CN103604825B - The method of testing of self-reactive mixture thermal compatibility - Google Patents

Abstract

The present invention relates to the method for testing of a kind of self-reactive mixture thermal compatibility, mainly solve test period length in prior art, problem that dangerous sample size high, required is big. The present invention, by adopting the method for testing of a kind of self-reactive mixture thermal compatibility, bathes as temperature control medium using Wood's metal, by, under different temperatures T, setting up containing the time τ required for self-reactive mixture generation autoreactionFunctional relationship, return out the reaction activity E containing self-reactive mixture and the constant C relevant with sample composition, draw respective function curve, by this self-reactive mixture compared with the temperature T of single pure self-reactive material and autoreaction time τ curve, the heat sensitivity of this self-reactive mixture is carried out qualitative and quantitative analysis, thus showing that in this mixture, the technical scheme of each materials compatibility result of determination solves the problems referred to above preferably, can be used in the screening test of self-reactive mixture thermal compatibility.

Description

The method of testing of self-reactive mixture thermal compatibility

Technical field

The present invention relates to the method for testing of a kind of self-reactive mixture thermal compatibility.

Technical background

, autoreaction can be there is because multiple different extraneous factor (such as hot, optical, electrical, spark etc.) causes, under household condition during independent accumulating, generally not show autoreaction danger in self-reactive chemical substance. And when occurring when such material and some organic peroxide matter, oxidizing substance, induced material etc. mixed storage or transportation come in contact; usually can reduce the autoreaction condition of self-reactive material, increase the dangerous sensitivity of its performance autoreaction and probability. So the blast joined rule and cause 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 self-reactive chemical substance thermal compatibility; the world not clear and definite at present or unification of the motherland standard; would generally utilize gram southern assay device or reaction calorimeter that the mixed storage situation of material is estimated, but this both of which also exists respective drawback.

Gram south test need sample size big, if the self-reactive material running into sensitivity has the danger of steel pipe explosion, there is potential safety hazard, and with propane burning for thermal source in experimentation, heating-up temperature cannot be controlled, cause that the assessment of sample heat sensitivity can only be rested on qualitative level by it; Although reaction calorimeter can provide reaction heat data accurately for self-reactive chemicals thermal compatibility situation, but the method test period is long, and instrument and equipment is expensive, and experimental condition is harsh, is unfavorable for promotion and application.

CN201210137946 discloses a kind of solid and insulating oil compatibility test device, and it includes oil tank and oil filler point thereof, it is characterised in that also include: below centrally through the tubular configured joint funnel that connect threaded with flowline on described oil tank;It is located at described oil tank one middle side part, and communicates with oil tank inner chamber, for arranging sample pipe and the gland thereof of test specimen; In described funnel tube straight coupling, it is provided with the upper end conical plug that to be cylindricality lower end be; It is located at described oil tank side lower curtate the petroleum pipeline communicated with oil tank inner chamber. This apparatus structure is simple, and easy to use, low cost and accuracy are high, putting in baking box equipped with test specimen and the test device filling oil, after being heated to time and the temperature of setting, oil taking-up oil colours spectrometry is measured the compatibility of solid and insulating oil.

For the self-reactive material of difference composition, the self-reacting sensitivity of thermic is had nothing in common with each other, thus when self-reactive material and other different materials, different proportion can be mixed storage, the heat sensitivity of performance mixes the measurement index of the storage compatibility as these two kinds of materials. By under different temperatures, the time required for mixture generation autoreaction containing self-reactive material sets up functional relationship, and draw respective function curve, the heat sensitivity of this mixture can be carried out quantitative analysis, these data are compared with heat sensitivity data before mixing, thus drawing each materials compatibility result of determination in this mixture. Situation according to existing literature search and market survey, domestic not yet have relevant mechanism to carry out the research of self-reactive chemical substance thermal compatibility in the method.

Summary of the invention

The problem that the technical problem to be solved is test period length in prior art, dangerous sample size high, required is big, it is provided that the method for testing of a kind of new self-reactive mixture thermal compatibility. The method is for, in the test of reactive mixture thermal compatibility, having the advantage that test period sample size low, required short, dangerous is little.

For solving above-mentioned technical problem, the technical solution used in the present invention is as follows: the method for testing of a kind of self-reactive mixture thermal compatibility, bathe as temperature control medium using Wood's metal, by, under different temperatures T, setting up containing the time τ required for self-reactive mixture generation autoreactionFunctional relationship, return out the reaction activity E containing self-reactive mixture and the constant C relevant with sample composition, draw respective function curve, by this self-reactive mixture compared with the temperature T of single pure self-reactive material and autoreaction time τ curve, the heat sensitivity of this self-reactive mixture is carried out qualitative and quantitative analysis, thus drawing each materials compatibility result of determination in this mixture.

In technique scheme, it is preferable that described test is the test of 5s lag phase bursting point.

In technique scheme, it is preferable that described blend sample is loaded into bottom described Can, and there is special copper plug tight for Can port plug, it is ensured that its air-tightness, and connect copper plug with connecting line, in case copper plug flies out after autoreaction occurs.

In technique scheme, it is preferable that after described Wood's metal body lotion reaches test requirements document temperature T, Can is inserted in alloy body lotion, and timer is started timing by sensing, and autoreaction occurs sample also with being heated, after copper plug on metal tube is jumped out, terminate timing, record this time.

In technique scheme, it is preferable that carry out at least three group parallel tests under each reaction temperature T described, it is thus achieved that at least three autoreaction time τ, then ask for average.

Self-reactive mixture for difference composition, the single pure self-reacting sensitivity of self-reactive material is had nothing in common with each other, thus when self-reactive material and other different materials, different proportion can be mixed storage, the heat sensitivity of performance mixes the measurement index of the storage compatibility as these two kinds of materials.By under different temperatures, the time required for mixture generation autoreaction containing self-reactive material sets up functional relationship, and draw respective function curve, the heat sensitivity of this mixture can be carried out quantitative analysis, these data are compared with heat sensitivity data before mixing, thus drawing each materials compatibility result of determination in this mixture. After recording reaction temperature T and average autoreaction time τ, carry out statistical computation according to the following formula:

$\mathrm{\τ}=C\·e^{\frac{E}{\mathrm{RT}}}$

In formula: the E-mixture reaction activation energy containing self-reactive material, J/mol;

R-gas constant, J/ (mol.K);

The constant that C-is relevant with sample composition;

τ-average autoreaction time, min;

T-reaction temperature, K.

Conversion can obtain:

Thus bring each temperature spot T correspondence autoreaction time τ into, can by simple regression method obtain lnC andThus drawing out respective function relation curve. By this mixture compared with the temperature T-autoreaction time τ curve of pure self-reactive material, straight slope difference is more big, then mixed storage is more big to stability influence, and follow-up compatibility test plays Preliminary screening and directive function.

The present invention adopts Wood's metal bath as temperature control medium, and by studying the time required for the mixture generation autoreaction at different temperatures, containing self-reactive material, thermal compatibility when self-reactive material and other materials are mixed storage carries out Preliminary screening. Required test specimen amount is only about 30mg, test period is about 60-90 minute, metal tube lowering or hoisting gear is adopted to may insure that the safety of experimenter in experimentation, experimental result meets qualitative, quantitative requirement, it is highly suitable as the Preliminary screening of self-reactive chemical substance thermal compatibility, achieves good technique effect.

Accompanying drawing explanation

Fig. 1 is the assay device 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: on and off switch; 7: function conversion key; 8: temperature sensor; 9: detonator; 10: Wood's metal is bathed; 11: detonator lowering or hoisting gear.

The invention will be further elaborated by the examples below, but is not limited only to the present embodiment.

Detailed description of the invention

[embodiment 1]

Test on device at 5s lag phase bursting point as shown in Figure 1, two kinds are treated the ratio mix homogeneously that mixed storage chemicals is investigated on demand, weighs biased sample 30mg, load bottom detonator with metal shell shell, with the special purpose copper plug with certain taper tight for capsule port plug, it is ensured that its air-tightness. Then the detonator equipped with sample is put into clamping in the jack of bath upper metal adjustable shelf, connect copper plug with connecting line, in case copper plug flies out after autoreaction occurs. Switch on power, heating Wood's metal body lotion, when body lotion reaches test requirements document temperature T, put down adjustable shelf, capsule being inserted the centre of alloy body lotion, now timer is started timing by sensing, and autoreaction occurs sample also with being heated, after copper plug on detonator is jumped out, terminate timing, record this time. Carry out three tests in the same way at such a temperature altogether, ask for this group and test average time, be mixture and autoreaction time τ occurs at such a temperature. The method is adopted to draw the corresponding autoreaction time equally at other temperature. According to test result to temperature spot T and average autoreaction time τ, carry out statistical computation according to the following formula:

$\mathrm{\τ}=C\·e^{\frac{E}{\mathrm{RT}}}$

Conversion can obtain:

Thus bring each temperature spot T correspondence autoreaction time τ into, can by simple regression method obtain lnC andThus drawing out respective function relation curve.

By this mixture compared with the temperature T-autoreaction time τ curve of pure self-reactive material, straight slope difference is more big, then mixed storage is more big to stability influence, and follow-up compatibility test plays Preliminary screening and directive function.

Claims (5)

1. a method of testing for self-reactive mixture thermal compatibility, bathes as temperature control medium using Wood's metal, by, under different temperatures T, setting up containing the time τ required for self-reactive mixture generation autoreactionFunctional relationship, return out the reaction activity E containing self-reactive mixture and the constant C relevant with sample composition, draw respective function curve, by this self-reactive mixture compared with the temperature T of single pure self-reactive material and autoreaction time τ curve, the heat sensitivity of this self-reactive mixture is carried out qualitative and quantitative analysis, thus drawing each materials compatibility result of determination in this mixture.

2. the method for testing of self-reactive mixture thermal compatibility according to claim 1, it is characterised in that described test is the test of 5s lag phase bursting point.

3. the method for testing of self-reactive mixture thermal compatibility according to claim 1, it is characterized in that described blend sample is loaded into bottom Can, and have special copper plug tight for Can port plug, ensure its air-tightness, and connect copper plug with connecting line, in case after autoreaction occurs, copper plug flies out.

4. the method for testing of self-reactive mixture thermal compatibility according to claim 1, after it is characterized in that described Wood's metal body lotion reaches test requirements document temperature T, Can is inserted in alloy body lotion, timer is started timing by sensing, autoreaction is there is in sample also with being heated, after copper plug on metal tube is jumped out, terminate timing, record this time.

5. the method for testing of self-reactive mixture thermal compatibility according to claim 1, it is characterised in that carry out at least three group parallel tests under each reaction temperature T described, it is thus achieved that at least three autoreaction time τ, then ask for average.