CN107255683A - A kind of hydrazine propellant analysis filling column preparation method - Google Patents
A kind of hydrazine propellant analysis filling column preparation method Download PDFInfo
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- CN107255683A CN107255683A CN201710539945.4A CN201710539945A CN107255683A CN 107255683 A CN107255683 A CN 107255683A CN 201710539945 A CN201710539945 A CN 201710539945A CN 107255683 A CN107255683 A CN 107255683A
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- Prior art keywords
- fixer
- hydrazine propellant
- hydrazine
- stainless steel
- analysis
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/60—Construction of the column
- G01N30/6052—Construction of the column body
Abstract
The invention discloses a kind of hydrazine propellant analysis filling column preparation method, the stationary phase of the packed column is porous polymer, and fixer is alcamines and KI mixture, and stationary phase is with fixer mass ratio：3~5:1；Stainless steel tube selects internal diameter 2mm, 2~4m of length, and inwall is through decontaminating Passivation Treatment.Packed column disclosed by the invention is used for gas chromatography analysis hydrazine propellant, by in the coated fixer of porous polymer class carrier, the adsorption/desorption process conducted in separation process is set to occur in fixer, realize efficiently separating for each component, can quick separating go out wherein impurity, solve peak hangover and peak be superimposed problem.Stainless steel pipe inner surface is passivated processing by the present invention, it is therefore prevented that reversible adsorption occurs for the material such as water, dimethylamine, inclined hydrazone and stainless steel chromatogram vial wall, improves the repeatability of analysis result.
Description
Technical field
The present invention relates to analytical chemistry field, more particularly to a kind of preparation side of hydrazine propellant analysis packed column
Method.
Background technology
Anhydrous hydrazine (Hz), methyl hydrazine (MMH), uns-dimethylhydrazine (UDMH) and their mixture are the conventional hydrazines of China
Propellant, in space industry, is widely used in guided missile, satellite and rocket launching as liquid propellant.With China's fire
Arrow launch mission increases year by year, and the demand to Hydrazine fuel is also increasing, and the requirement to property indices is more and more tighter
Lattice.China military standard GJB 1501-1992《Hydrazine propellant universaling analysis method》、GJB 98-1986《Anhydrous hydrazine》And
GJB 753-1989《Uns-dimethylhydrazine》In using chromatography measure Hydrazine propellant constituent content, wherein chromatographic column be with
GDX-403 is the packed column of carrier.Due to all there is stronger pole containing materials such as water, dimethylamine, inclined hydrazones in Hydrazine propellant
Property, therefore can occur reversible adsorption with stainless steel chromatogram vial wall；The oxidation product of Hydrazine propellant can be filled out with chromatographic column simultaneously
Expect that Irreversible Adsorption occurs for GDX-403.
Case above can cause chromatographic peak hangover, impurity peaks included in sample peak, sample component is lost and quantitative result
It is inaccurate, the problems such as data collimation is poor；In use for some time, chromatographic column post effect declines chromatographic column, sample distortion phenomenon
It is just even more serious, finally result in chromatographic column damage.
With chromatographic technological progress, GDX-403 stationary phases consumption is reduced, enterprise's production cost increase, the stationary phase
It is forced to stop production, and there is presently no similar substitute products in the market.Therefore develop a kind of to each group in Hydrazine propellant
Point can quick and complete separation gas chromatographic column packed column, be control Hydrazine propellant quality, it is ensured that aircraft smoothly transmitting and
The important leverage of operation.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of hydrazine propellant analysis filling column preparation method,
Packed column made from this method can be realized to anhydrous hydrazine, methyl hydrazine, uns-dimethylhydrazine and their oxygen by adsorption-desorption principle
Efficiently separating for compound and trace impurity, improves precision of analysis and repeatability, meets hydrazine propellant material
Detection need.
In order to solve the above technical problems, the concrete scheme of the present invention is as follows：
A kind of hydrazine propellant analysis filling column preparation method, its preparation process specifically includes following steps：
1）With styrene, divinylbenzene, acrylic acid, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, dimethylaminoethyl acrylate methyl amine
Ethyl ester is polymerized monomer, and porous polymer is prepared in polymerization under chain initiator, chain-transferring agent, pore-foaming agent, dispersant effect.
2）Alcamine compound and KI are dissolved in absolute ethyl alcohol by metering ratio, 20~30min is disperseed in ultrasonic wave,
Fixer is made.
3）The above-mentioned stationary phase prepared is proportionally mixed with fixer, carried out quantitative coated.
4）Stationary phase after will be coated is placed in 3~4h of baking in 80~90 DEG C of baking oven, is placed in drier and is cooled to room
Temperature, is used as filling monomer.
5）The stainless steel tube that internal diameter is 2mm is chosen, 2~4m is intercepted, is decontaminated, Passivation Treatment, and calculate stainless steel
Pipe pipe inner volume.
6）The gc column tube packing method is used into traditional vavuum pump suction method, vavuum pump vacuum is 0.05-
Populated chromatographic column is obtained after the completion of 0.08MPa, filling.
7）Populated chromatographic column is arranged in gas-chromatography, high pure nitrogen is passed through, nitrogen flow rate 10mL/min is controlled,
15h is activated at 180 DEG C.
The preparation method step 1）In prepare porous polymer and completed using suspension polymerization under the conditions of 25~30 DEG C
Polymerisation.
Styrene, divinylbenzene, acrylic acid, methylacryoyloxyethyl trimethyl are added when prepared by the porous polymer
Ammonium chloride, dimethylaminoethyl methacrylate, chain initiator, chain-transferring agent, pore-foaming agent, dispersant, distilled water mass ratio are：7
~9:9~11:2.5~3.5:1.5~2:2~3:0.4~0.6:0.2~0.3:1.8~2.4:2.3~3:60~75.
Preparation method step 1）Described in chain initiator be mass content 30% hydrogen peroxide and ascorbic acid in mass ratio 9:
1 mixture prepared.
The preparation method step 1）In chain-transferring agent used be TGA or mercaptopropionic acid, preferably mercaptopropionic acid.
The pore-foaming agent is from toluene known in field.
The dispersant is from sodium chloride and hydroxyethyl cellulose known in field.
The porous polymer pattern is circular granular, is prepared using solid forming machine, Task-size Controlling is in 60~120 mesh models
In enclosing, it is 80~100 purposes as stationary phase to filter out granularity.
The stationary phase heap density filtered out be 0.15~0.17g/mL, aperture be 80~100nm, pore volume be 2.5~
2.7mL/g, is 330~355m than surface2/g。
The preparation method step 2）Middle alcamines is in triethanolamine, methyl diethanolamine, diglycolamine, isopropanolamine
One or two, preferably triethanolamine or methyl diethanolamine.
The preparation method step 2）Middle fixer constitutes mass ratio：Alcamines：KI：Absolute ethyl alcohol=93~
96:4~7:100.
The preparation method step 3）In it is coated when stationary phase and fixer mass ratio be 3~5:1.
The preparation method step 3）In specific coated process be：The stationary phase for handling completion is uniformly mixed with fixer
In beaker, in the water bath with thermostatic control that beaker is placed in 80 DEG C, beaker is continuously shaken, steams to loose, dries.
The preparation method step 5）In to prevent that the generation of the materials such as moisture, dimethylamine, inclined hydrazone and stainless steel inside pipe wall can
Inverse absorption, processing method is handled using first decontamination post-passivation mode, and detailed process is：It is first molten with 40~50 DEG C of 5% sodium hydroxide
Immersion steeps stainless steel tube, to remove inwall greasy dirt, then is rinsed three times with 0.02mol/L watery hydrochloric acid, and it is 25 to be then injected into concentration
~30g/L sodium dichromate, in soaking 50~60min at 22~27 DEG C, is finally rinsed not with 40~50g/L sodium carbonate liquor
Rust steel pipe inner wall 5 times.It is placed in after finishing at 120 DEG C and toasts 2h, after cooling, nitrogen purging 0.6h.
The present invention has advantages below compared with prior art：
1. the present invention is by the coated fixer of porous polymer class carrier, making the adsorption-desorption mistake conducted in separation process
Cheng Fasheng realizes efficiently separating for each component in fixer, the problem of chromatographic peak seriously trails is solved, while preventing hydrazine
Irreversible Adsorption of the oxidation product of class propellant in stationary phase, improves precision of analysis.
2. stainless steel pipe inner surface is passivated processing by the present invention, it is therefore prevented that the material such as water, dimethylamine, inclined hydrazone and not
Reversible adsorption occurs for steel chromatographic column of becoming rusty tube wall, improves the repeatability of analysis result.
Embodiment
Embodiment 1
In equipped with thermometer, electric machine agitator, four mouthfuls of reaction bulbs of two constant flow pumps 8.6 grams of styrene of input, 10.3 gram two
Ethenylbenzene, 1.7 grams of MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chlorides, 2.6 grams of dimethylaminoethyl methacrylates, 2.1 grams of toluene
Stir.
The hydrogen peroxide of 0.45 gram mass content 30%, 2.6 grams of dispersants and 30 grams of water are added in 150mL beakers, are stirred to mixed
It is transferred to after closing uniformly in four mouthfuls of reaction bulbs, stirs 30min.
Load 2.0 grams of acrylic acid, 0.05 gram of ascorbic acid and 20 grams of distilled water in a graduated cylinder, No. 1 is labeled as, another
Load 1.0 grams of acrylic acid, 0.25 gram of mercaptopropionic acid and 18 grams of distilled water in an outer graduated cylinder, be labeled as No. 2, reaction temperature is 25
℃。
Mixing speed 300rpm is controlled, liquid in No. 1 graduated cylinder first is added dropwise with constant flow pump, controls the rate of addition to be
0.2mL/min, No. 1 liquid, which is added dropwise, to be started to start that No. 2 liquid are added dropwise after 20min, and it is 0.15mL/min to control rate of addition.No. 2
Liquid continues stirring reaction 3h after dripping, and stops reaction.
React reaction product suction filtration after terminating, eluted 2~3 times with distilled water, acetone, absolute ethyl alcohol, with toluene in rope
Extracted 12 hours in family name's extractor, obtain porous polymer particles, then particle is placed in baking oven and toasted 3 hours in 120 DEG C,
The particle for screening out 80~100 mesh is standby as stationary phase.
9.5 grams of triethanolamine is weighed, 0.5 gram of KI is dissolved in 10.0 grams of absolute ethyl alcohols, disperseed in ultrasonic wave
30min, is made fixer standby.
Weigh 15.0 grams of stationary phase and 3.0 grams of fixer is placed in 25mL beakers, beaker is placed in 80 DEG C of water bath with thermostatic control
In, beaker is continuously shaken, steams to loose, 4h is toasted in the baking oven for being subsequently placed in 90 DEG C, is finally placed in drier and is cooled to room
Temperature, is used as filling monomer.
Selection internal diameter is 2mm, and intercepted length 2m stainless steel tube first soaks stainless steel with 50 DEG C of 5% sodium hydroxide solution
Pipe, to remove inwall greasy dirt, then is rinsed three times with 0.02mol/L watery hydrochloric acid, is then injected into dichromic acid of the concentration for 30g/L
Sodium, in soaking 50min at 25 DEG C, finally rinses stainless steel inside pipe wall 5 times with 45g/L sodium carbonate liquor.120 are placed in after finishing
2h is toasted at DEG C, after cooling, nitrogen purging 0.6h.
Chromatogram column method is loaded according to traditional vavuum pump suction method, it is 0.05-0.08MPa to control vavuum pump vacuum,
Filling completes to can obtain populated chromatographic column.Populated chromatographic column is arranged in gas-chromatography, high pure nitrogen is passed through, controlled
Nitrogen flow rate 10mL/min processed, activates 15h at 180 DEG C, hydrazine propellant analysis is obtained after having activated and is filled out with gas-chromatography
Fill post.
Embodiment 2
8.0 grams of styrene, 9.5 grams of diethyls are put into equipped with thermometer, electric machine agitator, four mouthfuls of reaction bulbs of two constant flow pumps
Alkene benzene, 1.5 grams of MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chlorides, 2.2 grams of dimethylaminoethyl methacrylates, 2.3 grams of toluene are stirred
Mix uniform.
The hydrogen peroxide of 0.45 gram mass content 30%, 2.3 grams of dispersants and 30 grams of water are added in 150mL beakers, are stirred to mixed
It is transferred to after closing uniformly in four mouthfuls of reaction bulbs, stirs 30min.
Load 1.5 grams of acrylic acid, 0.05 gram of ascorbic acid and 20 grams of distilled water in a graduated cylinder, No. 1 is labeled as, another
Load 1.0 grams of acrylic acid, 0.25 gram of mercaptopropionic acid and 20 grams of distilled water in an outer graduated cylinder, be labeled as No. 2, reaction temperature is 25
℃。
Mixing speed 400rpm is controlled, liquid in No. 1 graduated cylinder first is added dropwise with constant flow pump, controls the rate of addition to be
0.2mL/min, No. 1 liquid, which is added dropwise, to be started to start that No. 2 liquid are added dropwise after 20min, and it is 0.15mL/min to control rate of addition.No. 2
Liquid continues stirring reaction 3h after dripping, and stops reaction.
React reaction product suction filtration after terminating, eluted 2~3 times with distilled water, acetone, absolute ethyl alcohol, with toluene in rope
Extracted 12 hours in family name's extractor, obtain porous polymer particles, then particle is placed in baking oven and toasted 3 hours in 120 DEG C,
The particle for screening out 80~100 mesh is standby as stationary phase.
9.5 grams of methyl diethanolamine is weighed, 0.5 gram of KI is dissolved in 10.0 grams of absolute ethyl alcohols, disperseed in ultrasonic wave
30min, is made fixer standby.
Fixer is coated to operate be the same as Example 1 in stationary phase.
Selection internal diameter is 2mm, and intercepted length 3m stainless steel tube first soaks stainless steel with 45 DEG C of 5% sodium hydroxide solution
Pipe, to remove inwall greasy dirt, then is rinsed three times with 0.02mol/L watery hydrochloric acid, is then injected into dichromic acid of the concentration for 25g/L
Sodium, in soaking 60min at 25 DEG C, finally rinses stainless steel inside pipe wall 5 times with 40g/L sodium carbonate liquor.120 are placed in after finishing
2h is toasted at DEG C, after cooling, nitrogen purging 0.6h.
Fill column packing method and burnin operation is same as Example 1.
Embodiment 3
In equipped with thermometer, electric machine agitator, four mouthfuls of reaction bulbs of two constant flow pumps 9.0 grams of styrene of input, 11.0 gram two
Ethenylbenzene, 2.0 grams of MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chlorides, 3.0 grams of dimethylaminoethyl methacrylates, 2.4 grams of toluene
Stir.
The hydrogen peroxide of 0.45 gram mass content 30%, 3.0 grams of dispersants and 35 grams of water are added in 150mL beakers, are stirred to mixed
It is transferred to after closing uniformly in four mouthfuls of reaction bulbs, stirs 30min.
Load 2.0 grams of acrylic acid, 0.05 gram of ascorbic acid and 20 grams of distilled water in a graduated cylinder, No. 1 is labeled as, another
Load 1.5 grams of acrylic acid, 0.25 gram of mercaptopropionic acid and 20 grams of distilled water in an outer graduated cylinder, be labeled as No. 2, reaction temperature is 25
℃。
Mixing speed 400rpm is controlled, liquid in No. 1 graduated cylinder first is added dropwise with constant flow pump, controls the rate of addition to be
0.2mL/min, No. 1 liquid, which is added dropwise, to be started to start that No. 2 liquid are added dropwise after 20min, and it is 0.15mL/min to control rate of addition.No. 2
Liquid continues stirring reaction 3h after dripping, and stops reaction.
React reaction product suction filtration after terminating, eluted 2~3 times with distilled water, acetone, absolute ethyl alcohol, with toluene in rope
Extracted 24 hours in family name's extractor, obtain porous polymer particles, then particle is placed in baking oven and toasted 3 hours in 120 DEG C,
The particle for screening out 80~100 mesh is standby as stationary phase.
5.0 grams of triethanolamine is weighed, 4.4 grams of methyl diethanolamine, 0.6 gram of KI is dissolved in 10.0 grams of absolute ethyl alcohols,
Disperse 30min in ultrasonic wave, fixer is made standby.
Fixer is coated to operate be the same as Example 1 in stationary phase.
Selection internal diameter be 2mm, intercepted length 4m stainless steel tube, stainless steel tube processing procedure, filling column packing method and
Burnin operation is same as Example 2.
Claims (9)
1. a kind of hydrazine propellant analysis filling column preparation method, it is characterised in that preparation process comprises the following steps：
1）With styrene, divinylbenzene, acrylic acid, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride, dimethylaminoethyl acrylate methyl amine
Ethyl ester is polymerized monomer, and porous polymer is prepared in polymerization under chain initiator, chain-transferring agent, pore-foaming agent, dispersant effect, is made
For the stationary phase of packed column；
2）Alcamine compound and KI are measured than being dissolved in absolute ethyl alcohol by mass, 20~30min is disperseed in ultrasonic wave,
Fixer is made；
3）By the above-mentioned stationary phase prepared and fixer according to mass ratio 3~5:1 mixing, is carried out coated；
4）Stationary phase after will be coated is placed in 3~4h of baking in 80~90 DEG C of baking oven, and room temperature is cooled in drier, as
Fill monomer；
5）The stainless steel tube that internal diameter is 2mm is chosen, 2~4m is intercepted, it is first stainless with 40~50 DEG C of 5% sodium hydroxide solution immersion
Steel pipe, to remove inwall greasy dirt, then is rinsed three times with 0.02mol/L watery hydrochloric acid, is then injected into the weight that concentration is 25~30g/L
Sodium chromate, in soaking 50~60min at 22~27 DEG C, finally rinses stainless steel inside pipe wall 5 with 40~50g/L sodium carbonate liquor
It is secondary, it is placed in after finishing at 120 DEG C and toasts 2h, after cooling, nitrogen purges 0.6h, standby；
6）By step 4）The filling monomer being made is filled to step 5）In the stainless steel tube of making, its method uses traditional vacuum
Pumping method, vavuum pump vacuum is 0.05-0.08MPa, and populated chromatographic column is obtained after the completion of filling；
7）By step 6）Populated chromatographic column is arranged in gas-chromatography, is passed through high pure nitrogen, control nitrogen flow rate 10mL/
Min, activates 15h at 180 DEG C, hydrazine propellant analysis packed column is made.
2. a kind of hydrazine propellant analysis filling column preparation method according to claim 1, it is characterised in that step
Rapid 1）Prepare porous polymer and use suspension polymerization, polymeric reaction temperature is 25~30 DEG C.
3. a kind of hydrazine propellant analysis filling column preparation method according to claim 1, it is characterised in that step
Rapid 1）Styrene, divinylbenzene, acrylic acid, methylacryoyloxyethyl trimethyl that described porous polymer is added when preparing
Ammonium chloride, dimethylaminoethyl methacrylate, chain initiator, chain-transferring agent, pore-foaming agent, dispersant, distilled water mass ratio are：7
~9:9~11:2.5~3.5:1.5~2:2~3:0.4~0.6:0.2~0.3:1.8~2.4:2.3~3:60~75.
4. a kind of hydrazine propellant analysis filling column preparation method according to claim 1 or 2, its feature exists
In：Described chain initiator is the hydrogen peroxide and ascorbic acid in mass ratio 9 of mass content 30%:1 mixture prepared.
5. a kind of hydrazine propellant analysis filling column preparation method according to claim 1 or 2, its feature exists
In：Described chain-transferring agent is one kind in TGA, mercaptopropionic acid.
6. a kind of hydrazine propellant analysis filling column preparation method according to claim 1, it is characterised in that：Institute
The porous polymer stated be circular granular, granularity be 80~100 mesh, heap density be 1.5~1.7g/mL, aperture be 80~
100nm, pore volume is 2.5~2.7mL/g, is 330~355m than surface2/g。
7. a kind of hydrazine propellant analysis, which is used, according to claim 1 fills column preparation method, it is characterised in that step
2）Middle alcamine compound is the mixing of one or both of triethanolamine, methyl diethanolamine, diglycolamine, isopropanolamine
Thing.
8. a kind of hydrazine propellant analysis, which is used, according to claim 1 fills column preparation method, it is characterised in that step
2）Middle fixer constitutes mass ratio：Alcamine compound：KI：Absolute ethyl alcohol=93~96:4~7:100.
9. a kind of hydrazine propellant analysis, which is used, according to claim 1 fills column preparation method, it is characterised in that step
3）In specific coated process be：The stationary phase completed will be handled and fixer is uniformly mixed in beaker, beaker is placed in 80 DEG C
Water bath with thermostatic control in, continuously shake beaker, steam to loose, dry.
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