CN103335921B - A kind of detect the method that effect kept in paper pulp by retention agent - Google Patents
A kind of detect the method that effect kept in paper pulp by retention agent Download PDFInfo
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- CN103335921B CN103335921B CN201310208496.7A CN201310208496A CN103335921B CN 103335921 B CN103335921 B CN 103335921B CN 201310208496 A CN201310208496 A CN 201310208496A CN 103335921 B CN103335921 B CN 103335921B
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- 230000014759 maintenance of location Effects 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 31
- 230000000694 effects Effects 0.000 title claims abstract description 24
- 229920001131 Pulp (paper) Polymers 0.000 title claims abstract description 16
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 36
- 239000000706 filtrate Substances 0.000 claims abstract description 31
- 239000002002 slurry Substances 0.000 claims abstract description 27
- 238000001514 detection method Methods 0.000 claims abstract description 17
- 239000002245 particle Substances 0.000 claims abstract description 15
- 230000033228 biological regulation Effects 0.000 claims abstract description 8
- 238000004043 dyeing Methods 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 238000010790 dilution Methods 0.000 claims abstract description 3
- 239000012895 dilution Substances 0.000 claims abstract description 3
- 239000008187 granular material Substances 0.000 claims description 16
- VOFUROIFQGPCGE-UHFFFAOYSA-N nile red Chemical compound C1=CC=C2C3=NC4=CC=C(N(CC)CC)C=C4OC3=CC(=O)C2=C1 VOFUROIFQGPCGE-UHFFFAOYSA-N 0.000 claims description 4
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 2
- 239000012498 ultrapure water Substances 0.000 claims description 2
- 239000012752 auxiliary agent Substances 0.000 abstract description 4
- 239000000523 sample Substances 0.000 description 16
- 239000007788 liquid Substances 0.000 description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 239000000945 filler Substances 0.000 description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 6
- 239000000470 constituent Substances 0.000 description 6
- 239000000835 fiber Substances 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 239000003643 water by type Substances 0.000 description 6
- 238000002156 mixing Methods 0.000 description 5
- 241000202567 Fatsia japonica Species 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 239000000700 radioactive tracer Substances 0.000 description 4
- 230000001105 regulatory effect Effects 0.000 description 4
- 239000000654 additive Substances 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L calcium carbonate Substances [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 description 3
- 230000009514 concussion Effects 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 239000011780 sodium chloride Substances 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 230000015271 coagulation Effects 0.000 description 2
- 238000005345 coagulation Methods 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 239000010893 paper waste Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000010008 shearing Methods 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000004448 titration Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- 240000003183 Manihot esculenta Species 0.000 description 1
- 235000016735 Manihot esculenta subsp esculenta Nutrition 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000012496 blank sample Substances 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000007850 fluorescent dye Substances 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 238000004848 nephelometry Methods 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/34—Paper
- G01N33/343—Paper pulp
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Medicinal Chemistry (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Paper (AREA)
Abstract
The invention discloses and a kind of detect the method that effect kept in paper pulp by retention agent, comprise the following steps: dynamic drainage instrument (DDJ) poured into by the slurry after (1) will discongest, setting speed is 300～3000r/min, adds retention agent, collects filtrate after stirring 10～60s；(2) above-mentioned filtrate is after dilution, adds stain lucifuge dyeing 3～10min, detects with laser particle analyzer, is guaranteed number≤1000 of the tiny component of detection per second by regulation flow velocity, obtains analytical data；(3) analytical data drawn according to step (2), can draw retention agent keeps effect.The present invention is capable of detecting when content and the size variation of tiny component in filtrate, it is possible to effectively assess the using effect of retention agent, and the retention effect for on-line checking auxiliary agent provides the most direct Technical Reference.
Description
Technical field
The present invention relates to field of papermaking, be specifically related to a kind of retention agent that detects in paper pulp, keep the side of effect
Method.
Background technology
The retention agent that paper mill uses at present is wide in variety, and quality standard disunity, structural behaviour difference is big.Make
Paper plant in use lacks the evaluation of set of system and determines the method for application conditions, have to be in actual applications
Grope, the most time-consuming, and production can be affected and be normally carried out.
The method of detection retention agent retention effect mainly has at present: utilize colloidal electric charge titrimetry and dynamic drainage
Instrument (DDJ), ultraviolet spectrophotometer or the retention effect of scopometer overall merit Retention Aid in Papermaking.But
Colloidal electric charge titrimetry, can only detect the change of its solution charge, during charge director color gradient
Easily produce subjectivity error, and the cohesion change of its paper pulp can not be detected, it is impossible to filter after accurately providing filter
Tiny component size distribution and the information of content in liquid.And utilize scopometer and ultraviolet spectrophotometer, just need
The quality of tiny component or obtain the absolute dry mass of l Water Paper on filter screen in Accurate Determining filtrate.Measure filter at present
In liquid, the quality method of tiny component mainly has two kinds: weighing method and nephelometry, and weighing method needs to gather drainage
Residual fiber and filler in tank, sucking filtration post-drying obtains keeping the absolute mass of long fibre and fines, but is joining
Slurry, to take the experimental error brought due to difference in operation during wet web, sucking filtration the biggest, step simultaneously
Loaded down with trivial details, time and effort consuming；The latter needs to measure filtrate turbidity, by setting up between turbidity and tiny concentration of component
Linear relationship conversion filter liquor concentration, and indirectly calculate the quality of all tiny components in paper pulp, though the method
Can indirectly reflect keeping of all tiny components, but turbidity measurements repeatability is poor.
Tiny component refers to the fine particle by 200 mesh nets, and it adsorbs two kinds by mechanical retention and colloid
Approach realizes keeping in page.Colloid absorption is the dominant mechanism kept of tiny component, including by pure carefully
The wadding polymers that small component is formed and the tiny component wadding polymers containing fiber, the most tiny component is adsorbed
On the fiber surface, these tiny components are padded along with shaping slurry is fixed and be combined in fiber at paper machine forming section
In.Then the tiny component being not left on slurry pad is just flowed in filtrate by net.Along with filtrate closed circulation
The raising of degree, staying the tiny component in filtrate will affect the quality of paper, causes microorganism to infect.Carefully
Small component itself contains Various Complex Organic substance, enters after Waste Paper Handling system, not only show hydrophobicity,
The multifrequency nature such as adsorptivity, charging property, and coagulation or dispersion phenomenon can occur under these characteristic effects,
Increase the difficulty that hydrophobic particle controls.The treatment effect of paste system is by traditional detection retention agent
Represented by the relative clarity of detection sample, do not detect that the content of tiny component and size are divided
The poly-situation of wadding of cloth and tiny component, and how to determine the quantity of tiny component in filtrate, observe tiny group
The change divided there is presently no solution, and this will be the subject matter run in a large amount of reuse of waste paper.At present, also
There is no a kind of method of tiny measured portions in pulp suspension of global general-use.
Summary of the invention
Instant invention overcomes detection retention agent keep in effect occur cannot accurately measure tiny constituent content
Problem and shortage with size distribution, it is proposed that a kind of new be used for detecting retention agent and keep effect in paper pulp
Method.The detection method of tiny component in filtrate after this filter that the present invention proposes, is for thin in filtrate
The change of small component content reflects the using effect of retention agent indirectly, by the main bar of system in paper machine operation
Part affects and condenses, thus this practical situation that paper machine operation and paper product quality are had a negative impact, mould
Intend the condition of paper machine system, in specific pretreatment unit, filtrate carried out pretreatment, then use spike
Agent and tiny component adsorb this principle, the tiny component that after detection DDJ filtration, in filtrate, coagulation gets up
Content, i.e. can react the service condition of retention agent, can detect the application effect of different retention agent simultaneously.
The object of the invention is achieved through the following technical solutions:
A kind of detect the method that effect kept in paper pulp by retention agent, comprise the following steps:
(1) dynamic drainage instrument (DDJ) poured into by the slurry after discongesting, and setting speed is 300～3000r/min,
Add retention agent, after stirring 10～60s, collect filtrate；
(2) above-mentioned filtrate is after dilution, adds stain lucifuge dyeing 3～10min, uses laser particle analyzer
Detection, is guaranteed number≤1000 of the tiny component of detection per second, obtains analytical data by regulation flow velocity；
(3) analytical data drawn according to step (2), can draw retention agent keeps effect.
The present invention includes sample concentration, speed of agitator through the treatment conditions of DDJ simulation auxiliary agent retention process
And several factors such as mixing time, concrete setting value in systems may according to filtrate during paper machine operation
The excursion of each condition being subject to.
Preferably, the rotating speed of step (1) described dynamic drainage instrument is 300～750r/min.
Preferably, the mass concentration of step (1) described slurry is 0.3%～0.5%, based on over dry.
Preferably, step (2) is diluted with ultra-pure water, and extension rate is 100～10000 times.
Preferably, the dyeing time described in step (2) is 5min.Wherein, described stain is a kind of
Have the tracer of specific stain to tiny component, this tracer color is red, is slightly soluble in water and has
Volatility.
Preferably, the number of step (2) described laser particle analyzer detection per second granule is 100～900.
The operation principle of the present invention is tiny component and tracer is all lyophobic dust, and paper pulp is hydrophilic
Material, the most hydrophobic tiny component surface can adsorb tracer, due to amount and the dyeing of tiny component
Agent adsorbance is proportional, therefore can come the most anti-with the change of tiny Individual uptake by stain
Reflect the change of tiny constituent content in slurry.When tiny component particles electronegative in pulp suspension is caught
After fluorescent dye, under the Stabilization of laser particle analyzer propulsion plant, it is single-row for making sample, and every tiny
Component particle passes sequentially through the laser irradiation area of instrument with the impartial time, by tiny group of fluorescent dyeing
Divide and send scattered light signal and fluorescence signal after being illuminated, after electricity system gathers, be transformed into electricity letter
Number, after professional software processes, obtain the information such as quantity and size of tiny component.
Compared with prior art, the invention have the advantages that
(1) tiny constituent content in filtrate after DDJ filters is detected by the present invention, testing result
Preferably being detected by laser particle analyzer, result characterizes with tiny component size and number, result accurately,
Error is little, intuitively and beneficially discriminatory analysis, tiny constituent content in filtrate during can using auxiliary agent
Change detects timely and effectively, thus draws the retention agent treatment effect to paste system, determines auxiliary agent
Using effect and result of practical application have good concordance, factory is selected and application retention agent by the method
Having preferable directive function, trend and the detection that can monitor wet end are not normal, control and maintain wet end chemistry to put down
Weighing apparatus, solves the abnormal phenomena in producing.
(2) the method operating procedure of the present invention is simple, respectively affects when can fully simulate paper machine operation in system
Condition in factor span so that testing result is credible and has actuality.
Detailed description of the invention
For being best understood from the present invention, below in conjunction with example, the present invention is described in further details, but this
Bright claimed scope is not limited thereto.
Embodiment 1
A kind of detect the method that effect kept in paper pulp by retention agent, specifically comprise the following steps that
First, take certain paper plant's newspaper machine without filler and the paper pulp of paper making additive, be configured to slurry over dry
Amount is the solution 500ml of 1.5g, and discongests 9000 turns with standard slurry fluffer.Then adjust with NaCl
The electrical conductivity saving the slurry after discongesting is 2000 μ s/cm, regulates with NaOH and hydrochloric acid and discongests disposed slurry pH
Value is 7.5.
After regulating slurry, add the filler CaCO of 30%3, by slurry and CaCO3Stir addition
In dynamic drainage instrument (DDJ), the retention agent (cationic tapioca slag) being subsequently adding different amounts stirs
Mixing, treatment conditions are: rotating speed 750r/min, and mixing time is 20s, and last turn on agitator collects filtrate.
The filtrate drawing 10 μ l with liquid rifle joins in sample cell, then draws 80 μ l ultra-pure waters with liquid rifle
Join in sample cell, shake up and draw 10 μ l stain (being mainly composed of Nile red) with liquid rifle afterwards and add
Entering in sample cell, concussion shakes up, and lucifuge places 5min, finally draws 900 μ l ultra-pure waters with liquid rifle and adds
Enter in sample cell, shake up, prepare complete, then detect with laser particle analyzer, regulation detection flow velocity
It it is 1000 granule/seconds.Recording the content of tiny component in blank sample is 4.124 × 106Individual/mL,
The average-size of grain is 3.52 μm, and when retention agent consumption is 0.5%, the content of tiny component is 1.670 × 106
Individual/mL, the average-size of granule is 3.85 μm.And record blank by DDJ with ultraviolet spectrophotometer
In sample, the first-past retention of tiny component is 58.3%, the one way of tiny component after the retention agent of addition 0.5%
Retention is 71.5%.
By the above results it can be seen that the knot that records of the method for the result recorded by traditional method and the present invention
Fruit is consistent.After adding retention agent, in filtrate, most tiny component is stayed on filter screen, tiny in filtrate
The content of component tails off, and improves the poly-degree of wadding of fiber fines after being simultaneously introduced retention agent, putting down of granule
All become large-sized.
Embodiment 2
A kind of detect the method that effect kept in paper pulp by retention agent, specifically comprise the following steps that
Taking certain paper plant's newspaper machine without filler and the paper pulp of paper making additive, being configured to slurry oven-dry weight is
The solution 500ml of 1.5g, and discongest 9000 turns with standard slurry fluffer.Then discongest with NaCl regulation
After the electrical conductivity of slurry be 2000 μ s/cm, regulate with NaOH and hydrochloric acid and discongest disposed slurry pH value and be
5～10, after regulating slurry, add the filler CaCO of 30%3, so by slurry and CaCO3Stir
Adding in dynamic drainage instrument (DDJ), the retention agent being subsequently adding certain consumption is stirred, treatment conditions
For: rotating speed is 750r/min, and mixing time is 20s, and last turn on agitator collects filtrate.
The filtrate drawing 10 μ l with liquid rifle joins in sample cell, then draws 80 μ l ultra-pure waters with liquid rifle
Join in sample cell, shake up and draw 10 μ l stain (being mainly composed of Nile red) with liquid rifle afterwards and add
Entering in sample cell, concussion shakes up, and lucifuge places 5min, finally draws 900 μ l ultra-pure waters with liquid rifle and adds
Enter in sample cell, shake up, prepare complete, then detect with laser particle analyzer, regulation detection flow velocity
It is 1000 granule/s.Recording the content of tiny component when pH is 5,6 is 7.100 × 106Individual/mL and
4.412×106Individual/mL, the average-size of granule is respectively 1.729 μm and 3.194 μm；It is 7 Hes at pH
When 8, the quantity of tiny component is respectively 1.916 × 106Individual/mL and 2.266 × 106Individual/mL, granule average
A size of 4.348 μm and 7.372 μm；When pH is 10, the quantity of tiny component is respectively 3.252 × 106
Individual/mL, the average-size of granule is 4.196 μm.And record pH by DDJ with ultraviolet spectrophotometer
Be 5,6 first-past retention be respectively 89.8%, 90.4%, pH is the one way of 7,8,10 tiny components
Retention is 90.9%, 90.5%, 89.9%.
By the result of embodiment 2 it can be seen that the method for the result recorded by traditional method and the present invention is surveyed
The result obtained is consistent.PH be the tiny constituent content under conditions of 7 and 8 than other pH under the conditions of
Tiny constituent content few, the average-size of granule is big.Can be seen that simultaneously and can be examined by laser particle analyzer
Measure the content of retention agent tiny component under condition of different pH and the poly-feelings of wadding of size distribution and granule
Condition.
Embodiment 3
A kind of detect the method that effect kept in paper pulp by retention agent, specifically comprise the following steps that
Taking certain paper plant's newspaper machine without filler and the paper pulp of paper making additive, being configured to slurry oven-dry weight is
The solution 500ml of 1.5g, and discongest 9000 turns with standard slurry fluffer.Then discongest with NaCl regulation
After the electrical conductivity of slurry be 2000 μ s/cm, regulating with NaOH and hydrochloric acid and discongesting disposed slurry pH value is 7.5,
After regulating slurry, add the filler CaCO of 30%3, by slurry and CaCO3Stir addition dynamically
In drainage instrument (DDJ), the retention agent being subsequently adding certain consumption is stirred, and treatment conditions are: rotating speed
500～3000r/min, mixing time is 20s, and last turn on agitator collects filtrate.
The filtrate drawing 10 μ l with liquid rifle joins in sample cell, then draws 80 μ l ultra-pure waters with liquid rifle
Join in sample cell, shake up and draw 10 μ l stain (being mainly composed of Nile red) with liquid rifle afterwards and add
Entering in sample cell, concussion shakes up, and lucifuge places 5min, finally draws 900 μ l ultra-pure waters with liquid rifle and adds
Enter in sample cell, shake up, prepare complete, then detect with laser particle analyzer, regulation detection flow velocity
It is 1000 granule/s.Record speed of agitator when being 500r/min, the tiny component in filtrate after filter
Content is 1.014/mL, and the average-size of granule is 3.59 μm；When 2000r/min after filter in filtrate
The content of tiny component be 5.220/mL, the average-size of granule is 2.60 μm.And pass through DDJ
When being 500r/min with ultraviolet spectrophotometer measuring rotating speed, the first-past retention of tiny component is 98.6%,
During 2000r/min, the first-past retention of tiny component is 78.3%.
By the result of embodiment 3 it can be seen that the method for the result recorded by traditional method and the present invention is surveyed
The result obtained is consistent.In shearing force hour filtrate, the comparision contents of tiny component is few, the average chi of granule
Very little bigger, the poly-degree of wadding of tiny component is bigger.Can be seen that simultaneously and can be examined by laser particle analyzer
Measure the retention agent content of tiny component and wadding of size distribution and granule under the conditions of different shearing forces to gather
Situation.
Claims (6)
1. one kind is detected the method that effect kept in paper pulp by retention agent, it is characterised in that include following step
Rapid:
(1) dynamic drainage instrument poured into by the slurry after discongesting, and setting speed is 300～3000r/min, adds
Enter retention agent, after stirring 10～60s, collect filtrate；
(2) above-mentioned filtrate is after dilution, adds stain lucifuge dyeing 3～10min, uses laser particle analyzer
Detection, is guaranteed number≤1000 of the tiny component of detection per second, obtains analytical data by regulation flow velocity；
(3) analytical data drawn according to step (2), can draw retention agent keeps effect；Described
Stain is mainly composed of Nile red.
Method the most according to claim 1, it is characterised in that: step (1) described dynamic drainage instrument
Rotating speed be 300～750r/min.
Method the most according to claim 1, it is characterised in that: the quality of step (1) described slurry
Concentration is 0.3%～0.5%, based on over dry.
Method the most according to claim 1, it is characterised in that: step (2) carries out dilute with ultra-pure water
Releasing, extension rate is 100～10000 times.
Method the most according to claim 1, it is characterised in that: during dyeing described in step (2)
Between be 5min.
Method the most according to claim 1, it is characterised in that: step (2) described laser particle analyzer
The number of detection granule per second is 100～900.
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| CN107271381B (en) * | 2017-05-25 | 2019-08-20 | 华南理工大学 | A kind of method of quick detection nano-cellulose retention in paper |
| CN108497543B (en) * | 2018-03-30 | 2021-05-14 | 昆明理工大学 | Method for evaluating retention effect of retention aid on paper-making reconstituted tobacco slurry |
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| DE4040463A1 (en) * | 1990-12-18 | 1992-06-25 | Basf Ag | MEASUREMENT METHOD FOR DETERMINING RESIN PARTICLES IN PAPER MATERIALS |
| US20090260767A1 (en) * | 2003-04-14 | 2009-10-22 | Every Penny Counts, Inc. | Use of hydrophobic dyes to monitor hydrophobic contaminants in a papermaking process |
| CN1280482C (en) * | 2004-10-10 | 2006-10-18 | 山东轻工业学院 | Method for raising rate of retaining paper stock |
| JP4389991B2 (en) * | 2007-10-26 | 2009-12-24 | ソニー株式会社 | Method and apparatus for optical measurement of fine particles |
| CN101333787B (en) * | 2008-07-28 | 2011-07-20 | 山东轻工业学院 | Method for controlling pitch trouble in paper-making process |
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| CF01 | Termination of patent right due to non-payment of annual fee |