CN105784638B - Vinylacetate rectifying On-line Product purity detecting device, control device and detection method - Google Patents
Vinylacetate rectifying On-line Product purity detecting device, control device and detection method Download PDFInfo
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- CN105784638B CN105784638B CN201610008152.5A CN201610008152A CN105784638B CN 105784638 B CN105784638 B CN 105784638B CN 201610008152 A CN201610008152 A CN 201610008152A CN 105784638 B CN105784638 B CN 105784638B
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- vinylacetate
- liquid bath
- rectifying
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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
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- General Health & Medical Sciences (AREA)
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The invention discloses a kind of vinylacetate rectifying On-line Product purity detecting device, control device and detection methods, detection device includes drawing liquid bath and index of refraction instrument, draw liquid bath and be connected to vinylacetate overhead product reservoir inlet pipeline and medium in the inlet pipeline is drawn into liquid bath in real time and establishes liquid level, and medium flows back to the inlet pipeline by drawing liquid bath in real time；Index of refraction instrument, which is set to, draws liquid bath for detecting the index of refraction for drawing the medium for establishing liquid level in liquid bath；The present invention forms online detection structure, is capable of the purity of real-time detection vinylacetate rectifying product, utilizes purity parameter obtained, technological parameter in adjustment rectifying column in time, to guarantee the purity of final products, so that production can stablize progress, product qualification rate is improved；Also, detection method is simple, realizes that simple calculating and processing can be obtained testing result using computer, real-time detection guarantees the timeliness to control of product quality.
Description
Technical field
The present invention relates to a kind of detection device for vinylacetate rectifying product, the controls using the detection device to fill
It sets and detection method.
Background technique
Vinylacetate is one of the industrial chemicals more generally used, and industrial production mainly uses acetylene in gas phase method at present
With ethylene vapor phase method, and the vinylacetate raw material to be refined is required to carry out separating-purifying using rectifying column, in rectifying
In the process, the purity of vinylacetate is the main indicator of control, influences final product quality.In the prior art, in acetic acid
In the production process of vinyl acetate, in order to guarantee that final product purity can reach standard, generally using artificial timing sampling
Mode is detected to carry out quality control；Manual sampling is detected, and more troublesome, monitoring data lag, Bu Nengshi are operated
When reflect state of arts in product quality and rectifying column, prevent operator is from the final purity according to product to work
The timely adjustment of skill causes substandard product to flow into next process, and then makes entirely to produce unstable, reduction product qualification
Rate.
Therefore, it is necessary to a kind of vinylacetate rectifying On-line Product purity detecting devices, being capable of real-time detection vinyl acetate
The purity of ester rectifying product provides foundation for the technological parameter in adjustment rectifying column in time, thus guarantee the purity of final products,
So that production can stablize progress, product qualification rate is improved.
Summary of the invention
In view of this, it is an object of the invention to provide a kind of vinylacetate rectifying On-line Product purity detecting devices, control
Device and detection method are capable of the purity of real-time detection vinylacetate rectifying product, using purity parameter obtained, in time
The technological parameter in rectifying column is adjusted, to guarantee the purity of final products, so that production can stablize progress, product is improved and closes
Lattice rate.
Vinylacetate rectifying On-line Product purity detecting device of the invention, including draw liquid bath and index of refraction instrument, it is described
Draw liquid bath and be connected to vinylacetate overhead product reservoir inlet pipeline and medium in the inlet pipeline is drawn into liquid bath in real time
And liquid level is established, and medium flows back to the inlet pipeline by drawing liquid bath in real time；The index of refraction instrument, which is set to, draws liquid bath for detecting
Draw the index of refraction that the medium of liquid level is established in liquid bath.
It further, further include being set in the inlet pipeline drainage plate to medium with drainage, the drainage
Medium is drawn liquid bath by drawing the communication port of liquid bath and the inlet pipeline by plate；
Further, the drainage plate is located at the side opposite with the communication port of the inlet pipeline with liquid bath is drawn perpendicular to institute
State the setting of inlet pipeline center line；
Further, the drainage plate is that semicircle and semicircular curved edge and inlet pipeline closing are arranged, institute
State the half that drainage plate radius is not less than the inlet pipeline internal diameter；
It is further, described that draw liquid bath concordant with liquid bath slot bottom is drawn with the lower edge of the communication port of the inlet pipeline；
Further, the probe of the index of refraction instrument, which from top to bottom protrudes into, draws liquid bath, the drainage plate face index of refraction instrument
It pops one's head in and draws between the slot bottom of liquid bath at half.
The invention also discloses a kind of automatic control dresses using vinylacetate rectifying On-line Product purity detecting device
It sets, comprising:
Detection unit is vinylacetate rectifying On-line Product purity detecting device；
Control unit, for receiving vinylacetate rectifying product index of refraction that detection unit transmits and obtaining purity number
According to；
Execution unit, the control command of reception control unit, and vinylacetate is delivered to by tower top according to control command
Product reservoir partly or entirely returns to rectifying column continuation rectifying.
Further, the execution unit includes:
Overhead product reservoir inlet pipeline electrically-controlled valve, for opening and closing or adjusting Jie of overhead product reservoir inlet pipeline
Matter；
Condenser reflux pipeline electrically-controlled valve, for opening and closing or adjusting, to be back to rectifying column by condenser media outlet again smart
The medium evaporated.
The invention also discloses a kind of detections using the vinylacetate rectifying On-line Product purity detecting device
Method, including the following steps:
A. the index of refraction of vinylacetate medium in overhead product reservoir inlet pipeline is obtained；
B. the purity parameter of the 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 vinylacetate medium
Purity parameter；In formula: C is vinyl acetate concentrations, nDFor medium index of refraction；
In step a, the index of refraction is corrected to the index of refraction of a normal temperature.
Beneficial effects of the present invention: vinylacetate rectifying On-line Product purity detecting device of the invention, control device
And detection method, using the device that real-time detection vinylacetate purity is arranged on overhead product reservoir inlet pipeline, and
And online detection structure is formed, and it is capable of the purity of real-time detection vinylacetate rectifying product, using purity parameter obtained,
Technological parameter in adjustment rectifying column in time, so that production can stablize progress, is improved and is produced to guarantee the purity of final products
Product qualification rate；Also, detection method is simple, realizes that simple calculating and processing can be obtained testing result using computer, real
When detect, guarantee to the timeliness of control of product quality.
Detailed description of the invention
The invention will be further described with reference to the accompanying drawings and examples.
Fig. 1 is control device application schematic diagram of the invention；
Fig. 2 is structure of the detecting device schematic diagram of the invention.
Specific embodiment
Fig. 1 is control device application schematic diagram of the invention；Fig. 2 is structure of the detecting device schematic diagram of the invention；Such as figure
Shown, of the invention vinylacetate rectifying On-line Product purity detecting device, including draw liquid bath 10 and index of refraction instrument 9, it is described
Draw liquid bath and is connected to 7 inlet pipeline of vinylacetate overhead product reservoir for medium (vinylacetate) in the inlet pipeline 8
Draw liquid bath 7 in real time and establish liquid level, and medium flows back to the inlet pipeline by drawing liquid bath 10 in real time；The index of refraction instrument setting
It is used to detect the index of refraction for drawing the medium for establishing liquid level in liquid bath in drawing liquid bath；The vinylacetate index of refraction of different purity is not yet
Together, and there is linear corresponding relation；In the present invention, medium draws liquid bath 10 in real time and establishes liquid level in inlet pipeline, is building
While vertical liquid level, which flows back to the inlet pipeline by drawing liquid bath in real time, guarantees to draw the medium real-time update in liquid bath 10, with
Medium in inlet pipeline 8 is consistent, avoids depositing and influencing testing result；7 inlet tube of vinylacetate overhead product reservoir
Road is vertically arranged, so that vinylacetate can flow into overhead product reservoir by gravity, details are not described herein.
As shown in the figure: the vinylacetate material liquid in raw material reservoir 1 is delivered to rectifying column 3, rectifying column by metering pump 2
Interior medium (material liquid) is heated by tower reactor heater 4, and vinylacetate steam enters condenser 5, condensed acetic acid second
Enester enters overhead product reservoir 7 by inlet pipeline 8, and the media fluid after the separation of tower bottom enters tower reactor product liquid storage
Slot is existing distillation system structure, and details are not described herein.
It further include being set in the inlet pipeline drainage plate 11 to medium with drainage in the present embodiment, institute
It states drainage plate and medium is drawn into liquid bath 10 by drawing the communication port of liquid bath 10 and the inlet pipeline 8；Due in inlet pipeline 8
Medium flows downward, and draws and is not easy to establish liquid level in liquid bath 10, guides medium to liquid bath is drawn using drainage plate 11, forms stable liquid
Position guarantees that index of refraction instrument is capable of the index of refraction of real-time collection medium, guarantees online real-time.
In the present embodiment, the drainage plate 11 be located at draw liquid bath 10 it is opposite with the communication port of the inlet pipeline 8 one
Side is arranged perpendicular to the inlet pipeline center line；After medium flows on drainage plate, can sufficiently it be drained to after liquid bath 10 again
It is back to inlet pipeline 8, is conducive to establish and stablizes liquid level.
In the present embodiment, the drainage plate 11 is that semicircle and semicircular curved edge and the inlet pipeline 8 are closed
Setting, 11 radius of drainage plate are not less than the half of the inlet pipeline internal diameter, and the present embodiment selects drainage plate radius
For the half of the inlet pipeline internal diameter, that is, the closing to inlet pipeline one side of something is formed, is enabled media to substantially stabilized
Into drawing liquid bath 10, and stable liquid level is formed, biggish disturbance does not occur, to guarantee that final testing result is accurate.
In the present embodiment, the lower edge of the communication port for drawing liquid bath 10 and the inlet pipeline 8 and draw 10 slot bottom of liquid bath
Concordantly；It is flowed out in time conducive to the medium for drawing liquid bath 10 is entered, enters vacating space for subsequent medium, guarantee real-time.
In the present embodiment, the probe of the index of refraction instrument 9, which from top to bottom protrudes into, draws liquid bath 10, the positive doubling of the drainage plate 11
Between the probe of refractoscope and the slot bottom for drawing liquid bath at half, using drainage plate to the pile up effect of medium, guarantee refractive power
The probe of rate instrument 9 can abundant detection data, and not will form the logical obstruction of normal stream.
The invention also discloses a kind of automatic control dresses using vinylacetate rectifying On-line Product purity detecting device
It sets, comprising:
Detection unit is vinylacetate rectifying On-line Product purity detecting device；
Control unit 15, for receiving vinylacetate rectifying product index of refraction that detection unit transmits and obtaining purity number
According to；The program by index of refraction calculated purity data is stored in control unit, and purity figure is obtained according to the index of refraction measured；
Execution unit, the control command of reception control unit, and vinylacetate is delivered to by tower top according to control command
Product reservoir partly or entirely returns to rectifying column continuation rectifying；When purity reaches the standard of setting, execution unit will be whole
Inlet pipeline is opened, medium is all sent into overhead product reservoir；When purity differs larger with the standard of setting, close into
Mouth pipeline opens return line 14 for medium and is transmitted back to rectifying column continuation rectifying；If purity differs smaller with the standard of setting,
The aperture of adjustable mouth pipeline and the aperture of return line, partial reflux rectifying again；The standard and inlet pipeline of setting
Aperture and the aperture of return line set and adjusted as needed, realize that details are not described herein using the program first set.
In the present embodiment, the execution unit includes:
Overhead product reservoir inlet pipeline electrically-controlled valve 12, for opening and closing or adjusting overhead product reservoir inlet pipeline
Medium；
Condenser reflux pipeline electrically-controlled valve 13 is back to rectifying column again by condenser media outlet for opening and closing or adjusting
The medium of rectifying.
The invention also discloses a kind of detections using the vinylacetate rectifying On-line Product purity detecting device
Method, including the following steps:
A. the index of refraction of vinylacetate medium in overhead product reservoir inlet pipeline is obtained；
B. the purity parameter of the 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, the vinylacetate is obtained
The purity parameter of medium；In formula: C is vinyl acetate concentrations, and nD is medium index of refraction；
Realize vinylacetate rectifying On-line Product purity detection method be: be respectively configured purity be 40%, 60%,
80%, 90%, 95%, 97%, 99%, 99.5%, 100% vinyl acetate solution tests its index of refraction at 20 DEG C, as a result
It is shown in Table 1.
1 vinyl acetate purity of table and index of refraction test result
The relation curve that index of refraction and concentration are made according to 1 data of table, obtains fit equation: C=2608.568nD-
3531.555, related coefficient reaches 0.9972, in specific implementation, to set Reinheitszahl required by technology controlling and process to control target
Value, converts index of refraction for Pureness control value by operation, for the realization pair of the difference of target index of refraction and index of refraction detected value
The judgement and control of rectifying column product purity.
In step a, the index of refraction is corrected to the index of refraction of a normal temperature, and the present embodiment normal temperature is 20 DEG C.It is existing
The index of refraction of different temperatures can be corrected into the index of refraction of normal temperature by some index of refraction instrument, if manual synchronizing is usually to establish temperature
The relation curve of degree and index of refraction, is obtained, details are not described herein by equation calculation.
Finally, it is stated that the above examples are only used to illustrate the technical scheme of the present invention and are not limiting, although referring to compared with
Good embodiment describes the invention in detail, those skilled in the art should understand that, it can be to skill of the invention
Art scheme is modified or replaced equivalently, and without departing from the objective and range of technical solution of the present invention, should all be covered at this
In the scope of the claims of invention.
Claims (6)
1. a kind of vinylacetate rectifying On-line Product purity detecting control device, it is characterised in that: include:
Detection unit is vinylacetate rectifying On-line Product purity detecting device；
Control unit, for receiving vinylacetate rectifying product index of refraction that detection unit transmits and obtaining purity data；
Execution unit, the control command of reception control unit, and vinylacetate is delivered to by overhead product according to control command
Reservoir partly or entirely returns to rectifying column continuation rectifying,
Vinylacetate rectifying On-line Product purity detecting device includes:
Draw liquid bath and index of refraction instrument, the liquid bath that draws is connected to vinylacetate overhead product reservoir inlet pipeline for the import
Pipeline internal medium draws liquid bath in real time and establishes liquid level, and medium flows back to the inlet pipeline by drawing liquid bath in real time；The refractive power
Rate instrument, which is set to, draws liquid bath for detecting the index of refraction for drawing the medium for establishing liquid level in liquid bath,
It further include being set in the inlet pipeline drainage plate to medium with drainage, the drainage plate passes through medium
The communication port for drawing liquid bath and the inlet pipeline draws liquid bath.
2. vinylacetate rectifying On-line Product purity detecting control device according to claim 1, it is characterised in that: institute
It states drainage plate and is located at the side opposite with the communication port of the inlet pipeline with liquid bath is drawn perpendicular to the inlet pipeline center line
Setting.
3. vinylacetate rectifying On-line Product purity detecting control device according to claim 1, it is characterised in that: institute
It states drainage plate to be arranged for semicircle and semicircular curved edge and inlet pipeline closing, the drainage plate radius is not less than
The half of the inlet pipeline internal diameter.
4. vinylacetate rectifying On-line Product purity detecting control device according to claim 1, it is characterised in that: institute
State that draw liquid bath concordant with liquid bath slot bottom is drawn with the lower edge of the communication port of the inlet pipeline.
5. vinylacetate rectifying On-line Product purity detecting control device according to claim 4, it is characterised in that: institute
The probe for stating index of refraction instrument, which from top to bottom protrudes into, draws liquid bath, the probe of the drainage plate face index of refraction instrument and the slot bottom for drawing liquid bath
Between at half.
6. vinylacetate rectifying On-line Product purity detecting control device according to claim 1, it is characterised in that: institute
Stating execution unit includes:
Overhead product reservoir inlet pipeline electrically-controlled valve, for opening and closing or adjusting the medium of overhead product reservoir inlet pipeline；
Condenser reflux pipeline electrically-controlled valve is back to rectifying column rectifying again by condenser media outlet for opening and closing or adjusting
Medium.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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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| 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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| CN105784638B true CN105784638B (en) | 2019-04-16 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107677643B (en) * | 2017-09-20 | 2020-07-03 | 宁波市鄞州赛弗兑食品科技有限公司 | Hand-held refractometer |
| CN107677642B (en) * | 2017-09-20 | 2020-07-03 | 宁波市鄞州赛弗兑食品科技有限公司 | Refractometer |
| CN113231118B (en) * | 2021-05-10 | 2022-08-05 | 海南医学院 | Fractionating device for organic chemistry experiment |
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| US6018388A (en) * | 1998-02-18 | 2000-01-25 | Nawracala; Bernd | Microtiter plate |
| EP2063254A2 (en) * | 2007-11-17 | 2009-05-27 | IAV GmbH Ingenieurgesellschaft Auto und Verkehr | Method of determining the phase transfer of a multiple component drop in a flow of gas, dissolved in the crystalline solids, solid |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS61219853A (en) * | 1985-03-26 | 1986-09-30 | Sumikin Coke Co Ltd | Method for automatically measuring concentration of ammonia |
| JPH08166345A (en) * | 1994-12-16 | 1996-06-25 | Shiroki Corp | Apparatus for measuring concentration of liquid |
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2016
- 2016-01-07 CN CN201610008152.5A patent/CN105784638B/en not_active Expired - Fee Related
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4781459A (en) * | 1985-05-17 | 1988-11-01 | Horiba, Ltd. | Apparatus for measuring the amount of minute particles contained in liquid |
| US6018388A (en) * | 1998-02-18 | 2000-01-25 | Nawracala; Bernd | Microtiter plate |
| EP2063254A2 (en) * | 2007-11-17 | 2009-05-27 | IAV GmbH Ingenieurgesellschaft Auto und Verkehr | Method of determining the phase transfer of a multiple component drop in a flow of gas, dissolved in the crystalline solids, solid |
Non-Patent Citations (1)
| Title |
|---|
| 精馏实验;秦婷婷;《百度文库》;20110414;1-7 |
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