CN1018584B - Reaction monitoring probe for producing azo dimethyamide - Google Patents

Reaction monitoring probe for producing azo dimethyamide

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Publication number
CN1018584B
CN1018584B CN 89102566 CN89102566A CN1018584B CN 1018584 B CN1018584 B CN 1018584B CN 89102566 CN89102566 CN 89102566 CN 89102566 A CN89102566 A CN 89102566A CN 1018584 B CN1018584 B CN 1018584B
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CN
China
Prior art keywords
probe
reaction
electrode
pipe
outer tube
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired
Application number
CN 89102566
Other languages
Chinese (zh)
Other versions
CN1046603A (en
Inventor
李定
陈长章
柳美玉
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Fujian Institute of Research on the Structure of Matter of CAS
Original Assignee
Fujian Institute of Research on the Structure of Matter of CAS
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Application filed by Fujian Institute of Research on the Structure of Matter of CAS filed Critical Fujian Institute of Research on the Structure of Matter of CAS
Priority to CN 89102566 priority Critical patent/CN1018584B/en
Publication of CN1046603A publication Critical patent/CN1046603A/en
Publication of CN1018584B publication Critical patent/CN1018584B/en
Expired legal-status Critical Current

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Abstract

The present invention discloses a reaction monitoring probe producing AC foaming agent. The probe adopts an electrochemical means and can accurately monitor the whole procedure of a procedure before reaction, a procedure during the reaction and a procedure after the reaction in time.

Description

Reaction monitoring probe for producing azo dimethyamide
When the present invention relates to a kind of production azobisformamide (being the AC gas-development agent), be inserted in the reaction pot, be used for the probe of monitoring reaction course.
The AC gas-development agent is made by the biruea oxidation.The reaction mechanism mechanism of reaction in past is difficult to monitoring, the existing reality of producing adopts hand sampling, with aqueous slkali dissolving AC gas-development agent, the biruea that detects by an unaided eye does not have and reacts completely, this method is usually brought inaccuracy, the sampling trouble, and whole process can't be monitored, reaction end is easy to excessive, and this brings difficulty often for the control reaction.Yet there are no in the world at present, in the AC gas-development agent is produced, adopt electrochemical means, the report of the probe of monitoring reaction course.
The objective of the invention is to provide a kind of monitoring probe that can be used for commercial production AC gas-development agent, it adopts electrochemical means, react pilot process and react three kinds of states that finish before can distinguishing reaction easily, reflect entire reaction course timely and accurately, be adapted to industrialness production, detect in real time, easy to operate, favorable reproducibility.
Its sonde configuration such as accompanying drawing.Among the figure, the platinumiridio electrode 3 of ability reaction solution corrosion, the outer tube 20 that is enclosed in the corrosion of ability reaction medium by epoxy resin 21 admittedly is as between plastics etc. and the interior pipe 4, and 16 is the inner and outer pipes supporting slice.Another meets the metallic copper 18 of producing the required degree of stability of AC gas-development agent reaction monitoring, is immersed in to form interior electrode in the interior pipe 4 of filling by copper/saturated copper sulphate solution 19.Interior pipe top rubber stopper 6 jam-packs, and seal up epoxy resin 17, the bottom pad is gone up cork 2 and sand stamen glass 22, screw on the teflon cover 1 that has center pit on the interior pipe bottom head, in the middle of the inner and outer pipes, for preventing that vigorous stirring causes vibration when reacting, so foam-filled plastics 5, outer tube top also is connected to the brace 7 of band internal and external threads, external thread connects probe and goes up cylinder 8, last cylinder intermediate adhesion one ring segment 9 magnification circuit plates 15 usefulness screws are fixed on it, input amplifier connects 3, ground connection termination 18, the center-side of output termination output cable seat 12, the outer shell joint earth terminal of output cable seat, output terminal also warp-64K resistance connects microampere gauge outfit 14, the amplifying circuit power supply connects 6V laminated cell 10 by laminated cell folder 11, amplifying circuit is made up of low power consumption integrated circuit LM324, input end is the 12 pin, earth terminal (negative power end) is the 11 pin, and positive power source terminal is the 4th pin, and output terminal is the 14 pin, the tenth tripod connects the 11 pin through the 9.1K metalfilmresistor, and another 22K metalfilmresistor is connected between the tenth tripod and the 14 pin.This circuit little power consumption, because the close electrode of amplifying circuit, so the influence of external interference is little, output cable reaches 30 meters, does not still influence work, its input impedance meets the requirement of inventing selected electrode.
For making oxygenant with sodium chlorate, before the reaction beginning, reaction medium is acid, and Main Ingredients and Appearance is a biruea; The reaction pilot process constantly adds sodium chlorate, but sodium chlorate also constantly consumes, biruea constantly reduces, the AC gas-development agent constantly generates, to exhaust be zero to biruea when reaction finished, be mainly the AC gas-development agent in the medium, also contain a small amount of sodium chlorate and other composition, the electrode material that invention is adopted can reflect the variation of three course media of entire reaction course sensitively.
During probe work, probe is placed reaction pot solution, and the gauge outfit of its probe can reflect the difference of process, also can receive the digital display portion of reaction monitor with output cable, digital display portion is significantly before the distinguishing reaction, the situation that reaction pilot process and reaction finish.
The invention discloses and a kind ofly can be fit to the monitoring probe that industrialness is produced the AC gas-development agent continuously, it has adopted the platinumiridio electrode that can reflect course of reaction, and amplifying circuit put do among the probe, improved antijamming capability, to adapt to the needs of production scene, when the probe immersion is done in the medium of producing the AC gas-development agent, finish with reaction before the reaction, the indicator of gauge outfit places minimum and maximum position respectively on the probe.The indicator of reaction pilot process gauge outfit is put and is done between the two, if show with the digital display portion of reaction monitor, then numeral is less than 200 before the reaction, and when reaction finished, numeral was greater than 250, and pilot process is between 200 and 250.
Implementation example:
Probe is inserted in the Gai Kongzhong of three kilolitre reaction pots, and make the bottom of popping one's head in the course of reaction all can touch reaction medium, the output cable seat is received the digital display portion of reaction monitor with 36 meters output cables, connect the stirrer power supply, add the biruea mother liquor to 2/3rds of reaction pot total measurement (volume), add vanadium catalyst again, when heating makes temperature rise to 60 ℃, numeral is presented at 156, adds the sodium chlorate aqueous solution slowly, 70 ℃ of the reaction pot maximum temperatures that probe is put, numeral is presented between 180 to 230, when finishing to reaction, digital displaying value is 250, at this moment, biruea is not for having in the qualitative analysis mother liquor, the sodium chlorate residual quantity is 11.7g/l in the quantitative test mother liquor, and the entire reaction time is 2 hours, and the result generates the orange-yellow AC gas-development agent that meets Chinese the Ministry of Chemical Industry primes standard promulgated by the ministries or commissions of the Central Government.

Claims (5)

1, a kind of probe that is used to monitor azobisformamide production reaction is characterized in that this probe is made up of two parts up and down.Top is made up of power supply, amplifying circuit, gauge outfit and shell; The bottom is made up of outer tube, alloy electrode, interior pipe and interior electrode.Two are partly connected together by brace.
2, probe as claimed in claim 1 is characterized in that described alloy electrode Main Ingredients and Appearance is a platinoiridita, and it is enclosed between outer tube and the interior pipe admittedly with epoxy resin, and exposes the bottom.
3, probe as claimed in claim 1 is characterized in that the teflon cover of cork pad, sand stamen glass and center drilling is arranged at described interior pipe bottom, is added with copper/saturated copper sulphate solution in the pipe, wherein is inserted with the fixing metallic copper of rubber stopper electrode in constituting.
4, as claim 1,2 and 3 described probes, it is characterized in that alloy electrode links to each other with earth terminal with the input end of amplifying circuit respectively with interior electrode, power supply adopts laminated cell, gauge outfit connects output terminal by a resistance, the output cable seat also is housed on the shell, its center termination output terminal, outer shell joint earth terminal.
5, probe as claimed in claim 1 is full of epoxy resin and polyfoam between pipe and the outer tube in it is characterized in that.
CN 89102566 1989-04-19 1989-04-19 Reaction monitoring probe for producing azo dimethyamide Expired CN1018584B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 89102566 CN1018584B (en) 1989-04-19 1989-04-19 Reaction monitoring probe for producing azo dimethyamide

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN 89102566 CN1018584B (en) 1989-04-19 1989-04-19 Reaction monitoring probe for producing azo dimethyamide

Publications (2)

Publication Number Publication Date
CN1046603A CN1046603A (en) 1990-10-31
CN1018584B true CN1018584B (en) 1992-10-07

Family

ID=4854794

Family Applications (1)

Application Number Title Priority Date Filing Date
CN 89102566 Expired CN1018584B (en) 1989-04-19 1989-04-19 Reaction monitoring probe for producing azo dimethyamide

Country Status (1)

Country Link
CN (1) CN1018584B (en)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1095390C (en) * 1996-05-30 2002-12-04 郑守樽 Method and apparatus for eliminating acid mist and acid liquor created by ADC foaming agent condensation process
CN104569167A (en) * 2013-10-17 2015-04-29 苏州市产品质量监督检验所 Liquid chromatography-tandem mass spectrometry detection method of hydrazo dicarbonamide
FR3013168A1 (en) * 2013-11-08 2015-05-15 Valeo Equip Electr Moteur ELECTRIC MACHINE BRUSH HOLDER FOR VEHICLE AND CORRESPONDING STARTER

Also Published As

Publication number Publication date
CN1046603A (en) 1990-10-31

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