CN106336516B - The preparation method of the pure colloidal sol of nitrate ester plasticized polyether propellant - Google Patents
The preparation method of the pure colloidal sol of nitrate ester plasticized polyether propellant Download PDFInfo
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- CN106336516B CN106336516B CN201510553796.8A CN201510553796A CN106336516B CN 106336516 B CN106336516 B CN 106336516B CN 201510553796 A CN201510553796 A CN 201510553796A CN 106336516 B CN106336516 B CN 106336516B
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Abstract
The present invention is the preparation method that a kind of purification for energetic material field prepares the pure colloidal sol of nitrate ester plasticized polyether propellant.It removes most of dangerous plasticizer nitroglycerine using solvent soaking washing methods（NG）, butanetriol trinitrate（BTTN）, ammonium perchlorate and octogen, colloidal sol is extracted in Soxhlet extractor using organic solvent, dialysis prepares the experimental procedures such as pure colloidal sol, prepares high-purity nitrate ester plasticized polyether propellant colloidal sol.The present invention is widely used in the purification of polymer in energetic material, can be effectively reduced sample treatment risk, simplify purification preparation process, cost-effective, and has the advantages that preparation method is simple and practicable, experimentation facilitates popularization.
Description
Technical field
The present invention relates to a kind of separation method of the high molecular material containing energy, specifically a kind of dialysis purifying nitrate
It is plasticized the method for Polyether propellants colloidal sol.
Background technology
Polymer elastomer is by condensed phase（Crosslinking curing network）The molten of plasticization is played with being filled between lattice chain
Glue phase（The linear and branched high polymer and plasticizer of chain growth and curing reaction）The elastomer of composition.Solid propellant is from originally
It is said in matter, is the polymer elastomer for being filled with a large amount of solid packings.
Network structure is the stent of solid propellant, influences the principal element of mechanical properties of propellant.At present, gel fraction
With crosslink density be characterize solid propellant network structure main means, and be also propellant failure and ageing predetermination institute according to
Bad major parameter.So-called polymer elastomer gel, it is considered that it is the part for forming elastomer network, that is, polymer
At a certain temperature, by for quite a long time, reaching undissolved part after Comparative dissolution balances in its good solvent, and
Colloidal sol is then the part of its elastomer network dissolving.In fact, the colloidal sol composition variation of not upper network, more can inherently react
The failure mechanism of solid propellant.
For HTPB propellant, the research of this respect was once done both at home and abroad, but the propellant of nitrate plasticising was come
It says, due to the presence of large dosage of nitrate, it is a technical bottleneck that separation, which prepares pure colloidal sol,.
Nitrate ester plasticized polyether propellant is exactly two functions being plasticized by nitroglycerine, the butantriol dinitrate of large dosage
The polyethylene glycol of degree（PEG）Adhesive, the net being cross-linked to form with isocyanates (N-100) curing agent of polyfunctionality by end
Network system is filled with the macromolecule compounded rubber body of the solid packings such as a large amount of ammonium perchlorate and octogen as stent
System.NEPE propellant colloidal sols are the parts for not forming cross-linked network in curing reaction, including the PEG segments reacted with N-100 and
The complete PEG of unreacted.Using ripe NEPE propellants as research object, the practical approach of colloidal sol preparation is obtained, can be
The propellant of other nitrate plasticising is provided with reference to technology.
There is document to show：Using ether washing by soaking propellant, most nitrate and a small amount of stabilization agent can be removed,
Chloroform recovery PEG colloidal sols are used again, also contain a small amount of oxidant ammonium perchlorate, octogen and nitric acid in obtained colloidal sol
The small molecular weight impurities such as ester.Since these small molecular weight impurities are easy to be wrapped in sticky polymeric sol, and in a solvent
Dissolution properties are similar, it is difficult to removal completely.Therefore, how small-molecule substance is removed, is still the work for having no document report.
In addition, bag filter is removed into small molecular weight impurity so far there are no document report for propellant field.
Invention content
The invention aims to provide a kind of preparation method of the pure colloidal sol of nitrate ester plasticized polyether propellant, it can have
Effect ground reduces sample treatment risk, simplifies preparation procedure, cost-effective, low toxicity, environmental protection.
The present invention removes most of dangerous plasticizer nitroglycerine using solvent soaking washing methods（NG）, butantriol three
Nitrate（BTTN）, ammonium perchlorate and octogen, colloidal sol is extracted in Soxhlet extractor using organic solvent, prepared by dialysis
The experimental procedures such as pure colloidal sol, prepare high-purity nitrate ester plasticized polyether propellant colloidal sol, and specific technical solution divides following steps：
StepIt prepares detection sample and is put into solvent to impregnate and remove most of small molecule：Propellant is cut into particulate,
It weighs to propellant particulate, adds in solvent, impregnate 1~2 day, wash and take out propellant particulate；Remove most of nitrate and
Stabilization agent.
StepColloidal sol is extracted using Soxhlet extractor：Propellant particulate is put into filtration paper cylinder, and is put into Soxhlet extraction
In device, solvent is added in, the heating and refluxing extraction 1~2 day at 60 DEG C~85 DEG C removes most of solvent, obtains thick colloidal sol；
StepPrepare pure colloidal sol：Thick colloidal sol is put into bag filter, after being dialysed 3~4 days using tap water, using matter
It measures the ethanol water than 10~30% to dialyse 3~4 days, is freeze-dried after taking out concentration, obtains pure colloidal sol.
Step of the present inventionIn solvent be methanol, petroleum ether, ether, isopropyl ether, one or more of benzene.
Step of the present inventionIn：During impregnating 1~2 day, replace 5~10 solvents and repeatedly washed with solvent
It is colourless to solution.
Step of the present inventionIn solvent be methanol, acetonitrile, acetone, one or more of chloroform.
Bag filter cutoff of the present invention is one kind in 500~2000.
The beneficial effects of the invention are as follows：Large dosage can only be dissolved by employing certain in the sample preparation procedure of the present invention
Dangerous nitrate and oxidant ammonium perchlorate and the organic solvent of octogen, then find and only dissolve having for macromolecular colloidal sol
Solvent and extraction sol gel process.It meanwhile will be big for propellant field purifying polymer for the bag filter in biological sample
Molecule solves the impurities removal of colloidal sol small molecular substance, and pure colloidal sol is made.The present invention is the sample cleanup in propellant field
New thinking is brought with removal of impurities, is conducive to propellant formulation research.The present invention is widely used in polymer in energetic material
Purification can be effectively reduced sample treatment risk, simplify purification preparation process, be cost-effective, and with preparation method letter
The advantages of single easy, experimentation facilitates popularization.
Description of the drawings
Fig. 1 is the infrared spectrogram of the 1 pure colloidal sol of gained of embodiment.
Fig. 2 is the infrared spectrogram of the 2 pure colloidal sol of gained of embodiment.
Specific embodiment
With reference to embodiment, the present invention is further described.
Embodiment 1：It is prepared by the purification of the pure colloidal sol of nitrate ester plasticized polyether propellant
Step 1 prepares propellant sample and is put into solvent and impregnates：Solvent chooses petroleum ether, impregnates 2 days, during which replaces
6 solvents are simultaneously repeatedly washed colourless to solution with a small amount of solvent.
Step 2 extracts colloidal sol using Soxhlet extractor.It is heated to reflux at 85 DEG C 2 days, solvent chooses chloroform, collects molten
Liquid after solvent volatilization recycling, obtains thick colloidal sol.
Step 3 prepares pure colloidal sol.Thick colloidal sol is put into bag filter, bag filter cutoff is 500~1000, is adopted
It dialyses 4 days after tap water dialysis 3 days, then using 10% ethanol water, takes out freeze-drying, obtain pure colloidal sol.
Fig. 1 is the infrared spectrogram of the pure colloidal sol of the gained of embodiment 1, and visible colloidal sol is polyether-polyurethane in figure, without nitric acid
The small molecular weight impurities such as ester, ammonium perchlorate and octogen.
Embodiment 2：It is prepared by the purification of the pure colloidal sol of nitrate ester plasticized polyether propellant
Step 1 prepares propellant sample and is put into solvent and impregnates：Solvent selects methanol, impregnates 2 days, during which replaces 10
Secondary solvent is simultaneously repeatedly washed colourless to solution with a small amount of solvent.
Step 2 extracts colloidal sol using Soxhlet extractor.Solvent chooses acetone, and heating and refluxing extraction 1 day at 70 DEG C is returned
Solution is received, after solvent is volatilized, obtains thick colloidal sol.
Step 3 prepares pure colloidal sol.Thick colloidal sol is put into bag filter, bag filter cutoff is 2000, using certainly
After water is dialysed 4 days, after being dialysed 3 days using 30% ethanol water, freeze-drying is taken out, obtains pure colloidal sol.
The infrared spectrogram of pure colloidal sol is shown in Fig. 2, and visible colloidal sol is polyether-polyurethane in figure, without nitrate, ammonium perchlorate
With the small molecular weight impurities such as octogen.
Claims (4)
1. a kind of preparation method of the pure colloidal sol of nitrate ester plasticized polyether propellant, includes the following steps：
StepIt prepares detection sample and is put into solvent to impregnate and remove most of small molecule：Propellant is cut into particulate, to pushing away
It weighs into agent particulate, adds in solvent, impregnate 1~2 day, wash and take out propellant particulate；
StepColloidal sol is extracted using Soxhlet extractor：Propellant particulate is put into filtration paper cylinder, and is put into Soxhlet extractor,
Solvent is added in, the heating and refluxing extraction 1~2 day at 60 DEG C~85 DEG C removes most of solvent, obtains thick colloidal sol；
StepPrepare pure colloidal sol：Thick colloidal sol is put into bag filter, after being dialysed 3~4 days using water, using 10~30% second
Alcohol solution is dialysed 3~4 days, is freeze-dried after taking out concentration, is obtained pure colloidal sol；
The bag filter cutoff is one kind in 500~2000.
2. a kind of preparation method of the pure colloidal sol of nitrate ester plasticized polyether propellant according to claim 1, it is characterised in that：Institute
State stepIn solvent be methanol, petroleum ether, ether, isopropyl ether, one or more of benzene.
3. a kind of preparation method of the pure colloidal sol of nitrate ester plasticized polyether propellant according to claim 1, it is characterised in that：Institute
State stepIn：During impregnating 1~2 day, replace 5~10 solvents and repeatedly washed with solvent colourless to solution.
4. a kind of preparation method of the pure colloidal sol of nitrate ester plasticized polyether propellant according to claim 1, it is characterised in that：Institute
State stepIn solvent be methanol, acetonitrile, acetone, one or more of chloroform.
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| CN109956455B (en) * | 2019-05-14 | 2020-11-10 | 中国人民解放军32181部队 | Method for ultrasonic-assisted extraction of ammonium perchlorate in scrapped four-component HTPB propellant |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103207243A (en) * | 2012-10-12 | 2013-07-17 | 湖北航天化学技术研究所 | Determination method for migration components in nitrate ester plasticized polyether (NEPE) propellant bonding system |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103207243A (en) * | 2012-10-12 | 2013-07-17 | 湖北航天化学技术研究所 | Determination method for migration components in nitrate ester plasticized polyether (NEPE) propellant bonding system |
Non-Patent Citations (2)
| Title |
|---|
| "NEPE推进剂凝胶分数测定方法研究";宋永莱等;《固体火箭技术》;20021231;第25卷(第4期);第35-37页 * |
| "丁羟弹性体溶胶表征方法研究";芦明等;《推进技术》;19941031(第5期);第73-80页 * |
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Application publication date: 20170118 Assignee: Nanjing Chenguang Group Co., Ltd. Assignor: Hubei Aerospace Chemical Technology Research Institute Contract record no.: 2019320000011 Denomination of invention: Preparation method of pure nitrate plasticized polyether propellant sol Granted publication date: 20180626 License type: Common License Record date: 20190118 |