CN103304380A - Production process for continuously hydrolyzing and producing hydroquinone through multi-kettles in series - Google Patents
Production process for continuously hydrolyzing and producing hydroquinone through multi-kettles in series Download PDFInfo
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Abstract
The invention belongs to the field of organic synthesis, and in particular relates to a production process for continuously hydrolyzing and producing hydroquinone through multi-kettles in series. The production process comprises the following steps of: adding materials including para aminophenol hydrochloride, hydrochloric acid and water into a dosing kettle and mixing the materials; after mixing the materials, adding the mixture into at least three serial reaction kettles, wherein the pressure in each reaction kettle is kept in balance, and a potential difference between the upper level and lower level of each reaction kettle is kept, so that reaction materials flow to the next stage of reaction kettle from the previous stage of reaction kettle for hydrolysis reaction; enabling a hydrolysate to flow out of the last stage of reaction kettle; enabling the hydrolysate to flow into a condenser; introducing the cooled hydrolysate into a continuous extraction tower; desolventizing an organic phase of the extraction tower to obtain a hydroquinone crude product. As water and acid are repeatedly used in a hydroquinone production process, waste water is remarkably reduced; as continuous production is adopted, the production efficiency is high; the production process has the advantages of high yield and simplicity in process control.
Description
Technical field
The invention belongs to the organic synthesis field, be specifically related to many still series connection continuous hydrolysis production Process of Hydroquinone Production techniques.
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, has wherein realized industrialized have 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, basically eliminate this method abroad, the most of manufacturer of China still continues to use this method.(2) diisopropylbenzene(DIPB) peroxidation method: under acidic conditions, benzene and propylene are carried out the synthetic diisopropylbenzene(DIPB) of alkylated reaction, generate the basic superoxide of diisopropyl (benzene) through peroxidation, get Resorcinol and Resorcinol by scission reaction again, separate obtaining Resorcinol.This method scale of investment is large, and present domestic diisopropylbenzene(DIPB) oxidation style not yet adopts, and does not have industrial production device.(3) phenol-hydrogen peroxide hydroxylation method: this method is take phenol as raw material, with hydroperoxidation, generates Resorcinol and pyrocatechol.Separate obtaining pyrocatechol and Resorcinol product, pyrocatechol output is 3 times of Resorcinol.This method is the height of quality, yield optionally, depends on to a great extent the activity of catalyzer.(4) diazotization hydrolysis method: through diazotization, hydrolysis obtains Resorcinol take p-aminophenol as raw material.Shortcoming is that reacting material concentration is low, and throughput is low, and quantity of three wastes is large.
Also have in addition a kind of method: the direct hydrolysis method, prepare Resorcinol technique take p-aminophenol as raw material through high temperature and high pressure hydrolysis, the 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 the 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 further are condensed into and generate pentanoic, triphenylamine polycondensate.
A series of bibliographical informations relevant research.Among the patent DE2459233, take the monoammonium sulfate aqueous solution as reaction medium, p-aminophenol direct hydrolysis in the airtight high-pressure stirring still of glass inner-lining prepares Resorcinol, adopt the intermittent type hydrolysis process, this technique main drawback is that p-aminophenol is hydrolyzed the easily a large amount of arborescens products of generation under the monoammonium sulfate medium.Among the patent EP0015876, take the methanesulfonic aqueous solution as reaction medium, the mol ratio of p-aminophenol and methanesulfonic is 1:1,240 ℃ of temperature of reaction, 3 hours reaction times, content in crude product 81.8%, yield: 72.7%, this technique exists per pass conversion and the low problem of hydrolysis yield.Among patent JP52057129, JP53002433, JP53012824, the JP53063330, p-aminophenol joins sulfuric acid, hydrochloric acid, hydrobromic autoclave confined reaction 3～10 hours, 200～300 ℃ of temperature of reaction, yield: 43.5%～93.7%.Among patent US3862247 and the GB1460655, take the monoammonium sulfate aqueous solution as reaction medium, monoammonium sulfate and p-aminophenol mol ratio are 1.5-4, temperature of reaction 240-280 ℃, reacted 2-6 hour, and yield is up to 72.7% at 58.4-72.7%.
The method that the p-aminophenol direct hydrolysis of having reported at present prepares Resorcinol mainly faces following three aspects: problem.
(1) produces a large amount of waste water.Because the hydrolysis reaction material concentration is low, after finishing, reaction produces a large amount of by products, and cause the waste water can not recycled, produce a large amount of acid-bearing wastewaters.
(2) adopt the intermittent type hydrolysis.Step still reaction exists material back-mixing, excessively hydrolysis reaction, reaction preference is poor, side reaction increases problem, easily produces a large amount of tar, blocking pipe.
(3) hydrolysis reaction carries out under high temperature and high 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 reasonable utilization, and large-scale production is lacked competitiveness.
Summary of the invention
The present invention is directed to the p-aminophenol direct hydrolysis, to produce in the Resorcinol technique wastewater flow rate large, and the problem that production capacity is low and energy consumption is large proposes a kind of many still series connection continuous hydrolysis production Process of Hydroquinone Production technique.
For achieving the above object, the present invention adopts technical scheme to be:
The production technique that a kind of many still series connection continuous hydrolysis are produced Resorcinol, to mix in material rodinal, hydrochloric acid and the water adding batching kettle, join after the mixing at least three cascade reaction stills, each reacting kettle inner pressure keeps balance, each keeps potential difference between the superior and the subordinate the series connection still, and then make reaction mass flow into voluntarily the next stage reactor from upper level, reaction is hydrolyzed, hydrolyzed solution from the last step reactor out after, enter condenser, cooled hydrolyzed solution enters continuous extraction tower, and the extraction tower organic phase obtains the Resorcinol crude product through precipitation.
Extraction tower water liquid is filtered rear filtrate and turns back in the batching kettle, as to the replenishing of material, keeps batching kettle Raw constant rate.
This process using device comprises batching kettle 1, volume pump 2, reactor 3, condenser 6, continuous extraction tower 7, strainer 8; Wherein the outlet of batching kettle 1 links to each other with an end of volume pump 2, at least three reactors of connecting between volume pump 2 and the condenser 6, the other end of volume pump 2 links to each other with first step reactor opening for feed, most end order reaction still discharge port links to each other with condenser 6, the discharge port of condenser 6 links to each other with continuous extraction tower 7 opening for feeds, and the outlet of continuous extraction tower 7 bottoms is by the feeding inlet 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 by pipeline respectively, is respectively equipped with the pressure valve of each reactor pressure of control at described pipeline.
Be connected in parallel between the pressure valve that arranges on described each reactor.Described reactor, condenser, extraction tower and material contact surface material adopt zirconium, tantalum with and alloy.
Further, the production technique that many still series connection continuous hydrolysis are produced 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) join the raw material that mixes in the first step reactor of three reactors of connecting at least by volume pump, then under the effect of potential difference, make reaction mass flow into voluntarily the next stage reactor from upper level, in each reactor with heating material to 220～240 ℃, by volume pump control material flow, making material total residence time in the reactor of series connection is 150～420 minutes, reaction is hydrolyzed, the pressure of hydrolyzed solution utilization reaction itself enters condenser, condensed hydrolyzed solution enters extraction tower, carries out the continuous extraction precipitation and obtains the Resorcinol crude product;
3) water after the extraction is through strainer, and gained filtrate turns back in the batching kettle, replenishes simultaneously rodinal and proceeds hydrolysis reaction.
Wherein, by volume pump control material flow, making material total residence time in the reactor of series connection is the reaction that is hydrolyzed in 150～420 minutes.Material flow is relevant with series connection still interior total volume of material and the residence time.(total volume of material/residence time in material flow=reactor)
Described in each reactor with heating material to 230 ℃.Described extraction agent agent is butylacetate, propyl carbinol or methyl iso-butyl ketone (MIBK).
Technological principle of the present invention:
Technique such as the series connection of three stills of accompanying drawing 1 correspondence, mol ratio according to rodinal and hydrochloric acid (concentration 30%) is 1:1-4, the mol ratio of rodinal and water is that the ratio preparation hydrolysis material liquid of 1:50-180 places batching kettle 1, raw material is squeezed in the first step reactor 3 of series connection by volume pump 2, after wherein stopping certain hour, under the effect of liquid level difference, flow into the second stage reactor 4 from first step reactor 3, from second stage reactor 4, flow in the third stage reactor 5 again, the pressure that reaches the hydrolyzed solution utilization reaction of requirement transformation efficiency itself enters condenser 6, condensed hydrolyzed solution enters extraction tower 7, carry out continuous extraction, water after the extraction is through strainer 8, remove insolubles and ammonium chloride, filtrate comprises water, hydrochloric acid and unreacted rodinal.Filtrate turns back in the batching kettle, and material ratio in the monitoring batching kettle is replenished rodinal and kept the material constant rate.
In order to make reaction mixture not flow to voluntarily another reactor by pump 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 be a kind of continuously, the Process of Hydroquinone Production technique of efficient, stable, cleaning, the technique major advantage embodies in the following areas:
1. hydrolysising mother liquid recycled, hydrolysising mother liquid is got back to batching kettle extracted the Resorcinol phase-splitting in extraction tower after, realizes that acid and water circuit apply mechanically, and need to add rodinal.Wastewater flow rate is significantly reduced, reduce waste water more than 80%.
2. continuous production processes solution still reaction at intermittence exists the material mixed effect poor, and excessively the problem of hydrolysis reaction reduces side reaction.Can significantly reduce input and output material and the non-cutting time of heating up, production efficiency improves, Effective Raise the reaction efficiency of hydrolysis device, reduce reaction time, improve the production capacity of unit volume.By above-mentioned processing method, the Resorcinol yield is more than 94%.
3. plural serial stage continuous reaction still, reaction mass adds continuously and discharges reactor, and there is not in the periodical operation problem non-cutting time in operate continuously, can be used for scale operation.After raw material adds immediately with still in thing since in the still material capacity large, good stability, operational safety can realize automatically, and is simple to operate, saves manpower.
Description of drawings
Fig. 1 is the technological process of production schematic diagram that many still series connection continuous hydrolysis are produced Resorcinol.
Embodiment
Below by the drawings and specific embodiments technical scheme of the present invention is described further, but protection scope of the present invention is not limited to this, reactor described in the embodiment, condenser, extraction tower and material contact surface material adopt zirconium.
By three grades of synthetic Resorcinol of series connection tank reactor, each reactor volume is 100L, keeps a poor location (potential difference can be 0.1-1 rice) between the superior and the subordinate's reactor, and each still is connected in series by pipeline, gas phase is connected in parallel, and makes pressure maintenance balance between the reactor.Add entry, 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 the material total amount is 2500L.By volume pump material is squeezed into the reactor from batching kettle, control flow 0.8L/min, keep under the equilibrium conditions at each reacting kettle inner pressure simultaneously, make reaction mass flow into voluntarily the next stage reactor from upper level, each material in reactor volume is 80L, making reaction mass is 300 minutes in the still internal reaction time, still interior reaction temperatures at different levels are controlled to be 230 ℃, the reaction that is hydrolyzed, hydrolysis material through the condenser cooling after, enter extraction tower, use n-butyl acetate extraction, the organic phase distillation, precipitation, then rectification under vacuum.The transformation efficiency of rodinal is 58% in the hydrolysis reaction.Water liquid is overanxious through filter from the extraction tower bottom after the extraction, in the batching kettle that returns, adds continuously into rodinal, keeps material proportions constant in the batching kettle.The reaction organic phase obtains purity after desolventizing distillation be 99.8% Resorcinol, yield: 94%.
Embodiment 2
By three grades of synthetic Resorcinol of series connection tank reactor, each reactor volume is 100L, keeps a poor location between the superior and the subordinate's reactor, and each still is connected in series by pipeline, and gas phase is connected in parallel, and makes pressure maintenance balance between the reactor.Add entry, 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 the material total amount is 2500L.By volume pump material is squeezed into the reactor from batching kettle, control flow 1.2L/min, keep under the equilibrium conditions at each reacting kettle inner pressure simultaneously, make reaction mass flow into voluntarily the next stage reactor from upper level, each material in reactor volume is 80L, making reaction mass is 200 minutes in the still internal reaction time, still interior reaction temperatures at different levels are controlled to be 230 ℃, the reaction that is hydrolyzed, hydrolysis material through the condenser cooling after, enter extraction tower, use n-butyl acetate extraction, the organic phase distillation, precipitation, then rectification under vacuum.The transformation efficiency of rodinal is 50% in the hydrolysis reaction, and water liquid is overanxious through filter from the extraction tower bottom after the extraction, and in the batching kettle that returns, batching kettle is added continuously into rodinal, keeps material proportions constant in the batching kettle.The reaction organic phase obtains purity after desolventizing distillation be 99.9% Resorcinol, yield: 96%.
By three grades of synthetic Resorcinol of series connection tank reactor, each reactor volume is 100L, keeps a poor location between the superior and the subordinate's reactor, and each still is connected in series by pipeline, and gas phase is connected in parallel, and makes pressure maintenance balance between the reactor.Add entry, 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 the material total amount is 2500L.By volume pump material is squeezed into the reactor from batching kettle, control flow 1.2L/min, keep under the equilibrium conditions at each reacting kettle inner pressure simultaneously, make reaction mass flow into voluntarily the next stage reactor from upper level, each material in reactor volume is 80L, making reaction mass is 200 minutes in the still internal reaction time, still interior reaction temperatures at different levels are controlled to be 230 ℃, the reaction that is hydrolyzed, hydrolysis material through the condenser cooling after, enter extraction tower, use n-butyl acetate extraction, the organic phase distillation, precipitation, then rectification under vacuum.The transformation efficiency of rodinal is 48% in the hydrolysis reaction, and water liquid is overanxious through filter from the extraction tower bottom after the extraction, in the storage tank that returns, adds continuously into rodinal, keeps material proportions constant in the storage tank.The reaction organic phase obtains purity after desolventizing distillation be 99.8% Resorcinol, yield: 95%.
By three grades of synthetic Resorcinol of series connection tank reactor, each reactor volume is 100L, keeps a poor location between the superior and the subordinate's reactor, and each still is connected in series by pipeline, and gas phase is connected in parallel, and makes pressure maintenance balance between the reactor.Add entry, 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 the material total amount is 2500L.By volume pump material is squeezed into the reactor from batching kettle, control flow 1.2L/min, keep under the equilibrium conditions at each reacting kettle inner pressure simultaneously, make reaction mass flow into voluntarily the next stage reactor from upper level, each material in reactor volume is 80L, making reaction mass is 200 minutes in the still internal reaction time, still interior reaction temperatures at different levels are controlled to be 240 ℃, the reaction that is hydrolyzed, hydrolysis material through the condenser cooling after, enter extraction tower, use n-butyl acetate extraction, the organic phase distillation, precipitation, then rectification under vacuum.The transformation efficiency of rodinal is 58% in the hydrolysis reaction, and water liquid is overanxious through filter from the extraction tower bottom after the extraction, in the batching kettle that returns, adds continuously into rodinal, keeps material proportions constant in the batching kettle.The reaction organic phase obtains purity after desolventizing distillation be 99.7% Resorcinol, yield: 94%.
By three grades of synthetic Resorcinol of series connection tank reactor, each reactor volume is 100L, keeps a poor location between the superior and the subordinate's reactor, and each still is connected in series by pipeline, and gas phase is connected in parallel, and makes pressure maintenance balance between the reactor.Add entry, 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 the material total amount is 2500L.By volume pump material is squeezed into the reactor from batching kettle, control flow 0.8L/min, keep under the equilibrium conditions at each reacting kettle inner pressure simultaneously, make reaction mass flow into voluntarily the next stage reactor from upper level, each material in reactor volume is 80L, making reaction mass is 300 minutes in the still internal reaction time, still interior reaction temperatures at different levels are controlled to be 230 ℃, the reaction that is hydrolyzed, hydrolysis material through the condenser cooling after, enter extraction tower, extract with methyl iso-butyl ketone (MIBK), the organic phase distillation, precipitation, then rectification under vacuum.The transformation efficiency of rodinal is 57% in the hydrolysis reaction, and water liquid is overanxious through filter from the extraction tower bottom after the extraction, in the batching kettle that returns, adds continuously into rodinal, keeps material proportions constant in the batching kettle.The reaction organic phase obtains purity after desolventizing distillation be 99.8% Resorcinol, yield: 96%.
By three grades of synthetic Resorcinol of series connection tank reactor, each reactor volume is 100L, keeps a poor location between the superior and the subordinate's reactor, and each still is connected in series by pipeline, and gas phase is connected in parallel, and makes pressure maintenance balance between the reactor.Add entry, 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 the material total amount is 2500L.By volume pump material is squeezed into the reactor from batching kettle, control flow 0.86L/min, keep under the equilibrium conditions at each reacting kettle inner pressure simultaneously, make reaction mass flow into voluntarily the next stage reactor from upper level, each material in reactor volume is 80L, making reaction mass is 280 minutes in the still internal reaction time, still interior reaction temperatures at different levels are controlled to be 240 ℃, the reaction that is hydrolyzed, hydrolysis material through the condenser cooling after, enter extraction tower, use n-butanol extraction, the organic phase distillation, precipitation, then rectification under vacuum.The transformation efficiency of rodinal is 55% in the hydrolysis reaction, and water liquid is overanxious through filter from the extraction tower bottom after the extraction, in the batching kettle that returns, adds continuously into rodinal, keeps material proportions constant in the batching kettle.The reaction organic phase obtains purity after desolventizing distillation be 99.8% Resorcinol, yield: 95%.
By three grades of synthetic Resorcinol of series connection tank reactor, each reactor volume is 100L, keeps a poor location between the superior and the subordinate's reactor, and each still is connected in series by pipeline, and gas phase is connected in parallel, and makes pressure maintenance balance between the reactor.Add entry, 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 the material total amount is 2500L.By volume pump material is squeezed into the reactor from batching kettle, control flow 0.57L/min, keep under the equilibrium conditions at each reacting kettle inner pressure simultaneously, make reaction mass flow into voluntarily the next stage reactor from upper level, each material in reactor volume is 80L, making reaction mass is 420 minutes in the still internal reaction time, still interior reaction temperatures at different levels are controlled to be 240 ℃, the reaction that is hydrolyzed, hydrolysis material through the condenser cooling after, enter extraction tower, extract with methyl iso-butyl ketone (MIBK), the organic phase distillation, precipitation, then rectification under vacuum.The transformation efficiency of rodinal is 65% in the hydrolysis reaction, and water liquid is overanxious through filter from the extraction tower bottom after the extraction, in the batching kettle that returns, adds continuously into rodinal, keeps material proportions constant in the batching kettle.The reaction organic phase obtains purity after desolventizing distillation be 99.8% Resorcinol, yield: 97%.
By the synthetic Resorcinol of level Four series connection tank reactor, each reactor volume is 100L, keeps a poor location between the superior and the subordinate's reactor, and each still is connected in series by pipeline, and gas phase is connected in parallel, and makes pressure maintenance balance between the reactor.Add entry, 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 the material total amount is 2500L.By volume pump material is squeezed into the reactor from batching kettle, control flow 1.28L/min, keep under the equilibrium conditions at each reacting kettle inner pressure simultaneously, make reaction mass flow into voluntarily the next stage reactor from upper level, each material in reactor volume is 80L, making reaction mass is 250 minutes in the still internal reaction time, still interior reaction temperatures at different levels are controlled to be 240 ℃, the reaction that is hydrolyzed, hydrolysis material through the condenser cooling after, enter extraction tower, extract with methyl iso-butyl ketone (MIBK), the organic phase distillation, precipitation, then rectification under vacuum.The transformation efficiency of rodinal is 55% in the hydrolysis reaction, and water liquid is overanxious through filter from the extraction tower bottom after the extraction, in the batching kettle that returns, adds continuously into rodinal, keeps material proportions constant in the batching kettle.The reaction organic phase obtains purity after desolventizing distillation be 99.8% Resorcinol, yield: 96%.
Embodiment 9
By the synthetic Resorcinol of Pyatyi series connection tank reactor, each reactor volume is 100L, keeps a poor location between the superior and the subordinate's reactor, and each still is connected in series by pipeline, and gas phase is connected in parallel, and makes pressure maintenance balance between the reactor.Add entry, 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 the material total amount is 2500L.By volume pump material is squeezed into the reactor from batching kettle, control flow 1.33L/min, keep under the equilibrium conditions at each reacting kettle inner pressure simultaneously, make reaction mass flow into voluntarily the next stage reactor from upper level, each material in reactor volume is 80L, making reaction mass is 300 minutes in the still internal reaction time, still interior reaction temperatures at different levels are controlled to be 240 ℃, the reaction that is hydrolyzed, hydrolysis material through the condenser cooling after, enter extraction tower, extract with methyl iso-butyl ketone (MIBK), the organic phase distillation, precipitation, then rectification under vacuum.The transformation efficiency of rodinal is 55% in the hydrolysis reaction, and water liquid is overanxious through filter from the extraction tower bottom after the extraction, in the batching kettle that returns, adds continuously into rodinal, keeps material proportions constant in the batching kettle.The reaction organic phase obtains purity after desolventizing distillation be 99.8% Resorcinol, yield: 98%.
Claims (8)
1. still more than kind series connection continuous hydrolysis is produced the production technique of Resorcinol, it is characterized in that: with the material rodinal, hydrochloric acid and water add in the batching kettle and mix, join after the mixing at least three cascade reaction stills, each reacting kettle inner pressure keeps balance, each keeps potential difference between the superior and the subordinate the series connection still, and then make reaction mass flow into voluntarily the next stage reactor from upper level, reaction is hydrolyzed, hydrolyzed solution from the last step reactor out after, enter condenser, cooled hydrolyzed solution enters continuous extraction tower, and the extraction tower organic phase obtains the Resorcinol crude product through precipitation.
2. the production technique of producing Resorcinol by many still series connection continuous hydrolysis claimed in claim 1 is characterized in that:
Extraction tower water liquid is filtered rear filtrate and turns back in the batching kettle, as to the replenishing of material, keeps batching kettle Raw constant rate.
3. the production technique of producing Resorcinol by many still series connection continuous hydrolysis claimed in claim 1, it is characterized in that: this process using device comprises batching kettle (1), volume pump (2), reactor (3), condenser (6), continuous extraction tower (7), strainer (8); Wherein the outlet of batching kettle (1) links to each other with an end of volume pump (2), at least three reactors of connecting between volume pump (2) and the condenser (6), the other end of volume pump (2) links to each other with first step reactor opening for feed, most end order reaction still discharge port links to each other with condenser (6), the discharge port of condenser (6) links to each other with continuous extraction tower (7) opening for feed, and the outlet of continuous extraction tower (7) bottom is by the feeding inlet 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 by pipeline respectively, is respectively equipped with the pressure valve of each reactor pressure of control at described pipeline.
4. the production technique of producing Resorcinol by many still series connection continuous hydrolysis claimed in claim 3 is characterized in that: be connected in parallel between the pressure valve that arranges on described each reactor.
5. the production technique of producing Resorcinol by many still series connection continuous hydrolysis claimed in claim 3 is characterized in that:
Described reactor, condenser, extraction tower and material contact surface material adopt zirconium, tantalum with and alloy.
6. the production technique of producing Resorcinol by many still series connection continuous hydrolysis claimed in claim 2 is characterized in that:
1) by batching kettle (1) 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) join the raw material that mixes in the first step reactor of three reactors of connecting at least by volume pump, then under the effect of potential difference, make reaction mass flow into voluntarily the next stage reactor from upper level, in each reactor with heating material to 220～240 ℃, by volume pump control material flow, making material total residence time in the reactor of series connection is 150～420 minutes, reaction is hydrolyzed, the pressure of hydrolyzed solution utilization reaction itself enters condenser, condensed hydrolyzed solution enters extraction tower, carries out the continuous extraction precipitation and obtains the Resorcinol crude product;
3) water after the extraction is through strainer, and gained filtrate turns back in the batching kettle, replenishes simultaneously rodinal and proceeds hydrolysis reaction.
7. the production technique of producing Resorcinol by many stills series connection continuous hydrolysis claimed in claim 6 is characterized in that: described in each reactor with heating material to 230 ℃.
8. the production technique of producing Resorcinol by many still series connection continuous hydrolysis claimed in claim 6, it is characterized in that: described extraction agent agent is butylacetate, propyl carbinol or methyl iso-butyl ketone (MIBK).
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