LU500872B1 - Method for adjusting size of lignosulfonate nanorod - Google Patents
Method for adjusting size of lignosulfonate nanorod Download PDFInfo
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- LU500872B1 LU500872B1 LU500872A LU500872A LU500872B1 LU 500872 B1 LU500872 B1 LU 500872B1 LU 500872 A LU500872 A LU 500872A LU 500872 A LU500872 A LU 500872A LU 500872 B1 LU500872 B1 LU 500872B1
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Abstract
The present disclosure relates to a method for adjusting a size of a lignosulfonate nanorod, which belongs to the preparation technique of biomass-based nanomaterials. The method comprises the following actual preparation steps: (1) fractionating lignosulfonate to screen out a lignosulfonate fraction (LS1) with a number average molecular weight greater than 10,000 mol/g; (2) dissolving the LS1 into a salt solution with different types and different concentrations; and (3) dialyzing the obtained solution in an organic solvent for several days, and centrifuging to separate out a nanorod particle with different sizes. The lignosulfonate nanorod with a length of 200-2,000 nm can be prepared according to requirements by selecting or adjusting the type and concentration of the salt solution in the step (2). The lignosulfonate nanorod can be uniformly dispersed in the commonly-used organic solvent and exhibit ultra-high stability. The present disclosure reports for the first time a method for preparing a lignin-based nanorod with controllable size by using lignosulfonate and the salt solution, which is environmentally friendly, and has low cost, simple steps, and good application prospects and market potential.
Description
BL-5320 1 METHOD FOR ADJUSTING SIZE OF LIGNOSULFONATE NANOROD LUs00872
[01] The present disclosure relates to the technical field of nanomaterials, and specifically relates to a method for adjusting a size of a lignosulfonate nanorod.
[02] Disclosure of the background information is only intended to understand the overall background of the present disclosure better, which is not necessarily regarded as an acknowledgement or any form of hint that the information constitutes the prior art known to those ordinarily skilled in the art.
[03] Currently, the renewable biomacromolecule polymers in nature mainly include cellulose, hemicellulose and lignin, which have great application potential in the field of nanomaterials due to their biodegradability, biocompatibility and low cost. Nanocellulose has been widely used in actual production and daily life, while relevant research on using lignin to prepare the nanomaterials makes progress slowly. So far, there is no method for preparing and adjusting the lignin-based nanorod except for some research on the preparation and adjusting the nanosphere.
[04] Recently, the applicant has reported for the first time a method of fractionating lignosulfonate by ethanol, and using the obtained fraction to produce a nanosphere and a nanorod, respectively. However, the subsequent studies found that although the size of the lignosulfonate nanosphere prepared by the method can be adjusted, the size of the nanorod cannot be adjusted. Obtaining the nanoparticle with controllable morphology and size is a necessary condition for improving its functional application in the field of biomass-based material synthesis. Therefore, adjusting the size of the nanorod is the key to realize the industrial application of the lignosulfonate nanorod.
[05] The present disclosure provides a method for adjusting a size of a lignosulfonate nanorod to solve the problems that the lignosulfonate nanorod has single size and cannot meet the needs of different experiments or applications.
[06] To achieve the above-mentioned objects, the present disclosure employs the following technical solutions:
[07] In the first aspect, the method for adjusting the size of the lignosulfonate nanorod is provided by the present disclosure, comprising:
[08] fractionating lignosulfonate LSO to screen out a lignosulfonate fraction LS1 with a number average molecular weight greater than 10,000 mol/g;
[09] dissolving the lignosulfonate fraction LS1 into an inorganic salt solution, to obtain a salt solution of lignosulfonate; and
[10] placing the salt solution of lignosulfonate in a dialysis bag filled with an organic solvent for dialysis, to obtain the lignosulfonate nanorod.
[11] The present disclosure proposes the method for adjusting the size of the lignosulfonate nanorod by adding the positively charged inorganic salt in the early dissolution stage to damage the electron double layer on the macromolecular surface of
BL-5320 2 lignosulfonate, and affecting the subsequent self-adsorption process to adjust the size LU500872 of the lignosulfonate nanorod. The method of the present disclosure can adjust the size of the lignosulfonate nanorod within the range of 200-2,000 nm, which is of great significance for the subsequent industrial application of the lignosulfonate nanorod.
[12] In the second aspect, the present disclosure proposes the lignosulfonate nanorod prepared by the above-mentioned method, and a length of the lignosulfonate nanorod is 200-2,000 nm.
[13] The lignosulfonate nanorod prepared by the present disclosure can be uniformly dispersed in the commonly-used organic solvent and exhibit ultra-high stability. Therefore, the method has good application prospects and market potential regardless of the function and role of the nanorod or the low preparation cost.
[14] In the third aspect, the present disclosure provides an application of the lignosulfonate nanorod in fields of nanomaterials and biomaterials.
[15] The steps for preparing the lignosulfonate nanorod with controllable size of the present disclosure is extremely simple and environmentally friendly. Therefore, it is expected to be widely used in the fields of nanomaterials and biomaterials.
[16] The beneficial effects of the present disclosure are as follows:
[17] (1) Compared with the prior art, the present disclosure reports for the first time the method for preparing the lignosulfonate nanorod with controllable size using lignosulfonate and the salt solution. There is no any harmful and toxic medicines added in the whole preparation process. The steps are extremely simple and environmentally friendly, and the costs of raw materials and other medicines are extremely low.
[18] (2) The present disclosure can adjust the size of the nanorod only according to the initial salt concentration, and prepare the lignosulfonate nanorod with the length of 200-2,000 nm using the method, which can meet the needs of different production experiments. In addition, the nanorod can be uniformly dispersed in the commonly- used organic solvent, and exhibit ultra-high stability. Therefore, the method has good application prospects and market potential regardless of the function and role of the nanorod or the low preparation cost.
[19] (3) The preparation method of the present disclosure has simple and convenient operation and good practicability, which is easy to popularize.
[20] The drawings as part of the present disclosure are used to further understand the present disclosure, and the exemplary examples and their descriptions of the present disclosure are used to illustrate the present disclosure, not to improperly limit the present disclosure.
[21] FIG. 1 is a technical roadmap of the present disclosure;
[22] FIG. 2 is a scanning electron micrograph of a nanorod with different sizes obtained in Example 1 of the present disclosure;
[23] FIG. 3 is a scanning electron micrograph of a nanorod with different sizes obtained in Example 2 of the present disclosure; and
[24] FIG. 4 is a scanning electron micrograph of a nanorod with different sizes obtained in Example 3 of the present disclosure.
BL-5320 3 LU5008 72
[25] It shall be noted that the following detailed descriptions are all exemplary, intended to further illustrate the present disclosure. Unless otherwise specified, all technical and scientific terms used in the present disclosure have the same meanings as commonly understood by those ordinarily skilled in the technical field to which the present disclosure belongs.
[26] It shall be noted that the terms used herein are only used to describe the specific examples, not intended to limit the exemplary examples of the present disclosure. Unless the context clearly indicates to the contrary, the terms used herein in the singular form shall include the plural form. In addition, it shall also be understood that the terms "includes" and/or "including" used in the description shall be deemed to indicate the features, steps, operations, devices, components, and/or combinations thereof.
[27] A method for adjusting the size of the lignosulfonate nanorod includes the following actual preparation steps that:
[28] Step 1: lignosulfonate is fractionated to obtain the lignosulfonate fraction with the number average molecular weight greater than 10,000 mol/g.
[29] For example, the 70% aqueous ethanol solution is used to dissolve lignosulfonate under stirring at room temperature, and the 40% aqueous ethanol solution is used to continue to dissolve the insoluble solid residue; then the 40% aqueous ethanol solution and ethanol in the aqueous phase are removed by rotary evaporation, to obtain the lignosulfonate fraction (LS1) under freeze-drying.
[30] In some examples, the method for fractionating lignosulfonate may also be other commonly-used fractionating methods, such as ultrafiltration method, organic solvent extraction method and the like.
[31] Step 2: the lignosulfonate fraction (LS1) and the inorganic salt with a certain mass, such as sodium chloride, calcium chloride and the like, are dissolved into the deionized water, to prepare the salt solution of lignosulfonate.
[32] In some examples, the type and mass of the inorganic salt added is the key to affect the size of the lignosulfonate nanorod in the later stage. The inorganic salt added can be one or any combinations in any proportions of sodium chloride, calcium chloride, magnesium chloride, sodium sulfate, and calcium sulfate.
[33] Step 3: the salt solution of lignosulfonate obtained is stirred in the magnetic stirrer, and then put in the dialysis bag filled with the organic solvent to dialyze for seven days, to obtain the lignosulfonate nanorod in the dialysis bag.
[34] Step 4: the organic solvent as the dialysate is put into the centrifuge tube for centrifuging in the high-speed centrifuge, the supernatant is removed, and ethanol and methanol used as the organic solvent are used to wash for several times, then the obtained solid precipitate is freeze-dried to obtain the lignosulfonate nanorod particle.
[35] The present disclosure will be further described in detail below in conjunction with specific examples. It shall be pointed out that the specific examples are only used to illustrate but not to limit the present disclosure.
[36] In the following examples, the percentages for mixing ethanol with water all refer to the volume percentage.
BL-5320 4
[37] Example 1 LU500872
[38] The dried lignosulfonate is weighed with 15 g to mix with 100 mL of 70% aqueous ethanol solution by stirring at 300 rpm and room temperature for 2 h, then filtration and separation are performed, and 100 mL of 40% aqueous ethanol solution is used to dissolve the insoluble residue, to obtain the aqueous ethanol solution fraction of lignosulfonate. Then, the rotary evaporation and freeze-drying are performed, to obtain the lignosulfonate fraction (LS1). The calcium chloride solid (1 wt%) with 0.001 g and the lignosulfonate fraction (LS1) with 0.099 g are weighed to dissolve in 100 mL of deionized water, to obtain the salt solution of lignosulfonate. The salt solution of lignosulfonate is put in the magnetic stirrer to stir at 800 rpm for 60 min, and then put in the dialysis bag to be completely soaked by ethanol to dialyze for 7 days with the dialysate being changed every other day, to obtain the ethanol dispersion phase of the lignosulfonate nanorod. The solid precipitate is obtained after centrifuging in the high- speed centrifuge and then washing with ethanol for 6 times, which is the lignosulfonate nanorod. The test result is shown in FIG. 2. The length of the lignosulfonate nanorod is about 600 nm.
[39] Example 2
[40] The dried lignosulfonate is weighed with 15 g to mix with 100 mL of 70% aqueous ethanol solution by stirring at 300 rpm and room temperature for 2 h, then filtration and separation are performed, and 100 mL of 40% aqueous ethanol solution is used to dissolve the insoluble residue, to obtain the aqueous ethanol solution fraction of lignosulfonate. Then, the rotary evaporation and freeze-drying are performed, to obtain the lignosulfonate fraction (LS1). The calcium chloride solid (2 wt%) with 0.002 g and the lignosulfonate fraction (LS1) with 0.098 g are weighed to dissolve in 100 mL of deionized water, to obtain the salt solution of lignosulfonate. The salt solution of lignosulfonate is put in the magnetic stirrer to stir at 800 rpm for 60 min, and then put in the dialysis bag to be completely soaked by ethanol to dialyze for 7 days with the dialysate being changed every other day, to obtain the ethanol dispersion phase of the lignosulfonate nanorod. The solid precipitate is obtained after centrifuging in the high- speed centrifuge and then washing with ethanol for 6 times, which is the lignosulfonate nanorod. The test result is shown in FIG. 3. The length of the lignosulfonate nanorod is about 800 nm.
[41] Example 3
[42] The dried lignosulfonate is weighed with 15 g to mix with 100 mL of 70% aqueous ethanol solution by stirring at 300 rpm and room temperature for 2 h, then filtration and separation are performed, and 100 mL of 40% aqueous ethanol solution is used to dissolve the insoluble residue, to obtain the aqueous ethanol solution fraction of lignosulfonate. Then, the rotary evaporation and freeze-drying are performed, to obtain the lignosulfonate fraction (LS1). The calcium chloride solid (10 wt%) with
0.010 g and the lignosulfonate fraction (LS1) with 0.090 g are weighed to dissolve in 100 mL of deionized water, to obtain the salt solution of lignosulfonate. The salt solution of lignosulfonate is put in the magnetic stirrer to stir at 800 rpm for 60 min, and then put in the dialysis bag to be completely soaked by ethanol to dialyze for 7 days with the dialysate being changed every other day, to obtain the ethanol dispersion phase
BL-5320 5 of the lignosulfonate nanorod. The solid precipitate is obtained after centrifuging in the LU500872 high-speed centrifuge and then washing with ethanol for 6 times, which is the lignosulfonate nanorod. The test result is shown in FIG. 4. The length of the lignosulfonate nanorod is about 5 um.
[43] Example 4
[44] The dried lignosulfonate is weighed with 15 g to mix with 100 mL of 70% aqueous ethanol solution by stirring at 300 rpm and room temperature for 2 h, then filtration and separation are performed, and 100 mL of 40% aqueous ethanol solution is used to dissolve the insoluble residue, to obtain the aqueous ethanol solution fraction of lignosulfonate. Then, the rotary evaporation and freeze-drying are performed, to obtain the lignosulfonate fraction (LS1). The sodium chloride solid (10 wt%) with
0.010 g and the lignosulfonate fraction (LS1) with 0.090 g are weighed to dissolve in 100 mL of deionized water, to obtain the salt solution of lignosulfonate. The salt solution of lignosulfonate is put in the magnetic stirrer to stir at 800 rpm for 60 min, and then put in the dialysis bag to be completely soaked by ethanol to dialyze for 7 days with the dialysate being changed every other day, to obtain the ethanol dispersion phase of the lignosulfonate nanorod. The solid precipitate obtained after centrifuging in the high-speed centrifuge and then washing with ethanol for 6 times is the lignosulfonate nanorod.
[45] Example 5
[46] The dried lignosulfonate is weighed with 15 g to mix with 100 mL of 70% aqueous ethanol solution by stirring at 300 rpm and room temperature for 2 h, then filtration and separation are performed, and 100 mL of 40% aqueous ethanol solution is used to dissolve the insoluble residue, to obtain the aqueous ethanol solution fraction of lignosulfonate. Then, the rotary evaporation and freeze-drying are performed, to obtain the lignosulfonate fraction (LS1). The magnesium chloride solid (10 wt%) with
0.010 g and the lignosulfonate fraction (LS1) with 0.090 g are weighed to dissolve in 100 mL of deionized water, to obtain the salt solution of lignosulfonate. The salt solution of lignosulfonate is put in the magnetic stirrer to stir at 800 rpm for 60 min, and then put in the dialysis bag to be completely soaked by ethanol to dialyze for 7 days with the dialysate being changed every other day, to obtain the ethanol dispersion phase of the lignosulfonate nanorod. The solid precipitate obtained after centrifuging in the high-speed centrifuge and then washing with ethanol for 6 times is the lignosulfonate nanorod.
[47] Example 6
[48] The dried lignosulfonate is weighed with 15 g to mix with 100 mL of 70% aqueous ethanol solution by stirring at 300 rpm and room temperature for 2 h, then filtration and separation are performed, and 100 mL of 40% aqueous ethanol solution is used to dissolve the insoluble residue, to obtain the aqueous ethanol solution fraction of lignosulfonate. Then, the rotary evaporation and freeze-drying are performed, to obtain the lignosulfonate fraction (LS1). The calcium sulfate solid (10 wt%) with 0.010 g and the lignosulfonate fraction (LS1) with 0.090 g are weighed to dissolve in 100 mL of deionized water, to obtain the salt solution of lignosulfonate. The salt solution of lignosulfonate is put in the magnetic stirrer to stir at 800 rpm for 60 min, and then put
BL-5320 6 in the dialysis bag to be completely soaked by ethanol to dialyze for 7 days with the LU500872 dialysate being changed every other day, to obtain the ethanol dispersion phase of the lignosulfonate nanorod. The solid precipitate obtained after centrifuging in the high- speed centrifuge and then washing with ethanol for 6 times is the lignosulfonate nanorod.
[49] Example 7
[50] The dried lignosulfonate is weighed with 15 g to mix with 100 mL of 70% aqueous ethanol solution by stirring at 300 rpm and room temperature for 2 h, then filtration and separation are performed, and 100 mL of 40% aqueous ethanol solution is used to dissolve the insoluble residue, to obtain the aqueous ethanol solution fraction of lignosulfonate. Then, the rotary evaporation and freeze-drying are performed, to obtain the lignosulfonate fraction (LS1). The sodium sulfate solid (10 wt%) with 0.010 g and the lignosulfonate fraction (LS1) with 0.090 g are weighed to dissolve in 100 mL of deionized water, to obtain the salt solution of lignosulfonate. The salt solution of lignosulfonate is put in the magnetic stirrer to stir at 800 rpm for 60 min, and then put in the dialysis bag to be completely soaked by ethanol to dialyze for 7 days with the dialysate being changed every other day, to obtain the ethanol dispersion phase of the lignosulfonate nanorod. The solid precipitate obtained after centrifuging in the high- speed centrifuge and then washing with ethanol for 6 times is the lignosulfonate nanorod.
[51] Example 8
[52] The dried lignosulfonate is weighed with 15 g to mix with 100 mL of 70% aqueous ethanol solution by stirring at 300 rpm and room temperature for 2 h, then filtration and separation are performed, and 100 mL of 40% aqueous ethanol solution is used to dissolve the insoluble residue, to obtain the aqueous ethanol solution fraction of lignosulfonate. Then, the rotary evaporation and freeze-drying are performed, to obtain the lignosulfonate fraction (LS1). The calcium sulfate solid (10 wt%) with 0.010 g and the lignosulfonate fraction (LS1) with 0.090 g are weighed to dissolve in 100 mL of deionized water, to obtain the salt solution of lignosulfonate. The salt solution of lignosulfonate is put in the magnetic stirrer to stir at 800 rpm for 60 min, and then put in the dialysis bag to be completely soaked by y-valerolactone to dialyze for 7 days with the dialysate being changed every other day, to obtain the ethanol dispersion phase of the lignosulfonate nanorod. The solid precipitate obtained after centrifuging in the high- speed centrifuge and then washing with ethanol for 6 times is the lignosulfonate nanorod.
[53] Example 9
[54] The dried lignosulfonate is weighed with 15 g to mix with 300 mL of 70% aqueous ethanol solution by stirring at 300 rpm and room temperature for 2 h, and then fractionation is performed using the ultrafiltration membrane, to obtain the lignosulfonate fraction (LS1) with the number average molecular weight greater than 10,000 mol/g. The calcium sulfate solid (10 wt%) with 0.010 g and the lignosulfonate fraction (LS1) with 0.090 g are weighed to dissolve in 100 mL of deionized water, to obtain the salt solution of lignosulfonate. The salt solution of lignosulfonate is put in the magnetic stirrer to stir at 800 rpm for 60 min, and then put in the dialysis bag to be
BL-5320 7 completely soaked by y-valerolactone to dialyze for 7 days with the dialysate being LU500872 changed every other day, to obtain the ethanol dispersion phase of the lignosulfonate nanorod. The solid precipitate obtained after centrifuging in the high-speed centrifuge and then washing with ethanol for 6 times is the lignosulfonate nanorod.
[55] In the end, it shall be noted that the above examples are only the preferred examples of the present disclosure, not intended to limit the present disclosure. Although the present disclosure has been described in detail with reference to the above examples, modifications or equivalent replacements of the technical solutions described in the above examples still can be made by those skilled in the art. Any modifications, equivalent replacements, and improvements made within the spirit and principle of the present disclosure shall be included in the protection scope of the present disclosure. Although the specific implementation of the present disclosure is described above, it is not used to limit the protection scope of the present disclosure. It shall be understood by those skilled in the art that various modifications or variations can be made by those skilled in the art without creative work on the basis of the technical solutions of the present disclosure, which shall fall within the protection scope of the present disclosure.
Claims (10)
1. A method for adjusting a size of a lignosulfonate nanorod, wherein, comprising: fractionating lignosulfonate LSO to screen out a lignosulfonate fraction LS1 with a number average molecular weight greater than 10,000 mol/g; dissolving the lignosulfonate fraction LS1 into an inorganic salt solution, to obtain a salt solution of lignosulfonate; and placing the salt solution of lignosulfonate in a dialysis bag filled with an organic solvent for dialysis, to obtain the lignosulfonate nanorod.
2. The method for adjusting the size of the lignosulfonate nanorod according to claim 1, wherein, the lignosulfonate nanorod 1s performed with solid-liquid separation, washing, and drying, to obtain a lignosulfonate nanorod particle.
3. The method for adjusting the size of the lignosulfonate nanorod according to claim 1, wherein, an inorganic salt in the inorganic salt solution 1s at least one of sodium chloride, calcium chloride, magnesium chloride, sodium sulfate, and calcium sulfate.
4. The method for adjusting the size of the lignosulfonate nanorod according to claim 1, wherein, a concentration of the inorganic salt solution is 1-10 wt%.
5. The method for adjusting the size of the lignosulfonate nanorod according to claim 1, wherein, a mass-volume ratio of the lignosulfonate fraction LS1 to the inorganic salt solution is 0.090-0.099 g:100 mL.
6. The method for adjusting the size of the lignosulfonate nanorod according to claim 1, wherein, specific steps for fractionating are as follows: mixing lignosulfonate with a 70% aqueous ethanol solution, and filtering to separate out an insoluble residue, then dissolving the insoluble residue with a 40% aqueous ethanol solution, to obtain an aqueous ethanol solution fraction of lignosulfonate; then performing rotary evaporation and freeze-drying to obtain the lignosulfonate fraction LS1.
7. The method for adjusting the size of the lignosulfonate nanorod according to claim 1, wherein, the dialysis is performed for 7-10 days under stirring conditions, and the organic solvent as a dialysate is changed every day.
8. The method for adjusting the size of the lignosulfonate nanorod according to claim 1, wherein, the organic solvent used for the dialysis is ethanol or y-valerolactone.
9. The method for adjusting the size of the lignosulfonate nanorod according to any one of claims 1-8, wherein, a length of the lignosulfonate nanorod is 200-2,000 nm.
10. An application of the lignosulfonate nanorod of claim 9 in fields of nanomaterials and biomaterials.
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| CN202011597833.2A CN112871101B (en) | 2020-12-29 | 2020-12-29 | Method for adjusting size of lignosulfonate nanorod |
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| US3271382A (en) * | 1963-09-26 | 1966-09-06 | Rayonier Inc | Recovery of lignosulfonates from spent sulfite liquors |
| US5286412A (en) * | 1991-10-16 | 1994-02-15 | Georgia-Pacific Corporation | Modified lignosulfonate dispersant for gypsum |
| CN101633513A (en) * | 2008-07-25 | 2010-01-27 | 中国科学院研究生院 | Method for preparing cerium hydroxide nano rod |
| BR112016012411B1 (en) * | 2013-12-12 | 2021-03-30 | Solenis Technologies, L.P. | METHOD FOR PREPARING A WATER DISPERSION OF LIGNINE NANOPARTICLES |
| CN110668420B (en) * | 2019-10-24 | 2021-07-02 | 四川大学 | Preparation method of lignin-based carbon material rich in mesopores or mesopores and macropores |
| CN111889044B (en) * | 2020-07-30 | 2022-05-27 | 齐鲁工业大学 | Preparation method of lignosulfonate nanosphere nanorod |
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