CN111289403A - Method for analyzing content of gelling agent in colloidal propellant - Google Patents
Method for analyzing content of gelling agent in colloidal propellant Download PDFInfo
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- CN111289403A CN111289403A CN201811501460.7A CN201811501460A CN111289403A CN 111289403 A CN111289403 A CN 111289403A CN 201811501460 A CN201811501460 A CN 201811501460A CN 111289403 A CN111289403 A CN 111289403A
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- gelling agent
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- organic solvent
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
Abstract
The invention relates to a propellant component content analysis technology, in particular to an analysis method for the content of a gelling agent in a colloidal propellant. The method selects a certain organic solvent to be added into a colloidal propellant sample, and the gelling agent in the colloidal propellant is separated out because the gelling agent is insoluble in the selected organic solvent. Meanwhile, the added organic solvent can also react with all or part of other components except the gelling agent in the colloidal propellant, and other components except the gelling agent in the reaction product and the sample which do not react with the added organic solvent can be dissolved in the added organic solvent, so that the independent separation and determination of the gelling agent can be realized. The method provided by the invention overcomes the defects in the content analysis of the salt-containing colloidal propellant gelling agent in the prior art, and can be applied to the analysis of colloidal propellants with more varieties and more complex compositions.
Description
Technical Field
The invention relates to a propellant component content analysis technology, in particular to an analysis method for the content of a gelling agent in a colloidal propellant.
Background
Colloidal propellants are a new class of propellants developed on the basis of liquid propellants, which can be prepared by adding a small amount of a gelling agent to a conventional liquid propellant to gelatinize the liquid propellant. The colloidal propellant integrates the respective advantages of the liquid propellant and the solid propellant to a certain extent, has the characteristics of high specific flushing of the liquid propellant, adjustable thrust, multiple starting and other service performances, and also has the advantages of the solid propellant in use and maintenance aspects of convenience in storage and transportation, difficulty in volatilization and leakage and the like.
In colloidal propellants, the gelling agent is a key component to achieve gelation of the liquid propellant. In hydrazine/hydroxylamine colloidal propellants, cellulose derivatives, polyvinyl alcohol, polyacrylamide, and other high molecular compounds having good solubility in the corresponding liquid propellant are often used as gelling agents. The content of the gelling agent in the colloidal propellant has important influence on the performances of the colloidal propellant such as rheology, atomization, combustion and the like, so that a corresponding analysis method of the content of the gelling agent in the colloidal propellant is necessary to perfect the quality control of the colloidal propellant.
When the content of the gelling agent in the colloidal propellant prepared from the traditional hydrazine liquid fuel such as anhydrous hydrazine, methyl hydrazine, unsym-dimethylhydrazine and the like is analyzed, the volatile hydrazine substances in the colloidal propellant can be removed by a reduced pressure distillation mode, so that the gelling agent in the colloidal propellant is separated and the content of the gelling agent is weighed and calculated. However, as liquid propellant fuels have been developed and the components contained therein have become more complex, salts of hydrazine, hydrazine derivatives, hydroxylamine, etc. with inorganic acids or small organic acids have been used in liquid propellant fuels to improve the performance of liquid propellant fuels in terms of energy density, specific impulse, low temperature start, etc. In the corresponding colloidal propellants, the above-mentioned salts, because of their non-volatility, cannot be separated from the gelling agent by distillation under reduced pressure.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide an analysis method capable of determining the content of a gelling agent in a colloidal propellant, particularly a salt-containing colloidal propellant.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method of analyzing the gelling agent content of a colloidal propellant, comprising:
the colloidal propellant contains a liquid propellant and the gelling agent, and the liquid propellant contains one or more of hydrazine, hydrazine derivatives with amino groups and hydroxylamine, and/or one or more of nitrate, hydrochloride, sulfate, phosphate, acetate, formate and oxalate of the substances;
adding an organic solvent into the colloidal propellant, wherein the organic solvent contains aldehyde and/or ketone compounds;
the organic solvent may react with all or some of the other components of the colloidal propellant other than the gelling agent, and the reaction product may be soluble in the organic solvent, e.g., components of the colloidal propellant other than the gelling agent that do not react with the organic solvent may be present and may also be soluble in the organic solvent;
the gelling agent in the colloidal propellant is separated out independently because the gelling agent is insoluble in the organic solvent, and the gelling agent is separated and weighed, and the content of the gelling agent in the colloidal propellant is calculated.
The gelling agent is a high-molecular gelling agent.
The high molecular gelling agent is one or more selected from cellulose derivatives, dextran, glucomannan, chitosan, starch, dextrin, guar gum, sesbania gum, carrageenan, xanthan gum, konjac gum, sodium alginate, gelatin, agar, acrylic polymers and polyvinyl alcohol.
The organic solvent of the present invention is preferably acetone.
The method comprises the following steps:
(1) weighing a certain amount of the colloidal propellant;
(2) adding the organic solvent to the colloidal propellant to precipitate the gelling agent;
(3) separating the precipitated gelling agent from the liquid component;
(4) washing the separated gelling agent;
(5) drying the washed gelling agent;
(6) and weighing the dried gelling agent, and calculating the content of the gelling agent in the colloidal propellant.
The dosage of the organic solvent is 1mL-100mL of the organic solvent added into each gram of the colloidal propellant, and preferably 2mL-10mL of the organic solvent added into each gram of the colloidal propellant.
When the organic solvent is added to the colloidal propellant, an amount of water may also be incorporated into the organic solvent at a level that does not interfere with the complete precipitation of the gelling agent.
Before the organic solvent is added to the colloidal propellant, the volatile components in the colloidal propellant can be completely or partially removed, so that the colloidal propellant is concentrated.
The method for analyzing the content of the gelling agent in the colloidal propellant separates out and separates the gelling agent by utilizing the characteristic that the gelling agent is insoluble in a specific organic solvent, and simultaneously makes use of the reaction between the organic solvent and other components in the colloidal propellant to make other components except the gelling agent in a sample be soluble in the added organic solvent, thereby avoiding the influence of the separation of other components along with the gelling agent on the determination of the content of the gelling agent. Compared with the prior art, the method provided by the invention can be applied to the analysis of colloidal propellants with more varieties and more complex compositions, and particularly overcomes the defects of the prior art in the content analysis of the salt-containing colloidal propellant gelling agent.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the following provides a clear and complete description of the technical solutions of the embodiments of the present invention. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the described embodiments of the invention without any inventive step, are within the scope of protection of the invention.
Embodiments of the present invention provide a method for analyzing the gelling agent content of a colloidal propellant. The method is applicable to colloidal propellants comprising a liquid propellant and a gelling agent. The liquid propellant contains one or more of hydrazine, hydrazine derivatives (such as methyl hydrazine, unsym-dimethyl hydrazine) with amino and hydroxylamine, and/or one or more of nitrate, hydrochloride, sulfate, phosphate, acetate, formate and oxalate of the above substances. For example, the liquid propellant is pure methylhydrazine, a hydrazine-ethanol mixture, an aqueous hydroxylamine nitrate solution, a hydroxylamine nitrate-hydrazine-water mixture, or the like.
The organic solvent used in the embodiment of the present invention contains an aldehyde compound, a ketone compound, or both an aldehyde compound and a ketone compound. For example, the organic solvent is pure acetone, an acetone-methanol mixed solvent, an acetaldehyde-ethyl acetate solution, a cyclohexanone-butyraldehyde-isopropanol solution, or the like.
The organic solvent used in the embodiment of the invention can react with all or part of other components except the gelling agent in the colloidal propellant, and the reaction product can be dissolved in the used organic solvent. When analyzing colloidal propellants comprising hydrazine salts, hydrazine derivative salts with amino groups, hydroxylamine salts, these salts cannot be dissolved in organic solvents by physical dissolution, but can be converted into substances soluble in organic solvents by reaction between the selected organic solvent and these salts. For example, when the organic solvent used is pure acetone, the acetone may react with hydrazine, hydrazine derivatives having amino groups, hydroxylamine and salts of the above in the colloidal propellant according to the following formula:
in the formula A-And HA is an acid radical ion salified with hydrazine, a hydrazine derivative and hydroxylamine and a corresponding acid thereof. The hydrazone, oxime, water and acid (HA in the reaction formula) generated in the reaction can be dissolved in acetone.
In at least one embodiment of the present invention, the colloidal propellant contains, in addition to the gelling agent, other components that do not react with the organic solvent used, and these components are also soluble in the organic solvent used. For example, acetone is added to a colloidal propellant consisting of hydroxylamine nitrate-isopropanol-water-gelling agent, in which isopropanol and water do not react with acetone, but both are soluble in acetone.
Thus, in the present example, the colloidal propellant is added with a sufficient amount of organic solvent to provide a mixed system in which the components other than the gelling agent are present in liquid/solution form.
The gelling agent contained in the colloidal propellant in the examples of the present invention precipitates alone because it is insoluble in the added organic solvent. Since only the gelling agent is separated out alone in the mixed system, the gelling agent can be separated from the liquid/solution components in the mixed system by means of solid-liquid separation. The separated gelling agent is washed and dried to remove other components attached to the gelling agent, and then the content of the gelling agent in the colloidal propellant can be calculated by weighing. For example, when acetone is added in a sufficient amount to a colloidal propellant composed of hydrazine-water-konjac gum, only the gelling agent konjac gum is precipitated as a flocculent precipitate, and the flocculent precipitate is filtered, washed, dried and weighed, and the content of the flocculent precipitate in the colloidal propellant of hydrazine-water-konjac gum is calculated.
In at least one embodiment of the present invention, the gelling agent is a polymer gelling agent, and the polymer gelling agent is one or more selected from cellulose derivatives, dextran, glucomannan, chitosan, starch, dextrin, guar gum, sesbania gum, carrageenan, xanthan gum, konjac gum, sodium alginate, gelatin, agar, acrylic polymers, and polyvinyl alcohol, for example, the gelling agent is cellulose sulfate, polyacrylamide, konjac gum-carrageenan mixture, and the like.
The organic solvent used in at least one embodiment of the present invention is preferably acetone. Among all aldehydes and ketones, acetone has a relatively small molecular weight, and acetone per unit mass can react with relatively many colloidal propellant samples; on the other hand, acetone has a relatively proper polarity, and as a weak-polarity organic solvent, acetone can be mutually soluble with solvents with stronger polarity, such as alcohol, water and the like which are common in propellants, and can also prevent a gelling agent dissolved in the strong-polarity solvent from being dissolved in the solvents, so that complete precipitation of the gelling agent is promoted.
In at least one embodiment of the present invention, the volume of organic solvent added per gram of colloidal propellant sample is between 1mL and 100mL, preferably between 2mL and 10 mL. When the added organic solvent is too little, the organic solvent cannot completely react the components capable of reacting with the organic solvent in the colloidal propellant (for example, 0.9mL of acetone is added into 1g of anhydrous hydrazine colloidal propellant, the added acetone can only react less than 40% of hydrazine, and more hydrazine is remained in the reaction system, and at this time, the gelling agent capable of dissolving in hydrazine cannot be completely separated out), or the components which do not react with the organic solvent except the gelling agent in the colloidal propellant still occupy a higher proportion in the mixed system (for example, 0.8mL of organic solvent is added into 1g of colloidal propellant containing 50% of water by mass fraction, the mass fraction of water in the obtained mixed system is not less than 30%, and at this time, the gelling agent capable of being easily dissolved in water cannot be completely separated out), so that the complete separation of the gelling agent is influenced. When the amount of the organic solvent is too much, the mass of the sample that can be analyzed is small in a reaction vessel having a certain capacity, which affects the precision of the analysis of the content of the gelling agent (for example, the density of the colloidal propellant is 1g/mL, in a vessel having a capacity of 30mL, if 5mL of the organic solvent is added per gram of the sample, the mass of the sample that can be analyzed at most at a single time is 5 g; if 149mL of the organic solvent is added per gram of the sample, the mass of the sample that can be analyzed at a single time is only 0.2g, which is limited by the precision of a balance for weighing the content of the gelling agent, and the latter is much less precise than the former in the measurement), and unnecessary waste.
In at least one embodiment of the present invention, when an organic solvent is added to the colloidal propellant, a certain amount of water may be added to the organic solvent. The small amount of water mixed into the organic solvent can properly improve the polarity of the organic solvent and enhance the solubility of the organic solvent to strong polar components in a reaction system. However, the amount of water incorporated should not be so large as to avoid partial or complete dissolution of the gelling agent therein, resulting in a measured amount of gelling agent that is lower than the actual value. For example, when a colloidal propellant containing a small amount of ammonium nitrate and polyacrylamide as a gelling agent is analyzed, the colloidal propellant can be treated with a mixed solvent of acetone and water (in a volume ratio of 90: 10) to completely precipitate polyacrylamide while preventing precipitation of ammonium nitrate.
In at least one embodiment of the present invention, the volatile component in the colloidal propellant is removed, either completely or partially, before the organic solvent is added to the colloidal propellant, to achieve concentration of the colloidal propellant, thereby reducing the amount of organic solvent used. For example, when the colloidal propellant consisting of unsymmetrical dimethylhydrazine, water and a gelling agent is analyzed, dry nitrogen is used for blowing the surface of the colloidal propellant in advance, so that partial unsymmetrical dimethylhydrazine in the colloidal propellant is volatilized and removed, and the amount of organic solvent required by the reaction is reduced.
The technical solutions of the present invention are further illustrated by the following specific examples, but the scope of the present invention is not limited by the specific conditions of these specific examples.
Example 1:
taking colloidal hydrazine-70 propellant (hydrazine-70 is composed of hydrazine and water, the used gelatinizer is konjac gum) in a 50mL centrifuge tube, and weighing the sample with the net mass of 3.0134 g. Adding 30mL of acetone into a centrifuge tube, separating out the gelatinizing agent konjac gum in the colloidal hydrazine-70 propellant in the acetone, reacting the hydrazine with the acetone, and dissolving the product of the reaction, namely the azino acetonide, water and the water contained in the colloidal hydrazine-70 in the acetone. After removing the supernatant by centrifugation, 20mL of acetone was added to the centrifuge tube and the gelling agent solids in the centrifuge tube were washed by shaking. Repeating the above steps twice to completely clean impurities adsorbed on the surface of the gelling agent. After removing the washing solvent by centrifugation, the centrifuge tube was dried in an oven at 60 ℃ to a constant weight, and the mass of the gelling agent was weighed to 0.0314g, and the mass fraction of the gelling agent in the sample was calculated to be 0.0314 ÷ 3.0134 × 100% ═ 1.04%.
Example 2:
taking a colloidal hydroxylamine nitrate-based propellant (the hydroxylamine nitrate-based propellant consists of hydroxylamine nitrate, isopropanol and water, and the used gelling agent is polyvinyl alcohol) in a 50mL centrifuge tube, and weighing the sample to obtain 4.1621g of net mass. The centrifuge tube was placed in a water bath at 60 ℃ and the sample was concentrated by evaporating volatile components from the sample by purging the surface of the sample with dry nitrogen. After about 4 hours of nitrogen purge, the mass of the sample remaining was about 1/3 of the original mass. The concentration was stopped, and after allowing the sample to stand and cool to room temperature, a mixed solvent of 13.5mL of acetone and 1.5mL of water was added thereto. Polyvinyl alcohol in the concentrated sample is separated out in the mixed solvent, hydroxylamine nitrate reacts with acetone, and acetone oxime, nitric acid, water as a reaction product, and isopropanol and water contained in the sample can be dissolved in the added mixed solvent. The supernatant was removed by centrifugation, and a mixed solvent of 13.5mL of acetone and 1.5mL of water was added to the centrifuge tube, and the gelling agent solid in the centrifuge tube was washed with shaking. Repeating the above steps twice to completely clean impurities adsorbed on the surface of the gelling agent. After removing the washing solvent by centrifugation, the centrifuge tube was dried in an oven at 60 ℃ to a constant weight, and the mass of the gelling agent was 0.0932g, and the mass fraction of the gelling agent in the sample was calculated to be 0.0932 ÷ 4.1621 × 100% ═ 2.24%.
Claims (9)
1. A method of analyzing the gelling agent content of a colloidal propellant, comprising:
the colloidal propellant contains a liquid propellant and the gelling agent, and the liquid propellant contains one or more of hydrazine, hydrazine derivatives with amino groups and hydroxylamine, and/or one or more of nitrate, hydrochloride, sulfate, phosphate, acetate, formate and oxalate of the substances;
adding an organic solvent into the colloidal propellant, wherein the organic solvent contains aldehyde and/or ketone compounds;
the organic solvent may react with all or some of the other components of the colloidal propellant other than the gelling agent, and the reaction product may be soluble in the organic solvent, e.g., components of the colloidal propellant other than the gelling agent that do not react with the organic solvent may be present and may also be soluble in the organic solvent;
the gelling agent in the colloidal propellant is separated out independently because the gelling agent is insoluble in the organic solvent, and the gelling agent is separated and weighed, and the content of the gelling agent in the colloidal propellant is calculated.
2. The method according to claim 1, characterized in that the gelling agent is a polymeric gelling agent.
3. The method according to claim 2, wherein the high molecular gelling agent is one or more selected from the group consisting of cellulose derivatives, dextran, glucomannan, chitosan, starch, dextrin, guar gum, sesbania gum, carrageenan, xanthan gum, konjac gum, sodium alginate, gelatin, agar, acrylic polymers, and polyvinyl alcohol.
4. The process according to claim 1, characterized in that the organic solvent is preferably acetone.
5. The method according to claim 1, characterized in that the method comprises the steps of:
(1) weighing a certain amount of the colloidal propellant;
(2) adding the organic solvent to the colloidal propellant to precipitate the gelling agent;
(3) separating the precipitated gelling agent from the liquid component;
(4) washing the separated gelling agent;
(5) drying the washed gelling agent;
(6) and weighing the dried gelling agent, and calculating the content of the gelling agent in the colloidal propellant.
6. The method according to claim 1 or 5, characterized in that the volume of the organic solvent added per gram of the colloidal propellant is between 1mL and 100 mL.
7. The method according to claim 6, characterized in that the volume of the organic solvent added per gram of the colloidal propellant is preferably between 2mL and 10 mL.
8. A method according to claim 1 or 5, characterised in that when the organic solvent is added to the colloidal propellant, an amount of water is also incorporated into the organic solvent, in an amount that does not affect the complete precipitation of the gelling agent.
9. The method according to claim 1 or 5, characterized in that before adding the organic solvent to the colloidal propellant, the colloidal propellant is concentrated by completely or partially removing volatile components from the colloidal propellant.
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| CN201811501460.7A CN111289403B (en) | 2018-12-10 | 2018-12-10 | Method for analyzing content of gelatinizing agent in colloid propellant |
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| CN115650808A (en) * | 2022-09-21 | 2023-01-31 | 南京理工大学 | Hydroxylamine nitrate based green pollution-free gel propellant and preparation method thereof |
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