CN207096197U - Liquid acidity continuous monitor system is aoxidized in hydrogen peroxide process - Google Patents

Liquid acidity continuous monitor system is aoxidized in hydrogen peroxide process Download PDF

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Publication number
CN207096197U
CN207096197U CN201720616333.6U CN201720616333U CN207096197U CN 207096197 U CN207096197 U CN 207096197U CN 201720616333 U CN201720616333 U CN 201720616333U CN 207096197 U CN207096197 U CN 207096197U
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liquid
acidity
hydrogen peroxide
valve
aoxidized
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谢兆明
顾潮春
吴琼水
万智
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NANJING HOPES TECHNOLOGY Co Ltd
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NANJING HOPES TECHNOLOGY Co Ltd
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Abstract

The utility model belongs to technical field of liquid detection, more particularly to oxidation liquid acidity continuous monitor system in hydrogen peroxide process, including sampling transmitting device, demarcation cleaning device, liquid-liquid extraction and emptier, acid determining device, signal acquisition process transmitting device and electrical control gear;The utility model automaticity is high, reduces dangerous, mitigation human error, shortening measurement period, and the utility model can will control within 15 minutes, and can be preferably applied to adjust hydrogen peroxide process oxidation operation acid adding amount in the sampling time.

Description

Liquid acidity continuous monitor system is aoxidized in hydrogen peroxide process
Technical field
The present invention relates to technical field of liquid detection, and liquid acidity continuous monitoring system is aoxidized more particularly to hydrogen peroxide process System.
Background technology
Because Stability of Hydrogen Peroxide is influenceed very big, neutral solution by pH value(pH=7)It is most stable;When pH value is low(pH< 7, in acidity)When, it is little to stability influence;But when pH value is high(pH>7, in alkalescence)When, stability drastically deteriorates, and decomposes speed Degree is obvious to be accelerated.
At present, most of Hydrogen Peroxide Productions are all using anthraquinone.It is anthraquinone that hydrogen carrier is used as using anthraquinone analog compound(Or work Make carrier), hydrogen and oxygen is reacted generation hydrogen peroxide, its main production process has hydrogenation process, oxidation operation, extraction process and net Chemical industry sequence.Because hydrogenation process hydride is in alkalescent, to reduce decomposing hydrogen dioxide solution in oxidation solution, it need to transmit reaction medium weak Acidity, therefore, hydride enter oxidation operation process and add a small amount of phosphoric acid as stabilizer.
To ensure that the stable of hydrogen hydrogen peroxide technique is performed, it is necessary to which Accurate Determining aoxidizes liquid acidity, to control making for phosphoric acid Dosage, supplies consumption is reduced, reduce cost, ensure product quality stability.
The measure of hydrogen hydrogen peroxide technique oxidation liquid acidity mainly uses off-line analysis method.Its principle is:In oxidation solution Hydrogen peroxide, the inorganic component such as phosphoric acid it is soluble in water, and working solution is insoluble in water, according to the difference of their solubility in water, It is the aqueous solution to be extracted the inorganic component in oxidation solution with pure water.The aqueous solution is layered with working solution, and the aqueous solution is located at lower floor, is collected The aqueous solution is to be analyzed.Analysis method typically uses AAS and acid-base titration.
Wherein,《Water and effluent monitoring analysis method(Fourth edition)》The molybdenum-antimony anti-spectrophotometric method and peacock green phosphorus of middle introduction Molybdenum heteropolyacid AAS can be used directly to orthophosphates concentration in water and waste water, so as to calculate oxidation liquid acidity indirectly. Its principle is:Under certain condition, soluble orthophosphates and developer, colored complex is generated, is carried out at a particular wavelength Measure.But the shortcomings that AAS, is:Developing time is grown, and needs to place about 15-30 min at room temperature;Reducing agent ascorbic acid is easy It is oxidized, is unfavorable for storing for a long time, should not use.
In real process, acid-base titration use is relatively more.Sodium hydroxide is used after indicator is added dropwise in the aqueous solution to be analyzed Titrated, titration end-point is judged by color, calculates sodium hydroxide usage amount, so as to calculate oxidation liquid acidity, time-consuming, right Operating personnel require high.
Off-line analysis method needs experimenter to carry sampler bag to scene, opens high-pressure sampling valve, takes certain volume oxygen Change liquid, carry out manual extraction, laboratory acidity analysis.Therefore, off-line analysis method has the dangerous big, sampling of field sampling and divided Analyse time length, the shortcomings of high, automaticity is low, poor in timeliness is required to operating personnel.
The content of the invention
In order to overcome the above-mentioned deficiencies of the prior art, the invention provides a kind of security is good, analytical cycle is short, automation Degree is high, ageing strong hydrogen peroxide process oxidation liquid acidity continuous monitor system.
The present invention is achieved through the following technical solutions above-mentioned purpose:Liquid acidity continuous monitoring system is aoxidized in hydrogen peroxide process System, including sampling transmitting device, demarcation cleaning device, liquid-liquid extraction and emptier, acid determining device, signal acquisition process Transmitting device and electrical control gear;The sampling transmitting device includes pneumatic operated valve(2), liquid pressure regulator valve(3), the first two three Three-way electromagnetic valve(4)And transfer line, the sampled transmitting device of sample and transfer line are directly entered the first overflow cup(13);It is described Demarcation cleaning device includes the second two-bit triplet magnetic valve(11), the first syringe pump(6), the second syringe pump(17), liquid storage ring (5), Multi-position rotation valve(7), liquid storing barrel and pipeline, the first syringe pump(6)By the first two-bit triplet electricity for sampling transmitting device Magnet valve(4)Standard liquid is drawn, is introduced into liquid storage ring(5), through Multi-position rotation valve(7)Switching, then by the first syringe pump(6)Push away Go out, into the first overflow cup(13), the aqueous solution is through the second syringe pump(17)Into the second overflow cup(15);The liquid-liquid extraction with Emptier includes the first overflow cup(13), the second overflow cup(15), the first two two-way electromagnetic valves(14), the second two two-ways Magnetic valve(16), the 3rd two two-way electromagnetic valve(19), liquid-liquid extraction device(18), the first check valve(20), the second check valve (21), peristaltic pump(25)And pipeline, into the first overflow cup(13), the second overflow cup(15)Solution enter liquid-liquid extraction device (18)After mix, extract, measurement lower floor extraction liquid acidity, emptied through discharge pipe line;The acidity test device senses including pH Device and pH- acidity measure instruments.
Liquid acidity continuous monitor system is aoxidized in hydrogen peroxide process of the present invention, wherein first syringe pump(6), the second note Penetrate pump(17)For Large Copacity high flow rate syringe pump, optional capacity is more than 10mL, and optional flow velocity is more than 5mL/min, it is preferred that uses Capacity is 100mL, and flow velocity is 100mL/min syringe pumps.
Liquid acidity continuous monitor system is aoxidized in hydrogen peroxide process of the present invention, wherein the liquid storage ring(5)Capacity is more than 10mL, it is preferred that liquid storage ring capacity is 50mL.
Liquid acidity continuous monitor system is aoxidized in hydrogen peroxide process of the present invention, wherein the Multi-position rotation valve(7)Optional 6 Position, 8,10, it is preferred that using 6 rotary valves.
Liquid acidity continuous monitor system is aoxidized in hydrogen peroxide process of the present invention, wherein first overflow cup(13), second Overflow cup(15)With scale, optional 10-200mL overflow cups, it is preferred that overflow cup(13)Using 25mL, overflow cup(15)Adopt Use 75mL.
Liquid acidity continuous monitor system is aoxidized in hydrogen peroxide process of the present invention, wherein the liquid-liquid extraction device(18)With electricity Magnetic heat insulation sheath and temperature controller, built-in magneton.
Liquid acidity continuous monitor system is aoxidized in hydrogen peroxide process of the present invention, wherein the pH sensors use vitreous electricity Pole, it is preferable using the pH combination electrodes with temperature-compensating.
The present invention compared with prior art, the beneficial effects of the invention are as follows:
1st, automaticity is high.The present invention is by sampling transmitting device, demarcation cleaning device, liquid-liquid extraction and emptying dress Put, acid determining device, signal acquisition process transmitting device and electrical control gear so that oxidation panel aoxidizes in hydrogen peroxide process Liquid acidity is changed into automatic on-line monitoring from off-line monitoring, and available for control hydrogen peroxide process oxidation operation acid adding amount.
2nd, reduce dangerous.Prior art is all spot sampling, and the present invention is sampled using autobarotropy, avoids operation Personnel may the danger caused by misoperation or leakage to spot sampling.
3rd, human error is mitigated:Off-line method is all that titration end-point is judged by way of titration by operating personnel, and originally Invention presupposition analysis method, judge without artificial, result is directly provided by acidity test device.
4th, measurement period is shortened:Existing off-line test technology typically one sample of interval collection in 1 hour, the present invention can incite somebody to action Sampling time was controlled within 15 minutes, can be preferably applied to adjust hydrogen peroxide process oxidation operation acid adding amount.
Brief description of the drawings
Fig. 1 is the principle schematic of continuous monitor system of the embodiment of the present invention.
Fig. 2 is that the typical attachment structure signal of liquid acidity continuous monitor system is aoxidized in hydrogen peroxide process of the embodiment of the present invention Figure.
In figure, 1- pipelines, 2- pneumatic operated valves, 3- liquid pressure regulator valves, 4- the first two-bit triplet magnetic valves, 11- the second two three Three-way electromagnetic valve, 5- liquid storage rings, the syringe pumps of 6- first, the syringe pumps of 17- second, 7- Multi-position rotation valves, 8- standard liquids I, 9- standards Solution II, 10- standard liquids III, the 12- aqueous solution, the overflow cups of 13- first, the overflow cups of 15- second, 14- the first two two are powered Magnet valve, the second two two-way electromagnetic valves of 16-, the 3rd two two-way electromagnetic valve of 19-, 18- liquid-liquid extraction devices, the check valves of 20- first, The check valves of 21- second, 22- acid determining devices, 23- signal acquisition process transmitting devices, 24-DCS Data Control Centers, 25- Peristaltic pump, 26- electric control systems.
Embodiment
Make with reference to the accompanying drawings and examples to aoxidizing liquid acidity continuous monitor system in hydrogen peroxide process of the present invention into one Walk explanation.
As shown in figure 1, to aoxidize the principle schematic of liquid acidity continuous monitor system in hydrogen peroxide process of the present invention, including 6 parts:Sample transmitting device, demarcation cleaning device, liquid-liquid extraction and emptier, acid determining device, signal acquisition process Transmitting device and electrical control gear.Electrical control gear controls sampling transmitting device, demarcation cleaning device and liquid liquid extraction respectively Take and emptier, acid determining device and signal acquisition process transmitting device are located at after liquid-liquid extraction emptier.Normally During sampling analysis, electrical control gear control sampling transmitting device collection sample is simultaneously transmitted to demarcation cleaning device, enters back into liquid Liquid extraction equipment and emptier, acid determining device measure extraction liquid acidity, then signal acquisition process transmitting device is passed to, Operating personnel determine whether to adjusting process acid adding amount according to obtained signal;During demarcation, electrical control gear control demarcation is clear Standard liquid is sucked liquid-liquid extraction and emptier, acid determining device measure extraction liquid acidity by cleaning device, and will survey acid Scale is set to standard value, then passes to signal acquisition process transmitting device.During cleaning, electrical control gear control demarcation cleaning dress Put and arrange cleaning fluid suction liquid-liquid extraction and emptier, detergent line, liquid-liquid extraction and emptier, cleaning fluid by row's mouth Go out.
Embodiment:As shown in Fig. 2 typically connected for oxidation liquid acidity continuous monitor system in hydrogen peroxide process of the present invention Structural representation.System includes pipeline(1), pneumatic operated valve(2), liquid pressure regulator valve(3), the first two-bit triplet magnetic valve(4)With Two two-bit triplet magnetic valves(11), liquid storage ring(5), the first syringe pump(6)With the second syringe pump(17), Multi-position rotation valve(7), storage Liquid bucket(Including standard liquid I 8, standard liquid II 9, standard liquid III 10 and the liquid storing barrel of the aqueous solution 12), taper first with a scale Overflow cup(13)With the second overflow cup(15), the first two two-way electromagnetic valves(14), the second two two-way electromagnetic valves(16), the 3rd Two two-way electromagnetic valves(19), liquid-liquid extraction device(18), the first check valve(20), the second check valve(21), acid determining device (22), signal acquisition process transmitting device(23), DCS Data Control Centers(24), peristaltic pump(25), electric control system(26) And pipeline.The connection of each part is as shown in Figure 2.
Wherein, sampling transmitting device includes pneumatic operated valve(2), liquid pressure regulator valve(3), the first two-bit triplet magnetic valve(4)And Transfer line, because sample pipe has elevated pressures, and sample has certain inflammable and explosive property, is connected using pneumatic operated valve Adapter road and transfer line.Pneumatic operated valve is normally off, is opened during normal sample.Demarcation cleaning device includes the second two-bit triplet Magnetic valve(11), the first syringe pump(6), the second syringe pump(17), liquid storage ring(5), Multi-position rotation valve(7), liquid storing barrel【Including mark Quasi- solution I(8), standard liquid II(9), standard liquid III(10)And the aqueous solution(12)Liquid storing barrel】And pipeline, the first syringe pump (6)With the second syringe pump(17)Capacity is all used as 100mL, flow velocity be 100mL/min Large Copacity high flow rate syringe pump, liquid storage Ring(5)Capacity is 50mL, Multi-position rotation valve(7)Using 6 rotary valves.Liquid-liquid extraction includes the first overflow cup with emptier (13), the second overflow cup(15), the first two two-way electromagnetic valves(14), the second two two-way electromagnetic valves(16), the 3rd two two Three-way electromagnetic valve(19), liquid-liquid extraction device(18), the first check valve(20), the second check valve(21), peristaltic pump(25)And pipeline.The One overflow cup(13)Using 25mL, the second overflow cup(15)Using 75mL, sample is 1 with extractant volume ratio:3, more than institute If the liquid of volume can be automatically drained out.Liquid-liquid extraction device(18)With electromagnetism heat insulation sheath, with temperature controller, built-in magnetic Son, temperature are generally located on 25 DEG C, and temperature change can be used for sample and extraction by timely adjustment of heating or freeze greatly Agent stirs and evenly mixs.Check valve and peristaltic pump are used to prevent waste liquid from flowing backwards, and peristaltic pump in time can discharge waste liquid.Acidity assaying Device(22)Including pH combination electrodes and pH- acidity measure instruments with temperature-compensating.Before use, first with pH=4.00, pH= 6.86 and the cushioning liquid of pH=9.18 demarcated, surveyed pH value can be converted directly into acidity by pH- acidity measure instruments, acid Degree enters DCS Data Control Centers by signal acquisition process transmitting device, and operating personnel are by acidity to hydrogen peroxide oxidation work The acid adding amount of section oxidation solution is adjusted.All magnetic valves, the first syringe pump(6)With the second syringe pump(17), Multi-position rotation valve (7), liquid-liquid extraction device(18), peristaltic pump(25)All by electric control system(26)Control.
Normal system operation:Malleation sample oxidation liquid is through pipeline(1), into pneumatic operated valve(2), liquid pressure regulator valve(3), Pressure regulator valve sample adjusts pressure to 0.1MPa, through the first two-bit triplet magnetic valve(4)R1-A1 ends, into 50mL liquid storage rings(5) And Multi-position rotation valve(7)3. number position enter 25mL overflow cups(13), unnecessary sample is from the first overflow cup(13)Rim of a cup is discharged. Capacity 100mL, flow velocity 100mL/min the second syringe pump(17)First from the second two-bit triplet magnetic valve(11)The suction of R2 ends it is few Air is measured, then from the second two-bit triplet magnetic valve(11)P2 ends suction the 80mL aqueous solution, enter the overflows of 75mL second from R2 ends Cup(15).Open the first two two-way electromagnetic valves(14)With the second two two-way electromagnetic valves(16), oxidation solution and the aqueous solution enter Liquid-liquid extraction device(18), stir and evenly mix and stand, acid determining device(22)Measure lower floor's extract pH value is simultaneously converted to acidity, Signal is through signal acquisition process transmitting device(23)Send DCS Data Control Centers to(25).Electric part is by electrical control system System(26)Control.Waste liquid passes through the first check valve(20)With the second check valve(21), by peristaltic pump(25)Waste liquid is discharged.
The invention provides a kind of security is good, analytical cycle is short, automaticity is high, ageing strong hydrogen peroxide process Aoxidize liquid acidity continuous monitor system.Embodiment described above is only that the preferred embodiment of the present invention is described, Not the scope of the present invention is defined, on the premise of design spirit of the present invention is not departed from, those of ordinary skill in the art The various modifications made to technical scheme and improvement, the protection domain of claims of the present invention determination all should be fallen into It is interior.

Claims (7)

1. liquid acidity continuous monitor system is aoxidized in a kind of hydrogen peroxide process, it is characterised in that:Including sampling transmitting device, demarcation Cleaning device, liquid-liquid extraction and emptier, acid determining device, signal acquisition process transmitting device and electrical control gear; The sampling transmitting device includes pneumatic operated valve(2), liquid pressure regulator valve(3), the first two-bit triplet magnetic valve(4)And transfer line, The sampled transmitting device of sample and transfer line are directly entered the first overflow cup(13);The demarcation cleaning device includes second liang Position-3-way solenoid valve(11), the first syringe pump(6), the second syringe pump(17), liquid storage ring(5), Multi-position rotation valve(7), liquid storing barrel And pipeline, the first syringe pump(6)By the first two-bit triplet magnetic valve for sampling transmitting device(4)Standard liquid is drawn, it is advanced Enter liquid storage ring(5), through Multi-position rotation valve(7)Switching, then by the first syringe pump(6)Release, into the first overflow cup(13), it is water-soluble Liquid is through the second syringe pump(17)Into the second overflow cup(15);The liquid-liquid extraction includes the first overflow cup with emptier (13), the second overflow cup(15), the first two two-way electromagnetic valves(14), the second two two-way electromagnetic valves(16), the 3rd two two Three-way electromagnetic valve(19), liquid-liquid extraction device(18), the first check valve(20), the second check valve(21), peristaltic pump(25)And pipeline, enter Enter the first overflow cup(13), the second overflow cup(15)Solution enter liquid-liquid extraction device(18)After mix, extract, measurement lower floor extraction Liquid acidity is taken, is emptied through discharge pipe line;The acidity test device includes pH sensors and pH- acidity conversion equipments.
2. liquid acidity continuous monitor system is aoxidized in hydrogen peroxide process according to claim 1, it is characterised in that:Described One syringe pump(6), the second syringe pump(17)For Large Copacity high flow rate syringe pump, capacity is more than 10mL, and flow velocity is more than 5mL/min.
3. liquid acidity continuous monitor system is aoxidized in hydrogen peroxide process according to claim 1, it is characterised in that:The storage Pendular ring(5)Capacity is more than 10mL.
4. liquid acidity continuous monitor system is aoxidized in hydrogen peroxide process according to claim 1, it is characterised in that:It is described more Position rotary valve(7)From 6,8 or 10 rotary valves.
5. liquid acidity continuous monitor system is aoxidized in hydrogen peroxide process according to claim 1, it is characterised in that:Described One overflow cup(13), the second overflow cup(15)With scale, 10-200mL overflow cups are selected.
6. liquid acidity continuous monitor system is aoxidized in hydrogen peroxide process according to claim 1, it is characterised in that:The liquid Liquid extraction equipment(18)With electromagnetism heat insulation sheath and temperature controller, built-in magneton.
7. liquid acidity continuous monitor system is aoxidized in hydrogen peroxide process according to claim 1, it is characterised in that:The pH Sensor uses glass electrode.
CN201720616333.6U 2017-05-31 2017-05-31 Liquid acidity continuous monitor system is aoxidized in hydrogen peroxide process Active CN207096197U (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107037106A (en) * 2017-05-31 2017-08-11 南京霍普斯科技有限公司 Liquid acidity continuous monitor system and monitoring method are aoxidized in hydrogen peroxide process
CN110873780A (en) * 2018-09-03 2020-03-10 宁波方太厨具有限公司 Intelligent titration system and intelligent titration method based on solution pH value
CN113551944A (en) * 2020-04-23 2021-10-26 中国石油化工股份有限公司 System and method for monitoring acidity of oxidizing liquid in device for producing hydrogen peroxide by anthraquinone process
CN113551943A (en) * 2020-04-23 2021-10-26 中国石油化工股份有限公司 System and method for monitoring hydrogen peroxide concentration in raffinate
CN113551942A (en) * 2020-04-23 2021-10-26 中国石油化工股份有限公司 System and method for monitoring acidity of oxidizing liquid in device for producing hydrogen peroxide by anthraquinone process

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107037106A (en) * 2017-05-31 2017-08-11 南京霍普斯科技有限公司 Liquid acidity continuous monitor system and monitoring method are aoxidized in hydrogen peroxide process
CN107037106B (en) * 2017-05-31 2019-03-12 南京霍普斯科技有限公司 Liquid acidity continuous monitor system and monitoring method are aoxidized in hydrogen peroxide process
CN110873780A (en) * 2018-09-03 2020-03-10 宁波方太厨具有限公司 Intelligent titration system and intelligent titration method based on solution pH value
CN113551944A (en) * 2020-04-23 2021-10-26 中国石油化工股份有限公司 System and method for monitoring acidity of oxidizing liquid in device for producing hydrogen peroxide by anthraquinone process
CN113551943A (en) * 2020-04-23 2021-10-26 中国石油化工股份有限公司 System and method for monitoring hydrogen peroxide concentration in raffinate
CN113551942A (en) * 2020-04-23 2021-10-26 中国石油化工股份有限公司 System and method for monitoring acidity of oxidizing liquid in device for producing hydrogen peroxide by anthraquinone process

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