CN105153720A - Lignin reverse phase nanometer colloid sphere as well as preparation method and application thereof - Google Patents
Lignin reverse phase nanometer colloid sphere as well as preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a preparation method and application of a lignin reverse phase nanometer colloid sphere. The preparation method comprises the following steps: dissolving 1-30 parts by weight of alkaline lignin into 150-1000 parts by weight of an organic solvent, and adding 7-500 parts by weight of a precipitating agent to change a microphase environment, so as to obtain the lignin reverse phase nanometer colloid sphere. According to the invention, the method is simple, the raw materials are rich in sources and low in price, the organic solvent used in production can be recycled, and the production cost is low; compared with a hydrophilic lignin nanometer microsphere, the prepared lignin reverse phase nanometer colloid sphere adopts a hydrophobic surface, has good compatibility with polymer materials like polyethylene, and can be used as organic nanometer filler to effectively improve the breakage tensile strain of polyethylene plastic, thereby being an environment-friendly regenerative nanometer material.
Description
Technical field
The present invention relates to reversed phase micelle, be specifically related to anti-phase nanometer colloid ball of a kind of xylogen and preparation method thereof application, belong to technical field of fine.
Technical background
Xylogen is extensively present in plant, and according to estimation, the whole world approximately can produce 6 × 10 every year
14t xylogen, the energy of biologically produce 40% is all stored in xylogen, therefore xylogen be described as 21 century can by one of the abundantest green resource of human use.Industrial lignin is mainly from pulping and paper-making waste liquid, and bio-ethanol by product, and its abundance is cheap.The whole world is about 4 × 10 from the industrial lignin output generated as by product in papermaking wastewater every year
7?5 × 10
7t (not comprising the East European countries), but the xylogen of about 90% can be burnt.According to the difference of pulping process, industrial lignin is generally divided into sulfonated lignin and alkali lignin two class.Sulfonated lignin are by products of acid polishing, have good solubility and reactive behavior, widespread use in multiple industries such as cement water reducing agent, pesticide dispersing agent, fuel dispersants.Alkali lignin is as the by product of soda pulp, water-soluble poor with reactive behavior, need carry out modification ability high-value-use, developing new application.Modern paper is based on alkaline process, industrial lignin is based on alkali lignin, the new application of exploitation alkali lignin, not only be conducive to promoting pulping and paper-making industry health, environmental protection development, be more conducive to solving the predicament that current alkali lignin output is too high, cause a large amount of environmental pollution and the wasting of resources.
Alkali lignin is dissolved in organic solvent to add precipitation agent to prepare xylogen reversed phase micelle be an original job.At present, the research preparing reversed phase micelle as cetyl trimethylammonium bromide (CTAB) for raw material with Small molecular surfactant has been reported.CTAB-n-hexyl alcohol-normal heptane-water quaternary reverse micelle system can synthesize cadmium sulfide nanoparticles (Science Bulletin, 2001,17:1423-1427) as " microreactor "; In CTAB reverse micelle, chloroperoxidase catalyzed oxidation indoles can show " superactivity " (Shaanxi Normal University's journal (natural science edition), 2009,37:56-59).Report is had no with the research that the natural polymers such as xylogen prepare reversed phase micelle for raw material.
Polyethylene is with the polymkeric substance of vinyl monomer addition polymerization, is a kind of thermoplastic resin material, and global polyethylene production occupies first of five large general resins.Different according to preparation technology, be divided into Low Density Polyethylene and high density polyethylene(HDPE).Low Density Polyethylene is high-pressure polyethylene again, and because density is low, quality is soft, mainly for the preparation of polythene bag and agricultural mulching; High density polyethylene(HDPE) is low pressure polyethylene again, compared with Low Density Polyethylene, there is good heatproof, oil resistant, resistance to water vapour penetration and environmental stress crack resistance, in addition electrical insulating property and shock resistance fine, main in blowing, injection moulding, the product of preparation comprises various net, band, container, cable coating, tubing, wire rod etc.Polyethylene is cheap, extensively should in industry, agricultural, medicine and multiple field such as daily living article.Meanwhile, in order to improve poly over-all properties and cost-saving, in polyethylene refining process, various filler and antiaging agent and tinting material etc. is usually added, to widen its range of application.The filler that current polyethylene is conventional has calcium carbonate, potter's clay, talcum powder, wood powder and Mierocrystalline cellulose etc.These materials can improve poly intensity to a certain extent, reduce costs simultaneously, but also there is certain defect, and such as calcium carbonate is easily reunited, thus forms stress point in polyethylene, reduce other mechanical property of matrix material on the contrary.
Xylogen degradable, toxicological harmless, and because have the feature structure such as phenyl ring, phenolic hydroxyl group, there is good anti-ultraviolet radiation and ageing resistance, therefore xylogen can be added in polyethylene (as high density polyethylene(HDPE)) as filler and prepare matrix material.But due to xylogen and poly interface compatibility poor, therefore must carry out surface modification to xylogen or polyethylene, add solubilizing agent, softening agent to be to increase both interface compatibilities.Add in polyethylene and polypropylene binary mixture blended with epoxychloropropane modified sulfonated lignin and 5% solubilizing agent, when the addition of xylogen is 5%, the tensile strength of matrix material and break-draw rate improve 20% and 25% (IndustrialCropsandProducts, 2004,20:261 ?273).The methylate xylogen of modification and high density polyethylene(HDPE) prepares matrix material, and when add-on is 2.5%, break-draw rate improves 24% in (synthetic resins and plastics, 2006,23:39 ?42).
Carry out surface modification to xylogen or add solubilizing agent, softening agent all making the preparation process of matrix material become complicated, though xylogen and high density polyethylene(HDPE) interface compatibility can be increased, but it is not remarkable to the raising of composite property, and cause cost to increase, be difficult to industrially apply.On the other hand, the modified-reaction for xylogen occurs in the phenolic hydroxyl group position of xylogen substantially, sacrifices the anti-aging of xylogen and part uvioresistant performance, does not also utilize the open air use of xylogen/composite polyethylene material.
Summary of the invention
The object of the invention is to for current only lignin-base colloidal spheres is hydrophilic hollow micella, anti-phase nanometer colloid ball of a kind of xylogen and preparation method thereof is provided, this xylogen reversed phase micelle is surface hydrophobicity, the nano-level sphere micella of inner hydrophilic, has good consistency with the hydrophobic material such as plastics, rubber.
The present invention also has an object, is to provide the anti-phase nanometer colloid ball of described xylogen as the application of plastics or loading material of rubber, significantly improves the mechanical property of plastics or rubber.
There is in view of alkali lignin the hydrophobic frameworks such as a large amount of phenyl ring, only have a small amount of hydroxyl, carboxyl, after the present invention is dissolved in organic solvent, add another precipitation agent that can dissolve each other with polar organic solvent again and change microfacies environment, alkali lignin self-assembly under the driving of precipitation agent forms nano level xylogen spherical reverse micelles.This xylogen reversed phase micelle be hydrophilic radical interior, hydrophobic grouping solid spherical micelle outside, formed surface hydrophobicity, the nano-level sphere micella of inner hydrophilic, nanometer colloid ball is that hydrodynamic radius is at 50 ~ 250nm.Contriver finds, the anti-phase nanometer colloid ball of this xylogen and high density polyethylene(HDPE) compound, the break-draw strain of matrix material increases substantially, reach 897.04%, also 52.63% is exceeded than pure high density polyethylene(HDPE), exceed 188.55% than alkali lignin/high-density polyethylene composite material, composite property obtains beyond thought improvement.Therefore, in field of polymer technology, xylogen reversed phase micelle has expanded the category of lignin-base nano material further, widen a large amount of, the high-valued Application Areas of xylogen, particularly have huge application prospect as hydrophobicity, degradable, uvioresistant, anti-aging filler in the field such as plastics, rubber.
Object of the present invention is achieved through the following technical solutions:
A preparation method for the anti-phase nanometer colloid ball of xylogen, comprises the following steps:
(1) 1 ~ 30 weight part alkali lignin is dissolved in 150 ~ 1000 weight parts organic solvent, forms the organic solution of alkali lignin; Described organic solvent is the one in tetrahydrofuran (THF), dioxane and dimethyl sulfoxide (DMSO);
(2) by the precipitant mix of the alkali lignin organic solution in step (1) and 7 ~ 500 weight parts, stir under normal temperature and pressure, form the anti-phase nanometer colloid ball of xylogen; Described precipitation agent is hexanaphthene, sherwood oil or Skellysolve A.
For realizing the object of the invention further, preferably, in step (1), alkali lignin concentration is in organic solvent 1 ~ 10g/L.
Preferably, in step (2), the add-on of precipitation agent is 10 ~ 150 weight parts.
Preferably, described alkali lignin is one or more the mixture in Wheat Straw Lignin from Alkali Pulping, bamboo pulp alkali lignin and wood pulp alkali xylogen.
The anti-phase nanometer colloid ball of a kind of xylogen, it is obtained by above-mentioned preparation method; Described nanometer colloid ball be hydrodynamic radius at 50 ~ 250nm, hydrophilic radical interior, hydrophobic grouping solid spherical micelle outside.
The anti-phase nanometer colloid ball of described xylogen is as the application of plastics or loading material of rubber.
The present invention compared with the prior art, has the following advantages and beneficial effect:
1, the present invention using abundance, cheap alkali lignin directly as raw material, only need by changing solvent, without the need to carrying out chemical modification, just the solution containing xylogen reversed phase micelle can be prepared, only need can obtain xylogen reversed phase micelle solid by the simple step such as sedimentation, drying, solvent can recycle simultaneously.Preparation process of the present invention is simple, and separating step is simple and easy, with low cost, can expand the high value added utilization of pulping and paper-making byproduct xylogen, promotes the enthusiasm that factory reclaims it to have economy and environmental protection double effect.
2, the xylogen reversed phase micelle that the present invention prepares is the spherical micelle of a kind of inner hydrophilic, outer hydrophobic, the consistency of itself and the hydrophobic material such as plastics, rubber is significantly better than not having treated alkali lignin, only need blended prepare plastics time add a small amount of reversed phase micelle, effectively can improve break-draw strain and the tensile strength of plastics, can be used as the degradable nano filler of plastics, rubber, have broad application prospects and market potential.In addition, alkali lignin derives from natural phant, itself has certain ultraviolet absorption ability, possesses certain anti-aging function simultaneously, add that anti-phase xylogen nanometer colloid ball can make plastics, the problem of aging of rubber is well solved, and has good application prospect and market potential.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope picture of the anti-phase nanometer colloid ball of embodiment 1 xylogen.
Fig. 2 is the grain size distribution of the anti-phase nanometer colloid ball of embodiment 1 xylogen.
Fig. 3 be in embodiment 1 water droplet at alkali lignin and xylogen anti-phase nanometer colloid ball surface static contact angle schematic diagram.
Embodiment
For understanding the present invention better, be described in detail of the present invention below in conjunction with drawings and Examples, but embodiments of the present invention are not limited thereto.
Embodiment 1
(1) 0.1g alkaline process straw pulp black liquor acid out alkali lignin (weight-average molecular weight 4200g/mol) is placed in the beaker of 1000ml, adds 100ml dioxane, stirred at ambient temperature dissolves, and obtains 1g/L alkali lignin dioxane solution.
(2) in step (1) gained alkali lignin dioxane solution, slowly add 50ml hexanaphthene, stir under normal temperature and pressure and form spherical micelle, obtain the suspension liquid containing the anti-phase nanometer colloid ball of xylogen.This suspension liquid is placed half an hour, after xylogen anti-phase nanometer colloid ball flocculating settling, removes supernatant liquor and vacuum-drying is carried out to beaker bottom throw out, obtaining the anti-phase nanometer colloid ball of xylogen.
Fig. 1 is the transmission electron microscope picture of the present embodiment 1 product xylogen reversed phase micelle by the shooting of Japanese HITACHIH-7650 transmission electron microscope, shows that this reversed phase micelle is the spherical micelle that the diameter with solid construction is less than 200nm.Fig. 2 is the grain size distribution of the anti-phase colloidal spheres of the present embodiment product xylogen recorded by German ALV-7004 sound state laser light scattering instrument, shows that the nanometer colloid ball formed is the homogeneous nano particle of hydrodynamic radius at 90 ~ 170nm.
Table 1 is by water droplet in alkali lignin coating, and the static contact angle in embodiment 1 in xylogen anti-phase nanometer colloid ball coating.When alkali lignin is dissolved in dioxane, a part of hydrophilic radical is distributed in molecular surface, and its static contact angle is 57.22 °; When hexanaphthene joins the dioxane solution of alkali lignin, the reversing of solution microfacies, become more hydrophobic, alkali lignin forms hydrophobic segment outside by molecular self-assembling, hydrophilic radical, in interior spherical reversed phase micelle structure, is coated on slide and is formed coating, due to hydrophobic segment outside, the static contact angle of water droplet in xylogen reversed phase micelle coating is comparatively large, is 80.52 °.Above data show that the anti-phase colloidal spheres of xylogen of the present invention is inner hydrophobic, the nanometer colloid ball of external hydrophilic.
Table 1 water droplet is at the static contact angle on alkali lignin and xylogen reversed phase micelle surface
| Top coat | Alkali lignin a | Xylogen reversed phase micelle b |
| Water droplet dwell angle | 57.22° | 80.52° |
In table 1, a: the dioxane solution of alkali lignin is uniformly coated on quartz slide, air-dry under 25 DEG C of conditions.B: the dioxane/hexanaphthene suspension liquid uniform settling of xylogen reversed phase micelle is on quartz slide, air-dry under 25 DEG C of conditions.
Alkali lignin derives from timber and other plant, and degradability is strong, and has certain uv-absorbing and resistance of aging, can be used as the filler of the material such as plastics, rubber.But because alkali lignin contains more hydrophilic radical, the interface compatibility of itself and plastics, rubber is bad, because which limit the application of alkali lignin in plastics, loading material of rubber.The alkali lignin of identical amount and the anti-phase nanometer colloid ball of xylogen of the present invention are added in high density polyethylene(HDPE) as organic particulate filler and carries out break-draw strain and tensile strength is tested, concrete outcome is as shown in table 2, the break-draw strain of alkali lignin/high-density polyethylene composite material is only 310.88%, have dropped 47.10% compared with pure high density polyethylene(HDPE), the break-draw strain of the xylogen reversed phase micelle/high-density polyethylene composite material adopting the present invention to prepare increases substantially, reach 897.04%, also 52.63% is exceeded than pure high density polyethylene(HDPE), 188.55% is exceeded than alkali lignin/high-density polyethylene composite material, along with the consumption of xylogen reversed phase micelle increases, the mechanical properties such as the break-draw strain of matrix material improve further, illustrate that the anti-phase colloidal spheres of xylogen and high density polyethylene(HDPE) have good consistency, xylogen reversed phase micelle/the high-density polyethylene composite material prepared has very high break-draw strain.In addition, xylogen reversed phase micelle of the present invention also to improve effect to the tensile strength of high density polyethylene(HDPE).Therefore xylogen of the present invention anti-phase nanometer colloid ball has good application prospect and market potential in the Performance Strength improving high density polyethylene(HDPE).
The performance of table 2 high density polyethylene(HDPE), alkali lignin/high density polyethylene(HDPE) and xylogen reversed phase micelle/high-density polyethylene composite material
| Material | Break-draw strain (%) | Tensile strength (MPa) |
| Alkali lignin/high density polyethylene(HDPE) | 310.88 | 22.08 |
| Xylogen reversed phase micelle/high density polyethylene(HDPE) | 897.04 | 22.35 |
| High density polyethylene(HDPE) | 587.72 | 21.85 |
Embodiment 2
(1) 3g alkaline process bamboo pulp black liquor acid out alkali lignin (weight-average molecular weight 3400g/mol) is placed in the beaker of 1000ml, add in 100ml dimethyl sulfoxide (DMSO), stirred at ambient temperature dissolves, and obtains 20g/L alkali lignin dimethyl sulphoxide solution.
(2) slowly add 0.7ml sherwood oil in step (1) gained containing in alkali lignin dimethyl sulphoxide solution, stir under normal temperature and pressure, obtain the suspension liquid containing xylogen reversed phase micelle.This suspension liquid is placed half an hour, after xylogen anti-phase nanometer colloid ball flocculating settling, removes supernatant liquor and vacuum-drying is carried out to beaker bottom throw out, obtaining the anti-phase nanometer colloid ball of xylogen.The scattering of light identical with embodiment 1 and static contact angle testing method is adopted to test size distribution and the hydrophilic and hydrophobic of the anti-phase colloidal spheres of xylogen, show that the hydrodynamic radius of the anti-phase colloidal spheres of gained is 50 ~ 250nm, static contact angle is 78.88 °, substantially identical with Fig. 2,3 respectively.
Embodiment 3
(1) 3g alkaline process pulp black liquor acid out alkali lignin (weight-average molecular weight 3500g/mol) is placed in the beaker of 1000ml, adds in 100ml tetrahydrofuran (THF), stirred at ambient temperature dissolves, and obtains 3g/L alkali lignin tetrahydrofuran solution.
(2) slowly add 20ml hexanaphthene in step (1) gained containing in alkali lignin tetrahydrofuran solution, stir under normal temperature and pressure, obtain the suspension liquid containing xylogen reversed phase micelle.This suspension liquid is placed half an hour, after xylogen anti-phase nanometer colloid ball flocculating settling, removes supernatant liquor and vacuum-drying is carried out to beaker bottom throw out, obtaining the anti-phase nanometer colloid ball of xylogen.Adopt the scattering of light identical with embodiment 1 and static contact angle testing method to test size distribution and the hydrophilic and hydrophobic of the anti-phase colloidal spheres of xylogen, show that the hydrodynamic radius of the anti-phase colloidal spheres of gained is 40 ~ 200nm, static contact angle is 79.56 °.Substantially identical with Fig. 2,3 respectively.
Embodiment 4
(1) 1.5g alkaline process straw pulp black liquor acid out alkali lignin (weight-average molecular weight 3500g/mol) is placed in the beaker of 1000ml, adds in 15ml dimethyl sulfoxide (DMSO), stirred at ambient temperature dissolves, and obtains 10g/L alkali lignin tetrahydrofuran solution.
(2) slowly add 1ml Skellysolve A in step (1) gained containing in alkali lignin tetrahydrofuran solution, stir under normal temperature and pressure, obtain the suspension liquid containing xylogen reversed phase micelle.This suspension liquid is placed half an hour, after xylogen anti-phase nanometer colloid ball flocculating settling, removes supernatant liquor and vacuum-drying is carried out to beaker bottom throw out, obtaining the anti-phase nanometer colloid ball of xylogen.Adopt the scattering of light identical with embodiment 1 and static contact angle testing method to test size distribution and the hydrophilic and hydrophobic of the anti-phase colloidal spheres of xylogen, show that the hydrodynamic radius of the anti-phase colloidal spheres of gained is 30 ~ 190nm, static contact angle is 81.06 °.Substantially identical with Fig. 2,3 respectively.
Embodiment 5
(1) 1g alkaline process pulp black liquor acid out alkali lignin (weight-average molecular weight 4200g/mol) is placed in the beaker of 1000ml, adds in 50ml dioxane, stirred at ambient temperature dissolves, and obtains 2g/L alkali lignin dioxane solution.
(2) slowly add 5ml Skellysolve A in step (1) gained containing in alkali lignin dioxane solution, stir under normal temperature and pressure, obtain the suspension liquid containing xylogen reversed phase micelle.This suspension liquid is placed half an hour, after xylogen anti-phase nanometer colloid ball flocculating settling, removes supernatant liquor and vacuum-drying is carried out to beaker bottom throw out, obtaining the anti-phase nanometer colloid ball of xylogen.The scattering of light identical with embodiment 1 and static contact angle testing method is adopted to test size distribution and the hydrophilic and hydrophobic of the anti-phase colloidal spheres of xylogen, show that the hydrodynamic radius of the anti-phase colloidal spheres of gained is 30 ~ 230nm, static contact angle is 80.06 °, substantially identical with Fig. 2,3 respectively.
Claims (6)
1. a preparation method for the anti-phase nanometer colloid ball of xylogen, is characterized in that comprising the following steps:
(1) 1 ~ 30 weight part alkali lignin is dissolved in 150 ~ 1000 weight parts organic solvent, forms the organic solution of alkali lignin; Described organic solvent is the one in tetrahydrofuran (THF), dioxane and dimethyl sulfoxide (DMSO);
(2) by the precipitant mix of the alkali lignin organic solution in step (1) and 7 ~ 500 weight parts, stir under normal temperature and pressure, form the anti-phase nanometer colloid ball of xylogen; Described precipitation agent is hexanaphthene, sherwood oil or Skellysolve A.
2. preparation method according to claim 1, is characterized in that: in step (1), alkali lignin concentration is in organic solvent 1 ~ 10g/L.
3. preparation method according to claim 1, is characterized in that: in step (2), the add-on of precipitation agent is 10 ~ 150 weight parts.
4. preparation method according to claim 1, is characterized in that: described alkali lignin is one or more the mixture in Wheat Straw Lignin from Alkali Pulping, bamboo pulp alkali lignin and wood pulp alkali xylogen.
5. the anti-phase nanometer colloid ball of xylogen, is characterized in that it is obtained by the preparation method described in any one of claim 1 ?4; Described nanometer colloid ball be hydrodynamic radius at 50 ~ 250nm, hydrophilic radical interior, hydrophobic grouping solid spherical micelle outside.
6. the anti-phase nanometer colloid ball of xylogen according to claim 5 is as the application of plastics or loading material of rubber.
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Cited By (6)
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| CN105968852A (en) * | 2016-05-25 | 2016-09-28 | 华南理工大学 | Anti-ultraviolet radiation lignin-based zinc oxide composite particles and preparation method and application thereof |
| CN106361591A (en) * | 2016-08-31 | 2017-02-01 | 华南理工大学 | Lignin nano-particles with high ultraviolet protection performance and preparation method of lignin nano-particle |
| CN107043462A (en) * | 2017-05-25 | 2017-08-15 | 湖南师范大学 | A kind of method that utilization reversed-phase emulsion prepares nano lignin |
| CN109972395A (en) * | 2019-04-09 | 2019-07-05 | 上海喜眠服饰有限公司 | Naked sense sweat absorption fabric, preparation method and naked sense nightwear |
| CN110684207A (en) * | 2019-11-18 | 2020-01-14 | 黄山学院 | Nano micelle prepared by using lignosulfonate and preparation method thereof |
| WO2020109671A1 (en) | 2018-11-29 | 2020-06-04 | Aalto University Foundation Sr | Lignin particle based hydrogel and the method for preparation of lignin colloidal particles by solvent evaporation process |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105968852A (en) * | 2016-05-25 | 2016-09-28 | 华南理工大学 | Anti-ultraviolet radiation lignin-based zinc oxide composite particles and preparation method and application thereof |
| CN106361591A (en) * | 2016-08-31 | 2017-02-01 | 华南理工大学 | Lignin nano-particles with high ultraviolet protection performance and preparation method of lignin nano-particle |
| CN107043462A (en) * | 2017-05-25 | 2017-08-15 | 湖南师范大学 | A kind of method that utilization reversed-phase emulsion prepares nano lignin |
| WO2020109671A1 (en) | 2018-11-29 | 2020-06-04 | Aalto University Foundation Sr | Lignin particle based hydrogel and the method for preparation of lignin colloidal particles by solvent evaporation process |
| CN109972395A (en) * | 2019-04-09 | 2019-07-05 | 上海喜眠服饰有限公司 | Naked sense sweat absorption fabric, preparation method and naked sense nightwear |
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| CN110684207B (en) * | 2019-11-18 | 2022-02-11 | 黄山学院 | Nano micelle prepared by using lignosulfonate and preparation method thereof |
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