CN102964220A - Pure sodium phenolate sulfuric acid continuous decomposition technology and equipment thereof - Google Patents
Pure sodium phenolate sulfuric acid continuous decomposition technology and equipment thereof Download PDFInfo
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- CN102964220A CN102964220A CN2012104960218A CN201210496021A CN102964220A CN 102964220 A CN102964220 A CN 102964220A CN 2012104960218 A CN2012104960218 A CN 2012104960218A CN 201210496021 A CN201210496021 A CN 201210496021A CN 102964220 A CN102964220 A CN 102964220A
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Abstract
The invention relates to the technical field of coal tar deep processing of the metallurgical coking industry, and particularly relates to a pure sodium phenolate sulfuric acid continuous decomposition technology and equipment thereof. A pure sodium phenolate solution and 40-60% dilute sulfuric acid are mixed by multiple levels of pipeline mixers, and then the mixture enters a sulfuric acid decomposition separation tank to realize continuous decomposition; a heating device is adopted in the mixing process and comprises a sodium phenolate pump, a dilute sulfuric acid pump and a jet mixer; the sodium phenolate pump and the dilute sulfuric acid pump are connected with an input port of the jet mixer through a pipeline respectively; an output port of the jet mixer is connected with 2-5 levels of pipeline mixers in turn; and 1-2 heaters are arranged among the pipeline mixers. Compared with the prior art, the invention has the beneficial effects that 1) the recovery rate of phenol exceeds 99%, and large-scale production can be realized; 2) 40-60% dilute sulfuric acid is used in reaction, the requirements for the materials of the equipment are low, the jet mixer can be effectively prevented from being corroded, and the operation environment can be effectively improved; and 3) the heating device is favorable for full reaction.
Description
Technical field
The present invention relates to metallurgical coking industry coal tar deep processing technical field, particularly a kind of clean phenol sodium sulfuric acid continuous decomposition process and equipment thereof.
Background technology
At present, the decomposition technique of clean phenol sodium generally adopts intermittent type sulfuric acid decomposition method and carbonic acid gas decomposition method.
Wherein the major equipment of intermittent type sulfuric acid decomposition method is the splitter at intermittence.Clean phenol sodium is packed in the splitter, then from the header tank sulfuric acid of slowly packing into, inject generally speaking 75% left and right sides sulfuric acid, stir simultaneously.The heat that decomposition course produces shifts out with indirect cooling water.Leave standstill a few hours after the reaction.Above the crude phenols that decomposition generates float over, below sodium sulfate sinks to.So put first the waste water of contains sodium sulfate, emit again crude phenols.
The weak point of intermittent type sulfuric acid decomposition method is, the concentration of sulfuric acid can not be low, and treatment capacity can not be too high, otherwise sulfonation reaction easily occurs, and sulfonated bodies is dissolved in crude phenols, and sulfonated bodies decomposes and produces sulfur dioxide gas during refining of crude phenol, etching apparatus, and affect product purity.Even 75% left and right sides sulfuric acid, under this condition, the heat of dilution of sulfuric acid is also very large, is subject to the structure of batch reactor, and the area of interchanger is little in the reactor, and the speed of acid adding can not be too fast.So, intermittent type sulfuric acid decomposition method small scale.
The carbonic acid gas decomposition method is to utilize blast furnace gas or CO2 concentration to decompose at 17～25% flue gases of cock oven.Decomposition is carried out in the continuous decomposition tower, and the tower bottom blowing enters blast furnace gas or purifying flue gas, and cat head sprays clean phenates, and counter current contact also generates crude phenols and Na at the tower internal reaction
2CO
3, crude phenols are discharged from tower top, Na
2CO
3Discharge from tower bottom.
The weak point of carbonic acid gas decomposition method is, has undecomposed complete phenates in the crude phenols, needs further decompose with sulfuric acid again.The carbonic acid gas decomposition method, the Technology mature and reliable is widely used in each big or middle scale tar process engineering, and greatly saves the sulfuric acid consumption.If but the producer that has does not adopt the condition of carbonic acid gas decomposition method, can only select sulfuric acid decomposition method, so, the intermittent type sulfuric acid decomposition method can not satisfy the processing of medium above scale tar.
Summary of the invention
The purpose of this invention is to provide a kind of clean phenol sodium sulfuric acid continuous decomposition process and equipment thereof, overcome the deficiencies in the prior art, medium above scale new construction under high for the environmental pollution requirement, as the not have carbonic acid gas condition, technical process is simple, easy handling is invested low, less energy consumption, environment protecting is good.
For achieving the above object, the present invention is achieved by the following technical solutions:
Clean phenol sodium sulfuric acid continuous decomposition process, clean sodium phenolate solution and 40%～60% dilute sulphuric acid enter sulfuric acid decomposition and separation groove and realize continuous decomposition after the multi-stage pipeline mixing tank mixes, be provided with heating unit in the mixing process, and its concrete steps are as follows:
1) flow 2～3m
340%～60% the dilute sulphuric acid of the clean sodium phenolate solution of the concentration 18%-20% of/h and flow 400～450 l/h mixes in jet mixer in proportion;
2) mixed solution mixes conveying through 2～5 grades of line mixers, PH behind the final stage line mixer is 1～2, be provided with 1～2 heating unit between the line mixer, mixed solution residence time in pipeline is 5～10 minutes, then enter in the sulfuric acid decomposition and separation groove one, in sulfuric acid decomposition and separation groove one, stop reaction after 180～240 minutes, get crude phenols one;
3) crude phenols enter sulfuric acid decomposition and separation groove two behind the crude phenols line mixer, and at crude phenols line mixer 7 front adding service waters, crude phenols one react to get product crude phenols two in sulfuric acid decomposition and separation groove two.
The heating medium of described heating unit is 75 ℃～80 ℃ warm water.
Clean phenol sodium sulfuric acid continuous decomposition equipment, comprise phenol sodium pump, dilute sulfuric acid pump, jet mixer, the phenol sodium pump links to each other with the input aperture of jet mixer respectively by pipeline with dilute sulfuric acid pump, the delivery port of jet mixer links to each other with 2～5 grades of line mixers successively, be provided with 1～2 well heater between the line mixer, the most end one-level export pipeline of described line mixer links to each other with sulfuric acid decomposition and separation groove one, crude phenols line mixer and sulfuric acid decomposition and separation groove two successively, and two outlets of sulfuric acid decomposition and separation groove link to each other with the crude phenols groove.
Described well heater is located between two line mixers, and the heat transferring medium pipeline links to each other with warm water tube.
Described sulfuric acid decomposition and separation groove one is horizontal groove, and material is 904L.
The material of described jet mixer is Hastelloy B.
Compared with prior art, the invention has the beneficial effects as follows:
1) the phenates rate of decomposition is high, and the rate of recovery of phenol can realize scale operation more than 99% in the decomposition course.2) use 40%～60% dilute sulphuric acid in the reaction, the dosing apparatus material is required low, meet clean phenol sodium water solution after, the heat of dilution is low, can prevent effectively that jet mixer is corroded, and can effectively improve operating environment.3) heating unit is set and is conducive to sufficient reacting.
Description of drawings
Fig. 1 is process flow diagram of the present invention.
Among the figure: the clean phenol sodium of 1-groove 2-phenol sodium pump 3-jet mixer 4-line mixer 5-well heater 6-sulfuric acid decomposition and separation groove one 7-crude phenols line mixer 8-sulfuric acid decomposes phenol pump 9-sulfuric acid decomposition and separation groove two 10-crude phenols grooves one 11-crude phenols pump one 12-crude phenols groove two 13-crude phenols pumps two 14-concentrated sulfuric acid groove 15-vitriol oil pump 16-dilute sulphuric acid Preparation tank 17-complex acid recycle pump 18-complex acid recirculation cooler 19-dilute sulfuric acid pump 20-circulating water heaters
Embodiment
Below in conjunction with accompanying drawing the specific embodiment of the present invention is described further:
See Fig. 1, it is the clean phenol sodium of the present invention sulfuric acid continuous processing schematic flow sheet, comprise clean phenol sodium groove 1, phenol sodium pump 2, jet mixer 3, first step line mixer 4-1, second stage line mixer 4-2, third stage line mixer 4-3, fourth stage line mixer 4-4, sulfuric acid decomposition and separation groove 1, sulfuric acid decomposition and separation groove 29, well heater one 5-1, well heater 5-2 and dilute sulfuric acid pump 19 etc., phenol sodium pump 2 links to each other with the input aperture of jet mixer 3 respectively by pipeline with dilute sulfuric acid pump 19, the delivery port of jet mixer 3 successively with first step line mixer 4-1, second stage line mixer 4-2, third stage line mixer 4-3 and fourth stage line mixer 4-4 link to each other, wherein be provided with well heater one 5-1 between first step line mixer 4-1 and the second stage line mixer 4-2, be provided with well heater 5-2 between third stage line mixer 4-3 and the fourth stage line mixer 4-4, the export pipeline of fourth stage line mixer 4-4 successively with sulfuric acid decomposition and separation groove 1, crude phenols line mixer 7 links to each other with sulfuric acid decomposition and separation groove 29,29 outlets of sulfuric acid decomposition and separation groove link to each other with crude phenols groove 1, and one 10 outlets of crude phenols groove are successively through crude phenols pump 1, crude phenols groove 2 12 and crude phenols pump 2 13.
Sulfuric acid decomposition and separation groove 1 is horizontal, and to prolong the Reaction Separation time, material is stainless steel 904L.
The material of jet mixer 3 is Hastelloy B.
In the technique, be stored in the clean phenol na concn 18%-20% in the clean phenol sodium groove 1, extract pressurization out by clean phenol sodium pump 2, be adjusted to 2～3m
3Behind/h the flow, deliver to jet mixer 3, fully mix with 40%～60% dilute sulphuric acid of being sent here 400～450 l/h by dilute sulfuric acid pump 19, the phenates in the rough segmentation solution phenol and sulfuric acid generation chemical reaction generate crude phenols and sodium sulfate.The pH value that the PH meter of the injection rate of dilute sulphuric acid after according to fourth stage line mixer 4-4 shows determines that adopt the mode of variable frequency adjustment dilute sulfuric acid pump 19 motor speeds, the control pH value is 1～2.
Because phenates decomposes and belongs to thermo-negative reaction, so mixed mixed solution will replenish certain heat, to impel the thorough of chemical reaction, the heat transferring medium pipeline of well heater 5 links to each other with warm water tube, in additional heat, by postorder level Four line mixer 4, impel liquid mixing even; The mixed solution of last crude phenols and sodium sulfate enters sulfuric acid decomposition and separation groove one 6 standing separation, and the aqueous sodium persulfate solution that discharge the bottom is in flowing into and tank.
The crude phenols one that sulfuric acid decomposition and separation groove one 6 standing separation go out decompose phenol pump 8 by sulfuric acid and send into crude phenols line mixer 7, and its flow is regulated according to the liquid level automatic frequency-conversion of sulfuric acid decomposition and separation groove 1.At crude phenols line mixer 7 front adding service waters, to wash the free acid in the crude phenols off.Add the mixed crude phenols of water and enter sulfuric acid decomposition and separation groove 29 standing separation and get crude phenols two, water then flows into drainage tray; Crude phenols two are got to crude phenols groove 2 12 by crude phenols pump 1 again from flowing into crude phenols groove 1, are sent to oil depot by crude phenols pump 2 13 again.
Sulfuric acid decomposes 40%～60% dilute sulphuric acid of usefulness and is intermittently prepared by the complex acid operation, 93% the vitriol oil is stored in the concentrated sulfuric acid groove 14, during preparation, the amount of water of joining a groove 40%～60% dilute sulphuric acid according to calculating, disposable to dilute sulphuric acid Preparation tank 16 injection service waters, then inject the vitriol oil by vitriol oil pump 15 to dilute sulphuric acid Preparation tank 16, note during this time the variation of monitoring temperature, when injecting the vitriol oil, start complex acid recycle pump 17, by getting back to dilute sulphuric acid Preparation tank 16 after 18 coolings of complex acid recirculation cooler, to shift out the heat of dilution.The dilution temperature of sulfuric acid can not surpass 60 ℃, as near 60 ℃ the time, will stop to inject the vitriol oil, after treating that temperature lowers, continue to inject again the vitriol oil, join calculate good liquid level after, stop acid filling, continue circulating cooling, make the acid tank temperature remain on 50 ℃ ± 2 ℃.
Give the warm water of well heater 5 heat supplies, by circulating water heater 20 heat supplies, adopt steam-heated mode, Warm water circulation uses.
Claims (6)
1. clean phenol sodium sulfuric acid continuous decomposition process is characterized in that, clean sodium phenolate solution and 40%～60% dilute sulphuric acid enter sulfuric acid decomposition and separation groove and realize continuous decomposition after the multi-stage pipeline mixing tank mixes, be provided with heating unit in the mixing process, and its concrete steps are as follows:
1) flow 2～3m
340%～60% the dilute sulphuric acid of the clean sodium phenolate solution of the concentration 18%-20% of/h and flow 400～450 l/h mixes in jet mixer in proportion;
2) mixed solution mixes conveying through 2～5 grades of line mixers, PH behind the final stage line mixer is 1～2, be provided with 1～2 heating unit between the line mixer, mixed solution residence time in pipeline is 5～10 minutes, then enter in the sulfuric acid decomposition and separation groove one, in sulfuric acid decomposition and separation groove one, stop reaction after 180～240 minutes, get crude phenols one;
3) crude phenols enter sulfuric acid decomposition and separation groove two behind the crude phenols line mixer, and at crude phenols line mixer 7 front adding service waters, crude phenols one react to get product crude phenols two in sulfuric acid decomposition and separation groove two.
2. clean phenol sodium sulfuric acid continuous decomposition process according to claim 1 is characterized in that, the heating medium of described heating unit is 75 ℃～80 ℃ warm water.
3. the clean phenol sodium sulfuric acid continuous decomposition equipment that uses of the described technique of claim 1, it is characterized in that, comprise the phenol sodium pump, dilute sulfuric acid pump, jet mixer, the phenol sodium pump links to each other with the input aperture of jet mixer respectively by pipeline with dilute sulfuric acid pump, the delivery port of jet mixer links to each other with 2～5 grades of line mixers successively, be provided with 1～2 well heater between the line mixer, the most end one-level export pipeline of described line mixer successively with sulfuric acid decomposition and separation groove one, the crude phenols line mixer links to each other with sulfuric acid decomposition and separation groove two, and two outlets of sulfuric acid decomposition and separation groove link to each other with the crude phenols groove.
4. clean phenol sodium sulfuric acid continuous decomposition equipment according to claim 3 is characterized in that described well heater is located between two line mixers, and the heat transferring medium pipeline links to each other with warm water tube.
5. clean phenol sodium sulfuric acid continuous decomposition equipment according to claim 3 is characterized in that described sulfuric acid decomposition and separation groove one is horizontal groove, and material is 904L.
6. clean phenol sodium sulfuric acid continuous decomposition equipment according to claim 3 is characterized in that the material of described jet mixer is Hastelloy B.
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| CN2012104960218A CN102964220A (en) | 2012-11-28 | 2012-11-28 | Pure sodium phenolate sulfuric acid continuous decomposition technology and equipment thereof |
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| CN2012104960218A CN102964220A (en) | 2012-11-28 | 2012-11-28 | Pure sodium phenolate sulfuric acid continuous decomposition technology and equipment thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103242877A (en) * | 2013-04-25 | 2013-08-14 | 新疆鑫联煤化工有限公司 | Method for washing and decomposing industrial naphthalene in oil tar processing process |
| CN105777213A (en) * | 2016-02-04 | 2016-07-20 | 河南心连心化肥有限公司 | Urea-ammonium nitrate solution production device and control method thereof |
| CN112939746A (en) * | 2021-02-04 | 2021-06-11 | 中冶焦耐(大连)工程技术有限公司 | Pre-pump mixing tower type continuous washing dephenolizing process |
| CN113351139A (en) * | 2021-06-21 | 2021-09-07 | 天津辰力工程设计有限公司 | Equipment and method for producing crude phenol by decomposing sodium phenolate with sulfuric acid |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101407725A (en) * | 2008-08-18 | 2009-04-15 | 辽宁科技大学 | Novel process flow and apparatus for decomposing phenate |
| CN101642660A (en) * | 2009-09-02 | 2010-02-10 | 山西宏特煤化工有限公司 | Method for treating exhaust gas in process of producing crude phenol from coal tar |
| CN202953965U (en) * | 2012-11-28 | 2013-05-29 | 中冶焦耐工程技术有限公司 | Continuous decomposition device for pure phenol sodium sulfate |
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2012
- 2012-11-28 CN CN2012104960218A patent/CN102964220A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101407725A (en) * | 2008-08-18 | 2009-04-15 | 辽宁科技大学 | Novel process flow and apparatus for decomposing phenate |
| CN101642660A (en) * | 2009-09-02 | 2010-02-10 | 山西宏特煤化工有限公司 | Method for treating exhaust gas in process of producing crude phenol from coal tar |
| CN202953965U (en) * | 2012-11-28 | 2013-05-29 | 中冶焦耐工程技术有限公司 | Continuous decomposition device for pure phenol sodium sulfate |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103242877A (en) * | 2013-04-25 | 2013-08-14 | 新疆鑫联煤化工有限公司 | Method for washing and decomposing industrial naphthalene in oil tar processing process |
| CN105777213A (en) * | 2016-02-04 | 2016-07-20 | 河南心连心化肥有限公司 | Urea-ammonium nitrate solution production device and control method thereof |
| CN112939746A (en) * | 2021-02-04 | 2021-06-11 | 中冶焦耐(大连)工程技术有限公司 | Pre-pump mixing tower type continuous washing dephenolizing process |
| CN113351139A (en) * | 2021-06-21 | 2021-09-07 | 天津辰力工程设计有限公司 | Equipment and method for producing crude phenol by decomposing sodium phenolate with sulfuric acid |
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Application publication date: 20130313 |