CN109142153A - A kind of cotton fiber Viscosity Analysis method - Google Patents
A kind of cotton fiber Viscosity Analysis method Download PDFInfo
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- CN109142153A CN109142153A CN201811405140.1A CN201811405140A CN109142153A CN 109142153 A CN109142153 A CN 109142153A CN 201811405140 A CN201811405140 A CN 201811405140A CN 109142153 A CN109142153 A CN 109142153A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N11/00—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties
- G01N11/02—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by measuring flow of the material
- G01N11/04—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by measuring flow of the material through a restricted passage, e.g. tube, aperture
- G01N11/06—Investigating flow properties of materials, e.g. viscosity, plasticity; Analysing materials by determining flow properties by measuring flow of the material through a restricted passage, e.g. tube, aperture by timing the outflow of a known quantity
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Abstract
The invention discloses a kind of cotton fiber Viscosity Analysis methods, comprising the following steps: (1) drying cotton fiber sample is dissolved in water, obtains test solution；(2) water and cupri-ethylene diamine solution are added into test solution, oscillation to test solution is completely dissolved；(3) test solution is injected in viscosimeter, solution is flowed out through viscosimeter, measures the delivery time；(4) viscosity ratio η is calculated according to the following formularatio: ηratio=h × t, wherein t is the delivery time for testing solution, and h is viscometer constant；(5) according to the viscosity than calculating viscosity number.Cotton fiber Viscosity Analysis method of the invention is compared with traditional cotton fiber Viscosity Analysis method, and analytical cycle is short and analysis result is more accurate.
Description
Technical field
The invention belongs to physico-chemical analysis fields, and in particular to a kind of cotton fiber Viscosity Analysis method.
Background technique
Cellulose ether production industry is usually using cotton fiber as raw material, wherein viscosity index is the key that cotton fiber
One of index.Traditional cotton fiber Viscosity Analysis method is dissolved in cotton fiber in ketone ammonia solution, flows through capillary by solution
Solution viscosity is calculated the time required to viscosimeter.In this method, cotton fiber longer (low viscous cotton the time required to being dissolved in ketone ammonia solution
Slurry needs 6-7 hours, and the viscous cotton pulp of height needs 12-14 hours), so as to cause cotton fiber Viscosity Analysis period longer (usually 8-
15 hours).In addition, high viscosity cotton fiber is easy to appear particle a small amount of undissolved or that dissolution is insufficient, may be influenced viscous
Spend precision of analysis.
Summary of the invention
The purpose of the present invention is to provide a kind of cotton fiber Viscosity Analysis methods, to overcome analysis existing in the prior art
Period is long, analyzes the problem of result inaccuracy.
To achieve the goals above, one aspect of the present invention provides a kind of cotton fiber Viscosity Analysis method, including following
Step: (1) being dissolved in water for drying cotton fiber sample, obtains test solution；(2) water is added into test solution and cupri ethylene diamine is molten
Liquid, oscillation to test solution are completely dissolved；(3) test solution is injected in viscosimeter, solution is flowed out through viscosimeter, measurement outflow
Time；(4) viscosity ratio η is calculated according to the following formularatio: ηratio=h × t, wherein t is the delivery time for testing solution, and h is
Viscometer constant；(5) according to the viscosity than calculating viscosity number.
Preferably, the test solution concentration in step (1) is 0.0024~0.0050g/ml.
Preferably, the duration of oscillation in step (2) is 15~20 minutes.
Preferably, in step (3), test solution flows out under the conditions of 25 DEG C through viscosimeter.
Preferably, the viscosimeter uses capillary viscometer.
Preferably, in step (5), according to the viscosities il and concentration with the viscosity than corresponding, known cotton fiber solution
The product η * c of c calculates the viscosity number of cotton fiber sample.
The cotton fiber Viscosity Analysis method of aforementioned aspect of the present invention is compared with traditional cotton fiber Viscosity Analysis method, analysis
Period is short and analysis result is more accurate.
Specific embodiment
Purpose and technical solution in order to enable those skilled in the art to better understand the present invention below will carry out the present invention
Clear, complete description.Obviously, described embodiment is a part of the embodiments of the present invention, instead of all the embodiments.
The description of this part be only it is exemplary and explanatory, should not have any restrictions effect to protection scope of the present invention.
Embodiments of the present invention provide a kind of cotton fiber Viscosity Analysis method, and this method is made molten using ketone second diamino
Agent can be realized cotton fiber in rapid dissolution wherein, and under the conditions of 25 DEG C, solution is flowed out through capillary viscometer, and record is logical
The time is spent, and is compared calculating with the numerical value of the cotton fiber solution of concentration with known-viscosity, to obtain cotton fiber sample
Viscosity.
The cotton fiber Viscosity Analysis method of embodiments of the present invention includes the following steps.
Step (1): drying cotton fiber sample (dry pulp) is dissolved in water, obtains test solution (slurry).
Specifically, firstly, the cotton fiber sample to selection is weighed, it is accurate to ± 0.5mg, it is ensured that sample, which has, to be represented
Property.
Secondly, test solution concentration is selected according to the following table 1, if it is not known that the general numerical value of the viscosity number of sample, can make
With solution of the concentration between 125mg/50ml~150mg/50ml.If the range of viscosity number obtained not in table 1
It is interior, solution concentration should be adjusted.
Table 1
| Viscosities il (ml/g) | Dry pulp weight (g) | It starches concentration c (g/ml) |
| < 400 | 0.25 | 0.0050 |
| 400~650 | 0.25 | 0.0050 |
| 650~850 | 0.20 | 0.0040 |
| 850~1100 | 0.15 | 0.0030 |
| 1100~1400 | 0.12 | 0.0024 |
For highly viscous accurate measurement, η * c should be as far as possible close to 3.0, and any situation is no more than 3.0 ± 0.1.If
The general viscosity of sample is not known, then should do an investigative test first, to select correct concentration.
Step (2): water and cupri-ethylene diamine solution being added into test solution, and oscillation to test solution is completely dissolved.
Specifically, it is drawn in such as 25ml distilled water or deionized water injection test solution with fat tripe pipette, is added simultaneously
Enter 5-10 piece (branch) copper wire, covers tightly bottle.With oscillator or the equipment of other same effect, violent vibration test liquid directly stops sample
It decomposes completely.
It is drawn in the cupri-ethylene diamine solution injection bottle of such as 25ml again, remaining gas is excluded with copper wire.Bottle is covered tightly again
Son is vibrated to test solution with oscillator be completely dissolved again.
Oscillation was for about 15 to 20 minutes.After slurry dissolution, bottle is immersed in water bath with thermostatic control to temperature reaches (25 ±
0.1) DEG C (about 20 minutes).Since oxygen has degradation to cellulose in cupri-ethylene diamine solution, it is careful to avoid
Cellulose in cupri ethylene diamine is contacted with air.This can be avoided by using the polyethylene degradation bottle with nut cap.
Step (3): by test solution injection viscosimeter, solution is flowed out through viscosimeter, measures the delivery time.
It specifically, will be in the test solution injection viscosimeter of sufficient amount of preparation with rubber pipette bulb.Solution is allowed to have no obstacle
Automatically (cleaning viscosity tube 2 to 3 times) is flowed out in ground.When meniscus is in upper graticule, start with manual time-keeping, until solution level arrives
When lower graticule (delivery time of solution), timing is accurate to 0.2S.It at least measures twice, measurement result relative mistake should be 2.5%
It is interior.Calculate average value.
Step (4): viscosity ratio η is calculated according to the following formularatio:
ηratio=η/η0=h × t, wherein
T- tests the delivery time of solution, and unit is the second.
H- viscometer constant, unit are (s per second-1) (calculation of h is shown in GB/T 1548-2004).
Step (5): according to the viscosity than calculating viscosity number.
By calculated viscosity ratio, corresponding η * c can be found in the following Table 2.Viscosity number η is calculated, is accurate to
1ml/g。
Calculated examples:
C=0.0024g/ml=dry pulp weight/copper second diamino ml=0.12g/50ml
The delivery time of t=100s test solution
H=0.0821s-1Constant (by proofreading obtained standard value)
Viscosity ratio ηratio=t*h=100*0.0821=8.21
It is 2.967 that η * c numerical value corresponding with 8.21 is found from table 2
Viscosities il (ml/g)=2.967/c=2.967/0.0024=1236ml/g ≈ 1235ml/g
Table 2
In order to compare the cotton fiber Viscosity Analysis method and traditional cotton fiber Viscosity Analysis method of embodiment of the present invention
Accuracy, the present inventor have carried out following control experiment.
6 inherent viscosities (cotton fiber viscosity of embodiment of the present invention point has been done respectively to the sample of identical high viscous Article Number
The viscosity that analysis method obtains) control experiment with traditional viscosity (viscosity that traditional cotton fiber Viscosity Analysis method obtains), data
As shown in table 5, the reproducibility of inherent viscosity is fine (difference between peak and minimum is only 50) as can be seen from the table,
And the reproducibility of traditional viscosity is general (difference between peak and minimum is 146), it was demonstrated that inherent viscosity is than tradition more viscous
The analysis result of degree is more stable, accuracy is higher.
Table 3
| Lot number | Article Number | Inherent viscosity | Traditional viscosity |
| S2012-CELL-200 | CP2400 | 2180 | 1925.377 |
| S2012-CELL-200 | CP2400 | 2210 | 1945.858 |
| S2012-CELL-200 | CP2400 | 2210 | 1876.527 |
| S2012-CELL-200 | CP2400 | 2210 | 1891.895 |
| S2012-CELL-200 | CP2400 | 2210 | 1991.553 |
| S2012-CELL-200 | CP2400 | 2230 | 2022.539 |
In addition, the analysis speed of inherent viscosity is faster compared with the analysis time of traditional viscosity.When the analysis of traditional viscosity
Between all relatively long, 8h is at least needed to go out for the viscosity of low viscous Article Number as a result, and the viscosity of high viscous Article Number is even more to need 15h that could go out to tie
Fruit, and the analysis time of inherent viscosity greatly reduces compared to the analysis time of traditional viscosity, comes out from test is started to result
It is only necessary to 1h.The situation that can know viscosity more in time in this way, preferably controls intermediate products.
The foregoing is merely preferable embodiments of the invention, are not intended to limit the invention, all in the present invention
Spirit and principle within made any modification, equivalent replacement, improvement etc., should be included in protection scope of the present invention it
It is interior.
Claims (6)
1. a kind of cotton fiber Viscosity Analysis method, which comprises the following steps:
(1) drying cotton fiber sample is dissolved in water, obtains test solution；
(2) water and cupri-ethylene diamine solution are added into test solution, oscillation to test solution is completely dissolved；
(3) test solution is injected in viscosimeter, solution is flowed out through viscosimeter, measures the delivery time；
(4) viscosity ratio η is calculated according to the following formularatio:
ηratio=h × t,
Wherein, t is the delivery time for testing solution, and h is viscometer constant；
(5) according to the viscosity than calculating viscosity number.
2. cotton fiber Viscosity Analysis method according to claim 1, which is characterized in that the test solution in step (1) is dense
Degree is 0.0024~0.0050g/ml.
3. cotton fiber Viscosity Analysis method according to claim 1 or 2, which is characterized in that the duration of oscillation in step (2)
It is 15~20 minutes.
4. cotton fiber Viscosity Analysis method according to any one of claim 1-3, which is characterized in that in step (3),
Test solution flows out under the conditions of 25 DEG C through viscosimeter.
5. cotton fiber Viscosity Analysis method described in any one of -4 according to claim 1, which is characterized in that the viscosimeter is adopted
Use capillary viscometer.
6. cotton fiber Viscosity Analysis method according to any one of claims 1-5, which is characterized in that in step (5),
, than the viscosities il of corresponding, known cotton fiber solution and the product η * c of concentration c, cotton fiber sample is calculated according to the viscosity
Viscosity number.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811405140.1A CN109142153A (en) | 2018-11-22 | 2018-11-22 | A kind of cotton fiber Viscosity Analysis method |
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| CN201811405140.1A CN109142153A (en) | 2018-11-22 | 2018-11-22 | A kind of cotton fiber Viscosity Analysis method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023222945A1 (en) * | 2022-05-16 | 2023-11-23 | Teknologian Tutkimuskeskus Vtt Oy | Estimating the viscosity of textile materials |
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| CN101551317A (en) * | 2009-05-14 | 2009-10-07 | 宜宾海丝特纤维有限责任公司 | Measuring method for viscosity of alkali cellulose |
| JP2012073089A (en) * | 2010-09-28 | 2012-04-12 | Gunze Ltd | Method for measuring degree of polymerization of cellulose |
| CN102967535A (en) * | 2011-09-01 | 2013-03-13 | 中国制浆造纸研究院 | Method for rapidly detecting viscosity of paper pulp |
| CN104407238A (en) * | 2014-05-20 | 2015-03-11 | 国家电网公司 | Oil paper insulation thermal aging life assessment method based on time temperature water superposition method |
| CN106442225A (en) * | 2016-10-09 | 2017-02-22 | 哈尔滨理工大学 | Diffusion measurement evaluation method for water in oil paper of oil-immersed transformer |
| CN108414398A (en) * | 2018-05-21 | 2018-08-17 | 亚太森博（山东）浆纸有限公司 | A kind of pulp viscosity detection method and device |
-
2018
- 2018-11-22 CN CN201811405140.1A patent/CN109142153A/en not_active Withdrawn
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101551317A (en) * | 2009-05-14 | 2009-10-07 | 宜宾海丝特纤维有限责任公司 | Measuring method for viscosity of alkali cellulose |
| JP2012073089A (en) * | 2010-09-28 | 2012-04-12 | Gunze Ltd | Method for measuring degree of polymerization of cellulose |
| CN102967535A (en) * | 2011-09-01 | 2013-03-13 | 中国制浆造纸研究院 | Method for rapidly detecting viscosity of paper pulp |
| CN104407238A (en) * | 2014-05-20 | 2015-03-11 | 国家电网公司 | Oil paper insulation thermal aging life assessment method based on time temperature water superposition method |
| CN106442225A (en) * | 2016-10-09 | 2017-02-22 | 哈尔滨理工大学 | Diffusion measurement evaluation method for water in oil paper of oil-immersed transformer |
| CN108414398A (en) * | 2018-05-21 | 2018-08-17 | 亚太森博（山东）浆纸有限公司 | A kind of pulp viscosity detection method and device |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2023222945A1 (en) * | 2022-05-16 | 2023-11-23 | Teknologian Tutkimuskeskus Vtt Oy | Estimating the viscosity of textile materials |
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| PB01 | Publication | ||
| PB01 | Publication | ||
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| SE01 | Entry into force of request for substantive examination | ||
| CB02 | Change of applicant information | ||
| CB02 | Change of applicant information |
Address after: 646605 High Dam in Longmatan District, Luzhou City, Sichuan Province Applicant after: North Tianpu Cellulose Co., Ltd. Address before: 646605 High Dam in Longmatan District, Luzhou City, Sichuan Province Applicant before: Northern Tian Pu Chemical Co., Ltd. |
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| WW01 | Invention patent application withdrawn after publication | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20190104 |