CN102002165A - Method for preparing nano lignin by using supercritical anti-solvent technology - Google Patents
Method for preparing nano lignin by using supercritical anti-solvent technology Download PDFInfo
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- CN102002165A CN102002165A CN2010102818685A CN201010281868A CN102002165A CN 102002165 A CN102002165 A CN 102002165A CN 2010102818685 A CN2010102818685 A CN 2010102818685A CN 201010281868 A CN201010281868 A CN 201010281868A CN 102002165 A CN102002165 A CN 102002165A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/582—Recycling of unreacted starting or intermediate materials
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Abstract
The invention discloses a method for preparing nano lignin by using supercritical anti-solvent technology. The method is characterized in that: the lignin is selected from papermaking black liquor. The method comprises the following steps of: performing acidulation precipitation on the papermaking black liquor to obtain crude industrial papermaking lignin; performing two times of acid dissolution and acid precipitation on the crude industrial papermaking lignin to obtain refined industrial lignin, wherein the alkali liquor and the acid liquor are sodium hydroxide solution and hydrochloric acid solution respectively; and drying the refined industrial lignin at a low temperature, then dissolving the dried refined industrial lignin by using dioxane, performing centrifugal separation of the solution to obtain insoluble lignin, reclaiming the insoluble lignin for reuse, and preparing the nano lignin from the obtained lignin-dioxane solution by using a carbon dioxide supercritical device and adopting a supercritical anti-solvent method. The operation process has the main characteristics that: the raw material is papermaking industrial waste pollutant, so the pollution problem of the papermaking industry is solved, and the high-performance nano lignin is obtained; because the supercritical anti-solvent technology is adopted and the solvent can be recycled, the method has no pollution; and the product has no solvent residue, so the method opens a broad prospect for wider application of the lignin.
Description
Affiliated technical field:
The present invention relates to the natural product chemistry field, particularly relate to a kind of method of utilizing the super-critical anti-solvent technology to prepare the nanometer xylogen.
Background technology:
Xylogen is that a kind of content is only second to cellulosic natural reproducible resource, and the same extensive being present in the higher plant somatocyte with Mierocrystalline cellulose is one of basic chemical constitution of coniferals, deciduous tree class and straw or like vegetable.According to estimates, the whole world can produce about 6 * 10 every year
14The ton xylogen.Wherein industrial lignin is the principal pollutant in the pulping waste liquor, is the principal element that causes river pollution.At present the paper industry xylogen of China is produced 4,500,000 tons every year approximately, along with the development of paper industry also can further increase.Therefore, the development and use xylogen is turned waste into wealth, and has not only alleviated the pressure that shortage of resources causes Economic development but also has alleviated the pollution of paper industry to environment, has huge economic and social benefit.
For these reasons, rationally utilize natural reproducible resource---xylogen, can improve the industrial lignin physicochemical property, obtain the nano level xylogen by this invention, widen its Application Areas, make it become a kind of widely used, pollution-free, non-harmful nano level raw material.
Summary of the invention:
A kind of method of utilizing the super-critical anti-solvent technology to prepare the nanometer xylogen, it is characterized in that: the xylogen that uses comes from black liquid, black liquid obtains paper industry rugose wood element through persalt acid out precipitation, paper industry rugose wood element is again through twice alkali dissolution Acid precipitation, employed alkali lye and acid solution are respectively sodium hydroxide solution and hydrochloric acid soln, obtain the highly industry xylogen, refining paper industry xylogen is through after the cryodrying, dissolve with dioxane, the insoluble lignin recovery of centrifugation is reused, obtain xylogen dioxane solution CO 2 supercritical equipment, adopt the super-critical anti-solvent legal system to be equipped with the nanometer xylogen.
The object of the present invention is to provide a kind of method of utilizing the super-critical anti-solvent technology to prepare the nanometer xylogen.
In order to achieve the above object, the technical solution used in the present invention comprises: black liquid obtains paper industry rugose wood element through persalt acid out precipitation, paper industry rugose wood element is again through twice alkali dissolution Acid precipitation, obtain the highly industry xylogen, through after the cryodrying, with the dioxane dissolving, the insoluble lignin recovery of centrifugation is reused, obtain xylogen dioxane solution CO 2 supercritical equipment, adopt the super-critical anti-solvent legal system to be equipped with the nanometer xylogen.
Advantage of the present invention is:
1. the present invention adopts the super-critical anti-solvent legal system to be equipped with the nanometer xylogen first, because what use is that supercritical co is as anti-solvent, so recycle of reagent is pollution-free, the product no solvent residue is for xylogen is used and bright prospects have been opened in exploitation widely.
2, be the nano level xylogen owing to obtaining, what its every performance obtained increases substantially, and as solubility property, antioxidant property, dispersing property etc., the application prospect of xylogen has also been widened in the raising of these performances.
Embodiment:
Below the invention process is described in further detail:
Black liquid obtains paper industry rugose wood element through persalt acid out precipitation, paper industry rugose wood element is again through twice alkali dissolution Acid precipitation, obtain the highly industry xylogen, through after the cryodrying, dissolve with dioxane, the insoluble lignin recovery of centrifugation is reused, and obtains xylogen dioxane solution CO 2 supercritical equipment, adopts the super-critical anti-solvent legal system to be equipped with the nanometer xylogen.
Below, the present invention will be further detailed with embodiment, but it is not limited to any or the similar example of these embodiment.
Embodiment 1:
The 2000mL black liquid, under 60 ℃ of water bath condition, add salt acid for adjusting pH value to 3, obtain the plain throw out of rugose wood, regulate pH value to 12 with sodium hydroxide solution again, obtain lignin liquor, filter to remove insolubles, add salt acid for adjusting pH value xylogen in 3 precipitation solutions, through obtaining refining xylogen twice alkali dissolution Acid precipitation process, 45 ℃ of refining xylogen of oven dry, get the refining xylogen 3g in dry back, add the 1000mL dioxane, obtaining strength of solution is 3mg/mL.Be used for the super-critical anti-solvent technology and prepare the nanometer xylogen, with carbonic acid gas as anti-solvent, temperature of reaction kettle is 35 ℃, reactor pressure is 30MPa, carbon dioxide flow is 20mL/min, xylogen dioxane solution flow velocity is 6mL/min, and nozzle bore is 150nm, and obtaining median size is 144 ± 30nm (see figure 1) nanometer xylogen.
Claims (4)
1. method of utilizing the super-critical anti-solvent technology to prepare the nanometer xylogen, it is characterized in that: the xylogen that uses comes from black liquid, black liquid obtains paper industry rugose wood element through persalt acid out precipitation, paper industry rugose wood element is again through twice alkali dissolution Acid precipitation, employed alkali lye and acid solution are respectively sodium hydroxide solution and hydrochloric acid soln, obtain the highly industry xylogen, refining paper industry xylogen is through after the cryodrying, dissolve with dioxane, the insoluble lignin recovery of centrifugation is reused, obtain xylogen dioxane solution CO 2 supercritical equipment, adopt the super-critical anti-solvent legal system to be equipped with the nanometer xylogen.
2. according to the described a kind of method of utilizing the super-critical anti-solvent technology to prepare the nanometer xylogen of claim 1, it is characterized in that: the plain and plain alkali extraction and acid precipitation treating process of rugose wood of black liquid acid out precipitation rugose wood, under 40～60 ℃ of water bath condition, the pH value is respectively 3.0～4.0 and 12～11.
3. according to the described a kind of method of utilizing the super-critical anti-solvent technology to prepare the nanometer xylogen of claim 1, it is characterized in that: preparation paper industry xylogen dioxane solution is carried out centrifugal with whizzer with 1000～3000r/min revolution, time is 5～10min, get supernatant liquor, its concentration is 4～6mg/mL, the throw out reuse.
4. according to the described a kind of method of utilizing the super-critical anti-solvent technology to prepare the nanometer xylogen of claim 1, it is characterized in that: adopt the anti-solvent method of supercritical co, with carbonic acid gas as anti-solvent, temperature of reaction kettle is 35 ℃～65 ℃, reactor pressure is 15～30MPa, carbon dioxide flow is 10mL/min～30mL/min, and xylogen dioxane solution flow velocity is 2～20mL/min, and nozzle bore is 100～300nm.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102719283A (en) * | 2012-07-05 | 2012-10-10 | 东北林业大学 | Production process of hemicellulose heavy oil |
| CN102732343A (en) * | 2012-07-05 | 2012-10-17 | 东北林业大学 | Production technology of amino-lignin diesel |
| CN102924728A (en) * | 2012-11-16 | 2013-02-13 | 湖南鸿鹰生物科技有限公司 | Method for preparing modified xylogen and applications thereof in wastewater treatment |
| CN103275331A (en) * | 2013-05-23 | 2013-09-04 | 广西大学 | Method for preparing lignin nanoparticles by taking papermaking black liquid as raw material |
| WO2015089456A1 (en) | 2013-12-12 | 2015-06-18 | Solenis Technologies, L.P. | Lignin nanoparticle dispersions and methods for producing and using the same |
| CN104957139A (en) * | 2015-06-15 | 2015-10-07 | 辽宁师范大学 | Application of nano lignosulphonate preparation in promoting growth of plant seedlings |
| CN107663453A (en) * | 2016-07-28 | 2018-02-06 | 东北林业大学 | A kind of preparation method of lignin fluorescent carbon nano-particles |
| CN109320738A (en) * | 2018-09-30 | 2019-02-12 | 杭州市第人民医院 | A method of preparing lignin nanoparticle |
| CN109456634A (en) * | 2018-09-30 | 2019-03-12 | 安徽开林新材料股份有限公司 | A kind of preparation method of wear-resistant paint |
| 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 |
| WO2020000008A1 (en) | 2018-06-27 | 2020-01-02 | Technische Universität Wien | Process for producing lignin particles |
| US11174354B2 (en) | 2016-12-23 | 2021-11-16 | Technische Universität Wien | Production of lignin particles |
| DE102021106727B4 (en) | 2021-03-18 | 2024-07-25 | Forschungszentrum Jülich GmbH | Process for the fractional separation of lignins |
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| CN1565761A (en) * | 2003-06-20 | 2005-01-19 | 郑庆义 | Comprehensive utilization of plant straw and pollution preventing and harnessing method in paper making process |
| CN101284028A (en) * | 2007-04-10 | 2008-10-15 | 李治 | Preparation method of nanometer granule of lignin active substance for cardiovascular medicaments |
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2010
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| US4493797A (en) * | 1983-12-22 | 1985-01-15 | Domtar Inc | Apparatus and method involving supercritical fluid extraction |
| CN1565761A (en) * | 2003-06-20 | 2005-01-19 | 郑庆义 | Comprehensive utilization of plant straw and pollution preventing and harnessing method in paper making process |
| CN101284028A (en) * | 2007-04-10 | 2008-10-15 | 李治 | Preparation method of nanometer granule of lignin active substance for cardiovascular medicaments |
Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102732343A (en) * | 2012-07-05 | 2012-10-17 | 东北林业大学 | Production technology of amino-lignin diesel |
| CN102719283A (en) * | 2012-07-05 | 2012-10-10 | 东北林业大学 | Production process of hemicellulose heavy oil |
| CN102924728A (en) * | 2012-11-16 | 2013-02-13 | 湖南鸿鹰生物科技有限公司 | Method for preparing modified xylogen and applications thereof in wastewater treatment |
| CN103275331A (en) * | 2013-05-23 | 2013-09-04 | 广西大学 | Method for preparing lignin nanoparticles by taking papermaking black liquid as raw material |
| CN103275331B (en) * | 2013-05-23 | 2015-08-12 | 广西大学 | A kind of take black liquid as the preparation method of the lignin nanoparticle of raw material |
| US10035928B2 (en) | 2013-12-12 | 2018-07-31 | Solenis Technologies, L.P. | Lignin nanoparticle dispersions and methods for producing and using the same |
| WO2015089456A1 (en) | 2013-12-12 | 2015-06-18 | Solenis Technologies, L.P. | Lignin nanoparticle dispersions and methods for producing and using the same |
| CN105829406A (en) * | 2013-12-12 | 2016-08-03 | 索理思科技公司 | Lignin nanoparticle dispersions and methods for producing and using the same |
| CN104957139A (en) * | 2015-06-15 | 2015-10-07 | 辽宁师范大学 | Application of nano lignosulphonate preparation in promoting growth of plant seedlings |
| CN107663453A (en) * | 2016-07-28 | 2018-02-06 | 东北林业大学 | A kind of preparation method of lignin fluorescent carbon nano-particles |
| CN107663453B (en) * | 2016-07-28 | 2022-01-11 | 东北林业大学 | Preparation method of lignin fluorescent carbon nanoparticles |
| US11174354B2 (en) | 2016-12-23 | 2021-11-16 | Technische Universität Wien | Production of lignin particles |
| WO2020000008A1 (en) | 2018-06-27 | 2020-01-02 | Technische Universität Wien | Process for producing lignin particles |
| CN112543782A (en) * | 2018-06-27 | 2021-03-23 | 维也纳科技大学 | Method for producing lignin particles |
| CN109320738A (en) * | 2018-09-30 | 2019-02-12 | 杭州市第人民医院 | A method of preparing lignin nanoparticle |
| CN109456634A (en) * | 2018-09-30 | 2019-03-12 | 安徽开林新材料股份有限公司 | A kind of preparation method of wear-resistant paint |
| 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 |
| DE102021106727B4 (en) | 2021-03-18 | 2024-07-25 | Forschungszentrum Jülich GmbH | Process for the fractional separation of lignins |
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