CN104132868A - Cellulose polymerization degree determination method - Google Patents
Cellulose polymerization degree determination method Download PDFInfo
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- CN104132868A CN104132868A CN201410338539.8A CN201410338539A CN104132868A CN 104132868 A CN104132868 A CN 104132868A CN 201410338539 A CN201410338539 A CN 201410338539A CN 104132868 A CN104132868 A CN 104132868A
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Abstract
The invention relates to a cellulose polymerization degree determination method. The cellulose polymerization degree determination method comprises the following steps of 1, stirring dimethyl sulfoxide and 1-ethyl-3-methylimidazolium acetate to obtain a uniform mixed solvent, 2, putting the mixed solvent into an Ubbelohde viscometer and measuring flowing time t0 of the mixed solvent in the Ubbelohde viscometer, 3, drying cellulose to be measured until weight is constant and adding the cellulose into the mixed solvent to obtain a cellulose solution having a concentration c, 4, putting the cellulose solution obtained by the step 3 into the Ubbelohde viscometer, putting the Ubbelohde viscometer with the cellulose solution into a thermostatic water bath having a temperature of 25 DEG C, carrying out thermostatic treatment for 20-30min, and determining flowing time t0 of the cellulose solution in the Ubbelohde viscometer, 5, calculating h<sp>/c according to the formula (I) and calculating an [Eta] value according to the formula (II), and 6, calculating a DP value according to the formula (III). The cellulose polymerization degree determination method has simple and easy processes, is free of expensive equipment, has a low cost, is convenient for use, has short determination time and produces accurate test data.
Description
Technical field
The present invention relates to polymerization degree measurement technical field, be specifically related to a kind of assay method of cellulosic degree of polymerization.
Background technology
The cellulosic molecule of cellulosic material is extremely long chain molecule, by D-glucopyranose base (C
6h
10o
5, dehydration glucose) form.In cellulosic molecule, the number of glucosyl group is called cellulosic degree of polymerization (DP).The size of cellulosic degree of polymerization characterizes the length of cellulose molecular chain and the power of cellulose intensity.Cellulosic degree of polymerization objectively quantitative response such as goes out to spin, knits, dyes at the degree of injury to fiber in actual process, is also an important indicator weighing fiber quality.
The method of measuring cellulosic degree of polymerization has end group chemical titration, boiling point rise method, osmometry, ultracentrifugal sedimentation method, diffusion method, light scattering method, viscosimetry, and wherein using simple method is viscosimetry.While adopting viscosimetry to measure cellulosic degree of polymerization, cellulose dissolution need be made in solvent to certain density cellulose solution.Up to now, dissolving cellulos solvent for use has copper ammon solution, cupri-ethylene diamine solution and cadmium ethylenediamine solution.Copper ammon solution and cupri-ethylene diamine solution all easily cause cellulosic severe oxidation degraded, and extremely unstable, difficult storage; And, prepare these two kinds of solution reagent used many, process for preparation is complicated, and preparation cycle is long; In addition,, owing to needing to add shot copper or copper sheet in dissolving cellulos process, cellulose can be clipped between shot copper or copper sheet, causes dissolving insufficient.By contrast, the stability of cadmium ethylenediamine solution is stronger, but also can cause cellulosic mild oxidation degraded.Obviously, with these dissolution with solvents celluloses, measure cellulosic degree of polymerization, except existing appeal defect, also can cause error relatively large, finally affect the accuracy of determination data.Although there is weak point, these solvents are still used so far, why like this, are because still there is no the alternative solvent that solute effect is better, performance is more stable.
Summary of the invention
The object of the invention is the deficiency for solving the problems of the technologies described above, a kind of assay method of cellulosic degree of polymerization is provided, use new alternative solvent (1-ethyl-3-methylimidazole acetate/dimethyl sulfoxide (DMSO) (EmimAc/DMSO)) dissolving cellulos, another reinforcing body cosolvent, be conducive to cellulosic whole dissolving, the accuracy of determination data is higher.
The present invention is the deficiency solving the problems of the technologies described above, and the technical scheme adopting is: a kind of assay method of cellulosic degree of polymerization, comprises the following steps:
(1) according to weight ratio 3:1, get dimethyl sulfoxide (DMSO) and 1-ethyl-3-methylimidazole acetate, 1-ethyl-3-methylimidazole acetate is added in dimethyl sulfoxide (DMSO), after stirring, obtain mixed solvent;
(2) get the mixed solvent that a part of step (1) obtains and pack in Ubbelohde viscometer, be then placed in the Water Tank with Temp.-controlled constant temperature 20～30min of 25 ℃, measure the flowing time t of mixed solvent in Ubbelohde viscometer
0;
(3) get cellulose to be measured and be dried to constant weight, then with cellulose proportionings different from mixed solvent, cellulose is added in mixed solvent, under 25～30 ℃ of conditions, stir 0.5～1h, obtain respectively the cellulose solution of variable concentrations c;
(4) cellulose solution that step (3) is obtained to variable concentrations is respectively charged in Ubbelohde viscometer, be then placed in 25 ℃ ℃ Water Tank with Temp.-controlled constant temperature 20～30min, the flowing time t of the cellulose solution of measuring variable concentrations in Ubbelohde viscometer;
(5) according to formula (I), calculate respectively the reduced viscosity value of variable concentrations cellulose solution
h sp/
c,according to formula (II), use again
η sp/
cc mapping is obtained to a fitting a straight line equation, the intercept of straight-line equation be inherent viscosity [
η];
Formula (I) is as follows:
，
Formula (II) is as follows:
；
(6) according to formula (III), calculate the degree of polymerization DP of cellulose solution, formula (III) is as follows:
。
beneficial effect
1, the solvent that the present invention uses can not cause cellulosic oxidative degradation, and during storage, stablize and do not decompose, non-corrosiveness, solvent preparation is fast and simple, and dissolution with solvents cellulose ability is strong;
2, assay method of the present invention is in cellulose dissolution process, and separately reinforcing body cosolvent, is conducive to cellulosic whole dissolving, thereby has improved the accuracy of determination data;
3, assay method of the present invention is easy to operation, does not need expensive device, and cost is low, easy to use, minute is short, and test data is accurate, practical, be applicable to the mensuration of unit to the cellulosic material degree of polymerization such as scientific research institution, universities and colleges, manufacturing enterprise.
Embodiment
An assay method for cellulosic degree of polymerization, comprises the following steps:
(1) according to weight ratio 3:1, get dimethyl sulfoxide (DMSO) and 1-ethyl-3-methylimidazole acetate, 1-ethyl-3-methylimidazole acetate is added in dimethyl sulfoxide (DMSO), after stirring, obtain mixed solvent;
(2) get the mixed solvent that 20ml step (1) obtains and pack in Ubbelohde viscometer (0.77mm Ubbelohde viscometer), be then placed in the Water Tank with Temp.-controlled constant temperature 25min of 25 ℃, measure the flowing time t of mixed solvent in Ubbelohde viscometer
0;
During mensuration, first with ear washing bulb, carefully mixed solvent is sucked in the spheroid of capillary viscometer upper end, when liquid level surpasses spheroid top graticule, decontrol ear washing bulb, treat that liquid level drops down onto the instantaneous beginning timing of top groove, stopwatch while reaching bottom groove to liquid level outflow spheroid, records delivery time t
0, continue in triplicate, average.
(3) get 1 g fibrous raw material, shred (length is no more than 1 mm), be placed in thermostatic drying chamber, at 102～105 ℃, be dried to constant weight, then get in the fibrous raw material and mixed solvent after constant weight, under 25 ℃ of conditions, stir 0.5h, respectively preparation to obtain concentration be the cellulose solution A of 0.3g/100 mL, the cellulose solution C of the cellulose solution B of 0.24g/100 mL, 0.18g/100 mL, the cellulose solution E of the cellulose solution D of 0.12g/100 mL and 0.06g/100 mL;
(4) cellulose solution (A-E) of 5 kinds of variable concentrations that step (3) obtained is respectively charged in Ubbelohde viscometer, be then placed in 25 ℃ ℃ Water Tank with Temp.-controlled constant temperature 20～30min, measure the flowing time t of cellulose solution in Ubbelohde viscometer
0;
During mensuration, first with ear washing bulb, carefully cellulose solution is sucked in the spheroid of capillary viscometer upper end, when surpassing spheroid top graticule, liquid level decontrols ear washing bulb, treat that liquid level drops down onto the instantaneous beginning timing of top groove, stopwatch while reaching bottom groove to liquid level outflow spheroid, record delivery time t, continue in triplicate, average.
(5) according to formula (I), calculate reduced viscosity value
h sp/
c,formula (I) is as follows:
，
Result is as shown in the table:
According to formula (II), formula (II) is as follows again:
; With
η sp/
cc mapping is obtained to a fitting a straight line equation, the intercept of straight-line equation be inherent viscosity [
η], [
η] be 1.7321;
(6) according to formula (III), calculate the degree of polymerization DP of cellulose solution, formula (III) is as follows:
; By [
η] be 1.7321, calculating DP is 437.
Claims (1)
1. an assay method for cellulosic degree of polymerization, is characterized in that: comprise the following steps:
(1) according to weight ratio 3:1, get dimethyl sulfoxide (DMSO) and 1-ethyl-3-methylimidazole acetate, 1-ethyl-3-methylimidazole acetate is added in dimethyl sulfoxide (DMSO), after stirring, obtain mixed solvent;
(2) get the mixed solvent that a part of step (1) obtains and pack in Ubbelohde viscometer, be then placed in the Water Tank with Temp.-controlled constant temperature 20～30min of 25 ℃, measure the flowing time t of mixed solvent in Ubbelohde viscometer
0;
(3) get cellulose to be measured and be dried to constant weight, then with cellulose proportionings different from mixed solvent, cellulose is added in mixed solvent, under 25～30 ℃ of conditions, stir 0.5～1h, obtain respectively the cellulose solution of variable concentrations c;
(4) cellulose solution that step (3) is obtained to variable concentrations is respectively charged in Ubbelohde viscometer, be then placed in 25 ℃ ℃ Water Tank with Temp.-controlled constant temperature 20～30min, the flowing time t of the cellulose solution of measuring variable concentrations in Ubbelohde viscometer;
(5) according to formula (I), calculate respectively the reduced viscosity value of variable concentrations cellulose solution
η sp/
c,according to formula (II), use again
η sp/
cc mapping is obtained to a fitting a straight line equation, the intercept of straight-line equation be inherent viscosity [
η];
Formula (I) is as follows:
，
Formula (II) is as follows:
；
According to formula (III), calculate the degree of polymerization DP of cellulose solution, formula (III) is as follows:
。
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| CN201410338539.8A CN104132868A (en) | 2014-07-16 | 2014-07-16 | Cellulose polymerization degree determination method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109187276A (en) * | 2018-09-25 | 2019-01-11 | 中国科学院过程工程研究所 | A kind of cellulose relative polymerization degree measuring method based on ion liquid solvent |
| CN111077123A (en) * | 2019-12-19 | 2020-04-28 | 齐鲁工业大学 | Method for rapidly determining average polymerization degree of cellulose based on fluorescence technology |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1154119A (en) * | 1995-03-31 | 1997-07-09 | 大赛璐化学工业株式会社 | Cellulose acetate having excellent physical strength and process for preparing the same |
| JP2012073089A (en) * | 2010-09-28 | 2012-04-12 | Gunze Ltd | Method for measuring degree of polymerization of cellulose |
| CN102565202A (en) * | 2011-12-29 | 2012-07-11 | 宜宾长毅浆粕有限责任公司 | Determination method of pulp polymerization degree distribution |
-
2014
- 2014-07-16 CN CN201410338539.8A patent/CN104132868A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1154119A (en) * | 1995-03-31 | 1997-07-09 | 大赛璐化学工业株式会社 | Cellulose acetate having excellent physical strength and process for preparing the same |
| JP2012073089A (en) * | 2010-09-28 | 2012-04-12 | Gunze Ltd | Method for measuring degree of polymerization of cellulose |
| CN102565202A (en) * | 2011-12-29 | 2012-07-11 | 宜宾长毅浆粕有限责任公司 | Determination method of pulp polymerization degree distribution |
Non-Patent Citations (3)
| Title |
|---|
| 杨之礼等: "纤维素新溶剂的研究_三_PF_DMSO溶剂测定纤维素聚合度的方法", 《广东化纤技术通讯》 * |
| 许爱荣: "阴离子功能化离子液体对生物质原料组分的溶解及选择性分离", 《CNKI优秀博士学位论文全文数据库》 * |
| 赵地顺等: "纤维素在离子液体1-丁基-3-甲基-咪唑乙酸盐中的溶解性能", 《化学工程》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109187276A (en) * | 2018-09-25 | 2019-01-11 | 中国科学院过程工程研究所 | A kind of cellulose relative polymerization degree measuring method based on ion liquid solvent |
| CN111077123A (en) * | 2019-12-19 | 2020-04-28 | 齐鲁工业大学 | Method for rapidly determining average polymerization degree of cellulose based on fluorescence technology |
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