CN108663338A - The method for monitoring polymer polyatomic alcohol product quality on-line - Google Patents
The method for monitoring polymer polyatomic alcohol product quality on-line Download PDFInfo
- Publication number
- CN108663338A CN108663338A CN201810437598.9A CN201810437598A CN108663338A CN 108663338 A CN108663338 A CN 108663338A CN 201810437598 A CN201810437598 A CN 201810437598A CN 108663338 A CN108663338 A CN 108663338A
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- China
- Prior art keywords
- sample
- polyatomic alcohol
- polymer polyatomic
- near infrared
- product quality
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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- 229920000642 polymer Polymers 0.000 title claims abstract description 36
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 31
- 238000012544 monitoring process Methods 0.000 title claims abstract description 23
- 239000000523 sample Substances 0.000 claims abstract description 60
- 238000001228 spectrum Methods 0.000 claims abstract description 21
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 6
- 238000005259 measurement Methods 0.000 claims abstract description 6
- 239000000126 substance Substances 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 4
- 238000004458 analytical method Methods 0.000 claims description 8
- 238000002329 infrared spectrum Methods 0.000 claims description 6
- 238000012795 verification Methods 0.000 claims description 6
- 230000004927 fusion Effects 0.000 claims description 4
- 238000000513 principal component analysis Methods 0.000 claims description 4
- 238000012937 correction Methods 0.000 claims description 3
- 238000012417 linear regression Methods 0.000 claims description 3
- 238000010606 normalization Methods 0.000 claims description 3
- 238000005516 engineering process Methods 0.000 abstract description 8
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 229920002635 polyurethane Polymers 0.000 abstract description 2
- 239000004814 polyurethane Substances 0.000 abstract description 2
- 238000002203 pretreatment Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000001514 detection method Methods 0.000 description 4
- 229920000570 polyether Polymers 0.000 description 3
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000004721 Polyphenylene oxide Substances 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- 210000004556 brain Anatomy 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229920005862 polyol Polymers 0.000 description 2
- 150000003077 polyols Chemical class 0.000 description 2
- 229920005830 Polyurethane Foam Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000010559 graft polymerization reaction Methods 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 239000011496 polyurethane foam Substances 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/359—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using near infrared light
Landscapes
- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The invention belongs to petrochemical industry polyurethanes technology fields, and in particular to a method of on-line monitoring polymer polyatomic alcohol product quality.The method of the on-line monitoring polymer polyatomic alcohol product quality, binding molecule spectrum, physicochemical data and Chemical Measurement establish the model of each key technical index, and polymer polyatomic alcohol product quality is monitored on-line by fibre-optical probe；Wherein, molecular spectrum is acquired using Fourier Transform Near Infrared instrument, and key technical index is：Hydroxyl value, viscosity and solid content, physicochemical data obtain by polymer polyatomic alcohol national standard detects.The present invention is not necessarily to sample pre-treatments, have the characteristics that not destroy fast sample, analyze speed, non-environmental-pollution, can implement to monitor technical target of the product on-line, sample molecule spectrum is acquired using Fourier Transform Near Infrared instrument, can show the key technical index of institute's established model simultaneously.
Description
Technical field
The invention belongs to petrochemical industry polyurethanes technology fields, and in particular to a kind of on-line monitoring polymer polyatomic alcohol product
The method of quality.
Background technology
It is basic polyethers that polymer polyatomic alcohol (POP), which is with soft bubble or high activity polyether, adds acrylonitrile, styrene and initiation
Agent etc. carries out the co-mixing system of copolymer or autopolymer made of free yl graft polymerization under 100 DEG C or so, nitrogen protection,
It is the particle dispersion system for the stabilization that micrograde polymer particle is formed in polyether polyol.Polymer polyatomic alcohol be molding and
One of important source material of slabstock polyurethane foam.The key technical index of polymer polyatomic alcohol has hydroxyl value, viscosity, contains admittedly
Amount, free styrene-content and acrylonitrile content etc..
To improve production efficiency, production cost is reduced, ensures product quality, develops new detection method, shortens detection week
Phase, while the key technical index for implementing to monitor on-line polymer polyatomic alcohol is very necessary and urgent.
The analytical technology Indexs measure of polymer polyatomic alcohol is longer using national standard detection time, cannot evaluate production in time
Quality causes technique to wait for sometimes, and needs to use poisonous and harmful chemical reagent when detection hydroxyl value, has to human body and environment
Damage.
Invention content
In view of the deficiencies of the prior art, the object of the present invention is to provide a kind of on-line monitoring polymer polyatomic alcohol product qualities
Method, be not necessarily to sample pre-treatments, have and do not destroy sample, analyze speed fast, non-environmental-pollution, on-line monitoring production can be implemented
The characteristics of product technical indicator, acquires a sample molecule spectrum using Fourier Transform Near Infrared instrument, can show simultaneously
The key technical index of institute's established model.
The method of on-line monitoring polymer polyatomic alcohol product quality of the present invention, binding molecule spectrum, physicochemical data
The model that each key technical index is established with Chemical Measurement monitors polymer polyatomic alcohol on-line by fibre-optical probe, online to divide
Division quality；Wherein, molecular spectrum is acquired using Fourier Transform Near Infrared instrument, and key technical index is：Hydroxyl value is glued
Degree and solid content, physicochemical data are obtained using national standard analysis.
The fibre-optical probe is diffusing reflection fibre-optical probe.
The method of the on-line monitoring polymer polyatomic alcohol product quality, is as follows：
1. collecting sample：
2. collecting the physicochemical data of sample, the theoretical value of model sample is established；
3. acquiring the molecular spectrum of collected sample by Fourier Transform Near Infrared instrument：
3.1 instrument：
Fourier Transform Near Infrared instrument, fibre-optical probe；
3.2 Fourier Transform Near Infrared instrument acquisition conditions：
Resolution ratio：8cm-1Or 16cm-1；
3.3 scan sample using Fourier Transform Near Infrared instrument, collect the molecular spectrum of sample；
4. binding molecule spectrum, physicochemical data and Chemical Measurement establish model：
The near infrared spectrum of sample is imported Fourier Transform Near Infrared instrument by 4.1 with corresponding sample physicochemical data
Software or Unscrambler softwares；
4.2 pairs of molecular spectrums pre-process, and fusion chemometrics method optimizes and establishes model：
Pretreatment mode is to be filtered, eliminate constant offset, first derivative, second dervative, vector normalization or more
One or more of first scatter correction；
Chemometrics method is one or more of offset minimum binary, principal component analysis or multiple linear regression；
4.3 carry out model verification (ensureing that model predication value is accurate and reliable) using verification sample collection, obtain model；
5. monitoring polymer polyatomic alcohol product quality on-line：
Fibre-optical probe is installed into process units, sweep parameter is set according to step 3.2, selects the corresponding pass established
The model of key technology index, Fourier Transform Near Infrared instrument is according to set Parameter analysis sample, in instrument software and DCS electricity
Result and real-time curve are shown on brain.
Wherein：
Collect sample requirement be：The variation range of the physicochemical data of polymer polyatomic alcohol sample should be able to cover sample to be tested
Actual change range.
The physicochemical data of sample is obtained using the national standard analysis of polymer polyatomic alcohol.
The scanning range of Fourier Transform Near Infrared instrument scans for gamut.
Compared with prior art, beneficial effects of the present invention are as follows：
1, near-infrared spectrum technique of the present invention is using part or full wave molecular spectrum fusion physicochemical data and chemistry
Meterological is modeled, and is a kind of green analytical technology, has that analyze speed is fast, does not need sample preprocessing, may be implemented in line
The advantages that monitoring technical target of the product.
2, quick, the real-time measuring data that near infrared spectrum on-line monitoring key technical index is provided can make polymer more
First alcohol production process keeps optimal control, while improving product quality, reduces production cost and energy consumption.
3, this method may extend to the monitoring of polymer polyatomic alcohol other technologies index.
4, this method may extend to the on-line monitoring of other polyol product quality.
Description of the drawings
Fig. 1 is the hydroxyl value model that embodiment 1 is established；
Fig. 2 is the Viscosity Model that embodiment 1 is established；
Fig. 3 is the solid content model that embodiment 1 is established；
Fig. 4 is the model proof diagram of embodiment 1.
Specific implementation mode
With reference to specific embodiment, the present invention is further elaborated, but the present invention is not limited to following embodiments.
Embodiment 1
The method of the on-line monitoring polymer polyatomic alcohol product quality, is as follows：
1. collecting sample：
The variation range of the physicochemical data of polymer polyatomic alcohol sample should be able to cover the actual change range of sample to be tested.
2. collecting the physicochemical data of sample using the national standard analysis of polymer polyatomic alcohol, the theory of model sample is established
Value；
3. acquiring the molecular spectrum of collected sample by Fourier Transform Near Infrared instrument：
3.1 instrument：
Fourier Transform Near Infrared instrument, diffusing reflection fibre-optical probe；
3.2 Fourier Transform Near Infrared instrument acquisition conditions：
Resolution ratio：8cm-1Or 16cm-1, scanning range：Gamut scans；
3.3 scan sample using Fourier Transform Near Infrared instrument, collect the molecular spectrum of sample；
4. binding molecule spectrum, physicochemical data and Chemical Measurement establish model：
The near infrared spectrum of sample is imported Fourier Transform Near Infrared instrument by 4.1 with corresponding sample physicochemical data
Software or Unscrambler softwares；
4.2 pairs of molecular spectrums pre-process, and fusion chemometrics method optimizes and establishes model：
Pretreatment mode is to be filtered, eliminate constant offset, first derivative, second dervative, vector normalization or more
One or more of first scatter correction；
Chemometrics method is in offset minimum binary (PLS), principal component analysis (PCA) or multiple linear regression (MLR)
One or more；
The model for each key technical index established is shown in attached drawing 1-3 respectively；
4.3 carry out model verification (ensureing that model predication value is accurate and reliable) using verification sample collection, obtain model；
Model proof diagram is shown in attached drawing 4；
5. monitoring polymer polyatomic alcohol product quality on-line：
Fibre-optical probe is installed into process units, sweep parameter is set according to step 3.2, selects the corresponding pass established
The model of key technology index, Fourier Transform Near Infrared instrument is according to set Parameter analysis sample, in instrument software and DCS electricity
Result and real-time curve are shown on brain.
Claims (6)
1. a kind of method of on-line monitoring polymer polyatomic alcohol product quality, it is characterised in that：Binding molecule spectrum, physicochemical data
The model that each key technical index is established with Chemical Measurement monitors polymer polyatomic alcohol on-line by fibre-optical probe, online to divide
Division quality；Wherein, molecular spectrum is acquired using Fourier Transform Near Infrared instrument, and key technical index is：Hydroxyl value is glued
Degree and solid content, physicochemical data are obtained using national standard analysis.
2. the method for on-line monitoring polymer polyatomic alcohol product quality according to claim 1, it is characterised in that：Described
Fibre-optical probe is diffusing reflection fibre-optical probe.
3. the method for on-line monitoring polymer polyatomic alcohol product quality according to claim 1, it is characterised in that：Specific step
It is rapid as follows：
1. collecting sample：
2. collecting the physicochemical data of sample, the theoretical value of model sample is established；
3. acquiring the molecular spectrum of collected sample by Fourier Transform Near Infrared instrument：
3.1 instrument：
Fourier Transform Near Infrared instrument, fibre-optical probe；
3.2 Fourier Transform Near Infrared instrument acquisition conditions：
Resolution ratio：8cm-1Or 16cm-1；
3.3 scan sample using Fourier Transform Near Infrared instrument, collect the molecular spectrum of sample；
4. binding molecule spectrum, physicochemical data and Chemical Measurement establish model：
The near infrared spectrum of sample is imported Fourier Transform Near Infrared instrument software by 4.1 with corresponding sample physicochemical data
Or Unscrambler softwares；
4.2 pairs of molecular spectrums pre-process, and fusion chemometrics method optimizes and establishes model：
Pretreatment mode is to be filtered, eliminate constant offset, first derivative, second dervative, vector normalization or polynary scattered
Penetrate one or more of correction；
Chemometrics method is one or more of offset minimum binary, principal component analysis or multiple linear regression；
4.3 carry out model verification using verification sample collection, obtain model；
5. monitoring polymer polyatomic alcohol product quality on-line：
Fibre-optical probe is installed into process units, sweep parameter is set according to step 3.2, selects the corresponding crucial skill established
The model of art index, Fourier Transform Near Infrared instrument is according to set Parameter analysis sample, on instrument software and DCS computers
Show result and real-time curve.
4. the method for on-line monitoring polymer polyatomic alcohol product quality according to claim 3, it is characterised in that：Collect sample
The requirement of product is：The variation range of the physicochemical data of polymer polyatomic alcohol sample should be able to cover the actual change model of sample to be tested
It encloses.
5. the method for on-line monitoring polymer polyatomic alcohol product quality according to claim 3, it is characterised in that：Sample
Physicochemical data is obtained using the national standard analysis of polymer polyatomic alcohol.
6. the method for on-line monitoring polymer polyatomic alcohol product quality according to claim 3, it is characterised in that：Fourier
The scanning range of transform near infrared spectrum instrument scans for gamut.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810437598.9A CN108663338A (en) | 2018-05-09 | 2018-05-09 | The method for monitoring polymer polyatomic alcohol product quality on-line |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810437598.9A CN108663338A (en) | 2018-05-09 | 2018-05-09 | The method for monitoring polymer polyatomic alcohol product quality on-line |
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| Publication Number | Publication Date |
|---|---|
| CN108663338A true CN108663338A (en) | 2018-10-16 |
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| CN201810437598.9A Pending CN108663338A (en) | 2018-05-09 | 2018-05-09 | The method for monitoring polymer polyatomic alcohol product quality on-line |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040084623A1 (en) * | 2002-11-06 | 2004-05-06 | Yicheng Long | NIR spectroscopy method for analyzing chemical process components |
| CN102393378A (en) * | 2011-11-01 | 2012-03-28 | 湖南省湘维有限公司 | Method for rapidly detecting alcoholysis degree and polymerization degree in production of polyvinyl alcohol by utilizing near infrared spectrum technology |
| CN102566533A (en) * | 2011-11-25 | 2012-07-11 | 福建中烟工业有限责任公司 | On-line monitoring device and method for preparing tobacco essence perfume |
| CN103439269A (en) * | 2013-09-06 | 2013-12-11 | 安徽古井贡酒股份有限公司 | Method for quickly detecting physicochemical indexes in fermented grains by near infrared |
| CN104132720A (en) * | 2014-07-25 | 2014-11-05 | 重庆医科大学 | Method for quickly detecting tablet weight of medicine tablets through near infrared spectroscopy |
| CN105548064A (en) * | 2015-12-15 | 2016-05-04 | 驻马店华中正大有限公司 | Method for determination of multiple nutrient compositions and antibiotic titer changes by using near infrared spectroscopy during production process of antibiotics from microbial fermentation |
| CN106353280A (en) * | 2015-07-15 | 2017-01-25 | 重庆医科大学 | Quick near infrared spectrum identification method of venlafaxine crystal |
-
2018
- 2018-05-09 CN CN201810437598.9A patent/CN108663338A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040084623A1 (en) * | 2002-11-06 | 2004-05-06 | Yicheng Long | NIR spectroscopy method for analyzing chemical process components |
| CN102393378A (en) * | 2011-11-01 | 2012-03-28 | 湖南省湘维有限公司 | Method for rapidly detecting alcoholysis degree and polymerization degree in production of polyvinyl alcohol by utilizing near infrared spectrum technology |
| CN102566533A (en) * | 2011-11-25 | 2012-07-11 | 福建中烟工业有限责任公司 | On-line monitoring device and method for preparing tobacco essence perfume |
| CN103439269A (en) * | 2013-09-06 | 2013-12-11 | 安徽古井贡酒股份有限公司 | Method for quickly detecting physicochemical indexes in fermented grains by near infrared |
| CN104132720A (en) * | 2014-07-25 | 2014-11-05 | 重庆医科大学 | Method for quickly detecting tablet weight of medicine tablets through near infrared spectroscopy |
| CN106353280A (en) * | 2015-07-15 | 2017-01-25 | 重庆医科大学 | Quick near infrared spectrum identification method of venlafaxine crystal |
| CN105548064A (en) * | 2015-12-15 | 2016-05-04 | 驻马店华中正大有限公司 | Method for determination of multiple nutrient compositions and antibiotic titer changes by using near infrared spectroscopy during production process of antibiotics from microbial fermentation |
Non-Patent Citations (1)
| Title |
|---|
| 上海高桥石油化工公司: "《石化企业的技术应用及管理》", 30 November 2003, 华东理工大学出版社 * |
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Application publication date: 20181016 |