the specific embodiments described herein are merely illustrative of the relevant utility model and not intended to limit the utility model. Furthermore, it should be noted that, for ease of description, only the parts related to the utility model are shown in the accompanying drawings. The terms "first," "second," etc., used in this utility model are provided for the convenience of describing the technical solution of this utility model and have no specific limiting effect; they are all general terms and do not constitute a limitation on the technical solution of this utility model. It should be noted that, in the absence of conflict, the embodiments and features in the embodiments of this application can be combined with each other. In the description of this utility model, it should be noted that the terms "center," "upper," "lower," "left," "right," "vertical," "horizontal," "inner," and "outer," etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings, and are only for the convenience of describing the utility model and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation, and therefore should not be construed as a limitation on this utility model. In addition, the terms "first," "second," and "third" are used for descriptive purposes only and should not be construed as indicating or implying relative importance. Unless otherwise explicitly specified and limited, the terms "installation," "connection," and "linking" should be interpreted broadly. For example, they can refer to fixed connections, detachable connections, or integral connections; they can refer to mechanical connections or electrical connections; they can refer to direct connections or indirect connections through an intermediate medium; and they can refer to the internal connection of two components. Those skilled in the art can understand the specific meaning of the above terms in this utility model based on the specific circumstances. Multiple technical solutions in the same embodiment, as well as multiple technical solutions in different embodiments, can be arranged and combined to form new technical solutions that do not contradict or conflict, all of which are within the scope of protection claimed by this utility model.

[0029] Example 1

[0030] Combined with appendix Figures 1-4 This embodiment provides a reaction vessel for the hydrolysis of fluorinated aromatic hydrocarbon benzyl chloride to prepare aldehydes, including a vessel cover 1, a reaction vessel body 2, and a stirrer system.

[0031] Furthermore, the lid 1 includes:

[0032] The thermometer mounting port 9, manhole port 11, first flange 13-1, jacketed steam inlet 19, nitrogen replacement port 20, raw material dripping port 21, rupture disc mounting port 22, pressure gauge mounting port 23 and mixer mounting port 24, the kettle cover 1 is made of glass enamel, and the part in contact with the material is coated with polytetrafluoroethylene coating 5.

[0033] Furthermore, the reaction vessel body 2 includes:

[0034] The second flange 13-2, the jacket cooling water outlet 15, the steam condensate outlet 16, the discharge port 17, the jacket cooling water inlet 18 and the jacket steam inlet 19 are made of glass lining.

[0035] Further, the stirrer system comprises:

[0036] The stirring impeller 4, the stirring shaft 3, the stirring frame 8 and the driving motor 6, the stirring frame 8 comprising a speed reducer and a mechanical seal.

[0037] Further, the polytetrafluoroethylene winding short section 7 is inserted into the reactor body 2 from top to bottom, the end of the polytetrafluoroethylene winding short section 7 and the second flange 13-2 partially overlap, and a Haifu 12 is used for fixed sealing, and the length of the polytetrafluoroethylene winding short section 7 is 1 / 2 of the height of the reactor body 2.

[0038] Further, the stirring shaft 3 is made of glass lining and is inserted between the mechanical seal and the reactor body 2, and the upper half of the shaft surface of the stirring shaft 3 is sprayed with a polytetrafluoroethylene coating 5.

[0039] Further, the thermometer insertion tube 10 penetrates into the reactor body 2 from the thermometer installation port 9, the thermometer insertion tube 10 is made of glass lining, and the upper part of the thermometer insertion tube 10 which does not contact the liquid material is sprayed with a polytetrafluoroethylene coating 5.

[0040] Further, the second polytetrafluoroethylene winding short section 25 is inserted into the raw material dropping port 21, and the third polytetrafluoroethylene winding short section 26 is inserted into the gas phase pipe port 27.

[0041] In specific use, when hydrolysis of fluorine-containing aromatic hydrocarbon chlorobenzyl is carried out to prepare aldehyde, first, the catalyst sulfuric acid or the mixture of sulfuric acid and Lewis acid is put into the reactor body 2 through the raw material dropping port 21, the steam valve is opened, and the steam is used to heat the material through the jacket steam inlet 19; when the temperature of the material reaches a specified value, the fluorine-containing aromatic hydrocarbon chlorobenzyl is added into the reactor body 2 through the raw material dropping port 21 for hydrolysis reaction, the hydrogen chloride gas produced in the reaction is introduced into the condenser through the gas phase pipe port 27 and the pipeline, the condensed water (hydrochloric acid) is returned to the reactor body 2 through the pipeline and the gas phase pipe port 27, the raw material dropping is completed, the heat preservation reaction is continued, and the reaction is ended; the material after the reaction is discharged through the discharge port 17 and is put into a post-treatment process, an organic phase is separated, and the organic phase is subjected to alkali washing, water washing and distillation to obtain the fluorine-containing aromatic aldehyde product.

[0042] The above describes the utility model and its embodiments in a schematic manner, and the description is not restrictive, and the drawings only show one of the embodiments of the utility model, and the actual structure is not limited thereto. Therefore, if a person of ordinary skill in the art is inspired thereby, without departing from the creative concept of the utility model, similar structural modes and embodiments are designed without creativity, and all should belong to the protection scope of the utility model.

Claims

1. A reactor for the hydrolysis of a fluorine-containing aromatic arylidene chlorobenzene to produce an aldehyde, characterized in that, The glass-lined reaction kettle body, the glass-lined kettle cover and the stirrer system, the surface of the side of the kettle cover in contact with the material is provided with a polytetrafluoroethylene coating, the inside of the reaction kettle body is provided with a polytetrafluoroethylene winding short section, and the length of the polytetrafluoroethylene winding short section is 1 / 2 of the height of the reaction kettle body.

2. The fluorine-containing aromatic hydrocarbon chloroformyl benzyl hydrolysis aldehyde preparation reaction kettle according to claim 1, characterized in that, The kettle cover is provided with a thermometer mounting port, a manhole, a first flange, a gas phase pipe port, a nitrogen replacement port, a raw material dropping port, a bursting disc mounting port, a pressure gauge mounting port and a stirrer mounting port; the reaction kettle body is provided with a second flange, a jacket cooling water outlet, a steam condensate outlet, a discharge port, a jacket cooling water inlet and a jacket steam inlet.

3. The reactor for hydrolysis of chlorofluoroaromatic benzylidene chloride to aldehyde according to claim 2, characterized in that, The polytetrafluoroethylene winding short section is inserted into the reaction kettle body from top to bottom, the end of the polytetrafluoroethylene winding short section overlaps with the second flange, and the sealing is fixed by a Haifu.

4. The fluorine-containing aromatic hydrocarbon reaction kettle for preparing aldehyde by hydrolyzing chlorobenzylidene according to claim 1, characterized in that, The stirrer system comprises a stirring paddle, a stirring shaft made of glass-lined material, a stirring frame and a driving motor, and the upper half of the shaft surface of the stirring shaft is provided with a polytetrafluoroethylene coating.

5. The fluorine-containing aromatic hydrocarbon chloroformyl benzyl hydrolysis aldehyde preparation reaction kettle according to claim 2, characterized in that, The first flange and the second flange are provided with a flange gasket.

6. The fluorine-containing aromatic hydrocarbon chloroformyl benzyl hydrolysis aldehyde preparation reaction kettle according to claim 1, characterized in that, The thermometer mounting port is provided with a thermometer insertion tube made of glass-lined material.

7. The reactor for hydrolysis of chlorofluoroaromatic benzylidene chloride to aldehyde according to claim 4, characterized in that, The thermometer insertion tube penetrates into the reaction kettle body from the thermometer mounting port, and the upper part of the thermometer insertion tube which is not in contact with the material is provided with a polytetrafluoroethylene coating.

8. The fluorine-containing aromatic hydrocarbon chloroformyl benzyl hydrolysis aldehyde preparation reaction kettle according to claim 1, characterized in that, The raw material dropping port is provided with a second polytetrafluoroethylene winding short section, and the gas phase pipe port is provided with a third polytetrafluoroethylene winding short section.

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