CN104004206B - A kind of cellosolve and its preparation method and application - Google Patents
A kind of cellosolve and its preparation method and application Download PDFInfo
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- CN104004206B CN104004206B CN201410194483.3A CN201410194483A CN104004206B CN 104004206 B CN104004206 B CN 104004206B CN 201410194483 A CN201410194483 A CN 201410194483A CN 104004206 B CN104004206 B CN 104004206B
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Abstract
The present invention relates to a kind of cellosolve and its preparation method and application, this cellosolve is the mixing solutions of N-butyl-3-picoline alkoxide and cosolvent, in room temperature under 50 DEG C of temperature condition, Mierocrystalline cellulose is joined in cellosolve, stir and obtain the cellulose solution that mass percent concentration is 1 ~ 50%.Cellosolve stable performance of the present invention, non-corrosiveness, and can at room temperature dissolving cellulos, cellulose dissolution degree is high, without dissolving side reaction, the Mierocrystalline cellulose of solubilized high-polymerization degree, and solvent can be recycled non-pollutant discharge, easily realizes industrialization promotion.
Description
Technical field
The present invention relates to cellosolve technical field, be specifically related to a kind of cellosolve and its preparation method and application.
Background technology
Along with exhaustion and the environmental degradation of fossil energy, the renewable resources meeting Sustainable development requirement utilizes and causes people's extensive concern.Mierocrystalline cellulose be nature reserves the abundantest, can bio-regeneration, biodegradable natural macromolecular material, can extract from the raw material of rich cellulose and obtain, these raw materials comprise cotton, trees, farm crop and other plant and residual body etc. thereof.The extensive application of alternative petroleum-based chemical product in weaving, papermaking, medical and health, food and coatings industry after cellulose dissolution transforms." national energy science and technology " 12 " planning (2011-2015) " liquid fuel prepared by cellulose hydrolysis and comprehensive utilization demonstration project is place as the priority.China is populous, natural resources shortage, develops the biomass resource transformation technology based on Mierocrystalline cellulose, is of great significance national energy security tool.
Be desired product cellulose conversion, usually need Mierocrystalline cellulose to dissolve in advance.But in cellulosic molecule and intermolecular huge hydrogen bond network and higher degree of crystallinity thereof, hinder the dissolving of Mierocrystalline cellulose at water and most of solvent, this is the biggest obstacle of the further Application and Development of Mierocrystalline cellulose always.Up to now, the industrial solvent system for dissolving cellulos mainly contains viscose process (NaOH/CS
2system) and N-methylmorpholine-N-oxide compound (NMMO).Viscose process is the traditional technology of producing viscose yarn and glassine paper, still occupy an leading position at present, but the method is owing to using heavy metallic salt, CS in a large number
2cause environmental pollution Deng harmful chemical and damage HUMAN HEALTH.Although NMMO system can be produced like the same non-derivative fiber of natural silk, the problems such as it exists solvent instability, the by product that responds, dissolution conditions harshness, fibrillation.NaOH/ urea (thiocarbamide), LiOH/ urea (thiocarbamide) system also can as cellulosic solvents, but this kind of solvent system will be pre-chilled to-5 DEG C ~-12 DEG C ability dissolving cellulos, and alkaline NaOH and LiOH not only can cause cellulosic degraded but also have severe corrosive, needs to use corrosion resistant apparatus.Alkyl imidazole type ionic liquid is considered to a class environmental type cellosolve, but the viscosity of this kind solvent and cellulose solution thereof is excessive, and the power consumption of whipping device is excessive.In addition, this kind solvent very easily absorbs water, and after water suction, cellulose solution is that gel even lumps, and is difficult to carry out spinning processing.Other studied solvent system has lithium chloride N,N-dimethylacetamide (LiCl/DMA), the tetrabutyl three water fluorochemical/dimethyl sulfoxide (DMSO) (TBAF/DMSO), LiClO43H
2o, 1-butyl-3-methylimidazolium chloride/DMI ([C
4mim] Cl/DMI) system etc.Although these solvent systems respectively have advantage, also there is following shortcoming: the operational condition etc. that solvent is unstable, solvent temperature is high, viscosity is high or harsh.
Summary of the invention
The object of the invention is the deficiency for solving the problems of the technologies described above, a kind of cellosolve and its preparation method and application is provided, the stable performance of this solvent, non-corrosiveness, and can at room temperature dissolving cellulos, cellulose dissolution degree is high, without dissolving side reaction, the Mierocrystalline cellulose of solubilized high-polymerization degree, solvent can be recycled non-pollutant discharge, easily realizes industrialization promotion.
The present invention is the deficiency solved the problems of the technologies described above, the technical scheme adopted is: a kind of cellosolve, described cellosolve is the mixing solutions of N-butyl-3-picoline alkoxide and cosolvent, wherein, N-butyl-3-picoline alkoxide accounts for 20 ~ 80% of solvent gross weight, and cosolvent accounts for 20 ~ 80% of solvent gross weight.
Described cosolvent is N-Methylimidazole or METHYLPYRROLIDONE.
The preparation method of above-mentioned cellosolve: the N-butyl-3-picoline villaumite getting vacuum-drying adds in cosolvent, sodium ethylate or sodium methylate is added again after stirring, continue stirring 5 ~ 24h, then freezing 0.5 ~ 1h at-8 ~-10 DEG C of temperature is placed in, eventually pass vacuum filtration, obtain filtrate and be cellosolve.
The application of above-mentioned cellosolve in cellulose solution preparation: in room temperature under 50 DEG C of temperature condition, Mierocrystalline cellulose is joined in cellosolve, stir and obtain the cellulose solution that mass percent concentration is 1 ~ 50%.
Described Mierocrystalline cellulose is one or more in following substances: natural cotton, absorbent cotton, wood pulp cellulose, crop waste fibres, bacterial fibers and life waste paper.
Beneficial effect
(1), cellosolve preparation condition of the present invention is gentle, and solvent nature is stablized, and do not need special safety technique to invest, thus greatly can reduce the requirement to operating equipment, thus do not need high pressure resistant equipment, investment of production is few, and cost is low.
(2), cellosolve of the present invention all can prepare cellulose solution under room temperature (0 DEG C ~ 50 DEG C), do not need freezing or heating, thus without the need to heating installation or refrigerating apparatus, not only save energy, and decreases facility investment.
(3), at room temperature cellulose dissolution degree is high for cellosolve of the present invention, such as, when 25 DEG C, in 60%N-butyl-3-picoline methylate solvent, can prepare 50% cellulose solution.And, without dissolving side reaction during cellosolve dissolving cellulos of the present invention, the Mierocrystalline cellulose of the insoluble high-polymerization degree of solubilized (such as, the polymerization degree up to 5000 natural cotton).
(4), cellosolve stable performance of the present invention, non-corrosiveness, solvent is recyclable to be recycled, non-pollutant discharge, therefore without the need to using corrosion resistant apparatus, can economize in raw materials, cost of investment is low, practical, easily realize industrialization promotion.
Embodiment
A kind of cellosolve, described cellosolve is the mixing solutions of N-butyl-3-picoline alkoxide and cosolvent, and wherein, N-butyl-3-picoline alkoxide accounts for 20 ~ 80% of solvent gross weight, and cosolvent accounts for 20 ~ 80% of solvent gross weight.
The structural formula of described N-butyl-3-picoline alkoxide is as follows:
Described cosolvent is N-Methylimidazole or METHYLPYRROLIDONE.
The preparation method of above-mentioned cellosolve: N-butyl-3-picoline villaumite (75.7 ~ 18.9g) getting vacuum-drying adds in cosolvent (20.0 ~ 80.0g), sodium ethylate (75.7 ~ 7.0g) or sodium methylate (22.0 ~ 5.5g) is added again after stirring, continue stirring 5 ~ 24h, then freezing 0.5 ~ 1h at-8 ~-10 DEG C of temperature is placed in, eventually pass vacuum filtration, obtain filtrate and be cellosolve.
The application of above-mentioned cellosolve in cellulose solution preparation: in room temperature under 50 DEG C of temperature condition, Mierocrystalline cellulose is joined in cellosolve, stir and obtain the cellulose solution that mass percent concentration is 1 ~ 50%.
Described Mierocrystalline cellulose is one or more in following substances: natural cotton, absorbent cotton, wood pulp cellulose, crop waste fibres (comprising wheat stalk fiber, straw fibers, corn stalk fiber, producing fibre from cotton stalk, Pericarppium arachidis hypogaeae fiber etc.), bacterial fibers and life waste paper.
Below specific embodiments of the invention:
Embodiment 1
A kind of preparation method of cellosolve: the N-butyl methyl pyridine villaumite getting 50g vacuum-drying adds in the N-Methylimidazole (NMI) of 50g, 18.3g sodium ethylate is added again after stirring, continue to stir 12h, then freezing 1h under being placed in-10 DEG C of temperature, eventually pass vacuum filtration, obtain cellosolve.
Get 50g cellosolve and be placed in container, then add 30g Microcrystalline Cellulose, after stirring, obtain the cellulose solution of 37.5%.
Embodiment 2
A kind of preparation method of cellosolve: the N-butyl methyl pyridine villaumite getting 60g vacuum-drying adds in the METHYLPYRROLIDONE of 25g, 20g sodium methylate is added again after stirring, continue to stir 12h, then freezing 1h under being placed in-10 DEG C of temperature, eventually pass vacuum filtration, obtain cellosolve.
Get 10g cellosolve and be placed in container, then add 5g absorbent cotton, after stirring, obtain the cellulose solution of 41.5%.
Embodiment 3
A kind of preparation method of cellosolve: the N-butyl methyl pyridine villaumite getting 20g vacuum-drying adds in the METHYLPYRROLIDONE of 75g, 40g sodium ethylate is added again after stirring, continue to stir 12h, then freezing 1h under being placed in-10 DEG C of temperature, eventually pass vacuum filtration, obtain cellosolve.
Get 10g cellosolve and be placed in container, then add 5g Pericarppium arachidis hypogaeae fiber, after stirring, obtain the cellulose solution of 45.5%.
Claims (1)
1. the preparation method of a cellosolve, it is characterized in that: described cellosolve is the mixing solutions of N-butyl-3-picoline alkoxide and cosolvent, wherein, N-butyl-3-picoline alkoxide accounts for 20 ~ 80% of solvent gross weight, cosolvent accounts for 20 ~ 80% of solvent gross weight, cosolvent is N-Methylimidazole or METHYLPYRROLIDONE, N-butyl-3-picoline the villaumite getting vacuum-drying adds in cosolvent, sodium ethylate or sodium methylate is added again after stirring, continue stirring 5 ~ 24h, then freezing 0.5 ~ 1h at-8 ~-10 DEG C of temperature is placed in, eventually pass vacuum filtration, obtain filtrate and be cellosolve.
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| CN201410194483.3A CN104004206B (en) | 2014-05-09 | 2014-05-09 | A kind of cellosolve and its preparation method and application |
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| CN104004206B true CN104004206B (en) | 2016-04-20 |
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| CN104651542B (en) * | 2015-01-30 | 2019-01-18 | 华南理工大学 | A method of reduced sugar is prepared with the ionic liquid-catalyzed hydrolysis duckweed of heteropoly acid type |
| CN105061800B (en) * | 2015-08-28 | 2018-05-11 | 河南科技大学 | A kind of method that biogas gel is prepared using corncob cellulose as raw material |
| CN108559662B (en) * | 2017-12-27 | 2021-12-14 | 山东恒联新材料股份有限公司 | Cleaning agent for filter element of filter and use method thereof |
| CN111662642B (en) * | 2020-07-13 | 2021-07-23 | 万华化学集团电子材料有限公司 | Sapphire polishing composition and preparation method thereof |
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| CN101560258A (en) * | 2009-05-22 | 2009-10-21 | 河南师范大学 | Solvent of cellulose |
| GB2483427A (en) * | 2010-07-07 | 2012-03-14 | Innovia Films Ltd | Process for dissolving cellulose and casting films |
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