A kind of preparation method of lignin micro/nanosphere

A lignin and nanosphere technology, applied in nanotechnology and other directions, can solve the problems of complicated operation, difficult large-scale production, and high equipment requirements, and achieve the effects of cheap reagents, environmentally friendly process, and low risk.

Active Publication Date: 2020-12-29
SOUTH CHINA AGRI UNIV
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  • Application Information

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Problems solved by technology

However, the organic solvent used has certain toxicity, and at the same time, the dialysis takes a long time and the operation is complicated, which is not conducive to mass production
Chinese patent CN109012608A discloses a preparation method of lignin nano-microspheres. First, the lignin is hydrophobically modified by microwave acetylation, and then the acetylated lignin is dissolved in THF solvent. and ultrasonic-assisted method to prepare nano-microspheres with the advantages of uniform appearance, regular shape, good dispersion, single-hole distribution and high yield, but this method changes the chemical structure of lignin, and the whole process has certain limitations. toxic THF
Chinese patent CN108940218A uses imidazole ionic liquid as a solvent, and under the condition of microwave-assisted dissolution and stirring, phytic acid water is added to the ionic liquid-lignin solution to obtain lignin microspheres. The preparation of the ionic liquid used in this method is tedious and expensive. Difficult to mass produce
The preparation method of the lignin-based nano-microspheres is easy to operate, and effectively avoids the change of the chemical structure of the lignin and the use of toxic reagents, but in addition to the use of acid which requires high equipment, the prepared particles are irregular in shape and difficult to obtain. not really microspheres

Method used

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Experimental program
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Effect test

Embodiment 1

[0043] According to technical scheme A, a kind of preparation method of lignin microsphere with smooth surface comprises the following steps:

[0044] (1) Dissolve 1 g of organic solvent lignin in 400 mL of dichloromethane, then add 400 mL of water, and emulsify with a high-speed dispersing emulsifier at a speed of 10,000 r / min for 60 s to obtain a stable and uniform emulsion;

[0045] (2) The emulsion obtained in step (1) was stirred at a constant speed (200 rpm) for 3 h in an open environment at a temperature of 25°C until all the organic solvents evaporated to obtain a lignin microsphere-water mixture;

[0046] (3) Take out the mixed liquid obtained in step (2) and put it into a centrifuge, adjust the rotating speed to 8000 r / min, centrifuge for 10 min, repeat the centrifugation twice, remove the centrifuged liquid and then repeat the centrifugation at a centrifugal speed of 2000 r / min, wash After the lignin ball is colorless to the centrifugal liquid, take the solid in the...

Embodiment 2

[0049] According to technical scheme A, a kind of preparation method of lignin nanosphere with smooth surface comprises the following steps:

[0050] (1) Dissolve 1 g of organic solvent lignin in 400 mL of ethyl acetate, then add 400 mL of aqueous solution containing polyvinyl alcohol (0.2% by mass fraction), and use a high-speed dispersing emulsifier at a speed of 10,000 r / min Emulsify for 30 s to obtain a stable and uniform emulsion;

[0051] (2) The emulsion obtained in step (1) was stirred at a constant speed (500 rpm) for 3 h in an open environment at a temperature of 25°C until all organic solvents were evaporated to obtain a lignin nanosphere-water mixture;

[0052] (3) Take out the mixed liquid obtained in step (2) and put it into a centrifuge, adjust the rotation speed to 10000 r / min, centrifuge for 15 min, repeat the centrifugation twice, remove the centrifugate and then repeat the centrifugation at a centrifugal speed of 2000 r / min, wash After the lignin ball is co...

Embodiment 3

[0055] According to technical scheme A, a kind of preparation method of lignin nanosphere with smooth surface comprises the following steps:

[0056] (1) Dissolve 1 g of organic solvent lignin in 400 mL of dichloromethane, then add 400 mL of an aqueous solution containing sodium dodecylbenzenesulfonate (1% mass fraction), and use a high-speed dispersing and emulsifying machine at 10,000 Emulsify at a speed of r / min for 30 s to obtain a stable and uniform emulsion;

[0057] (2) The emulsion obtained in step (1) was stirred at a constant speed (500 rpm) for 3 h in an open environment at a temperature of 25°C until all organic solvents were evaporated to obtain a lignin nanosphere-water mixture;

[0058] (3) Take out the mixed liquid obtained in step (2) and put it into a centrifuge, adjust the rotation speed to 10000 r / min, centrifuge for 15 min, repeat the centrifugation twice, remove the centrifugate and then repeat the centrifugation at a centrifugal speed of 2000 r / min, wash...

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Abstract

The invention provides a preparation method of lignin micro / nano spheres, which mainly relates to preparation of lignin spherical micro / nanoparticles in an organic solvent-water system and can fulfillshape and size controllable aim by controlling preparation conditions such as organic solvent type, temperature, surfactant, stirring speed and solvent dropping speed. The preparation method of the lignin micro / nano spheres comprises the following steps: dissolving a proper amount of lignin into the organic solvent and adding water to obtain uniform mixed liquid; and evaporating the organic solvent to obtain the lignin micro / nano spheres with uniform size and regular shape. The preparation method of the lignin micro / nano spheres is simple and convenient in operation, low in equipment requirement and short in production period, chemical modification of the lignin and use of chemical agents with high toxicity are avoided, cost is saved and environmental pollution is reduced; furthermore, raw materials are low in price and wide in source, and high-value utilization of lignin resources can be realized.

Description

technical field [0001] The invention belongs to the technical field of lignin preparation, and in particular relates to a simple, green, economical method for preparing lignin micro / nano balls with controllable appearance and particle size. Background technique [0002] Lignin accounts for 25% in woody plants and is the second most abundant natural organic matter in the world. It has excellent biocompatibility and excellent antibacterial effect. Its unique chemical structure and high reactivity enable lignin to Widely used in the field of production and life. Lignin is a biopolymer with a three-dimensional network structure formed by connecting three phenylpropane units through ether bonds and carbon-carbon bonds. There are aromatic groups, phenolic hydroxyl groups, alcoholic hydroxyl groups, and carbon-based conjugated double bonds in the molecular structure. Reactive groups, so can carry out a variety of chemical reactions. Despite its promising chemical structure potent...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J3/12C08J3/07C08L97/00B82Y40/00
CPCB82Y40/00C08J3/07C08J3/12C08J2397/00
Inventor 董先明龙海波虎良可蔡奇龙周武艺罗颖
Owner SOUTH CHINA AGRI UNIV
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