CN107589158A - A kind of online test method and device of the sulfate pulping process paper pulp kappa number based on double electrochemical sensors - Google Patents
A kind of online test method and device of the sulfate pulping process paper pulp kappa number based on double electrochemical sensors Download PDFInfo
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- CN107589158A CN107589158A CN201710672423.1A CN201710672423A CN107589158A CN 107589158 A CN107589158 A CN 107589158A CN 201710672423 A CN201710672423 A CN 201710672423A CN 107589158 A CN107589158 A CN 107589158A
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Abstract
The invention discloses a kind of online test method and device of the sulfate pulping process paper pulp kappa number based on double electrochemical sensors.Online test method comprises the following steps：S1. since the slurrying, continue to release the black liquor in the reactor of slurrying, after being cooled to 20 ~ 100 DEG C, the electrical conductivity S of black liquor during detection reaction starting0, and the electrical conductivity S of the black liquor of tt；S2. when the electrical conductivity of black liquor is less than 32mS/cm from, start continue detection black liquor t pH value pHt；S3. calculating paper pulp kappa number is carried out using PLS.On-line measuring device includes sampling pipe, cooling device, pH value detect tank, the pH value electrode being arranged in pH value detect tank, electrical conductivity detect tank, conductivity electrode and the computer being connected with the reactor of slurrying.The detection means and online test method are that sulfate process starches the on-line checking of Kappa number and control has important practical significance.
Description
Technical field
The present invention relates to the technical field of paper pulp kappa number measure, more particularly to a kind of based on double electrochemical sensings
The online test method and device of the sulfate pulping process paper pulp kappa number of device.
Background technology
In modern pulp and paper industry, boiling be pulping and paper-making production important workshop section, how in boiling degraded and
The more lignins of dissolution, the cellulose and hemicellulose of more intact fibre forms are left, improve the quality of paper pulp, be boiling
The process to be controlled.Delignification degree is one of important indicator to be controlled in digestion process, and digestion process pulp quality is
By controlling the Kappa number of paper pulp, the determination of Kappa number represents the determination of pulp quality, by stablizing the Kappa number of paper pulp also
The yield of paper pulp can be improved.
China on Kappa number online measuring technique compared with foreign countries, it is also relatively backward, but lead over being averaged for the world
It is horizontal.It is mainly reflected in, does not can apply to the on-line measurement sensor of production scene, external Kappa number sensor is uncomfortable
For the technological process of production of the country, and external equipment price is too high, and most domestic enterprise is not used widely.Mesh
Preceding domestic Kappa number measurement still uses Optical Analysis Method and the class of chemical analysis two.Chemical analysis must be examined with final products
Survey analysis after, can just feed back in actual production, this method in detection process there is error, influence whether entirely to make
Starch the monitoring of production.And Optical Analysis Method high resolution, com-parison and analysis are quick, it is not necessary to sample is handled, to determinand
Adaptive faculty is strong, it is possible to achieve on-line checking.But use ultraviolet spectroscopy there is also it is certain the problem of, such as cooking liquor absorb
It is too strong, it is necessary to by dilution, so to establish the dilution system of precision.In addition, in the mechanism model and actual production established
Testing model has to pass through demonstration repeatedly and could implemented, and so just can guarantee that model prediction is accurate.
The content of the invention
The technical problem to be solved in the present invention is to overcome drawbacks described above, there is provided a kind of sulphur based on double electrochemical sensors
The online test method of hydrochlorate method pulping process paper pulp kappa number.
Another object of the present invention is to provide a kind of sulfate pulping process paper pulp based on double electrochemical sensors
The on-line measuring device of Kappa number.
The present invention is achieved through the following technical solutions：
A kind of online test method of the sulfate pulping process paper pulp kappa number based on double electrochemical sensors, including
Following steps：
S1. since the slurrying, continue to release the black liquor in the reactor of slurrying, after being cooled to 20~100 DEG C, inspection
The electrical conductivity S of black liquor when surveying reaction starting0, and the electrical conductivity S of the black liquor of tt；
S2. when the electrical conductivity of black liquor is less than 32mS/cm from, start continue detection black liquor t pH values pHt；
S3. calculating paper pulp kappa number is carried out using PLS, the relational expression of dependent variable and independent variable is as follows：
Kt=f (S0,St,pHt,SW,pHW)
In formula：K --- Kappa number, dimensionless；S0、St--- reaction starting when and t black liquor electrical conductivity, mS/cm；
SW--- the electrical conductivity of white liquor, mS/cm；pHt--- the pH value of t black liquor, dimensionless； pHW--- the theoretical pH value of white liquor,
Dimensionless.
A kind of on-line measuring device of the sulfate pulping process paper pulp kappa number based on double electrochemical sensors, including
The sampling pipe that is connected with the reactor of slurrying, cooling device, pH value detect tank, the pH value being arranged in pH value detect tanks
Electrode, electrical conductivity detect tank, the conductivity electrode and computer for being arranged at electrical conductivity detect tank；The sampling pipe and cooling
Device is connected, and the cooling device is connected with pH value detect tank and electrical conductivity detect tank respectively by pipeline, the pH value detection
Groove and electrical conductivity detect tank pass through black liquor recovery pipeline communication with reactor；The pH value electrode and conductivity electrode respectively with meter
Calculation machine connects；The sampling pipe and/or pipeline are provided with valve and/or pump.
Preferably, cleaning liquid bath is additionally provided with, the cleaning liquid bath is connected by pipeline with sampling pipe, and pipeline is provided with valve
Door and/or pump.
Preferably, waste liquid tank is additionally provided with, the waste liquid tank is provided with valve by pipeline and black liquor recovery pipeline communication, pipeline
Door and/or pump.
Preferably, the cooling device is included with bosh, cooler and the hot water storgae of pipeline communication, on the pipeline
Provided with pump and/or valve；The cooler is connected with sampling pipe.
A kind of detection method based on the on-line measuring device, comprises the following steps：
S11. since the slurrying, sampling pipe continues to release the black liquor in the reactor of slurrying, and black liquor is through cooling
After device is cooled to 20~100 DEG C, it is passed through in electrical conductivity detect tank, the electrical conductivity of black liquor when conductivity electrode detection reaction originates
S0, and the electrical conductivity S of the black liquor of tt, and be recorded in computer；
S12. when the electrical conductivity of black liquor is less than 32mS/cm from, black liquor after apparatus for supercooling is cooled to 20~100 DEG C,
It is passed through in pH value detect tank, pH value electrode starts to continue pH value pH of the detection black liquor in tt；
S13. calculating paper pulp kappa number is carried out using PLS, the relational expression of dependent variable and independent variable is as follows：
Kt=f (S0,St,pHt,SW,pHW)
In formula：K --- Kappa number, dimensionless；S0、St--- reaction starting when and t black liquor electrical conductivity, mS/cm；
SW--- the electrical conductivity of white liquor, mS/cm；pHt--- the pH value of t black liquor, dimensionless； pHW--- the theoretical pH value of white liquor,
Dimensionless.
A kind of detection method based on the on-line measuring device, comprises the following steps：
S21. before starting slurrying, pH value detect tank and electrical conductivity are entered after the cleaning fluid cleaned in liquid bath is passed through into cooler
Detect tank；The pH value and conductivity value of pH value electrode and conductivity electrode measurement cleaning fluid, and according to the pH value and electricity of cleaning fluid
Conductance is corrected to two electrodes；
S22. since the slurrying, sampling pipe continues to release the black liquor in the reactor of slurrying, and black liquor is through cooling
After device is cooled to 20~100 DEG C, it is passed through in electrical conductivity detect tank, the electrical conductivity of black liquor when conductivity electrode detection reaction originates
S0, and the electrical conductivity S of the black liquor of tt, and be recorded in computer；
S23. when the electrical conductivity of black liquor is less than 32mS/cm from, black liquor after apparatus for supercooling is cooled to 20~100 DEG C,
It is passed through in pH value detect tank, pH value electrode starts to continue pH value pH of the detection black liquor in tt；
S24. calculating paper pulp kappa number is carried out using PLS, the relational expression of dependent variable and independent variable is as follows：
Kt=f (S0,St,pHt,SW,pHW)
In formula：K --- Kappa number, dimensionless；S0、St--- reaction starting when and t black liquor electrical conductivity, mS/cm；
SW--- the electrical conductivity of white liquor, mS/cm；pHt--- the pH value of t black liquor, dimensionless； pHW--- the theoretical pH value of white liquor,
Dimensionless.
Compared with now with technology, the invention has the advantages that：
The on-line checking side of sulfate pulping process paper pulp kappa number of the present invention based on double electrochemical sensors
Method regardless of whether raw material (timber, bamboo, wheat straw, bagasse etc.) is pre-processed, pre-processed before slurrying after whether pour out it is pre-
Extract, electrical conductivity, pH values, the electrical conductivity of white liquor and the pH value of paper pulp kappa number and black liquor after sulfate pulping are present
The relation highly relied on, by the Kappa number for detecting the i.e. predictable paper pulp of black liquor electrical conductivity and pH value.
The on-line measuring device of the present invention has electrical conductivity and pH calibration functions, can effectively reduce detection error.And
And by the control of black liquor temperature, the precision of testing result is also further ensured that.The on-line measuring device realizes paper pulp card
The detection in real time of uncle's value, reduces the hysteresis quality of laboratory detection result, regulation and control and management to actual production technique bring pole
Big is ageing.
The online test method of the present invention is respectively provided with good prediction effect to sulfate process paper pulp kappa number.The detection fills
It is that sulfate process starches the on-line checking of Kappa number and control has important practical significance to put with online test method.
Brief description of the drawings
Fig. 1 is the online test method and dress of the sulfate pulping process paper pulp kappa number based on double electrochemical sensors
Put.
Wherein, 1-reactor；21st, 22,23,24,25,26-valve；3-cooler；4-bosh；51、52、
53-delivery pump；6-hot water storgae；7-pH value detect tank；8-electrical conductivity detect tank；9-pH value electrode；10-electro conductivity
Pole；11-computer；12-cleaning liquid bath；13-waste liquid tank.
Embodiment
The present invention is further illustrated with reference to specific embodiment.Unless stated otherwise, used in the embodiment of the present invention
Raw material and method are this area routinely raw material purchased in market and conventional use of method.
A kind of online test method of the sulfate pulping process paper pulp kappa number based on double electrochemical sensors, including
Following steps：
S1. since the slurrying, continue to release the black liquor in the reactor of slurrying, after being cooled to 20~100 DEG C, inspection
The electrical conductivity S of black liquor when surveying reaction starting0, and the electrical conductivity S of the black liquor of tt；
S2. when the electrical conductivity of black liquor is less than 32mS/cm from, start continue detection black liquor t pH values pHt；
S3. calculating paper pulp kappa number is carried out using PLS, the relational expression of dependent variable and independent variable is as follows：
Kt=f (S0,St,pHt,SW,pHW)
In formula：K --- Kappa number, dimensionless；S0、St--- reaction starting when and t black liquor electrical conductivity, mS/cm；
SW--- the electrical conductivity of white liquor, mS/cm；pHt--- the pH value of t black liquor, dimensionless； pHW--- the theoretical pH value of white liquor,
Dimensionless.
A kind of detection method based on the on-line measuring device, comprises the following steps：
S11. since the slurrying, sampling pipe continues to release the black liquor in the reactor of slurrying, and black liquor is through cooling
After device is cooled to 20~100 DEG C, it is passed through in electrical conductivity detect tank, the electrical conductivity of black liquor when conductivity electrode detection reaction originates
S0, and the electrical conductivity S of the black liquor of tt, and be recorded in computer；
S12. when the electrical conductivity of black liquor is less than 32mS/cm from, black liquor after apparatus for supercooling is cooled to 20~100 DEG C,
It is passed through in pH value detect tank, pH value electrode starts to continue pH value pH of the detection black liquor in tt；
S13. calculating paper pulp kappa number is carried out using PLS, the relational expression of dependent variable and independent variable is as follows：
Kt=f (S0,St,pHt,SW,pHW)
In formula：K --- Kappa number, dimensionless；S0、St--- reaction starting when and t black liquor electrical conductivity, mS/cm；
SW--- the electrical conductivity of white liquor, mS/cm；pHt--- the pH value of t black liquor, dimensionless； pHW--- the theoretical pH value of white liquor,
Dimensionless.
Embodiment 1
A kind of on-line measuring device of the sulfate pulping process paper pulp kappa number based on double electrochemical sensors, including
Sampling pipe, cooling device, pH value detect tank 7, the pH being arranged in pH values detect tank 7 being connected with the reactor of slurrying
Value electrode 9, electrical conductivity detect tank 8, the conductivity electrode 10 and computer 11 for being arranged at electrical conductivity detect tank 8.
Sampling pipe connects with cooling device, and sampling pipe is provided with valve 21.Cooling device by pipeline respectively with pH value
Detect tank 7 connects with electrical conductivity detect tank 8, and pipeline is provided with valve 22 and valve 23.
PH value detect tank 7 and electrical conductivity detect tank 8 pass through black liquor recovery pipeline communication, black liquor recovery pipeline with reactor 1
It is provided with valve 26 and pump 53.
PH value electrode 7 and conductivity electrode 10 are connected with computer 11 respectively.
Cooling device includes bosh 4, cooler 3 and the hot water storgae 6 with pipeline communication, and pipeline is provided with pump 51, cold
But device 3 is connected with sampling pipe.
Cleaning liquid bath 12 is additionally provided with, cleaning liquid bath 12 is connected by pipeline with sampling pipe, and pipeline is provided with the He of valve 24
Pump 52.Waste liquid tank 13 is additionally provided with, waste liquid tank 13 is provided with valve 25 by pipeline and black liquor recovery pipeline communication, pipeline.
A kind of detection method based on above-mentioned on-line measuring device, comprises the following steps：
Before reactor 1 starts slurrying, on-line measuring device is brought into operation step 1., and valve 22,23,24,25 is opened,
Pump 52,53 is opened, and coutroi velocity is 0.05~5L/min, cleans cleaning fluid (i.e. clear water, pH value 5.0~9.0, the conductance of liquid bath
Rate is 10-50uS/cm) enter pH value detect tank 7 and electrical conductivity detect tank 8 after subcooler 3, then entered by valve 25
Enter waste liquid tank 13.PH value electrode 9 and conductivity electrode 10 start to measure the pH value and conductivity value of cleaning fluid, and according to cleaning fluid
Accurate pH value and electrical conductivity two electrodes are corrected.
After step 2. electrode alignment, reactor 1 is brought into operation, and valve 22,24,25 and pump 52 are closed, valve 21,26
Opened with pump 51, black liquor by reactor 1 enter cooler 3, by bosh 4 cold water through cooler 3 to black liquor carry out it is cold
But, the black liquor after cooling (temperature is 20~100 DEG C) is introduced into electrical conductivity detect tank 8, is most back to reactor 1 through pump 53 afterwards.
Black liquor electrical conductivity in electrical conductivity detect tank 8 is detected by conductivity electrode 10, and the real-time electricity by computer 11 to black liquor
Conductance is recorded.
Step 3. when the electrical conductivity of measure is less than 32mS/cm, closed, valve 22 is opened, and black liquor does not enter back into by valve 23
Electrical conductivity detect tank 8, then enter pH value detect tank 7, pH value electrode 9 is detected in real time to the pH values of black liquor, and by by
The record data of computer 11.
Step 4. by measured continuity data (>8 point/h), substitute into the mathematical forecasting model pre-established, it is real
When the paper pulp kappa number in reactor 1 is calculated, when reaching predetermined Kappa number, reactor 1 is stopped, starts to put
Pot.
Valve 21,26 close, detection architecture is cleaned according to the operation of step 1, finally close all valves and
Pump, on-line measuring device are stopped.
Calculating paper pulp kappa number is carried out using PLS, the relation between dependent variable and independent variable is as follows：
Kt=f (S0,St,pHt,SW,pHW)
In formula：K --- Kappa number, dimensionless；S0、St--- reaction starting when and t black liquor electrical conductivity, mS/cm；
SW--- the electrical conductivity of white liquor, mS/cm；pHt--- the pH value of t black liquor, dimensionless； pHW--- the theoretical pH value of white liquor,
Dimensionless；
Embodiment 2
The present embodiment selects the sulfate pulping workshop section of 4 bench scales to be implemented, by the embodiment of the present invention 1
On-line measuring device and method, carry out on-line checking.Meanwhile each corresponding pulp sample of experiment is left and taken by GB/T 1546-
2004《The measure of paper pulp kappa number》Detected in laboratory.
The pulping process condition of the sulfate pulping workshop section of 4 bench scales is as shown in table 1, in order to GB/T 1546-
2004 testing result is compared, black when the present embodiment is terminated with the sulfate pulping workshop section slurrying of 4 bench scales
Liquid is detected and obtains testing result；And slurrying will be obtained Kappa number, testing result such as table are detected with GB/T 1546-2004
Shown in 1.
Mathematical prediction equation is is calculated using PLS in the present embodiment, the relation of dependent variable and independent variable
Formula is as follows：
The bamboo sulfate pulping Kappa number on-line checking accuracy table * of table 1
* pre-hydrolyzed solution is than 1:3rd, 170 DEG C of temperature, time 30-180min, cooking liquor is than 1:5th, 165 DEG C of temperature, time 60-
120min, alkali charge 17.8%, sulphidity 21.5%.
As can be known from Table 1, the sulfate pulping process paper pulp kappa number based on double electrochemical sensors of the invention
Line detecting method and detection means, paper pulp kappa number can be accurately and reliably detected, its testing result and GB/T 1546-
2004《The measure of paper pulp kappa number》Testing result deviation be less than ± 6.65%.
Claims (7)
1. a kind of online test method of the sulfate pulping process paper pulp kappa number based on double electrochemical sensors, its feature
It is, comprises the following steps：
S1. since the slurrying, continue to release the black liquor in the reactor of slurrying, after being cooled to 20~100 DEG C, detection is anti-
The electrical conductivity S of black liquor when should originate0, and the electrical conductivity S of the black liquor of tt；
S2. when the electrical conductivity of black liquor is less than 32mS/cm from, start continue detection black liquor t pH value pHt；
S3. calculating paper pulp kappa number is carried out using PLS, the relational expression of dependent variable and independent variable is as follows：
Kt=f (S0,St,pHt,SW,pHW)
In formula：K --- Kappa number, dimensionless；S0、St--- reaction starting when and t black liquor electrical conductivity, mS/cm；
SW--- the electrical conductivity of white liquor, mS/cm；pHt--- the pH value of t black liquor, dimensionless；pHW--- the theoretical pH value of white liquor,
Dimensionless.
2. a kind of on-line measuring device of the sulfate pulping process paper pulp kappa number based on double electrochemical sensors, its feature
Be, including be connected with the reactor of slurrying sampling pipe, cooling device, pH value detect tank, be arranged at pH value detect tank
Interior pH value electrode, electrical conductivity detect tank, the conductivity electrode and computer for being arranged at electrical conductivity detect tank；The probe tube
Road is connected with cooling device, and the cooling device is connected with pH value detect tank and electrical conductivity detect tank respectively by pipeline, described
PH value detect tank and electrical conductivity detect tank pass through black liquor recovery pipeline communication with reactor；The pH value electrode and conductivity electrode
It is connected respectively with computer；The sampling pipe and/or pipeline are provided with valve and/or pump.
3. detection means according to claim 2, it is characterised in that be additionally provided with cleaning liquid bath, the cleaning liquid bath passes through pipe
Road connects with sampling pipe, and pipeline is provided with valve and/or pump.
4. detection means according to claim 3, it is characterised in that be additionally provided with waste liquid tank, the waste liquid tank by pipeline with
Black liquor recovery pipeline communication, pipeline are provided with valve and/or pump.
5. detection means according to claim 4, it is characterised in that the cooling device includes the cooling water with pipeline communication
Groove, cooler and hot water storgae, the pipeline are provided with pump and/or valve；The cooler is connected with sampling pipe.
6. a kind of detection method based on on-line measuring device described in claim 2, it is characterised in that comprise the following steps：
S11. since the slurrying, sampling pipe continues to release the black liquor in the reactor of slurrying, and black liquor is through cooling device
After being cooled to 20~100 DEG C, it is passed through in electrical conductivity detect tank, the electrical conductivity S of black liquor when conductivity electrode detection reaction originates0,
And the electrical conductivity S of the black liquor of tt, and be recorded in computer；
S12. when the electrical conductivity of black liquor is less than 32mS/cm from, black liquor is passed through after apparatus for supercooling is cooled to 20~100 DEG C
In pH value detect tank, pH value electrode starts to continue pH value pH of the detection black liquor in tt；
S13. calculating paper pulp kappa number is carried out using PLS, the relational expression of dependent variable and independent variable is as follows：
Kt=f (S0,St,pHt,SW,pHW)
In formula：K --- Kappa number, dimensionless；S0、St--- reaction starting when and t black liquor electrical conductivity, mS/cm；
SW--- the electrical conductivity of white liquor, mS/cm；pHt--- the pH value of t black liquor, dimensionless；pHW--- the theoretical pH value of white liquor,
Dimensionless.
7. a kind of detection method based on on-line measuring device described in claim 3, it is characterised in that comprise the following steps：
S21. before starting slurrying, the cleaning fluid cleaned in liquid bath is passed through after cooler and enters pH value detect tank and electrical conductivity detection
Groove；The pH value and conductivity value of pH value electrode and conductivity electrode measurement cleaning fluid, and according to the pH value and electrical conductivity of cleaning fluid
Two electrodes are corrected；
S22. since the slurrying, sampling pipe continues to release the black liquor in the reactor of slurrying, and black liquor is through cooling device
After being cooled to 20~100 DEG C, it is passed through in electrical conductivity detect tank, the electrical conductivity S of black liquor when conductivity electrode detection reaction originates0,
And the electrical conductivity S of the black liquor of tt, and be recorded in computer；
S23. when the electrical conductivity of black liquor is less than 32mS/cm from, black liquor is passed through after apparatus for supercooling is cooled to 20~100 DEG C
In pH value detect tank, pH value electrode starts to continue pH value pH of the detection black liquor in tt；
S24. calculating paper pulp kappa number is carried out using PLS, the relational expression of dependent variable and independent variable is as follows：
Kt=f (S0,St,pHt,SW,pHW)
In formula：K --- Kappa number, dimensionless；S0、St--- reaction starting when and t black liquor electrical conductivity, mS/cm；
SW--- the electrical conductivity of white liquor, mS/cm；pHt--- the pH value of t black liquor, dimensionless；pHW--- the theoretical pH value of white liquor,
Dimensionless.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108380151A (en) * | 2018-04-23 | 2018-08-10 | 河南应用技术职业学院 | The reaction end automatic control device and its control method of ester plasticizer |
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| CN1312465A (en) * | 2001-04-12 | 2001-09-12 | 华南理工大学 | On-line paper pulp kappa number spectrometric system and method for pulping digestion process |
| CN2482074Y (en) * | 2001-04-17 | 2002-03-13 | 华南理工大学 | Paper pulp Kappa number in-line spectrum measuring device in pulping digestion process |
| US20020144795A1 (en) * | 1999-12-23 | 2002-10-10 | Bourbonnais Robert Ernest | Electrochemical method for determinating lignin content of pulp |
| CN103630501A (en) * | 2013-11-14 | 2014-03-12 | 华南理工大学 | Rapid tester for paper pulp kappa number and control method of rapid tester |
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2017
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61176854A (en) * | 1985-01-31 | 1986-08-08 | Yokogawa Electric Corp | Instrument for measuring cooking degree |
| US20020144795A1 (en) * | 1999-12-23 | 2002-10-10 | Bourbonnais Robert Ernest | Electrochemical method for determinating lignin content of pulp |
| CN1312465A (en) * | 2001-04-12 | 2001-09-12 | 华南理工大学 | On-line paper pulp kappa number spectrometric system and method for pulping digestion process |
| CN2482074Y (en) * | 2001-04-17 | 2002-03-13 | 华南理工大学 | Paper pulp Kappa number in-line spectrum measuring device in pulping digestion process |
| CN103630501A (en) * | 2013-11-14 | 2014-03-12 | 华南理工大学 | Rapid tester for paper pulp kappa number and control method of rapid tester |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108380151A (en) * | 2018-04-23 | 2018-08-10 | 河南应用技术职业学院 | The reaction end automatic control device and its control method of ester plasticizer |
| CN108380151B (en) * | 2018-04-23 | 2019-12-03 | 河南应用技术职业学院 | The control method of the reaction end automatic control device of ester plasticizer |
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| CN107589158B (en) | 2019-09-06 |
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