CN105542194B - Dissolve sodium hydroxide/sodium cyclohexylsulfamate aqueous solvent system of pulp cellulose - Google Patents
Dissolve sodium hydroxide/sodium cyclohexylsulfamate aqueous solvent system of pulp cellulose Download PDFInfo
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- CN105542194B CN105542194B CN201610135569.8A CN201610135569A CN105542194B CN 105542194 B CN105542194 B CN 105542194B CN 201610135569 A CN201610135569 A CN 201610135569A CN 105542194 B CN105542194 B CN 105542194B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L1/00—Compositions of cellulose, modified cellulose or cellulose derivatives
- C08L1/02—Cellulose; Modified cellulose
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/02—Cellulose; Modified cellulose
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Abstract
The invention discloses a kind of sodium hydroxide/sodium cyclohexylsulfamate aqueous solvent system for dissolving pulp cellulose.Sodium hydroxide/sodium cyclohexylsulfamate aqueous solvent system of present invention dissolving pulp cellulose, the dissolving pulp of different weight percent concentration is put into 7%NaOH solution, then adds sodium cyclohexylsulfamate according to the percentage by weight of oven dry stock；Wherein relative to the oven dry stock of 1g mass, the control of addition sodium cyclohexylsulfamate is 16% 20%.The dissolving of the low high polymerization degree cellulosic molecule of accessibility in cellulosic molecule is promoted using the cellulose aqueous solution dicyandiamide solution of the present invention.
Description
Technical field
The present invention relates to the sodium hydroxide of cellulose/additive aqueous solvent system, more particularly to dissolving pulp fibres
Sodium hydroxide/sodium cyclohexylsulfamate aqueous solvent system of element.
Background technology
High polymer material environmental pollution is synthesized with the worsening shortages of petroleum resources and using oil as raw material increasingly
Aggravate, the natural polymer cellulose most abundant as annual production on the earth is increasingly valued by people.Hinder at present fine
The wide variety of key issue of dimension element is to find the feasible dicyandiamide solution of industrialization that i.e. environmentally friendly and can preferably dissolves cellulose.
The solvent of dissolving cellulose has aqueous solvent and the major class of nonaqueous solvents two.The original such as environmental pollution caused by some solvent recoveries
Cause, N-methylmorpholine-N- oxides (NMMO), ionic liquid and sodium hydroxide water solvent system are considered as preferable green
Dicyandiamide solution.Only NMMO has been truly realized the industry of casing packing film in the Viskase companies of Chicago,U.S at present
Metaplasia is produced.But NMMO costs are higher, and there are strict requirements to water content and solution temperature, while NMMO work is used in the U.S.
Factory's personnel casualty accidentses caused by its blast also happen occasionally.Ionic liquid is also because high production cost fails to obtain widely
Industrialized production.And NaOH water system dissolution in low temperature cellulose systems cause extensively because of the characteristics of its is inexpensive environmentally friendly, dissolving is quick
Concern.The researchers such as Tokyo Univ Japan, domestic Wuhan University, Donghua University, Zhejiang University, Chinese University of Science and Technology pass through
Added in the NaOH aqueous solution in terms of urea, thiocarbamide, polyethylene glycol (PEG) etc. prepare material of regenerated cellulose dissolving cellulose
There is comparison system in-depth study.At present using cellulose solvent systems such as NaOH/ urea, NaOH/ thiocarbamides in laboratory
Novel cellulose silk, film, chromatographic column filler, composite and cellulose derivative etc. are prepared, and has successfully been spun by pilot scale
Silk.Compared with pure cerium hydroxide sodium solution, the addition of NaOH aqueous solution small molecular compounds and medium molecule changes to a certain extent
It has been apt to the solvability of this system and the stability of the cellulose solution of generation.But the system is divided soluble cellulose
Son amount and concentration have certain limitation, and the unstable easy gel of cellulose solution after dissolving, also have one from the industrialization of film forming
Segment distance.French researcher Nicolas Le Moigne in 2009 et al. have studied lumber fibre cellulose fiber in the NaOH aqueous solution
In dissolution mechanism, the results showed that sodium hydrate aqueous solution to the degree of polymerization of the solvability of cellulose chain independent of cellulose,
And it is relevant with the chemical environment residing for cellulose molecular chain in fibre structure, as long as retaining the prototype structure form of natural fiber
(i.e. retain cellulose Ⅰ cell configuration), timber, cotton, the dissolving machine of other strings and some fibre element derivative as far as possible
Reason is almost identical.
With the quick rise of cotton price, from now in addition to cotton linter (cotton linter), with timber and bamboo
Dissolving pulp etc. the high cellulose content of plant production will play the part of prior role in the raw material of industry.Dissolving pulp has high
The bleach chemical pulp of content of cellulose, higher brightness and uniform molecular weight distribution.Different from paper grade (stock) pulp, dissolving pulp pair
The form and intensity of pulp fibers do not require, but to the degree of polymerization and chemical composition of fiber, particularly alpha-cellulose content
(i.e. the non-cellulosic carbohydrate of cellulose and alkali resistant) and whiteness have higher requirement.Dissolving pulp can be processed into viscose glue fibre
Dimension, glassine paper, pharmaceuticals industry sterilising filtration paper, acetate fiber, nitrocellulose, carboxymethyl cellulose, microcrystalline cellulose, cellulose
Ether etc. and be widely used in the field such as textile and tire, thickener, paint, cigarette filter, medicine, food, casing, cosmetics.
Recent decades scientists all think that whether cellulose dissolves the physical arrangement and alkali all with cellulose in the NaOH aqueous solution
Concentration is relevant, and the cellulose that can be dissolved is typically all the high low polymerization degree cellulose of accessibility.I do recently with dissolving
The dissolving of pulp cellulose it is relevant test result indicates that, choose the suitable additive with hydrogen bond receptor and hydrogen bond donor very
The dissolving of the high polymerization degree cellulosic molecule that accessibility is low in cellulosic molecule may be promoted.
The content of the invention
In view of the above fact, the present invention provides a kind of sodium hydroxide/sodium cyclohexylsulfamate water for dissolving pulp cellulose
Solution solvent system, it not only have developed a kind of new sodium hydroxide/additive aqueous solution cellulose solvent system, and the fibre
Tie up plain dicyandiamide solution and the aqueous solution cellulose solvent body such as NaOH/ urea (or thiocarbamide) is better than to the solvability for dissolving pulp cellulose
System.
Sodium hydroxide/sodium cyclohexylsulfamate aqueous solvent system of the dissolving pulp cellulose of the present invention, by difference
The dissolving pulp of weight percent concentration is put into 7%NaOH solution, then adds cyclohexyl according to the percentage by weight of oven dry stock
Sulfamic acid sodium；Wherein relative to the oven dry stock of 1g mass, addition sodium cyclohexylsulfamate control is in 16%-20%；Hexamethylene
The addition of base sulfamic acid sodium can select desired value according to species, the degree of polymerization, alpha-cellulose content of dissolving pulp etc..For acid
Property sulphite process needlebush dissolving pulp for, 7%NaOH/20% sodium cyclohexylsulfamates aqueous solvent system dissolving effect
Fruit is optimal；For prehydrolytic sulfate process needlebush dissolving pulp, the 7%NaOH/16% sodium cyclohexylsulfamate aqueous solution
Dicyandiamide solution solute effect is optimal；For leaf wood dissolving pulp, the 7%NaOH/20% sodium cyclohexylsulfamate aqueous solution
Dicyandiamide solution solute effect is optimal；For bamboo dissolved pulp, 7%NaOH/20% sodium cyclohexylsulfamate aqueous solution solvents
System solute effect is optimal.
Described dissolving pulp includes needlebush dissolving pulp, the broad-leaved that acid sulfite process or prehydrolytic sulfate process produce
Wooden dissolving pulp or bamboo dissolved pulp.
The degree of polymerization of described dissolving pulp is 650-1500.
Described dissolving pulp dissolving pulp alpha-cellulose content >=92%.
Compared with prior art, the beneficial effects of the invention are as follows：
1st, for the dissolving pulp of identical weight percent concentration, the cellulose aqueous solution dicyandiamide solution using the present invention is molten
The viscosity for solving the cellulose solution of its generation significantly improves.
2nd, the low high polymerization of accessibility in cellulosic molecule is promoted using the cellulose aqueous solution dicyandiamide solution of the present invention
Spend the dissolving of cellulosic molecule.
Embodiment
Present disclosure is described in more detail below in conjunction with specific embodiment.In addition, removed in this specification
Non-specifically record, otherwise for concentration etc. all on the basis of weight, number range includes end points.
Experiment 1. is applied to needlebush dissolving pulp
Embodiment 1：It is 97.3% to select content of cellulose, and the acid sulfite process needlebush that degree of polymerization DP is 1520 is molten
Solution slurry.So that 2% slurry is dense as an example, dissolving pulp and 7%NaOH are added in transparent sample bottle, adds 20% (based on oven dry stock
Percentage by weight) sodium cyclohexylsulfamate.It is sufficiently stirred after scattered swollen after being put into the storage 2 hours of (- 12 DEG C) of refrigerator low temperature,
Defrosting stirring obtains dissolving pulp cellulose dissolution system, is then centrifuged for separating, and extracts upper strata transparency cellulose solution 0.9-1.0
Type determination of ubbelohde viscometer its viscosity, viscosity size are represented with the relative time passed through.Undissolved part passes through alkaline-resisting core
Funnel is filtered, and is transferred to after washing neutrality in frosting ware, and it is compacted to pressing under wet condition with 2 cover glasses,
Room temperature is weighed after air-drying to calculate the dissolving percentage of dissolving pulp cellulose.Then the vacuum drying oven of drier is put it into again
XRD analysis are done after drying water removal completely.
Comparative example 1：Only use the 7%NaOH aqueous solution, do not add sodium cyclohexylsulfamate, it is other it is same as Example 1 enter
The observation of row dissolving pulp cellulose dissolution effect.
As comparative example 2,7%NaOH/12% aqueous solution of urea only is used, does not add sodium cyclohexylsulfamate, Qi Tayu
The identical observation for carrying out dissolving pulp cellulose dissolution effect of embodiment 1.
As comparative example 3,9.5%NaOH/4.5% thiourea solutions do not add sodium cyclohexylsulfamate, it is other with it is real
Apply the identical observation for carrying out dissolving pulp cellulose dissolution effect of example 1.
Table 1. tests the result of 1 embodiment 1
Table 1 represents that identical weight percentage starches the fibre generated after dense needlebush dissolving pulp dissolves in variety classes solvent
Tie up the viscosity and dissolving ratio of plain solution.The dissolving life of the sodium cyclohexylsulfamate aqueous solvent system of 7% sodium hydroxide/20%
Into the viscosity of cellulose solution significantly improve, dissolution rate also significantly increases, and shows molten using the cellulose aqueous solution of the present invention
Agent system promotes cellulosic molecule and preferably dissolved.
Embodiment 2：Content of cellulose is selected to be more than or equal to 93.55%, degree of polymerization DP is 1190 prehydrolytic sulfate process
Needlebush dissolving pulp.So that 2% slurry is dense as an example, dissolving pulp and 7%NaOH are added in transparent sample bottle, adds 8% (based on exhausted
The percentage by weight of dry pulp) sulfamic acid sodium.Other observations same as Example 1 for carrying out dissolving pulp cellulose dissolution effect.
Comparative example 1：The 7%NaOH aqueous solution only is used, does not add sulfamic acid sodium, it is other same as Example 1 to be dissolved
The observation of pulp cellulose solute effect.
As comparative example 2,7%NaOH/12% aqueous solution of urea only is used, does not add sulfamic acid sodium, other and embodiment 1
The identical observation for carrying out dissolving pulp cellulose dissolution effect.
As comparative example 3,9.5%NaOH/4.5% thiourea solutions, sulfamic acid sodium, other and embodiment 1 are not added
The identical observation for carrying out dissolving pulp cellulose dissolution effect.
Table 2. tests the result of 1 embodiment 2
Table 2 represents that identical weight percentage starches the fibre generated after dense needlebush dissolving pulp dissolves in variety classes solvent
Tie up the viscosity and dissolving ratio of plain solution.The dissolving life of the sodium cyclohexylsulfamate aqueous solvent system of 7% sodium hydroxide/16%
Into the viscosity of cellulose solution significantly improve, high viscosity and relatively low dissolution rate show water-soluble using the cellulose of the present invention
Liquid dicyandiamide solution promotes the dissolving of the low high polymerization degree cellulosic molecule of accessibility in cellulosic molecule.
Experiment 2. is applied to leaf wood dissolving pulp
Embodiment 1：It is >=92% to select content of cellulose, and degree of polymerization DP is 800 leaf wood dissolving pulp.It is dense with 2% slurry
Exemplified by, dissolving pulp and 7%NaOH are added in transparent sample bottle, adds 20% (percentage by weight based on oven dry stock) hexamethylene
Base sulfamic acid sodium.It is other identical with embodiment 1 in experiment 1..
As comparative example 1, the 7%NaOH aqueous solution only is used, does not add sodium cyclohexylsulfamate, it is other with the phase of embodiment 1
With the observation for carrying out dissolving pulp cellulose dissolution effect.
As comparative example 2,7%NaOH/12% aqueous solution of urea only is used, does not add sodium cyclohexylsulfamate, Qi Tayu
The identical observation for carrying out dissolving pulp cellulose dissolution effect of embodiment 1.
As comparative example 3,9.5%NaOH/4.5% thiourea solutions do not add sodium cyclohexylsulfamate, it is other with it is real
Apply the identical observation for carrying out dissolving pulp cellulose dissolution effect of example 1.
The result of the experiment of table 3. 2
Table 3 represents that identical weight percentage is starched after dense leaf wood dissolving pulp dissolves in variety classes solvent and generated
Cellulose solution viscosity and dissolving ratio.7% sodium hydroxide/20% sodium cyclohexylsulfamate aqueous solvent system is molten
The viscosity for solving the cellulose solution of generation significantly improves, and high viscosity and relatively low dissolution rate show to utilize cellulose of the invention
Aqueous solvent system promotes the dissolving of the low high polymerization degree cellulosic molecule of accessibility in cellulosic molecule.
Experiment 3. is applied to bamboo dissolved pulp
Embodiment 1：It is >=92% to select content of cellulose, the bamboo dissolved pulp that degree of polymerization DP is about 800.It is so that 2% slurry is dense
Example, dissolving pulp and 7%NaOH are added in transparent sample bottle, adds 20% (percentage by weight based on oven dry stock) cyclohexyl
Sulfamic acid sodium.It is other identical with embodiment 1 in experiment 1..
As comparative example 1, the 7%NaOH aqueous solution only is used, does not add sodium cyclohexylsulfamate, it is other with the phase of embodiment 1
With the observation for carrying out dissolving pulp cellulose dissolution effect.
As comparative example 2,7%NaOH/12% aqueous solution of urea only is used, does not add sodium cyclohexylsulfamate, Qi Tayu
The identical observation for carrying out dissolving pulp cellulose dissolution effect of embodiment 1.
As comparative example 3,9.5%NaOH/4.5% thiourea solutions do not add sodium cyclohexylsulfamate, it is other with it is real
Apply the identical observation for carrying out dissolving pulp cellulose dissolution effect of example 1.
The result of the experiment of table 4. 3
Table 4 represents that identical weight percentage starches the cellulose generated after dense bamboo dissolved pulp dissolves in variety classes solvent
The viscosity and dissolving ratio of solution.The dissolving generation of the sodium cyclohexylsulfamate aqueous solvent system of 7% sodium hydroxide/20%
The viscosity of cellulose solution significantly improves, and high viscosity and relatively low dissolution rate show to utilize the cellulose aqueous solution of the present invention molten
Agent system promotes the dissolving of the low high polymerization degree cellulosic molecule of accessibility in cellulosic molecule.
The present invention is sodium hydroxide/additive aqueous solvent system on cellulose, fine more particularly to dissolving pulp
Tie up sodium hydroxide/additive aqueous solvent system of element.Additive sodium cyclohexylsulfamate is that a kind of food additives are white
Color powder, is commonly called as honey element, is dissolved in water, solubility >=10g/100ml water in 20 DEG C of water；There is 1 hydrogen bond donor in molecule
With 4 hydrogen bond receptors, the effect for destroying hydrogen bond in cellulosic molecule can be preferably played.
Present invention dissolving cellulose object is in addition to dissolving pulp cellulose, cotton linter pulp, bleached wood pulp, microcrystalline cellulose
Can also, because the addition of the factor sodium cyclohexylsulfamates such as crystallinity, a content of cellulose differences will be in 16%-20% models
Optimum value is found in enclosing.
When implementing of the invention, compared with current 7%NaOH/12% aqueous solution of urea dicyandiamide solutions, the fibre of generation
The viscosity (being represented with the relative time second) for tieing up plain solution is improved more than about 2 times and (averagely must based on the hemicellulose in biomass
Rate).Compared with current 9.5%NaOH/4.5% thiourea solution dicyandiamide solutions, the viscosity of the cellulose solution of generation is (with phase
Second time is represented) improve about 3 times.
Claims (3)
1. a kind of sodium hydroxide/sodium cyclohexylsulfamate aqueous solvent system for dissolving pulp cellulose, it is characterized in that, will not
Dissolving pulp with weight percent concentration is put into 7%NaOH solution, then adds hexamethylene according to the percentage by weight of oven dry stock
Base sulfamic acid sodium；Wherein relative to the oven dry stock of 1g mass, the amount for adding sodium cyclohexylsulfamate is controlled in 16%-
20%；The dissolving pulp includes needlebush dissolving pulp, the leaf wood that prehydrolysis sulphite process or prehydrolytic sulfate process produce
Dissolving pulp or bamboo dissolved pulp；The degree of polymerization of the dissolving pulp is 650-1520.
2. sodium hydroxide/sodium cyclohexylsulfamate aqueous solution solvent body of dissolving pulp cellulose according to claim 1
System, it is characterized in that, dissolving pulp alpha-cellulose content >=92%.
3. sodium hydroxide/sodium cyclohexylsulfamate aqueous solution solvent body of dissolving pulp cellulose according to claim 1
System, it is characterized in that, for acid sulfite process needlebush dissolving pulp, using 7%NaOH/20% cyclohexylsulfamics
Sodium water solution dicyandiamide solution；For prehydrolytic sulfate process needlebush dissolving pulp, using 7%NaOH/16% cyclohexyl ammonia
Base sodium sulfonate aqueous solvent system；For leaf wood dissolving pulp, using 7%NaOH/20% sodium cyclohexylsulfamates
Aqueous solvent system；For bamboo dissolved pulp, using 7%NaOH/20% sodium cyclohexylsulfamate aqueous solution solvent bodies
System.
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| CN106185929A (en) * | 2016-07-19 | 2016-12-07 | 句容市百诚活性炭有限公司 | A kind of preparation method of the activated carbon with flourishing pore structure |
| CN111391352A (en) * | 2020-03-18 | 2020-07-10 | 天津商业大学 | Forming method of dissolving pulp fiber buffer packaging material |
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| CN1318575A (en) * | 2000-04-17 | 2001-10-24 | 武汉大学 | Solvent composition and its use |
| CN101135120A (en) * | 2007-09-17 | 2008-03-05 | 云南昌宁建星纸业有限公司 | Process for manufacturing natural antibiotic bamboo pulp by dendrocalamus giganteus non-sulfate method |
| CN102432891A (en) * | 2011-09-15 | 2012-05-02 | 喻翠云 | Method for dissolving cellulose |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1318575A (en) * | 2000-04-17 | 2001-10-24 | 武汉大学 | Solvent composition and its use |
| CN101135120A (en) * | 2007-09-17 | 2008-03-05 | 云南昌宁建星纸业有限公司 | Process for manufacturing natural antibiotic bamboo pulp by dendrocalamus giganteus non-sulfate method |
| CN102432891A (en) * | 2011-09-15 | 2012-05-02 | 喻翠云 | Method for dissolving cellulose |
Non-Patent Citations (2)
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| "有关氢键理论研究的现状及前景";王海燕等;《河北师范大学学报》;20050331;第29卷(第2期);第177-181页 * |
| "纤维素溶剂进展";吕昂等;《高分子学报》;20071031(第10期);第937-944页 * |
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