CN103304380B - Multi-floating bodies continuous hydrolysis produces the production technique of Resorcinol - Google Patents
Multi-floating bodies continuous hydrolysis produces the production technique of Resorcinol Download PDFInfo
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Abstract
The invention belongs to organic synthesis field, be specifically related to multi-floating bodies continuous hydrolysis production Process of Hydroquinone Production technique.Material rodinal, hydrochloric acid and water are added in batching kettle and mixes, join at least three cascade reaction stills after mixing, each reacting kettle inner pressure keeps balance, series connection still respectively keeps potential difference between the superior and the subordinate, and then makes reaction mass flow into next stage reactor voluntarily from upper level, and be hydrolyzed reaction, hydrolyzed solution from last step reactor out after, enter condenser, cooled hydrolyzed solution enters continuous extraction tower, and extraction tower organic phase obtains Resorcinol crude product through precipitation.Process of Hydroquinone Production technique of the present invention realizes the recycled of water and acid, and waste water significantly reduces; Continuous prodution, production efficiency is high; There is yield high, the simple advantage of technology controlling and process.
Description
Technical field
The invention belongs to organic synthesis field, be specifically related to multi-floating bodies continuous hydrolysis production Process of Hydroquinone Production technique.
Background technology
It is a kind of important meticulous Organic Chemicals that Resorcinol has another name called quinhydrones, is widely used in the industries such as medicine, agricultural chemicals, dyestuff, rubber, auxiliary agent.The synthetic method of Resorcinol is more, and wherein having realized industrializedly has aniline oxidation style, p-Diisopropylbenzene peroxidation method, phenol-hydrogen peroxide hydroxylation method etc.
(1) aniline oxidation style: aniline is oxidized to para benzoquinone with Manganse Dioxide (or sodium dichromate 99) in sulfuric acid medium, and then para benzoquinone is reduced into Resorcinol.Produce a large amount of waste water and waste residue in the method production process, substantially eliminate this method abroad, major part manufacturer of China still continues to use this method.(2) diisopropylbenzene(DIPB) peroxidation method: in acid condition benzene and propylene are carried out alkylated reaction and synthesize diisopropylbenzene(DIPB), diisopropyl (benzene) base superoxide is generated through peroxidation, obtain Resorcinol and Resorcinol by scission reaction again, be separated and obtain Resorcinol.This method scale of investment is large, and current domestic diisopropylbenzene(DIPB) oxidation style not yet adopts, and does not have industrial production device.(3) phenol-hydrogen peroxide hydroxylation method: this method take phenol as raw material, with hydroperoxidation, generates Resorcinol and pyrocatechol.Separation obtains pyrocatechol and Resorcinol product, and pyrocatechol output is 3 times of Resorcinol.This method optionally quality, yield height, depend on the activity of catalyzer to a great extent.(4) diazotization hydrolysis method: with p-aminophenol be raw material through diazotization, hydrolysis obtain Resorcinol.Shortcoming is that reacting material concentration is low, and throughput is low, and quantity of three wastes is large.
Also has a kind of method in addition: direct hydrolysis method, be that raw material prepares Resorcinol technique through high temperature and high pressure hydrolysis with p-aminophenol, reaction of atomic economy is high, has raw material and is easy to get, the advantage that reaction process is short.Main drawback is that equipment material requirement is high, and cost is high, and technology content requires high.Its reaction equation is as follows:
1, reaction principle: take p-aminophenol as raw material, catalytic hydrolysis in acidic medium.
Side reaction: the Resorcinol of generation and raw material p-aminophenol are condensed into further and generate pentanoic, triphenylamine polycondensate.
The research that a series of bibliographical information is relevant.In patent DE2459233, with the monoammonium sulfate aqueous solution for reaction medium, p-aminophenol direct hydrolysis in the airtight HV XLPE power cables of glass inner-lining prepares Resorcinol, adopt intermittent type hydrolysis process, this technique main drawback is that p-aminophenol is hydrolyzed the easily a large amount of arborescens product of generation under monoammonium sulfate medium.In patent EP0015876, with the methanesulfonic aqueous solution for reaction medium, the mol ratio of p-aminophenol and methanesulfonic is 1:1, temperature of reaction 240 DEG C, 3 hours reaction times, content in crude product 81.8%, yield: 72.7%, there is per pass conversion and the lower problem of hydrolysis yield in this technique.In patent JP52057129, JP53002433, JP53012824, JP53063330, p-aminophenol joins sulfuric acid, hydrochloric acid, hydrobromic autoclave confined reaction 3 ~ 10 hours, temperature of reaction 200 ~ 300 DEG C, yield: 43.5% ~ 93.7%.In patent US3862247 and GB1460655, with the monoammonium sulfate aqueous solution for reaction medium, monoammonium sulfate and p-aminophenol mol ratio are 1.5-4, temperature of reaction 240-280 DEG C, and reaction 2-6 hour, yield, at 58.4-72.7%, is up to 72.7%.
The method that the p-aminophenol direct hydrolysis reported at present prepares Resorcinol mainly faces following three aspect problems.
(1) a large amount of waste water is produced.Because hydrolysis reaction material concentration is low, reaction terminates a large amount of by product of rear generation, causes waste water can not recycled, produces a large amount of acid-bearing wastewaters.
(2) intermittent type hydrolysis is adopted.There is the problem that material back-mixing, excessively hydrolysis reaction, reaction preference are poor, side reaction increases in step still reaction, the tar that easily generation is a large amount of, blocking pipe.
(3) hydrolysis reaction carries out at high temperature and pressure, and cold material needs heating, and thermal material needs cooling, and energy consumption is large, and the non-cutting time of intensification and cooling is long, and production efficiency is low.Energy can not get Appropriate application, and large-scale production is lacked competitiveness.
Summary of the invention
The present invention is directed to wastewater flow rate in p-aminophenol direct hydrolysis production Resorcinol technique large, the problem that production capacity is low and energy consumption is large, proposes a kind of multi-floating bodies continuous hydrolysis production Process of Hydroquinone Production technique.
For achieving the above object, the present invention adopts technical scheme to be:
A kind of multi-floating bodies continuous hydrolysis produces the production technique of Resorcinol, material rodinal, hydrochloric acid and water are added in batching kettle and mixes, join at least three cascade reaction stills after mixing, each reacting kettle inner pressure keeps balance, series connection still respectively keeps potential difference between the superior and the subordinate, and then make reaction mass flow into next stage reactor voluntarily from upper level, be hydrolyzed reaction, hydrolyzed solution from last step reactor out after, enter condenser, cooled hydrolyzed solution enters continuous extraction tower, and extraction tower organic phase obtains Resorcinol crude product through precipitation.
Extraction tower aqueous phase liquid is filtered rear filtrate and turns back in batching kettle, as supplementing material, keeps batching kettle Raw constant rate.
This technique adopts device to comprise batching kettle 1, volume pump 2, reactor 3, condenser 6, continuous extraction tower 7, strainer 8; Wherein the outlet of batching kettle 1 is connected with one end of volume pump 2, to connect between volume pump 2 with condenser 6 at least three reactors, the other end of volume pump 2 is connected with first step reactor opening for feed, most end order reaction still discharge port is connected with condenser 6, the discharge port of condenser 6 is connected with continuous extraction tower 7 opening for feed, and the outlet of continuous extraction tower 7 bottom is communicated by the opening for feed of strainer 8 with batching kettle 1;
Wherein, the upper level of cascade reaction still and next stage keep potential difference; The air outlet of each reactor of series connection is connected respectively by pipeline, and described pipeline is respectively equipped with the pressure valve controlling each reactor pressure.
Be connected in parallel between the pressure valve that each reactor described is arranged.Described reactor, condenser, extraction tower and material contact surface material adopt zirconium, tantalum and its alloy.
Further, multi-floating bodies continuous hydrolysis produces the production technique of Resorcinol,
1) by batching kettle, material rodinal, hydrochloric acid and water are mixed; Wherein, the mol ratio of rodinal and hydrochloric acid (concentration 30%) is 1:1-4, and the mol ratio of rodinal and water is 1:50-180;
2) raw material mixed is joined by volume pump in the first step reactor of at least series connection three reactors, under the effect of potential difference, then make reaction mass flow into next stage reactor voluntarily from upper level, in each reactor by heating material to 220 ~ 240 DEG C, control material flow by volume pump, material total residence time in the reactor of series connection is made to be 150 ~ 420 minutes, be hydrolyzed reaction, hydrolyzed solution utilizes the pressure of reaction itself to enter condenser, condensed hydrolyzed solution enters extraction tower, carries out continuous extraction precipitation and obtains Resorcinol crude product;
3) aqueous phase after extraction is through strainer, and gained filtrate turns back in batching kettle, supplements rodinal simultaneously and proceeds hydrolysis reaction.
Wherein, control material flow by volume pump, make material total residence time in the reactor of series connection be the reaction that is hydrolyzed for 150 ~ 420 minutes.Material flow is relevant with the residence time to volume of material total in series connection still.(in material flow=reactor total volume of material/residence time)
Described in each reactor by heating material to 230 DEG C.Described extraction agent agent is butylacetate, propyl carbinol or methyl iso-butyl ketone (MIBK).
Present invention process principle:
As the technique of three still series connection of accompanying drawing 1 correspondence, be 1:1-4 according to the mol ratio of rodinal and hydrochloric acid (concentration 30%), the mol ratio of rodinal and water is that the proportions hydrolysis material liquid of 1:50-180 is placed in batching kettle 1, by volume pump 2, raw material is squeezed in the first step reactor 3 of series connection, after wherein stopping certain hour, flow into second stage reactor 4 from first step reactor 3 under the effect of liquid level difference, flow into from second stage reactor 4 again in third stage reactor 5, the hydrolyzed solution reaching requirement transformation efficiency utilizes the pressure of reaction itself to enter condenser 6, condensed hydrolyzed solution enters extraction tower 7, carry out continuous extraction, aqueous phase after extraction is through strainer 8, removing insolubles and ammonium chloride, filtrate comprises water, hydrochloric acid and unreacted rodinal.Filtrate turns back in batching kettle, material ratio in monitoring batching kettle, supplements rodinal and keeps material constant rate.
In order to make reaction mixture not flow to another reactor by pump voluntarily by a reactor, between each reactor, pressure equalizing pipe is housed, the mounting height of reactor is reduced to third stage reactor 5 successively by first step reactor 3, has a poor location.The pressure of reactor depends primarily on temperature of reaction, and reactive mode adopts the temperature and pressure of each stage reactor identical.
The present invention is a kind of continuous, efficient, stable, clean Process of Hydroquinone Production technique, and technique major advantage embodies in the following areas:
1. hydrolysising mother liquid recycled, hydrolysising mother liquid gets back to batching kettle extracted Resorcinol phase-splitting in extraction tower after, realizes the recycled of acid and water, only needs to add rodinal.Wastewater flow rate is significantly reduced, reduces waste water more than 80%.
2. continuous production processes solves batch tank reaction to there is material mixed effect poor, the problem of excessive hydrolysis reaction, minimizing side reaction.Significantly can reduce input and output material and heat up non-cutting time, production efficiency improves, and effectively improves the reaction efficiency of hydrolysis device, reduces reaction time, improves the production capacity of unit volume.By above-mentioned processing method, Resorcinol yield is more than 94%.
3. plural serial stage continuous reaction still, reaction mass adds continuously and discharges reactor, operate continuously, to there is not in periodical operation problem non-cutting time, can be used for scale operation.After raw material adds immediately with thing in still because material capacity in still is large, good stability, operational safety, can realize automatically, simple to operate, saves manpower.
Accompanying drawing explanation
Fig. 1 is the technological process of production schematic diagram that multi-floating bodies continuous hydrolysis produces Resorcinol.
Embodiment
Be described further technical scheme of the present invention below by the drawings and specific embodiments, but protection scope of the present invention is not limited thereto, reactor described in embodiment, condenser, extraction tower and material contact surface material adopt zirconium.
Embodiment 1
By thtee-stage shiplock tank reactor synthesis Resorcinol, each reactor volume is 100L, and keep a poor location (potential difference can be 0.1-1 rice) between the superior and the subordinate's reactor, each still is connected by placed in series, gas phase is connected in parallel, and makes pressure between reactor keep balance.Add water, 30% hydrochloric acid and rodinal in the batching kettle of 3000L, determine rodinal: hydrochloric acid: the mol ratio of water is 1:3:100, and material total amount is 2500L.By volume pump, material is squeezed into reactor from batching kettle, control flow 0.8L/min, simultaneously under each reacting kettle inner pressure keeps equilibrium conditions, reaction mass is made to flow into next stage reactor voluntarily from upper level, each material in reactor volume is 80L, reaction mass reaction times in still is made to be 300 minutes, it is 230 DEG C that still interior reaction temperature at different levels controls, be hydrolyzed reaction, and hydrolysis material, after condenser cooling, enters extraction tower, with n-butyl acetate extraction, organic phase is distilled, precipitation, then rectification under vacuum.In hydrolysis reaction, the transformation efficiency of rodinal is 58%.After extraction, aqueous phase liquid is overanxious through filter bottom extraction tower, in the batching kettle returned, adds continuously into rodinal, keeps material proportions constant in batching kettle.Reaction organic phase obtains the Resorcinol that purity is 99.8%, yield: 94% after desolventizing distillation.
Embodiment 2
By thtee-stage shiplock tank reactor synthesis Resorcinol, each reactor volume is 100L, keeps a poor location between the superior and the subordinate's reactor, and each still is connected by placed in series, and gas phase is connected in parallel, and makes pressure between reactor keep balance.Add water, 30% hydrochloric acid and rodinal in the batching kettle of 3000L, determine rodinal: hydrochloric acid: the mol ratio of water is 1:3:100, and material total amount is 2500L.By volume pump, material is squeezed into reactor from batching kettle, control flow 1.2L/min, simultaneously under each reacting kettle inner pressure keeps equilibrium conditions, reaction mass is made to flow into next stage reactor voluntarily from upper level, each material in reactor volume is 80L, reaction mass reaction times in still is made to be 200 minutes, it is 230 DEG C that still interior reaction temperature at different levels controls, be hydrolyzed reaction, and hydrolysis material, after condenser cooling, enters extraction tower, with n-butyl acetate extraction, organic phase is distilled, precipitation, then rectification under vacuum.In hydrolysis reaction, the transformation efficiency of rodinal is 50%, and after extraction, aqueous phase liquid is overanxious through filter bottom extraction tower, and in the batching kettle returned, batching kettle is added continuously into rodinal, keeps material proportions constant in batching kettle.Reaction organic phase obtains the Resorcinol that purity is 99.9%, yield: 96% after desolventizing distillation.
Embodiment 3
By thtee-stage shiplock tank reactor synthesis Resorcinol, each reactor volume is 100L, keeps a poor location between the superior and the subordinate's reactor, and each still is connected by placed in series, and gas phase is connected in parallel, and makes pressure between reactor keep balance.Add water, 30% hydrochloric acid and rodinal in the batching kettle of 3000L, determine rodinal: hydrochloric acid: the mol ratio of water is 1:4:50, and material total amount is 2500L.By volume pump, material is squeezed into reactor from batching kettle, control flow 1.2L/min, simultaneously under each reacting kettle inner pressure keeps equilibrium conditions, reaction mass is made to flow into next stage reactor voluntarily from upper level, each material in reactor volume is 80L, reaction mass reaction times in still is made to be 200 minutes, it is 230 DEG C that still interior reaction temperature at different levels controls, be hydrolyzed reaction, and hydrolysis material, after condenser cooling, enters extraction tower, with n-butyl acetate extraction, organic phase is distilled, precipitation, then rectification under vacuum.In hydrolysis reaction, the transformation efficiency of rodinal is 48%, and after extraction, aqueous phase liquid is overanxious through filter bottom extraction tower, in the storage tank returned, adds continuously into rodinal, keeps material proportions constant in storage tank.Reaction organic phase obtains the Resorcinol that purity is 99.8%, yield: 95% after desolventizing distillation.
Embodiment 4
By thtee-stage shiplock tank reactor synthesis Resorcinol, each reactor volume is 100L, keeps a poor location between the superior and the subordinate's reactor, and each still is connected by placed in series, and gas phase is connected in parallel, and makes pressure between reactor keep balance.Add water, 30% hydrochloric acid and rodinal in the batching kettle of 3000L, determine rodinal: hydrochloric acid: the mol ratio of water is 1:3:100, and material total amount is 2500L.By volume pump, material is squeezed into reactor from batching kettle, control flow 1.2L/min, simultaneously under each reacting kettle inner pressure keeps equilibrium conditions, reaction mass is made to flow into next stage reactor voluntarily from upper level, each material in reactor volume is 80L, reaction mass reaction times in still is made to be 200 minutes, it is 240 DEG C that still interior reaction temperature at different levels controls, be hydrolyzed reaction, and hydrolysis material, after condenser cooling, enters extraction tower, with n-butyl acetate extraction, organic phase is distilled, precipitation, then rectification under vacuum.In hydrolysis reaction, the transformation efficiency of rodinal is 58%, and after extraction, aqueous phase liquid is overanxious through filter bottom extraction tower, in the batching kettle returned, adds continuously into rodinal, keeps material proportions constant in batching kettle.Reaction organic phase obtains the Resorcinol that purity is 99.7%, yield: 94% after desolventizing distillation.
Embodiment 5
By thtee-stage shiplock tank reactor synthesis Resorcinol, each reactor volume is 100L, keeps a poor location between the superior and the subordinate's reactor, and each still is connected by placed in series, and gas phase is connected in parallel, and makes pressure between reactor keep balance.Add water, 30% hydrochloric acid and rodinal in the batching kettle of 3000L, determine rodinal: hydrochloric acid: the mol ratio of water is 1:3:100, and material total amount is 2500L.By volume pump, material is squeezed into reactor from batching kettle, control flow 0.8L/min, simultaneously under each reacting kettle inner pressure keeps equilibrium conditions, reaction mass is made to flow into next stage reactor voluntarily from upper level, each material in reactor volume is 80L, reaction mass reaction times in still is made to be 300 minutes, it is 230 DEG C that still interior reaction temperature at different levels controls, be hydrolyzed reaction, and hydrolysis material, after condenser cooling, enters extraction tower, extract by methyl iso-butyl ketone (MIBK), organic phase is distilled, precipitation, then rectification under vacuum.In hydrolysis reaction, the transformation efficiency of rodinal is 57%, and after extraction, aqueous phase liquid is overanxious through filter bottom extraction tower, in the batching kettle returned, adds continuously into rodinal, keeps material proportions constant in batching kettle.Reaction organic phase obtains the Resorcinol that purity is 99.8%, yield: 96% after desolventizing distillation.
Embodiment 6
By thtee-stage shiplock tank reactor synthesis Resorcinol, each reactor volume is 100L, keeps a poor location between the superior and the subordinate's reactor, and each still is connected by placed in series, and gas phase is connected in parallel, and makes pressure between reactor keep balance.Add water, 30% hydrochloric acid and rodinal in the batching kettle of 3000L, determine rodinal: hydrochloric acid: the mol ratio of water is 1:3:100, and material total amount is 2500L.By volume pump, material is squeezed into reactor from batching kettle, control flow 0.86L/min, simultaneously under each reacting kettle inner pressure keeps equilibrium conditions, reaction mass is made to flow into next stage reactor voluntarily from upper level, each material in reactor volume is 80L, reaction mass reaction times in still is made to be 280 minutes, it is 240 DEG C that still interior reaction temperature at different levels controls, be hydrolyzed reaction, and hydrolysis material, after condenser cooling, enters extraction tower, with n-butanol extraction, organic phase is distilled, precipitation, then rectification under vacuum.In hydrolysis reaction, the transformation efficiency of rodinal is 55%, and after extraction, aqueous phase liquid is overanxious through filter bottom extraction tower, in the batching kettle returned, adds continuously into rodinal, keeps material proportions constant in batching kettle.Reaction organic phase obtains the Resorcinol that purity is 99.8%, yield: 95% after desolventizing distillation.
Embodiment 7
By thtee-stage shiplock tank reactor synthesis Resorcinol, each reactor volume is 100L, keeps a poor location between the superior and the subordinate's reactor, and each still is connected by placed in series, and gas phase is connected in parallel, and makes pressure between reactor keep balance.Add water, 30% hydrochloric acid and rodinal in the batching kettle of 3000L, determine rodinal: hydrochloric acid: the mol ratio of water is 1:3:180, and material total amount is 2500L.By volume pump, material is squeezed into reactor from batching kettle, control flow 0.57L/min, simultaneously under each reacting kettle inner pressure keeps equilibrium conditions, reaction mass is made to flow into next stage reactor voluntarily from upper level, each material in reactor volume is 80L, reaction mass reaction times in still is made to be 420 minutes, it is 240 DEG C that still interior reaction temperature at different levels controls, be hydrolyzed reaction, and hydrolysis material, after condenser cooling, enters extraction tower, extract by methyl iso-butyl ketone (MIBK), organic phase is distilled, precipitation, then rectification under vacuum.In hydrolysis reaction, the transformation efficiency of rodinal is 65%, and after extraction, aqueous phase liquid is overanxious through filter bottom extraction tower, in the batching kettle returned, adds continuously into rodinal, keeps material proportions constant in batching kettle.Reaction organic phase obtains the Resorcinol that purity is 99.8%, yield: 97% after desolventizing distillation.
Embodiment 8
By level Four series connection tank reactor synthesis Resorcinol, each reactor volume is 100L, keeps a poor location between the superior and the subordinate's reactor, and each still is connected by placed in series, and gas phase is connected in parallel, and makes pressure between reactor keep balance.Add water, 30% hydrochloric acid and rodinal in the batching kettle of 3000L, determine rodinal: hydrochloric acid: the mol ratio of water is 1:3:120, and material total amount is 2500L.By volume pump, material is squeezed into reactor from batching kettle, control flow 1.28L/min, simultaneously under each reacting kettle inner pressure keeps equilibrium conditions, reaction mass is made to flow into next stage reactor voluntarily from upper level, each material in reactor volume is 80L, reaction mass reaction times in still is made to be 250 minutes, it is 240 DEG C that still interior reaction temperature at different levels controls, be hydrolyzed reaction, and hydrolysis material, after condenser cooling, enters extraction tower, extract by methyl iso-butyl ketone (MIBK), organic phase is distilled, precipitation, then rectification under vacuum.In hydrolysis reaction, the transformation efficiency of rodinal is 55%, and after extraction, aqueous phase liquid is overanxious through filter bottom extraction tower, in the batching kettle returned, adds continuously into rodinal, keeps material proportions constant in batching kettle.Reaction organic phase obtains the Resorcinol that purity is 99.8%, yield: 96% after desolventizing distillation.
Embodiment 9
By Pyatyi series connection tank reactor synthesis Resorcinol, each reactor volume is 100L, keeps a poor location between the superior and the subordinate's reactor, and each still is connected by placed in series, and gas phase is connected in parallel, and makes pressure between reactor keep balance.Add water, 30% hydrochloric acid and rodinal in the batching kettle of 3000L, determine rodinal: hydrochloric acid: the mol ratio of water is 1:3:150, and material total amount is 2500L.By volume pump, material is squeezed into reactor from batching kettle, control flow 1.33L/min, simultaneously under each reacting kettle inner pressure keeps equilibrium conditions, reaction mass is made to flow into next stage reactor voluntarily from upper level, each material in reactor volume is 80L, reaction mass reaction times in still is made to be 300 minutes, it is 240 DEG C that still interior reaction temperature at different levels controls, be hydrolyzed reaction, and hydrolysis material, after condenser cooling, enters extraction tower, extract by methyl iso-butyl ketone (MIBK), organic phase is distilled, precipitation, then rectification under vacuum.In hydrolysis reaction, the transformation efficiency of rodinal is 55%, and after extraction, aqueous phase liquid is overanxious through filter bottom extraction tower, in the batching kettle returned, adds continuously into rodinal, keeps material proportions constant in batching kettle.Reaction organic phase obtains the Resorcinol that purity is 99.8%, yield: 98% after desolventizing distillation.
Claims (6)
1. the production technique of a multi-floating bodies continuous hydrolysis production Resorcinol, it is characterized in that: by material rodinal, hydrochloric acid and water add in batching kettle and mix, join at least three cascade reaction stills after mixing, each reacting kettle inner pressure keeps balance, series connection still respectively keeps potential difference between the superior and the subordinate, and then make reaction mass flow into next stage reactor voluntarily from upper level, be hydrolyzed reaction, hydrolyzed solution from last step reactor out after, enter condenser, cooled hydrolyzed solution enters continuous extraction tower, extraction tower organic phase obtains Resorcinol crude product through precipitation,
Extraction tower aqueous phase liquid is filtered rear filtrate and turns back in batching kettle, as supplementing material, keeps batching kettle Raw constant rate;
Be specially:
1) by batching kettle (1), material rodinal, hydrochloric acid and water are mixed; Wherein, rodinal and concentration are the mol ratio of 30% hydrochloric acid is 1:1-4, and the mol ratio of rodinal and water is 1:50-180;
2) raw material mixed is joined by volume pump in the first step reactor of at least series connection three reactors, under the effect of potential difference, then make reaction mass flow into next stage reactor voluntarily from upper level, in each reactor by heating material to 220 ~ 240 DEG C, control material flow by volume pump, material total residence time in the reactor of series connection is made to be 150 ~ 420 minutes, be hydrolyzed reaction, hydrolyzed solution utilizes the pressure of reaction itself to enter condenser, condensed hydrolyzed solution enters extraction tower, carries out continuous extraction precipitation and obtains Resorcinol crude product;
3) aqueous phase after extraction is through strainer, and gained filtrate turns back in batching kettle, supplements rodinal simultaneously and proceeds hydrolysis reaction.
2. produce the production technique of Resorcinol by multi-floating bodies continuous hydrolysis according to claim 1, it is characterized in that: this technique adopts device to comprise batching kettle (1), volume pump (2), reactor (3), condenser (6), continuous extraction tower (7), strainer (8); Wherein the outlet of batching kettle (1) is connected with one end of volume pump (2), to connect between volume pump (2) with condenser (6) at least three reactors, the other end of volume pump (2) is connected with first step reactor opening for feed, most end order reaction still discharge port is connected with condenser (6), the discharge port of condenser (6) is connected with continuous extraction tower (7) opening for feed, and the outlet of continuous extraction tower (7) bottom is communicated by the opening for feed of strainer (8) with batching kettle (1);
Wherein, the upper level of cascade reaction still and next stage keep potential difference; The air outlet of each reactor of series connection is connected respectively by pipeline, and described pipeline is respectively equipped with the pressure valve controlling each reactor pressure.
3. produce the production technique of Resorcinol by multi-floating bodies continuous hydrolysis according to claim 2, it is characterized in that: be connected in parallel between the pressure valve that each reactor described is arranged.
4. produce the production technique of Resorcinol by multi-floating bodies continuous hydrolysis according to claim 2, it is characterized in that:
Described reactor, condenser, extraction tower and material contact surface material adopt zirconium, tantalum and its alloy.
5. produce the production technique of Resorcinol by multi-floating bodies continuous hydrolysis according to claim 1, it is characterized in that: described in each reactor by heating material to 230 DEG C.
6. produce the production technique of Resorcinol by multi-floating bodies continuous hydrolysis according to claim 1, it is characterized in that: extraction agent is butylacetate, propyl carbinol or methyl iso-butyl ketone (MIBK).
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| CN101497558A (en) * | 2008-02-01 | 2009-08-05 | 浙江龙盛化工研究有限公司 | Method for preparing resorcin by hydrolyzing m-phenylenediamine |
| CN102276423A (en) * | 2011-06-28 | 2011-12-14 | 江苏科圣化工机械有限公司 | Method for producing hydroquinone by direct hydrolysis of p-phenylenediamine |
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