CN103604825A - Method for testing self-reaction mixture thermal compatibility - Google Patents
Method for testing self-reaction mixture thermal compatibility Download PDFInfo
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- CN103604825A CN103604825A CN201310488267.5A CN201310488267A CN103604825A CN 103604825 A CN103604825 A CN 103604825A CN 201310488267 A CN201310488267 A CN 201310488267A CN 103604825 A CN103604825 A CN 103604825A
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Abstract
The invention relates to a method for testing a self-reaction mixture thermal compatibility, which mainly solves the problems of long test period, high danger and large required sample amount in prior art. The invention uses employs a method for testing self-reaction mixture thermal compatibility, which comprises the following steps: Wood's alloy bath is used as a temperature control medium; at different temperatures, a function relationship about time t needed by self-reaction of self-reaction mixture is established; reaction activation energy E of self-reaction mixture and constant C about sample component are analyzed by a regression analysis and a corresponding function curve is drawn; the self-reaction mixture is compared with temperature T and self-reaction temperature t of single pure self-reaction material; the thermal sensitivity of the self-reaction mixture is analyzed qualitatively and quantitatively, thereby the thermal compatibility of each substance in the mixture is obtained, and according to the prior art, the problem is solved; the method can be applied to the screening test for thermal compatibility of the self-reaction mixture.
Description
Technical field
The present invention relates to a kind of method of testing of autoreaction potpourri thermal compatibility.
Technical background
, can there is autoreaction because of multiple different extraneous factor (as hot, optical, electrical, spark etc.) in autoreaction chemical substance, during under household condition independent accumulating, generally do not show autoreaction danger.And while coming in contact in the mixed storage of the generations such as such material and some organic peroxide matter, oxidizing substance, induced material or transportation; usually can reduce the autoreaction condition of autoreaction material, increase susceptibility and the possibility of its performance autoreaction danger.So the blast of joining rule and causing because of autoreaction for prevention is prohibited in the mixed storage of such material of preliminary screening, the serious accident such as out of control occurs and safety in transportation and storage important in inhibiting.
Evaluation and formulation for autoreaction chemical substance thermal compatibility; do not have at present the clear and definite world or unification of the motherland standard; conventionally can utilize gram southern test unit or reaction calorimeter to assess the mixed storage situation of material, but these two kinds of methods all exist drawback separately.
Gram south test needs sample size large, if run into the danger that responsive autoreaction material has steel pipe explosion, there is potential safety hazard, and in experimentation, take propane burning as thermal source, cannot control heating-up temperature, cause its assessment to sample temperature-sensitive sensitivity can only rest on qualitative level; Although reaction calorimeter can provide reaction heat data accurately for autoreaction chemicals thermal compatibility situation, the method test period is long, and instrument and equipment is expensive, and test condition is harsh, is unfavorable for promotion and application.
CN201210137946 discloses a kind of solid and insulating oil compatibility test device, and it comprises oil tank and oil hole thereof, characterized by further comprising: the funnel that center is threaded and is communicated with flowline on described oil tank by tubular configured joint below; Be located at described oil tank one middle side part, and communicate with oil tank inner chamber, for sample pipe and the gland thereof of test specimen are set; In described filler tube straight coupling, being provided with upper end is the conical plug that cylindricality lower end is; Be located at described oil tank one side lower curtate, and the petroleum pipeline communicating with oil tank inner chamber.This apparatus structure is simple, and easy to use, low cost and accuracy are high, test specimen being housed and filling oily proving installation, puts into baking box, is heated to after the time and temperature of setting, oil is taken out to the compatibility of measuring solid and insulating oil with oil colours spectrometry.
The autoreaction material forming for difference, the self-reacting susceptibility of thermic is had nothing in common with each other, thereby can be using the temperature-sensitive sensitivity of autoreaction material performance during with other different materials, the mixed storage of different proportion as the mixed measurement index that stores up compatibility of these two kinds of materials.By under different temperatures, the needed time of potpourri generation autoreaction containing autoreaction material is set up funtcional relationship, and draw respective function curve, can carry out quantitative test to the temperature-sensitive sensitivity of this potpourri, by these data with mix before thermo-responsive degrees of data comparison, thereby draw each substances compatible sex determination result in this potpourri.According to the situation of existing literature search and market survey, domestic not yet have relevant mechanism to carry out the research of autoreaction chemical substance thermal compatibility according to the method.
Summary of the invention
Technical matters to be solved by this invention is the large problem of long, dangerous high, required sample size of test period in prior art, and a kind of method of testing of new autoreaction potpourri thermal compatibility is provided.The method, for the test of reactive mixture thermal compatibility, has advantages of that short, dangerous low, required sample size of test period is little.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows: a kind of method of testing of autoreaction potpourri thermal compatibility, the Wood's metal of usining is bathed as temperature control medium, by under different temperatures T, contains the needed time τ of autoreaction potpourri generation autoreaction and sets up
funtcional relationship, return out reaction activity E and the constant C relevant with sample composition containing autoreaction potpourri, draw respective function curve, this autoreaction potpourri is compared with temperature T and the autoreaction time τ curve of single pure autoreaction material, temperature-sensitive sensitivity to this autoreaction potpourri is carried out qualitative and quantitative analysis, thereby draws each substances compatible sex determination result in this potpourri.
In technique scheme, preferably, described test is the test of 5s lag phase bursting point.
In technique scheme, preferably, described blend sample is loaded into described Can bottom, and has special-purpose copper plug Can port jam-pack, guarantees its impermeability, and connects copper plug with connecting line, in case rear copper plug occurs autoreaction, flies out.
In technique scheme, preferably, described Wood's metal body lotion reaches after testing requirements temperature T, Can is inserted in alloy body lotion, and timer is subject to induction to start timing, and autoreaction also occurs along with being heated sample, until copper plug on metal tube, after being jumped out, stop timing, record this time.
In technique scheme, preferably, under described each temperature of reaction T, carry out at least three group parallel experiments, obtain at least three autoreaction time τ, then ask for average.
The autoreaction potpourri forming for difference, the self-reacting susceptibility of single pure autoreaction material is had nothing in common with each other, thereby the temperature-sensitive sensitivity of performance can be using autoreaction material and other different materials, the mixed storage of different proportion time is as the measurement index of the mixed storage of these two kinds of materials compatibility.By under different temperatures, the needed time of potpourri generation autoreaction containing autoreaction material is set up funtcional relationship, and draw respective function curve, can carry out quantitative test to the temperature-sensitive sensitivity of this potpourri, by these data with mix before thermo-responsive degrees of data comparison, thereby draw each substances compatible sex determination result in this potpourri.Record after temperature of reaction T and average autoreaction time τ, carry out according to the following formula statistical computation:
In formula: E-is containing the potpourri reaction activity of autoreaction material, J/mol;
R-gas law constant, J/ (mol*K);
The constant that C-is relevant with sample composition;
Τ-average autoreaction time, min;
T-temperature of reaction, K.
Conversion can obtain:
Bring thus the corresponding autoreaction time τ of each temperature spot T into, can by simple regression method obtain lnc and
thereby draw out respective function relation curve.This potpourri is compared with temperature T-autoreaction time τ curve of pure autoreaction material, and it is larger that straight slope differs, and mixed storage is larger to stability influence, and follow-up compatibility test is played to preliminary screening and directive function.
The present invention adopts Wood's metal to bathe as temperature control medium, and by studying under different temperatures, containing the needed time of potpourri generation autoreaction of autoreaction material, the thermal compatibility during to autoreaction material and the mixed storage of other materials carries out preliminary screening.Required test specimen amount is only 30mg left and right, test period is about 60-90 minute, adopt metal tube jacking gear can guarantee the safety of experimenter in experimentation, experimental result meets qualitative, quantitative requirement, be suitable as very much the preliminary screening of autoreaction chemical substance thermal compatibility, obtained good technique effect.
Accompanying drawing explanation
Fig. 1 is the test unit structural representation that the method for the invention adopts.
1: configuration switch; 2: thermostat; 3: electrical secondmeter; 4: reset switch; 5: start/stop time switch; 6: power switch; 7: function conversion key; 8: temperature sensor; 9: detonator; 10: Wood's metal is bathed; 11: detonator jacking gear.
Below by embodiment, the invention will be further elaborated, but be not limited only to the present embodiment.
Embodiment
[embodiment 1]
On 5s lag phase bursting point proving installation as shown in Figure 1, two kinds of ratios for the treatment of that mixed storage chemicals is investigated are on demand mixed, take biased sample 30mg, pack detonator with metal shell shell bottom into, use special purpose copper plug with certain taper capsule port jam-pack, guarantee its impermeability.Then the jack of the detonator that sample is housed being put into bath upper metal tressel clamps, and with connecting line, connects copper plug, in case autoreaction occur after copper plug fly out.Switch on power, heating Wood's metal body lotion, when body lotion reaches testing requirements temperature T, put down tressel, capsule is inserted to the centre of alloy body lotion, now timer is subject to induction to start timing, and autoreaction also occurs along with being heated sample, until copper plug on detonator, after being jumped out, stop timing, record this time.With same method, at this temperature, carry out altogether three tests, ask for this group and test averaging time, be potpourri and issue and be conigenous reaction time τ in this temperature.At other temperature, adopt equally the method to draw the corresponding autoreaction time.According to test result, to temperature spot T and average autoreaction time τ, carry out according to the following formula statistical computation:
Conversion can obtain:
Bring thus the corresponding autoreaction time τ of each temperature spot T into, can by simple regression method obtain lnc and
thereby draw out respective function relation curve.
This potpourri is compared with temperature T-autoreaction time τ curve of pure autoreaction material, and it is larger that straight slope differs, and mixed storage is larger to stability influence, and follow-up compatibility test is played to preliminary screening and directive function.
Claims (5)
1. a method of testing for autoreaction potpourri thermal compatibility, the Wood's metal of usining is bathed as temperature control medium, and by under different temperatures T, containing autoreaction potpourri generation autoreaction, needed time τ sets up
funtcional relationship, return out reaction activity E and the constant C relevant with sample composition containing autoreaction potpourri, draw respective function curve, this autoreaction potpourri is compared with temperature T and the autoreaction time τ curve of single pure autoreaction material, temperature-sensitive sensitivity to this autoreaction potpourri is carried out qualitative and quantitative analysis, thereby draws each substances compatible sex determination result in this potpourri.
2. the method for testing of autoreaction potpourri thermal compatibility according to claim 1, is characterized in that described test is the test of 5s lag phase bursting point.
3. the method for testing of autoreaction potpourri thermal compatibility according to claim 1, it is characterized in that described blend sample is loaded into described Can bottom, and there is special-purpose copper plug Can port jam-pack, guarantee its impermeability, and connect copper plug with connecting line, in case rear copper plug occurs autoreaction, fly out.
4. the method for testing of autoreaction potpourri thermal compatibility according to claim 1, it is characterized in that described Wood's metal body lotion reaches after testing requirements temperature T, Can is inserted in alloy body lotion, timer is subject to induction to start timing, also along with being heated, there is autoreaction in sample, until copper plug on metal tube, after being jumped out, stop timing, record this time.
5. the method for testing of autoreaction potpourri thermal compatibility according to claim 1, is characterized in that carrying out at least three group parallel experiments under described each temperature of reaction T, obtains at least three autoreaction time τ, then asks for average.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103969289A (en) * | 2014-04-11 | 2014-08-06 | 中国石油化工股份有限公司 | Method for testing compatibility of chemical through microcalorimetry |
| CN104007228A (en) * | 2014-04-11 | 2014-08-27 | 中国石油化工股份有限公司 | Method for determining influences of impurities on thermal stability of solid self-reactive substance |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103969289A (en) * | 2014-04-11 | 2014-08-06 | 中国石油化工股份有限公司 | Method for testing compatibility of chemical through microcalorimetry |
| CN104007228A (en) * | 2014-04-11 | 2014-08-27 | 中国石油化工股份有限公司 | Method for determining influences of impurities on thermal stability of solid self-reactive substance |
| CN104007228B (en) * | 2014-04-11 | 2016-03-23 | 中国石油化工股份有限公司 | Judge that impurity is to the thermally-stabilised sex method of solid kind self reactive substances |
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