CN115078342A - Gas-sensitive film for monitoring chemical aging degree of composite solid propellant and preparation method thereof - Google Patents
Gas-sensitive film for monitoring chemical aging degree of composite solid propellant and preparation method thereof Download PDFInfo
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- CN115078342A CN115078342A CN202110263869.5A CN202110263869A CN115078342A CN 115078342 A CN115078342 A CN 115078342A CN 202110263869 A CN202110263869 A CN 202110263869A CN 115078342 A CN115078342 A CN 115078342A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
- G01N21/783—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour for analysing gases
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N2021/775—Indicator and selective membrane
Abstract
The invention discloses a preparation method of a gas-sensitive film for monitoring chemical aging degree of a composite solid propellant. The method takes bromothymol blue-methyl red indicator as CO x Monitoring indicator, bromcresol purple indicator is NO x Monitoring the indicator for CO x Monitoring indicator liquid and NO x The monitoring indicator liquid is respectively coated on the polylactic acid film to prepare the gas-sensitive film. According to the invention, by utilizing the characteristics of sensitivity correspondence and color change of different indicators to specific gases, the prepared gas-sensitive film can simultaneously monitor CO released by the propellant in the chemical aging process x ，NO x The gas-sensitive film is small, exquisite and light, can be transported along with the propellant and can experience the same environment, so that the detection result is real and reliable.
Description
Technical Field
The invention relates to the technical field of chemistry, in particular to a gas-sensitive film for monitoring chemical aging degree of a composite solid propellant and a preparation method thereof.
Background
The aging of propellants is divided into physical damage and chemical aging. Compared with the means for monitoring physical damage, the means for monitoring chemical aging of the propellant is not accurate and rapid at present. And the chemical aging of the propellant is usually related to the change of the internal molecular structure of the propellant, so the chemical aging is usually irreversible, so the monitoring of the chemical aging degree of the propellant is very critical. Document 1 uses a gas-selective electrode to monitor the composition and concentration of gas generated by propellant aging for the purpose of characterizing the degree of propellant aging (Jingsong Li, Hao Deng, Juan Sun, et al 2 O andH 2 O detection using a single square rubber sensor based on horizontal-dispersive techniques. Sensors and Actuators B Chemical,2016,231: 723-. Document 2 discloses a self-developed small-volume negative pressure sample injection system for monitoring the composition of trace gases generated by propellant aging (Yan Du, Shi Gao, Zhenghao Mao, et al 2 sensingsensors fabricated by diffusion membranes depositing on Pt-ZnO film.Sensors&Actuators b.chemical 2017,252 239 @.). both of these methods, while providing relatively accurate monitoring of the chemical degradation of the propellant, are complex and expensive to detect and require destruction of the sealed storage environment of the propellant.
Disclosure of Invention
The invention aims to provide a gas-sensitive film for monitoring the chemical aging degree of a composite solid propellant and a preparation method thereof. The gas-sensitive film reflects CO generated by the propellant in the process of chemical aging through the color change of the indicator on the film x ，NO x And the amount of the gas is equal, so that the purpose of qualitatively detecting the chemical aging degree of the propellant is realized.
The technical scheme for realizing the purpose of the invention is as follows:
the preparation method of the gas-sensitive film for monitoring the chemical aging degree of the composite solid propellant comprises the following steps:
step 1, preparing a gas-sensitive film substrate: crushing polylactic acid (PLA), adding into chloroform, heating to completely dissolve the PLA, standing and cooling to room temperature, pouring the PLA on the surface of a glass mold, and naturally drying until the chloroform is completely volatilized;
step 2, CO x Preparation of monitoring and indicating liquid: adding plasticizer polyethylene glycol-6000 and adhesive methylcellulose into water, heating and stirring until completely dissolved, adding bromothymol blue-methyl red indicator, stirring uniformly, and adjusting pH to 7.10 + -0.05;
step 3, NO x Preparation of monitoring and indicating liquid: adding a plasticizer glycerol into water, uniformly stirring, adding an adhesive hydroxyethyl cellulose, uniformly stirring, naturally cooling to room temperature, adding a bromocresol purple indicator, uniformly stirring, and adjusting the pH value to 4.00 +/-0.05;
step 4, adding CO x Monitoring indicator liquid and NO x And (3) respectively coating the monitoring indicating liquid on different areas of the PLA film prepared in the step (1), and obtaining the gas-sensitive film, wherein the coating thicknesses are consistent.
Preferably, in step 1, the bromothymol blue-methyl red composite indicator is prepared by a volume ratio of 3:2 of bromothymol blue indicator and methyl red indicator.
Preferably, in steps 2 and 3, the heating temperature is 70 ℃.
Preferably, in step 2, the concentration of polyethylene glycol-6000 is 10g/L, and the concentration of methylcellulose is 30 g/L.
Preferably, in step 3, the concentration of glycerol is 50mL/L and the concentration of hydroxyethyl cellulose is 17 g/L.
Preferably, in step 4, to avoid CO x Monitoring indicator liquid and NO x And (3) mixing the monitoring indicating liquids, adopting a star-shaped mold to separate partial areas, adding the bromothymol blue-methyl red indicating liquid, taking out the mold after the indicating liquid is dried, and filling the blank area on the PLA base film with the bromocresol purple indicating liquid.
The invention also provides the gas-sensitive film prepared by the preparation method.
Compared with the prior art, the invention has the following advantages:
the invention utilizes the characteristics of sensitive correspondence and color change of different indicators to specific gases to prepare the propellant capable of being monitored simultaneouslyCO released during chemical ageing x ，NO x A gas. The gas-sensitive film can be used for nondestructively monitoring the chemical aging degree of the propellant and giving visual and reliable feedback, and the chemical aging information of the propellant can be obtained without professional knowledge of detection personnel, so that whether the propellant can be used or not can be judged. The gas-sensitive film is small, exquisite and light, can be transported along with the propellant and can be subjected to the same environment, so that the detection result is real and reliable.
Drawings
FIG. 1 is a schematic prototype of the gas sensitive film of the present invention, the central light yellow star portion being a bromocresol purple indicating film for indicating NO x The green part of the edge is bromothymol blue-methyl red indicating film for indicating CO x 。
FIG. 2 is a flow chart of a process for preparing a gas sensitive film.
Detailed Description
The invention is described in further detail below with reference to the figures and the specific embodiments.
Examples
The invention monitors the generation of CO in the chemical aging decomposition process of the propellant x ，NO x The gases are used for qualitatively characterizing the chemical aging degree of the propellant. The propellant has complex components, but contains elements such as C, H, O, N and the like, so that the propellant generates CO when being aged and decomposed x ，NO x And the like. These gases can be monitored using indicators that specifically detect their presence and concentration. The indicator is compounded together by a certain method and made into a film, and the chemical aging degree of the propellant is represented by the color change of the film.
As shown in fig. 2, the preparation method of the gas-sensitive film for monitoring the chemical aging degree of the composite solid propellant comprises the following steps:
(1) and (3) preparing an indicator: broomthymol blue-methyl red composite indicator selected for CO monitoring x The generated concentration is that bromothymol blue is prepared into 1g/L bromothymol blue ethanol solution, methyl red is prepared into 1g/L methyl red ethanol solution, and two kinds of indicating liquid are prepared into bromoberylPhenol blue: a volume ratio of 3:2 methyl red is configured to mix the indicator; bromocresol violet indicator selected for monitoring NO x The bromcresol purple indicator is prepared into 1g/L bromcresol purple ethanol solution.
(2) Preparation of gas-sensitive film substrate: pulverizing polylactic acid (PLA), adding into chloroform, heating at 30 deg.C for 40min to dissolve completely, standing to room temperature, pouring onto the surface of glass mold, and naturally drying for 1.5 hr until chloroform volatilizes completely.
(3)CO x Preparation of monitoring and indicating liquid: and (3) preserving the heat of 300mL of distilled water in a constant-temperature water bath box at 70 ℃, adding 3g of polyethylene glycol-6000 serving as a plasticizer, adding 9g of methylcellulose serving as an adhesive, immediately taking out, and magnetically stirring uniformly. Adding 1mL of prepared bromothymol blue-methyl red mixed indicator, stirring at high speed to form gel solution, and adjusting pH to 7.10 + -0.05 to obtain CO x The indicator liquid is monitored.
(4)NO x Preparation of monitoring and indicating liquid: putting 200mL of distilled water into a constant-temperature water bath box at 70 ℃ for heat preservation, then adding 10mL of glycerol as a plasticizer, uniformly stirring, then adding 3.4g of hydroxyethyl cellulose as an adhesive, uniformly stirring, naturally cooling to room temperature, adding 16mL of bromocresol purple indicator, stirring to form a uniform hydroxyethyl cellulose gel solution, and adjusting the pH value to 4.00 +/-0.05 to obtain the indicating liquid.
(5) Preparation of the gas-sensitive film: placing a star mold on the PLA base film, and placing CO x The monitoring indicator solution was uniformly applied on the PLA base film at a thickness of 4 mm. Drying the film at 40 ℃ for 12h to obtain a dry film. Taking out the star-shaped mold, and using the prepared NO for the star-shaped blank area on the PLA base film x And (3) completely filling the monitoring and indicating liquid, wherein the coating thickness is still 4mm, drying the monitoring and indicating liquid at 40 ℃ for 12h, taking out the PLA base film from a glass mold after the PLA base film is completely dried, and wrapping the PLA base film by using a food-grade polyethylene film to obtain the double-indication gas-sensitive film. The prototype of the film prepared is shown in FIG. 1.
Claims (7)
1. The preparation method of the gas-sensitive film for monitoring the chemical aging degree of the composite solid propellant is characterized by comprising the following steps of:
step 1, preparing a gas-sensitive film substrate: crushing polylactic acid, adding the crushed polylactic acid into chloroform, heating to completely dissolve the polylactic acid, standing and cooling to room temperature, pouring the polylactic acid on the surface of a glass mold, and naturally drying until the chloroform is completely volatilized;
step 2, CO x Preparation of monitoring and indicating liquid: adding plasticizer polyethylene glycol-6000 and adhesive methylcellulose into water, heating and stirring until completely dissolved, adding bromothymol blue-methyl red indicator, stirring uniformly, and adjusting pH to 7.10 + -0.05;
step 3, NO x Preparation of monitoring indicator liquid: adding a plasticizer glycerol into water, uniformly stirring, adding an adhesive hydroxyethyl cellulose, uniformly stirring, naturally cooling to room temperature, adding a bromocresol purple indicator, uniformly stirring, and adjusting the pH value to 4.00 +/-0.05;
step 4, adding CO x Monitoring indicator liquid and NO x And (3) respectively coating the monitoring indicating liquid on different areas of the PLA film prepared in the step (1), and obtaining the gas-sensitive film, wherein the coating thicknesses are consistent.
2. The preparation method according to claim 1, wherein in step 1, the bromothymol blue-methyl red composite indicator is prepared from a bromothymol blue indicator and a methyl red indicator in a volume ratio of 3: 2.
3. The method according to claim 1, wherein the heating temperature in steps 2 and 3 is 70 ℃.
4. The method according to claim 1, wherein the concentration of polyethylene glycol-6000 is 10g/L and the concentration of methylcellulose is 30g/L in step 2.
5. The method according to claim 1, wherein the concentration of glycerin in step 3 is 50mL/L and the concentration of hydroxyethyl cellulose is 17 g/L.
6. The method of claim 1, wherein in step 4, a star-shaped mold is used to separate partial areas, bromothymol blue-methyl red indicator liquid is added, the mold is taken out after the bromothymol blue-methyl red indicator liquid is dried, and the blank area on the PLA base membrane is filled with bromocresol purple indicator liquid.
7. The gas-sensitive film produced by the production method according to any one of claims 1 to 6.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110263869.5A CN115078342A (en) | 2021-03-11 | 2021-03-11 | Gas-sensitive film for monitoring chemical aging degree of composite solid propellant and preparation method thereof |
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| CN202110263869.5A CN115078342A (en) | 2021-03-11 | 2021-03-11 | Gas-sensitive film for monitoring chemical aging degree of composite solid propellant and preparation method thereof |
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- 2021-03-11 CN CN202110263869.5A patent/CN115078342A/en active Pending
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