CN101929950A - Method and device for monitoring glycolonitrile preparation technology in real time - Google Patents

Method and device for monitoring glycolonitrile preparation technology in real time Download PDF

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CN101929950A
CN101929950A CN 201010264675 CN201010264675A CN101929950A CN 101929950 A CN101929950 A CN 101929950A CN 201010264675 CN201010264675 CN 201010264675 CN 201010264675 A CN201010264675 A CN 201010264675A CN 101929950 A CN101929950 A CN 101929950A
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sample
spectrum
preparation technology
glycolonitrile
monitoring
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冯红年
吴继明
叶华俊
陈英斌
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Focused Photonics Hangzhou Inc
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Focused Photonics Hangzhou Inc
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Abstract

The invention relates to a method for monitoring a glycolonitrile preparation technology process in real time, comprising the following steps: a. selecting a group of samples and collecting a spectrum, wherein the spectrum scanning range is 400-2500 nm; building an analysis model by utilizing the content of sample component and the corresponding spectrum; b. collecting the spectrum of an unknown sample in the glycolonitrile preparation process, and inputting the spectrum into the analysis model; and determining the content of the unknown sample component. The invention also provides a device for monitoring the glycolonitrile preparation technology in real time. The invention has the advantages of quickness, instantaneity, simple operation, no pollution, high analysis accuracy and the like.

Description

A kind of method and device that glycolonitrile preparation technology is monitored in real time
Technical field
The present invention relates to monitoring, especially a kind of method and device that glycolonitrile preparation technology is carried out real time on-line monitoring to glycolonitrile preparation technology.
Background technology
It is a kind of system that the hydroxyacetonitrile preparation process is monitored that hydroxyacetonitrile prepares the on-line analysis device.At present, the main means that the hydroxyacetonitrile preparation process is monitored are the content of formaldehyde that adopt in the manual assays method detection reaction process, with its Rule of judgment as reaction terminating.
Classic method can be monitored the hydroxyacetonitrile preparation process, but also has the following disadvantages:
1, length consuming time, analysis speed are slow
The reaction time of glycolonitrile preparation technology, lab assistant is analyzed 1 sample usually needed about 1 hour at 2-3 hour, parameters such as formaldehyde, hydroxyacetonitrile in the main analytical reactions process; Consuming time longer, analysis speed is slow, can't satisfy demands such as fast detecting such as production process control;
2, the analysis result human factor is big
The traditional analysis method adopts laboratory manual assays method, and it need be equipped with a plurality of lab analysis personnel, and can there be bigger difference in different analysts to the analysis result of sample;
3, not environmental protection
The traditional analysis process need adopts chemical reagent, has environmental pollution; Simultaneously, sample toxicity is big, the harm personal safety.
Summary of the invention
In order to solve above-mentioned deficiency of the prior art, the invention provides a kind of hydroxyacetonitrile real-time, simple to operate, pollution-free, with high accuracy fast and prepare on-line analysis method and device.
For achieving the above object, the present invention adopts following technical scheme:
A kind of method that glycolonitrile preparation technology is monitored in real time may further comprise the steps:
A, choose one group of sample and gather spectrum, the spectral scan scope is 400~2500nm;
Set up analytical model by content of sample component and corresponding with it spectrum;
B, gather the spectrum of unknown sample in the hydroxyacetonitrile preparation process and it is imported above-mentioned analytical model;
Determine the unknown sample component concentration.
As preferably, the characteristic absorption wave band of the sample of choosing when setting up analytical model is in following arbitrary spectrum district scope: 800~1000nm, 1300~1500nm, 1650~1750nm, 1900~2300nm.
As preferably, in sample pipe or after the sampling, sample is carried out pre-service, and gather pretreated sample spectra.
Further, described pre-treatment step comprises bubble and the solid impurity of removing in the sample.
As preferably, described pre-treatment step comprises carries out constant temperature and/or constant current is handled to sample.
As preferably, in step a,, again next sample is carried out same operation to simple sample collection spectrum and after analyzing its corresponding component concentration;
Or to behind all samples collection spectrum, the corresponding component concentration of each sample of unified Analysis.
Further, described component concentration is meant formaldehyde and/or hydroxyacetonitrile content.
As preferably, the component concentrations scope is set up different analytical models per sample; Collect the spectrum of unknown sample, qualitatively judge the unknown sample component concentration ranges earlier, select corresponding analytical model to calculate, obtain corresponding unknown sample components contents according to it.
Further, described qualitative judgement method is meant: the spectrum of sample in unknown sample spectrum and each concentration range is mated, select the good spectrum of matching degree, the component concentration ranges that it is corresponding is as the component concentration ranges of unknown sample correspondence.
The present invention also provides a kind of glycolonitrile preparation technology has been carried out real-time device for monitoring, comprising:
Light source, its spectral range are 300~2500nm;
Light receiving unit;
Processing module links to each other with light receiving unit, comprises the component concentration and the analytical model of the spectrum foundation of correspondence per sample with it.
Further, described device also comprises sampling unit that is installed on the sample pipe and the sample cell that links to each other with described sampling unit.
Further, described light source and light receiving unit are arranged on the two ends of sample pipe or sample cell.
As preferably, described device also comprises pretreatment unit, is arranged in the sample pipe or between sampling unit and the sample cell.
Further, described pretreatment unit comprises de-bubble module and filtering module, removes bubble and solid impurity in the sample.
As preferably, described pretreatment unit comprises constant temperature and/or constant flow module, is used to eliminate the influence to sample spectra of temperature and/or flow velocity.
The present invention compared with prior art has following beneficial effect:
1, weak point consuming time, analysis speed are fast
Need not to adopt chemical reagent that sample is analyzed, directly can obtain the information of unknown sample according to the spectrum of analytical model and unknown sample, the single polycomponent measurement of concetration time is less than 1 minute, weak point consuming time, analysis speed is fast, can satisfy demands such as fast detecting such as production process control;
2, pollution-free
Analytic process need not to consume chemical reagent, and the daily servicing expense is low; And the sample of analyzing enters hydroxyacetonitrile again and prepares in the pipeline, does not pollute the environment;
3, analyze data and be not subjected to man's activity
Can obtain the information of unknown sample according to the spectrum of analytical model and unknown sample, the centre does not have manual operation, can not introduce because the influence that artificial individual difference is brought analysis result, analyze data objective reliable, accuracy is high.
Description of drawings
Fig. 1 is the apparatus structure synoptic diagram among the embodiment 1;
Fig. 2 is the apparatus structure synoptic diagram among the embodiment 2;
Fig. 3 is the apparatus structure synoptic diagram when setting up analytical model among the embodiment 2;
Fig. 4 is the spectrogram of the sample that collects among the embodiment 2;
Fig. 5 is for carrying out the spectrum that obtains after the pre-service to the spectrum of Fig. 4 among the embodiment 2;
Fig. 6 is the apparatus structure synoptic diagram among the embodiment 3;
Fig. 7 is the apparatus structure synoptic diagram among the embodiment 4;
Fig. 8 is the apparatus structure synoptic diagram among the embodiment 5.
Embodiment
Embodiment 1
See also Fig. 1, a kind of glycolonitrile preparation technology carried out real-time device for monitoring, comprising: light source 51, light receiving unit 52 and processing module 53;
A pair of optical fiber is installed in the both sides of sample pipe 1 by ring flange, light source 51 and light receiving unit 52 link to each other with optical fiber wherein respectively, and two optical fiber in opposite directions and right, so that the transmission of the light that light source 51 sends process optical fiber sees through the sample in the sample pipe 1 later on, can be received by light receiving unit 52;
In the present embodiment, light source 51 is a halogen tungsten lamp, and spectral range is 300~2500nm; Light receiving unit 52 comprises light-splitting device and photoelectric commutator; Described light-splitting device is the grating beam splitting device;
The light that described light source 51 sends is by Optical Fiber Transmission one side to sample pipe 1, after seeing through the sample in the sample pipe 1, received by light-splitting device by another optical fiber relative again with above-mentioned optical fiber, photoelectric commutator will be converted to electric signal by the light signal that light-splitting device receives, give processing module 53 with this electrical signal transfer afterwards, processing module 53 is analyzed these electric signal, according to the analytical model that its inside embeds, analyzes the formaldehyde that obtains in the sample and/or the content of hydroxyacetonitrile.
Present embodiment also provides a kind of method that glycolonitrile preparation technology is monitored in real time, utilizes that present embodiment is described to carry out real-time device for monitoring to glycolonitrile preparation technology; May further comprise the steps:
A, set up analytical model, specifically may further comprise the steps:
A1, in the laboratory simulation glycolonitrile preparation technology, according to concrete operating mode situation, methyl alcohol and hydrogen cyanide are mixed with certain proportion, react, get a certain amount of course of reaction sample at regular intervals, gather its spectrum, and adopt chemical analysis method to analyze the content of formaldehyde and hydroxyacetonitrile, and with the content of formaldehyde, hydroxyacetonitrile as with sample spectra chemical score one to one; Wherein, sample number is 30 parts;
A2, set up analytical model:
Each the stage sample spectra that collects is carried out pre-service: pre-service such as the spectrum to sample carries out smoothly, differentiate, polynary scatter correction, standard normal variable conversion, remove redundant information to greatest extent and eliminate the spectrum deviation that various disturbing factors cause;
Choosing the characteristic absorption wave band of sample component, is 800~1000nm; Use Chemical Measurement software, from spectrum, extract data message, carry out the partial least square method analysis, set up the analytical model between formaldehyde, hydroxyacetonitrile content and the spectrum respectively in the mathematical operation mode;
B, determine the component concentration of unknown sample, concrete steps are as follows:
The light that b1, light source 51 send is by coupled Optical Fiber Transmission one side to sample pipe 1, see through the sample in the sample pipe 1, the Optical Fiber Transmission that the light that has a sample signal is connected with light-splitting device is to light-splitting device, photoelectric commutator will be converted to electric signal by the light signal that light-splitting device receives, and obtain sample spectra;
The unknown sample spectrum that collects is carried out pre-service, spectrum is carried out pretreated concrete operations with step a2;
B3, will input to the analytical model of setting up among the step a2 through pretreated unknown sample spectrum;
B4, choose the characteristic absorption wave band of unknown sample component, the characteristic absorption wave band of choosing when setting up analytical model among the step a2 is identical;
B5, by the calculating of analytical model, obtain the content of formaldehyde, hydroxyacetonitrile.
Embodiment 2
See also Fig. 2, Fig. 3, a kind of glycolonitrile preparation technology is carried out real-time device for monitoring, different with embodiment 1 described device is: described device also comprises pretreatment unit 3;
In the present embodiment, de-bubble module in the pretreatment unit 3 and filtering module are same parts screen pack, are arranged on the inside of sample pipe 1, are used for removing the bubble and the solid impurity of sample in the sample pipe 1;
Simultaneously, optical fiber to be installed in position on the sample pipe 1 near pretreatment unit 3 below correspondence position on the sample pipe 1, so that what gather is spectrum through the sample after pretreated;
The device of correspondence when setting up the analytical model in the processing module 53, than above-mentioned glycolonitrile preparation technology is carried out real-time device for monitoring, also comprise sampling unit 2, sampling unit 2 is arranged on the sample pipe 1, and its be arranged on the sample pipe 1 the position also near pretreatment unit 3 below relevant position on the sample pipe 1 be sample after handling through pretreatment unit 3 so that sampling unit 2 gathers;
After sampling unit 2 is obtained sample, with collection samples such as corresponding chemical reagent bottles, and the component concentration of employing chemical analysis method analytic sample.
Present embodiment also provides a kind of method that glycolonitrile preparation technology is monitored in real time, utilizes the device of correspondence when present embodiment is described to carry out real-time device for monitoring and set up model glycolonitrile preparation technology; May further comprise the steps:
A, set up analytical model, specifically may further comprise the steps:
A1, pretreatment unit 3 are removed bubble and the solid impurity in the sample in the sample pipe 1;
The spectrum of sample after a2, the collection pre-service:
The light that light source 51 sends is by coupled Optical Fiber Transmission one side to sample pipe 1, see through through pretreatment unit 3 pretreated samples, the Optical Fiber Transmission that the light that has a sample signal is connected with light-splitting device is to light-splitting device, photoelectric commutator will be converted to electric signal by the light signal that light-splitting device receives, and obtain sample spectra; Wherein, wavelength scanning range is at 1000~1800nm, and the spectrum of the sample that wherein collects is seen Fig. 4;
A3, collect sample and analyze corresponding content of sample component, as with sample spectra chemical score one to one:
Sample after 2 pairs of sampling units are handled through pretreatment unit 3 is sampled, and collects sample with corresponding chemical reagent bottle etc., with the above-mentioned formaldehyde of the sample to the reagent bottle, the content of hydroxyacetonitrile gathered of chemical analysis method analysis; And with the content of formaldehyde, hydroxyacetonitrile as with sample spectra chemical score one to one; Adopting the formaldehyde of the sample in the chemical analysis method analysis hydroxyacetonitrile preparation process, the content of hydroxyacetonitrile is the prior art of hydroxyacetonitrile preparation field, does not repeat them here;
Because sample has certain flow rate, simultaneously, optical fiber ring flange and sampling unit 2 are arranged on the sample pipe 1 near the position of pretreatment unit 3 belows, can be similar to think that the sample of taking a sample in sample that analyzed unit gathers spectrum and sampled unit 2 is same sample;
Be back to step a1 then, the sample in the sample pipe 1 is carried out pre-service, gathers spectrum and collection, behind corresponding formaldehyde, the hydroxyacetonitrile content, again next sample is carried out same operation in the sample that analysis is simultaneously collected;
The set of one group of 50 duplicate samples is formed in above-mentioned circulation step continued operation 50 times;
A4, set up analytical model:
The sample spectra of gathering among the step a2 is carried out pre-service: pre-service such as the spectrum to sample carries out smoothly, differentiate, polynary scatter correction, standard normal variable conversion, remove redundant information to greatest extent and eliminate the spectrum deviation that various disturbing factors cause; Spectrum to Fig. 4 correspondence is seen Fig. 5 through the later spectrum of mathematics pre-service;
Choosing the characteristic absorption wave band of sample component, is 1300~1500nm and 1650~1750nm; Use Chemical Measurement software, from spectrum, extract data message, carry out the partial least square method analysis, set up the analytical model between formaldehyde, hydroxyacetonitrile content and the spectrum respectively in the mathematical operation mode;
B, determine the component concentration of unknown sample, concrete steps are as follows:
B1, according to the method pre-service unknown sample of step a1;
B2, gather the spectrum of unknown sample according to the method for step a2; The unknown sample spectrum that collects is carried out pre-service, spectrum is carried out pretreated concrete operations with step a4;
B3, will input to the analytical model of setting up among the step a4 through pretreated unknown sample spectrum;
B4, choose the characteristic absorption wave band of unknown sample component, the characteristic absorption wave band of choosing when setting up analytical model among the step a4 is identical;
B5, by the calculating of analytical model, obtain the content of formaldehyde, hydroxyacetonitrile.
The formaldehyde of the analytical model working sample of setting up with present embodiment, hydroxyacetonitrile content are as predicted value, and the formaldehyde, hydroxyacetonitrile content that adopt the respective sample that chemical gauging collects simultaneously are as chemical score, both compare, and measurement result sees Table one.By the result as seen, the measurement result of two kinds of assay methods is very close, and deviate is smaller, shows that the inventive method has higher mensuration accuracy.
Table one
Figure BSA00000246444300081
Above-mentioned analytic process need not artificial participation, can not introduce the influence that analysis result is brought owing to artificial individual difference, and it is objective reliable to analyze data.
Embodiment 3
See also Fig. 6, a kind of glycolonitrile preparation technology is carried out real-time device for monitoring, what corresponding device was different when setting up analytical model with embodiment 2 is described is:
Described real-time device for monitoring also comprises sample cell 4; Sample cell 4 links to each other with sampling unit 2 by input port 41;
Described light source 51 and light receiving unit 52 are separately positioned on the two ends of sample cell 4, so that received by the light-splitting device in the light receiving unit 52 behind the sample in the light transmission sample cell 4 that light source 51 sends, photoelectric commutator in the light receiving unit 52 will be converted to electric signal by the light signal that light-splitting device receives, give processing module 53 with this electrical signal transfer afterwards, processing module 53 is analyzed this electric signal, according to the analytical model that its inside embeds, analyze the formaldehyde that obtains in the sample and/or the content of hydroxyacetonitrile;
When setting up the analytical model in the processing module 53, delivery outlet 42 collected specimens by sample cell 4 are also carried out chemical analysis and are calculated, and obtain the component concentration of respective sample;
The device of correspondence when present embodiment is set up analytical model is with above-mentioned that glycolonitrile preparation technology is carried out real-time device for monitoring is identical.
Present embodiment also provides a kind of method that glycolonitrile preparation technology is monitored in real time, with described in the embodiment 2 in real time the method for monitoring different be: corresponding device when utilizing the described real-time device for monitoring of present embodiment and setting up model;
In step a2, the sample after 2 pairs of processes of sampling unit pretreatment unit 3 is handled is sampled, and the sample that collects flows into sample cells 4 by input port 41;
Sample in the light transmission sample cell 4 that light source 51 sends, the light that has sample signal is received by light-splitting device, and photoelectric commutator will be converted to electric signal by the light signal that light-splitting device receives, and obtain sample spectra;
In step a3, collect sample from the output terminal 42 of sample cell 4;
After gathering the spectrum of 50 duplicate samples and collecting sample, the corresponding content of sample component of unified Analysis, as with sample spectra chemical score one to one;
Adopt chemical analysis method to analyze, obtain the corresponding component concentration of each sample.
Embodiment 4
See also Fig. 7, a kind of glycolonitrile preparation technology is carried out real-time device for monitoring, different with embodiment 3 described real-time device for monitoring is: pretreatment unit 30 is arranged on outside the sample pipe 1, links to each other with sample cell 4 with sampling unit 2 respectively; Described pretreatment unit 30 comprises de-bubble module 31 and filtering module 32; Wherein, de-bubble module 31 can be screen pack, also can be the fluid sample bubble trap; Filtering module 32 is a screen pack; In the present embodiment, the de-bubble module is a screen pack, and the filter screen aperture of filtering module 32 is less than the filter screen aperture of de-bubble module screen pack, so that further filter through the solid impurity in the sample after the de-bubble;
The device of correspondence when present embodiment is set up analytical model is with above-mentioned that glycolonitrile preparation technology is carried out real-time device for monitoring is identical.
Present embodiment also provides a kind of method that glycolonitrile preparation technology is monitored in real time, with described in the embodiment 3 in real time the method for monitoring different be: corresponding device when utilizing the described real-time device for monitoring of present embodiment and setting up model;
In step a1, the sample in 2 pairs of sample pipes of sampling unit 1 is taken a sample, and respective sample is fed pretreatment unit 30;
De-bubble module 31 in the pretreatment unit 30 and filtering module 32 are removed bubble and the solid impurity in the sample that obtains of sampling;
In step a2, flow into sample cells 4 by input port 41 through the sample after pretreatment unit 30 processing;
In step a4, when setting up analytical model, because the concentration range broad of sample component formaldehyde, hydroxyacetonitrile for improving online model analysis precision, is divided into two concentration ranges with it and sets up analytical model; Concentration range 1: formaldehyde is 150~350g/L, and hydroxyacetonitrile is 50~300g/L; Concentration range 2: formaldehyde is 5~150g/L, and hydroxyacetonitrile is 300~500g/L;
In step b, carry out pre-service and gather the spectrum step identical with present embodiment step a1 and a2 to unknown sample; According to the spectrum of unknown sample, qualitatively judge earlier the sample component concentration range, select the analytical model set up among corresponding step a4 according to it, thereby obtain the content of formaldehyde, hydroxyacetonitrile;
The step of judgement sample component concentration ranges is: the spectrum of sample in unknown sample spectrum and each concentration range is mated, calculate the mahalanobis distance between the spectrum, mahalanobis distance is little, illustrates that the matching degree between the spectrum is good, the similarity height; Select the good spectrum of matching degree, the component concentration ranges that it is corresponding is as the component concentration ranges of unknown sample correspondence.
With present embodiment per sample the analytical model set up respectively of concentration measure the formaldehyde, hydroxyacetonitrile content of unknown sample as predicted value, and the formaldehyde, hydroxyacetonitrile content that adopt the respective sample that chemical gauging collects simultaneously are as chemical score, both compare, and measurement result sees Table two.By the result as seen, the measurement result of two kinds of assay methods is very close, and deviate is smaller, shows that the inventive method has higher mensuration accuracy.The concentration difference is set up corresponding analytical model respectively per sample simultaneously, makes deviation littler, and is more accurate to the real-time monitoring of glycolonitrile preparation technology.
Table two
Figure BSA00000246444300111
Embodiment 5
See also Fig. 8, present embodiment also provides a kind of glycolonitrile preparation technology has been carried out real-time device for monitoring, and different with embodiment 4 described real-time device for monitoring is:
Pretreatment unit 30 also comprises thermostat module 33 and constant flow module 34, is used to eliminate the influence to sample spectra of temperature and flow velocity;
Wherein, de-bubble module 31 is the fluid sample bubble trap;
Thermostat module 33 comprises well heater/refrigerator, thermal detector, Temperature Feedback controller etc., is the prior art in temperature control field, does not repeat them here;
Constant flow module 34 comprises flowmeter, flow controller etc., is the prior art in flow control field, does not repeat them here;
The output terminal 42 of described sample cell 4 links to each other with sample pipe 1, is used for the sample in the sample cell 4 is entered in the sample pipe 1;
The constant temperature of sample is handled and can before sample cell 4 thermostat module be set, make the temperature of the sample that flow to sample cell 4 remain on uniform temperature; Or thermostat module is set directly on the sample cell, sample cell 4 is carried out constant temperature handle; Or de-bubble module 31, filtering module 32, constant flow module 34 and flow cell 4 put to a constant temperature oven, realize thermostatic control to overall flow paths; The constant temperature processing of present embodiment is a kind of mode wherein;
The device of correspondence when present embodiment is set up analytical model is with above-mentioned that glycolonitrile preparation technology is carried out real-time device for monitoring is identical.
Present embodiment also provides a kind of method that glycolonitrile preparation technology is monitored in real time, and different with the method for embodiment 4 described real-time monitorings is: corresponding device when utilizing the described real-time device for monitoring of present embodiment and setting up model;
In step a1, the sample that thermostat module 33 in the pretreatment unit 30 and constant flow module 34 obtain sampling respectively again carries out constant temperature and constant current is handled, to eliminate the influence to sample spectra of temperature and flow velocity;
In step a2 and b, gathered the spectrum of the sample in the sample cell 4 after, sample is entered in the sample pipe 1 by delivery outlet 42, free from environmental pollution, do not waste sample simultaneously;
In step a4, the characteristic absorption wave band of choosing sample component when setting up analytical model is 1900~2300nm;
In step b, carry out pre-service and gather the spectrum step identical with present embodiment step a1 and a2 to unknown sample; According to the spectrum of unknown sample, qualitatively judge the sample component concentration range earlier, select the analytical model of the foundation among the corresponding step a4 according to it, thereby obtain the content of formaldehyde, hydroxyacetonitrile.
Above-mentioned embodiment should not be construed as limiting the scope of the invention.Key of the present invention is: by setting up analytical model, the method that adopts near-infrared analysis is to hydroxyacetonitrile preparation realization on-line monitoring.Under the situation that does not break away from spirit of the present invention, any type of change that the present invention is made all should fall within protection scope of the present invention.

Claims (15)

1. method that glycolonitrile preparation technology is monitored in real time may further comprise the steps:
A, choose one group of sample and gather spectrum, the spectral scan scope is 400~2500nm;
Set up analytical model by content of sample component and corresponding with it spectrum;
B, gather the spectrum of unknown sample in the hydroxyacetonitrile preparation process and it is imported above-mentioned analytical model;
Determine the unknown sample component concentration.
2. the method that glycolonitrile preparation technology is monitored in real time according to claim 1 is characterized in that: the characteristic absorption wave band of the sample of choosing when setting up analytical model is in following arbitrary spectrum district scope: 800~1000nm, 1300~1500nm, 1650~1750nm, 1900~2300nm.
3. the method that glycolonitrile preparation technology is monitored in real time according to claim 1 is characterized in that: in sample pipe or after the sampling sample is carried out pre-service, and gather pretreated sample spectra.
4. the method that glycolonitrile preparation technology is monitored in real time according to claim 3 is characterized in that: described pre-treatment step comprises bubble and the solid impurity of removing in the sample.
5. according to claim 3 or the 4 described methods that glycolonitrile preparation technology is monitored in real time, it is characterized in that: described pre-treatment step comprises carries out constant temperature and/or constant current processing to sample.
6. the method that glycolonitrile preparation technology is monitored in real time according to claim 1 is characterized in that: in step a, to simple sample collection spectrum and after analyzing its corresponding component concentration, again next sample is carried out same operation;
Or to behind all samples collection spectrum, the corresponding component concentration of each sample of unified Analysis.
7. according to claim 1 or the 6 described methods that glycolonitrile preparation technology is monitored in real time, it is characterized in that: described component concentration is meant formaldehyde and/or hydroxyacetonitrile content.
8. the method that glycolonitrile preparation technology is monitored in real time according to claim 1 is characterized in that: component concentrations scope per sample, set up different analytical models; Collect the spectrum of unknown sample, qualitatively judge the unknown sample component concentration ranges earlier, select corresponding analytical model to calculate, obtain corresponding unknown sample components contents according to it.
9. the method that glycolonitrile preparation technology is monitored in real time according to claim 8, it is characterized in that: described qualitative judgement method is meant: the spectrum of sample in unknown sample spectrum and each concentration range is mated, select the good spectrum of matching degree, the component concentration ranges that it is corresponding is as the component concentration ranges of unknown sample correspondence.
10. one kind is carried out real-time device for monitoring to glycolonitrile preparation technology, comprising:
Light source, its spectral range are 300~2500nm;
Light receiving unit;
Processing module links to each other with light receiving unit, comprises the component concentration and the analytical model of the spectrum foundation of correspondence per sample with it.
11. according to claim 10 glycolonitrile preparation technology is carried out real-time device for monitoring, it is characterized in that: described device also comprises sampling unit that is installed on the sample pipe and the sample cell that links to each other with described sampling unit.
12. described glycolonitrile preparation technology is carried out real-time device for monitoring according to claim 10 or 11, it is characterized in that: described light source and light receiving unit are arranged on the two ends of sample pipe or sample cell.
13. according to claim 12 glycolonitrile preparation technology is carried out real-time device for monitoring, it is characterized in that: described device also comprises pretreatment unit, is arranged in the sample pipe or between sampling unit and the sample cell.
14. according to claim 13 glycolonitrile preparation technology is carried out real-time device for monitoring, it is characterized in that: described pretreatment unit comprises de-bubble module and filtering module, removes bubble and solid impurity in the sample.
15. described glycolonitrile preparation technology is carried out real-time device for monitoring according to claim 13 or 14, it is characterized in that: described pretreatment unit comprises constant temperature and/or constant flow module, is used to eliminate the influence to sample spectra of temperature and/or flow velocity.
CN 201010264675 2010-08-24 2010-08-24 Method and device for monitoring glycolonitrile preparation technology in real time Pending CN101929950A (en)

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Application publication date: 20101229