CN108752485A - A kind of preparation method of the cationization nano-cellulose containing lignin - Google Patents
A kind of preparation method of the cationization nano-cellulose containing lignin Download PDFInfo
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Abstract
The preparation method for the cationization nano-cellulose that the present invention relates to a kind of containing lignin, belongs to cellulose modified technical field.It is mixed with aqueous slkali, cationic etherifying agent after agricultural wastes are crushed, is reacted using microwave and ultrasonic wave combination one kettle way and by cellulose nanosizing, i.e. one kettle way prepares the cation nanometer cellulose containing lignin.Preparation process of the present invention is simple, reduces reaction temperature, saves the reaction time, and industrialization possibility is high.The cationization nano-cellulose containing lignin has the advantages that stability is good, film strength is high, antibiotic property is good obtained by simultaneously, and good effect can be obtained by using it for the absorption of heavy metal ion in water.Therefore, the cation nanometer cellulose that prepared by this method has great application value in the fields such as antibacterial and absorption.
Description
Technical field
The preparation method for the cationization nano-cellulose that the present invention relates to a kind of containing lignin, belongs to cellulose modified
Technical field.
Background technology
Nano-cellulose is that native cellulose is obtained by nanotechnology treatments, has nanoscale, higher compares table
The advantages that area and excellent stability.Therefore, nano-cellulose is in necks such as packaging, biological medicine, photoelectric technology, water process
Domain is widely used (Nanoscale.2017,9 (39):14758-14781；Nanoscale.2016,8(27):
13131-13154；Environ Sci:Nano.2014,1(4):302-316).
The preparation method of nano-cellulose mainly has acid-hydrolysis method, TEMPO catalytic oxidations, Mechanical Method etc. at present
(Progress in Chemistry.2017,30(4):448-462).Preparation for the nano-cellulose of cationization is led to
It is often cellulose is quaternized, the cellulose being cationized by more than cationic etherifying agent and fibrin reaction 8h, then leads to
It crosses high pressure homogenization method and reduces its size, the nano-cellulose being cationized with two-step pretreatment.Application number
It is disclosed in 201310585231.9 and fibrous raw material is subjected to mashing processing first, added cationic etherifying agent and cation is made
Cellulose, subsequent nanosizing processing is to be made cation nanometer cellulose.Application No. is disclosed in 201110058981.1
Method a kind of first to prepare nano-cellulose, then that cation modifying is carried out to nano-cellulose by adding KOH and etherifying agent,
And obtained cation nanometer cellulose to be used to improve the intensity and gas permeability of cigarette paper.Application No. is 201710373719.3
In disclose and be modified nano-cellulose sample by cation quaternary ammonium salt, the method for obtaining cationization nano-cellulose.
Therefore, method disclosed in above-mentioned patent and documents and materials is two-step method, i.e., first prepares cationization fiber
Element prepares cation nanometer cellulose using nanosizing, or first prepares nano-cellulose, using cationization prepare sun from
Sub- nano-cellulose.Meanwhile these methods, with softwood, broadleaf and grass fiber etc. for raw material, these are traditional
Fibrous raw material have some limitations, and cost is higher.In recent years, the energy of agriculture waste biomass and materialized
Using increasingly being paid close attention to by scientist or even masses.Especially China is large agricultural country, the agricultures such as all kinds of stalks generated every year
Industry abandoned biomass is more than 900,000,000 tons, wherein about 30% returning to the field, 20% to 30% is used as life in the countryside fuel, and 10% to 15% makees
For raw materials of industry such as feed or papermaking, remaining is wasted in the fields.This not only causes a large amount of wastes of resource, also results in ring
The problems such as border is polluted (for example, crop straw burning).
In addition, with the development of microwave-ultrasonic joint technology, obtained extensively in fields such as chemical reaction, extractions
Application.But using it for preparing modified nanometer cellulose is rarely reported.
Invention content
It is an object of the invention to propose a kind of preparation method of the cationization nano-cellulose containing lignin.
To achieve the above object, the invention adopts a technical scheme as：
It is a kind of containing lignin cationization nano-cellulose preparation method, after agricultural wastes are crushed with alkali soluble
Liquid, cationic etherifying agent mixing, using microwave and ultrasonic wave combination one kettle way is reacted and cellulose nanosizing, i.e.,
One kettle way prepares the cation nanometer cellulose containing lignin.
Further, agricultural wastes powder, cationic etherifying agent and the alkali after crushing are mixed to join organic molten
In agent, then reaction and nanosizing in ultrasonic microwave chemical reactor, are filtered after reaction, and precipitation is the sun containing lignin
Ion nano-cellulose.
Liquids recovery is applied mechanically obtained by the filtering.
It is described that agricultural wastes powder, cationic etherifying agent and alkali after crushing are mixed to join in organic solvent, it is organic
The dosage of solvent is 10-300 times of agricultural wastes powder quality, and cationic etherifying agent dosage is agricultural wastes powder quality
0.5-20 times, base amount be agricultural wastes powder quality 0.2%-5%.
It is preferred that the cationic etherifying agent dosage is 1-10 times of agricultural wastes powder quality, base amount is preferably agriculture
The 0.5%-3% of industry waste powder quality, the dosage of organic solvent are preferably 20-200 times of agricultural wastes powder quality.
It is described that reaction solution is added in ultrasonic microwave chemical reactor, microwave frequency 500MHz-2450MHz/10W-
1000W, ultrasonic frequency 10KHz-40KHz/50W, reaction temperature are 30 DEG C -70 DEG C, reaction time 30min-6h.
It is preferred that the ultrasonic microwave reaction condition is microwave frequency 2000MHz-2400MHz/1000W, ultrasonic frequency
30KHz-40KHz/50W, reaction temperature are 40 DEG C -70 DEG C, react 1h-5h.
It is therein that the agricultural wastes refer to bracteal leaf of corn, corncob, tobacco rod, Chinese alpine rush, maize straw, straw, bagasse
It is one or more of；
The cationic etherifying agent be 2,3- epoxypropyltrimethylchloride chlorides, 3- chloro-2-hydroxypropyl-trimethyl ammonium chlorides,
Cetyl trimethylammonium bromide, Cetyltrimethylammonium bromide, hexadecylpyridinium chloride, tetradecyltrimethylammonium bromination
Ammonium, dodecyl pyridinium chloride are one such or several；It is preferred that the cationic etherifying agent is 2,3- glycidyl front threes
Ammonium chloride, 3- chloro-2-hydroxypropyl-trimethyl ammonium chlorides, cetyl trimethylammonium bromide, Cetyltrimethylammonium bromide
It is one such or several；
The organic solvent is DMAC, DMF, DMSO, NMP, NH4One or more of SCN, NMMO；
It is preferred that the organic solvent is one or more of DMAC, DMF, DMSO.
The alkali refers to one or both of NaOH, KOH.
The present invention is had the following advantages：
(1) raw material that the present invention uses is agriculture waste biomass, this is not only the recycling profit of a large amount of agricultural wastes
It is to tally with the national condition the problems such as effectively avoiding environmental pollution caused by burning or shelving and take up an area with new approaches are provided
The processing method of agriculture waste biomass (refer to what the Ministry of Agriculture printed and distributed《About propulsion agricultural wastes recycling pilot
Scheme》).
(2) present invention involves microwave combination by means of ultrasound and prepares cation nanometer cellulose, and the superposition of two kinds of energy can
Rapidly to destroy the Hydrogenbond of cellulose, reduce the size of cellulose.Meanwhile after microwave and ultrasonic wave auxiliary, reaction
System heating is very fast and uniform, promotes the progress of quaternization reaction.Therefore, the present invention can be substantially reduced reaction temperature, section
The reaction time is saved, realizes the production of high-efficiency cleaning metaplasia.
(3) in addition, preparation method of the present invention prepares cation nanometer cellulose using microwave and ultrasonic wave auxiliary one kettle way,
This method directly obtains cation-modified from agricultural wastes simple and easy to get without the separation of intermediate (cellulose)
Nano-cellulose.The present invention greatly simplifies preparation process (we compared with the preparation method (two-step method) having disclosed
Method is without complicated separating, washing process and delignification's process), low for equipment requirements, economic performance is high, is easy to scale metaplasia
It produces and environmentally friendly, is a kind of preparation method of green.Meanwhile the nano-cellulose containing lignin obtained after reaction is wet
Intensity is higher and has preferable water resistance, has great application potential in wet environment after film forming, effectively realizes agriculture
The high-valued application of industry abandoned biomass.
Description of the drawings
Fig. 1 is the TEM figures that the present invention is the cation nanometer cellulose prepared by raw material of tobacco rod that example provides.
Fig. 2 is that the present invention is the cation nanometer cellulose film forming pictorial diagram prepared by raw material of tobacco rod that example provides.
Fig. 3 is the TEM figures that the present invention is the cation nanometer cellulose prepared by raw material of bracteal leaf of corn that example provides.
Fig. 4 is that the present invention is the pictorial diagram that forms a film by base cationic nano-cellulose of bracteal leaf of corn that example provides.
Fig. 5 is that the present invention is the variation that the cation nanometer cellulose that example provides adsorbs magnesium ion front and back conductivity.
It is the cation nanometer cellulose that provides of example to solution after magnesium ion absorption 2min and 4min that Fig. 6, which is the present invention,
Variation.
Specific implementation mode
The feasibility of this method is further described below by way of specific implementation example, but is not intended that the invention be limited to
These examples.
The present invention mixes after first crushing agricultural wastes with aqueous slkali, cationic etherifying agent, utilizes microwave and ultrasound
Wave combined system promotes reaction to carry out, while can cellulose nanosizing, i.e. one kettle way be prepared the cation containing lignin and be received
Rice cellulose.Preparation process of the present invention is simple, while reducing reaction temperature, saves the reaction time, and industrialization possibility is high.Simultaneously
The acquired cationization nano-cellulose containing lignin has the advantages that stability is good, film strength is high, antibiotic property is good, by it
Absorption for heavy metal ion in water can obtain good effect.Therefore, the cation nanometer fiber that prepared by this method
Element has great application value in the fields such as antibacterial and absorption.
Embodiment 1
Cationization nano-cellulose is prepared by raw material of tobacco rod
It is crushed after tobacco rod is removed the peel, feedstock analysis is as shown in table 1.By tobacco rod powder, 2,3- epoxypropyl trimethylammonium chlorides
Ammonium, KOH mixing are added in DMAC, wherein 2,3- epoxypropyltrimethylchloride chloride dosages are 1 times of tobacco rod powder quality, KOH
Dosage is that 0.5%, the DMAC dosages of tobacco rod powder quality are 20 times of tobacco rod powder quality.Ultrasonic microwave is added in reaction solution
Microwave 2000MHz/1000W is arranged in chemical reactor, and ultrasonic frequency 30KHz/50W reacts 5h at 40 DEG C, by what is obtained
Liquid filters, and the filtrate recycling containing DMAC can be recycled, and filter residue is washed with deionized 5 times, you can be cationized
Nano-cellulose.
Verification 1
By TEM tests it can be seen that embodiment 1 has successfully obtained the nano-cellulose fibril (figure that diameter is about 50nm
1).It can be seen that in tobacco rod containing about 24.3% lignin (table 1) by the feedstock analysis of the tobacco rod powder in embodiment 1.
Due to there is no delignified process in this method, contain partial lignin in the nano-cellulose being prepared.It will be positive
The nano-cellulose of ionization can be prepared by nano-cellulose film by vacuum filtration, by TAPPI T497 and
TAPPIT456 standards carry out mechanical performance detection to it, as shown in table 2.From Table 2, it can be seen that passing through by raw material of tobacco rod
The nano-cellulose film of cationization prepared by one kettle way has higher dry strength (179.7MPa) and wet strength
(80.1MPa).Due to the effect of lignin, the color of film is brown, but with preferable transparent (Fig. 2).In addition, reference
GB/T 21510-2008 standards, the cation-modified nano-cellulose for being 0.6% in mass concentration containing 0.1g by microbionation
In common bacteria culture medium, the results show that above-mentioned cation-modified nano-cellulose to Escherichia coli killing rate be more than 99%, and
And 99% is more than to the killing rate of staphylococcus aureus.Therefore, it can be obtained at lower temperature (40 DEG C) by this method
To the nano-cellulose of cationization, and what is prepared forms a film not only by base cationic nano-cellulose of tobacco rod with higher
Dry strength and wet strength, while there is preferable antibiotic property.
Embodiment 2
Cationization nano-cellulose is prepared by raw material of bracteal leaf of corn
Bracteal leaf of corn is crushed, feedstock analysis is as shown in table 3.By bracteal leaf of corn powder, tetradecyltrimethylammonium bromination
Ammonium, KOH mixing are added in DMF, wherein tetradecyltrimethylammonium bromide dosage is 10 times of bracteal leaf of corn powder quality, KOH
Dosage is that 3%, the DMF dosages of bracteal leaf of corn powder quality are 200 times of bracteal leaf of corn powder quality.Ultrasound is added in reaction solution
Microwave 2400MHz/800W, ultrasonic frequency 40KHz/50W is arranged in wave microwave chemical reactor, and 1h is reacted at 40 DEG C, will
The liquid filtering arrived, the filtrate recycling containing DMF can be recycled, filter residue be washed with deionized 5 times, you can obtain cation
The nano-cellulose of change.
Verification 2
By TEM tests it can be seen that embodiment 2 has successfully obtained nano-cellulose fibril (figure of the diameter less than 40nm
3) it, can be seen that in tobacco rod containing about 11.6% lignin by the feedstock analysis of the bracteal leaf of corn powder in embodiment 2.
Due to there is no delignified process in this method, contain partial lignin in the nano-cellulose being prepared.It will be positive
The nano-cellulose of ionization can be prepared by nano-cellulose film by casting, and mechanical performance is as shown in table 4.From table 4
As can be seen that being done with higher using the nano-cellulose film that bracteal leaf of corn is the cationization that raw material is prepared by one kettle way
Intensity (152.1MPa) and wet strength (39.8MPa).Likewise, the color of film is since the effect of lignin is brown, but
With preferable transparent (Fig. 4).
The absorption of metal ion is used for using cation nanometer cellulose as adsorbent.Specific method is：Take 0.1g over dry
Cation nanometer cellulose, 100mL 2mg/mL MgSO are added4Solution, testing conductivity.Absorption is stirred at room temperature, inhales
The attached time is respectively 2min, 4min, 6min, 8min, 10min；10mL centrifugations are sampled, the conductivity of supernatant is tested.From test
As a result conductivity declines rapidly when (Figures 5 and 6) can be seen that the absorption of cation nanometer cellulose, can reach after about 4min
Balance.It can also be seen that apparent wadding coagulation drop occurs for cation nanometer cellulose from Fig. 6.Therefore, cation nanometer fiber
Element is preferable to magnesium ion adsorption effect.
Embodiment 3
Cationization nano-cellulose is prepared by raw material of Chinese alpine rush
Chinese alpine rush is crushed, feedstock analysis is as shown in table 5.Take the chloro- 2- Hydroxyproyl Trimethyls chlorination of Chinese alpine rush powder, 3-
Ammonium, NaOH mixing are added in DMSO, wherein 3- chloro-2-hydroxypropyl-trimethyl ammonium chloride dosages are the 5 of Chinese alpine rush powder quality
Times, NaOH dosages are that 1%, the DMSO dosages of Chinese alpine rush powder quality are 100 times of Chinese alpine rush powder quality.Reaction solution is added
Ultrasonic microwave chemical reactor, is arranged microwave 2300MHz/1000W, and ultrasonic frequency 35KHz/50W reacts at 65 DEG C
4h filters obtained liquid, and the filtrate recycling containing DMSO can be recycled, and filter residue is washed with deionized 5 times, you can
To the nano-cellulose for the cationization that diameter is about 40nm.
Embodiment 4
Cationization nano-cellulose is prepared by raw material of bagasse
Bagasse is crushed, feedstock analysis is as shown in table 6.Take bagasse, 2,3- epoxypropyltrimethylchloride chlorides, KOH mixing
It is added in DMSO, wherein 2,3- epoxypropyltrimethylchloride chloride dosages are 3 times of bagasse powder quality, and KOH dosages are bagasse
2%, the DMSO dosages of powder quality are 50 times of bagasse powder quality.Ultrasonic microwave chemical reactor is added in reaction solution,
Microwave 2400MHz/1000W is set, and ultrasonic frequency 40KHz/50W reacts 5h at 50 DEG C, and obtained liquid is filtered, is contained
The filtrate recycling of DMSO can be recycled, and filter residue is washed with deionized 5 times, you can obtain the cation that diameter is about 60nm
The nano-cellulose product of change, wherein content of lignin are about 16%, consistent with content of lignin in Bagasse Material.
Embodiment 5
Cationization nano-cellulose is prepared by raw material of straw
Straw is crushed, takes straw, dodecyl pyridinium chloride, NaOH mixing to be added in NMMO, wherein dodecyl
Pyridinium chloride dosage is 20 times of straw powder quality, and NaOH dosages are that 5%, the NMMO dosages of straw powder quality are straw
300 times of powder quality.Ultrasonic microwave chemical reactor is added in reaction solution, microwave 2450MHz/1000W, ultrasonic wave are set
Frequency 40KHz/50W reacts 4h at 60 DEG C, and obtained liquid is filtered, and the filtrate recycling containing NMMO can be recycled, and will filter
Slag is washed with deionized 5 times, you can obtains the nano-cellulose product for the cationization that diameter is about 30nm.
Embodiment 6
Using bracteal leaf of corn and straw mixture cationization nano-cellulose is prepared as raw material
It is 1 by mass ratio:1 bracteal leaf of corn and straw is crushed and is uniformly mixed, and takes bracteal leaf of corn and straw mixture, 2,
3 epoxypropyltrimethylchloride chlorides, NaOH mixing are added in DMF, wherein 2,3 epoxypropyltrimethylchloride chloride dosages are jade
10 times of rice bract and straw mixture quality, NaOH dosages are 3%, the DMF dosages of bracteal leaf of corn and straw mixture quality
For bracteal leaf of corn and 200 times of straw mixture quality.Ultrasonic microwave chemical reactor is added in reaction solution, microwave is set
2400MHz/900W, ultrasonic frequency 40KHz/50W react 5h at 70 DEG C, obtained liquid are filtered, the filtrate containing DMF
Recycling can be recycled, and filter residue is washed with deionized 5 times, you can obtain the nanometer of cationization of the diameter in 30-70nm
Cellulose products.
The feedstock analysis of tobacco rod in 1 embodiment 1 of table
| Extract (%) | Lignin (%) | Cellulose (%) | Hemicellulose (%) | Total (%) | |
| Tobacco rod | 12.60±1.08 | 24.30±0.2 | 40.47±0.6 | 16.51±0.10 | 93.87 |
Mechanical performance after cation nanometer cellulose film forming prepared by 2 embodiment 1 of table
The feedstock analysis of bracteal leaf of corn in 3 embodiment 2 of table
| Extract (%) | Lignin (%) | Cellulose (%) | Hemicellulose (%) | Total (%) | |
| Bracteal leaf of corn | 7.07±0.90 | 11.6±0.80 | 43.42±0.10 | 29.93±0.60 | 92.01 |
Mechanical performance after cation nanometer cellulose film forming prepared by 4 embodiment 2 of table
Table 5 is the feedstock analysis of Chinese alpine rush in embodiment 3
| Extract (%) | Lignin (%) | Cellulose (%) | Hemicellulose (%) | Total (%) | |
| Chinese alpine rush | 13.27±0.05 | 16.40±1.10 | 41.25±0.88 | 24.71±0.33 | 95.63 |
Table 6 is the feedstock analysis of bagasse in embodiment 4.
| Extract (%) | Lignin (%) | Cellulose (%) | Hemicellulose (%) | Total (%) | |
| Bagasse | 5.49±0.34 | 22.64±0.73 | 45.26±0.98 | 24.28±1.21 | 97.67 |
In summary example, the present invention is based on the preparation methods of the cationization nano-cellulose of agricultural wastes, not only
Reaction temperature can be reduced, shorten the reaction time, and cation can be directly obtained from fibrous raw material by one kettle way
Nano-cellulose greatly simplifies preparation process.Meanwhile the obtained cationization nano-cellulose containing lignin is not only
There is chelation with excellent fungistatic effect, higher film strength, and to underwater gold category ion.Therefore, it is this sun from
Sonization nano-cellulose has broad application prospects in the fields such as antibacterial and wastewater treatment.
Claims (9)
1. a kind of preparation method of the cationization nano-cellulose containing lignin, it is characterised in that：Agricultural wastes are crushed
It mixes, is reacted using microwave and ultrasonic wave combination one kettle way and by cellulose with aqueous slkali, cationic etherifying agent afterwards
Nanosizing, i.e. one kettle way prepare the cation nanometer cellulose containing lignin.
2. the preparation method of the cationization nano-cellulose as described in claim 1 containing lignin, it is characterised in that：By powder
Agricultural wastes powder, cationic etherifying agent and alkali after broken are mixed to join in organic solvent, then in ultrasonic microwave
Reaction and nanosizing in reactor are learned, is filtered after reaction, precipitation is the cation nanometer cellulose containing lignin.
3. the preparation method of the cationization nano-cellulose as described in claim 1 containing lignin, it is characterised in that：It is described
Filtering gained liquids recovery is applied mechanically.
4. the preparation method of the cationization nano-cellulose as described in claim 1 or 2 containing lignin, it is characterised in that：
Agricultural wastes powder, cationic etherifying agent and alkali after crushing are mixed to join in organic solvent, the dosage of organic solvent is
10-300 times of agricultural wastes powder quality, cationic etherifying agent dosage are 0.5-20 times of agricultural wastes powder quality,
Base amount is the 0.2%-5% of agricultural wastes powder quality.
5. the preparation method of the cationization nano-cellulose as described in claim 4 containing lignin, it is characterised in that：It is described
Cationic etherifying agent dosage is 1-10 times of agricultural wastes powder quality, and base amount is agricultural wastes powder quality
0.5%-3%, the dosage of organic solvent are 20-200 times of agricultural wastes powder quality.
6. the preparation method of the cationization nano-cellulose as described in claim 1 or 2 containing lignin, it is characterised in that：
It is described that reaction solution is added in ultrasonic microwave chemical reactor, microwave frequency 500MHz-2450MHz/10W-1000W, ultrasound
Wave frequency rate 10KHz-40KHz/50W, reaction temperature are 30 DEG C -70 DEG C, reaction time 30min-6h.
7. the preparation method of the cationization nano-cellulose as described in claim 6 containing lignin, it is characterised in that：It is described
Ultrasonic microwave reaction condition be microwave frequency 2000MHz-2400MHz/1000W, ultrasonic frequency 30KHz-40KHz/50W,
Reaction temperature is 40 DEG C -70 DEG C, reacts 1h-5h.
8. the preparation method of the cationization nano-cellulose as described in claim 1 or 2 containing lignin, it is characterised in that：
It is one such or several that the agricultural wastes refer to bracteal leaf of corn, corncob, tobacco rod, Chinese alpine rush, maize straw, straw, bagasse
Kind；
The cationic etherifying agent is 2,3- epoxypropyltrimethylchloride chlorides, 3- chloro-2-hydroxypropyl-trimethyl ammonium chlorides, 16
Alkyl trimethyl ammonium bromide, Cetyltrimethylammonium bromide, hexadecylpyridinium chloride, tetradecyltrimethylammonium bromide,
Dodecyl pyridinium chloride is one such or several；
The organic solvent is DMAC, DMF, DMSO, NMP, NH4One or more of SCN, NMMO, the alkali refer to NaOH, KOH
One or both of.
9. the preparation method of the cationization nano-cellulose as described in claim 8 containing lignin, it is characterised in that：It is described
Cationic etherifying agent is 2,3- epoxypropyltrimethylchloride chlorides, 3- chloro-2-hydroxypropyl-trimethyl ammonium chlorides, cetyl front three
Base ammonium bromide, Cetyltrimethylammonium bromide are one such or several；
The organic solvent is one or more of DMAC, DMF, DMSO.
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| CN110257041B (en) * | 2019-06-26 | 2021-05-14 | 滨州学院 | Guar gum-nano cellulose fiber crosslinking thickener for fracturing fluid and preparation method thereof |
| CN111733600A (en) * | 2020-01-05 | 2020-10-02 | 天津科技大学 | Preparation method of tobacco-based cellulose nanofiber |
| CN114478809A (en) * | 2022-02-21 | 2022-05-13 | 浙江隆腾医用新材料有限公司 | Preparation method of carboxymethyl cellulose fiber |
| CN114478809B (en) * | 2022-02-21 | 2023-05-16 | 浙江隆腾医用新材料有限公司 | Preparation method of carboxymethyl cellulose fiber |
| CN114737200A (en) * | 2022-04-20 | 2022-07-12 | 国家纳米科学中心 | Dechlorination and corrosion inhibition method for iron object |
| CN114737200B (en) * | 2022-04-20 | 2024-05-28 | 国家纳米科学中心 | Dechlorination and corrosion inhibition method for iron articles |
| CN115672282A (en) * | 2022-10-13 | 2023-02-03 | 青岛科技大学 | Preparation method of simple and reproducible biogas residue-based anion adsorbent |
| CN115572111A (en) * | 2022-10-14 | 2023-01-06 | 中建商品混凝土（福建）有限公司 | Preparation method of modified nano-cellulose reinforced high-crack-resistance cement |
| CN115572111B (en) * | 2022-10-14 | 2023-11-03 | 中建商品混凝土（福建）有限公司 | Preparation method of modified nanocellulose reinforced high-crack-resistance cement |
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