CN106365124B - A kind of system and technique for dioxygen water security extracting and purifying - Google Patents

A kind of system and technique for dioxygen water security extracting and purifying Download PDF

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Publication number
CN106365124B
CN106365124B CN201610761819.9A CN201610761819A CN106365124B CN 106365124 B CN106365124 B CN 106365124B CN 201610761819 A CN201610761819 A CN 201610761819A CN 106365124 B CN106365124 B CN 106365124B
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extraction
raffinate
gas
extraction tower
working solution
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CN106365124A (en
Inventor
肖光
张文杰
付晓华
王东
曹倩
李红燕
刘立彬
荣红焕
孙景双
陶红
李静敏
甄亭亭
杨莉
许婷婷
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Liaocheng Luxi Chemical Engineering Co Ltd
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Liaocheng Luxi Chemical Engineering Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B15/00Peroxides; Peroxyhydrates; Peroxyacids or salts thereof; Superoxides; Ozonides
    • C01B15/01Hydrogen peroxide
    • C01B15/013Separation; Purification; Concentration

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Physical Water Treatments (AREA)

Abstract

The invention discloses a kind of system and technique for dioxygen water security extracting and purifying, including extraction tower, extraction raffinate separator, working solution measuring tank and inert gas source, the raffinate on the top of extraction tower enters working solution measuring tank after entering extraction raffinate separator separation water, and inert gas source pours inert gas to the gas-phase space of the gas-phase space of extraction tower, the gas-phase space of extraction raffinate separator and working solution measuring tank respectively.The raffinate on extraction tower top, separated by stainless steel metal filler, extraction raffinate separator is entered by raffinate outlet guillotine overflow, raffinate enters working solution measuring tank after water is separated in extraction raffinate separator, and the water of extraction raffinate separator bottom mutually enters spent acidic working solution storage tank;Inert gas is passed through to the gas-phase space progress inert gas shielding of extraction tower, extraction raffinate separator, working solution measuring tank;Extraction tower is individually vented, and working solution measuring tank is vented after merging with extraction raffinate separator blow-down pipe.

Description

A kind of system and technique for dioxygen water security extracting and purifying
Technical field
The present invention relates to a kind of system and technique for dioxygen water security extracting and purifying.
Background technology
At present, the leading technology of Hydrogen Peroxide Production is palladium catalyst -- anthraquinone hydrogenation process, and it is single which is divided into hydrogenation Member, oxidation unit, extracting and purifying unit, post-processing unit, alkali evaporation etc..The technique extracting and purifying cell process flow is as follows: Using the difference and the density contrast of working solution and water of solubility of the hydrogen peroxide in water and working solution, pure water is used in extraction tower The working solution containing hydrogen peroxide is extracted, obtains the aqueous solution of hydrogen peroxide.The aqueous solution of hydrogen peroxide is in purifying column through weight Aromatic hydrocarbons purified treatment, you can obtain the hydrogen peroxide that concentration is 27.5%.The raffinate on extraction tower top overflows to extraction by pipeline After extraction raffinate separator, into post-processing unit.
The dangerous string from extraneous different material of extracting and purifying process mixes the introducing of impurity.In extraction tower cleaning system In there are hydrogen peroxide, every impurity that it can be promoted to decompose (such as:Metal ion, lye, catalyst fines, alumina powder Deng) it can make its decomposition, active oxygen is produced, and release heat, cause temperature, pressure to raise rapidly, material is from system drain Or equipment weakness sprays, burning, explosion occurs.
Extracting and purifying unit is atmospheric operation, as shown in Figure 1, extraction tower 101, extraction raffinate separator 102 in traditional handicraft Emptying is concentrated again after being concomitantly introduced into high-order material collecting tank 104 with the blow-down pipe of working solution measuring tank 103.101 top of extraction tower Raffinate outlet to 102 import of extraction raffinate separator there are about 10 meters of potential differences, and during raffinate overflow, substantial amounts of air is from extraction tower 101 top drains enter, and enter extraction raffinate separator 102 with raffinate, extremely easy to produce static electricity.Furthermore extraction tower 101 pushes up Portion is aromatic hydrocarbons steam, if misoperation or other reasons cause that decomposing hydrogen dioxide solution is uncontrollable in extraction tower 101, it is easy to make extraction Take the heavy aromatics generation sudden strain of a muscle in 101 top gas phase space of tower quick-fried.
The content of the invention
The defects of to overcome the prior art, the invention discloses a kind of system and work for dioxygen water security extracting and purifying Skill, solve in traditional handicraft extraction tower top gas phase space dodge it is quick-fried, and the problem of cause security incident to occur.
To achieve the above object, the technical scheme is that:
Stainless steel is filled in a kind of extraction tower for dioxygen water security extracting and purifying, the upper part of the extraction tower from section Filler, the gas-phase space of the upper part of the extraction tower is interior to be equipped with gas distributor, the stainless steel helices and gas distributor Between raffinate outlet at be equipped with raffinate outlet guillotine, gas-liquid separation is equipped with the top drain of the extraction tower and is filled Put, wherein, the raffinate outlet guillotine is the pipeline stretched at raffinate outlet to extraction tower inside, and the pipeline is remote One end closure at raffinate outlet, and the pipeline for blocking side is semicanal, the semicanal is that the section axially sectioned along pipeline is The groove of " U " row.
The raffinate guillotine can shut off raffinate, and raffinate is gone out extraction tower along groove overflow of " U " row.
Preferably, it is equipped with oxygen content in-line analyzer in the gas-phase space of the extraction tower.Extraction tower can be monitored in real time The oxygen content of gas-phase space.
Preferably, the semicanal is arranged on the underface of the gas-liquid separation device.It can ensure overwhelming majority extraction of shutting off Extraction raffinate.
Preferably, the groove two-arm top is equipped with some fillet saw-tooth-type structures.Be conducive to relieving stagnant Qi, reduce raffinate Outlet line liquid band gas problem.
Preferably, the gas distributor is the endless tube for opening up several holes.
Preferably, the gas-liquid separation device includes inner cylinder and outer barrel, and the inner cylinder is arranged in outer barrel, the inner cylinder with The axial direction of outer barrel is identical, and gap is equipped between the outer barrel and inner cylinder, and baffle, the inner cylinder side wall are equipped with the top of the inner cylinder Some uniform strip holes are opened up, some diversion pipes are equipped with the downside of the gap between the outer barrel and inner cylinder.
It is further preferred that the diameter of the baffle is slightly larger than inner diameter of steel flue, and the diameter of the baffle is straight less than outer barrel Footpath.It is further ensured that and efficiently carries out gas-liquid separation.
Preferably, the raffinate outlet pipeline guides to tower top by a gas phase pipe.Be conducive to extraction tower top and raffinate Outlet line balances.
A kind of application of above-mentioned extraction tower in dioxygen water security extracting and purifying system or technique.
A kind of system for dioxygen water security extracting and purifying, including above-mentioned extraction tower.
A kind of system for dioxygen water security extracting and purifying, including above-mentioned extraction tower, inert gas source, the inert gas source Outlet connection gas distributor.
A kind of system for dioxygen water security extracting and purifying, including above-mentioned extraction tower, extraction raffinate separator, working solution meter Measuring tank and inert gas source, the raffinate on the top of the extraction tower, which enters after extraction raffinate separator separates water, enters working solution metering Groove, inert gas source pour inert gas to the gas-phase space of extraction tower, the gas-phase space of extraction raffinate separator and work respectively The gas-phase space of liquid measuring tank, the blow-down pipe at the top of the extraction tower is separately provided, and is not merged with other blow-down pipes, institute The blow-down pipe for stating working solution measuring tank merges with extraction raffinate separator blow-down pipe.
Preferably, the connecting pipe between the inert gas source and extraction tower is equipped with inflation regulating valve.
A kind of technique of safe extracting and purifying using said system, the raffinate on extraction tower top, by stainless steel gold Belong to filler to be separated, extraction raffinate separator is entered by raffinate outlet guillotine overflow, raffinate is in extraction raffinate separator Enter working solution measuring tank after separation water, the water of extraction raffinate separator bottom mutually enters spent acidic working solution storage tank;By indifferent gas Body is passed through extraction tower, extraction raffinate separator, the gas-phase space of working solution measuring tank and carries out inert gas shielding;Extraction tower is individually put Sky, working solution measuring tank are vented after merging with extraction raffinate separator blow-down pipe.
Preferably, control extraction column overhead keeps micro-positive pressure, while controls extraction tower gas-phase space oxygen content to be less than 8%.
Preferably, the inert gas is nitrogen, and the inert gas source is source nitrogen.Using nitrogen, cost is reduced.
Compared with traditional handicraft, beneficial effects of the present invention are:Reduce extraction tower, extraction raffinate separator and working solution metering The gas-phase space in groove top portion, by 35.9m3Reduce to 24.3m3;Extraction tower top segregation section, which is provided with, has special efficient separation effect The stainless steel helices of fruit, ensure that raffinate is far below normal process index in raffinate under 108% load;Emptying at the top of extraction tower Gas-liquid separation device is provided with mouthful, reduces the consumption of heavy aromatics in system;Extraction tower, extraction raffinate separator and working solution meter The top gas phase such as measuring tank space, which takes, rushes nitrogen safeguard measure, whole gas-phase space oxygen content is less than 8%, ensure that hydrogen peroxide Device long period safe and stable operation.
Brief description of the drawings
Fig. 1 is the process flow chart of traditional extraction clean unit;
Fig. 2 is the process flow chart of the present invention;
Fig. 3 is the structure diagram on extraction tower top of the present invention;
Wherein, 101. extraction tower, 102. extraction raffinate separators, 103. working solution measuring tanks, 104. high-order material collecting tanks, 1. extractions Taking tower, 2. extraction raffinate separators, 3. working solution measuring tanks, 4. source nitrogens, 5. rush nitrogen regulating valve, 21. raffinate outlet guillotines, 22. stainless steel metal filler, 23. nitrogen distributors, 24. gas-liquid separation devices, 25. diversion pipes, v. connected entrances.
Embodiment
The invention will be further described below in conjunction with the accompanying drawings.
A kind of extraction tower for dioxygen water security extracting and purifying, as shown in figure 3, the segregation section of the upper part of extraction tower is filled out Stainless steel helices 22 is filled, nitrogen distributor 23, stainless steel helices 22 and nitrogen are equipped with the gas-phase space of the upper part of extraction tower Raffinate outlet guillotine 21 is equipped with raffinate outlet between distributor 23, gas-liquid is equipped with the top drain of extraction tower Separator 24, wherein, raffinate outlet guillotine 21 is the pipeline stretched at raffinate outlet to extraction tower inside, and pipeline is remote From one end closure at raffinate outlet, and the pipeline for blocking side is semicanal, and semicanal is that the section axially sectioned along pipeline is " U " Capable groove.
Semicanal is arranged on the underface of gas-liquid separation device 24, can ensure most raffinates that shut off.Groove two-arm Top is equipped with some fillet saw-tooth-type structures.Be conducive to relieving stagnant Qi, reduce raffinate outlet pipeline liquid band gas problem.Raffinate goes out Mouth pipeline guides to top gaseous phase connected entrance v by a gas phase pipe.Be conducive to balance with raffinate outlet pipeline at the top of extraction tower;At the same time Ensure that the portion gas in outlet line is returned at the top of extraction tower, reduce excessive gas and enter extraction raffinate separator.
Nitrogen distributor 23 is the endless tube for opening up several holes.
Gas-liquid separation device 24 includes inner cylinder and outer barrel, and inner cylinder is arranged in outer barrel, and inner cylinder is identical with the axial direction of outer barrel, and Gap is equipped between outer barrel and inner cylinder, is equipped with baffle at the top of inner cylinder, the diameter of baffle is slightly larger than inner diameter of steel flue, and the diameter of baffle Less than outer barrel diameter, inner cylinder side wall opens up some uniform strip holes, and the long side of strip hole is parallel with the axis of inner cylinder, outer barrel with it is interior 4 diversion pipes 25 are uniformly provided with the downside of gap between cylinder.
Extract column overhead and two sets of far transmission level meters of tool are set, control interlocking, ceiling value termination of pumping, system are formed with oxidation liquid pump Parking.
Extract column overhead and oxygen content on-line analysis mouth is set, the detector of oxygen content in-line analyzer divides online from oxygen content Analysis mouth stretches to the gas-phase space of extraction tower.
A kind of system for dioxygen water security extracting and purifying, as shown in Fig. 2, being separated including above-mentioned extraction tower 1, raffinate Device 2, working solution measuring tank 3 and source nitrogen 4, the raffinate on the top of the extraction tower 1 enter after extraction raffinate separator 2 separates water Into working solution measuring tank 3, source nitrogen 4 pours inert gas to the gas-phase space of extraction tower 1, extraction raffinate separator 2 respectively Gas-phase space and working solution measuring tank 3 gas-phase space, the blow-down pipe at the top of the extraction tower 1 is separately provided, and not with Other blow-down pipes merge, and the blow-down pipe of the working solution measuring tank 3 merges with 2 blow-down pipe of extraction raffinate separator, no longer High-order material collecting tank after emptying is set.Connecting pipe between source nitrogen 4 and extraction tower 1, which is equipped with, rushes nitrogen regulating valve 5.
A kind of technique for dioxygen water security extracting and purifying, as Figure 2-3,
(1) raffinate on 1 top of extraction tower, is separated by the efficient stainless steel metal filler 22 in top, passes through outlet 21 overflow of guillotine enters extraction raffinate separator 2, and raffinate enters working solution measuring tank 3 after water is separated in extraction raffinate separator 2; The water of 2 bottom of extraction raffinate separator mutually enters spent acidic working solution storage tank.
(2) extraction tower 1, extraction raffinate separator 2, the gas-phase space of working solution measuring tank 3 carry out rushing nitrogen protection.Extraction tower 1 The oxygen content on-line analysis that upper gaseous phase space is provided with, forms control loop with rushing nitrogen regulating valve 5, ensures the top of extraction tower 1 Micro-positive pressure, gas-phase space Control for Oxygen Content is below 8%.
(3) extraction tower 1 is individually vented, and working solution measuring tank 3 is vented after merging with 2 blow-down pipe of extraction raffinate separator, no High-order material collecting tank after emptying is set again.
Although above-mentioned be described the embodiment of the present invention with reference to attached drawing, not to invention protection domain Limitation, those skilled in the art should understand that, on the basis of technical scheme, those skilled in the art are not required to Make the creative labor the various modifications that can be made or deformation is still within the scope of the present invention.

Claims (6)

1. a kind of system for dioxygen water security extracting and purifying, it is characterized in that, including extraction tower, extraction raffinate separator, work Liquid measuring tank and inert gas source, the raffinate on the top of the extraction tower, which enters after extraction raffinate separator separates water, enters working solution Measuring tank, inert gas source inert gas is filled with respectively to the gas-phase space of extraction tower, extraction raffinate separator gas-phase space and The gas-phase space of working solution measuring tank, the blow-down pipe at the top of the extraction tower are separately provided, and are not closed with other blow-down pipes And the blow-down pipe of the working solution measuring tank merges with extraction raffinate separator blow-down pipe;
Stainless steel helices is filled in the upper part of the extraction tower from section, is equipped with the gas-phase space of the upper part of the extraction tower Gas distributor, is equipped with raffinate outlet guillotine at the raffinate outlet between the stainless steel helices and gas distributor, Gas-liquid separation device is equipped with the top drain of the extraction tower, wherein, the raffinate outlet guillotine goes out for raffinate The pipeline stretched at mouthful to extraction tower inside, the pipeline block the pipeline of side away from one end closure at raffinate outlet For semicanal, the semicanal is the groove that the section axially sectioned along pipeline is U-typed.
2. the system as claimed in claim 1, it is characterized in that, the semicanal is arranged on the underface of the gas-liquid separation device.
3. the system as claimed in claim 1, it is characterized in that, the groove two-arm top is equipped with some fillet sawtooth pattern knots Structure.
4. the system as claimed in claim 1, it is characterized in that, the gas-liquid separation device includes inner cylinder and outer barrel, the inner cylinder It is arranged in outer barrel, the inner cylinder is identical with the axial direction of outer barrel, and gap is equipped between the outer barrel and inner cylinder, the inner cylinder top Portion is equipped with baffle, and the inner cylinder side wall opens up some uniform strip holes, if being equipped with the downside of the gap between the outer barrel and inner cylinder Dry diversion pipe.
5. the system as claimed in claim 1, it is characterized in that, the raffinate outlet pipeline guides to tower top by a gas phase pipe.
6. a kind of technique of the safe extracting and purifying of system using as described in claim 1-5 is any, the extraction on extraction tower top Extraction raffinate, is separated by stainless steel metal filler, enters extraction raffinate separator, raffinate by raffinate outlet guillotine overflow Enter working solution measuring tank after water is separated in extraction raffinate separator, the water of extraction raffinate separator bottom mutually enters spent acidic and works Liquid storage tank;Inert gas is passed through to the gas-phase space progress inert gas guarantor of extraction tower, extraction raffinate separator, working solution measuring tank Shield;Extraction tower is individually vented, and working solution measuring tank is vented after merging with extraction raffinate separator blow-down pipe.
CN201610761819.9A 2016-08-30 2016-08-30 A kind of system and technique for dioxygen water security extracting and purifying Active CN106365124B (en)

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Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110860099B (en) * 2019-11-14 2022-03-04 聊城市鲁西化工工程设计有限责任公司 Multi-quality hydrogen peroxide concentration device and process and application thereof
CN114162789B (en) * 2021-12-30 2023-03-24 连云港市工投集团利海化工有限公司 Process and device for preparing hydrogen peroxide

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0782540B1 (en) * 1994-09-21 1999-05-12 Solvay Interox Limited Reactor and process for producing calcium peroxide
CN202387249U (en) * 2011-12-28 2012-08-22 湖南兴鹏化工科技有限公司 Combined perforated-plate extraction tower
CN103449380A (en) * 2012-06-04 2013-12-18 扬州荣祥化工技术开发设计有限公司 Anthraquinone method hydrogen peroxide extraction tower
CN204211485U (en) * 2014-11-04 2015-03-18 杭州名鑫双氧水有限公司 Hydrogen peroxide production system
CN105731385A (en) * 2016-03-29 2016-07-06 福建永荣科技有限公司 Hydrogen peroxide oxidization extracting tower and method

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0782540B1 (en) * 1994-09-21 1999-05-12 Solvay Interox Limited Reactor and process for producing calcium peroxide
CN202387249U (en) * 2011-12-28 2012-08-22 湖南兴鹏化工科技有限公司 Combined perforated-plate extraction tower
CN103449380A (en) * 2012-06-04 2013-12-18 扬州荣祥化工技术开发设计有限公司 Anthraquinone method hydrogen peroxide extraction tower
CN204211485U (en) * 2014-11-04 2015-03-18 杭州名鑫双氧水有限公司 Hydrogen peroxide production system
CN105731385A (en) * 2016-03-29 2016-07-06 福建永荣科技有限公司 Hydrogen peroxide oxidization extracting tower and method

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