CN107661733A - One kind is used for13The reactor of C urea synthesizings - Google Patents

One kind is used for13The reactor of C urea synthesizings Download PDF

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Publication number
CN107661733A
CN107661733A CN201610605180.5A CN201610605180A CN107661733A CN 107661733 A CN107661733 A CN 107661733A CN 201610605180 A CN201610605180 A CN 201610605180A CN 107661733 A CN107661733 A CN 107661733A
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Prior art keywords
connector
air inlet
inlet pipe
extension pipeline
pressure
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Granted
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CN201610605180.5A
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Chinese (zh)
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CN107661733B (en
Inventor
章高发
范国民
黄晋杰
沈桂富
闫长斌
陈世雄
魏翠雯
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SHENZHEN ZHONGHE HEADWAY BIO SCI&TECH CO Ltd
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SHENZHEN ZHONGHE HEADWAY BIO SCI&TECH CO Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/008Details of the reactor or of the particulate material; Processes to increase or to retard the rate of reaction
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07BGENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
    • C07B59/00Introduction of isotopes of elements into organic compounds ; Labelled organic compounds per se
    • C07B59/001Acyclic or carbocyclic compounds
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C273/00Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups
    • C07C273/02Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups of urea, its salts, complexes or addition compounds
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008Controlling the process
    • B01J2208/00017Controlling the temperature
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008Controlling the process
    • B01J2208/00539Pressure
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07BGENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
    • C07B2200/00Indexing scheme relating to specific properties of organic compounds
    • C07B2200/05Isotopically modified compounds, e.g. labelled

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Exhaust Gas After Treatment (AREA)

Abstract

The present invention relates to one kind to be used for13The reactor of C urea synthesizings, including pressure-resistant bottle (100), communication means (200);Wherein, the communication means (200) include the cross connecting tube (210) of inner hollow and the air inlet pipe (220) through the cross connecting tube (210), the cross connecting tube (210) includes the first connector (211), second connector (212), 3rd connector (213), 4th connector (214), sealed between the air inlet pipe (220) and the 3rd connector (213), and the air inlet pipe (220) through first connector (211) and the 3rd connector (213) and extends into pressure-resistant bottle (100) inside.The reactor is easy to13CO and NH3Fast Filling, gas filling before and reaction after the completion of waste gas discharge can also simply and easily carry out, urea synthesis reaction is directly used in after closed, and can connect correlation detection probe, the moment detection reaction progress.

Description

One kind is used for13The reactor of C- urea synthesizings
Technical field
The present invention relates to chemical equipment, in particular, is related to one kind and is used for13The reactor of C- urea synthesizings.
Background technology
Helicobacter pylori (Helicobacter pylori, abbreviation Hp), is a kind of monopole, more flagellums, end blunt circle, spiral shell The bacterium of shape bending is revolved, in nineteen eighty-two by Barry Marshall (Barry J.Marshall) and sieve guest's Warren (J.Robin Warren) find first, therefore two people obtain the Nobel prize's soul of 2005.Subsequent research confirms this bacterium Really gastritis, chronic gastroenteritis, gastric ulcer, duodenal ulcer, non-ulcer dyspepsia and part stomach cancer, pylorus can be caused Therefore helicobacter is attracted attention by medical field, helicobacter pylori infections turn into global gastrointestinal disease over more than 30 years with gastrointestinal disease relation to be infected The focus and difficult point of research.
The method of check up and appraisal helicobacter pylori (Hp) mainly has quick urease test, helicobacter pylori (Hp) antibody at present Experiment,13C or14The methods of C breath tests, histopathologic slide, Bacteria Culture.Wherein,13C or14The accuracy of C breath tests Highest, up to more than 95-96%.13C- urea is production13The necessary bulk drug of C breath test detection reagents, its prepare with scale Technology and technique still belong to difficult point.
The content of the invention
The technical problem to be solved in the present invention is:One kind is provided to be used for13The reactor of C- urea synthesizings, solves existing skill There is no suitable reactor to accommodate in art13CO、S、NH3Make its urea synthesis and follow-up exhausting waste gas work can be completed.
The present invention is in order to solve the above problems, there is provided technical scheme be:One kind is provided to be used for13The reaction of C- urea synthesizings Kettle, including for accommodating the pressure-resistant bottle of reactive material, the communication means on the pressure-resistant bottle entrance;Wherein, institute Stating communication means includes the cross connecting tube of inner hollow and the air inlet pipe through the cross connecting tube, the cross connection Pipe connects including the first connector, the second connector and described first of connection installation relief valve connected with pressure-resistant bottle entrance The 3rd connector that interface is oppositely arranged, the 4th connector for gas disengaging, the air inlet pipe and the 3rd connector Between seal, and the air inlet pipe through first connector and the 3rd connector and is extended into pressure bottle body Portion.
Provided by the present invention for13In the reactor of C- urea synthesizings, the communication means also include connecting described the First extension pipeline of one connector and the pressure-resistant bottle entrance;It is described first extension pipeline inner hollow, one end with it is described The sealing connection of first connector, the other end connect with the pressure-resistant bottle inlet seal.
Provided by the present invention for13In the reactor of C- urea synthesizings, the communication means are also described including being connected to Second on second connector extends pipeline, and the relief valve is mounted with the second extension pipeline;Second extension The one end on road connects with second connector sealing, other end sealing.
Provided by the present invention for13In the reactor of C- urea synthesizings, the communication means are also described including being connected to The 3rd extension pipeline on 3rd connector, the air inlet pipe are contained in the described 3rd close to one end of the 3rd connector and prolonged Stretch channel interior;One end and the 3rd connector sealing of the 3rd extension pipeline connects, the described 3rd extend pipeline and Sealing structure is set in gap between the air inlet pipe.
Provided by the present invention for13In the reactor of C- urea synthesizings, the 3rd extension great distance is from the described 3rd The other end of connector is connected to air inlet pipe extension pipeline, the air inlet pipe extend pipeline inner hollow and with the air inlet pipe phase Connection;The first globe type of control valve and temperature, pressure detector are provided with the air inlet pipe extension pipeline.
Provided by the present invention for13In the reactor of C- urea synthesizings, the communication means are also described including being connected to The 4th extension pipeline on 4th connector, one end of the 4th extension pipeline connect with the 4th connector sealing, separately One end connects with feed gas source or outlet pipe;The second globe type of control valve is provided with the 4th extension pipeline.
Implement the present invention, have the advantages that:The reactor of the present invention is easy to13CO and NH3Fast Filling, gas Waste gas discharge before filling and after the completion of reaction can also be carried out simply and easily, and urea synthesis reaction is directly used in after closed, And the detection probe of correlation can be connected, the progress of monitoring reaction in real time.
Brief description of the drawings
Below in conjunction with drawings and Examples, the invention will be further described, in accompanying drawing:
Fig. 1 is the dimensional structure diagram of reactor preferred embodiment of the present invention;
Fig. 2 is the front view of reactor preferred embodiment of the present invention;
Fig. 3 is the structural representation of reactor communication means of the present invention.
Embodiment
Embodiments of the invention are specifically described below in conjunction with accompanying drawing.
13The main component of expiration detection reagent is used in C breath tests13C- urea, that is, use13In C flag urea Carbon, also referred to as carbon【13C】- urea【13CO(NH2)2】Or carbon【13C】- urea, what it was carried13C is12C same position Element.If helicobacter pylori (Hp) in patient's stomach be present, its caused urease will resolve into urea13CO2, use necessary instrument Check in patient's exhaled gas13C amount, so that it may which whether diagnosis infects helicobacter pylori (Hp).Contain13The carbon of C flag【13C】- Urea prepare with scale technology and technique are always industrial difficult point.Side of the invention based on Franz R.A. and Applegath F. Method carries out carbon【13C】Prepared by-urea, general principle is shown in organic chemistry (1961), volume 26, the 2604-2605 pages, the change of reaction It is as follows to learn equation:
13CO+S+2NH3→H2N13CONH2+H2S
Due in reaction system13CO and NH3It is liquid in reaction bulb, S is solid-state, in order to realize13CO and NH3Gas Filling and the H of reaction generation2The discharge of S gases, communication means 200, the communication means 200 are installed on pressure-resistant bottle 100 Mainly include cross connecting tube 210 and run through cross connecting tube 210 from top to bottom and extend into the air inlet of pressure-resistant bottle 100 Pipe 220, the cross connecting tube 210 include being used for the 4th connector 214 of gas disengaging, and purgative gas is mainly nitrogen and helium edge Air inlet pipe 220 to enter inside pressure-resistant bottle 100, air or the H of reaction generation are excluded from the 4th connector 2142S gases; In unstripped gas13CO and NH3It is gaseous in filling process13CO and NH3Enter from the 4th connector 214 and flow into pressure bottle body 100, pressure-resistant bottle 100 has inside the cooling effect lower bottle body of ultralow temperature cooling agent to be less than13CO and NH3The temperature of boiling point, And then will be gaseous13CO and NH3It is cooled to liquid, and then the generation urea of the simple substance reaction of Salmon-Saxl with being pre-charged with.
Fig. 1 shows the stereochemical structure of reactor preferred embodiment of the present invention, as shown in figure 1, this is used for13C- urea synthesizings Reactor, including pressure-resistant bottle 100 and communication means 200.Pressure-resistant bottle 100 is used to accommodate reactive material, reactive material bag Include liquid13CO and NH3And the elemental sulfur of solid-state.Communication means 200 are arranged on the pressure-resistant entrance of bottle 100, communication means 200 include the cross connecting tube 210 of inner hollow and the air inlet pipe 220 through cross connecting tube 210;Cross connecting tube 210 Including four connectors, respectively the first connector 211, the second connector 212, the 3rd connector 213, the 4th connector 214, The inner hollow of cross connecting tube 210, it is interconnected between four connectors;First connector 211 and the pressure-resistant entrance of bottle 100 Connection, by the inner space of the pressure-resistant bottle 100 of connection and the inside of cross connecting tube 210 of the first connector 211 Space does not have obstruction, forms connection;3rd connector 213 is oppositely arranged with the first connector 211, the air inlet of long straight pipe shape Pipe 220 is through the first connector 211 and the 3rd connector 213 and extends into inside pressure-resistant bottle 100;Cross connecting tube 210 Remaining two connectors are the second connector 212, the 4th connector 214, and relief valve 240 is installed in the connection of the second connector 212, For keeping the pressure inside cross connecting tube 210 and pressure-resistant bottle 100 to be no more than preset value, avoid because pacifying caused by superpressure The generation of full situation;4th connector 214 is oppositely arranged with the second connector 212, is duplex channel, can both be used as unstripped gas Entrance, can also be as the outlet of waste gas.
In addition, being sealed between the connector 213 of air inlet pipe 220 and the 3rd, i.e., the 3rd connector 213 is not used to any material Disengaging, sealing, the work of the 3rd connector 213 are realized by sealing mechanism in air inlet pipe 220 and the gap of the 3rd connector 213 With being to allow air inlet pipe 220 to be mainly that nitrogen and helium enter pressure-resistant bottle along air inlet pipe 220 by, purgative gas inside it Inside 100.
Fig. 2 shows the front view structure of reactor preferred embodiment of the present invention, as shown in Fig. 2 communication means 200 also include Connect the first extension pipeline 231 of the first connector 211 and the pressure-resistant entrance of bottle 100, be connected on the second connector 212 the Two extension pipelines 232, the 3rd extension pipeline 233 being connected on the 3rd connector 213, it is connected on the 4th connector 214 4th extension pipeline 234.
The first extension inner hollow of pipeline 231, one end connect with the sealing of the first connector 211, the other end and pressure-resistant bottle 100 inlet seals connect.By the connection function of the first extension pipeline 231, communication means 200 were both fixed on pressure-resistant bottle On 100 entrances, the connection between the inner space of pressure-resistant bottle 100 and the inner hollow of cross connecting tube 210 is realized again.
Relief valve 240 is mounted with second extension pipeline 232, ensures that the pressure in reaction system is less than preset value;Second The one end for extending pipeline 232 connects with the sealing of the second connector 212, other end sealing.Preferably, the relief valve 240 is machinery The ratio unloading valve of formula, can independently set critical pressure, can automatically turn on pressure release during more than setting value.
One end of 3rd extension pipeline 233 connects with the sealing of the 3rd connector 213, another away from the 3rd connector 213 End is connected to air inlet pipe 220 and extends pipeline;Air inlet pipe 220 is contained in the 3rd extension pipeline close to one end of the 3rd connector 213 Inside 233, sealing structure is set in the gap between the 3rd extension pipeline and air inlet pipe 220.Air inlet pipe 220 extends channel interior It is hollow and be connected with air inlet pipe 220;Air inlet pipe 220 extends is provided with the first globe type of control valve 251 and temperature, pressure on pipeline Detector 260.First globe type of control valve 251 is used for manual-lock and opens air inlet pipe 220, controls the flowing of purgative gas, temperature Temperature and pressure state in the moment of pressure detector 260 detection air inlet pipe 220.
One end of 4th extension pipeline 234 connects with the sealing of the 4th connector 214, the other end and feed gas source or outlet Pipeline connection;Already previously mentioned, the 4th connector 214 has double action, and the entrance of unstripped gas or the discharge of waste gas are all It is to be carried out in the 4th connector 214, when the 4th extension pipeline 234 connects with feed gas source, unstripped gas can flow through the 4th successively Connector 214, the first connector 211, and then enter pressure-resistant bottle 100;When the 4th extension pipeline 234 connects with outlet pipe When, waste gas can flow through the first connector 211, the 4th connector 214 successively, and then enter outlet pipe to discharge.Waste gas includes Purge the gases such as the purgative gas flowed into during reactor from air inlet pipe 220 and the air taken out of from pressure-resistant bottle 100;Also include urine The purgative gas flowed into from air inlet pipe 220 and the H taken out of from pressure-resistant bottle 100 after plain synthetic reaction is completed2The gases such as S.The The second globe type of control valve 252 is provided with four extension pipelines 234, controls the closing and unlatching of the 4th connector 214, and then control The entrance of unstripped gas or the discharge of waste gas.
Fig. 3 shows the structure of reactor communication means 200 of the present invention, as shown in figure 3, the air inlet pipe of long straight pipe shape 220 run through the first connector 211 and the 3rd connector 213 and extend into inside pressure-resistant bottle 100;The effect of air inlet pipe 220 It is that guiding purgative gas enters pressure-resistant bottle 100, but has single without the effect for discharging any gas, i.e. air inlet pipe 220 To air inlet act on.Due to the reactor relate separately to purge reactor, filling reaction gas, urea synthesizing in use it is anti- Answer, four basic steps of scavenging, the structure of first association reaction kettle is explained respectively.
When purging reactor, the first globe type of control valve 251 and the second globe type of control valve 252 are all in opening, air inlet Pipe 220 connects with source of purge gas, and the 4th connector 214 connects with outlet pipe, and purgative gas now is helium;Helium is along entering Tracheae 220 enters inside pressure-resistant bottle 100, and is mixed with the air in pressure-resistant bottle 100, and mixed gas flows through the first company successively Interface 211, the 4th connector 214, and enter outlet pipe, through helium purge after a while, it is used for emptying before inflation Residual air in reactor, and then close the first globe type of control valve 251 and the second globe type of control valve 252.
When filling reaction gas, the second globe type of control valve 252 is opened, the first globe type of control valve 251 is still within closed mode, 4th connector 214 connects with feed gas source, and unstripped gas can flow through the 4th connector 214, the first connector 211 successively, and then Into pressure-resistant bottle 100, liquid is cooled under strong refrigeration, falls into the bottom of bottle of pressure-resistant bottle 100, the lasting stream of unstripped gas Enter to complete the filling of unstripped gas, close the first globe type of control valve 251 and the second globe type of control valve 252 to carry out subsequent reactions.
During urea synthesis reaction, the first globe type of control valve 251 and the second globe type of control valve 252 all in closed mode, this When whole reactor there is no a substance circulating with extraneous, inside reactor13CO、S、NH3Reaction generation carbon【13C】- urea and H2S。
During scavenging, urea synthesis reaction has been completed.Because other raw materials are excessively launched to cause13CO can fill Divide reaction complete, so also remaining unreacted complete S, NH in reactor3With the H of reaction generation2S.First globe type of control valve 251 and second globe type of control valve 252 connected all in opening, air inlet pipe 220 with source of purge gas, the 4th connector 214 with Outlet pipe connects, and purgative gas now is nitrogen;Nitrogen along air inlet pipe 220 enter pressure-resistant bottle 100 inside, and with it is pressure-resistant Gas mixing in bottle 100, mixed gas flows through the first connector 211, the 4th connector 214 successively, and enters escape pipe Road, purged through nitrogen after a while, be used for emptying residual exhaust gases in reactor before inflation, and then close the first spherical control The globe type of control valve 252 of valve 251 and second processed.
Embodiments of the invention are described above in conjunction with accompanying drawing, but the invention is not limited in above-mentioned specific Embodiment, above-mentioned embodiment is only schematical, rather than restricted, one of ordinary skill in the art Under the enlightenment of the present invention, in the case of present inventive concept and scope of the claimed protection is not departed from, it can also make a lot Form, these are belonged within the protection of the present invention.

Claims (6)

1. one kind is used for13The reactor of C- urea synthesizings, it is characterised in that including the pressure-resistant bottle for accommodating reactive material (100), the communication means (200) on pressure-resistant bottle (100) entrance;Wherein, the communication means (200) include The cross connecting tube (210) of inner hollow and the air inlet pipe (220) through the cross connecting tube (210), the cross connect The first connector (211) that adapter (210) includes connect with pressure-resistant bottle (100) entrance, connection install the of relief valve (240) Two connectors (212), the 3rd connector (213) being oppositely arranged with first connector (211), for gas disengaging Four connectors (214), sealed between the air inlet pipe (220) and the 3rd connector (213), and the air inlet pipe (220) Through first connector (211) and the 3rd connector (213) and extend into pressure-resistant bottle (100) inside.
2. according to claim 1 be used for13The reactor of C- urea synthesizings, it is characterised in that the communication means (200) Also include connecting first connector (211) and the first extension pipeline (231) of pressure-resistant bottle (100) entrance;It is described First extension pipeline (231) inner hollow, one end and first connector (211) seal and connected, the other end with it is described pressure-resistant Bottle (100) inlet seal connects.
3. according to claim 1 be used for13The reactor of C- urea synthesizings, it is characterised in that the communication means (200) Also include the second extension pipeline (232) being connected on second connector (212), described second extends on pipeline (232) It is mounted with the relief valve (240);One end of the second extension pipeline (232) connects with second connector (212) sealing It is logical, the other end sealing of the second extension pipeline (232).
4. according to claim 1 be used for13The reactor of C- urea synthesizings, it is characterised in that the communication means (200) Also include the 3rd extension pipeline (233) being connected on the 3rd connector (213), the air inlet pipe (220) is close to described It is internal that one end of 3rd connector (213) is contained in the 3rd extension pipeline (233);The 3rd extension pipeline (233) One end connects with the 3rd connector (213) sealing, between the 3rd extension pipeline (233) and the air inlet pipe (220) Gap in sealing structure is set.
5. according to claim 4 be used for13The reactor of C- urea synthesizings, it is characterised in that the 3rd extension pipeline (233) other end away from the 3rd connector (213) is connected to air inlet pipe (220) extension pipeline, the air inlet pipe (220) Extension pipeline inner hollow is simultaneously connected with the air inlet pipe (220);First is provided with air inlet pipe (220) the extension pipeline Globe type of control valve (251) and temperature, pressure detector (260).
6. according to claim 1 be used for13The reactor of C- urea synthesizings, it is characterised in that the communication means (200) Also include the 4th extension pipeline (234) being connected on the 4th connector (214), the 4th extension pipeline (234) The sealing of one end and the 4th connector (214) connect, the other end and feed gas source of the 4th extension pipeline (234) or Outlet pipe connects;The second globe type of control valve (252) is provided with the 4th extension pipeline (234).
CN201610605180.5A 2016-07-27 2016-07-27 Is used for13Reaction kettle for synthesizing C-urea Active CN107661733B (en)

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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20060254645A1 (en) * 2005-05-13 2006-11-16 Barker Joseph R Enhanced purge effect in gas conduit
CN2864181Y (en) * 2005-12-16 2007-01-31 中国科学院力学研究所 Feed equipment with injection function
CN202010548U (en) * 2011-03-15 2011-10-19 禹州市维立特化工有限公司 Air intake device of chlorine reaction kettle
CN202015607U (en) * 2011-03-18 2011-10-26 东营市诺尔化工有限责任公司 Over-temperature and over-pressure automatically-controllable reaction kettle
CN102946987A (en) * 2010-03-31 2013-02-27 科学工业研究委员会 Hydrogen/syngas generator
CN204017807U (en) * 2014-03-05 2014-12-17 华东理工大学 Catalyzed chemical reaction device and for the air supply part of this device
CN205095752U (en) * 2015-11-04 2016-03-23 江西万里药业有限公司 Intermediate's improved generation gasification feed arrangement
CN205109638U (en) * 2015-11-11 2016-03-30 临海市建新化工有限公司 Sulfur bromide reation kettle

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20060254645A1 (en) * 2005-05-13 2006-11-16 Barker Joseph R Enhanced purge effect in gas conduit
CN2864181Y (en) * 2005-12-16 2007-01-31 中国科学院力学研究所 Feed equipment with injection function
CN102946987A (en) * 2010-03-31 2013-02-27 科学工业研究委员会 Hydrogen/syngas generator
CN202010548U (en) * 2011-03-15 2011-10-19 禹州市维立特化工有限公司 Air intake device of chlorine reaction kettle
CN202015607U (en) * 2011-03-18 2011-10-26 东营市诺尔化工有限责任公司 Over-temperature and over-pressure automatically-controllable reaction kettle
CN204017807U (en) * 2014-03-05 2014-12-17 华东理工大学 Catalyzed chemical reaction device and for the air supply part of this device
CN205095752U (en) * 2015-11-04 2016-03-23 江西万里药业有限公司 Intermediate's improved generation gasification feed arrangement
CN205109638U (en) * 2015-11-11 2016-03-30 临海市建新化工有限公司 Sulfur bromide reation kettle

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