CN103693730B - A kind of device and method of supercritical water oxidation method process high concentration hard-degraded organic waste water - Google Patents
A kind of device and method of supercritical water oxidation method process high concentration hard-degraded organic waste water Download PDFInfo
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Abstract
The present invention relates to a kind of device of supercritical water oxidation method process high concentration hard-degraded organic waste water, this device comprises jacketed type reactor (1), hydraulic efficiency plant (2), reactor pressure interlock control apparatus (3), sorbent material filling device (4), compressor (5), topping-up pump (6), intensification heating system (7), water cooler (8), back pressure control valve (9), gas-liquid separator (10); The present invention is by adding a certain amount of sorbent material (activated silica powder) in organic waste water, the two Homogeneous phase mixing is made together by agitator, enter in reactor, activated silica powder size is very little, can not result in blockage to pipeline, and can adsorb reacting the inorganic salt generated in reactor, then enter settling tank with product outflow reactor, by adding flocculation agent or natural sedimentation, after realizing sorbent material and process in settling tank, liquid is separated.This overcritical device, by the cooperation of jacketed type and hydraulic efficiency system, decreases the corrosion of equipment under supercritical state, reduces equipment cost; Simultaneously by adding sorbent material, avoiding the blockage problem of inorganic salt precipitation to equipment, being easy to realize industrialization.
Description
Technical field
The present invention relates to supercritical water oxidation method process high concentration hard-degraded organic waste water field, particularly a kind of device and method of supercritical water oxidation method process high concentration hard-degraded organic waste water, belongs to water treatment field.
Background technology
A kind of there is strong adaptability, applied widely, the consumption of save energy, the high concentration hard-degraded organic waste water treatment technology of processing efficiency high at supercritical water oxidation method (SCWO).Because supercritical water oxidation processing condition are harsh, high to the requirement of equipment, and the problem of the precipitation deposition occluding device of the corrosion of reactor and inorganic salt is not still effectively solved, and hinders the industrial applications of this technology.For this reason, corrosion and problem of saltouing is solved by being optimized design to reactor and complete assembly.
Supercritical water oxidation mainly contains for the main corrosion type of steel alloy: chemical corrosion and stress corrosion.Wherein, stress corrosion is the most dangerous, and ubiquity, serious destruction is caused to overcritical water oxidization reactor.The necessary requirement that stress corrosion cracking produces: one is have sensitive metal; Two is there is the medium had metal protection; Three is have stress to there is (usually having the greatest impact in case depositing of tensile stress).
The solubleness of inorganic salt in supercritical water is very little, compares with organism, and inorganic salt are almost insoluble, especially when temperature is more than 475 DEG C, inorganics solubleness in supercritical water reduces fast, and even does not dissolve completely, and inorganic salt will be separated out completely in supercritical water.The precipitation of inorganic salt, causes the Severe blockage of equipment Pipe-Line.
Summary of the invention
The object of the invention is to the equipment blocking avoiding the stress corrosion of reactor and the deposition of inorganic salt to cause, provide a set of supercritical water oxidation method process high concentration hard-degraded organic waste water device.
The present invention specifically provides following technical scheme: a kind of device of supercritical water oxidation method process high concentration hard-degraded organic waste water, is characterized in that: this device comprises jacketed type reactor (1), hydraulic efficiency plant (2), reactor pressure interlock control apparatus (3), sorbent material filling device (4), compressor (5), topping-up pump (6), intensification heating system (7), water cooler (8), back pressure control valve (9), gas-liquid separator (10); The hydraulic efficiency oil of jacketed type reactor is imported and exported and is connected by pipeline with hydraulic efficiency plant respectively; The automatic control system of hydraulic efficiency plant is connected by circuit with reactor pressure interlock control apparatus; Compressor inleting pipe road exports with oxygen canister and is connected, and compressor outlet is connected with the import of oxygen preheat device; Topping-up pump inlet ductwork exports with waste water tank and is connected, and booster pump outlet is connected with the import of waste water preheater; Oxygen preheat device export pipeline is connected with jacketed type reactor inner core reaction medium inlet pipeline by threeway with waste water preheater export pipeline; Jacketed type reactor inner core reaction medium export pipeline is connected with water cooler with reactor pressure interlock control apparatus respectively, and the pipeline connection of complete assembly all adopts thread connecting mode; Described sorbent material filling device (4), first sorbent material is chosen to be activated silica powder, and the number of its loadings, will determine according to the content of the concentration of handled waste water and impurity element; Sorbent material filling device (4) is arranged on the top of waste water tank, by the amount of filling regulating adsorbent outlet valve to control sorbent material, arranges an agitator simultaneously, after waste water and sorbent material are mixed uniformly, enter topping-up pump in waste water tank; The inorganic salt that sorbent material can be separated out in active adsorption reaction, and can with reaction product outflow reactor; Finally determine to realize in pond being separated of sorbent material and liquid heavy; To accelerate velocity of separation, appropriate flocculation agent can be added;
The inner core (19) of above-mentioned jacketed type reactor (1) is provided with inner core retaining plate (18), inner core (19) and urceolus (20) lower end are dome head, upper end is by upper end cover (12) and lower flange (13), pad (17) is placed up and down at inner core retaining plate (18), the isolated of the sealing of realization response still and inner core (19) and urceolus (20) is connected with bolt, inner core (19) medium is supercritical water oxidation medium, chuck layer medium between inner core (19) and urceolus (20) is hydraulic efficiency oil, urceolus is provided with 2 adapters, one of them adapter (14) makes hydraulic efficiency oil enter chuck layer between inner core (19) and urceolus (20), another adapter (15) is hydraulic oil outlet.
In said apparatus, oxygen is by compressor (5) supercharging, and organic waste water is by topping-up pump (6) supercharging, and the oxygen after supercharging and organic waste water are mixed into reactor inner core (19); Hydraulic efficiency oil injects in the chuck layer of reactor by hydraulic efficiency plant (2), reactor pressure interlock control apparatus (3) is connected with hydraulic efficiency system (2) with inner core (19) respectively, thus ensure that the interior pressure that the suffered reaction medium of inner core (19) causes is equal with the external pressure moment that chuck layer medium causes, such inner core (19) does not produce stress, and then avoids stress corrosion.
Above-mentioned inner core (19) Material selec-tion is the alloy material of corrosion-resistant (chemical corrosion), and without the need to considering the mechanical property of material, and wall thickness is thinner; Urceolus (20) Material selec-tion is the metallic substance of high temperature high voltage resistant, without the need to considering the corrosion resistance nature of material.
Above-mentioned jacketed type reactor (1) upper end adopts and detachably connects, and comprising: upper end cover, inner core retaining plate, lower flange, upper lower gasket, stud and nut; Its effect is: can repair inner core according to the extent of corrosion of inner core or change.
Present invention also offers a kind of method using the device of described supercritical water oxidation method process high concentration hard-degraded organic waste water to carry out wastewater treatment, it is characterized in that, described sorbent material filling device (4), first sorbent material is chosen to be activated silica powder, the number of its loadings, will determine according to the content of the concentration of handled waste water and impurity element; Sorbent material filling device (4) is arranged on the top of waste water tank, by the amount of filling regulating adsorbent outlet valve to control sorbent material, arranges an agitator simultaneously, after waste water and sorbent material are mixed uniformly, enter topping-up pump in waste water tank; The inorganic salt that sorbent material can be separated out in active adsorption reaction, and can with reaction product outflow reactor; Finally determine to realize in pond being separated of sorbent material and liquid heavy; Described jacketed type reactor (1) upper end adopts and detachably connects, and comprising: upper end cover, inner core retaining plate, lower flange, upper lower gasket, stud and nut; It can be repaired inner core according to the extent of corrosion of inner core or change.
Preferably, determine in pond, to add appropriate flocculation agent, to accelerate velocity of separation above-mentioned sinking;
Preferably, above-mentioned sorbent material is chosen to be activated silica powder.
Described activated silica powder take flyash as raw material, prepares as follows:
(1) weigh a certain amount of flyash, add the sodium hydroxide solution of 8mol/L, maintenance solid-to-liquid ratio is 1:2-1:3, heats and stirs, reaction 1-2 hour; Suction filtration, gets filtrate stirred, and adds the surfactant polyethylene being about solute NaSiO3 quality 1%-5% in the process stirred, and passes into carbon dioxide gas precursor reactant 1-2 hour subsequently; Get filter residue after suction filtration to produce to bubble-free with the hydrochloric acid drip washing of 5%-10%, vacuum-drying, obtained nano SiO 2 particle;
(2) get polyacrylonitrile (PAN) and be fully dissolved in DMF (DMF), be configured to the PAN/DMF solution of 10-15%.
(3) getting nano SiO 2 particle is dissolved in PAN/DMF solution, and fully stir, mix, wherein the mol ratio of PAN and silica dioxide granule is 1:1-1:2.
(4) be receptor with aluminium foil and accompany by high-voltage power supply and carry out spinning;
(5) by tube furnace calcination, remove the organism in tunica fibrosa, obtain silica fiber;
(6) reduce with MAGNESIUM METAL or gac the silica fiber obtained, then use the dilute hydrochloric acid solution of 5%-10%, soak removal of impurities and obtain activated silica sorbing material.
A certain amount of sorbent material (activated silica powder) is dosed in organic waste water, and make the two Homogeneous phase mixing together by agitator, enter in reactor, activated silica powder granularity is very little, can not result in blockage to pipeline, and can adsorb reacting the inorganic salt generated in reactor, then with product outflow reactor, last in settling tank, by adding flocculation agent or natural sedimentation, after realizing sorbent material and processing, liquid is separated.Wherein, the number of adsorbent inventory, will determine according to the content of the concentration of handled waste water and impurity element.
The present invention has the following advantages:
(1) be jacketed kettle reactor by reactor design, this reactor thoroughly can be avoided the most serious in supercritical Water Oxidation Technology and endanger maximum stress corrosion phenomena to equipment.Thus in equipment running process, can not stress corrosion cracking be produced, ensure that the long-term safety of equipment is run, the work-ing life of extension reactor.In addition, the wall ratio of inner core is thinner, has greatly saved the use of corrosion-resisting alloy steel.
(2) hydraulic efficiency system and reactor pressure interlock control apparatus ensure that reactor inner core is identical with the chuck stressor layer moment.Avoid inner core be flattened due to the existence of pressure difference in operational process or crush.
(3) in organic waste water, dose a certain amount of activated silica powder, the inorganic salt can separated out in active adsorption reaction process, effectively reduce the fouling of inorganic salt at inner core inwall, on the one hand, the deposition avoiding inorganic salt causes the blocking of pipeline; On the other hand, improve heat transfer efficiency.
(4) upper end cover of reactor is designed to dismountable flange connect, inner core is fixed on inner core retaining plate, inner core retaining plate has pad respectively with upper end cover and lower flange by tools for bolts ' pretension compress gasket, realize sealing.Removably connect, according to the corrosion condition of inner core, inner core can be repaired or change.
Below in conjunction with the drawings and specific embodiments, the invention will be further described.
Accompanying drawing explanation
Fig. 1 is supercritical water oxidation method process high concentration hard-degraded organic waste water device of the present invention, wherein, 1, jacketed type reactor 2, hydraulic efficiency plant 3, reactor pressure interlock control apparatus 4, sorbent material filling device 5, compressor 6, topping-up pump 7, intensification heating system 8, water cooler 9, back pressure control valve 10, gas-liquid separator 21, waste water tank 22, agitator 23, oxygen canister 24, hand increasing pressure pump 25, settling tank A, cold water enters B, cold water goes out C, gas D, water after process;
Fig. 2 is the structural representation of jacketed type reactor of the present invention, wherein, 11, inner core reaction medium inlet 12, upper end cover 13, lower flange 14, urceolus hydraulic oil inlet 15, urceolus hydraulic oil outlet 16, inner core reacting product outlet 17, pad 18, inner core retaining plate 19, inner core 20, urceolus.
Embodiment
As shown in Figure 1, supercritical water oxidation method process high concentration hard-degraded organic waste water device of the present invention, comprises jacketed type reactor (1), hydraulic efficiency plant (2), reactor pressure interlock control apparatus (3), sorbent material filling device (4), compressor (5), topping-up pump (6), intensification heating system (7), water cooler (8), back pressure control valve (9), gas-liquid separator (10).
As shown in Figure 2, jacketed type reactor (1) feature is: reactor form is jacketed type, inner core (19) is provided with inner core retaining plate (18), inner core (19) and urceolus (20) lower end are dome head, upper end is by upper end cover (12) and lower flange (13), and place pad (17) up and down at inner core retaining plate (18), the isolated of the sealing of realization response still and inner core (19) and urceolus (20) is connected with bolt, inner core (19) medium is supercritical water oxidation medium, chuck layer medium between inner core (19) and urceolus (20) is hydraulic efficiency oil.Urceolus is provided with 2 adapters, and one of them adapter (14) makes hydraulic efficiency oil enter chuck layer between inner core (19) and urceolus (20), and another takes over (15) is hydraulic oil outlet.Be provided with 2 adapters at upper end cover, an adapter (11) is reaction medium entrance, and another adapter (16) is reacting product outlet.
Specific works process is as follows:
Oxygen is squeezed in respective preheater by compressor (5) and topping-up pump (6) with the organic waste water having dosed sorbent material (activated silica powder) respectively, and the oxygen after preheating enters reactor inner core (19) after mixing with the organic waste water after preheating.Reactor is provided with heating system, and heats up to the medium entered in reactor, is warming up to more than supercritical temperature.Pressure in device carries out regulating and controlling by hand increasing pressure pump and back pressure control valve (9), to slowly carry out at boost process, the amplitude of each boosting is 2MPa to the maximum, until inner core (19) pressure medium and hydraulic efficiency oil in urceolus (20) pressure-stabilisation and identical after, carry out the boosting of next time.The pressure medium of reactor inner core (19) is provided by topping-up pump (6) and compressor (5), chuck layer hydraulic fluid pressure between urceolus and inner core is provided by hydraulic efficiency plant (2), reactor pressure interlock control apparatus (3) exports with inner core (19) respectively and hydraulic efficiency plant (2) is connected, to ensure that inner core (19) pressure and chuck stressor layer moment keep identical.When pressure-stabilisation is more than supercritical water pressure, there is fully reaction in the reaction medium in reactor, organism is fully degraded.Impurity element in reaction process except C, H, O changes corresponding inorganic salt into, and separates out in reactor, dosing of activated silica powder, can effectively adsorb the inorganic salt of separating out, and avoids the blocking of inorganic salt at inner core encrustation and pipeline.Activated silica powder after absorption inorganic salt can leave reactor jointly with reaction product, after supercooler (8) is lowered the temperature, enters gas-liquid separator (10), realize gas-liquid separation through back pressure control valve (9).Liquid after separation enters settling tank, and in settling tank, realize being separated of sorbent material and liquid, its method is natural subsidence, to accelerate its velocity of separation, can add appropriate flocculation agent.
Claims (8)
1. a device for supercritical water oxidation method process high concentration hard-degraded organic waste water, is characterized in that: this device comprises jacketed type reactor (1), hydraulic efficiency plant (2), reactor pressure interlock control apparatus (3), sorbent material filling device (4), compressor (5), topping-up pump (6), intensification heating system (7), water cooler (8), back pressure control valve (9), gas-liquid separator (10); The hydraulic efficiency oil of jacketed type reactor is imported and exported and is connected by pipeline with hydraulic efficiency plant respectively; The automatic control system of hydraulic efficiency plant is connected by circuit with reactor pressure interlock control apparatus; Compressor inleting pipe road exports with oxygen canister and is connected, and compressor outlet is connected with the import of oxygen preheat device; Topping-up pump inlet ductwork exports with waste water tank and is connected, and booster pump outlet is connected with the import of waste water preheater; Oxygen preheat device export pipeline is connected with jacketed type reactor inner core reaction medium inlet pipeline by threeway with waste water preheater export pipeline; Jacketed type reactor inner core reaction medium export pipeline is connected with water cooler with reactor pressure interlock control apparatus respectively, and the pipeline connection of complete assembly all adopts thread connecting mode; Described sorbent material filling device (4), first sorbent material is chosen to be activated silica powder, and the number of its loadings, will determine according to the content of the concentration of handled waste water and impurity element; Sorbent material filling device (4) is arranged on the top of waste water tank, by the amount of filling regulating adsorbent outlet valve to control sorbent material, arranges an agitator simultaneously, after waste water and sorbent material are mixed uniformly, enter topping-up pump in waste water tank.
2. the device of supercritical water oxidation method process high concentration hard-degraded organic waste water as claimed in claim 1, it is characterized in that, the inner core (19) of described jacketed type reactor (1) is provided with inner core retaining plate (18), inner core (19) and urceolus (20) lower end are dome head, upper end is by upper end cover (12) and lower flange (13), pad (17) is placed up and down at inner core retaining plate (18), the isolated of the sealing of realization response still and inner core (19) and urceolus (20) is connected with bolt, inner core (19) medium is supercritical water oxidation medium, chuck layer medium between inner core (19) and urceolus (20) is hydraulic efficiency oil, urceolus is provided with 2 adapters, one of them adapter (14) makes hydraulic efficiency oil enter chuck layer between inner core (19) and urceolus (20), another adapter (15) is hydraulic oil outlet.
3. the device of supercritical water oxidation method process high concentration hard-degraded organic waste water as claimed in claim 2, it is characterized in that, oxygen is by compressor (5) supercharging, organic waste water is by topping-up pump (6) supercharging, and the oxygen after supercharging and organic waste water are mixed into reactor inner core (19); Hydraulic efficiency oil is injected in the chuck layer of reactor by hydraulic efficiency plant (2), and reactor pressure interlock control apparatus (3) is connected with hydraulic efficiency plant (2) with inner core (19) respectively.
4. the device of supercritical water oxidation method process high concentration hard-degraded organic waste water as claimed in claim 2, it is characterized in that, described inner core (19) Material selec-tion is the alloy material of corrosion-resistant (chemical corrosion), and without the need to considering the mechanical property of material, and wall thickness is thinner; Urceolus (20) Material selec-tion is the metallic substance of high temperature high voltage resistant, without the need to considering the corrosion resistance nature of material.
5. the device of supercritical water oxidation method process high concentration hard-degraded organic waste water as claimed in claim 2, it is characterized in that, described jacketed type reactor (1) upper end adopts and detachably connects, and comprising: upper end cover, inner core retaining plate, lower flange, upper lower gasket, stud and nut.
6. the method using the device of the supercritical water oxidation method process high concentration hard-degraded organic waste water as described in any one of claim 1-5 to carry out wastewater treatment, it is characterized in that, described sorbent material filling device (4), first sorbent material is chosen to be activated silica powder, the number of its loadings, will determine according to the content of the concentration of handled waste water and impurity element; Sorbent material filling device (4) is arranged on the top of waste water tank, by the amount of filling regulating adsorbent outlet valve to control sorbent material, arranges an agitator simultaneously, after waste water and sorbent material are mixed uniformly, enter topping-up pump in waste water tank; The inorganic salt that sorbent material can be separated out in active adsorption reaction, and can with reaction product outflow reactor; Finally determine to realize in pond being separated of sorbent material and liquid heavy; To accelerate velocity of separation, add appropriate flocculation agent; Described jacketed type reactor (1) upper end adopts and detachably connects, and comprising: upper end cover, inner core retaining plate, lower flange, upper lower gasket, stud and nut; It to be repaired inner core according to the extent of corrosion of inner core or changes.
7. method as claimed in claim 6, it is characterized in that, described activated silica powder take flyash as raw material, prepares as follows:
(1) weigh a certain amount of flyash, add the sodium hydroxide solution of 8mol/L, maintenance solid-to-liquid ratio is 1:2-1:3, heats and stirs, reaction 1-2 hour; Suction filtration, gets filtrate stirred, and is incorporated as solute NaSiO in the process stirred
3the surfactant polyethylene of quality 1%-5%, passes into carbon dioxide gas precursor reactant 1-2 hour subsequently; Get filter residue after suction filtration to produce to bubble-free with the hydrochloric acid drip washing of 5%-10%, vacuum-drying, obtained nano SiO 2 particle;
(2) get polyacrylonitrile (PAN) and be fully dissolved in DMF (DMF), be configured to the PAN/DMF solution of 10-15%;
(3) getting nano SiO 2 particle is dissolved in PAN/DMF solution, and fully stir, mix, wherein the mol ratio of PAN and silica dioxide granule is 1:1-1:2;
(4) be receptor with aluminium foil and accompany by high-voltage power supply and carry out spinning;
(5) by tube furnace calcination, remove the organism in tunica fibrosa, obtain silica fiber;
(6) reduce with MAGNESIUM METAL or gac the silica fiber obtained, then use the dilute hydrochloric acid solution of 5%-10%, soak removal of impurities and obtain activated silica sorbing material.
8. method as claimed in claims 6 or 7, is characterized in that, describedly heavyly determines to add appropriate flocculation agent in pond, to accelerate velocity of separation.
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| CN105540697B (en) * | 2016-01-21 | 2018-10-19 | 西南石油大学 | The processing unit and method of a kind of high temperature and pressure to waste liquid of drilling |
| CN107698012B (en) * | 2017-10-20 | 2024-02-13 | 吴丹丹 | Horizontal self-balancing supercritical reaction device |
| CN108726774A (en) * | 2018-05-29 | 2018-11-02 | 内蒙古工业大学 | Device and method that is a kind of while removing salt and organic pollution in organic wastewater |
| CN108751383B (en) * | 2018-08-16 | 2023-11-21 | 成都九翼环保科技有限公司 | Countercurrent supercritical water oxidation kettle type reactor and preparation method and application thereof |
| CN109351284A (en) * | 2018-10-26 | 2019-02-19 | 北京航天新风机械设备有限责任公司 | A kind of organic liquid waste feed process applied to continuous supercritical water method for oxidation |
| CN109991157B (en) * | 2019-04-08 | 2021-04-13 | 中国核动力研究设计院 | High-temperature high-pressure water corrosion product dissolution and release device |
| CN110527943B (en) * | 2019-08-06 | 2021-01-19 | 西安交通大学 | Device and method for performing anti-corrosion treatment on magnesium and magnesium alloy by using supercritical carbon dioxide |
| CN111573819B (en) * | 2020-06-01 | 2022-04-26 | 中国科学院重庆绿色智能技术研究院 | Anti-blocking agent for supercritical water heat treatment system of high-salinity organic waste and anti-blocking method for equipment |
| CN114735801A (en) * | 2022-03-16 | 2022-07-12 | 石家庄新奥环保科技有限公司 | Supercritical water oxidation reactor |
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