CN103145999A - Preparation method of nano lignin with controllable particle size - Google Patents
Preparation method of nano lignin with controllable particle size Download PDFInfo
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Abstract
The invention discloses a preparation method of nano lignin with a controllable particle size, relates to a preparation method of nano lignin and aims to solve the problems of higher preparation technology requirement, complexity in operation and uncontrollable particle size of the prepared nano lignin in the traditional nano lignin preparation method. The method comprises the following steps of: firstly, pretreating alkali lignin; secondly, carrying out grinding treatment; thirdly, preparing an alkali lignin suspension liquid; fourthly, preparing a nano lignin sol; and fifthly, preparing powder to obtain nano lignin. The preparation method has the advantages that the particle size is controlled between 10nm and 70nm, the average particle size is about 30nm, and the content of particles with the particle size of about 26nm is the highest; and the method is simple in process, easy to operate and free of environment pollution. The preparation method is mainly used for preparing the nano lignin.
Description
Technical field
The present invention relates to a kind of preparation method of nano wood quality.
Background technology
Xylogen is a kind of complicated phenol polymer that is formed by four kinds of alcohol monomers (to tonquinol, lubanol, 5-hydroxyl lubanol, sinapyl alcohol).Xylogen is that occurring in nature is only second to cellulosic second largest renewable resources, and alkali lignin is the main component of papermaking digesting waste liquor, and abundant as renewable resources output, low price has degradability.Xylogen is as the secondary metabolites in growth and development of plants, in the cell walls lignification, xylogen penetrates in cell walls, be filled in the cell walls framework, strengthened the hardness of cell walls, strengthen mechanical holding power or the ultimate compression strength of cell, promoted the formation of mechanical tissue, be conducive to consolidate and support the effects such as plant materials and water conduction.Due to the chemical property of xylogen, make the plant xylem have Surface hydrophobicity of cell as insolubility and complicated phenol polymer simultaneously.Woodenly usually have a extensive future in fields such as biochemical industries as dispersion agent, sorbent material etc.The characteristics such as the high-specific surface area of nano wood quality have a extensive future in fields such as tensio-active agent, support of the catalyst, photochemical catalysis.But existing nano wood quality is mainly to utilize the dissolving of dioxane equal solvent, and technology of preparing is had relatively high expectations, as adopting supercritical technology etc., and complicated operation, and the nano wood quality particle diameter for preparing is uncontrollable.
Summary of the invention
The objective of the invention is to solve the existing method that prepare the nano wood quality and exist technology of preparing to have relatively high expectations, complicated operation, and the uncontrollable problem of nano wood quality particle diameter for preparing, and a kind of preparation method of particle diameter controllable nano xylogen is provided.
A kind of preparation method of particle diameter controllable nano xylogen specifically completes: one, alkali lignin pre-treatment: utilize the alkali extraction and acid precipitation method that alkali lignin is processed, namely obtain refining alkali lignin according to the following steps; Two, milled processed: the refining alkali lignin that step 1 is obtained carries out milled processed, then crosses 80～120 mesh sieves, namely obtains particle diameter less than the alkali lignin of 0.2mm; Three, preparation alkali lignin suspension: particle diameter is put into deionized water less than the alkali lignin of 0.2mm, then carry out supersound process 5min～15min, namely obtain alkali lignin suspension; Four, preparation nano wood quality colloidal sol: the alkali lignin suspension that step 3 is obtained is placed in high pressure homogenizer, is to circulate under 900bar～l000bar 2～3 times at pressure, namely obtains nano wood quality colloidal sol; Five, powder process: temperature for-18 ° of C～-the nano wood quality colloidal sol that step 4 obtained under 2O ° C carries out freezingly, freezing 24h～26h, and then be-45 ° of C～-55 ° C lyophilize 24h～26h in temperature namely obtains the nano wood quality; Particle diameter described in step 3 is (1g～3g): 100mL less than the volume ratio of the quality of the alkali lignin of 0.2mm and deionized water.
Advantage of the present invention: one, the present invention utilizes the nano wood quality of supersound process and high-pressure homogeneous processing preparation, and nano wood quality particle diameter is controlled between 10mm～70mn, and median size is for being about 30nm, and particle diameter is that to be about the particle content of 26nm maximum; Two, technique of the present invention is simple, and is easy to operate, do not adopt the dioxane equal solvent, avoids environmental pollution, and the nano wood quality of the present invention's preparation has a extensive future in field of functional materials such as photochemical catalysis.
Description of drawings
Fig. 1 is infrared spectrogram, and in Fig. 1, a is the infrared spectrogram of the nano wood quality of test one preparation, and in Fig. 1, b is the infrared spectrogram of the refining alkali lignin of test one simultaneous test step 1 preparation;
Fig. 2 is the histogram of particle size distribution of the nano wood quality of test one simultaneous test preparation;
Fig. 3 is the histogram of particle size distribution of the nano wood quality of test one preparation;
Fig. 4 is the transmission electron microscope figure of the nano wood quality of test one preparation.
Embodiment
Embodiment one: present embodiment is a kind of preparation method of particle diameter controllable nano xylogen, specifically completes according to the following steps: one, alkali lignin pre-treatment: utilize the alkali extraction and acid precipitation method that alkali lignin is processed, namely obtain refining alkali lignin; Two, milled processed: the refining alkali lignin that step 1 is obtained carries out milled processed, then crosses 80～120 mesh sieves, namely obtains particle diameter less than the alkali lignin of 0.2mm; Three, preparation alkali lignin suspension: particle diameter is put into deionized water less than the alkali lignin of 0.2mm, then carry out supersound process 5min-15min, namely obtain alkali lignin suspension; Four, preparation nano wood quality colloidal sol: the alkali lignin suspension that step 3 is obtained is placed in high pressure homogenizer, is to circulate under 900bar～1000bar 2～3 times at pressure, namely obtains nano wood quality colloidal sol; Five, powder process: carry out freezingly in temperature for the nano wood quality colloidal sol that under-18 ° of C～-20 ° C, step 4 is obtained, freezing 24h～26h, and then be-45 ° of C～-55 ° C lyophilize 24h～26h in temperature namely obtains the nano wood quality; Particle diameter described in step 3 is (1g～3g): 100mL less than the volume ratio of the quality of the alkali lignin of 0.2mm and deionized water.
Present embodiment is utilized the nano wood quality of supersound process and high-pressure homogeneous processing preparation, and nano wood quality particle diameter is controlled between 10nm-70nm, and median size is for being about 30nm, and particle diameter is that to be about the particle content of 26nm maximum.
Present embodiment technique is simple, and is easy to operate, do not adopt the dioxane equal solvent, avoids environmental pollution, and the nano wood quality of present embodiment preparation has a extensive future in field of functional materials such as photochemical catalysis.
embodiment two: the difference of present embodiment and embodiment one is: the alkali extraction and acid precipitation method specific operation process described in step 1 is as follows: at first alkali lignin is dissolved in the NaOH solution that concentration is 0.5mol/L-1.5mol/L, then carry out centrifugation, obtain supernatant liquor, to adopt massfraction under the water bath with thermostatic control of 55 ° of C～65 ° C of temperature be 12% aqueous hydrochloric acid transfers to the pH value of supernatant liquor till 6～7, and then carry out centrifugation, obtain the brown precipitation, adopt deionized water wash brown precipitation, wash be neutrality to the pH value of filtrate till, then be under 40 ° of C-50 ° of C, the precipitation after washing to be carried out drying in temperature, dry 20h～28h, namely obtain refining alkali lignin, the quality of described alkali lignin and concentration are that the volume ratio of the NaOH solution of 0.5mol/L～1.5mol/L is 1g:(5lnL-7lnL).Other are identical with embodiment one.
Embodiment three: present embodiment and one of embodiment one or two difference are: the refining alkali lignin that in step 2, step 1 is obtained carries out crossing 100 mesh sieves after milled processed.Other are identical with embodiment one or two.
Embodiment four: one of present embodiment and embodiment one to three difference is: the supersound process specific operation process described in step 3 is as follows: in ultrasonic frequency during to be the particle diameter that step 2 obtained under auxiliary of the ultrasonic wave of 40Hz～50Hz be scattered in deionized water less than the alkali lignin of 0.2mm.Other are identical with embodiment one to three.
Embodiment five: one of present embodiment and embodiment one to four difference is: circulate 2 times under 1000bar in step 4.Other are identical with embodiment one to four.
Adopt following verification experimental verification effect of the present invention
Test one: a kind of preparation method of particle diameter controllable nano xylogen, specifically complete: one, alkali lignin pre-treatment: utilize the alkali extraction and acid precipitation method that alkali lignin is processed, namely obtain refining alkali lignin according to the following steps; Two, milled processed: the refining alkali lignin that step 1 is obtained carries out milled processed, then crosses 80 mesh sieves, namely obtains particle diameter less than the alkali lignin of 0.2mm; Three, preparation alkali lignin suspension: the 10g particle diameter is put into the 500mL deionized water less than the alkali lignin of 0.2mm, then carry out supersound process 5min, namely obtain alkali lignin suspension; Four, preparation nano wood quality colloidal sol: the alkali lignin suspension that step 3 is obtained is placed in high pressure homogenizer, is to circulate under 1000bar 2～3 times at pressure, namely obtains nano wood quality colloidal sol; Five, powder process: carry out freezingly in temperature for the nano wood quality colloidal sol that under-18 ° of C, step 4 is obtained, freezing 24h, and then be-50 ° of C lyophilize 24h in temperature namely obtains the nano wood quality.
Alkali lignin described in this testing sequence one is the industrial soda xylogen.
Alkali extraction and acid precipitation method specific operation process described in this testing sequence one is as follows: hundred first are dissolved in the 30g alkali lignin in the NaOH solution that 180mL concentration is 1.0mol/L, so carry out centrifugation, obtain supernatant liquor, to adopt massfraction under the water bath with thermostatic control of 60 ° of C of temperature be 12% aqueous hydrochloric acid transfers to the pH value of supernatant liquor till 6～7, obtain the brown precipitation, adopt deionized water wash brown precipitation, wash be neutrality to the pH value of filtrate till, then be under 45 ° of C, the precipitation after washing to be carried out drying in temperature, dry 24h namely obtains refining alkali lignin.
Under supersound process specific operation process described in this testing sequence three adds: in ultrasonic frequency during to be the particle diameter that step 2 obtained under auxiliary of the ultrasonic wave of 45Hz be scattered in deionized water less than the alkali lignin of 0.2mm.
Test a simultaneous test: a kind of preparation method of nano wood quality, specifically complete: one, alkali lignin pre-treatment: utilize the alkali extraction and acid precipitation method that alkali lignin is processed, namely obtain refining alkali lignin according to the following steps; Two, milled processed: the refining alkali lignin that step 1 is obtained carries out milled processed, then crosses 80 mesh sieves, namely obtains particle diameter less than the alkali lignin of 0.2mm; Three, preparation alkali lignin suspension: the 10g particle diameter is put into the 500mL deionized water less than the alkali lignin of 0.2mm, then carry out supersound process 5min, namely obtain alkali lignin suspension; Four, powder process: carry out freezingly in temperature for the alkali lignin suspension that under-18 ° of C, step 3 is obtained, freezing 24h, and then be-50 ° of C lyophilize 24h in temperature namely obtains the nano wood quality.
Alkali lignin described in this testing sequence one is the industrial soda xylogen.
Alkali extraction and acid precipitation method specific operation process described in this testing sequence one is as follows: hundred first are dissolved in the 30g alkali lignin in the NaOH solution that 180mL concentration is 1.0mol/L, so carry out centrifugation, obtain Pu liquid, to adopt massfraction under the water bath with thermostatic control of 60 ° of C of temperature be 12% aqueous hydrochloric acid transfers to the pH value of supernatant liquor till 6～7, obtain the brown precipitation, adopt deionized water wash brown precipitation, wash be neutrality to the pH value of filtrate till, then be under 45 ° of C, the precipitation after washing to be carried out drying in temperature, dry 24h namely obtains refining alkali lignin.
Adopt Fourier transform infrared spectrometer to detect and test the refining alkali lignin of step 1 in a nano wood quality for preparing and test one simultaneous test, detected result as shown in Figure 1, Fig. 1 is infrared spectrogram, in Fig. 1, a is the infrared spectrogram of the nano wood quality of test one preparation, and in Fig. 1, b is the infrared spectrogram of the refining alkali lignin of step 1 in test one; As can be seen from Figure 1, the position of both main absorption peaks is consistent, and the intensity at peak is slightly had any different, and illustrates that homogenizing process is a physical process, does not relate to chemical reaction.Main absorption peak ownership in Fig. 1 is respectively: 1032.56cm
-1The place is methylol (CH
2OH) absorption peak of C-O in, 1118.02cm
-1The place is the stretching vibration absorption peak of ehter bond-O-, 1606.23cm
-1, 1462.54cm
-1The place is the vibration absorption peak of xylogen aromatic ring frame, 2937.68cm
-1Be the stretching vibration absorption peak of methylene radical C-H, 3427.2lcm
-1It is hydroxyl O-H stretching vibration absorption peak, result shown in Figure 1 shows that the nano wood quality of test one preparation contains abundant oxygen-containing functional group, homogenizing process is a physical process, therefore do not relate to chemical reaction, testing step 1 in the nano wood quality of a preparation and test one simultaneous test, to make with extra care the infrared analysis functional group of alkali lignin be consistent.
Adopt particle-size analyzer to detect the nano wood quality of test one simultaneous test preparation and the nano wood quality of test one preparation, detected result as shown in Figures 2 and 3; Fig. 2 is the histogram of particle size distribution of the nano wood quality of test one simultaneous test preparation; Fig. 3 is the histogram of particle size distribution of the nano wood quality of test one preparation; The nano wood quality particle diameter of testing as shown in Figure 3 a preparation is controlled between 10nm～60nm, and the nano wood quality median size of test one preparation is 31.3nm, and wherein particle diameter is that the particle content of 26.5nm is maximum; Test as shown in Figure 3 one and utilize the nano wood quality size distribution of supersound process and high-pressure homogeneous processing preparation more even, particle diameter distribution width is narrower.
Adopt the nano wood quality of transmission electron microscope observation test one preparation, observations as shown in Figure 4, Fig. 4 is the transmission electron microscope figure of the nano wood quality of test one preparation; Testing as shown in Figure 4 one utilizes the nano wood quality size distribution of supersound process and high-pressure homogeneous processing preparation more even.
Test two: this test with the difference of test one is: the refining alkali lignin that in step 2, step 1 is obtained carries out crossing 100 mesh sieves after milled processed.Other are identical with test one.
Test three: this test with the difference of test one is: the refining alkali lignin that in step 2, step 1 is obtained carries out crossing 120 mesh sieves after milled processed.Other are identical with test one.
Test four: this test with the difference of test one is: in step 3, the 12.5g particle diameter is put into the 500mL deionized water less than the alkali lignin of 0.2mm, then carry out supersound process 5min, namely obtain alkali lignin suspension.Other are identical with test one.
Test five: this test with the difference of test one is: in step 3, the 15g particle diameter is put into the 500mL deionized water less than the alkali lignin of 0.2mm, then carry out supersound process 5min, namely obtain alkali lignin suspension.Other are identical with test one.
Test six: this test with the difference of test one is: in step 3, the 10g particle diameter is put into the 500mL deionized water less than the alkali lignin of 0.2mm, then carry out supersound process 10min, namely obtain alkali lignin suspension.Other are identical with test one.
Test seven: this test with the difference of test one is: in step 3, the 10g particle diameter is put into the 500mL deionized water less than the alkali lignin of 0.2mm, then carry out supersound process 15min, namely obtain alkali lignin suspension.Other are identical with test one.
Adopt particle-size analyzer to detect test one to the nano wood quality of test seven preparations, and calculate particle diameter mean value and the maximum particle diameter of content, as shown in table 1; The nano wood quality particle diameter of the present invention preparation is controlled as can be known by table 1.
Table 1
| ? | Median size/nm | Particle diameter/nm that content is maximum |
| Test one | 31.3 | 26.5 |
| Test two | 30.7 | 25.4 |
| Test three | 30.5 | 25.4 |
| Test four | 32.6 | 27.2 |
| Test five | 35.2 | 28.3 |
| Test six | 30.9 | 25.4 |
| Test seven | 30.4 | 25.3 |
Claims (5)
1. the preparation method of a particle diameter controllable nano xylogen, the preparation method who it is characterized in that particle diameter controllable nano xylogen completes according to the following steps: one, alkali lignin pre-treatment: utilize the alkali extraction and acid precipitation method that alkali lignin is processed, namely obtain refining alkali lignin; Two, milled processed: the refining alkali lignin that step 1 is obtained carries out milled processed, then crosses the 80-120 mesh sieve, namely obtains particle diameter less than the alkali lignin of 0.2mm; Three, preparation alkali lignin suspension: particle diameter is put into deionized water less than the alkali lignin of 0.2mm, then carry out supersound process 5min～15min, namely obtain alkali lignin suspension; Four, preparation nano wood quality colloidal sol: the alkali lignin suspension that step 3 is obtained is placed in high pressure homogenizer, is to circulate under 900bar～1000bar 2～3 times at pressure, namely obtains nano wood quality colloidal sol; Five, powder process: carry out freezingly in temperature for the nano wood quality colloidal sol that under-18 ° of C～-20 ° C, step 4 is obtained, freezing 24h～26h, and then be-45 ° of C～-55 ° C lyophilize 24h～26h in temperature namely obtains the nano wood quality; Particle diameter described in step 3 is (1g～3g): 100mL less than the volume ratio of the quality of the alkali lignin of 0.2mm and deionized water.
2. the preparation method of a kind of particle diameter controllable nano xylogen according to claim 1, it is characterized in that the alkali extraction and acid precipitation method specific operation process described in step 1 is as follows: at first alkali lignin is dissolved in the NaOH solution that concentration is 0.5mol/L～1.5mol/L, then carry out centrifugation, obtain supernatant liquor, to adopt massfraction under the water bath with thermostatic control of 55 ° of C～65 ° C of temperature be 12% aqueous hydrochloric acid transfers to the pH value of supernatant liquor till 6～7, and then carry out centrifugation, obtain the brown precipitation, adopt deionized water wash brown precipitation, wash be neutrality to the pH value of filtrate till, then be under 40 ° of C～5O ° of C, the precipitation after washing to be carried out drying in temperature, dry 20h～28h, namely obtain refining alkali lignin, the quality of described alkali lignin and concentration are that the volume ratio of the NaOH solution of 0.5mol/L～1.5mol/L is 1g: (5mL～7mL).
3. the preparation method of a kind of particle diameter controllable nano xylogen according to claim 1 and 2, is characterized in that the refining alkali lignin that in step 2, step 1 is obtained carries out crossing 100 mesh sieves after milled processed.
4. the preparation method of a kind of particle diameter controllable nano xylogen according to claim 1 and 2 is characterized in that the supersound process specific operation process described in step 3 is as follows: in ultrasonic frequency during to be the particle diameter that step 2 obtained under auxiliary of the ultrasonic wave of 40Hz～50Hz be scattered in deionized water less than the alkali lignin of 0.2mm.
5. the preparation method of a kind of particle diameter controllable nano xylogen according to claim 1 and 2, is characterized in that circulating 2 times under 1000bar in step 4.
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| 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 |
| CN105803017A (en) * | 2016-04-14 | 2016-07-27 | 南京林业大学 | Method for improving wood fiber material enzyme hydrolysis saccharification efficiency |
| CN107428946A (en) * | 2015-04-02 | 2017-12-01 | 斯道拉恩索公司 | Activated wooden promotor composition, for its manufacture method with and application thereof |
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| 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 |
| CN105803017B (en) * | 2016-04-14 | 2020-07-07 | 南京林业大学 | Method for improving enzymatic hydrolysis saccharification efficiency of wood fiber raw material |
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Application publication date: 20130612 |