CN108166089A - A kind of method that false indigo using salt-soda soil plantation prepares regenerated cellulose - Google Patents
A kind of method that false indigo using salt-soda soil plantation prepares regenerated cellulose Download PDFInfo
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- CN108166089A CN108166089A CN201711455101.8A CN201711455101A CN108166089A CN 108166089 A CN108166089 A CN 108166089A CN 201711455101 A CN201711455101 A CN 201711455101A CN 108166089 A CN108166089 A CN 108166089A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
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Abstract
The present invention relates to a kind of methods that cellulose extractive technique field more particularly to false indigo using salt-soda soil plantation prepare regenerated cellulose, prepare and post-process including pretreatment, Acid treatment, soda boiling processing, bleaching, spinning solution.The regenerated cellulose of better performances has been obtained using the preparation method of the present invention.
Description
Technical field
The present invention relates to chemical fiber fields more particularly to a kind of false indigo using salt-soda soil plantation to prepare regeneration
The method of cellulose.
Background technology
False indigo is a kind of perennial pulse family machaka, and since it has growth fast, reproductive capacity is strong, wide adaptability, resistance to
The characteristics such as saline-alkali water is wet in strand and saline-alkali wetland area, since false indigo has the function of to improve salt-soda soil, are used extensively
Make alkaline land soil improvement seeds.
The main chemical compositions of false indigo are cellulose, hemicellulose, lignin ash content, and part false indigo is used to make at present
Papermaking, fiberboard and composite plate are starched, some uses yule logs fuel, and energy utilization rate is low.Regenerated cellulose in the prior art
It is raw material mainly from wood pulp, bamboo pulp, cotton pulp, is prepared using viscose process or solvent method, but regenerated cellulose product performance one
As, therefore the present invention establishes a kind of method for preparing regenerated cellulose using false indigo for raw material.
Invention content
The technical problems to be solved by the invention are：In view of the deficienciess of the prior art, offer is a kind of to utilize salt-soda soil
The method that the false indigo of plantation prepares regenerated cellulose, can preferable regenerated cellulose product using this method available.
In order to solve the above technical problems, the technical scheme is that：
A kind of method that false indigo using salt-soda soil plantation prepares regenerated cellulose, the described method comprises the following steps：
(1) it pre-processes：False indigo is removed the peel, crush, be sieved, dry, is cooled down, obtains false indigo wood powder；
(2) Acid treatment：False indigo wood powder in step (1) is taken, adds in the mixed of organic solvent-organic acid-surfactant
Close liquid, stirring, heating boiling, cooling, filtering after the filter residue of collection is rinsed repeatedly with organic solvent, then are rinsed with deionized water；
(3) soda boiling is handled：Rinsed by organic solvent into step (2), added in the filter residue that deionized water is rinsed lye-
The mixed liquor of organic solvent by being ultrasonically treated, heats boiling, adding in bleaching agent after keeping the temperature a period of time reheats, by drift
Obtain false indigo pulp in vain；
(4) prepared by spinning solution：False indigo pulp in step (3) is taken, by impregnating, squeezing, crushing, experienced, yellow, molten
Deaeration and spinning solution is obtained by filtration in solution；
(5) it post-processes：Spinning solution is obtained into false indigo regeneration through coagulating bath spinning, traction molding, using refining, drying
Cellulose.
As an improvement technical solution, in step (2) in the mixed liquor of organic solvent-organic acid-surfactant
Organic solvent is ethyl alcohol, n-butanol or isopropanol；Organic acid is citric acid, tartaric acid or oxalic acid；Surfactant is dodecane
Base benzene sulfonic acid sodium salt or Tween-60.
As a kind of perferred technical scheme, the mixed liquor of the organic solvent-organic acid-surfactant is second
The mixed liquor of alcohol/isopropanol-tartaric acid-Tween-60.
As a kind of further preferred technical solution, the volumetric concentration of the ethyl alcohol is 65%-80%.
As an improvement technical solution, the temperature of boiling is 120-180 DEG C in step (2), and the time of boiling is 1-
3h。
As a kind of perferred technical scheme, temperature when step (3) is ultrasonically treated is 80-120 DEG C, time 1-4h,
The power of ultrasonic wave is 200-400w.
As an improvement technical solution, the mixed liquor of lye-organic solvent in step (3) is 0.5-1mol hydrogen-oxygens
Change the mixed liquor of sodium solution/potassium hydroxide solution-isopropanol.
As an improvement technical solution, in step (4) bleaching agent be tetraacetyl ethylene diamine, sodium hypochlorite, sulfurous acid
Sodium.
As a kind of perferred technical scheme, bleaching temperature is 60-100, bleaching time 1-2h in step (4).
As an improvement technical solution, the temperature of coagulating bath is 35-60 DEG C in step (6), and the composition of coagulating bath is
Sulfuric acid 80-120g/l, zinc sulfate 13-18g/l and sodium sulphate 325-350g/l, drafting multiple 1.6-2.0.
After employing above-mentioned technical proposal, the beneficial effects of the invention are as follows：
Compared with prior art, the present invention mainly has the following advantages：
The present invention is using the false indigo that salt-soda soil is planted as raw material, by Acid treatment after false indigo is crushed, add in ethyl alcohol-
Tartaric acid-Tween-60 mixed liquor, by thermophilic digestion, ethyl alcohol-tartaric acid-Tween-60 enters cell interior, and and groups of cells
It knits and comes into full contact with, increase the contact area of lignin and mixed liquor so that a large amount of lignin are degraded and are dissolved in ethyl alcohol, simultaneously
Also degrade part hemicellulose；The mixed liquor of sodium hydroxide solution/potassium hydroxide solution-isopropanol is added, by ultrasound
Processing and boiling processing, can destroy the cross-linked structure between cellulose and hemicellulose, make a large amount of hemicellulose degradations and be dissolved in
In isopropanol；By bleaching, the preparation and post processing of spinning solution, obtained purple fringe are carried out using false indigo pulp as raw material
Chinese scholartree regenerated cellulose has preferable performance, does by force in 2.01-2.15cN-dtex, wet by force in 1.05-1.18cN-dtex, does
State elongation at break is in 21.5-21.72%, and wet break elongation is in 12.83-12.89%, mechanical property and viscose rayon phase
When.
Specific embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
Example 1
A kind of method that false indigo of salt-soda soil plantation prepares regenerated cellulose, includes the following steps：
(1) it pre-processes：False indigo is removed the peel, crush, be sieved, dry, is cooled down, obtains false indigo wood powder；
(2) Acid treatment：False indigo wood powder in step (1) is taken, adds in the organic molten of false indigo wood powder 8 times of volumes of weight
Mixed liquor (mixed liquor of the volumetric concentration for 65% ethyl alcohol-tartaric acid-Tween-60, and second of agent-organic acid-surfactant
The volume ratio of alcohol, tartaric acid and Tween-60 is 1:1:0.5) it, stirs, heat temperature to 120 DEG C, boiling 1h, cooling, filtering are collected
Filter residue rinsed repeatedly with organic solvent after, then rinsed with deionized water；
(3) soda boiling is handled：It rinsed into step (2) by organic solvent, add in filter residue in the filter residue that deionized water is rinsed
Lye-the organic solvent of 5 times of volumes of weight mixed liquor (0.5mol sodium hydroxide solutions/potassium hydroxide solution-isopropanol it is mixed
Close liquid, and the volume ratio 1 of lye and isopropanol:1), heating temperature is to 80 DEG C, and the power of ultrasonic wave is under conditions of 200w, surpasses
Sonication 1h, is again heated to 130 DEG C of boiling 1h, and heat preservation 0.5h adds bleaching agent (tetraacetyl ethylene diamine mixed liquor), heating temperature
Degree most 60 bleaches 1h, obtains false indigo pulp；
(4) prepared by spinning solution：False indigo pulp in step (3) is taken, by impregnating, squeezing, crushing, experienced, yellow, molten
Deaeration and spinning solution is obtained by filtration in solution；
(5) it post-processes：Spinning solution is obtained into false indigo regeneration through coagulating bath spinning, traction molding, using refining, drying
The temperature of cellulose, wherein coagulating bath is 35 DEG C, and the composition of coagulating bath is sulfuric acid 80g/l, zinc sulfate 13g/l and sodium sulphate
325g/l, drafting multiple 1.6.
The false indigo regenerated cellulose that false indigo regenerated cellulose obtains under this process conditions does strong 2.01cN-dtex, wet
Strong 1.05cN-dtex, water free breaking elongation rate 21.5%, wet break elongation 12.83%.
Example 2
A kind of method that false indigo of salt-soda soil plantation prepares regenerated cellulose, includes the following steps：
(1) it pre-processes：False indigo is removed the peel, crush, be sieved, dry, is cooled down, obtains false indigo wood powder；
(2) Acid treatment：False indigo wood powder in step (1) is taken, adds in the organic molten of false indigo wood powder 10 times of volumes of weight
Mixed liquor (mixed liquor of the volumetric concentration for 70% ethyl alcohol-tartaric acid-Tween-60, and second of agent-organic acid-surfactant
The volume ratio of alcohol, tartaric acid and Tween-60 is 2:1:1) it, stirs, heat temperature to 135 DEG C, boiling 1.8h, cooling, filtering are collected
Filter residue rinsed repeatedly with organic solvent after, then rinsed with deionized water；
(3) soda boiling is handled：It rinsed into step (2) by organic solvent, add in filter residue in the filter residue that deionized water is rinsed
Lye-the organic solvent of 8 times of volumes of weight mixed liquor (mixed liquor of 0.6mol sodium hydroxide solutions-isopropanol, and lye with
The volume ratio 2 of isopropanol:1), heating temperature is to 90 DEG C, and the power of ultrasonic wave is under conditions of 280w, is ultrasonically treated 2h, then add
Heat adds bleaching agent (sodium hypochlorite) to 138 DEG C of boiling 1.5h, heat preservation 0.8h, and most 80 DEG C of heating temperature bleaches 1.5h,
Obtain false indigo pulp；
(4) prepared by spinning solution：False indigo pulp in step (3) is taken, by impregnating, squeezing, crushing, experienced, yellow, molten
Deaeration and spinning solution is obtained by filtration in solution；
(5) it post-processes：Spinning solution is obtained into false indigo regeneration through coagulating bath spinning, traction molding, using refining, drying
Cellulose；Wherein the temperature of coagulating bath is 43 DEG C, and the composition of coagulating bath is sulfuric acid 88g/l, zinc sulfate 14g/l and sodium sulphate
330g/l, drafting multiple 1.7.
Under this process condition, the false indigo regenerated cellulose obtained does strong 2.05cN-dtex, wet strong 1.08cN-dtex,
Water free breaking elongation rate 21.6%, wet break elongation 12.85%.
Example 3
A kind of method that false indigo of salt-soda soil plantation prepares regenerated cellulose, includes the following steps：
(1) it pre-processes：False indigo is removed the peel, crush, be sieved, dry, is cooled down, obtains false indigo wood powder；
(2) Acid treatment：False indigo wood powder in step (1) is taken, adds in the organic molten of false indigo wood powder 12 times of volumes of weight
Mixed liquor (the mixed liquor of isopropanol-tartaric acid-Tween-60, and ethyl alcohol, tartaric acid and spit of agent-organic acid-surfactant
The volume ratio of temperature -60 is 3.5:2:1) it, stirs, heat temperature to 155 DEG C, boiling 2.5h, cooling, filtering, the filter residue of collection is with having
After solvent is rinsed repeatedly, then rinsed with deionized water；
(3) soda boiling is handled：It rinsed into step (2) by organic solvent, add in filter residue in the filter residue that deionized water is rinsed
The mixed liquor of the lye-organic solvent of 12 times of volumes of weight be (0.8mol sodium hydroxide solutions/potassium hydroxide solution-isopropanol
Mixed liquor, and the volume ratio 3 of lye and isopropanol:1), heating temperature is to 115 DEG C, the power of ultrasonic wave under conditions of 365w,
3h is ultrasonically treated, 145 DEG C of boiling 2.5h is again heated to, the mixed liquor of sodium tripolyphosphate-sodium sulfite is added after heat preservation 1.2h,
Most 95 DEG C of heating temperature bleaches 1.8h, obtains false indigo pulp；
(4) prepared by spinning solution：False indigo pulp in step (3) is taken, by impregnating, squeezing, crushing, experienced, yellow, molten
Deaeration and spinning solution is obtained by filtration in solution；
(5) it post-processes：Spinning solution is obtained into false indigo regeneration through coagulating bath spinning, traction molding, using refining, drying
Cellulose；The temperature of coagulating bath is 52 DEG C, and the composition of coagulating bath is sulfuric acid 113g/l, zinc sulfate 17g/l and sodium sulphate 343g/l,
Drafting multiple is 1.9.
The false indigo regenerated cellulose obtained under this process condition does strong 2.15cN-dtex, wet strong 1.18cN-dtex,
Water free breaking elongation rate 21.72%, wet break elongation 12.89%.
Example 4
A kind of method that false indigo of salt-soda soil plantation prepares regenerated cellulose, includes the following steps：
(1) it pre-processes：False indigo is removed the peel, crush, be sieved, dry, is cooled down, obtains false indigo wood powder；
(2) Acid treatment：False indigo wood powder in step (1) is taken, adds in the organic molten of false indigo wood powder 15 times of volumes of weight
Mixed liquor (mixed liquor of the volumetric concentration for 80% ethyl alcohol-tartaric acid-Tween-60, and second of agent-organic acid-surfactant
The volume ratio of alcohol, tartaric acid and Tween-60 is 5:3:2) it, stirs, heat temperature to 180 DEG C, boiling 3h, cooling, filtering, collection
After filter residue is rinsed repeatedly with organic solvent, then rinsed with deionized water；
(3) soda boiling is handled：It rinsed into step (2) by organic solvent, add in filter residue in the filter residue that deionized water is rinsed
Lye-the organic solvent of 15 times of volumes of weight mixed liquor (mixed liquor of 1mol sodium hydroxide solutions-isopropanol, and lye with
The volume ratio 3.5 of isopropanol:1), heating temperature is to 120 DEG C, the power of ultrasonic wave under conditions of 400w, to be ultrasonically treated 4h, then
150 DEG C of boiling 3h are heated to, add sodium sulfite after keeping the temperature 1.5h, most 100 DEG C of heating temperature bleaches 2h, obtains purple fringe
Chinese scholartree pulp；
(4) prepared by spinning solution：False indigo pulp in step (3) is taken, by impregnating, squeezing, crushing, experienced, yellow, molten
Deaeration and spinning solution is obtained by filtration in solution；
(5) it post-processes：Spinning solution is obtained into false indigo regeneration through coagulating bath spinning, traction molding, using refining, drying
Cellulose；The temperature of coagulating bath is 58 DEG C, and the composition of coagulating bath is sulfuric acid 118g/l, zinc sulfate 17.5g/l and sodium sulphate 348g/
L, drafting multiple 2.0.
The false indigo regenerated cellulose obtained under this process condition of false indigo regenerated cellulose under this process condition
Dry strong 2.12cN-dtex, wet strong 1.16cN-dtex, water free breaking elongation rate 21.65%, wet break elongation are
12.87%.
In order to preferably prove that the preparation method using the present invention can obtain the regeneration of better performances to extract cellulose
Cellulose, the present invention have done 2 comparative examples simultaneously.
Comparative example 1
As different from Example 3, step (2) addition is the mixed liquor of ethyl alcohol and tartaric acid, remaining condition is identical, this
False indigo regenerated cellulose is dry by force in 1.78cN-dtex under process conditions, wet by force in 0.86cN-dtex, water free breaking elongation
Rate is 19.89%, and wet break elongation is 12.56%.
Comparative example 2
As different from Example 3, step (3) addition is ethyl alcohol and acid, is not ultrasonically treated, remaining condition phase
Together, under this process conditions false indigo regenerated cellulose it is dry by force in 1.74cN-dtex, it is wet by force in 0.82cN-dtex, dry state fracture
Elongation is 19.84%, and wet break elongation is 12.51%.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement made within refreshing and principle etc., should all be included in the protection scope of the present invention.
Claims (10)
- A kind of 1. false indigo method for preparing regenerated cellulose using salt-soda soil plantation, it is characterised in that the method includes with Lower step：(1) it pre-processes：False indigo is removed the peel, crush, be sieved, dry, is cooled down, obtains false indigo wood powder；(2) Acid treatment：False indigo wood powder in step (1) is taken, adds in the mixed liquor of organic solvent-organic acid-surfactant, Stirring, heating boiling, cooling, filtering after the filter residue of collection is rinsed repeatedly with organic solvent, then are rinsed with deionized water；(3) soda boiling is handled：It is rinsed by organic solvent into step (2), lye-organic is added in the filter residue that deionized water is rinsed The mixed liquor of solvent by being ultrasonically treated, heats boiling, adding bleaching agent after keeping the temperature a period of time is bleached, and obtains purple Fringe Chinese scholartree pulp；(4) prepared by spinning solution：False indigo in step (3) is taken to starch in vain, by impregnating, squeezing, crushing, experienced, yellow, dissolving, de- It steeps and spinning solution is obtained by filtration；(5) it post-processes：Spinning solution is obtained into false indigo regenerated fiber through coagulating bath spinning, traction molding, using refining, drying Element.
- 2. the method that a kind of false indigo using salt-soda soil plantation according to claim 1 prepares regenerated cellulose, special Sign is：Organic solvent is ethyl alcohol, n-butanol or different in the mixed liquor of organic solvent-organic acid-surfactant in step (2) Propyl alcohol；Organic acid is citric acid, tartaric acid or oxalic acid；Surfactant is neopelex or Tween-60.
- 3. the method that a kind of false indigo using salt-soda soil plantation according to claim 1 prepares regenerated cellulose, special Sign is：The mixed liquor of the organic solvent-organic acid-surfactant is ethyl alcohol/isopropanol-tartaric acid-Tween-60 Mixed liquor.
- 4. the method that a kind of false indigo using salt-soda soil plantation according to claim 3 prepares regenerated cellulose, special Sign is：The volumetric concentration of the ethyl alcohol is 65%-80%.
- 5. the method that a kind of false indigo using salt-soda soil plantation according to claim 1 prepares regenerated cellulose, special Sign is：The temperature of boiling is 120-180 DEG C in step (2), and the time of boiling is 1-3h.
- 6. the method that a kind of false indigo using salt-soda soil plantation according to claim 1 prepares regenerated cellulose, special Sign is：Temperature when step (3) is ultrasonically treated is 80-120 DEG C, time 1-4h, and the power of ultrasonic wave is 200-400w.
- 7. the method that a kind of false indigo using salt-soda soil plantation according to claim 1 prepares regenerated cellulose, special Sign is：The mixed liquor of lye-organic solvent in step (3) is 0.5-1mol sodium hydroxide solutions/potassium hydroxide solution-different The mixed liquor of propyl alcohol.
- 8. the method that a kind of false indigo using salt-soda soil plantation according to claim 1 prepares regenerated cellulose, special Sign is：Bleaching agent tetraacetyl ethylene diamine, sodium hypochlorite, sodium sulfite in step (3).
- 9. the method that a kind of false indigo using salt-soda soil plantation according to claim 1 prepares regenerated cellulose, special Sign is：Bleaching temperature is 60-100 DEG C in step (3), bleaching time 1-2h.
- 10. the method that a kind of false indigo using salt-soda soil plantation according to claim 1 prepares regenerated cellulose, special Sign is：The temperature of coagulating bath is 35-60 DEG C in step (5), and the composition of coagulating bath is sulfuric acid 80-120g/l, zinc sulfate 13- 18g/l and sodium sulphate 325-350g/l, drafting multiple 1.6-2.0.
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| CN201711455101.8A CN108166089B (en) | 2017-12-28 | 2017-12-28 | Method for preparing regenerated cellulose by utilizing amorpha fruticosa planted in saline-alkali soil |
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| CN102277760A (en) * | 2011-08-30 | 2011-12-14 | 内蒙古科技大学 | Pre-processing method in process of producing paper pulp |
| CN104233495A (en) * | 2014-10-15 | 2014-12-24 | 钱景 | Salix mongolica regenerated cellulose and preparation method thereof |
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2017
- 2017-12-28 CN CN201711455101.8A patent/CN108166089B/en active Active
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| US2781275A (en) * | 1951-05-12 | 1957-02-12 | American Enka Corp | Viscose solution and method of spinning |
| GB1434232A (en) * | 1972-07-05 | 1976-05-05 | Mo Och Domsjoe Ab | Method of producing cellulose pulp by means of oxygen gas delignification |
| CN1088273A (en) * | 1992-12-12 | 1994-06-22 | 宋述河 | The manufacture method of corn wrapper fibre |
| CN102277760A (en) * | 2011-08-30 | 2011-12-14 | 内蒙古科技大学 | Pre-processing method in process of producing paper pulp |
| CN104233495A (en) * | 2014-10-15 | 2014-12-24 | 钱景 | Salix mongolica regenerated cellulose and preparation method thereof |
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