CN107129600A - Nano micro crystal cellulose/phyllosilicate hybrid and preparation method thereof - Google Patents
Nano micro crystal cellulose/phyllosilicate hybrid and preparation method thereof Download PDFInfo
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- CN107129600A CN107129600A CN201710385231.2A CN201710385231A CN107129600A CN 107129600 A CN107129600 A CN 107129600A CN 201710385231 A CN201710385231 A CN 201710385231A CN 107129600 A CN107129600 A CN 107129600A
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- phyllosilicate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/346—Clay
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
- C08B15/02—Oxycellulose; Hydrocellulose; Cellulosehydrate, e.g. microcrystalline cellulose
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
- C08B15/05—Derivatives containing elements other than carbon, hydrogen, oxygen, halogens or sulfur
- C08B15/06—Derivatives containing elements other than carbon, hydrogen, oxygen, halogens or sulfur containing nitrogen, e.g. carbamates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
Abstract
The invention discloses nano micro crystal cellulose/phyllosilicate hybrid and preparation method thereof.The preparation method prepares nano micro crystal cellulose first with sulphuric acid hydrolysis, it is dispersed in basification in diluent, catalyst, cationic etherifying agent is subsequently added, fiber is well mixed and is reacted under base catalyst with etherifying agent, cationic cellulose dispersion liquid is made；Different types of phyllosilicate is mixed with the dispersion liquid of cation nanometer microcrystalline cellulose, intercalation is carried out, the nano hybridization body of nano micro crystal cellulose/phyllosilicate is finally made.The phyllosilicate that the present invention is used is cheap and easy to get, and the preparation of the nano micro crystal cellulose organic inorganic hybridization body prepared suitable for all kinds of natural plant fibres, the heat endurance of nano-cellulose can not only be effectively improved by hydridization, the intercalation of phyllosilicate can also be realized, and then makes one-dimensional, two-dimensional nano filler hydridization that hybrid coexists into multidimensional.
Description
Technical field
The present invention relates to nano micro crystal cellulose, more particularly to a kind of nano micro crystal cellulose/phyllosilicate hydridization
Body and preparation method thereof, belongs to field of nanometer material technology.
Background technology
Nano micro crystal cellulose comes from natural polymerses, with cost is low, intensity is high, light, economical, environmentally friendly etc.
Feature, its theoretical Young's modulus is 250GPa, and specific tensile strength is 5200kNm/kg, is 18 times of Titanium, and with spy
Different physics and optical property, due to its special performance, the research of nano micro crystal cellulose receives much concern in recent years.Nano microcrystalline
Cellulose is widely used in composite, papermaking, food, medicine and other fields, and nano micro crystal cellulose is used for as reinforcement
It is one of most important application field that nano composite material is prepared in high polymer material.Compared with protofibre element, due to separation
The influence of process, the heat endurance of nano micro crystal cellulose is poor, for high polymer material injection moulding, twin-screw extrusion etc.
Degraded blackening phenomena easily occurs for melt-processed process (generally more than 200 DEG C), it is impossible to play reinforcing effect.Therefore by improving it
Heat endurance, is expected to make nano micro crystal cellulose turn into a kind of environmental type reinforcing material and be used in high polymer material.
Improve nano-cellulose heat endurance at present is concentrated mainly on following 2 aspects：(1) extraction process is improved, is subtracted
The introducing of few sulfonic acid group, such as replaces sulphuric acid hydrolysis fibrous raw material, or reaction to be used after terminating in sodium hydroxide with hydrochloric acid, phosphoric acid
With, although the thermally-stabilised of nano-cellulose is increased made from this method, but surface charge is reduced, and is easily reunited, and is disperseed
Property is poor.(2) nano-cellulose surface is modified, and the hydroxyl on nano micro crystal cellulose surface such as is substituted by into acetyl group or other resistance to
Hot radical group, it is thermally-stabilised that nano-cellulose surface can effectively improve its by means such as in-situ preparation coated high molecular polymer
Property, but improvement is still limited.
The content of the invention
Patent of the present invention provides a kind of nano micro crystal cellulose/phyllosilicate hybrid and preparation method thereof, can have
Imitate and overcome the problem of nano micro crystal cellulose heat endurance is poor, and obtain the nanometer of the more excellent organic inorganic hybridization of performance and fill out
Material.
The purpose of the present invention is achieved through the following technical solutions：
A kind of preparation method of nano micro crystal cellulose/phyllosilicate hybrid, comprises the following steps and process conditions：
(1) sulphuric acid hydrolysis cellulosic material is utilized, nano micro crystal cellulose is prepared, is freeze-dried into standby after powder；
(2) in terms of mass fraction, 1 part of nano micro crystal cellulose is added to 5~30 parts of deionized waters and 10~20 parts dilute
Release and be uniformly dispersed in agent mixed liquor, add the base catalyst that consumption is nano micro crystal cellulose absolute dry mass 5~20%, 25~50
1~3h of basification at DEG C；
(3) step (2) products therefrom is warming up to 30~100 DEG C, addition consumption be nano micro crystal cellulose quality 10%~
60% cationic etherifying agent, is mixed evenly, and is etherified 3~5h, regulation pH is neutral after reaction terminates, and is obtained after centrifuge washing
Must be cationized the dispersion liquid of nano micro crystal cellulose；The cationic etherifying agent is pressed for epoxypropyl trimethylammonium chloride, chlorine third
Base trimethyl ammonia chloride is pressed, dimethyl diallyl chlorination is pressed and at least one of (the chloro- 2- hydroxypropyls of 3-) trimethyl ammonium chloride；
(4) be ultrasonically treated 30 under the conditions of 3~12 in pH by dispersion liquid obtained by phyllosilicate and step (3)~
100min, is well mixed, and it is 0.5~5%, cation nanometer cellulose to prepare and obtain the mass percent concentration of phyllosilicate
Mass percent concentration is 10~24h of magnetic agitation at 1~5%, 50~90 DEG C, by mixed liquor centrifuge washing to neutrality, is dried,
Grinding, obtains the organosilicon/inorganic nano-hybrid body of nano-cellulose intercalated montmorillonite.
Cellulosic material described in step (1) is at least one in stalk, wood powder, bamboo powder, bagasse powder what microcrystalline cellulose
Kind.
Diluent described in step (2) is at least one of isopropanol, ethanol and acetone.
Base catalyst described in step (3) is sodium hydroxide or potassium hydroxide.
Regulation pH is that neutrality is adjusted with watery hydrochloric acid after reaction described in step (3) terminates.
The temperature of step (4) described drying is 50~80 DEG C.
Phyllosilicate used is sodium base or calcium-base montmorillonite in step (4).
The number of material is weight in upper method, and the purity of chemical reagent and raw material used is that analysis is pure.
A kind of nano micro crystal cellulose/phyllosilicate hybrid, is made by above-mentioned preparation method.
Relative to prior art, the present invention has the advantages that：
1) nano micro crystal cellulose of the present invention is intercalation into the piece interlayer of montmorillonite, can due to montmorillonite layer iris action
To improve nano micro crystal cellulose/phyllosilicate hybrid heat endurance by a relatively large margin；
2) after nano-cellulose cationization of the present invention, the compatibility with high polymer material, also, surface hydroxyl can be increased
Radix mesh is reduced, and can reduce reunion；
3) multidimensional can be formed between nano-cellulose of the present invention and montmorillonite and hybrid coexists, both possess organic and inorganic
Nano filling features, have the property that hydridization coexists in multidimensional concurrently again；It is thermally-stabilised in being processed applied to melt polymer material
Property and mechanical performance are more excellent.
Brief description of the drawings
Fig. 1 is the nano micro crystal cellulose, the thermogravimetric curve figure of hybrid that prepare in embodiment 1.
Fig. 2 is the X-ray spectrogram of the montmorillonite of embodiment 1 and hybrid.
Fig. 3 is that mass fraction prepared by embodiment 4 is that 1% nano micro crystal cellulose, sodium-based montmorillonite, hybrid etc. suspend
Dispersity figure of the liquid after static 5 days.
Fig. 4 is that the hybrid of the gained of embodiment 1 is added to the obtained product of ABS resin and ABS resin and nano-cellulose
Add the photo of ABS resin resulting product sum.
Embodiment
To more fully understand the present invention, the present invention is further illustrated with reference to the accompanying drawings and examples, but this hair
Bright embodiment is not limited so.
Embodiment 1：
Cotton stalk is hydrolyzed with the concentrated sulfuric acid, cotton stalk nano microcrystalline cellulose is obtained, nano microcrystalline is obtained after freeze-drying fine
The plain powder of dimension.
In terms of mass fraction, the cotton stalk nano microcrystalline cellulose of 1.5 parts of sulphuric acid hydrolysis is dispersed in 10 parts of deionized waters
In 15 parts of alcohol mixeding liquids, it is well mixed, then adds ultrasonic agitation reaction 1.5h at 0.1 part, 30 DEG C of potassium hydroxide, prepare
Go out fluffy alkalization nano-cellulose；
In terms of mass fraction, (the chloro- 2- hydroxypropyls of 3-) trimethyl ammonia chloride ammonium salt solution 0.5 that mass fraction is 65% is added
Part, etherification reaction 3h at 50 DEG C prepares cationic nano micro crystal cellulose dispersion liquid.
In PH it is ultrasonically treated 50min under the conditions of 8 by sodium-based montmorillonite and gained dispersion liquid, is well mixed, preparation is obtained
The mass percent concentration of phyllosilicate is 3%, and cation nanometer cellulose mass percent concentration is 2%, is then placed in
Magnetic agitation 24h in 50 DEG C of oil bath, reaction terminates to dry after mixed liquor centrifuge washing to neutrality, and finally obtained cation is received
The hybrid of rice microcrystalline cellulose intercalation sodium-based montmorillonite.
Because nano micro crystal cellulose is intercalation into the piece interlayer of montmorillonite, montmorillonite layer serves iris action, can be with
Improve the heat endurance of cellulose.Fig. 1 is the nano micro crystal cellulose, the thermogravimetric curve figure of hybrid that prepare in the present embodiment
(method of testing：The thermal weight loss behavior of nano-cellulose, hybrid is measured using thermogravimetric analyzer, test condition is：Nitrogen
Gas shielded, 10 DEG C/min of heating rate, temperature range：30-600 DEG C), table 1 loses for the heat of rear nano micro crystal cellulose before modified
Tuple evidence, from Fig. 1 and table 1 as can be seen that compared with pure nano micro crystal cellulose, nano-cellulose/montmorillonite hybrid
Starting weightless temperature be greatly improved：The temperature of wherein weightlessness 5% brings up to 280 DEG C, the temperature of weightlessness 10% from 211 DEG C
Degree brings up to 306 DEG C from 246 DEG C, and maximum weightless temperature brings up to 324 DEG C from 316 DEG C, and the heat endurance of modified cellulose is obtained
Significantly improve.
Table 1
Fig. 2 is the X-ray spectrogram of montmorillonite and hybrid, as shown in Figure 2, montmorillonite, hybrid characteristic diffraction peak it is strong
2 θ are spent respectively at 6.92 °, 6.23 °, and interlamellar spacing, wherein λ correspondences are calculated according to Bragg equation λ=2dsin θ (λ=0.154)
In the wavelength of X-ray, d is interlamellar spacing, is computed understanding, the interlamellar spacing of pure montmorillonite is 1.27nm, the interlamellar spacing of hybrid
It is changed into 1.42nm, interlamellar spacing increase shows that the cellulose of cationization is inserted into montmorillonite layer, lamellar structure is softened, covered
De- soil lamella serves iris action, so as to improve the heat endurance of cellulose.
Fig. 3 is that mass fraction manufactured in the present embodiment is that 1% nano micro crystal cellulose, sodium-based montmorillonite, hybrid etc. hang
Dispersity of the supernatant liquid after static 5 days, from figure 3, it can be seen that cation nanometer cellulose is conducive to cellulose and montmorillonite
Effect, the metal cation between commutative cheating engaging layer, the montmorillonite hybrid material energy that this cationized cellulose is modified
It is stably dispersed in the aqueous solution.
The present invention realizes the intercalation modifying of phyllosilicate, and then makes one-dimensional, two-dimensional nano filler hydridization common into multidimensional
Hybrid is deposited, and with collaboration peptizaiton, more excellent performance is played in Polymer moulding.By the present embodiment institute
The hybrid obtained is added in ABS resin, and the composite materials property obtained by melting extrusion is as shown in table 2, wherein fine
The mass fraction of dimension element and hybrid is 2%, from Table 2, it can be seen that compared with the system for being directly added into cellulose, hydridization
Body can be such that the mechanical property of ABS material further improves；Product is obtained using melt-processed, from products appearance it can be seen that (figure
4) modified ABS plastic color change, is strengthened less by hybrid, heat endurance is kept.
Table 2
| Sample | Tensile strength/MPa | Bending strength/MPa | Bending modulus/MPa | Impact strength/KJ/m2 |
| ABS | 30.2 | 60.4 | 2010 | 19.72 |
| ABS/ celluloses | 33.1 | 62.6 | 2121 | 9.71 |
| ABS/ hybrids | 34.5 | 64.3 | 2223 | 15.66 |
Nano micro crystal cellulose/phyllosilicate hybrid performance obtained by example below is substantially similar to embodiment, no
Illustrate one by one.
Embodiment 2：
Bagasse powder is hydrolyzed with the concentrated sulfuric acid, nano micro crystal cellulose powder is obtained after freeze-drying.
In terms of mass fraction, 1 part of nano micro crystal cellulose is dispersed in 5 parts of deionized waters and 15 parts of aqueous isopropanols,
0.15 part of sodium hydroxide is added, at room temperature ultrasonically treated 1h；
In terms of mass fraction, the epoxypropyl trimethylammonium chloride for adding 65wt% presses 0.6 part of the aqueous solution, 45 DEG C of water bath conditions
Lower reaction 5h, obtains the nano-cellulose dispersion liquid that is cationized；
In PH it is ultrasonically treated 80min under the conditions of 10 by sodium-based montmorillonite and gained dispersion liquid, is well mixed, preparation is obtained
The mass percent concentration of phyllosilicate is 1%, and cation nanometer cellulose mass percent concentration is 1%, is then placed in
Magnetic agitation 24h in 50 DEG C of oil bath, reaction terminates to dry after mixed liquor centrifuge washing to neutrality, and finally obtained cation is received
The hybrid of rice microcrystalline cellulose intercalation sodium-based montmorillonite.
Embodiment 3：
Wood powder is hydrolyzed with the concentrated sulfuric acid, nano micro crystal cellulose powder is obtained after freeze-drying.
In terms of mass fraction, the mixing that 1 part of nano micro crystal cellulose is dispersed in into 20 parts of deionized waters and 10 parts of ethanol is molten
In liquid, 0.15 part of sodium hydroxide is added, at room temperature ultrasonically treated 2h；
In terms of mass fraction, 40wt% (the chloro- 2- hydroxypropyls of 3-) 0.6 part, 45 DEG C of trimethyl ammonia chloride aqueous ammonium is added
5h is reacted under water bath condition, the nano-cellulose dispersion liquid that is cationized is obtained；
In PH it is ultrasonically treated 50min under the conditions of 5 by calcium-base montmorillonite and gained dispersion liquid, is well mixed, preparation is obtained
The mass percent concentration of phyllosilicate is 1%, and cation nanometer cellulose mass percent concentration is 1%, is then placed in
Magnetic agitation 24h in 50 DEG C of oil bath, reaction terminates to dry after mixed liquor centrifuge washing to neutrality, and finally obtained cation is received
The hybrid of rice microcrystalline cellulose intercalation calcium-base montmorillonite.
Embodiment 4：
Use and nano micro crystal cellulose powder is obtained after concentrated sulfuric acid hydrolyzing microcrystalline cellulose, freeze-drying.
In terms of mass fraction, 1 part of nano micro crystal cellulose is dispersed in 20 parts of deionized waters and 15 parts of acetone solns, plus
Enter 0.15 part of potassium hydroxide, at room temperature ultrasonically treated 2h；
Addition 60wt% dimethyl diallyl chlorination is pressed reacts 5h under 0.4 part of the aqueous solution, 45 DEG C of water bath conditions, obtains
Be cationized nano-cellulose dispersion liquid；
In PH it is ultrasonically treated 50min under the conditions of 5 by sodium-based montmorillonite and gained dispersion liquid, is well mixed, preparation is obtained
The mass percent concentration of phyllosilicate is 1%, and cation nanometer cellulose mass percent concentration is 1%, is then placed in
Magnetic agitation 24h in 50 DEG C of oil bath, reaction end obtains nano micro crystal cellulose/montmorillonite hybrid mixed liquor.Will mixing
Dried after liquid centrifuge washing to neutrality, the hybrid of final obtained cation nanometer microcrystalline cellulose intercalation sodium-based montmorillonite.
Claims (9)
1. the preparation method of nano micro crystal cellulose/phyllosilicate hybrid, it is characterised in that comprise the following steps and technique
Condition：
(1) sulphuric acid hydrolysis cellulosic material is utilized, nano micro crystal cellulose is prepared, is freeze-dried into standby after powder；
(2) in terms of mass fraction, 1 part of nano micro crystal cellulose is added to 5~30 parts of deionized waters and 10~20 parts of diluents
It is uniformly dispersed, is added at the base catalyst that consumption is nano micro crystal cellulose absolute dry mass 5~20%, 25~50 DEG C in mixed liquor
1~3h of basification；
(3) step (2) products therefrom is warming up to 30~100 DEG C, and addition consumption is nano micro crystal cellulose quality 10%~60%
Cationic etherifying agent, be mixed evenly, be etherified 3~5h, regulation pH is neutrality after reaction terminates, and sun is obtained after centrifuge washing
Ionize the dispersion liquid of nano micro crystal cellulose；The cationic etherifying agent is pressed for epoxypropyl trimethylammonium chloride, chloropropyl three
Methyl chloride is pressed, dimethyl diallyl chlorination is pressed and at least one of (the chloro- 2- hydroxypropyls of 3-) trimethyl ammonium chloride；
(4) it is ultrasonically treated 30~100min under the conditions of 3~12 in pH by dispersion liquid obtained by phyllosilicate and step (3), mixes
Close uniform, it is 0.5~5%, cation nanometer cellulose quality percentage to prepare and obtain the mass percent concentration of phyllosilicate
Specific concentration is 10~24h of magnetic agitation at 1~5%, 50~90 DEG C, by mixed liquor centrifuge washing to neutrality, is dried, and grinding is obtained
To the organosilicon/inorganic nano-hybrid body of nano-cellulose intercalated montmorillonite.
2. the preparation method of nano micro crystal cellulose according to claim 1/phyllosilicate hybrid, its feature exists
In：Cellulosic material described in step (1) is at least one of stalk, wood powder, bamboo powder, bagasse powder what microcrystalline cellulose.
3. the preparation method of nano micro crystal cellulose according to claim 1/phyllosilicate hybrid, its feature exists
In：Diluent described in step (2) is at least one of isopropanol, ethanol and acetone.
4. the preparation method of nano micro crystal cellulose according to claim 1/phyllosilicate hybrid, its feature exists
In：Base catalyst described in step (3) is sodium hydroxide or potassium hydroxide.
5. the preparation method of nano micro crystal cellulose according to claim 1/phyllosilicate hybrid, its feature exists
In：Regulation pH is that neutrality is adjusted with watery hydrochloric acid after reaction described in step (3) terminates.
6. the preparation method of nano micro crystal cellulose according to claim 1/phyllosilicate hybrid, its feature exists
In：The temperature of step (4) described drying is 50~80 DEG C.
7. the preparation method of nano micro crystal cellulose according to claim 1/phyllosilicate hybrid, its feature exists
In：Phyllosilicate used is sodium base or calcium-base montmorillonite in step (4).
8. the preparation method of nano micro crystal cellulose according to claim 1/phyllosilicate hybrid, its feature exists
In：The purity of chemical reagent and raw material used is that analysis is pure.
9. a kind of nano micro crystal cellulose/phyllosilicate hybrid, it is characterised in that it is as described in claim any one of 1-8
Preparation method is made.
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| CN112457721A (en) * | 2020-12-03 | 2021-03-09 | 上海瑞君电泳涂料有限公司 | Color paste for epoxy electrophoretic coating, electrophoretic coating and preparation process thereof |
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Cited By (6)
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| WO2019053602A1 (en) * | 2017-09-13 | 2019-03-21 | Pirelli Tyre S.P.A. | Tyre for vehicle wheels comprising a composite reinforcing filler |
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| CN112457721B (en) * | 2020-12-03 | 2023-02-03 | 上海瑞君电泳涂料有限公司 | Color paste for epoxy electrophoretic coating, electrophoretic coating and preparation process thereof |
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Application publication date: 20170905 |