CN105784638A - Vinyl acetate rectified product purity online detection device, control device and detection method - Google Patents
Vinyl acetate rectified product purity online detection device, control device and detection method Download PDFInfo
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- CN105784638A CN105784638A CN201610008152.5A CN201610008152A CN105784638A CN 105784638 A CN105784638 A CN 105784638A CN 201610008152 A CN201610008152 A CN 201610008152A CN 105784638 A CN105784638 A CN 105784638A
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- vinylacetate
- inlet pipeline
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- rectification
- liquid bath
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- 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
- G01N21/41—Refractivity; Phase-affecting properties, e.g. optical path length
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/42—Regulation; Control
Abstract
The invention discloses a vinyl acetate rectified product purity online detection device, control device and detection method; the detection device comprises a liquid guiding tank and a refractive index instrument; the liquid guiding tank communicates with an inlet pipeline of a product liquid storage tank of a vinyl acetate tower top, a medium in the inlet pipeline is real-timely guided into the liquid guiding tank, a liquid level is built, and the medium real-timely flows back to the inlet pipeline from the liquid guiding tank; the refractive index instrument is arranged in the liquid guiding tank and is used for detecting the refractive index of the medium building the liquid level in the liquid guiding tank; the online detection structure is formed, and the purity of a vinyl acetate rectified product can be real-timely detected; with use of obtained purity parameters, process parameters in a rectification tower are timely adjusted, so as to ensure the purity of final products, enable the production to be stably carried out and improve the rate of qualified products; and moreover, the detection method is simple, simple calculation and treatment are achieved with use of a computer, the detection result can be obtained, real-time detection is achieved, and the timeliness of product quality control is ensured.
Description
Technical field
The present invention relates to a kind of detecting device for vinylacetate rectification product, utilize control device and the detection method of this detecting device.
Background technology
Vinylacetate is one of industrial chemicals of comparatively commonly using, current commercial production mainly adopts acetylene in gas phase method and ethylene vapor phase method, and to obtain the vinylacetate raw material refined, all need to adopt rectifying column to be easily separated purification, in distillation process, the purity of vinylacetate is the leading indicator controlled, and affects final product quality.In prior art, in the production process of vinylacetate, in order to ensure that final product purity can reach standard, the mode being generally adopted artificial timing sampling carries out detection to carry out quality control；Manual sampling detects, operate cumbersome, Monitoring Data is delayed, the state of arts in product quality and rectifying column can not be reflected in real time, the timely of technique can not be adjusted by operator according to the final purity of product, cause that substandard product flows into next process, and then make the whole instability that produces, reduction conforming product rate.
Therefore, need a kind of vinylacetate rectification On-line Product purity detecting device, the purity of vinylacetate rectification product can be detected in real time, foundation is provided for adjusting the technological parameter in rectifying column in time, thus ensureing the purity of final products, production can stably be carried out, improve conforming product rate.
Summary of the invention
In view of this, it is an object of the invention to provide a kind of vinylacetate rectification On-line Product purity detecting device, control device and detection method, the purity of vinylacetate rectification product can be detected in real time, utilize the purity parameter obtained, adjust the technological parameter in rectifying column in time, thus ensureing the purity of final products so that produce and can stably carry out, improve conforming product rate.
The vinylacetate rectification On-line Product purity detecting device of the present invention, including drawing liquid bath and index of refraction instrument, the described liquid bath that draws is communicated in vinylacetate overhead product reservoir inlet pipeline and medium in this inlet pipeline is introduced liquid bath in real time and sets up liquid level, and medium flows back to this inlet pipeline by drawing liquid bath in real time；Described index of refraction instrument is arranged at and draws liquid bath for detecting the index of refraction drawing the medium setting up liquid level in liquid bath.
Further, also including being arranged at the drainage plate that medium has in described inlet pipeline drainage, medium is drawn liquid bath by drawing the connected entrance of liquid bath and described inlet pipeline by described drainage plate；
Further, described drainage plate is positioned at the side relative with the connected entrance drawing liquid bath and described inlet pipeline and is perpendicular to described inlet pipeline centrage and arranges；
Further, described drainage plate is that semicircle and semicircular curved edge closes setting with described inlet pipeline, and described drainage plate radius is not less than 1/2nd of described inlet pipeline internal diameter；
Further, liquid bath is drawn described in concordant with drawing liquid bath bottom land with the lower limb of the connected entrance of described inlet pipeline；
Further, the probe of described index of refraction instrument from top to bottom stretches into and draws liquid bath, 1/2nd places between probe and the bottom land drawing liquid bath of the positive doubling refractoscope of described drainage plate.
The invention also discloses a kind of automaton utilizing vinylacetate rectification On-line Product purity detecting device, including:
Detection unit, for vinylacetate rectification On-line Product purity detecting device；
Control unit, for receiving the detection vinylacetate rectification product index of refraction that transmits of unit and obtaining purity data；
Performance element, the control command of reception control unit, and according to control command, vinylacetate is delivered to overhead product reservoir, partly or entirely returns rectifying column and continue rectification.
Further, described performance element includes:
Overhead product reservoir inlet pipeline electrically-controlled valve, for opening and closing or adjust the medium of overhead product reservoir inlet pipeline；
Condenser reflux pipeline electrically-controlled valve, for opening and closing or adjust the medium being back to rectifying column rectification again by condenser media outlet.
The invention also discloses a kind of detection method utilizing described vinylacetate rectification On-line Product purity detecting device, comprise the following steps:
A. the index of refraction of vinylacetate medium in overhead product reservoir inlet pipeline is obtained；
B. the purity parameter of described vinylacetate medium is obtained according to the index of refraction of step a.
Further, in step b, according to formula C=2608.568nD-3531.555, obtain the purity parameter of described vinylacetate medium；In formula: C is vinyl acetate concentrations, nDFor medium index of refraction；
In step a, described index of refraction is corrected to the index of refraction of a standard temperature.
Beneficial effects of the present invention: the vinylacetate rectification On-line Product purity detecting device of the present invention, control device and detection method, adopt and the device detecting vinylacetate purity in real time is set on overhead product reservoir inlet pipeline, and form on-line checking structure, the purity of vinylacetate rectification product can be detected in real time, utilize the purity parameter obtained, adjust the technological parameter in rectifying column in time, thus ensureing the purity of final products, production can stably be carried out, improve conforming product rate；Further, detection method is simple, utilizes computer to realize simple calculating and process can obtain testing result, detect in real time, it is ensured that the promptness to control of product quality.
Accompanying drawing explanation
Below in conjunction with drawings and Examples, the invention will be further described.
Fig. 1 is the control device application schematic diagram of the present invention；
Fig. 2 is the structure of the detecting device schematic diagram of the present invention.
Detailed description of the invention
The vinylacetate rectification On-line Product purity detecting device of the present invention, including drawing liquid bath 10 and index of refraction instrument 9, the described liquid bath that draws is communicated in vinylacetate overhead product reservoir 7 inlet pipeline and is drawn liquid bath 7 and set up liquid level in real time by medium (vinylacetate) in this inlet pipeline 8, and medium flows back to this inlet pipeline by drawing liquid bath 10 in real time；Described index of refraction instrument is arranged at and draws liquid bath for detecting the index of refraction drawing the medium setting up liquid level in liquid bath；The vinylacetate index of refraction of different purity is also different, and has linear corresponding relation；In the present invention, in inlet pipeline, medium introduces liquid bath 10 in real time and sets up liquid level, while setting up liquid level, this medium flows back to this inlet pipeline by drawing liquid bath in real time, ensure the medium real-time update drawing in liquid bath 10, consistent with the medium in inlet pipeline 8, it is to avoid to deposit and affect testing result；Vinylacetate overhead product reservoir 7 inlet pipeline, for being vertically arranged, so that vinylacetate can flow into overhead product reservoir by gravity, does not repeat them here.
As shown in the figure: the vinylacetate material liquid in raw material reservoir 1 is delivered to rectifying column 3 by dosing pump 2, medium (material liquid) in rectifying column heats through tower reactor heater 4, vinylacetate steam enters condenser 5, condensed vinylacetate enters overhead product reservoir 7 by inlet pipeline 8, media fluid after separation at the bottom of tower enters tower reactor product reservoir, for existing distillation system structure, do not repeat them here.
In the present embodiment, also including being arranged at the drainage plate 11 that medium has in described inlet pipeline drainage, medium is drawn liquid bath 10 by drawing the connected entrance of liquid bath 10 and described inlet pipeline 8 by described drainage plate；Owing in inlet pipeline 8, medium flows downward, draw and in liquid bath 10, not easily set up liquid level, utilize drainage plate 11 to guide medium to drawing liquid bath, form stable liquid level, it is ensured that index of refraction instrument can the index of refraction of Real-time Collection medium, it is ensured that online real-time.
In the present embodiment, described drainage plate 11 is positioned at the side relative with the connected entrance of described inlet pipeline 8 with drawing liquid bath 10 and is perpendicular to the setting of described inlet pipeline centrage；Medium stream to drainage plate after, inlet pipeline 8 can be back to again after being fully drained to liquid bath 10, be beneficial to foundation stablize liquid level.
In the present embodiment, described drainage plate 11 is that semicircle and semicircular curved edge closes setting with described inlet pipeline 8, described drainage plate 11 radius is not less than 1/2nd of described inlet pipeline internal diameter, the present embodiment selects drainage plate radius to be 1/2nd of described inlet pipeline internal diameter, namely form the closing that inlet pipeline is half of, enable media to substantially stabilized entrance and draw liquid bath 10, and liquid level is stablized in formation, there is not bigger disturbance, thus ensureing that final testing result is accurate.
In the present embodiment, described in draw liquid bath 10 concordant with drawing liquid bath 10 bottom land with the lower limb of the connected entrance of described inlet pipeline 8；It is beneficial to enter and draws the medium of liquid bath 10 and flow out in time, enter vacating space for follow-up medium, it is ensured that real-time.
In the present embodiment, the probe of described index of refraction instrument 9 from top to bottom stretches into and draws liquid bath 10, / 2nd places between probe and the bottom land drawing liquid bath of the described positive doubling refractoscope of drainage plate 11, utilize the drainage plate pile up effect to medium, ensure that the probe of index of refraction instrument 9 can fully detect data, and the obstruction that normal stream is logical will not be formed.
The invention also discloses a kind of automaton utilizing vinylacetate rectification On-line Product purity detecting device, including:
Detection unit, for vinylacetate rectification On-line Product purity detecting device；
Control unit, for receiving the detection vinylacetate rectification product index of refraction that transmits of unit and obtaining purity data；Store the program by index of refraction calculated purity data in control unit, obtain purity figure according to the index of refraction recorded；
Performance element, the control command of reception control unit, and according to control command, vinylacetate is delivered to overhead product reservoir, partly or entirely returns rectifying column and continue rectification；When purity reaches the standard set, performance element will all open inlet pipeline, and medium is all sent into overhead product reservoir；When purity differs bigger with the standard of setting, close inlet pipeline, open reflux pipe 14 and medium is transmitted back to rectifying column continuation rectification；If purity differs less with the standard of setting, the aperture of adjustable mouth pipeline and the aperture of reflux pipe, partial reflux is rectification again；The standard set and the aperture of inlet pipeline and the aperture of reflux pipe are set as required and adjust, and utilize the program first set to realize, do not repeat them here.
In the present embodiment, described performance element includes:
Overhead product reservoir inlet pipeline electrically-controlled valve 12, for opening and closing or adjust the medium of overhead product reservoir inlet pipeline；
Condenser reflux pipeline electrically-controlled valve 13, for opening and closing or adjust the medium being back to rectifying column rectification again by condenser media outlet.
The invention also discloses a kind of detection method utilizing described vinylacetate rectification On-line Product purity detecting device, comprise the following steps:
A. the index of refraction of vinylacetate medium in overhead product reservoir inlet pipeline is obtained；
B. the purity parameter of described vinylacetate medium is obtained according to the index of refraction of step a.
In the present embodiment, in step b, according to formula C=2608.568nD-3531.555, obtain the purity parameter of described vinylacetate medium；In formula: C is vinyl acetate concentrations, nD is medium index of refraction；
The detection method realizing vinylacetate rectification On-line Product purity is: be respectively configured the vinyl acetate solution that purity is 40%, 60%, 80%, 90%, 95%, 97%, 99%, 99.5%, 100%, tests its index of refraction at 20 DEG C, and result is in Table 1.
Table 1 vinyl acetate purity and index of refraction test result
| Purity/% | 40 | 60 | 80 | 90 | 95 | 97 | 99 | 99.5 | 100 |
| Index of refraction | 1.3694 | 1.3770 | 1.3840 | 1.3876 | 1.3900 | 1.3913 | 1.3918 | 1.3922 | 1.3927 |
The relation curve of index of refraction and concentration is made according to table 1 data, obtain fit equation: C=2608.568nD-3531.555, correlation coefficient reaches 0.9972, in being embodied as, with required by technology controlling and process set Reinheitszahl as control desired value, by computing, control of purity value being converted into index of refraction, the difference for target index of refraction and index of refraction detected value realizes the judgement to rectifying column product purity and control.
In step a, described index of refraction is corrected to the index of refraction of a standard temperature, and the present embodiment standard temperature is 20 DEG C.The index of refraction of different temperatures can be corrected into the index of refraction of standard temperature by existing index of refraction instrument, if the relation curve of temperature and index of refraction usually set up by manual synchronizing, is obtained by Equation for Calculating, does not repeat them here.
What finally illustrate is, above example is only in order to illustrate technical scheme and unrestricted, although the present invention being described in detail with reference to preferred embodiment, it will be understood by those within the art that, technical scheme can be modified or equivalent replacement, without deviating from objective and the scope of technical solution of the present invention, it all should be encompassed in the middle of scope of the presently claimed invention.
Claims (10)
1. a vinylacetate rectification On-line Product purity detecting device, it is characterized in that: include drawing liquid bath and index of refraction instrument, the described liquid bath that draws is communicated in vinylacetate overhead product reservoir inlet pipeline and medium in this inlet pipeline is introduced liquid bath in real time and sets up liquid level, and medium flows back to this inlet pipeline by drawing liquid bath in real time；Described index of refraction instrument is arranged at and draws liquid bath for detecting the index of refraction drawing the medium setting up liquid level in liquid bath.
2. vinylacetate rectification On-line Product purity detecting device according to claim 1, it is characterized in that: also include being arranged at the drainage plate that medium has in described inlet pipeline drainage, medium is drawn liquid bath by drawing the connected entrance of liquid bath and described inlet pipeline by described drainage plate.
3. vinylacetate rectification On-line Product purity detecting device according to claim 2, it is characterised in that: described drainage plate is positioned at the side relative with the connected entrance of described inlet pipeline with drawing liquid bath and is perpendicular to the setting of described inlet pipeline centrage.
4. vinylacetate rectification On-line Product purity detecting device according to claim 2, it is characterized in that: described drainage plate is that semicircle and semicircular curved edge closes setting with described inlet pipeline, and described drainage plate radius is not less than 1/2nd of described inlet pipeline internal diameter.
5. vinylacetate rectification On-line Product purity detecting device according to claim 2, it is characterised in that: described in draw liquid bath concordant with drawing liquid bath bottom land with the lower limb of the connected entrance of described inlet pipeline.
6. vinylacetate rectification On-line Product purity detecting device according to claim 5, it is characterized in that: the probe of described index of refraction instrument from top to bottom stretches into and draws liquid bath, 1/2nd places between probe and the bottom land drawing liquid bath of the positive doubling refractoscope of described drainage plate.
7. the automaton utilizing vinylacetate rectification On-line Product purity detecting device, it is characterised in that: including:
Detection unit, for claim 1-6 arbitrary vinylacetate rectification On-line Product purity detecting device；
Control unit, for receiving the detection vinylacetate rectification product index of refraction that transmits of unit and obtaining purity data；
Performance element, the control command of reception control unit, and according to control command, vinylacetate is delivered to overhead product reservoir, partly or entirely returns rectifying column and continue rectification.
8. automaton according to claim 7, it is characterised in that: described performance element includes:
Overhead product reservoir inlet pipeline electrically-controlled valve, for opening and closing or adjust the medium of overhead product reservoir inlet pipeline；
Condenser reflux pipeline electrically-controlled valve, for opening and closing or adjust the medium being back to rectifying column rectification again by condenser media outlet.
9. the detection method of the vinylacetate rectification On-line Product purity detecting device that a kind utilizes described in claim 1-6, it is characterised in that: comprise the following steps:
A. the index of refraction of vinylacetate medium in overhead product reservoir inlet pipeline is obtained；
B. the purity parameter of described vinylacetate medium is obtained according to the index of refraction of step a.
10. detection method according to claim 9, it is characterised in that: in step b, according to formula C=2608.568nD-3531.555, obtain the purity parameter of described vinylacetate medium；In formula: C is vinyl acetate concentrations, nDFor medium index of refraction；
In step a, described index of refraction is corrected to the index of refraction of a standard temperature.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610008152.5A CN105784638B (en) | 2016-01-07 | 2016-01-07 | Vinylacetate rectifying On-line Product purity detecting device, control device and detection method |
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| CN201610008152.5A CN105784638B (en) | 2016-01-07 | 2016-01-07 | Vinylacetate rectifying On-line Product purity detecting device, control device and detection method |
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| CN105784638B CN105784638B (en) | 2019-04-16 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107677642A (en) * | 2017-09-20 | 2018-02-09 | 宁波市鄞州赛弗兑食品科技有限公司 | A kind of refractometer |
| CN107677643A (en) * | 2017-09-20 | 2018-02-09 | 宁波市鄞州赛弗兑食品科技有限公司 | A kind of hand-hold refractometer |
| CN113231118A (en) * | 2021-05-10 | 2021-08-10 | 海南医学院 | Fractionating device for organic chemistry experiment |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107677642A (en) * | 2017-09-20 | 2018-02-09 | 宁波市鄞州赛弗兑食品科技有限公司 | A kind of refractometer |
| CN107677643A (en) * | 2017-09-20 | 2018-02-09 | 宁波市鄞州赛弗兑食品科技有限公司 | A kind of hand-hold refractometer |
| CN113231118A (en) * | 2021-05-10 | 2021-08-10 | 海南医学院 | Fractionating device for organic chemistry experiment |
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