CN109438945A - A kind of degradable composite material and the preparation method and application thereof - Google Patents
A kind of degradable composite material and the preparation method and application thereof Download PDFInfo
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- CN109438945A CN109438945A CN201811472453.9A CN201811472453A CN109438945A CN 109438945 A CN109438945 A CN 109438945A CN 201811472453 A CN201811472453 A CN 201811472453A CN 109438945 A CN109438945 A CN 109438945A
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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
- C08L67/04—Polyesters derived from hydroxycarboxylic acids, e.g. lactones
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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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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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
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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Abstract
The present invention provides a kind of degradable composite material, is made of following components in parts by weight: 100 parts of PHBV, 1-1.5 parts of dispersing agent, and 2-3 parts of lubricant, 4-5 parts of compatilizer, capsular fibers 3-5 parts in shaddock ped, 4-6 parts of snail shell powder.The invention also discloses the preparation methods of the degradable composite material.The hardness of degradable composite material provided by the invention is higher, and toughness, oxidative age resistance and heat resistance are preferable.
Description
Technical field
The present invention relates to a kind of composite material, more particularly to a kind of degradable composite material and preparation method thereof with answer
With.
Background technique
Degradable composite material refer to the regular hour and it is certain under conditions of, can be by microorganism or its secretion in enzyme
Or the lower composite material degraded of chemical breakdown effect.Degradable composite material mainly has both sides purposes: (1) utilizing it
Degradability solves problem of environmental pollution, to guarantee the sustainable development of environment for human survival.At present to the place of high polymer material
Managing 3 kinds of methods such as mainly has landfill, burns and be recycled, but these types of method has its drawback.If landfill method is to soil
There are long-term hazards, and can not continue to carry out with the increasingly reduction of landfill；Incineration method releases a large amount of pernicious gases；Recycling
Method of reutilization, because the collection of material, sorting difficulty, higher cost are difficult to promote.(2) its degradability is utilized, biology doctor is used as
Use material.It can include polylactic acid (PLA), poly- 8 one caprolactone (PCL), polyethylene with the degradability material that chemical synthesis produces
Alcohol (PVA), poly-β-hydroxybutyric acid (PHB), 3-hydroxybutyrate ester and copolymer (PHBV) of 3- hydroxyl valerate etc..
Application No. is the Chinese patent of CN201710549922.1 disclose a kind of medical antibacterial PHBV composite material and its
Preparation method, the composite material include following component, based on parts by weight: 100 parts of PHBV, 30-40 parts of PBAT, and NCC 10-
17 parts, 8-10 parts of polydioxanone, 1-2 parts of GMA, 11-19 parts of chitosan, 30-44 parts of modified Nano powder.This is compound
For material the problem is that hardness is general, toughness, oxidative age resistance and heat resistance are poor.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of degradable composite materials, and hardness is higher, and toughness, antioxygen
Change aging and heat resistance is preferable.
In order to solve the above technical problems, the technical scheme is that
A kind of degradable composite material, is made of following components in parts by weight: 100 parts of PHBV, 1-1.5 parts of dispersing agent, and lubricant
2-3 parts, 4-5 parts of compatilizer, capsular fibers 3-5 parts in shaddock ped, 4-6 parts of snail shell powder.
Further, dispersing agent of the present invention is polyethylene glycol.
Further, lubricant of the present invention is castor oil.
Further, compatilizer of the present invention is epoxidized soybean oil.
Further, in shaddock ped of the present invention capsular fibers preparation step are as follows:
Shaddock ped capsula interna is obtained after the epidermis of fresh shaddock ped is removed, shaddock ped capsula interna is put into soaking at room temperature 3 in the water of 10 times of weight
It is taken out after hour, crushed 40 meshes after drying at 70 DEG C and obtain shaddock ped capsula interna powder, by the water of the weight such as shaddock ped capsula interna powder addition
In after grinding, be transferred in centrifuge and be centrifugally separating to obtain filter residue and filtrate, by filter residue be added 8 times of weight water in, be transferred to microwave
It obtains fiber first within Microwave Extraction 2.5 minutes after being heated to 45 DEG C in furnace, filtrate is added in the dehydrated alcohol of 15 times of weight, heating
It is extracted 25 minutes after to 55 DEG C and obtains fiber second, fiber first and fiber second 70 DEG C drying 2 hours after mixing smash it through
40 meshes obtain capsular fibers in shaddock ped.
Further, the power of micro-wave oven is 400W when Microwave Extraction of the present invention.
Further, the preparation step of snail shell powder of the present invention are as follows:
It is rinsed with water 5 minutes after snail shell is removed surface impurity, is crushed after air-drying and obtains snail shell coarse powder, by snail shell coarse powder
It is added in the sodium hydroxide solution of 15 times of weight, keeps the temperature 10 hours after being heated to 50 DEG C, be rinsed with water after taking-up 5 minutes, filter
Afterwards will be 2 hours dry at 100 DEG C of filter residue obtained, it smashes it through 80 meshes and obtains snail shell powder.
Further, the mass fraction of sodium hydroxide solution of the present invention is 10%.
Another technical problem to be solved by the present invention is that providing the preparation method of above-mentioned degradable composite material.
In order to solve the above technical problems, technical solution is:
A kind of preparation method of degradable composite material, comprising the following steps:
Each component is weighed by weight, and each component is added to the mixer mixing and obtains blend composition within 15 minutes, blend composition is transferred to
It is squeezed out in double screw extruder and obtains extruded stock, water cooling to room temperature obtains degradable composite wood after extruded stock is granulated with pelletizer
Material.
Further, the mixing temperature of the mixing machine is 110 DEG C, and the extrusion temperature of double screw extruder is 160-180
DEG C, the revolving speed of screw rod is 25rpm.
Therefore compared with prior art, the invention has the following advantages:
1) snail shell is the skin portion of spiral shell, can generally be treated as waste material discarding, and the present invention removes the surface impurity of snail shell
Remove, rinse, air-drying, it is broken obtain snail shell coarse powder, by its with rinsed after sodium hydroxide solution isothermal holding, filtering, dry, powder
Broken obtained snail shell powder, hardness and mechanical performance are preferable, can effectively improve the hardness and toughness of composite material, in addition, its
Heat resistance is stronger, and sodium hydroxide solution isothermal holding expands its surface area, to effectively improve composite material
Heat resistance.
2) shaddock ped capsula interna is the part after shaddock ped removal epidermis, can generally be treated as waste material discarding, the present invention will be in shaddock ped
Capsule grinds by water immersion, dries pulverizing plus water, is centrifugally separating to obtain filter residue and filtrate, and filter residue is micro- by Extraction solvent of water
Wave extracts to obtain fiber first, and filtrate is extracted to obtain fiber second as Extraction solvent using dehydrated alcohol, then by fiber first and fiber
Second mixes, is dry, crushing capsular fibers in obtained shaddock ped, and capsular fibers have very strong toughness and oxidative age resistance in the shaddock ped
Can, can effectively improve the toughness and oxidative age resistance of composite material, and its can also effectively improve snail shell powder and PHBV it
Between compatibility, to further increase the hardness and heat resistance of composite material.
Specific embodiment
Below in conjunction with specific embodiment, the present invention will be described in detail, herein illustrative examples and explanation of the invention
For explaining the present invention, but it is not as a limitation of the invention.
Embodiment 1
Degradable composite material is made of following components in parts by weight: 100 parts of PHBV, 1 part of polyethylene glycol, and 3 parts of castor oil, ring
4.5 parts of oxygen soybean oil, 3.5 parts of capsular fibers in shaddock ped, 4.8 parts of snail shell powder.
Preparation method includes the following steps:
(1) shaddock ped capsula interna is obtained after removing the epidermis of fresh shaddock ped, shaddock ped capsula interna is put into room temperature in the water of 10 times of weight and is soaked
Bubble takes out after 3 hours, crushed 40 meshes after drying at 70 DEG C and obtains shaddock ped capsula interna powder, by weight such as shaddock ped capsula interna powder additions
Grinding, is transferred in centrifuge and is centrifugally separating to obtain filter residue and filtrate after in water, filter residue is added in the water of 8 times of weight, is transferred to micro-
It obtains fiber first within Microwave Extraction 2.5 minutes under 400W power after being heated to 45 DEG C in wave furnace, filtrate is added to the nothing of 15 times of weight
It in water-ethanol, is extracted 25 minutes after being heated to 55 DEG C and obtains fiber second, by fiber first and the 70 DEG C of dryings 2 after mixing of fiber second
Hour, it smashes it through 40 meshes and obtains capsular fibers in shaddock ped；
(2) it is rinsed with water 5 minutes after snail shell being removed surface impurity, is crushed after air-drying and obtains snail shell coarse powder, by snail shell
The mass fraction that 15 times of weight is added in coarse powder is to keep the temperature 10 hours after being heated to 50 DEG C in the sodium hydroxide solution of 10 %, is taken out
After be rinsed with water 5 minutes, will smash it through 80 meshes dry 2 hours at 100 DEG C of filter residue obtained after filtering and obtain snail shell
Powder；
(3) each component is weighed by weight, and each component is added to the mixer mixing and obtains blend composition within 15 minutes, blend composition is turned
Enter to squeeze out in double screw extruder and obtain extruded stock, water cooling to room temperature obtains degradable compound after extruded stock is granulated with pelletizer
Material, the mixing temperature of mixing machine are 110 DEG C, and the extrusion temperature of double screw extruder is 160-180 DEG C, and the revolving speed of screw rod is
25rpm。
Embodiment 2
Degradable composite material is made of following components in parts by weight: 100 parts of PHBV, 1.5 parts of polyethylene glycol, and 2 parts of castor oil,
4.8 parts of epoxidized soybean oil, 4.5 parts of capsular fibers in shaddock ped, 4 parts of snail shell powder.
Preparation method is same as Example 1.
Embodiment 3
Degradable composite material is made of following components in parts by weight: 100 parts of PHBV, 1.2 parts of polyethylene glycol, and castor oil 2.5
Part, 4.2 parts of epoxidized soybean oil, 4 parts of capsular fibers in shaddock ped, 5.5 parts of snail shell powder.
Preparation method is same as Example 1.
Embodiment 4
Degradable composite material is made of following components in parts by weight: 100 parts of PHBV, 1.4 parts of polyethylene glycol, and castor oil 2.8
Part, 5 parts of epoxidized soybean oil, 3 parts of capsular fibers in shaddock ped, 6 parts of snail shell powder.
Preparation method is same as Example 1.
Embodiment 5
Degradable composite material is made of following components in parts by weight: 100 parts of PHBV, 1.1 parts of polyethylene glycol, and castor oil 2.4
Part, 4 parts of epoxidized soybean oil, 5 parts of capsular fibers in shaddock ped, 5 parts of snail shell powder.
Preparation method is same as Example 1.
Comparative Examples 1
It does not include capsular fibers in shaddock ped in component, other components and preparation method are same as Example 3.
Comparative Examples 2
It does not include snail shell powder in component, other components and preparation method are same as Example 3.
Comparative example
Comparative example is the embodiment 1 of the Chinese invention application No. is CN201710549922.1.
Experimental example one: hardness test
Test the Rockwell hardness of each composite material.Test result is as shown in table 1:
| Rockwell hardness (HRB) | |
| Embodiment 1 | 64.5 |
| Embodiment 2 | 64.2 |
| Embodiment 3 | 64.7 |
| Embodiment 4 | 64.4 |
| Embodiment 5 | 64.0 |
| Comparative Examples 1 | 61.1 |
| Comparative Examples 2 | 57.6 |
| Comparative example | 57.3 |
Table 1
As seen from Table 1, the hardness of 1-5 of the embodiment of the present invention is obviously higher than comparative example.The constituent part of Comparative Examples 1,2
Different from embodiment 1-5, wherein the hardness of Comparative Examples 1 is declined, and illustrates that capsular fibers can effectively improve spiral shell in shaddock ped
The compatibility of shell powder and PHBV；There are many hardness decline of Comparative Examples 2, illustrate that snail shell powder can greatly improve composite material
Hardness.
Experimental example two: toughness test
The impact strength of each composite material is tested with reference to GB/T 1043-1992, impact strength is higher to show that toughness is better.Test
The results are shown in Table 2:
| Impact strength (kJm-2) | |
| Embodiment 1 | 61.2 |
| Embodiment 2 | 60.8 |
| Embodiment 3 | 61.7 |
| Embodiment 4 | 61.3 |
| Embodiment 5 | 60.4 |
| Comparative Examples 1 | 46.6 |
| Comparative Examples 2 | 45.5 |
| Comparative example | 37.1 |
Table 2
As seen from Table 2, it is preferable to show that the present invention has obviously higher than comparative example for the impact strength of 1-5 of the embodiment of the present invention
Toughness.The constituent part of Comparative Examples 1,2 is different from embodiment 1-5, wherein the impact strength of Comparative Examples 1,2 under
Drop is many, illustrates that capsular fibers and snail shell powder can effectively improve the toughness of composite material in shaddock ped.
Experimental example three: oxidative age resistance test
Each composite material is made in the hydrogen peroxide solution for 10% mass fraction for being soaked in 60 DEG C after film, is determined after 90 hours
Quality retention, quality retention=post-test quality/pre-test quality × 100%, quality retention is higher show it is anti-oxidant old
Change performance is better, and test result is as shown in table 3:
| Quality retention (%) | |
| Embodiment 1 | 90.6 |
| Embodiment 2 | 90.3 |
| Embodiment 3 | 91.2 |
| Embodiment 4 | 90.8 |
| Embodiment 5 | 90.5 |
| Comparative Examples 1 | 78.4 |
| Comparative Examples 2 | 90.7 |
| Comparative example | 72.9 |
Table 3
As seen from Table 3, the quality retention of 1-5 of the embodiment of the present invention is obviously higher than comparative example, show the present invention have compared with
Good oxidative age resistance.The constituent part of Comparative Examples 1,2 is different from embodiment 1-5, wherein the quality of Comparative Examples 1
There are many conservation rate decline, illustrate that capsular fibers can greatly improve the oxidative age resistance of composite material in shaddock ped；Comparative Examples 2
Quality retention and embodiment 1-5 are similar, illustrate that snail shell powder has little effect oxidative age resistance.
Experimental example four: heat resistance test
The temperature of initial decomposition of each composite material is tested using thermogravimetric analyzer, heating rate is 10 DEG C/min, and temperature elevating range is
30-500 DEG C, temperature of initial decomposition is higher to show that heat resistance is better, and test result is as shown in table 4:
| Temperature of initial decomposition (DEG C) | |
| Embodiment 1 | 253.0 |
| Embodiment 2 | 253.7 |
| Embodiment 3 | 254.5 |
| Embodiment 4 | 252.6 |
| Embodiment 5 | 253.4 |
| Comparative Examples 1 | 245.8 |
| Comparative Examples 2 | 227.9 |
| Comparative example | 221.3 |
Table 4
As seen from Table 4, the temperature of initial decomposition of 1-5 of the embodiment of the present invention shows that the present invention has obviously higher than comparative example
Preferable heat resistance.The constituent part of Comparative Examples 1,2 is different from embodiment 1-5, wherein the initial decomposition of Comparative Examples 1
Temperature is declined, and illustrates that capsular fibers can effectively improve snail shell powder and the compatibility of PHBV in shaddock ped；At the beginning of Comparative Examples 2
There are many decline of beginning decomposition temperature, illustrate that snail shell powder can greatly improve the heat resistance of composite material.
The above-described embodiments merely illustrate the principles and effects of the present invention, and is not intended to limit the present invention.It is any ripe
The personage for knowing this technology all without departing from the spirit and scope of the present invention, carries out modifications and changes to above-described embodiment.Cause
This, institute is complete without departing from the spirit and technical ideas disclosed in the present invention by those of ordinary skill in the art such as
At all equivalent modifications or change, should be covered by the claims of the present invention.
Claims (10)
1. a kind of degradable composite material, it is characterised in that: be made of following components in parts by weight: 100 parts of PHBV, dispersing agent
1-1.5 parts, 2-3 parts of lubricant, 4-5 parts of compatilizer, capsular fibers 3-5 parts in shaddock ped, 4-6 parts of snail shell powder.
2. a kind of degradable composite material according to claim 1, it is characterised in that: the dispersing agent is polyethylene glycol.
3. a kind of degradable composite material according to claim 1, it is characterised in that: the lubricant is castor oil.
4. a kind of degradable composite material according to claim 1, it is characterised in that: the compatilizer is epoxy soybean
Oil.
5. a kind of degradable composite material according to claim 1, it is characterised in that: the preparation of capsular fibers in the shaddock ped
Step are as follows:
Shaddock ped capsula interna is obtained after the epidermis of fresh shaddock ped is removed, shaddock ped capsula interna is put into soaking at room temperature 3 in the water of 10 times of weight
It is taken out after hour, crushed 40 meshes after drying at 70 DEG C and obtain shaddock ped capsula interna powder, by the water of the weight such as shaddock ped capsula interna powder addition
In after grinding, be transferred in centrifuge and be centrifugally separating to obtain filter residue and filtrate, by filter residue be added 8 times of weight water in, be transferred to microwave
It obtains fiber first within Microwave Extraction 2.5 minutes after being heated to 45 DEG C in furnace, filtrate is added in the dehydrated alcohol of 15 times of weight, heating
It is extracted 25 minutes after to 55 DEG C and obtains fiber second, fiber first and fiber second 70 DEG C drying 2 hours after mixing smash it through
40 meshes obtain capsular fibers in shaddock ped.
6. a kind of degradable composite material according to claim 5, it is characterised in that: the power of micro-wave oven when Microwave Extraction
For 400W.
7. a kind of degradable composite material according to claim 1, it is characterised in that: the preparation step of the snail shell powder
Are as follows:
It is rinsed with water 5 minutes after snail shell is removed surface impurity, is crushed after air-drying and obtains snail shell coarse powder, by snail shell coarse powder
It is added in the sodium hydroxide solution of 15 times of weight, keeps the temperature 10 hours after being heated to 50 DEG C, be rinsed with water after taking-up 5 minutes, filter
Afterwards will be 2 hours dry at 100 DEG C of filter residue obtained, it smashes it through 80 meshes and obtains snail shell powder.
8. a kind of degradable composite material according to claim 7, it is characterised in that: the quality of the sodium hydroxide solution
Score is 10%.
9. the preparation method of degradable composite material according to any one of claims 1 to 8, it is characterised in that: including with
Lower step:
Each component is weighed by weight, and each component is added to the mixer mixing and obtains blend composition within 15 minutes, blend composition is transferred to
It is squeezed out in double screw extruder and obtains extruded stock, water cooling to room temperature obtains degradable composite wood after extruded stock is granulated with pelletizer
Material.
10. the preparation method of degradable composite material according to claim 9, it is characterised in that: the mixing machine mixes
Closing temperature is 110 DEG C, and the extrusion temperature of double screw extruder is 160-180 DEG C, and the revolving speed of screw rod is 25rpm.
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Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201811472453.9A CN109438945A (en) | 2018-12-04 | 2018-12-04 | A kind of degradable composite material and the preparation method and application thereof |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101760037A (en) * | 2008-12-23 | 2010-06-30 | 金发科技股份有限公司 | Completely degraded plant powder modified thermoplastics composite material and preparation method thereof |
| US20140275351A1 (en) * | 2013-03-14 | 2014-09-18 | Georgia-Pacific Chemicals Llc | Hydrophobizing agents for use in making composite lignocellulose products |
| CN107033520A (en) * | 2016-10-21 | 2017-08-11 | 广西师范学院 | The preparation method of wear-resisting SBS material for sole of shoe |
| CN108641215A (en) * | 2018-03-21 | 2018-10-12 | 佛山市高明区创奇装饰材料有限公司 | A kind of novel foam polyvinyl chloride plate |
-
2018
- 2018-12-04 CN CN201811472453.9A patent/CN109438945A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101760037A (en) * | 2008-12-23 | 2010-06-30 | 金发科技股份有限公司 | Completely degraded plant powder modified thermoplastics composite material and preparation method thereof |
| US20140275351A1 (en) * | 2013-03-14 | 2014-09-18 | Georgia-Pacific Chemicals Llc | Hydrophobizing agents for use in making composite lignocellulose products |
| CN107033520A (en) * | 2016-10-21 | 2017-08-11 | 广西师范学院 | The preparation method of wear-resisting SBS material for sole of shoe |
| CN108641215A (en) * | 2018-03-21 | 2018-10-12 | 佛山市高明区创奇装饰材料有限公司 | A kind of novel foam polyvinyl chloride plate |
Non-Patent Citations (1)
| Title |
|---|
| 潘明珠等: "聚乙二醇对稻秸纤维/PHBV复合材料性能的影响", 《南京林业大学学报（自然科学版）》 * |
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