CN104422623A - Quantitative analysis method for effect of bonding agent in solid propellant - Google Patents
Quantitative analysis method for effect of bonding agent in solid propellant Download PDFInfo
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- CN104422623A CN104422623A CN201310401386.2A CN201310401386A CN104422623A CN 104422623 A CN104422623 A CN 104422623A CN 201310401386 A CN201310401386 A CN 201310401386A CN 104422623 A CN104422623 A CN 104422623A
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Abstract
The invention relates to a quantitative analysis method for an effect of a bonding agent in a solid propellant. The quantitative analysis method is used for evaluating a mechanical property of a composite solid propellant. The method comprises the steps of a sample preparation step, a condition selection step, a detection implementation step and a data analysis step, wherein in the condition selection step, a high-grade expansive rheometer is used as a detection instrument, a parallel-plate measurement system is used as a detection way, a set frequency is set, so that a sinusoidal strain is applied in a given range in a logarithm mode, and a dynamic strain scanning curve of the propellant is used as a detection object; in the data analysis step, the variation situation of modulus in a strain scanning curve is observed, and a strain rate of a modulus curve is analyzed to form a criterion; dynamic strain scanning analysis is carried out on a detected sample by utilizing the top-grade rheometer and the parallel-plate measurement system, a curve with an elasticity modulus and a viscosity modulus varied along with the strain scanning is acquired, and the effect of the bonding agent in the propellant is judged by utilizing the strain rate corresponding to a cross point of the modulus curves. The method has advantages of safety in operation, expense conservation, short detection time and high test efficiency.
Description
Technical field
The present invention relates to the quantitative analysis method of bonding agent action effect in a kind of composite solidpropellant mechanical property evaluation technology, particularly a kind of solid propellant.
Background technology
Bonding agent in composite solidpropellant is a kind of function additive, and its effect is used to the adhesive effect and the interface performance that improve solid packing and adhesive interface.Bonding agent is played a role by the chemical reaction participated in propellant, because component in composite solidpropellant is various, reaction complicated, so just brings certain difficulty to the action effect evaluating bonding agent.
In prior art, be used for evaluating solid packing and the adhesive effect of adhesive interface and the test method of interface performance more, as surface tension test, scanning electron microscope observation, electron spectroscopy analysis etc., the defect of these methods is: sample making course is complicated, testing conditions is harsh, do not have quantitative data, only do qualitative analysis.
Chinese periodical " solid-rocket technology " first phase in 1997 reports document and " characterizes the action effect of composite propellant coupling agent by dynamic-analysis method ", this document propose a kind of dynamic mechanical analysis method DMA, characterize by setting up transition phase model and introducing the action effect that factors A evaluates bonding agent, realize the quantitatively characterizing of bonding agent action effect.Although this method has theoretical depth, lack application example.
Chinese periodical " solid-rocket technology " fourth phase in 2000 reports document " in evaluating combined solid propellant the interactional new method of Filler/Binder ", this document propose a kind of K value that can characterize Filler/Binder effect, and pass judgment on the action effect of bonding agent with K value quantitatively.This method utilizes the action effect of unilateral stretching data judgement bonding agent, can not be used for the screening of novel key mixture.
Summary of the invention
The object of the invention is the quantitative analysis method that bonding agent action effect in a kind of solid propellant will be provided, it can be applicable to the exploitation screening evaluating the action effect of bonding agent and novel key mixture effectively, reliably the action effect of bonding agent in quantitative evaluation solid propellant.
Technical scheme of the present invention is: the quantitative analysis method designing bonding agent action effect in a kind of solid propellant, comprises the following steps: sample preparation, and condition is chosen, and detects and implements, data analysis; The stage is chosen in condition, detecting instrument adopts level expansion flow graph, detection mode is parallel plate measuring system, frequency range is 3.14rad/s to 12.56rad/s, sinusoidal strain sweep limit is 0.002% to 100%, scan pattern is logarithmic form, and detected object is the dynamic strain scanning curve that bonding agent and composite solidpropellant formula are subject to sample product; At data analysis phase, observe the situation of change of modulus in strain sweep curve, analyze the rate of strain of modulus curve, judge the action effect of bonding agent.Namely according to strain sweep curve, more resilient modulus G ' and viscous modulus G " intersections of complex curve G '=G " corresponding to rate of strain, rate of strain is larger, and bonding agent action effect is better.
Advantageous Effects of the present invention is: have employed level expansion flow graph and parallel plate measuring system owing to choosing the stage in condition, thus simple, the testing process science of detection method.Simultaneously because detected object is that bonding agent and composite solidpropellant fill a prescriptions the dynamic strain scanning curve of sample, thus require simply by the preparation inspecting sample, the minimizing of sample materials, be subject to examine time shorten.In addition owing to have employed analytic curve characteristic at data analysis phase, compare rate of strain and pass judgment on the mode of bonding agent effect, thus data reliable, quantitatively accurately, can coincide with the data of demonstration test.The present invention also has handling safety, expense is saved, detection time is short and test efficiency is high advantage.
Accompanying drawing explanation
Fig. 1 is the composite solidpropellant blank formula dynamic strain scanning curve figure not adding bonding agent.
Fig. 2 is the composite solidpropellant setting formula dynamic strain scanning curve figure having added bonding agent.
In figure, horizontal ordinate represents rate of strain γ, and unit is %; Ordinate represents modulus G, and unit is Pa; Wherein G ' is elastic modulus, G " be viscous modulus.
Embodiment
The present invention is further described to divide four groups below in conjunction with embodiment.
First group, bonding agent MAPO(tri-(-2 methylaziridine-1) phosphine oxide in HTPB propellant formula) action effect quantitative test.
Step one, sample preparation: mixed by HTPB propellant recipe ingredient, makes the blank sample (specimen finish is Ф 8 ~ 50mm, and thickness is 1.5 ~ 2.5mm) of disc-shaped after solidification; Bonding agent MAPO is mixed with HTPB propellant recipe ingredient, after solidification, makes identical sample.
Step 2, condition is chosen: choose the stage in condition, detecting instrument adopts level expansion flow graph, detection mode is parallel plate measuring system, in the frequency range of 3.14rad/s to 12.56rad/s, the detection frequency of selection is 5.00rad/s to 10.00rad/s, and sinusoidal strain sweep limit is 0.002% to 100%, scan pattern is logarithmic form, and detected object is the dynamic strain scanning curve of blank sample and the HTPB propellant adding bonding agent MAPO formula sample.
Step 3, detects and implements: the sinusoidal strain applying above-mentioned scope with constant frequency, carries out dynamic strain scanning analysis, obtain the strain sweep curve of sample to the sample of preparation.
Step 4, data analysis: the situation of change of observing modulus in strain sweep curve, analyzes the rate of strain of modulus curve, judges the action effect of bonding agent.According to strain sweep curve, more resilient modulus G ' and viscous modulus G " intersections of complex curve G '=G " corresponding to rate of strain, rate of strain is larger, and bonding agent action effect is better.
The strain sweep curve of said sample presents the Changing Pattern similar to accompanying drawing.Increase with rate of strain, elastic modulus, viscous modulus reduce gradually, when intersection point (G '=G ") appears in elastic modulus curve and viscous modulus curve, write down the rate of strain of now correspondence.To the HTPB propellant blank formula not adding bonding agent MAPO, G '=G " time, rate of strain A%=1.2%; To the propellant formulation adding bonding agent MAPO, G '=G " time, rate of strain B%=8.3%, is greater than A%.Visible, bonding agent MAPO has good bonding action to this HTPB propellant formula.Now tested by the action effect of one directional tensile test para-linkage agent MAPO.
Table 1 is blank formula and the HTPB propellant formula ambient temperature mechanical properties data adding bonding agent MAPO.In table, G ' is elastic modulus, G " be viscous modulus, σ
mfor the maximum tensile strength, unit is MPa, ε
mfor maximum elongation rate, unit is %.Table 1 is visible, and after adding bonding agent MAPO, propellant room temperature tensile strength and length growth rate all increase substantially, and therefore bonding agent MAPO has good bonding action to this HTPB propellant formula, matches with rate of strain data.
Table 1 is blank formula and the HTPB propellant formula ambient temperature mechanical properties data adding bonding agent MAPO
Second group, phenyl-diformyl (2-methylaziridine) between bonding agent JH-01(in highly filled HTPB propellant formula), JH-02(1,3,5-benzene three formyl (2-ethylaziridine)) action effect quantitative test.
Step one, sample preparation: mixed by highly filled HTPB propellant recipe ingredient, after reaching semi-cured state, makes the blank sample (specimen finish is Ф 8 ~ 50mm, and thickness is 1.5 ~ 2.5mm) of disc-shaped; Respectively bonding agent JH-01, JH-02 are mixed with this HTPB propellant recipe ingredient, after reaching semi-cured state, make identical sample.
Step 2, condition is chosen: choose the stage in condition, detecting instrument adopts level expansion flow graph, detection mode is parallel plate measuring system, in the frequency range of 3.14rad/s to 12.56rad/s, the detection frequency of selection is 5.00rad/s to 10.00rad/s, and sinusoidal strain sweep limit is 0.002% to 100%, scan pattern is logarithmic form, and detected object is the dynamic strain scanning curve of blank sample and the highly filled HTPB propellant formula sample adding bonding agent JH-01, JH-02.
Step 3, detects and implements: the sinusoidal strain applying above-mentioned scope with constant frequency, carries out dynamic strain scanning analysis, obtain the strain sweep curve of sample to the sample of preparation.
Step 4, data analysis: the situation of change of observing modulus in strain sweep curve, analyzes the rate of strain of modulus curve, judges the action effect of bonding agent.According to strain sweep curve, more resilient modulus G ' and viscous modulus G " intersections of complex curve G '=G " corresponding to rate of strain, rate of strain is larger, and bonding agent action effect is better.
The strain sweep curve of said sample presents the Changing Pattern similar to accompanying drawing.Increase with rate of strain, elastic modulus, viscous modulus reduce gradually, when intersection point (G '=G ") appears in elastic modulus curve and viscous modulus curve, write down the rate of strain of now correspondence.To the blank formula not adding bonding agent, G '=G " time, rate of strain A%=2.0%; To the propellant formulation adding bonding agent JH-01, G '=G " time, rate of strain B1%=8.0%, is greater than A%; To the propellant formulation adding bonding agent JH-02, G '=G " time, rate of strain B2%=9.5%, is greater than A%, is also greater than B1%.Illustrate that bonding agent JH-01, JH-02 have good bonding action to this HTPB propellant formula system, and the bonding effect of bonding agent JH-02 is slightly better than bonding agent JH-01.
Below by one directional tensile test, two groups of bonding agent action effects are tested.Table 2 is blank formula and the highly filled HTPB propellant formula ambient temperature mechanical properties data adding bonding agent.In table, G ' is elastic modulus, G " be viscous modulus, σ
mfor the maximum tensile strength, unit is MPa, ε
mfor maximum elongation rate, unit is %.Table 2 is visible, adds bonding agent JH-01, when length growth rate is suitable, can improve the tensile strength of propellant; Add bonding agent JH-02, when tensile strength is suitable, the length growth rate of propellant can be increased substantially.Visible, add the mechanical property that bonding agent JH-01, JH-02 can improve highly filled HTPB propellant, wherein the bonding effect of bonding agent JH-02 is more excellent.
Table 2 is blank formula and the highly filled HTPB propellant ambient temperature mechanical properties data adding bonding agent
3rd group, novel key mixture JA-01(fatty acid diethanolamine borate in glycidyl azide polymer propellant formulation), JA-02(triethanolamine borate ester), JA-03(boric acid amido triethyl) action effect analysis.
Step one, sample preparation: glycidyl azide polymer propellant formulation component mixed, makes the blank sample (specimen finish is Ф 8 ~ 50mm, and thickness is 1.5 ~ 2.5mm) of disc-shaped after solidification; Respectively bonding agent JA-01, JA-02, JA-03 are mixed with glycidyl azide polymer propellant formulation component, after solidification, make identical sample.
Step 2, condition is chosen: choose the stage in condition, detecting instrument adopts level expansion flow graph, detection mode is parallel plate measuring system, in the frequency range of 3.14rad/s to 12.56rad/s, the detection frequency selected is 5.00rad/s to 10.00rad/s, sinusoidal strain sweep limit is 0.002% to 100%, scan pattern is logarithmic form, and detected object is the dynamic strain scanning curve of blank sample and the glycidyl azide polymer propellant formulation sample adding novel key mixture JA-01, JA-02, JA-03.
Step 3, detects and implements: the sinusoidal strain applying above-mentioned scope with constant frequency, carries out dynamic strain scanning analysis, obtain the strain sweep curve of sample to the sample of preparation.
Step 4, data analysis: the situation of change of observing modulus in strain sweep curve, analyzes the rate of strain of modulus curve, judges the action effect of bonding agent.According to strain sweep curve, more resilient modulus G ' and viscous modulus G " intersections of complex curve G '=G " corresponding to rate of strain, rate of strain is larger, and bonding agent action effect is better.
The strain sweep curve of said sample presents the Changing Pattern similar to accompanying drawing.Increase with rate of strain, elastic modulus, viscous modulus reduce gradually, when intersection point (G '=G ") appears in elastic modulus curve and viscous modulus curve, write down the rate of strain of now correspondence.To the blank formula not adding bonding agent, G '=G " time, rate of strain A%=3.8%; To the propellant formulation adding bonding agent JA-01, G '=G " time, rate of strain B1%=2.9%, is less than A%; To the propellant formulation adding bonding agent JA-02, G '=G " time, rate of strain B2%=7.5%, is greater than A%.To the propellant formulation adding bonding agent JA-03, G '=G " time, rate of strain B3%=3.6%, is less than A%.Explanation only has bonding agent JA-02 to have good bonding action to this glycidyl azide polymer propellant formulation system.
Action effect below by the agent of one directional tensile test para-linkage JA-01, JA-02, JA-03 is tested.Table 3 is blank formula and the glycidyl azide polymer propellant formulation ambient temperature mechanical properties data adding bonding agent.In table, G ' is elastic modulus, G " be viscous modulus, σ
mfor the maximum tensile strength, unit is MPa, ε
mfor maximum elongation rate, unit is %.Table 3 is visible, adds bonding agent JA-01, JA-03, and this glycidyl azide polymer propellant ambient temperature mechanical properties does not improve; And add bonding agent JA-02, can when tensile strength be suitable, improve propellant length growth rate, kiss very much with rate of strain determining method and.Therefore, the screening of propellant novel key mixture can be carried out by the rate of strain size of dynamic strain scanning curve.
Table 3 is blank formula and the glycidyl azide polymer propellant ambient temperature mechanical properties data adding bonding agent
4th group, HTPB propellant formula in the tartaric reactant of bonding agent JMT(2mol MAPO and 1mol) optimum amount analysis.
Step one, sample preparation: mixed by HTPB propellant recipe ingredient, makes the blank sample (specimen finish is Ф 8 ~ 50mm, and thickness is 1.5 ~ 2.5mm) of disc-shaped after solidification; Respectively by bonding agent JMT with 0.03%, 0.06%, 0.09% additional proportion mix with HTPB propellant recipe ingredient, make identical sample after solidification.
Step 2, condition is chosen: choose the stage in condition, detecting instrument adopts level expansion flow graph, detection mode is parallel plate measuring system, in the frequency range of 3.14rad/s to 12.56rad/s, the detection frequency of selection is 5.00rad/s to 10.00rad/s, and sinusoidal strain sweep limit is 0.002% to 100%, scan pattern is logarithmic form, and detected object is the dynamic strain scanning curve of blank sample and the HTPB propellant adding bonding agent JMT formula sample.
Step 3, detects and implements: the sinusoidal strain applying above-mentioned scope with constant frequency, carries out dynamic strain scanning analysis, obtain the strain sweep curve of sample to the sample of preparation.
Step 4, data analysis: the situation of change of observing modulus in strain sweep curve, analyzes the rate of strain of modulus curve, judges the action effect of bonding agent.According to strain sweep curve, more resilient modulus G ' and viscous modulus G " intersections of complex curve G '=G " corresponding to rate of strain, rate of strain is larger, and bonding agent action effect is better.
The strain sweep curve of said sample presents the Changing Pattern similar to accompanying drawing.Increase with rate of strain, elastic modulus, viscous modulus reduce gradually, when intersection point (G '=G ") appears in elastic modulus curve and viscous modulus curve, write down the rate of strain of now correspondence.To the blank formula not adding bonding agent, G '=G " time, rate of strain A%=4.0%; The propellant formulation of para-linkage agent JMT content 0.03%, G '=G " time, rate of strain B1%=6.0%; The propellant formulation of para-linkage agent JMT content 0.06%, G '=G " time, rate of strain B2%=7.5%; The propellant formulation of para-linkage agent JMT content 0.09%, G '=G " time, rate of strain B3%=7.4%.Visible, increase with bonding agent JMT content, strain takes the lead in increasing rear reduction, and when bonding agent JMT content is 0.06%, rate of strain reaches maximum, and therefore the optimum amount of bonding agent JMT in this HTPB propellant should be 0.06%.
Test below by one directional tensile test para-linkage agent content effect.Table 4 is blank formula and the HTPB propellant formula ambient temperature mechanical properties data adding bonding agent JMT.In table, G ' is elastic modulus, G " be viscous modulus, σ
mfor the maximum tensile strength, unit is MPa, ε
mfor maximum elongation rate, unit is %.Table 4 is visible, increase with bonding agent JMT content, propellant room temperature tensile strength and length growth rate increase, when bonding agent JMT addition is 0.06%, HTPB propellant ambient temperature mechanical properties reaches optimum value, when bonding agent JMT content reaches 0.09%, HTPB propellant mechanical property slightly declines, with rate of strain data kiss very much and.Visible, can be selected bonding agent optimum amount in HTPB propellant by dynamic strain scanning, realize the quantitatively characterizing of bonding agent action effect.
Table 4 is blank formula and the HTPB propellant formula ambient temperature mechanical properties data adding bonding agent JMT
Claims (2)
1. the quantitative analysis method of bonding agent action effect in a solid propellant, comprise following four steps: sample preparation, condition is chosen, detect and implement, data analysis, it is characterized in that: choose the stage in condition, detecting instrument adopts level expansion flow graph, detection mode is parallel plate measuring system, frequency range is 3.14rad/s to 12.56rad/s, sinusoidal strain sweep limit is 0.002% to 100%, and scan pattern is logarithmic form, and detected object is that bonding agent and composite solidpropellant are filled a prescription the dynamic strain scanning curve of sample; At data analysis phase, observe the situation of change of modulus in strain sweep curve, analyze the rate of strain of modulus curve, judge the action effect of bonding agent.
2. the quantitative analysis method of bonding agent action effect in the solid propellant according to right 1, it is characterized in that: at data analysis phase, according to strain sweep curve, more resilient modulus G ' and viscous modulus G " intersections of complex curve G '=G " corresponding to rate of strain, rate of strain is larger, and bonding agent action effect is better.
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Cited By (4)
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| KR20180023204A (en) * | 2016-08-25 | 2018-03-07 | 주식회사 엘지화학 | comparison evaluation method for dispersion of sample |
| CN108763792A (en) * | 2017-12-07 | 2018-11-06 | 上海航天化工应用研究所 | The theoretical calculation method of bonding agent optimum amount in a kind of composite solidpropellant |
| CN110501478A (en) * | 2019-09-24 | 2019-11-26 | 中策橡胶集团有限公司 | A kind of detection method of natural rubber molecular weight |
| CN112457142A (en) * | 2020-10-26 | 2021-03-09 | 南京理工大学 | Method for determining bonding agent adsorption time in 3D printing propellant mixing process |
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| US4000023A (en) * | 1968-12-09 | 1976-12-28 | Aerojet-General Corporation | Bonding agents for polyurethane |
| CN103217335A (en) * | 2012-10-12 | 2013-07-24 | 湖北航天化学技术研究所 | Method for rapidly detecting main curve of tensile strength for unidirectional stretching of solid propellant |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20180023204A (en) * | 2016-08-25 | 2018-03-07 | 주식회사 엘지화학 | comparison evaluation method for dispersion of sample |
| KR102101159B1 (en) | 2016-08-25 | 2020-04-16 | 주식회사 엘지화학 | comparison evaluation method for dispersion of sample |
| CN108763792A (en) * | 2017-12-07 | 2018-11-06 | 上海航天化工应用研究所 | The theoretical calculation method of bonding agent optimum amount in a kind of composite solidpropellant |
| CN108763792B (en) * | 2017-12-07 | 2022-08-12 | 上海航天化工应用研究所 | Theoretical calculation method for optimal dosage of bonding agent in composite solid propellant |
| CN110501478A (en) * | 2019-09-24 | 2019-11-26 | 中策橡胶集团有限公司 | A kind of detection method of natural rubber molecular weight |
| CN112457142A (en) * | 2020-10-26 | 2021-03-09 | 南京理工大学 | Method for determining bonding agent adsorption time in 3D printing propellant mixing process |
| CN112457142B (en) * | 2020-10-26 | 2023-05-12 | 南京理工大学 | Method for determining bonding agent adsorption time in 3D printing propellant mixing process |
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