CN106289580A - The calorimetric pond of flowing phase it is uniformly added in calorimetry apparatus - Google Patents
The calorimetric pond of flowing phase it is uniformly added in calorimetry apparatus Download PDFInfo
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- CN106289580A CN106289580A CN201610586387.2A CN201610586387A CN106289580A CN 106289580 A CN106289580 A CN 106289580A CN 201610586387 A CN201610586387 A CN 201610586387A CN 106289580 A CN106289580 A CN 106289580A
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- reaction tank
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- flowing phase
- calorimetric
- disperser
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K17/00—Measuring quantity of heat
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/20—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
- G01N25/48—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity on solution, sorption, or a chemical reaction not involving combustion or catalytic oxidation
- G01N25/4873—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity on solution, sorption, or a chemical reaction not involving combustion or catalytic oxidation for a flowing, e.g. gas sample
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/20—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
- G01N25/48—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity on solution, sorption, or a chemical reaction not involving combustion or catalytic oxidation
- G01N25/4873—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity on solution, sorption, or a chemical reaction not involving combustion or catalytic oxidation for a flowing, e.g. gas sample
- G01N25/488—Details
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Abstract
The present invention relates to a kind of calorimetric pond being uniformly added into flowing phase in calorimetry apparatus, mainly solve the problem that in prior art, mixed effect is bad.The present invention is by using a kind of calorimetric pond being uniformly added into flowing phase in calorimetry apparatus, including reaction tank shell, temperature and pressure sensor probe, fixing phase injection port, flowing phase sample intake passage, porous disperser, reaction tank top is provided with sleeve pipe, described temperature sensor probe is placed in the pipe box of concave, directly do not contact with sample, pressure transducer probe is positioned in reaction tank top gas phase space, fixing phase injection port is positioned at the top of reaction tank, flowing phase sample intake passage is positioned at reaction tank top, stretch into the one end within reaction tank to be connected with porous disperser, described porous disperser spreaded type is dispersed in bottom reaction tank or technical scheme in helically ascending manner is distributed in the space of reaction tank preferably solves the problems referred to above, can be used in calorimetric test.
Description
Technical field
The present invention relates to a kind of calorimetric pond being uniformly added into flowing phase in calorimetry apparatus.
Background technology
The hot blast danger of one concrete technology is evaluated, needs to obtain rate of heat release, thermal discharge, adiabatic temperature rise, thermal insulation
The parameters such as pressure liter, the acquisition of these parameters then must throughput Thermal test.Conventional calorimetry apparatus mainly includes preferable heat flow flux type
Calorimeter (C80, C600, DSC etc.) and accumulation heat flow flux type calorimeter (ARC, VSP2 etc.).
The object of calorimetric test typically has two kinds: the heat of transformation of one matter, decomposition heat and the heat of mixing of many kinds of substance, change
Learn reaction heat etc..Wherein, the mixing of many kinds of substance often refers to flow phase (gas phase, liquid phase) and fixing phase (liquid phase or liquid-solid mixed
Compound) mixing.
As a example by gas phase mixing in the liquid phase: a kind of common reaction formation is to be passed through in liquid phase by vapor-phase reactant,
Leave liquid phase after being fully contacted and enter gas-phase space.In order to ensure that gas phase is sufficiently mixed with liquid phase, more satisfactory situation is gas
It is separated as some small size bubbles, it is ensured that enough gas-to-liquid contact interfaces.In the industry, the dispersion of gas phase is often through installing additional
Allotter realizes.But this type of allotter cannot accommodate in small-sized calorimeter assembly, it is therefore desirable to one can be placed in small-sized calorimetric
The fluid foods of continuous feed is disperseed by the fluid dispersion structure in device reaction pond.
At present, multiple calorimeter is all with the reaction tank design allowing gas phase continuous feed.VSP such as FAI company joins
The reaction tank with feeding line (referring to VSP2 User ' s Manual and Test Method) put, Sai Talamu company
C80 configured gas circular response pond (http://www.setaram.cn/setaram-products/ calorimetric/calorimetric-
Calorimetric/c80-4/) etc..But above several designs all only one of which gaseous phase outlets, gas phase often generates after being passed in liquid phase
Large volume bubble, from bottom to top by entering gas-phase space after liquid phase.Gas phase is little with the contact area of liquid phase, the time is short, reaction
It is difficult to fully carry out.
The present invention is directed to that reaction tank improves gas phase and propose a kind of novel dispersion knot with the problem of liquid-phase mixing efficiency
Structure.
Summary of the invention
The technical problem to be solved is the problem that in prior art, mixed effect is bad, it is provided that a kind of new
Calorimetry apparatus is uniformly added into the calorimetric pond of flowing phase.The advantage that this calorimetric pond has good mixing effect.
For solving the problems referred to above, the technical solution used in the present invention is as follows: one is uniformly added into flowing in calorimetry apparatus
The calorimetric pond of phase, including reaction tank shell, temperature and pressure sensor probe, fixing phase injection port, flowing phase sample intake passage, many
Hole disperser, reaction tank top is provided with sleeve pipe, and described temperature sensor probe is placed in the pipe box of concave, not straight with sample
Contact, pressure transducer probe is positioned in reaction tank top gas phase space, and fixing phase injection port is positioned at the top of reaction tank, stream
Dynamic phase sample intake passage is positioned at reaction tank top, stretches into the one end within reaction tank and is connected with porous disperser, and described porous is disperseed
Device spreaded type is dispersed in bottom reaction tank or in helically ascending manner is distributed in the space of reaction tank, opening of described porous disperser
Porosity is 3%～15%, and porous disperser occupies volume is reaction tank volume 1%～the 7% of reaction tank.
In technique scheme, it is preferable that reaction tank shell is thin wall type or heavy wall type, calorimetry apparatus is preferable heat flow flux type
Or accumulation heat flow flux type.
In technique scheme, it is preferable that when porous disperser spreaded type is dispersed in bottom reaction tank, porous disperser is
Coiled or lantern ring type.
In technique scheme, it is preferable that calorimetric pond is additionally provided with standby injection port, other is kept for need the material added
With.
In technique scheme, it is preferable that as required, calorimetric pond arranges magnetic stirring equipment, and magneton needs are placed on many
The lower section of hole disperser.
The present invention relates to a kind of flowing phase feed arrangement being applicable to calorimetry apparatus and method, main purpose is to strengthen
Heat and mass effect between liquid phase in reaction tank.Technological difficulties to be solved by this invention are: 1) flowing phase (gas phase or
Liquid phase) continuous feed, system may need be fully contacted instead with high pressure, flowing and fixing phase (original material in reaction tank)
In the case of Ying, it is provided that a kind of new the two contact area of increase, the device of raising mixing efficiency.2) one is provided in contrast
That answers realizes mixed uniformly method.The invention provides a kind of reaction tank device being applicable to continuous feed calorimetric process and side
Method, compared with prior art, the present invention can intensified response heat and mass, promote the rapid mixing of material, shorten the response time,
Reduce possible side reaction, achieve preferable technique effect.
Accompanying drawing explanation
Fig. 1 is one of the structural representation in calorimetric pond of the present invention.
Fig. 2 is the two of the structural representation in calorimetric pond of the present invention.
Fig. 3 is the three of the structural representation in calorimetric pond of the present invention.
In Fig. 1-Fig. 3,1-reaction tank shell, 2-temperature sensor probe, 3-pressure transducer are popped one's head in and fix phase sample introduction
Mouthful, 4-flows phase sample intake passage, 5-porous disperser.
Below by embodiment, the invention will be further elaborated, but is not limited only to the present embodiment.
Detailed description of the invention
[embodiment 1]
A kind of calorimetric pond being uniformly added into flowing phase in calorimetry apparatus, as it is shown in figure 1, include outside reaction tank, reaction tank
Shell, temperature and pressure sensor probe, fixing phase injection port, flowing phase sample intake passage, porous disperser, reaction tank top is provided with
Sleeve pipe, described temperature sensor probe is placed in the pipe box of concave, does not directly contact with sample, pressure transducer probe position
In reaction tank top gas phase space, fixing phase injection port is positioned at the top of reaction tank, and flowing phase sample intake passage is positioned at reaction tank
Top, stretches into the one end within reaction tank and is connected with porous disperser, and described porous disperser spreaded type is dispersed at the bottom of reaction tank
Portion or in helically ascending manner is distributed in the space of reaction tank, the percent opening of described porous disperser is 7%, and porous disperser accounts for
Respond volume is reaction tank volume the 2% of pond.
Reaction tank shell: depend on used calorimetric instrument classification, reaction tank shell be thin wall type (as VSP,
PhiTECII), calorimetry apparatus is preferable heat flow flux type.
Temperature and pressure transmitter is popped one's head in: temperature sensor probe can be placed in the pipe box of a concave, not with sample
Product directly contact.Pressure transducer probe needs to be placed in reaction tank top gas phase space.
Fixing phase injection port: fix and be generally contained in the most in advance in reaction tank mutually, this injection port can be in reaction
During close.
Flowing phase sample intake passage: connect outside material source (such as gas cylinder, high-pressure pump etc.) and disperser.
Porous disperser: disperser spreaded type is dispersed in bottom reaction tank, disperser is coiled.
Other injection port: other can be kept for need the material added.
Stirring: owing to flowing has served the effect of stirring mixing during by fixing phase, in reaction tank
Electromagnetic agitation can not be set.If needing to arrange extra stirring, magneton needs to be placed on the lower section of disperser.
The using method in this calorimetric pond is:
Disperser should be preset in pond when processing reaction tank.By fixing phase sample introduction before reaction tank is put into calorimeter
Mouth puts into fixing phase sample, places temperature, pressure transducer probe, connects injection port and outside material source.Keep outside injection port
Portion's valve closing.
Course of reaction needs when adding flowing phase materials, open valve, it is provided that flowing after certain pressure mutually will be by dividing
Loose structure on scattered device enters in fixing mutually.When flowing is gas mutually, the size of bubble depends on gas phase flow velocity and duct
Size, can change the size of bubble and the speed of charging by changing gas phase flow velocity.When flowing is to dissolve each other mutually with fixing mutually
During liquid phase, flowing i.e. mixes with fixing phase after by disperser at once, owing to disperser outlet is covered with at the bottom of whole reaction tank
Portion, the two time diffusing into one another needs is shorter, can improve mass transfer and heat transfer rate.When flowing is mutually immiscible with fixing mutually
Liquid time, flowing mutually will fixing mutually in form oil/water or water/fluid drip, same, the size of drop depends on the phase that flows
Flow velocity and the size in duct, by change flow rate of mobile phase can change the size of drop and the speed of charging.
This reaction tank is utilized to carry out calorimetric test on VSP2
Experimental procedure:
(1) weigh fixing phase sample, add in reaction tank；
(2) heater is installed, reaction tank is put in outer still, connect feeding line, heater and temperature sensor lead,
Reaction tank ground connection, to get rid of signal noise；Glass cotton is filled up in space between reaction tank and outer still, covers kettle cover, seal height
Pressure still；
(3) by table test lead connection state and insulating properties, set heating schedule parameter, start VSP2 system and to temperature
Degree, piezometry system are corrected；
(4) open the electromagnetic valve on vacuum pipeline, start vacuum pump, pressure in outer still is evacuated to-0.09MPa (g) below
Rear holding ten minutes, the air-tightness of trial inspection system；
(5) open compensation gas bottle valve, open pressure automatic tracking system；Open the counterbalance valve on circuit of releasing, adjust
Joint pressure is to 1MPa.Flowing phase feeding line accesses hydrogen cylinder, squeezes into hydrogen in reaction tank.
(6) start heating system, start super magnetic stirring apparatus, start to heat up by setup program.Start cooling system with
Protection pressure transducer.
(7) observation experiment pressure, variations in temperature, record experimental phenomena is until experiment terminates.
By increasing Gas distribution, increase gas liquid interfacial area, simulate actual condition more accurately, make result more accurate
The most reliable, decrease the gas-liquid mixed impact on reaction.
[embodiment 2]
According to the condition described in embodiment and step, as in figure 2 it is shown, disperser spreaded type is dispersed in bottom reaction tank, point
Scattered device is lantern ring type.Reaction tank shell is heavy wall type (such as ARC, C80), and calorimetry apparatus is accumulation heat flow flux type.Described porous is disperseed
The percent opening of device is 5%, and porous disperser occupies volume is reaction tank volume the 4% of reaction tank.
[embodiment 3]
According to the condition described in embodiment and step, as it is shown on figure 3, disperser helically ascending manner is distributed in reaction tank
In space, disperser is lantern ring type.The percent opening of described porous disperser is 10%, and porous disperser occupies the volume of reaction tank
For reaction tank volume 5%.
[comparative example]
Conventional calorimetric pond and calorimetric pond of the present invention is utilized to do the oxychloride reaction of N, N-dimethyl-4,4-coupling pyridine.
A certain amount of water and N, N-dimethyl-4,4-coupling pyridine, experimental procedure such as embodiment 1 institute it is initially charged in calorimetric pond
State.Conventional calorimetric pond is all passed through a certain amount of chlorine with calorimetric pond of the present invention.Experimental data shows, utilizes calorimetric pond of the present invention to detect
To the temperature that detects with conventional pond of exothermic temperature Billy low 3 DEG C, this is owing to calorimetric pond of the present invention gas-liquid mixed is preferable, increases
Big gas liquid interfacial area, is beneficial to reaction, and additionally Temperature Distribution is more uniform, beneficially instrument detection.At a certain temperature anti-
Answering end reaction temperature the most more conventional calorimetric pond high 10 DEG C, this is owing to increasing gas liquid interfacial area, and gas-liquid mixed is preferable, instead
The amount of chlorine answered increases, and exothermic heat of reaction is more, closer to actual condition.
Claims (5)
1. in calorimetry apparatus, it is uniformly added into a calorimetric pond for flowing phase, including reaction tank shell, temperature and pressure sensor
Probe, fixing phase injection port, flowing phase sample intake passage, porous disperser, reaction tank top is provided with sleeve pipe, described temperature sensor
Probe placement, in the pipe box of concave, does not directly contact with sample, and it is empty that pressure transducer probe is positioned at reaction tank top gas phase
In between, fixing phase injection port is positioned at the top of reaction tank, and flowing phase sample intake passage is positioned at reaction tank top, stretches into inside reaction tank
One end be connected with porous disperser, described porous disperser spreaded type is dispersed in bottom reaction tank or helically ascending manner distribution
In the space of reaction tank, the percent opening of described porous disperser is 3%～15%, and porous disperser occupies the volume of reaction tank
For reaction tank volume 1%～7%.
The calorimetric pond of flowing phase it is uniformly added into the most according to claim 1, it is characterised in that outside reaction tank in calorimetry apparatus
Shell is thin wall type or heavy wall type, and calorimetry apparatus is preferable heat flow flux type or accumulation heat flow flux type.
The calorimetric pond of flowing phase it is uniformly added into the most according to claim 1, it is characterised in that porous is disperseed in calorimetry apparatus
When device spreaded type is dispersed in bottom reaction tank, porous disperser is coiled or lantern ring type.
The calorimetric pond of flowing phase it is uniformly added into the most according to claim 1, it is characterised in that calorimetric pond is also in calorimetry apparatus
It is provided with standby injection port, keeps for other to need the material added to use.
The calorimetric pond of flowing phase it is uniformly added into the most according to claim 1, it is characterised in that as required in calorimetry apparatus,
Calorimetric pond arranges magnetic stirring equipment, and magneton needs to be placed on the lower section of porous disperser.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610586387.2A CN106289580B (en) | 2016-07-22 | 2016-07-22 | The calorimetric pond of mobile phase is uniformly added into calorimetry apparatus |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610586387.2A CN106289580B (en) | 2016-07-22 | 2016-07-22 | The calorimetric pond of mobile phase is uniformly added into calorimetry apparatus |
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| CN106289580B CN106289580B (en) | 2019-06-25 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109781779A (en) * | 2018-12-29 | 2019-05-21 | 西安交通大学 | A kind of method and device suitable for measuring molten air-flow body specific heat capacity at constant pressure |
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| CN103196784A (en) * | 2013-04-08 | 2013-07-10 | 北京科技大学 | Device and method for measuring gas-liquid chemical reaction rate based on volumetric method |
| CN104492295A (en) * | 2014-12-04 | 2015-04-08 | 苏州国环环境检测有限公司 | Pre-mixing and dispersing system for detection |
| CN104730106A (en) * | 2015-04-02 | 2015-06-24 | 中国工程物理研究院总体工程研究所 | Liquid constant pressure specific heat measurement device |
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2016
- 2016-07-22 CN CN201610586387.2A patent/CN106289580B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4809190A (en) * | 1987-04-08 | 1989-02-28 | General Signal Corporation | Calorimetry system |
| US6335464B1 (en) * | 1997-09-08 | 2002-01-01 | Chugai Seiyaku Kabushiki Kaisha | Process for selectively oxidizing primary hydroxyl groups of organic compounds, and resin containing adsorbed catalyst for use therein |
| CN1530467A (en) * | 2003-03-17 | 2004-09-22 | 四川大学 | Automatic calorimeter in electrolytic process |
| CN2746389Y (en) * | 2004-07-27 | 2005-12-14 | 徐江兴 | Gas-solid phase photocatalysis reaction transition process calorimetric device |
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| CN103196784A (en) * | 2013-04-08 | 2013-07-10 | 北京科技大学 | Device and method for measuring gas-liquid chemical reaction rate based on volumetric method |
| CN104492295A (en) * | 2014-12-04 | 2015-04-08 | 苏州国环环境检测有限公司 | Pre-mixing and dispersing system for detection |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109781779A (en) * | 2018-12-29 | 2019-05-21 | 西安交通大学 | A kind of method and device suitable for measuring molten air-flow body specific heat capacity at constant pressure |
| CN109781779B (en) * | 2018-12-29 | 2021-01-19 | 西安交通大学 | Method and device suitable for measuring specific constant pressure heat capacity of dissolved gas fluid |
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| CN106289580B (en) | 2019-06-25 |
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