CN1959394A - Calorimetry instrument in accelerated speed - Google Patents

Calorimetry instrument in accelerated speed Download PDF

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Publication number
CN1959394A
CN1959394A CN 200610147145 CN200610147145A CN1959394A CN 1959394 A CN1959394 A CN 1959394A CN 200610147145 CN200610147145 CN 200610147145 CN 200610147145 A CN200610147145 A CN 200610147145A CN 1959394 A CN1959394 A CN 1959394A
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China
Prior art keywords
gas
calorimetric
ball
vapor
accelerated speed
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CN 200610147145
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CN100578207C (en
Inventor
谢传欣
王慧欣
黄飞
金满平
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China Petroleum and Chemical Corp
China Petrochemical Corp
Sinopec Qingdao Safety Engineering Institute
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China Petroleum and Chemical Corp
Sinopec Qingdao Safety Engineering Institute
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Publication of CN1959394A publication Critical patent/CN1959394A/en
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Abstract

A calorimeter of acceleration rate consists of air source, buffer tank, precise air flow-meter, ARC adiabatic environment and its data recording/ processing unit. It is featured as connecting above-said units in sequence, setting saturated steam air generator between air flow-meter and calorimetric bomb in sample chamber at ARC adiabatic environment, setting air exhaust pipe outlet on calorimetric bomb and connecting air outlet pipe of said generator to sample reaction chamber and to calorimetric bomb.

Description

Calorimetry instrument in accelerated speed
Technical field
The present invention relates to estimate the improvement of the thermal analyzer of material thermal stability, specifically is a kind of Calorimetry instrument in accelerated speed, and it belongs to material thermal measurement instrument and equipment technical field.
Background technology
Calorimetry instrument in accelerated speed of the prior art (abbreviates as: ARC) be a kind of thermal analyzer based on the adiabatic principle design.Its principle is the adiabatic environment that reaction system is placed ARC, by the operation of heating-wait-search (H-W-S) and two kinds of patterns of isothermal, and heat, the pressure hazard of the potential runaway reaction of analogue measurement and some chemicals of quantification and potpourri.Current, Calorimetry instrument in accelerated speed has become one of means of testing commonly used of estimating the material thermal stability in the world, and progressively develops to being called the standard method of test direction.Yet this instrument can be a research object with the closed system only, is difficult to simulate the operating environment of industrialized unit.And often be to be research object in industrial practical application with the open system.In order to expand the usable range of ARC, make that the gas system of ARC is a research object with the open system, make it use the operating environment that more is intended for industrialized unit; This just needs to increase open gas system, joins in the ARC system.The steam generator of prior art generally is a boiler formula high temperature and high pressure steam system.Yet the working environment that Simulated Water steam exists in the ARC system does not need high temperature and high pressure steam.Technological difficulties to be solved by this invention are: 1) how to satisfy the demand to the steady supply of the cryogenic gas of adjustable certain flow, how to design more stable gas supply system; 2) how to satisfy the requirement of the adiabatic environment of ARC; 3) how to satisfy carrying the demand of saturated vapor secretly; 4) how to satisfy the problem of effective solution vapor-liquid separation.According to the situation of literature search and market survey, still there is not the test unit that similarly supplies the working environment that Simulated Water steam exists in the ARC system both at home and abroad.
Summary of the invention
The objective of the invention is to provide a kind of to open the Calorimetry instrument in accelerated speed that gas system is a research object, expand the usable range of ARC, make its application more can be intended for the operating environment of industrialized unit, thereby satisfied the safety assessment of the operating environment in the simulation petrochemical equipment.
The objective of the invention is to realize that by following technical scheme developed a kind of Calorimetry instrument in accelerated speed, it comprises: the source of the gas of Jie Tonging successively, surge tank, accurate gas meter, ARC adiabatic environment and data recording thereof.Open stabilizing gas supply line is set in the sample chamber of ARC adiabatic environment, the gas generator of saturated vapor promptly is set between the calorimetric ball in this gas meter and ARC adiabatic environment sample chamber, the gas outlet tube termination of this generator passes in this calorimetric ball, this calorimetric ball also is provided with exhaust pipe mouth, and this exhaust pipe mouth turns on the gas emptying mouth of pipe place of sample chamber again.
Described gas outlet tube is before turning on this calorimetric ball, and its pipeline twines at least one week around this calorimetric ball outer wall profile earlier, is switched in this calorimetric ball again.
The gas generator of described saturated vapor, it is for having electric heater, temperature controller, the water bath with thermostatic control airtight container of upper and lower water pipeline; Appropriate position in this container water layer upper cavity is provided with the vapor-liquid separation layer, the gas feed pipe end that passes this chamber wall immerses in the water layer bottom, gas outlet tube one end is arranged on the appropriate position in the vapor-liquid separation layer upper cavity, and the other end of this gas outlet tube passes this chamber wall and is switched in the example reaction chamber.
Described vapor-liquid separation layer, it is the glass fiber cotton layer, or be perlite matter layer, or is the asbestine layer; The thickness of this vapor-liquid separation layer is at 1-5mm.
Described water bath with thermostatic control airtight container, the temperature controlling range of its temperature controller customization is at 5-100 ℃.
Described gas, itself or be the air of certain flow, or be the nitrogen of certain flow; This gas flow scope is below 200mL/min.
The invention has the advantages that: because open stabilizing gas supply line is set in the sample chamber of ARC adiabatic environment, the gas generator of saturated vapor promptly is set between the calorimetric ball in this gas meter and ARC adiabatic environment sample chamber, the gas outlet tube termination of this generator passes in this calorimetric ball, this calorimetric ball also is provided with exhaust pipe mouth, and this exhaust pipe mouth turns on the gas emptying mouth of pipe place of sample chamber again.Make that ARC of the present invention can be a research object to open gas system.Expand the usable range of ARC like this, made its application more can be intended for the operating environment of industrialized unit, thereby satisfied the safety assessment of the operating environment in the simulation petrochemical equipment.Because described gas outlet tube is before turning on this calorimetric ball, its pipeline twines at least one week around this calorimetric ball outer wall profile earlier, is switched in this calorimetric ball again.Can make the flow of cryogenic gas adjustable and steadily be supplied in this calorimetric ball like this.
Owing to developed a kind of saturated water vapor generator, it comprises: have electric heater, temperature controller, the water bath with thermostatic control airtight container of upper and lower water pipeline.Appropriate position in this container water layer upper cavity is provided with the vapor-liquid separation layer, the gas feed pipe end that passes this chamber wall immerses in the water layer bottom, gas outlet tube one end is arranged on the appropriate position in the vapor-liquid separation layer upper cavity, and the other end of this gas outlet tube passes in the example reaction chamber that this chamber wall is switched to system.Because electrically heated rod in the water bath with thermostatic control airtight container and temperature controller can be controlled in temperature 5-100 ℃ of water bath with thermostatic control, to obtain the temperature of the desired water vapour of experiment.When bottom that the air (or nitrogen) of certain flow is continued to feed water bath with thermostatic control via stainless-steel tube, sufficient the contact arranged with the water of specified temp, increase along with the internal pressure of water bath with thermostatic control, the air of carrying water vapour (containing fine drop) secretly via glass silk flosssilk wadding layer (or for perlite matter layer, or be the asbestine layer) time, thereby tiny drop is adsorbed the effect of having played vapor-liquid separation by vapor-liquid separation layers such as glass silk flosssilk waddings, and the air (or nitrogen) of then carrying water vapour secretly leaves water bath with thermostatic control via gas outlet tube.The present invention can simulate heat, the pressure hazard of potential runaway reaction and some chemicals of quantification and potpourri because the saturated water vapor generator of ARC exploitation has been expanded the usable range of ARC, promptly is used to study the thermostability and the assessment of hot harmfulness of material.
Description of drawings
Fig. 1 is the structural representation of Calorimetry instrument in accelerated speed.
Fig. 2 is the structural representation of the air inlet pipeline of calorimetric ball around its ball outer wall profile.
Fig. 3 is the sectional structure synoptic diagram of saturated water vapor generator.
Embodiment
Embodiments of the invention further specify as follows in conjunction with experiment and accompanying drawing thereof:
Referring to a kind of Calorimetry instrument in accelerated speed that Fig. 1-3 makes, it comprises: the source of the gas of connecting surge tank 10 successively---air steel cylinder 8, nitrogen steel cylinder 9, accurate gas meter 11, ARC adiabatic environment casing 12 and data recording 13 thereof.Open stabilizing gas supply line is set in the sample chamber 14 of ARC adiabatic environment, the gas generator 17 of saturated vapor promptly is set between the calorimetric ball 16 in this gas meter 11 and ARC adiabatic environment sample chamber 14, gas outlet tube 2 ends of this generator 17 are switched in this calorimetric ball 16 by pipeline 15, this calorimetric ball 16 also is provided with exhaust pipe mouth 18, and this exhaust pipe mouth 18 turns on the gas emptying mouth of pipe 19 places of sample chamber again.
Described gas outlet tube 2 is before turning on this calorimetric ball 16, and its pipeline twines at least one week around these calorimetric ball 16 outer wall profiles earlier, is switched in this calorimetric ball 16 again.
Described saturated water vapor generator, it comprises: have electric heater 4, temperature controller (not drawing among the figure), the water bath with thermostatic control airtight container 5 of upper and lower water pipeline 6,7.Appropriate position in this container water layer upper cavity is provided with the vapor-liquid separation layer 1 of glass silk floss, gas inlet tube 3 ends that pass this chamber wall immerse in the water layer bottom, gas outlet tube 2 one ends are arranged on the appropriate position in vapor-liquid separation layer 1 upper cavity, and the other end of this gas outlet tube 2 passes in the example reaction chamber (not drawing among the figure) that these container 5 walls are switched to system.Described vapor-liquid separation layer 1, it is the glass fiber cotton layer, or is the asbestine layer; The thickness of this vapor-liquid separation layer is at 2mm.Described water bath with thermostatic control airtight container 5, the temperature controlling range of its temperature controller customization is at 5-100 ℃.Described gas, itself or be the air of certain flow, or be the nitrogen of certain flow; This gas flow scope is 200,150,100 or 60mL/min.
After Calorimetry instrument in accelerated speed of the present invention completes, utilize ARC to carry out the research of spontaneous burning mechanism of FeS in sulfur, device ruuning situation is stable in the experiment, and temperature control is good, and the vapor-liquid separation effect is obvious, has reached experiment effect preferably.
Those of ordinary skill in the art can understand, and in protection scope of the present invention, makes amendment for the foregoing description, and it all is possible adding and replacing, and it does not all exceed protection scope of the present invention.

Claims (6)

1, a kind of Calorimetry instrument in accelerated speed, it comprises: the source of the gas of Jie Tonging successively, surge tank, accurate gas meter, ARC adiabatic environment and data recording thereof, it is characterized in that: open stabilizing gas supply line is set in the sample chamber of ARC adiabatic environment, the gas generator of saturated vapor promptly is set between the calorimetric ball in this gas meter and ARC adiabatic environment sample chamber, the gas outlet tube termination of this generator passes in this calorimetric ball, this calorimetric ball also is provided with exhaust pipe mouth, and this exhaust pipe mouth turns on the gas emptying mouth of pipe place of sample chamber again.
2, according to the described Calorimetry instrument in accelerated speed of claim 1, it is characterized in that: described gas outlet tube is before turning on this calorimetric ball, and its pipeline twines at least one week around this calorimetric ball outer wall profile earlier, is switched in this calorimetric ball again.
3, according to the described Calorimetry instrument in accelerated speed of claim 1, it is characterized in that: the gas generator of described saturated vapor, it is for having electric heater, temperature controller, the water bath with thermostatic control airtight container of upper and lower water pipeline; Appropriate position in this container water layer upper cavity is provided with the vapor-liquid separation layer, the gas feed pipe end that passes this chamber wall immerses in the water layer bottom, gas outlet tube one end is arranged on the appropriate position in the vapor-liquid separation layer upper cavity, and the other end of this gas outlet tube passes this chamber wall and is switched in the example reaction chamber.
4, according to the described Calorimetry instrument in accelerated speed of claim 3, it is characterized in that: described vapor-liquid separation layer, it is the glass fiber cotton layer, or be perlite matter layer, or is the asbestine layer; The thickness of this vapor-liquid separation layer is at 1-5mm.
5, according to the described Calorimetry instrument in accelerated speed of claim 3, it is characterized in that: described water bath with thermostatic control airtight container, the temperature controlling range of its temperature controller customization is at 5-100 ℃.
6, according to claim 1 or 2 or 3 described Calorimetry instrument in accelerated speed, it is characterized in that: described gas, itself or be the air of certain flow, or be the nitrogen of certain flow; This gas flow scope is below 200mL/min.
CN200610147145A 2006-08-23 2006-11-04 Calorimetry instrument in accelerated speed Expired - Fee Related CN100578207C (en)

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CN200610147145A CN100578207C (en) 2006-08-23 2006-11-04 Calorimetry instrument in accelerated speed

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CN200610068572.9 2006-08-23
CN200610068572 2006-08-23
CN200610147145A CN100578207C (en) 2006-08-23 2006-11-04 Calorimetry instrument in accelerated speed

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CN1959394A true CN1959394A (en) 2007-05-09
CN100578207C CN100578207C (en) 2010-01-06

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101413862B (en) * 2008-11-11 2010-12-01 中国石油化工股份有限公司 Apparatus for testing velocity of inflammable gas given out by substance when contacting with water
CN103180463A (en) * 2010-10-22 2013-06-26 霍夫曼-拉罗奇有限公司 A conjugate between a thiophilic solid phase and an oligonucleotide comprising a thiooxonucleotide
CN104330743A (en) * 2014-11-28 2015-02-04 南京工业大学 lithium ion battery thermal runaway test analysis system
CN104655671A (en) * 2014-12-31 2015-05-27 威仕英索(北京)仪器设备有限公司 Adiabatic accelerating rate calorimeter and detection method thereof
CN106289580A (en) * 2016-07-22 2017-01-04 中国石油化工股份有限公司 The calorimetric pond of flowing phase it is uniformly added in calorimetry apparatus

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101413862B (en) * 2008-11-11 2010-12-01 中国石油化工股份有限公司 Apparatus for testing velocity of inflammable gas given out by substance when contacting with water
CN103180463A (en) * 2010-10-22 2013-06-26 霍夫曼-拉罗奇有限公司 A conjugate between a thiophilic solid phase and an oligonucleotide comprising a thiooxonucleotide
CN103180463B (en) * 2010-10-22 2014-12-31 霍夫曼-拉罗奇有限公司 A conjugate between a thiophilic solid phase and an oligonucleotide comprising a thiooxonucleotide
US8981070B2 (en) 2010-10-22 2015-03-17 Roche Diagnostics Operations, Inc. Conjugate between a thiophilic solid phase and an oligonucleotide comprising a thiooxonucleotide
CN104330743A (en) * 2014-11-28 2015-02-04 南京工业大学 lithium ion battery thermal runaway test analysis system
CN104330743B (en) * 2014-11-28 2017-02-22 南京工业大学 lithium ion battery thermal runaway test analysis system
CN104655671A (en) * 2014-12-31 2015-05-27 威仕英索(北京)仪器设备有限公司 Adiabatic accelerating rate calorimeter and detection method thereof
CN104655671B (en) * 2014-12-31 2017-08-25 威仕英索(北京)仪器设备有限公司 Adiabatic accelerating calorimeter and detection method
CN106289580A (en) * 2016-07-22 2017-01-04 中国石油化工股份有限公司 The calorimetric pond of flowing phase it is uniformly added in calorimetry apparatus
CN106289580B (en) * 2016-07-22 2019-06-25 中国石油化工股份有限公司 The calorimetric pond of mobile phase is uniformly added into calorimetry apparatus

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