CN107129669A - A kind of preparation method of high interface binding intensity jute lactic acid composite material - Google Patents
A kind of preparation method of high interface binding intensity jute lactic acid composite material Download PDFInfo
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- CN107129669A CN107129669A CN201710416408.0A CN201710416408A CN107129669A CN 107129669 A CN107129669 A CN 107129669A CN 201710416408 A CN201710416408 A CN 201710416408A CN 107129669 A CN107129669 A CN 107129669A
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- fiber
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- dioxide gel
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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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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/77—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
- D06M11/79—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof with silicon dioxide, silicic acids or their salts
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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
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Reinforced Plastic Materials (AREA)
Abstract
The invention discloses a kind of preparation method of high interface binding intensity jute lactic acid composite material, it is characterised in that comprises the following steps：--- silicon dioxide gel processing --- hydrolysis process --- prepares modified flaxen fiber lactic acid composite material for pretreatment；Wherein：Fiber pretreatment can remove the non-cellulosic material for being covered in fiber surface, process of fiber surface is produced groove, be conducive to producing machinery nail anchor effect when preparing enhancing composite, while pretreatment can assign fiber homogeneous color and luster；Silicon dioxide gel and hydrolysis process, in fiber surface formation coarse structure, further improve tool nail anchor effect of the PLA in fiber surface；Present invention process is simple, condition is easy to control, and tossa has good compatibility with PLA, and interface binding intensity is high, and the composite enhancing effect produced is notable, cost is relatively low.
Description
Technical field：
The invention belongs to composite manufacture field, and in particular to a kind of high interface binding intensity jute PLA composite wood
The preparation method of material.
Background technology：
Fibre reinforced composites are because proportion is small, specific strength and the excellent properties such as specific modulus is big, are widely used in space flight
The fields such as aviation, national defence, traffic, physical culture.In recent years, with people's environmental consciousness continuous improvement and fossil resources it is increasingly withered
Exhaust, staple fibre (such as glass fibre, aramid fiber and carbon fiber) of the tradition by raw material of fossil resources strengthens the disadvantage of composite
First day of the lunar year benefit shows.String is a kind of biodegradable renewable resource, just progressively replaces people in many application fields
Fiber is made as the topmost reinforcing material of polymeric matrix.Early-stage Study finds that natural plant fibre is because with stronger suction
Moist and polarity, it is poor with non-polar polymer matrix interface compatibility and caking property, and also easily aggregation forms fiber-rich area,
Mechanical strength and intensity distribution to composite, which are produced, to be had a strong impact on." bridge " being connected as reinforcement with matrix, interface
Microstructure and binding ability decide the overall performance of composite, composite material interface performance is multiple as fiber reinforcement
The study hotspot in condensation material field.
At present, by handling reduction fiber surface hydroxy radical content, hydrophilic radical is replaced with hydrophobic group, improved with this
The main method of interface compatibility between fiber and resin matrix.So far, researcher using Physical (such as be heat-treated,
Ion processing etc.) and chemical method (such as alkali process, acetylation process, surface grafting, interface coupling) fiber surface is changed
Property, the compatibility of fiber and interlaminar resin is improved to a certain extent, but result shows single surface hydrophobic modification to interface
The raising of adhesion strength has certain limitation.
Li etc. have studied influence of the Fiber strength to interface shear strength by Single fiber pull-out test, it is found that warp
The force-displacement curve when sisal fiber for crossing silane treatment is extracted is occurred in that after power reaches maximum drastically to be declined, and occurs interface
Unsticking phenomenon, and it is relatively rough by potassium permanganate and cumyl peroxide processing fiber surface, serve machinery nail anchor and make
With force-displacement curve reaches and steadily declined after maximum during extraction.As can be seen here, it is coarse microcosmic in fiber surface structure hydrophobicity
Structure, can be effectively improved the interface compatibility and adhesive property of fiber and interlaminar resin.
By silane coupler to nano silicon (SiO2) colloidal sol processing fiber surface modified, can be in fiber table
A kind of micro-nano coarse structure of hydrophobicity is constructed in face, is currently used primarily in the preparation of superhydrophobic fibers product.Ground in composite
Study carefully middle discovery, nano silicon dioxide sol processing can assign fiber good hydrophobicity, but roughness is smaller, cause compound
Machinery nail anchor effect in material is weaker；Surface roughness can further improve using basic hydrolysis, so as to be more beneficial for machinery
Engagement.
The content of the invention：
It is an object of the invention to provide a kind of preparation method of high interface binding intensity jute/lactic acid composite material,
Present invention process is simple, condition is easy to control, and tossa has good compatibility with PLA, and interface binding intensity is high, system
The composite enhancing effect that takes is notable, cost is relatively low.
To reach above-mentioned purpose, the technical scheme is that：
A kind of preparation method of high interface binding intensity jute lactic acid composite material, it is characterised in that including following step
Suddenly：
(1) pre-process：
In 5-10min, sequentially add 10-20g/L sodium hydroxide, 5-10g/L hydrogen peroxide, 3-5g/L sodium metasilicate,
1-3g/L penetrating agent JFC, weight bath raio is 1：10-20,80-100 DEG C is warming up to 1-3 DEG C/min, is incubated 90-180min,
Washing, pickling to neutrality is washed, dehydration；
(2) silicon dioxide gel is handled：
1. silicon dioxide gel is prepared：
Reaction solution is constituted：10-50g/L presomas, 0.1-0.5g/L neopelexes, 1-5g/L hydrochloric acid；
Reaction condition：Neopelex is added in 1-5g/L aqueous hydrochloric acid solutions, stirred under the conditions of 30 DEG C,
Neopelex is fully dissolved, presoma is gradually added into 20-30min, after presoma is added, continue to stir
30-60min, is then warming up to 50-70 DEG C with 1-3 DEG C/min, 3-6h is reacted under conditions of stirring；
Presoma is selected from：Tetraethyl orthosilicate, MTMS, MTES, ethyl trimethoxy
One or more in silane, ethyl triethoxysilane；
2. fibre modification：
It is 5-6 that silicon dioxide gel is adjusted to pH value by the sodium hydroxide solution for being 10% with mass concentration, at room temperature, is adopted
Fiber is modified with the methods rolled of two leaching two, pick-up is to dry 20-30min, 120- under the conditions of 80-100%, 80-100 DEG C
150 DEG C bake 10-20min, 80-100 DEG C of drying；
(3) hydrolysis process：
Under the conditions of 40-60 DEG C, the flaxen fiber that silicon dioxide gel is handled is placed in 5-15g/L sodium hydroxide solution
10-30min is hydrolyzed, bath raio is 1：10-20, is washed to neutrality, 80-10 DEG C of drying；
(4) modified flaxen fiber lactic acid composite material is prepared：
Flaxen fiber and PLA after step (3) processing in 80-100 DEG C of drying 2-4h is removed into moisture removal, using being hot pressed into
Type method prepares enhancing composite, and tossa content is 10-30%.
Further it is provided in：
In step (2), during the mixture of presoma selection MTMS and ethyl trimethoxy silane, it is combined
The performance of material is optimal.
In step (2), the silicon dioxide gel of preparation, silicon dioxide gel particle diameter is 50~100nm.
In step (2), the method rolled using two leachings two is modified to fiber, pick-up 90%.
The principle that the present invention is used is as follows：
(1) fiber is pre-processed：
Tossa contains the non-cellulosic materials such as 20-40% pectin, lignin, hemicellulose, pigment, these materials
Fiber surface is covered in, such flaxen fiber surface is smooth, color and luster heterogeneity.In sodium hydroxide and hydrogen peroxide treatment, lead to
Condition control is crossed, the non-cellulosic material for being covered in fiber surface can be removed, process of fiber surface is produced groove, is conducive to
Machinery nail anchor effect is produced when preparing enhancing composite, while pretreatment can assign fiber homogeneous color and luster.
(2) silicon dioxide gel pH value is adjusted：
Effective hydrolysis of presoma is the basis for preparing silicon dioxide gel, and acidity regulation is conducive to the hydrolysis of presoma.
However, poor as the tossa acid resistance of cellulose fibre.Silicon dioxide gel pH value is adjusted to 5-6, will not both be led
The great condensation of sol particles is caused, obvious influence will not be also caused on fibre strength, improves enhancing effect.
(3) hydrolysis process：
Silicon dioxide gel processing fiber surface degree of roughness is weaker, using silicone hydroxyl (Si-OH) condensation product in alkaline bar
The characteristic of facile hydrolysis under part, coarse structure is formed on surface by basic hydrolysis, further improves tool of the PLA in fiber surface
Follow closely anchor effect.
The beneficial effects of the invention are as follows：
The preparation method of jute/lactic acid composite material is modified by using a kind of obtained surface of the present invention, it is and existing
Technology is compared, with advantage following prominent and good effect：
(1) technique is simple, and technological parameter is stablized easy to control；
(2) method of modifying influences small to fibrous mechanical property；
(3) modified jute and PLA compatibility are good, easily scattered；
(4) modified flaxen fiber and PLA interfacial adhesion are strong；
(5) the composite enhancing effect produced is notable.
Below in conjunction with the drawings and specific embodiments, the present invention will be further described.
Brief description of the drawings：
Fig. 1 is using fiber surface structure figure after the non-caustic dip processing of silicon dioxide gel；
Fig. 2 is using the fiber surface structure figure after hydrolysis process of the present invention.
Embodiment：
A kind of surface of the present invention is modified the preparation method of jute lactic acid composite material, comprises the following steps：
(1) pre-process：
Under room temperature condition, sequentially add 10-20g/L sodium hydroxide, 5-10g/L hydrogen peroxide, 3-5g/L sodium metasilicate,
1-3g/L penetrating agent JFC, weight bath raio is 1：10-20,80-100 DEG C is warming up to 1-3 DEG C/min, is incubated 90-180min,
Washing, pickling to neutrality is washed, dehydration；
Traditional use retting cut-out carries out alkali process again, due to colloid in root fiber, middle part fiber and taper fiber
Content is different, therefore, the intensity of different parts fiber can be caused irregular, causes the composite prepared using different parts fiber
Intensity there is significant difference.
The present invention takes kiering to pre-process, and adjusts kiering handling process parameter, so that the intensity of composite is equal
It is even consistent.
(2) silicon dioxide gel is handled：
1. silicon dioxide gel is prepared：
Reaction solution is constituted：10-50g/L presomas, 0.1-0.5g/L neopelexes, 1-5g/L hydrochloric acid (quality
36.5%) concentration be.
Reaction condition：Neopelex is added in 1-5g/L aqueous hydrochloric acid solutions, stirred under the conditions of 30 DEG C,
Neopelex is fully dissolved, presoma is gradually added into 20-30min, after presoma is added, continue to stir
30-60min, is then warming up to 50-70 DEG C with 1-3 DEG C/min, 3-6h is reacted under conditions of stirring.
Presoma is：Tetraethyl orthosilicate, MTMS, MTES, ethyl trimethoxy silicon
One or more of mixtures in alkane, ethyl triethoxysilane.
2. fibre modification：
It is 5-6 that silicon dioxide gel is adjusted to pH value by the sodium hydroxide solution for being 10% with mass concentration, at room temperature, is adopted
Fiber is modified with the methods rolled of two leaching two, pick-up is to dry 20-30min, 120- under the conditions of 80-100%, 80-100 DEG C
150 DEG C bake 10-20min, 80-100 DEG C of drying.
Table 1, the tossa performance control of different method of modifying processing
From table 1：
The hygroscopicity of acetylation process fiber is larger, and hygroscopicity and the waterproofing agent of silicon dioxide gel modified fibre are modified fibre
That ties up is close, because, acetylation process is that the hydroxyl in fiber is esterified, and is not only difficult to carry out ester to all hydroxyls
Change, and the hydrophobicity of ester bond is limited, and waterproofing agent is modified and silicon dioxide gel modification is dredged for one layer in fiber surface formation
Aqueous film, so the hydrophobicity of modified fibre is preferable.
The intensity of acetylated modification fiber reinforcement PLA composites is minimum, and the enhancing of silicon dioxide gel modified fibre is compound
The maximum intensity of material.Because, the hydrophobicity and morphosis of fiber surface are influence fibre reinforced composites intensity
Two principal elements.Not only hydrophobicity is weaker for acetylated modification fiber, and acetylation is carried out in acid condition, and
Cellulose facile hydrolysis in acid condition, the damage to fibre strength is the most serious, so acetylated modification fiber-reinforced composite
The intensity of material is minimum.
Though it can assign fiber relatively low water imbibition as shown in figure 1, waterproofing agent is modified, the hydrophobic-film surfaces' light formed
It is sliding, and silicon dioxide gel surface modification treatment, what is obtained is coarse hydrophobic surface (as shown in Figure 2), not only with PLA interfaces
Compatibility is good, and can produce good machinery nail anchor effect, improves interface binding intensity.
Fiber surface structure plays decisive role to the mechanical strength of composite, and influences modified fibre surface texture
4 principal elements have the size of hydrophobic grouping in presoma, the size of aerosol particle size (by adjust presoma consumption, reaction
Temperature, reaction time etc. are controlled), be attached to fiber surface silicon dioxide gel content (by adjusting dip time, it is preceding
Bulk concentration, liquid carrying rate etc. is driven to be controlled) and naoh concentration.Above-mentioned 4 principal elements are to fiber hygroscopicity and composite wood
The affecting laws of material mechanical strength are shown in Table 2.
The influence of table 2, different disposal technique to fiber hygroscopicity and the mechanical intensity of composite
Note：Data are single factor test data in table, that is, when studying a certain factor, only change the technique bar of the factor
Part, the process conditions of other all factors are identical.
As shown in table 2：
Silicon dioxide gel prepared by a, different presomas, the mechanical intensity of hygroscopicity and composite to fiber has bright
Aobvious influence.This is probably because silicon dioxide gel prepared by tetraethyl orthosilicate does not contain hydrophobic alkyl, with its modification
The hygroscopicity of fiber is preferable, and the intensity of composite is less than normal.Silicon dioxide gel prepared by alkyl trimethoxysilane contains
Hydrophobic alkyl, can improve the hydrophobicity of fiber, while hydrophobic alkyl has good compatibility with PLA.Alkyl is bigger,
Hydrophobicity is better, but aerosol particle size is also bigger.As can be seen from Table 4, presoma selection MTMS and second
During the mixture of base trimethoxy silane, the performance of composite is optimal.
B, silicon dioxide gel particle diameter have obvious influence to fiber hygroscopicity and the mechanical strength of composite.This can
Can be because, when aerosol particle size is smaller or larger, in the basic conditions be condensed easily produce slight crack, formed by film fail by
Fiber surface is coated completely.Table 4 shows, when silicon dioxide gel is 50~100nm, best results.
C, pick-up are bigger, and the colloidal sol amount being adsorbed on fiber is more.When pick-up is smaller, silicon dioxide gel is in alkali
Property under the conditions of be condensed, slight crack is easily produced, and fiber surface can not completely be coated, so as to influence fiber hygroscopicity and composite wood
The intensity of material.After the colloidal sol being adsorbed on fiber is enough to form the coarse film of densification in fiber surface, continues increase and roll remaining
Rate, will not further improve fiber hygroscopicity and the intensity of composite.Table 4 shows that 90% pick-up can meet requirement.
(3) hydrolysis process
Under the conditions of 40-60 DEG C, the flaxen fiber that silicon dioxide gel is handled is placed in 5-15g/L sodium hydroxide solution
10-30min is hydrolyzed, bath raio is 1：10-20, is washed to neutrality, 80-10 DEG C of drying.
As shown in figure 1, the fiber surface after silicon dioxide gel processing is smooth, existed using silicone hydroxyl (Si-OH) condensation product
The characteristic of facile hydrolysis under alkalescence condition, forms coarse structure (see Fig. 2) on surface by hydrolysis process, realizes PLA in fiber
The machinery nail anchor effect on surface, improves the interface binding intensity of fiber and PLA.
(4) modified flaxen fiber lactic acid composite material is prepared：
Flaxen fiber and PLA after step (3) processing is removed into moisture removal in 80-100 DEG C of drying 2-4h, using conventional heat
Molded method prepares enhancing composite, and tossa content is 10-30%.
Claims (4)
1. a kind of preparation method of high interface binding intensity jute lactic acid composite material, it is characterised in that comprise the following steps：
（1）Pretreatment：
In 5-10min, 10-20g/L sodium hydroxide, 5-10g/L hydrogen peroxide, 3-5g/L sodium metasilicate, 1- is sequentially added
3g/L penetrating agent JFC, weight bath raio is 1：10-20,80-100 DEG C is warming up to 1-3 DEG C/min, is incubated 90-180min, water
Wash, pickling to neutrality, wash, dehydration；
（2）Silicon dioxide gel processing：
Prepare silicon dioxide gel：
Reaction solution is constituted：10-50g/L presomas, 0.1-0.5g/L neopelexes, 1-5g/L hydrochloric acid；
Reaction condition：Neopelex is added in 1-5g/L aqueous hydrochloric acid solutions, is stirred under the conditions of 30 DEG C, makes ten
Dialkyl benzene sulfonic acids sodium is fully dissolved, and presoma is gradually added into 20-30min, after presoma is added, and continues to stir 30-
60min, is then warming up to 50-70 DEG C with 1-3 DEG C/min, 3-6h is reacted under conditions of stirring；
Presoma is selected from：Tetraethyl orthosilicate, MTMS, MTES, ethyl trimethoxy silane,
One or more in ethyl triethoxysilane；
Fibre modification：
It is 5-6 that silicon dioxide gel is adjusted to pH value by the sodium hydroxide solution for being 10% with mass concentration, at room temperature, using two
The methods rolled of leaching two are modified to fiber, and pick-up is to dry 20-30min, 120-150 DEG C under the conditions of 80-100%, 80-100 DEG C
Bake 10-20min, 80-100 DEG C of drying；
（3）Hydrolysis process：
Under the conditions of 40-60 DEG C, the flaxen fiber that silicon dioxide gel is handled is placed in 5-15g/L sodium hydroxide solution and hydrolyzed
10-30min, bath raio is 1：10-20, is washed to neutrality, 80-10 DEG C of drying；
（4）Prepare modified flaxen fiber lactic acid composite material：
By step（3）Flaxen fiber and PLA after processing remove moisture removal in 80-100 DEG C of drying 2-4h, using hot pressing formation process
Enhancing composite is prepared, tossa content is 10-30%.
2. a kind of preparation method of high interface binding intensity jute lactic acid composite material according to claim 1, it is special
Levy and be：Step（2）In, during the mixture of presoma selection MTMS and ethyl trimethoxy silane, it is combined
The performance of material is optimal.
3. a kind of preparation method of high interface binding intensity jute lactic acid composite material according to claim 1, it is special
Levy and be：Step（2）In, the silicon dioxide gel of preparation, silicon dioxide gel particle diameter is 50~100nm.
4. a kind of preparation method of high interface binding intensity jute lactic acid composite material according to claim 1, it is special
Levy and be：Step（2）In, the method rolled using two leachings two is modified to fiber, pick-up 90%.
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Cited By (5)
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|---|---|---|---|---|
| CN107236267A (en) * | 2017-06-06 | 2017-10-10 | 绍兴文理学院 | A kind of surface is modified the preparation method of jute lactic acid composite material |
| CN108060577A (en) * | 2017-12-19 | 2018-05-22 | 绍兴文理学院 | A kind of preparation method of flaxen fiber reinforced resin based composites |
| CN108084677A (en) * | 2017-12-19 | 2018-05-29 | 绍兴文理学院 | A kind of preparation method of heat-resisting flaxen fiber enhancing lactic acid composite material |
| CN110420356A (en) * | 2019-08-09 | 2019-11-08 | 福州大学 | A kind of Dual-functional integrated bone-cartilage complex tissue engineering rack for osteosarcoma clinical treatment |
| CN115160750A (en) * | 2022-07-26 | 2022-10-11 | 扬州丽华汽车内饰件有限公司 | Environment-friendly degradable jute fiber reinforced polylactic acid composite material and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107236267A (en) * | 2017-06-06 | 2017-10-10 | 绍兴文理学院 | A kind of surface is modified the preparation method of jute lactic acid composite material |
| CN108060577A (en) * | 2017-12-19 | 2018-05-22 | 绍兴文理学院 | A kind of preparation method of flaxen fiber reinforced resin based composites |
| CN108084677A (en) * | 2017-12-19 | 2018-05-29 | 绍兴文理学院 | A kind of preparation method of heat-resisting flaxen fiber enhancing lactic acid composite material |
| CN110420356A (en) * | 2019-08-09 | 2019-11-08 | 福州大学 | A kind of Dual-functional integrated bone-cartilage complex tissue engineering rack for osteosarcoma clinical treatment |
| CN110420356B (en) * | 2019-08-09 | 2021-03-02 | 福州大学 | Dual-function integrated bone-cartilage composite tissue engineering scaffold for clinical treatment of osteosarcoma |
| CN115160750A (en) * | 2022-07-26 | 2022-10-11 | 扬州丽华汽车内饰件有限公司 | Environment-friendly degradable jute fiber reinforced polylactic acid composite material and preparation method thereof |
| CN115160750B (en) * | 2022-07-26 | 2024-04-02 | 扬州丽华汽车内饰件有限公司 | Environment-friendly degradable jute fiber reinforced polylactic acid composite material and preparation method thereof |
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Application publication date: 20170905 |