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CN103058406A - Device and technology employed to hydrogen peroxide purification - Google Patents

Device and technology employed to hydrogen peroxide purification Download PDF

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Publication number
CN103058406A
CN103058406A CN2013100117237A CN201310011723A CN103058406A CN 103058406 A CN103058406 A CN 103058406A CN 2013100117237 A CN2013100117237 A CN 2013100117237A CN 201310011723 A CN201310011723 A CN 201310011723A CN 103058406 A CN103058406 A CN 103058406A
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China
Prior art keywords
hydrogen peroxide
film separating
separating system
pump
phase separator
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Pending
Application number
CN2013100117237A
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Chinese (zh)
Inventor
杨积志
李海波
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SHANGHAI ANHORN MECHANICAL EQUIPMENT CO Ltd
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SHANGHAI ANHORN MECHANICAL EQUIPMENT CO Ltd
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Priority to CN2013100117237A priority Critical patent/CN103058406A/en
Publication of CN103058406A publication Critical patent/CN103058406A/en
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Abstract

The invention discloses a device and a technology employed to hydrogen peroxide purification and relates to the removing of organisms specifically anthraquinone compounds in hydrogen peroxide industrial production. According to the method and the device, the organisms in the hydrogen peroxide are removed deeply by using the method of phase separator and film separation combined technology; the phase separator is the patented product of the company, which is developed by using the principle that the microfiber can coagulate micro liquid drops and thus the phase separator can separate the organisms in the hydrogen peroxide to the solubility limit; then the hydrogen peroxide solution containing saturated organisms enters the film system, wherein the film has the characteristics of selectively transmitting particles and therefore can effectively prevent organism particles from penetrating through and allow the hydrogen peroxide to penetrate through; after the film separation, the content of the organisms in the hydrogen peroxide of a clear solution side can be reduced to about several parts per million (ppm); and the concentrated hydrogen peroxide returns back to the phase separator to separate. With the adoption of the device and the technology, the content of organic carbon in the hydrogen peroxide can be effectively reduced with relatively low investment, and thus the requirement of the sequent processes is satisfied and the national energy conservation policy is met.

Description

A kind of device and technique that is applied to the hydrogen peroxide purification
Technical field
The present invention relates to a kind of device and technique, relate in particular to and a kind ofly can improve the hydrogen peroxide precision, provide high-quality raw material for the downstream produces, improve the quality of derived product, energy consumption is low, level of automation is high is applied to device and the technique that hydrogen peroxide purifies.
Background technology
Hexanolactam is a kind of important production nylon 6 engineering plastic and nylon 6 fiber.Caprolactam production mainly is to adopt ketone-oxime operational path production, in the traditional oximate and Beckmann rearrangement, pimelinketone, ammonia, hydrogen peroxide is placed same reactor, the one-step synthesis cyclohexanone-oxime.Middle organic carbon concentration to hydrogen peroxide in the reaction needs and will be low to moderate below the 50ppm.
High-purity hydrogen peroxide is the deep processed product of industrial hydrogen peroxide, and electron trade is the main application fields of high-purity hydrogen peroxide, mainly as the remover of clean-out system, etching reagent and the photoresist material of semiconductor crystal sheet.According to relevant department prediction, " 12 " afterwards, the demand growth of China's high purity reagent is rapid, market outlook are very wide.The development of China's high purity reagent was started in for 20 century 70 mid-terms, although obtained certain breakthrough, integral level and advanced international standard still have larger gap.The production of high-purity hydrogen peroxide generally is that technical grade hydrogen peroxide take anthraquinone production is as raw material, wherein except containing a certain amount of inorganics impurity and mechanical impurity, the organic impurities that also contains 10 ~ 500mg/L, these organic impurities comprise anthraquinone compounds and ester, alcohol, phenol, ketone compounds etc., and they derive from the processes such as additive in the production and materiel machining, conveying, storage.
In order to remove these organic impurities in the technical grade hydrogen peroxide product, since the 1950's, people have developed many purifying methods in succession, sum up following several: the combination of rectifying, absorption, ion-exchange, extraction, crystallization, membrane sepn and several method etc.
What present industrial application was commonplace is rectification method and the ion exchange resin method of purification.Rectification method generally is used to concentrated hydrogen peroxide because the organism boiling point is higher, be removed so be enriched in the liquid that do not gasify, thereby so that hydrogen peroxide be purified.But, because separating, enterprise not exclusively reaches carrying of fog-like liquid, volatile organism can follow hydrogen peroxide steam to enter distillation system, so purity generally can be very not high.Can be used as the purifying method in early stage of other purification techniquess.
The ion exchange resin method of purification not only can be removed organic carbon, and part that can be removed impurity metal ion such as Fe, Al, Sn plasma.The resin regeneration process is simple, and resin reuses repeatedly.But in the practical application, ion exchange resin needs to consume a large amount of energy consumptions when regeneration, and because the class gummy solid occurs, causes resin that the problems such as obstruction occur.
Membrane sepn is by absorption and the effects such as kapillary circulation, screening, so that hydrogen peroxide solution obtains purifying.
Summary of the invention
For the problems referred to above, main purpose of the present invention is to provide a kind of can improve the hydrogen peroxide precision, provides high-quality raw material for the downstream produces, and improves the quality of derived product, energy consumption is low, level of automation the is high device and the technique that are applied to the hydrogen peroxide purification.
The present invention solves above-mentioned technical problem by following technical proposals: a kind of device that is applied to the hydrogen peroxide purification, described device comprises original fluid container, strainer, phase separator, film separating system, a cover chemical cleaning system, the conventional cleaning system of a cover, described original fluid container is connected with strainer by liquid feeding pump, two cover strainers are connected with phase separator, phase separator is by high-pressure pump junctional membrane separation system, be connected with chemically-cleaning device and conventional washing unit on the film separating system, described strainer is two covers, and described film separating system also is two covers.
In specific embodiments of the invention, described conventional washing unit comprises a cleaning water tank, a scavenging pump and the valve that switches for control; Described cleaning water tank links to each other with the product dioxygen mouth of a river of film separating system, the opening for feed of scavenging pump links to each other with the cleaning water tank, scavenging pump outlet links to each other with original fluid container with the film separating system import respectively, and on the pipeline that scavenging pump is connected valve is set and controls the flow direction that scavenging pump exports liquid.
In specific embodiments of the invention, the scavenging pump outlet of described conventional washing unit connects two cover film separating systems, is provided with one group on the water-in pipeline of two cover film separating systems and can controls the valve that scavenging pump outlet liquid enters any cover film separating system in two covers.
In specific embodiments of the invention, described chemically-cleaning device comprises a matting water tank, a chemical cleaning pump and the valve that switches for control; The matting water tank of described device links to each other with the product mouth of a river of film separating system, and the chemical cleaning pump water-in links to each other with the matting water tank, and the matting pump discharge links to each other with original fluid container with the membrane sepn import respectively and the flow direction that the valve control pump exports liquid is set.
In specific embodiments of the invention, the contained matting pump discharge of described chemically-cleaning device connects on the inlet line of film separating system of two cover operations and is provided with one group of valve, and control matting pump discharge liquid enters any cover film separating system.
A kind of said apparatus that utilizes is applied to the technique that hydrogen peroxide purifies, and described technique comprises the steps:
(1), the technical grade hydrogen peroxide is introduced into original fluid container;
(2), the original fluid container mixed solution enters strainer and carries out pre-treatment after liquid feeding pump pressurization;
(3), hydrogen peroxide after pretreatment enters that phase separator does not dissolve organic phase and hydrogen peroxide two is separated, light phase organism is discharged system after separating, the saturated organic hydrogen peroxide solution of heavy phase enters the subsequent film separation system;
(4), in film separating system, finish organic removing in the hydrogen peroxide.
In specific embodiments of the invention, described original fluid container is used for raw material and concentrated mixing of materials and phase separator charging buffering;
Described liquid feeding pump is used for the mixed solution pressurization with original fluid container, enters strainer;
The strainer of two cover alternate runs be used for to be removed the particulate matter of mixed solution, enters afterwards phase separator and carries out two and be separated;
Phase separator is for dissolved organic matter and hydrogen peroxide two are not separated, phase separator has the effect of microscopic droplets in the cohesion mixed solution, drop after the cohesion is through behind the standing demix, organic phase is discharged system from light phase export, the hydrogen peroxide solution heavy and light that organism is saturated exports discharge mutually, enters film separating system after the high-pressure pump pressurization;
The film separating system of two cover alternate runs, the film of selection has selectivity and stops organic characteristic, and through behind the membrane sepn, the hydrogen peroxide that contains micro-content organism produces the dioxygen mouth of a river from film separating system and discharges, and the hydrogen peroxide that is concentrated is back to original fluid container; Also be provided with valve on this film separating system inlet/outlet pipeline;
Conventional washing unit is used for film separating system is carried out normal developing regeneration;
Chemically-cleaning device is used for film separating system is carried out matting regeneration.
In specific embodiments of the invention, described film separating system is according to the target separation accuracy, selects but is not limited to ultra-filtration membrane, a kind of in nanofiltration membrane and the reverse osmosis membrane; Mould material is selected but is not limited to ceramic membrane, pvdf membrane, polyamide membrane.
Positive progressive effect of the present invention is: the present invention and existing same device and method compare, and the present invention improves the hydrogen peroxide precision, provide high-quality raw material for the downstream produces, and improve the quality of derived product; Energy consumption of the present invention is low, and level of automation is high.Phase separator is removed organism and is belonged to static separation, and operational condition is gentle, and the film system exempts the high energy consumption of evaporation, and the total system energy consumption is lower; Phase separator and the operation of film system can be fully by PLC control or DCS controls, and level of automation is high.
Description of drawings
Fig. 1 is device and the process flow diagram that hydrogen peroxide purifies that be applied to provided by the invention.
Fig. 2 is device and the process flow sheet that hydrogen peroxide purifies that be applied to provided by the invention.
Embodiment
Provide preferred embodiment of the present invention below in conjunction with accompanying drawing, to describe technical scheme of the present invention in detail.
Fig. 1 is a kind of device and process flow diagram that hydrogen peroxide purifies that be applied to of the present invention.As shown in Figure 1: technique provided by the invention is finished by following steps: (a) the technical grade hydrogen peroxide is introduced into original fluid container; (b) the original fluid container mixed solution enters strainer and carries out pre-treatment after pump pressurization; (c) hydrogen peroxide after pretreatment enters that phase separator does not dissolve organic phase and hydrogen peroxide two is separated, and light phase organism is discharged system after separating, and the saturated organic hydrogen peroxide solution of heavy phase enters the subsequent film separation system; (d) in film separating system, finish organic removing in the hydrogen peroxide.
Below in conjunction with accompanying drawing 2, the device that removes that adopts aforesaid method is done further specific description.
Accompanying drawing is a kind of device that hydrogen peroxide purifies that is applied to of the present invention, and it comprises: one of a. is used for the original fluid container 1 of hydrogen peroxide raw material and concentrated mixing of materials and phase separator charging buffering; B. a liquid feeding pump 2 is used for entering strainer after the mixed solution pressurization with original fluid container; C. the strainer 3a of two cover alternate runs, 3b be used for to remove the particulate matter of mixed solution, enters afterwards phase separator and carries out two and be separated; D. one is used for not dissolved organic matter and the phase separator 4 that hydrogen peroxide two is separated, and has the effect of condensing microscopic droplets in the mixed solution; This phase separator arranges opening for feed 5, heavy out 6 and light phase export 7, drop after the cohesion is through behind the standing demix, organic phase is from light phase export 7 discharge systems, and the hydrogen peroxide solution heavy and light that organism is saturated exports mutually 6 and discharges, and enters film separating system after high-pressure pump 8 pressurizations; E. two the cover alternate runs film separating system 9a, 9b, separatory membrane has the characteristic that selectivity stops organic molecule to see through, through behind the membrane sepn, the reflexive film separating system of hydrogen peroxide that contains micro-content organism produces dioxygen mouth of a river 12a, 12b discharges, and the hydrogen peroxide that is concentrated is back to original fluid container 11a, and 11b discharges and be back to original fluid container 1; This film separating system also is provided with valve 19,20,21,22 on the turnover pipeline; F. the conventional washing unit of a cover is used for film separating system is carried out normal developing regeneration; G. a cover chemically-cleaning device is used for film separating system is carried out matting regeneration.Described conventional washing unit comprises 13, one scavenging pumps 14 of a cleaning water tank and is used for the valve 17 ~ 28,33 ~ 37 that control is switched; This device cleans the product dioxygen mouth of a river 12a of water tank 13 and film separating system, 12b links to each other, the scavenging pump import with clean water tank 13 and link to each other, scavenging pump exports respectively and membrane sepn water-in 10a, 10b links to each other with original fluid container 1 and the flow direction that valve 27,28 control pumps export liquid is set.Described conventional washing unit scavenging pump outlet connects on the two cover film separating system water-in pipelines and is provided with one group of valve 17 ~ 20, can control scavenging pump outlet liquid and enter any cover film separating system.Described chemically-cleaning device comprises 15, one chemical cleaning pumps 16 of a matting water tank and is used for the valve 17 ~ 24,29 ~ 37 that control is switched; The matting water tank 15 of described device and the product mouth of a river 10a of film separating system, 10b links to each other, the chemical cleaning pump water-in links to each other with matting water tank 15, the chemical cleaning pump water outlet respectively with membrane sepn water-in 10a, 10b links to each other with original fluid container 1 and the flow direction that valve 31,32 control pumps export liquid is set.The contained matting pump discharge of described chemically-cleaning device connects on the film separating system water-in pipeline of two cover operations and is provided with one group of valve 17 ~ 20, and controlled inhibition and generation scavenging pump outlet liquid enters any one and overlaps film separating system 9a, 9b.
The present invention improves the hydrogen peroxide precision, and improving downstream production provides high-quality raw material, improves the quality of derived product; Energy consumption of the present invention is low, and level of automation is high.Phase separator is removed organism and is belonged to static separation, and operational condition is gentle, and the film system exempts the high energy consumption of evaporation, and the total system energy consumption is lower; Phase separator and the operation of film system can be fully by PLC control or DCS controls, and level of automation is high.
More than show and described ultimate principle of the present invention and principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; that describes in above-described embodiment and the specification sheets just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications; these changes and improvements all fall in the claimed scope of the invention, and the claimed scope of the present invention is defined by appending claims and equivalent thereof.

Claims (8)

1. one kind is applied to the device that hydrogen peroxide purifies, it is characterized in that: described device comprises original fluid container, strainer, phase separator, film separating system, a cover chemical cleaning system, the conventional cleaning system of a cover, described original fluid container is connected with strainer by liquid feeding pump, two cover strainers are connected with phase separator, phase separator is by high-pressure pump junctional membrane separation system, be connected with chemically-cleaning device and conventional washing unit on the film separating system, described strainer is two covers, and described film separating system also is two covers.
2. according to claim 1ly be applied to the device that hydrogen peroxide purifies, it is characterized in that: described conventional washing unit comprises a cleaning water tank, a scavenging pump and be used for the valve that control is switched; Described cleaning water tank links to each other with the product dioxygen mouth of a river of film separating system, the opening for feed of scavenging pump links to each other with the cleaning water tank, scavenging pump outlet links to each other with original fluid container with the film separating system import respectively, and on the pipeline that scavenging pump is connected valve is set and controls the flow direction that scavenging pump exports liquid.
3. according to claim 2ly be applied to the device that hydrogen peroxide purifies, it is characterized in that: the scavenging pump outlet of described conventional washing unit connects two cover film separating systems, is provided with one group on the water-in pipeline of two cover film separating systems and can controls the valve that scavenging pump outlet liquid enters any cover film separating system in two covers.
4. according to claim 2ly be applied to the device that hydrogen peroxide purifies, it is characterized in that: described chemically-cleaning device comprises a matting water tank, a chemical cleaning pump and be used for the valve that control is switched; The matting water tank of described device links to each other with the product mouth of a river of film separating system, and the chemical cleaning pump water-in links to each other with the matting water tank, and the matting pump discharge links to each other with original fluid container with the membrane sepn import respectively and the flow direction that the valve control pump exports liquid is set.
5. according to claim 2ly be applied to the device that hydrogen peroxide purifies, it is characterized in that: the contained matting pump discharge of described chemically-cleaning device connects on the inlet line of film separating system of two cover operations and is provided with one group of valve, and control matting pump discharge liquid enters any cover film separating system.
6. one kind is utilized the described application of installation of claim 1 in the technique of hydrogen peroxide purification, and it is characterized in that: described technique comprises the steps:
(1), the technical grade hydrogen peroxide is introduced into original fluid container;
(2), the original fluid container mixed solution enters strainer and carries out pre-treatment after liquid feeding pump pressurization;
(3), hydrogen peroxide after pretreatment enters that phase separator does not dissolve organic phase and hydrogen peroxide two is separated, light phase organism is discharged system after separating, the saturated organic hydrogen peroxide solution of heavy phase enters the subsequent film separation system;
(4), in film separating system, finish organic removing in the hydrogen peroxide.
7. technique according to claim 6 is characterized in that: described original fluid container is used for raw material and concentrated mixing of materials and phase separator charging buffering;
Described liquid feeding pump is used for the mixed solution pressurization with original fluid container, enters strainer;
The strainer of two cover alternate runs be used for to be removed the particulate matter of mixed solution, enters afterwards phase separator and carries out two and be separated;
Phase separator is for dissolved organic matter and hydrogen peroxide two are not separated, phase separator has the effect of microscopic droplets in the cohesion mixed solution, drop after the cohesion is through behind the standing demix, organic phase is discharged system from light phase export, the hydrogen peroxide solution heavy and light that organism is saturated exports discharge mutually, enters film separating system after the high-pressure pump pressurization;
The film separating system of two cover alternate runs, the film of selection has selectivity and stops organic characteristic, and through behind the membrane sepn, the hydrogen peroxide that contains micro-content organism produces the dioxygen mouth of a river from film separating system and discharges, and the hydrogen peroxide that is concentrated is back to original fluid container; Also be provided with valve on this film separating system inlet/outlet pipeline;
Conventional washing unit is used for film separating system is carried out normal developing regeneration;
Chemically-cleaning device is used for film separating system is carried out matting regeneration.
8. technique according to claim 6 is characterized in that: described film separating system is according to the target separation accuracy, selects but is not limited to ultra-filtration membrane, a kind of in nanofiltration membrane and the reverse osmosis membrane; Mould material is selected but is not limited to ceramic membrane, pvdf membrane, polyamide membrane.
CN2013100117237A 2013-01-11 2013-01-11 Device and technology employed to hydrogen peroxide purification Pending CN103058406A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104445735A (en) * 2014-11-26 2015-03-25 柳州化工股份有限公司 Treatment method of wastewater in hydrogen peroxide industry
CN109205569A (en) * 2017-06-30 2019-01-15 中国石油化工股份有限公司 The purification process of the hydrogen peroxide of anthraquinone production
CN109205568A (en) * 2017-06-30 2019-01-15 中国石油化工股份有限公司 A method of purification hydrogen peroxide
CN109205571A (en) * 2017-06-30 2019-01-15 中国石油化工股份有限公司 A method of isolating and purifying hydrogen peroxide
CN111921263A (en) * 2020-07-23 2020-11-13 江苏理文化工有限公司 Novel purification process of hydrogen peroxide
CN112190996A (en) * 2020-09-07 2021-01-08 泰兴瑞深新材科技有限公司 High-concentration hydrogen peroxide filtering device using antioxidant filtering sheet

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101249953A (en) * 2008-04-01 2008-08-27 苏州市晶协高新电子材料有限公司 Technique and equipment for manufacturing super-clean high-pure electronic grade hydrogen peroxide
CN102020366A (en) * 2009-09-11 2011-04-20 上海安赐机械设备有限公司 Method and device for deeply removing aniline from water
JP2012012274A (en) * 2010-07-05 2012-01-19 Mitsubishi Gas Chemical Co Inc Method for producing purified hydrogen peroxide aqueous solution

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101249953A (en) * 2008-04-01 2008-08-27 苏州市晶协高新电子材料有限公司 Technique and equipment for manufacturing super-clean high-pure electronic grade hydrogen peroxide
CN102020366A (en) * 2009-09-11 2011-04-20 上海安赐机械设备有限公司 Method and device for deeply removing aniline from water
JP2012012274A (en) * 2010-07-05 2012-01-19 Mitsubishi Gas Chemical Co Inc Method for producing purified hydrogen peroxide aqueous solution

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104445735A (en) * 2014-11-26 2015-03-25 柳州化工股份有限公司 Treatment method of wastewater in hydrogen peroxide industry
CN104445735B (en) * 2014-11-26 2016-04-13 柳州化工股份有限公司 The treatment process of waste water in a kind of hydrogen peroxide industry
CN109205569A (en) * 2017-06-30 2019-01-15 中国石油化工股份有限公司 The purification process of the hydrogen peroxide of anthraquinone production
CN109205568A (en) * 2017-06-30 2019-01-15 中国石油化工股份有限公司 A method of purification hydrogen peroxide
CN109205571A (en) * 2017-06-30 2019-01-15 中国石油化工股份有限公司 A method of isolating and purifying hydrogen peroxide
CN109205571B (en) * 2017-06-30 2020-10-27 中国石油化工股份有限公司 Method for separating and purifying hydrogen peroxide
CN109205569B (en) * 2017-06-30 2021-04-06 中国石油化工股份有限公司 Method for purifying hydrogen peroxide produced by anthraquinone process
CN111921263A (en) * 2020-07-23 2020-11-13 江苏理文化工有限公司 Novel purification process of hydrogen peroxide
CN112190996A (en) * 2020-09-07 2021-01-08 泰兴瑞深新材科技有限公司 High-concentration hydrogen peroxide filtering device using antioxidant filtering sheet

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Application publication date: 20130424