CN104897606B - A kind of rapid analysis method of methyl hydrazine reaction process logistics - Google Patents
A kind of rapid analysis method of methyl hydrazine reaction process logistics Download PDFInfo
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Abstract
The invention discloses a kind of rapid analysis method of methyl hydrazine reaction process logistics, this method extracts one material as tributary from process-stream, and tributary material is analyzed using near infrared spectroscopy, acquires the near infrared spectrum of anti-product output stream；Reaction process logistics with chemical score is used into Partial Least Squares, correction light harvesting spectrum is passed through into the pretreated data of selectivity and corresponding chemical score linear correlation, establish calibration model, using institute's established model, the concentration of various ingredients in reaction process stream is directly obtained according to the near infrared spectrum of acquisition reaction product output stream；According to the demand of aminating reaction and identified various ingredients concentration, the concentration of monomethyl amine component in inlet flow is adjusted.The present invention has many advantages, such as that easy to operate, analysis is succinct, quick, realizes the on-line analysis of methyl hydrazine reaction, is advantageously implemented automation, is controlled convenient for industrial processes, be mainly used for the quick analysis of methyl hydrazine reaction process logistics.
Description
Technical field
The invention belongs to the analysis and testing technology field of chemical process, it is related to a kind of the quick of methyl hydrazine reaction process logistics
Analysis method.
Background technology
Methyl hydrazine (monomethylhydrazine, MMH) is a kind of important hydrazine derivative, its energy (density ratio
Punching) it is higher than uns-dimethylhydrazine, and it is safe in anhydrous hydrazine, it can be used for aerospace control propulsion system and secondary propulsion system (SPS), be empty
Between important energy source material in technical field.In addition, using methyl hydrazine as raw material, many good pesticides and desinsection can be synthesized
Agent, and also have important application in medicine.It has become a kind of rising special new chemical materials.
Raschig process is the method for industrial synthesizing methyl hydrazine earliest, is reacted with ammonia using sodium hypochlorite, then again with a first
Amine reaction generates methyl hydrazine.Reaction product can obtain the very high methyl hydrazine of purity by the separation of the techniques such as desalination, rectifying.
During Separation ＆ Purification, the methyl hydrazine content in solution is very low, is less than 2%, while intermediate material contains a large amount of salt, alkali group
Point.Currently, methyl hydrazine process analysis uses titration, gas chromatography, spectrophotometry etc., because of depositing for a large amount of inorganic bases
This analysis method is needed by a large amount of pre-treatment steps, and cumbersome, labor intensity is big, and analysis time is long, Bu Nengshi
Present line analysis greatly affected automatically controlling and adjusting for commercial plant.
Invention content
The object of the present invention is to provide a kind of rapid analysis methods of methyl hydrazine reaction process logistics, have operating procedure letter
Advantage single, analysis time is short, can realize on-line analysis, be conducive to automatically controlling and adjusting for commercial plant.
According to the present invention, a kind of rapid analysis method of methyl hydrazine reaction process logistics is provided, this method includes：
(1) one material is extracted from process-stream as tributary；
(2) the near infrared light spectrum information of collection technology tributary material analyzes tributary material using near infrared spectroscopy；
(3) by the concentration chemical score of the corresponding material component of near infrared spectrum of reaction process logistics material using inclined
Least square method, which is associated, establishes quantitative calibration models, wherein the chemical score of methyl hydrazine reaction process logistics using titration with
Gas chromatography determine, methyl hydrazine content be 15~20g/L, free alkali content be 4~7g/L, monomethyl amine content be 80~
100g/L, ammonia content are 35~45g/L, and hydrazine hydrate and Dimethylhydrazine content are respectively less than 1.5g/L；
(4) institute's established model is used, methyl hydrazine in reaction process logistics, trip are directly determined by the near infrared spectrum obtained
Concentration from alkali, monomethyl amine, ammonia, hydrazine hydrate, Dimethylhydrazine；
(5) according to methyl hydrazine, free alkali, ammonia, monomethyl amine, two in the demand of aminating reaction and identified tributary material
The concentration of methylhydrazine and hydrazine hydrate adjusts the concentration of monomethyl amine component in inlet flow.
The foundation of the quantitative calibration models is that the reaction process logistics with chemical score is divided into calibration set and verification
Collection, calibration set will correct light harvesting for establishing model, accuracy of the verification collection for verifying model using Partial Least Squares
Spectrum establishes calibration model, utilizes above-mentioned straightening die by the pretreated data of selectivity and corresponding chemical score linear correlation
Type predicts verification collection, by predicted value and chemical score contrast verification model.
Methyl hydrazine can be by quantitative SPECTRAL REGION 9234 to 7842cm in the process-stream-1, free alkali can be by quantitative
SPECTRAL REGION 7286 is to 6662cm-1, ammonia can be by quantitative SPECTRAL REGION 6668 to 6057cm-1, monomethyl amine can be by quantitative spectrum
Region 9634 is to 7946cm-1, hydrazine hydrate can be by quantitative SPECTRAL REGION 7244 to 6019cm-1, Dimethylhydrazine can be by quantitative spectrum
Region 6012 is to 5452cm-1。
In the rapid analysis method of the methyl hydrazine reaction process logistics, the methyl hydrazine in methyl hydrazine reaction process logistics contains
Amount is 18.5g/L, and free alkali content 5.3g/L, monomethyl amine content is 86.0g/L, ammonia content 36.3g/L, hydrazine hydrate content
For 1.0g/L, Dimethylhydrazine content is 0.6g/L.
Advantages of the present invention：
(1) the near infrared light spectrum information of present invention acquisition tributary material, is analyzed using near infrared spectroscopy, with gas-chromatography
Method, titration are compared, and sample pre-treatments step is eliminated, and operating procedure is simple.
(2) present invention uses institute's established model, can be straight in 1 minute according to the near infrared spectrum of acquisition product output stream
It connects to obtain the concentration of various ingredients in reaction process stream, analysis time is short, has the advantages that succinct, quick.
(3) present invention adjusts a first in inlet flow according to the concentration of the demand and identified various ingredients of aminating reaction
The concentration of amine or ammonia components can realize the on-line analysis of methyl hydrazine reaction, be advantageously implemented automation, be convenient for industrial production mistake
Process control.
Specific implementation mode
The present invention is described in further detail for the embodiment provided below in conjunction with inventor.
Fig. 1 is the quick analysis schematic diagram of methyl hydrazine reaction process logistics.Including first stage reactor (2), second stage reactor
(3), NIR flow cells (5), NIR light spectrometer (1), optical fiber cable (110) and (109), separator (6), regulating valve (9).103、
104,105,106,108,111,112,113,114 be pipeline.
In the present invention, NIR analyzers are available commercially near infrared spectrometers, and main element includes light source, optics
System and detector.NIR light spectrometer (1) manufactures Fourier transformation type spectrometer for Brooker company.NIR light spectrometer (1) passes through
Optical cable and optical fibres are connect with NIR flow cells (5).The NIR flow cell materials used are low hydroxyl quartz, optical path length 5mm.
First stage reactor is that sodium hypochlorite reacts generation chloramines with ammonia, and equation is：
NaOCl+NH3→NH2Cl+NaOH
Second stage reactor is that monomethyl amine reacts generation methyl hydrazine with chloramines, and equation is：
NH2Cl+CH3NH2+NaOH→CH3NH2NH2+NaCl+H2O
In NIR analyzers in use, technique input logistics sodium hypochlorite, liquefied ammonia component are respectively by 103,104 points of pipeline
It is not input to first stage reactor (2), is reacted in first stage reactor (2) and generates chloramines, reaction product includes water, chloramines, hydroxide
Sodium and unreacted ammonia.Sodium hydroxide is free alkali.
The product stream is as second-stage reaction logistics, with the monomethylamine aqueous solution from pipeline 105 through pipeline 112, into two
Section reactor (3) react generate methyl hydrazine, reaction product be mainly comprising methyl hydrazine, monomethyl amine, ammonia, sodium hydroxide, sodium chloride,
And the aqueous solution of by-product hydrazine hydrate, Dimethylhydrazine.Second-stage reaction product flows through pipeline 106, is detached into separator (6), gas
Mutually by being detached after regulating valve (9) after pipeline 114, liquid phase enters rectification working process by 113.
Second-stage reaction product stream leads to NIR flow cells (5) by branch line 108, is sent into after tested through pipeline 111
Separator (6).NIR flow cells (5) are connected to NIR light spectrometer (1), NIR flow cells (5) by optical fiber cable (110) and (109)
In mixture by NIR light spectrometer (1) analyze, spectrometer scanning wavelength ranging from 12500 to 4000cm-1, resolution ratio 8cm-1,
Light path 5mm, using optical cable and optical fibres loop as reference.
According to production technology demand, it is thus necessary to determine that methyl hydrazine, free alkali, ammonia, monomethyl amine, diformazan in second-stage reaction product stream
The concentration of hydrazine and hydrazine hydrate.The chemical analysis method difference of each key component concentration is as follows：Monomethyl amine concentration of component is using oxidation
Reductometry；Free alkali and ammonia components concentration use acid-base titration；Methyl hydrazine, hydrazine hydrate and Dimethylhydrazine use gas-chromatography
Method.
Second-stage reaction product stream is divided into calibration set and verification collects, calibration set is for establishing model, using offset minimum binary
Method, by correction light harvesting spectrum by the pretreated data of selectivity and above-mentioned corresponding chemical score linear correlation, wherein two sections anti-
Answer product stream by quantitative SPECTRAL REGION be 9634cm-1~5452cm-1, methyl hydrazine can by quantitative SPECTRAL REGION 9234 to
7842cm-1, establish the calibration model of second-stage reaction product stream.Verification collection is predicted using above-mentioned calibration model, will be predicted
Value and above-mentioned chemical score contrast verification model.
Using above-mentioned institute's established model, the near infrared spectrum that output stream is reacted according to acquisition directly obtains second-stage reaction product stream
The concentration of middle methyl hydrazine, ammonia, monomethyl amine, free alkali, hydrazine hydrate, Dimethylhydrazine.
According to methyl hydrazine, ammonia, monomethyl amine, free alkali, hydration in second-stage reaction product stream determined by near infrared spectroscopy
The concentration ratio demand of hydrazine, the concentration of Dimethylhydrazine and reaction adjusts in 101 pipelines a first in ammonia components input quantity or 105 pipelines
The input quantity of amine component.
Embodiment 1：
As shown in Figure 1, in NIR analyzers in use, technique input logistics sodium hypochlorite, liquefied ammonia component enter one section of reaction
Device (2) reaction generates chloramines, and reaction product includes water, chloramines, sodium hydroxide and unreacted ammonia.The product stream is anti-as two sections
Logistics is answered, entering second stage reactor (3) with the monomethylamine aqueous solution from 105 pipelines reacts generation methyl hydrazine, reaction product packet
Aqueous, methyl hydrazine, ammonia, sodium chloride and unreacted monomethyl amine and sodium hydroxide and by-product are hydrated hydrazine and its derivative.
Second-stage reaction product stream leads to NIR flow cells (5) by branch line 108, is sent into after tested through pipeline 111
Separator (6).NIR flow cells (5) are connected to NIR light spectrometer (1), NIR flow cells (5) by optical fiber cable (110) and (109)
In mixture by NIR light spectrometer (1) analyze, spectrometer scanning wavelength ranging from 12500 to 4000cm-1, resolution ratio 8cm-1,
The scanning times of light path 5mm, every spectrum are 32 times, using optical cable and optical fibres loop as reference.
The chemical analysis method difference of each key component concentration is as follows in second-stage reaction product stream：Monomethyl amine concentration of component is adopted
Use oxidimetry；Acid-base titration is respectively adopted in free alkali and ammonia components concentration；Methyl hydrazine, hydrazine hydrate and Dimethylhydrazine are adopted
Use gas chromatography.Wherein a concentration of 15~20g/L of methyl hydrazine, free alkali concentration be 4~7g/L, monomethyl amine a concentration of 80~
100g/L, ammonia density are 35~45g/L, and the concentration of hydrazine hydrate and Dimethylhydrazine is respectively less than 1.5g/L.
Second-stage reaction product stream is divided into calibration set and verification collects, calibration set is for establishing model, and verification collection is for verifying
The accuracy of model will correct light harvesting spectrum after selectively pre-processing using Partial Least Squares in certain SPECTRAL REGION
Data establish the calibration model of second-stage reaction product stream with above-mentioned corresponding chemical score linear correlation, utilize above-mentioned straightening die
Type predicts verification collection, by predicted value and above-mentioned chemical score contrast verification model.
Wherein second-stage reaction product stream is 9634~5452cm by quantitative SPECTRAL REGION-1, methyl hydrazine can be by quantitative light
Region 9234 is composed to 7842cm-1。
The preprocess method of use has：Without Pretreated spectra, multiplicative scatter correction, vector normalization method, min-max normalizing
Change, first derivative, first derivative+vector normalization method, first derivative+MSC (additional dispersion correction), second dervative etc..Verification collection
Accuracy for verifying model has choosing using Optimized models such as different pretreatments method, different dimensions, different spectral bands
The rejecting abnormalities sample selected predicts verification collection using above-mentioned calibration model, predicted value and the comparison of above-mentioned chemical score is tested
Card optimizes and determines model, and the major parameter of model optimization is optimal spectrum quantification range, the Pretreated spectra of each measured portions
The coefficient of determination (the R of method, model2), model cross validation root-mean-square-deviation (RMSECV) and verification collection root-mean-square-deviation
(RMSEP).Methyl hydrazine, free alkali, ammonia, monomethyl amine, Dimethylhydrazine and six kinds of components of hydrazine hydrate are dense in the process products stream established
The model parameter of degree is shown in Table 1.
Using above-mentioned institute's established model, the near infrared spectrum that output stream is reacted according to acquisition directly obtains second-stage reaction product stream
Middle methyl hydrazine, ammonia, free alkali, monomethyl amine, hydrazine hydrate, Dimethylhydrazine concentration and acquire 18 samples and carried out using chemical method
The standard value of analysis, near infrared spectroscopy predicted value and chemical determination is shown in Table 2.
Compare one section of reaction stream in monomethyl amine, liquefied ammonia component concentration, with the determined second-stage reaction of near infrared spectroscopy
Methyl hydrazine, ammonia, monomethyl amine and by-product hydrazine hydrate, Dimethylhydrazine, concentration, calculate the conversion ratio of monomethyl amine, product in product stream
Selectivity.Association reaction requires monomethyl amine and chloramines molar ratio is 7.5 ︰ 1, and the concentration that near infrared spectroscopy is measured adjusts 101
In pipeline in ammonia components input quantity or 105 pipelines monomethyl amine component input quantity.
Table 1 exports the parameter list of six kinds of component near-infrared spectroscopies of logistics
| Model name | Quantitative spectrometric range/cm-1 | Preprocessing procedures | R2 | RMSECV/g/L | RMSEP/g/L |
| Methyl hydrazine | 9234~7842 | Single order leads+MSC | 0.99 | 0.29 | 0.28 |
| Free alkali | 7286~6662 | SNV | 0.97 | 0.15 | 0.14 |
| Ammonia | 6668~6057 | Single order is led | 0.98 | 0.47 | 0.39 |
| Monomethyl amine | 9634~7946 | Single order leads+SNV | 0.98 | 0.63 | 0.55 |
| Hydrazine hydrate | 7244~6019 | SNV | 0.96 | 0.13 | 0.11 |
| Dimethylhydrazine | 6012~5452 | MSC | 0.93 | 0.12 | 0.12 |
Table 2 is using near infrared spectroscopy predicted value and the standard value for using chemical determination
Claims (2)
1. a kind of rapid analysis method of methyl hydrazine reaction process logistics, this method include：
(1) one material is extracted from process-stream as tributary；
(2) the near infrared light spectrum information of collection technology tributary material, is analyzed using near infrared spectroscopy；
(3) the concentration chemical score use of the corresponding material component of near infrared spectrum of reaction process logistics material is partially minimum
Square law, which is associated, establishes quantitative calibration models, and wherein the chemical score of methyl hydrazine reaction process logistics uses titration and gas phase
Chromatography determines that methyl hydrazine content is 15~20g/L, and free alkali content is 4~7g/L, and monomethyl amine content is 80~100g/L,
Ammonia content is 35~45g/L, and hydrazine hydrate and Dimethylhydrazine content are respectively less than 1.5g/L；
(4) institute's established model is used, methyl hydrazine in reaction process logistics is directly determined by the near infrared spectrum obtained, is dissociated
The concentration of alkali, monomethyl amine, ammonia, hydrazine hydrate, Dimethylhydrazine；
(5) according to methyl hydrazine, free alkali, ammonia, monomethyl amine, Dimethylhydrazine in the demand of aminating reaction and identified tributary material
With the concentration of hydrazine hydrate, the concentration of monomethyl amine component in inlet flow is adjusted；
The foundation of the quantitative calibration models is that the reaction process logistics with chemical score is divided into calibration set and verification collection, school
Positive collection is passed through correction light harvesting spectrum using Partial Least Squares for establishing model, accuracy of the verification collection for verifying model
The pretreated data of selectivity and corresponding chemical score linear correlation, establish calibration model, using above-mentioned calibration model to testing
Card collection is predicted, by predicted value and chemical score contrast verification model；
Methyl hydrazine can be by quantitative SPECTRAL REGION 9234 to 7842cm in the process-stream-1, free alkali can be by quantitative spectrum
Region 7286 is to 6662cm-1, ammonia can be by quantitative SPECTRAL REGION 6668 to 6057cm-1, monomethyl amine can be by quantitative SPECTRAL REGION
9634 to 7946cm-1, hydrazine hydrate can be by quantitative SPECTRAL REGION 7244 to 6019cm-1, Dimethylhydrazine can be by quantitative SPECTRAL REGION
6012 to 5452cm-1。
2. according to claim 1 in the rapid analysis method of methyl hydrazine reaction process logistics, methyl hydrazine reaction process logistics
In methyl hydrazine content be 18.5g/L, free alkali content 5.3g/L, monomethyl amine content be 86.0g/L, ammonia content 36.3g/
L, hydrazine hydrate content are 1.0g/L, and Dimethylhydrazine content is 0.6g/L.
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