CN205473476U - Production system to hydroxybenzaldehyde - Google Patents

Abstract

The utility model discloses a production system to hydroxybenzaldehyde, including consecutive reation kettle, stills, first filter, acidizing cauldron, first crystallization kettle, a centrifuge, decoloration cauldron, second filter, second crystallization kettle, the 2nd centrifuge and flash drying machine. The utility model discloses carry out further decoloration and refined crystallization process to thick product, the product that obtains has higher purity, waste gas, waste water and waste residue and then discharge after all concentrating and handling, and be very little to the pollution of environment, still have advantages such as yield height, easy operation.

Description

A kind of production system of hydroxy benzaldehyde

Technical field

This utility model relates to the production system of a kind of hydroxy benzaldehyde.

Background technology

Hydroxy benzaldehyde is a kind of highly important fine-chemical intermediate, be widely used in spice, medicine, The fields such as pesticide, cosmetics, plating.Such as, anisic aldehyde, chinese cymbidium can be synthesized with hydroxy benzaldehyde The much precious spice such as element, heliotropin, syringic aldehyde, fennel and Fructus Rubi.Para hydroxybenzene in terms of medicine Formaldehyde be mainly used in synthetic antimicrobial synergist TMP, hydroxyl ampicillin, hydroxyl benzyl head satisfy Mycin, TMB, to hydroximethanon glucose, D-pHPG, expectorant farrerol, Artificial Rhizoma Gastrodiae, esmolol etc. it can also be used to synthesize anti-high-pressure medicine, antihyperlipidemic, cardiovascular disease etc., Treatment dermatosis and the medicine etc. of ophthalmic.Agriculturally, the halogenide of hydroxy benzaldehyde can synthesize enemy's grass Nitrile and Brominal, they use conveniently, and production technology is simple, and low cost, is a kind of rising Herbicide.Can be with synthetic pesticide, biocide, fungistat, disinfection preservative with hydroxy benzaldehyde Deng intermediate.The halogenide of hydroxy benzaldehyde, whether a halides or dihalo thing, all have and press down The function of growth of microorganism processed, can be used for the biocide of medicine etc., the most especially with 3, and 5-bis-chloro-4-hydroxy benzenes The bactericidal action of formaldehyde is maximally efficient.Hydroxy benzaldehyde and its methyl ester p-anisaldehyde increase for alkaline zinc plating Bright, all can play brightener and the effect of even varnish at non-cyanogen with having in cyanogen plating.

The method of industrial synthesis hydroxy benzaldehyde is a lot.Patent 1 (application number: 201310206481.7) Utilize mixed phenol to prepare hydroxy benzaldehyde and m-hydroxybenzaldehyde, relate to the product separation process of complexity.This is special Profit makes crude product be layered by adding the water of 13～15 times of mixed phenol inventorys, is subsequently adding 1.5～3 times of aqueous phases The ethyl acetate of amount extracts, and saturated aqueous common salt washs, distillation removing ethyl acetate, obtains para hydroxybenzene Formaldehyde crude product.Crude product is dissolved by the benzene amount of 3～5 times amount finally adding crude product, purification.For terrible To pure hydroxy benzaldehyde, this patent employs substantial amounts of organic solvent ethyl acetate and has bigger poison Property benzene, environmental pollution is big, relatively costly.Patent 2 (application number: 201210534372.3) prepare right Substantial amounts of toluene and dimethylformamide (DMF) is employed as solvent, cost during hydroxy benzaldehyde Higher, and environmental pollution is serious.Only be by simply washing after product synthesis, separatory, desolventizing, dry Dry, obtain faint yellow solid, it is difficult to the hydroxy benzaldehyde that preparation purity is high.Patent 3 (application number: 200810060216.1) use the chloroform that toxicity is bigger to synthesize hydroxy benzaldehyde as organic solvent, slightly produce Thing is that product purity is relatively low, and environmental pollution is big through simple recrystallization.Patent 4 (application number: 201310076288.6) with substituted benzimidazole or substituted imidazoline as raw material, through metallic sodium-ethanol also Former, acidic hydrolysis, synthesize hydroxy benzaldehyde.The method raw material mix is complicated, is not easy to obtain, relatively costly, Cannot be used for industrialized production.Patent 5 (application number: 200910243127.5) uses metalloporphyrin as urging Agent, catalysis oxidation p-cresol prepares hydroxy benzaldehyde.The catalyst structure of this patent report is complicated, Preparation difficulty, it is difficult to carry out large-scale production.

But, the production system used by the above method the most all exists that product yield is low, purity is low, ring Environment pollution is serious, equipment investment is big, product separates the problems such as difficulty.

Summary of the invention

The shortcoming that this utility model aims to overcome that above-mentioned technology, it is provided that the production of a kind of hydroxy benzaldehyde System.

This utility model solves technical problem and be the technical scheme is that a kind of hydroxy benzaldehyde produces work The production system of skill, described production system include reactor, distillating still, the first filter, acidifying still, the One crystallization kettle, the first centrifuge, decolouring still, the second filter, the second crystallization kettle, the second centrifuge and sudden strain of a muscle Steam drying machine；Some raw material storage tanks and oxygen inlet, the discharging opening of described reactor it is connected with on described reactor Being connected with the charging aperture of described distillating still, described distillating still is provided with distillation assembly and the first water inlet, described Material outlet in distillation assembly is connected with described reactor, the discharging opening of described distillating still and described first mistake The charging aperture of filter is connected, and the discharging opening of described first filter is connected with the charging aperture of described acidifying still, institute State and be connected with hydrochloric acid tank on acidifying still, the charging aperture phase of the discharging opening of described acidifying still and described first crystallization kettle Even, the discharging opening of described first crystallization kettle is connected with described first centrifuge, the solid phase of described first centrifuge Discharging opening is connected with the charging aperture of described decolouring still, and described decolouring still is provided with activated carbon storage tank and the second water inlet Mouthful, the discharging opening of described decolouring still is connected with the charging aperture of described second filter, described second filter Discharging opening is connected with the charging aperture of described second crystallization kettle, the discharging opening of described second crystallization kettle and described second The charging aperture of centrifuge is connected, and the solid phase discharging opening of described second centrifuge is connected with described flash dryer.

Further, the some raw material storage tanks on described reactor include methanol tank, sodium hydroxide storage tank, P-methyl phenol storage tank and cobaltous acetate storage tank.

Further, in described distillation assembly, be provided with Methanol Recovery storage tank, described Methanol Recovery storage tank with Described methanol tank is connected.

Further, described reactor is provided with waste gas outlet, described first centrifuge and the second centrifuge On be equipped with wastewater outlet, described first filter and the second filter are equipped with waste residue outlet；Described Waste gas outlet, wastewater outlet and waste residue outlet are connected to three-protection design system.

The beneficial effects of the utility model are: compared with prior art, the para hydroxybenzene that this utility model provides In the production technology of formaldehyde and production system thereof, the thick product of hydroxy benzaldehyde is carried out further activity Carbon decoloring and refining crystallization process, and the product obtained has higher purity；Whole production process produces Row discharge again after processing all concentrated by waste gas, waste water and waste residue, and the pollution to environment is the least；Additionally, Also there is the advantages such as yield is high, simple to operate.

Accompanying drawing explanation

Fig. 1 is production system schematic diagram of the present utility model.

Fig. 2 is production technological process of the present utility model.

Wherein, 1-methanol tank；2-reactor；3-sodium hydroxide storage tank；4-p-methyl phenol storage tank；5- Cobaltous acetate storage tank；6-oxygen inlet；7-the first water inlet；8-distills assembly；9-Methanol Recovery storage tank；10- Distillating still；11-the first filter；12-hydrochloric acid tank；13-is acidified still；14-the first crystallization kettle；15-first Centrifuge；16-the second water inlet；17-decolours still；18-activated carbon storage tank；19-the second filter；20- Two crystallization kettles；21-the second centrifuge；22-flash dryer.

Detailed description of the invention

Below in conjunction with the accompanying drawings and detailed description of the invention, be further elucidated with this utility model, it should be understood that following specifically Embodiment is merely to illustrate this utility model rather than limits scope of the present utility model.

As it is shown in figure 1, the production system of a kind of hydroxy benzaldehyde production technology, described production system includes Reactor 2, distillating still the 10, first filter 11, acidifying still the 13, first crystallization kettle the 14, first centrifuge 15, decolouring still the 17, second filter the 19, second crystallization kettle the 20, second centrifuge 21 and flash dryer 22；Some raw material storage tanks and oxygen inlet 6 it is connected with, some former on described reactor 2 on described reactor 2 Material storage tank includes methanol tank 1, sodium hydroxide storage tank 3, p-methyl phenol storage tank 4 and cobaltous acetate storage tank 5. The discharging opening of described reactor 2 is connected with the charging aperture of described distillating still 10, and described distillating still 10 is provided with Distillation assembly 8 and the first water inlet 7, be provided with Methanol Recovery storage tank 9 in described distillation assembly 8, described Methanol Recovery storage tank 9 is connected with described methanol tank 1.The discharging opening of described distillating still 10 and described first mistake The charging aperture of filter 11 is connected, the discharging opening of described first filter 11 and the charging aperture of described acidifying still 13 It is connected, described acidifying still 13 is connected with hydrochloric acid tank 12, the discharging opening of described acidifying still 13 and described first The charging aperture of crystallization kettle 14 is connected, the discharging opening of described first crystallization kettle 14 and described first centrifuge 15 phase Even, the solid phase discharging opening of described first centrifuge 15 is connected with the charging aperture of described decolouring still 17, described de- Color still 17 is provided with activated carbon storage tank 18 and the second water inlet 16, and the discharging opening of described decolouring still 17 is with described The charging aperture of the second filter 19 is connected, the discharging opening of described second filter 19 and described second crystallization kettle The charging aperture of 20 is connected, the discharging opening of described second crystallization kettle 20 and the charging aperture of described second centrifuge 21 Being connected, the solid phase discharging opening of described second centrifuge 21 is connected with described flash dryer 22.

Described reactor 2 is provided with waste gas outlet, on described first centrifuge 15 and the second centrifuge 21 It is equipped with wastewater outlet, described first filter 11 and the second filter 19 are equipped with waste residue outlet；Institute Waste gas outlet, wastewater outlet and the waste residue outlet stated are connected to three-protection design system.

As in figure 2 it is shown, the production technology of the production system of above-mentioned hydroxy benzaldehyde, described production technology bag Include sodium salt reaction, oxidation reaction, acidification reaction and product purification to process；The concrete steps of above-mentioned each reaction are such as Under:

(1) sodium salt reaction: a certain proportion of p-methyl phenol, sodium hydroxide, methanol are added in reactor, Stirring makes it be thoroughly mixed dissolving, and p-methyl phenol forms p-methyl phenol sodium salt under the effect of sodium hydroxide；

(2) oxidation reaction: add a certain amount of cobaltous acetate in the reactor of above-mentioned formation sodium salt, will reaction Still seals, and starts to be passed through oxygen and carry out oxidation reaction after being warming up to 55 DEG C, keeps temperature in the kettle to exist during reaction Between 75～85 DEG C；In described oxidation reaction process, in still, pressure is about 0.2MPa, oxidation reaction time Between about 12 hours；

(3) acidification reaction: the mixed material that above-mentioned oxidation reaction obtains is boiled off solvent methanol and recycles, Dead catalyst it is filtered to remove after being dissolved in water；It is subsequently adding hydrochloric acid to carry out saltouing, crystallizing, then by after crystallization Solidliquid mixture is centrifuged separating, and i.e. can get the thick product of hydroxy benzaldehyde；

(4) refinement treatment: after being dissolved in water by thick for above-mentioned hydroxy benzaldehyde product, adds activated carbon decolorizing, It is filtered to remove activated carbon breeze；Again by filtrate refining crystallization, the solidliquid mixture after crystallization is centrifuged separating, The white crystal that last expansion drying obtains is hydroxy benzaldehyde fine work.

Embodiment of above is merely to illustrate this utility model, and is not limitation of the utility model, relevant The those of ordinary skill of technical field, in the case of without departing from spirit and scope of the present utility model, also may be used To make a variety of changes and modification, the technical scheme of the most all equivalents falls within category of the present utility model, Scope of patent protection of the present utility model should be defined by the claims.

Claims (4)

1. the production system of a hydroxy benzaldehyde, it is characterised in that: described production system includes reactor, steaming Evaporate still, the first filter, acidifying still, the first crystallization kettle, the first centrifuge, decolouring still, the second filtration Device, the second crystallization kettle, the second centrifuge and flash dryer；The storage of some raw materials it is connected with on described reactor Tank and oxygen inlet, the discharging opening of described reactor is connected with the charging aperture of described distillating still, described distillation Still is provided with distillation assembly and the first water inlet, the material outlet in described distillation assembly and described reactor Being connected, the discharging opening of described distillating still is connected with the charging aperture of described first filter, and described first filters The discharging opening of device is connected with the charging aperture of described acidifying still, and described acidifying still is connected with hydrochloric acid tank, described The discharging opening of acidifying still is connected with the charging aperture of described first crystallization kettle, the discharging opening of described first crystallization kettle It is connected with described first centrifuge, the solid phase discharging opening of described first centrifuge and the charging of described decolouring still Mouth is connected, and described decolouring still is provided with activated carbon storage tank and the second water inlet, the discharging opening of described decolouring still It is connected with the charging aperture of described second filter, the discharging opening of described second filter and described second crystallization The charging aperture of still is connected, the charging aperture phase of the discharging opening of described second crystallization kettle and described second centrifuge Even, the solid phase discharging opening of described second centrifuge is connected with described flash dryer.

The production system of a kind of hydroxy benzaldehyde the most according to claim 1, it is characterised in that: described instead The some raw material storage tanks on still are answered to include methanol tank, sodium hydroxide storage tank, p-methyl phenol storage tank and vinegar Acid cobalt storage tank.

The production system of a kind of hydroxy benzaldehyde the most according to claim 1, it is characterised in that: described Being provided with Methanol Recovery storage tank in distillation assembly, described Methanol Recovery storage tank is connected with described methanol tank.

The production system of a kind of hydroxy benzaldehyde the most according to claim 1, it is characterised in that: described Reactor is provided with waste gas outlet, and described first centrifuge and the second centrifuge are equipped with wastewater outlet, Waste residue outlet it is equipped with on described first filter and the second filter；Described waste gas outlet, waste water go out Mouth and waste residue outlet are connected to three-protection design system.