CN109666269A - One kind is containing the modified polyadipate/butylene terephthalate composite material and preparation method of nano micro crystal cellulose - Google Patents
One kind is containing the modified polyadipate/butylene terephthalate composite material and preparation method of nano micro crystal cellulose Download PDFInfo
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- CN109666269A CN109666269A CN201710954396.7A CN201710954396A CN109666269A CN 109666269 A CN109666269 A CN 109666269A CN 201710954396 A CN201710954396 A CN 201710954396A CN 109666269 A CN109666269 A CN 109666269A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/06—Biodegradable
Abstract
The invention discloses one kind containing the modified polyadipate/butylene terephthalate composite material of nano micro crystal cellulose, component including following mass parts: 100 parts of polyadipate/butylene terephthalates and 1-20 parts of modified Nano microcrystalline celluloses, extruding pelletization after being blended by high speed；The modified Nano microcrystalline cellulose is prepared via a method which: nano micro crystal cellulose being mixed with dehydrated alcohol, ultrasonic disperse obtains nano micro crystal cellulose suspension；Coupling agent is dissolved in dehydrated alcohol and is made into coupling agent solution；The nano micro crystal cellulose suspension and coupling agent solution are mixed, 75-85 DEG C of reflux 2-4h；Be cooled to room temperature, be centrifuged, dry after obtain the modified Nano microcrystalline cellulose.The present invention through organically-modified, can be effectively reduced interfacial resistance, improve its compatibility with basis material, be able to satisfy polyadipate/butylene terephthalate modification demand by nano micro crystal cellulose.
Description
Technical field
The present invention relates to the field of polymer composite material of fully biodegradable, more particularly to one kind are fine containing nano microcrystalline
Modified polyadipate/butylene terephthalate the composite material and preparation method of dimension element.
Background technique
Polyadipate/butylene terephthalate has excellent processing performance, leads in industry, agricultural, household, packaging etc.
Domain has very broad application prospect.But single polyadipate/butylene terephthalate have tensile strength it is insufficient,
The disadvantages of at high cost, needs to improve its mechanical performance by modified and reduces cost.
Cellulose is a kind of polysaccharide that content is most in nature, accounts for 50% or more of plant kingdom's carbon content, is to prepare to receive
The primary raw material of rice microcrystalline cellulose.Cotton fiber, bamboo fibre, banana fiber, timber, sugarcane 2 etc. are all the abundant of cellulose
Source.Cotton is one of highest plant of content of cellulose, contained by cellulose it is soft, intensity is big, is that quality is best
Plant fiber.It can be used for producing cellulose esters, cellulose ether and nano micro crystal cellulose after diluted alkaline is handled；From bamboo
The bamboo fibre of extraction cannot be only used for papermaking, it can also be used to manufacture special fiber, and the Quanzhou City, Fujian Province in China is generation
Maximum bamboo fibre production base in boundary can provide a large amount of raw material for the preparation of bamboo fibre；Timber is not only paper industry
As long as raw material and cellulose chemistry industry valuable source.In addition to plant kingdom, bacterium, animal are also the important of cellulose
Source.Compared with plant cellulose, bacteria cellulose without the by-products such as lignin and hemicellulose, have higher molecular weight,
Crystallinity, hyperfine network structure and content of cellulose are had higher pure by the nano micro crystal cellulose that it is prepared
Degree.Since nano micro crystal cellulose has nanoscale reticular structure, nanometer size effect and high-specific surface area and strong mechanical performance,
It is set to possess superior mechanical performance, as reinforcement, mechanical performance and thermal stability to composite material etc. are had a significant impact,
And nano micro crystal cellulose will not produce bigger effect the characteristic of original material.It has biological decomposition characteristic simultaneously, this
Allow the reinforcing agent as polymeric substrates that it is more and more extensive.Since nano micro crystal cellulose not only has cellulose origin
Extensively, the advantages that nontoxic, biodegradable, also have large specific surface area, transparent, intensity is high, nanometer size effect, chemistry is facilitated to change
Property and the advantages such as functionalization, nano micro crystal cellulose in enhancing composite material, catalyst carrier, be separated by filtration, pharmaceutical carrier etc.
Field has a wide range of applications potentiality.
Therefore nano micro crystal cellulose is modified, and be introduced into polyadipate/butylene terephthalate system
The composite material containing nano micro crystal cellulose of developing renewable resources has considerable economic benefit and social value.It there is no at present
Nano micro crystal cellulose is applied to the report of degrading composite.
Summary of the invention
The object of the present invention is to provide one kind modified polyadipate/butylene terephthalate containing nano micro crystal cellulose is multiple
Condensation material and preparation method thereof, to solve drawbacks described above existing for background technique.
The present invention realizes by the following technical solutions: one kind is containing the modified polyadipate of nano micro crystal cellulose/right
Terephtha-late composite material, the component including following mass parts: 100 parts of polyadipate/butylene terephthalates and
1-20 parts of modified Nano microcrystalline celluloses, extruding pelletization after being blended by high speed；The modified Nano microcrystalline cellulose is by such as
The preparation of lower section method:
Step 1 mixes nano micro crystal cellulose with dehydrated alcohol, and ultrasonic disperse obtains nano micro crystal cellulose suspension；
Coupling agent is dissolved in dehydrated alcohol and is made into coupling agent solution by step 2；
Step 3 mixes the nano micro crystal cellulose suspension and coupling agent solution, 75-85 DEG C of reflux 2-4h；
Step 4 is cooled to room temperature, be centrifuged, dry after obtain the modified Nano microcrystalline cellulose.
The additive amount of the coupling agent is the 0.5-2% of nano micro crystal cellulose quality as a preferred technical solution,.
Silane coupling agent, such as gamma-aminopropyl-triethoxy silicon can be used in the coupling agent as a preferred technical solution,
Alkane coupling agent (KH550) or γ-glycidyl ether oxygen propyl trimethoxy silicane (KH560).
It is described containing the modified polyadipate/butylene terephthalate of nano micro crystal cellulose as a preferred technical solution,
Composite material further includes the component of following mass parts:
The lubricant is the mixing of one or both of zinc stearate or calcium stearate as a preferred technical solution,
Object.
The antioxidant was four (β-(3,5- three-level butyl -4- hydroxy phenyl) propionic acid) seasons as a preferred technical solution,
The mixture of one or both of Doutrate or bis- (3,5- three-level butyl -4- hydroxy phenyl) thioethers.
The heat stabilizer is one of maleic anhydride or epoxidized soybean oil or two as a preferred technical solution,
The mixture of kind.
The photosensitizer is one of aminodithioformic acid iron or ferric stearate or two as a preferred technical solution,
The mixture of kind.
As a preferred technical solution, the number-average molecular weight of the polyadipate/butylene terephthalate be 3.6 ×
104。
A second object of the present invention is to provide it is a kind of prepare it is above-mentioned containing the modified polyadipate of nano micro crystal cellulose/to benzene
The method of dioctyl phthalate fourth diester composite material specifically uses following steps:
The nano micro crystal cellulose is placed in high speed altogether by step 1 together with polyadipate/butylene terephthalate
It is mixed in mixed machine；
It is described micro- containing nanometer to be placed in extruding pelletization acquisition in double screw extruder by step 2 for above-mentioned uniformly mixed raw material
Crystalline cellulose is modified polyadipate/butylene terephthalate composite material.
It as a preferred technical solution, further include by the lubricant, antioxidant, heat stabilizer, photosensitizer in step 1
It is blended together with polyadipate/butylene terephthalate with the nano micro crystal cellulose.
As a preferred technical solution, further include following steps:
Step 3 will be modified polyadipate/terephthalic acid (TPA) fourth two containing nano micro crystal cellulose described in step 2 acquisition
Profile is made through injection molding in ester composite material.
The present invention through organically-modified, can be effectively reduced interfacial resistance, improve itself and matrix by nano micro crystal cellulose
The compatibility of material is able to satisfy polyadipate/butylene terephthalate modification demand.And the introducing of photosensitizer can also have
Effect shortens using the composite material as the degradation cycle of the disposable product of substrate.
Specific embodiment
The present invention is illustrated below by specific embodiment, but is not intended to limit the present invention.
Embodiment 1
One kind is containing the modified polyadipate/butylene terephthalate composite material of nano micro crystal cellulose and its preparation side
Method is calculated according to the mass fraction, and composition and content are as follows:
Above-mentioned formula is reacted according to the following steps:
(1) a certain amount of above-mentioned nano micro crystal cellulose is mixed with 50ml dehydrated alcohol, ultrasonic disperse 10min must disperse
Even suspension；By gamma-aminopropyl-triethoxy-silane coupling agent (KH550) (by nano micro crystal cellulose mass fraction
0.5% is added) it is dissolved in 50ml dehydrated alcohol；Unit for uniform suspension is uniformly mixed at 80 DEG C the 3-5h that flows back with coupling agent solution；
It is cooled to room temperature, is centrifuged, dried in 80 DEG C of vacuum drying ovens.Obtain coupling agent modified nano micro crystal cellulose；
(2) by above-mentioned modified Nano microcrystalline cellulose and polyadipate/butylene terephthalate, lubricant, antioxidant,
Heat stabilizer, photosensitizer together, are placed in high speed blender and are mixed；
(3) above-mentioned uniformly mixed raw material is placed in extruding pelletization in double screw extruder；
(4) standard testing batten is made through injection molding in above-mentioned composite particles, spare.
Embodiment 2
One kind is containing the modified polyadipate/butylene terephthalate composite material of nano micro crystal cellulose and its preparation side
Method is calculated according to the mass fraction, and composition and content are as follows:
Above-mentioned formula is reacted according to the following steps:
(1) a certain amount of above-mentioned nano micro crystal cellulose is mixed with 50ml dehydrated alcohol, ultrasonic disperse 10min must disperse
Even suspension；By gamma-aminopropyl-triethoxy-silane coupling agent (KH550) (by nano micro crystal cellulose mass fraction
0.5% is added) it is dissolved in 50ml dehydrated alcohol；Unit for uniform suspension is uniformly mixed at 80 DEG C the 3-5h that flows back with coupling agent solution；
It is cooled to room temperature, is centrifuged, dried in 80 DEG C of vacuum drying ovens.Obtain coupling agent modified nano micro crystal cellulose；
(2) by above-mentioned modified Nano microcrystalline cellulose and polyadipate/butylene terephthalate, lubricant, antioxidant,
Heat stabilizer, photosensitizer together, are placed in high speed blender and are mixed；
(3) above-mentioned uniformly mixed raw material is placed in extruding pelletization in double screw extruder；
(4) standard testing batten is made through injection molding in above-mentioned composite particles, spare.
Embodiment 3
One kind is containing the modified polyadipate/butylene terephthalate composite material of nano micro crystal cellulose and its preparation side
Method is calculated according to the mass fraction, and composition and content are as follows:
Above-mentioned formula is reacted according to the following steps:
(1) a certain amount of above-mentioned nano micro crystal cellulose is mixed with 50ml dehydrated alcohol, ultrasonic disperse 10min must disperse
Even suspension；By gamma-aminopropyl-triethoxy-silane coupling agent (KH550) (by nano micro crystal cellulose mass fraction
0.5% is added) it is dissolved in 50ml dehydrated alcohol；Unit for uniform suspension is uniformly mixed at 80 DEG C the 3-5h that flows back with coupling agent solution；
It is cooled to room temperature, is centrifuged, dried in 80 DEG C of vacuum drying ovens.Obtain coupling agent modified nano micro crystal cellulose；
(2) by above-mentioned modified Nano microcrystalline cellulose and polyadipate/butylene terephthalate, lubricant, antioxidant,
Heat stabilizer, photosensitizer together, are placed in high speed blender and are mixed；
(3) above-mentioned uniformly mixed raw material is placed in extruding pelletization in double screw extruder；
(4) standard testing batten is made through injection molding in above-mentioned composite particles, spare.
Embodiment 4
One kind is containing the modified polyadipate/butylene terephthalate composite material of nano micro crystal cellulose and its preparation side
Method is calculated according to the mass fraction, and composition and content are as follows:
Above-mentioned formula is reacted according to the following steps:
(1) a certain amount of above-mentioned nano micro crystal cellulose is mixed with 50ml dehydrated alcohol, ultrasonic disperse 10min must disperse
Even suspension；γ-glycidyl ether oxygen propyl trimethoxy silicane (KH560) (is pressed into nano micro crystal cellulose mass fraction
0.5% be added) be dissolved in 50ml dehydrated alcohol；Unit for uniform suspension is uniformly mixed at 80 DEG C the 3- that flows back with coupling agent solution
5h；It is cooled to room temperature, is centrifuged, dried in 80 DEG C of vacuum drying ovens.Obtain coupling agent modified nano micro crystal cellulose；
(2) by above-mentioned modified Nano microcrystalline cellulose and polyadipate/butylene terephthalate, lubricant, antioxidant,
Heat stabilizer, photosensitizer together, are placed in high speed blender and are mixed；
(3) above-mentioned uniformly mixed raw material is placed in extruding pelletization in double screw extruder；
(4) standard testing batten is made through injection molding in above-mentioned composite particles, spare.
Embodiment 5
One kind is containing the modified polyadipate/butylene terephthalate composite material of nano micro crystal cellulose and its preparation side
Method is calculated according to the mass fraction, and composition and content are as follows:
Above-mentioned formula is reacted according to the following steps:
(1) a certain amount of above-mentioned nano micro crystal cellulose is mixed with 50ml dehydrated alcohol, ultrasonic disperse 10min must disperse
Even suspension；γ-glycidyl ether oxygen propyl trimethoxy silicane (KH560) (is pressed into nano micro crystal cellulose mass fraction
0.5% be added) be dissolved in 50ml dehydrated alcohol；Unit for uniform suspension is uniformly mixed at 80 DEG C the 3- that flows back with coupling agent solution
5h；It is cooled to room temperature, is centrifuged, dried in 80 DEG C of vacuum drying ovens.Obtain coupling agent modified nano micro crystal cellulose；
(2) by above-mentioned modified Nano microcrystalline cellulose and polyadipate/butylene terephthalate, lubricant, antioxidant,
Heat stabilizer, photosensitizer together, are placed in high speed blender and are mixed；
(3) above-mentioned uniformly mixed raw material is placed in extruding pelletization in double screw extruder；
(4) standard testing batten is made through injection molding in above-mentioned composite particles, spare.
Embodiment 6
One kind is containing the modified polyadipate/butylene terephthalate composite material of nano micro crystal cellulose and its preparation side
Method is calculated according to the mass fraction, and composition and content are as follows:
Above-mentioned formula is reacted according to the following steps:
(1) a certain amount of above-mentioned nano micro crystal cellulose is mixed with 50ml dehydrated alcohol, ultrasonic disperse 10min must disperse
Even suspension；γ-glycidyl ether oxygen propyl trimethoxy silicane (KH560) (is pressed into nano micro crystal cellulose mass fraction
0.5% be added) be dissolved in 50ml dehydrated alcohol；Unit for uniform suspension is uniformly mixed at 80 DEG C the 3- that flows back with coupling agent solution
5h；It is cooled to room temperature, is centrifuged, dried in 80 DEG C of vacuum drying ovens.Obtain coupling agent modified nano micro crystal cellulose；
(2) by above-mentioned modified Nano microcrystalline cellulose and polyadipate/butylene terephthalate, lubricant, antioxidant,
Heat stabilizer, photosensitizer together, are placed in high speed blender and are mixed；
(3) above-mentioned uniformly mixed raw material is placed in extruding pelletization in double screw extruder；
(4) standard testing batten is made through injection molding in above-mentioned composite particles, spare.
Comparative example 1
Unmodified polyadipate/butylene terephthalate is squeezed according to 6 step of embodiment (3) and (4) same method
It is granulated out, injection molding.
Comparative example 2
With unmodified nano micro crystal cellulose substituting modification nano micro crystal cellulose, i.e. omission step (1), remaining is the same as real
Apply example 6.
Using universal electrical tensile testing machine (SUN500 type is manufactured by Italian GALDABINI company) to above-mentioned implementation
Example 1-6 is final preparation-obtained a kind of containing the modified polyadipate/butylene terephthalate composite wood of nano micro crystal cellulose
Material and the tensile strength of comparative example, elongation at break are measured, and the result is shown in shown in table 1:
Table 1
| Tensile strength/MPa | Elongation at break/% | |
| Embodiment 1 | 32.7 | 312.3 |
| Embodiment 2 | 37.5 | 323.5 |
| Embodiment 3 | 39.9 | 331.4 |
| Embodiment 4 | 33.6 | 309.5 |
| Embodiment 5 | 39.2 | 318.2 |
| Embodiment 6 | 40.0 | 323.4 |
| Comparative example 1 | 23.5 | 290.8 |
| Comparative example 2 | 29.3 | 301.5 |
As can be seen from the table, containing the modified polyadipate/terephthalic acid (TPA) of nano micro crystal cellulose prepared by the invention
Fourth diester composite material has good mechanical property, and modified material its tensile strength has different degrees of raising,
Meet the application requirement of general-purpose plastics, and production cost can be reduced, weakens it as waste pressure caused by environment, mention
High efficiency.
The above shows and describes the basic principle, main features and advantages of the invention.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (10)
1. one kind is containing the modified polyadipate/butylene terephthalate composite material of nano micro crystal cellulose, which is characterized in that packet
The component of following mass parts: 100 parts of polyadipate/butylene terephthalates and 1-20 parts of modified Nano microcrystalline celluloses is included,
Extruding pelletization after being blended by high speed；The modified Nano microcrystalline cellulose is prepared via a method which:
Step 1 mixes nano micro crystal cellulose with dehydrated alcohol, and ultrasonic disperse obtains nano micro crystal cellulose suspension；
Coupling agent is dissolved in dehydrated alcohol and is made into coupling agent solution by step 2；
Step 3 mixes the nano micro crystal cellulose suspension and coupling agent solution, 75-85 DEG C of reflux 2-4h；
Step 4 is cooled to room temperature, be centrifuged, dry after obtain the modified Nano microcrystalline cellulose.
2. it is modified polyadipate/butylene terephthalate composite material containing nano micro crystal cellulose as described in claim 1,
It is characterized in that, the additive amount of the coupling agent is the 0.5-2% of nano micro crystal cellulose quality.
3. it is modified polyadipate/butylene terephthalate composite material containing nano micro crystal cellulose as described in claim 1,
It is characterized in that, the coupling agent is silane coupling agent.
4. it is modified polyadipate/butylene terephthalate composite material containing nano micro crystal cellulose as described in claim 1,
It is characterized in that, further including the component of following mass parts:
5. it is modified polyadipate/butylene terephthalate composite material containing nano micro crystal cellulose as claimed in claim 4,
It is characterized in that, the lubricant is the mixture of one or both of zinc stearate or calcium stearate；The antioxidant is
Four (β-(3,5- three-level butyl -4- hydroxy phenyl) propionic acid) pentaerythritol esters or bis- (3,5- three-level butyl -4- hydroxy phenyl) sulphur
The mixture of one or both of ether.
6. it is modified polyadipate/butylene terephthalate composite material containing nano micro crystal cellulose as claimed in claim 4,
It is characterized in that, the heat stabilizer is the mixture of one or both of maleic anhydride or epoxidized soybean oil；It is described
Photosensitizer is the mixture of one or both of aminodithioformic acid iron or ferric stearate.
7. it is modified polyadipate/butylene terephthalate composite material containing nano micro crystal cellulose as described in claim 1,
It is characterized in that, the number-average molecular weight of the polyadipate/butylene terephthalate is 3.6 × 104。
8. a kind of prepare as described in claim any one of 1-7 containing the modified polyadipate/terephthalic acid (TPA) of nano micro crystal cellulose
The method of fourth diester composite material, which comprises the steps of:
The nano micro crystal cellulose is placed in high speed blender together with polyadipate/butylene terephthalate by step 1
In mixed；
It is described fine containing nano microcrystalline to be placed in extruding pelletization acquisition in double screw extruder by step 2 for above-mentioned uniformly mixed raw material
Modified polyadipate/butylene terephthalate the composite material of dimension element.
9. a kind of method as claimed in claim 8, which is characterized in that further include in step 1 by the lubricant, antioxidant,
Heat stabilizer, photosensitizer are blended together with polyadipate/butylene terephthalate with the nano micro crystal cellulose, the profit
Lubrication prescription is the mixture of one or both of zinc stearate or calcium stearate；The antioxidant is four (β-(3,5- three-level fourths
Base -4- hydroxy phenyl) propionic acid) one or both of pentaerythritol ester or bis- (3,5- three-level butyl -4- hydroxy phenyl) thioethers
Mixture；The heat stabilizer is the mixture of one or both of maleic anhydride or epoxidized soybean oil；The light
The quick dose of mixture for one or both of aminodithioformic acid iron or ferric stearate.
10. a kind of method as claimed in claim 8, which is characterized in that further include following steps:
Step 3, modified polyadipate/butylene terephthalate containing nano micro crystal cellulose described in step 2 acquisition is multiple
Profile is made through injection molding in condensation material.
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| CN113201208A (en) * | 2021-05-31 | 2021-08-03 | 浙江华峰环保材料有限公司 | PBAT composite material and preparation method and application thereof |
| CN113402857A (en) * | 2021-06-09 | 2021-09-17 | 华南理工大学 | Lignin/PBAT composite material and preparation method and application thereof |
| CN113876961A (en) * | 2021-09-28 | 2022-01-04 | 珠海市东辰制药有限公司 | Co-processing auxiliary material and preparation method and application thereof |
| CN113876961B (en) * | 2021-09-28 | 2024-01-30 | 珠海市东辰制药有限公司 | Co-processing auxiliary material and preparation method and application thereof |
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Application publication date: 20190423 |