CN104497561A - Biomass nanocrystal enhanced type nylon composite material, composite master batch and preparation method - Google Patents
Biomass nanocrystal enhanced type nylon composite material, composite master batch and preparation method Download PDFInfo
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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
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
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- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/06—Polyamides derived from polyamines and polycarboxylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Abstract
The invention relates to the field of polymer composite materials and relates to a preparation method of a biomass nanocrystal enhanced type nylon composite material. The preparation method of the biomass nanocrystal enhanced type nylon composite material is characterized by comprising the following steps: firstly, dissolving 15-20 parts by weight of nylon into 50-100 parts by weight of methanoic acid solution at the temperature of 60-100 DEG C; secondly, dispersing 1-10 parts by weight of biomass nanocrystal into 50-100 parts by weight of methanoic acid solution at the temperature of 60-100 DEG C, and carrying out ultrasonic treatment for 5-30 minutes; thirdly, mixing the two solutions obtained in the first step and the second step to obtain a mixed solution, stirring for 10-60 minutes, adding the obtained mixed solution into 120-200 parts by weight of ethanol aqueous solution, and carrying out suction filtration; and fourthly, washing a product obtained after suction filtration is carried out in distilled water at the temperature of 60-100 DEG C, carrying out suction filtration, and drying for 3-24 hours at the temperature of 80-120 DEG C, thus the biomass nanocrystal enhanced type nylon composite material is obtained. Nano fiber and a nylon-6 matrix form a hydrogen bond and interact each other, so that interface interaction effect of the nano fiber and the nylon 6 matrix can be obviously improved, and thermal stability can also be improved.
Description
Technical field
The present invention relates to field of polymer composite material, relate to the preparation method of the brilliant reinforced nylon matrix material of a kind of biomass nano, the brilliant reinforced nylon composite master batch of biomass nano and preparation method thereof.
Background technology
Thermoplas tic resin composite has shaping simple, with short production cycle and the advantage such as can to reuse, and becomes the important branch of matrix material.Polymeric amide is commonly called as nylon, and English name is Polyamide (PA), and be the general name of the thermoplastic resin containing repetition acid amides group-NHCO-on molecular backbone chain, its main products is nylon 6 and nylon66 fiber.Polyamide plastics is the product that in five large general engineering plastic, output is maximum, kind maximum, purposes is the widest.Along with the miniaturization of automobile, the high performance of electronic electric equipment, the light-weighted progress faster of mechanical means, will more Gao Geng great to the demand of nylon.Particularly nylon is as structural material, proposes very high requirement to aspects such as its intensity, thermotolerance, winter hardiness, and properties of nylons can not meet require that of relevant industries development.Now generally improve its mechanical property, dimensional stability, thermotolerance, ageing resistance and fatigue resistance by adding glass fibre.But due to nylon molecules chain existing strong polar group, cause the interfacial interaction of nylon matrix and glass fibre more weak.In addition.The additional proportion of glass fibre is larger, and it is larger to the wearing and tearing of the plasticizing element of injection moulding machine.
If add a kind of strong polar nano fiber in nylon material, interaction of hydrogen bond is formed by nanofiber and nylon matrix, the interfacial interaction of nanofiber and nylon matrix can be significantly improved, not only can improve the mechanical property of nylon matrix, its thermostability can also be improved.Biomass nano crystalline substance is a kind of novel polysaccharide nano-crystalline, there is following advantage in actual use: (1) biomass nano crystalline substance is a kind of natural synthesis polymer, extensively be present in animal, plant, microbe, the wide material sources of material, cheap, renewable; (2) have lower density, compared with conventional inorganic fillers, density and the polymeric matrix of biomass nano crystalline substance are close, excessively can not increase the proportion of material after filling; (3) have stronger rigidity speciality, demonstrate very high strength and modulus, the modulus as Cellulose nanocrystal can reach 145GPa; (5) the brilliant rich surface hydroxyl of biomass nano, amino, kharophen Deng Qiang polarity group, can produce very strong interaction with the nylon molecules chain of strong polarity, significantly improve mechanical property and the dimensional stability of nylon matrix.
Patent CN 1837435B discloses a kind of composite nano-grade silk fiber product, it is the nonwoven fabric be made up of nano-grade silk fibroin/nylon 6 conjugated fibre, conjugated fibre diameter 50-300 nanometer, the weight ratio of natural silk and nylon 6 is between 9: 1 to 1: 9.Its preparation method, first prepares spinning solution, and adopt electrospinning process to obtain nonwoven fabric, then carry out aftertreatment, wherein, the preparation of described spinning solution comprises, and (1) prepares silk fibroin solution, drying and forming-film; The fibroin membrane of acquisition is dissolved in formic acid, obtains regenerated silk solution; (2) nylon 6 slice is dissolved in formic acid, obtains nylon 6 solution; (3) the dissolution homogeneity mixing (1) and (2) obtained, obtains required spinning solution.Utilize solution blended process to prepare spinning solution although described patent discloses, according to processing parameter disclosed in it, the concentration of its nylon solution is obviously on the low side; And further do not process after blend solution, finished product homogeneity will be affected, finally affect overall performance; CN 102383213A discloses a kind of preparation method of ultrahigh molecular weight polyethylene/biomass nanocrystal composite fibers, although described in patent discloses biomass nano crystalline substance and can be compound in polyethylene to strengthen the property, but when being applied in nylon material by biomass nano crystalline substance, the problems such as processing condition and material selection will be overcome; The brilliant reinforced nylon matrix material of current biomass nano, composite master batch and preparation technology rarely have report.
For the deficiencies in the prior art, present inventor, through researchs such as a large amount of component proportions, temperature condition, finally provides the preparation method of a kind of good mechanical performance, the brilliant reinforced nylon matrix material of thermally-stabilised good, high strength, high-modulus, good stability of the dimension biomass nano.
Summary of the invention
Technology of the present invention is dealt with problems and is to overcome the deficiencies in the prior art, provides the preparation method of a kind of good mechanical performance, the brilliant reinforced nylon matrix material of thermally-stabilised good, high strength, high-modulus, good stability of the dimension, low cost biomass nano.
Present invention also offers the brilliant reinforced nylon matrix material of a kind of biomass nano.
Present invention also offers the preparation method of the brilliant reinforced nylon composite master batch of a kind of biomass nano.
Present invention also offers the brilliant reinforced nylon composite master batch of a kind of biomass nano.
A preparation method for the brilliant reinforced nylon matrix material of biomass nano, is characterized in that comprising the following steps:
The first step, 15-20 weight part nylon is dissolved in 50-100 weight part, temperature is in the formic acid solution of 60 DEG C-100 DEG C;
Second step, the biomass nano of 1-10 weight part crystalline substance is scattered in 50-100 weight part, temperature is in the formic acid solution of 60 DEG C-100 DEG C, supersound process 5-30 minute;
3rd step, the two kinds of solution the first step and second step prepared are mixed to get mixing solutions, stir 10-60 minute; Described mixing solutions is joined in the aqueous solution of 120-200 parts by weight of ethanol, suction filtration;
4th step, the product continuation washing, the suction filtration in 60 DEG C of-100 DEG C of distilled water that will obtain after suction filtration, in 80 DEG C of-120 DEG C of dry 3-24 hour, thus obtain the brilliant reinforced nylon matrix material of biomass nano.
The preparation method of the brilliant reinforced nylon matrix material of a kind of biomass nano provided by the invention, can also comprise following technical characteristic:
Wherein, described nylon is nylon 6 or nylon66 fiber.
Wherein, the mass percent of described formic acid solution is 81%-88%.
Wherein, in the 3rd step, the blending means of solution is that limit is toppled over, limit is stirred.
Wherein, described biomass nano crystalline substance is that fibrous biomass nano is brilliant, bacteria cellulose, and described fibrous biomass nano crystalline substance is that Cellulose nanocrystal or chitin are nanocrystalline; Described Cellulose nanocrystal is by acid hydrolyzation or mechanical phonograph recorder separation preparation; Described chitin is nanocrystalline to be prepared by acid hydrolyzation.
Present invention also offers the brilliant reinforced nylon matrix material of a kind of biomass nano, it is characterized in that: comprise nylon, biomass nano is brilliant, the weight part ratio of described biomass nano crystalline substance and described nylon is between 1-10: 15-20.
Present invention also offers the preparation method of the brilliant reinforced nylon composite master batch of a kind of biomass nano, it is characterized in that comprising the following steps:
The first step, to prepare the brilliant reinforced nylon matrix material of biomass nano according to method described above;
Second step, biomass nano brilliant reinforced nylon matrix material 40-60 part prepared by the first step, nylon 50-250 part, the mixing of oxidation inhibitor 0.5-1.5 part, through two/single screw extrusion machine melt blending, extrude, obtained nylon enhancement type composite master batch, processing parameter is: melt temperature is 190 DEG C-220 DEG C, screw speed is 40-60 rev/min.
Wherein, described oxidation inhibitor is any one in antioxidant 1010, antioxidant 1076, antioxidant CA, oxidation inhibitor 164 or anti-oxidant DLTP.
Present invention also offers the brilliant reinforced nylon composite master batch of a kind of biomass nano, it is characterized in that: comprise biomass nano brilliant reinforced nylon matrix material 40-60 part, nylon 50-250 part, oxidation inhibitor 0.5-1.5 part melt blending is extruded; In the brilliant reinforced nylon matrix material of described biomass nano, the weight part ratio of biomass nano crystalline substance and nylon is between 1-10: 15-20.
Wherein, the brilliant reinforced nylon composite master batch of a kind of biomass nano provided by the invention, is further defined to: comprise biomass nano brilliant reinforced nylon matrix material 45-55 part, nylon 100-200 part, oxidation inhibitor 0.5-1.5 part melt blending is extruded; In the brilliant reinforced nylon matrix material of described biomass nano, the weight part ratio of biomass nano crystalline substance and nylon is between 5-10: 15-20.
Enforcement of the present invention comprises following technique effect:
The biomass nano crystalline substance used in the present invention is natural synthetic product, and output is large, renewable, is with a wide range of applications.
The brilliant surface of the biomass nano that the present invention uses is containing a large amount of polar group, interaction of hydrogen bond is formed by nanofiber and nylon matrix, the interfacial interaction of nanofiber and nylon matrix can be significantly improved, not only can improve the mechanical property of nylon matrix, its thermostability can also be improved.。
Mixing solutions after blended joins suction filtration in the aqueous solution of 120-200 parts by weight of ethanol causes the brilliant reinforced nylon matrix material of the biomass nano that obtains to have more excellent homogeneity and easily and liquid separation, the restriction of the condition such as proportioning, strength of solution, temperature of nylon of the present invention, biomass nano crystalline substance make the matrix material that obtains and composite master batch mechanical property more superior; And preparation technology is simple, has very strong market popularization value.
Accompanying drawing explanation
Fig. 1 is the nanocrystalline transmission electron microscope figure of chitin
Fig. 2 is the transmission electron microscope figure of polymkeric substance/chitin nanocrystalline composite material
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is described in detail, it is pointed out that described embodiment is only intended to be convenient to the understanding of the present invention, and any restriction effect is not play to it.
Prepare fibrous biomass nano brilliant, described fibrous biomass nano crystalline substance is that Cellulose nanocrystal or chitin are nanocrystalline; Cellulose nanocrystal is generally by acid hydrolyzation or mechanical phonograph recorder separation preparation; Chitin is nanocrystalline generally to be prepared by acid hydrolyzation; Its preparation method can use following method:
The method preparing Cellulose nanocrystal is: cellulose crystallite is added the sulphuric acid soln that mass content is 40 ~ 60%, wherein the mass ratio of cellulose crystallite and sulphuric acid soln is 4 ~ 10: 100,1 ~ 6h is stirred at 20 ~ 60 DEG C, add deionized water to dilute, obtain the suspension that Cellulose nanocrystal concentration is 10 ~ 15g/L; Suspension is centrifugal, removes supernatant liquor, precipitation is added deionized water and dilutes, obtain the acidic suspension that cellulose crystallite concentration is 20 ~ 40g/L; The acidic suspension obtained is transferred in dialysis tubing, dialyses in deionized water, changed a deionized water every 2 ~ 6 hours, until pH value to 5 ~ 7 of acidic suspension in dialysis tubing; Acidic suspension lyophilize after dialysis, obtains Cellulose nanocrystal;
The method preparing chitin nanocrystalline is: chitin is added the KOH aqueous solution that concentration is 40 ~ 100g/L, and stirring boils boils 6 ~ 40 hours, removes protein, obtains the chitin suspension after deproteinization; Often liter of KOH aqueous solution adds 20 ~ 40g chitin; With the chitin after sodium hypochlorite solution bleaching delignification protein 2 ~ 8 hours at 60 ~ 80 DEG C, clean with deionized water rinsing, it is in the HCl solution of 2 ~ 8mol/L that the chitin after cleaning is added concentration, and stirring boils to boil carries out acidolysis in 1 ~ 4 hour, obtains acid solution; Every gram clean after chitin add 20 ~ 50 milliliters of HCl solution; The acid solution obtained is transferred in dialysis tubing, dialyses in deionized water, changed a deionized water every 2 ~ 6 hours, until pH value to 5 ~ 7 of acid solution in dialysis tubing; Acid solution lyophilize after dialysis, obtains chitin nanocrystalline;
A preparation method for the brilliant reinforced nylon matrix material of biomass nano, comprises the following steps:
The first step, 15-20 weight part nylon 6 or nylon66 fiber are dissolved in 50-100 weight part 60-100 DEG C of concentration is in the formic acid solution of 81-88wt.%; The preferred 83-87wt.% of formic acid solution concentration; Described condition fully can dissolve nylon material;
Second step, by the biomass nano of 1-10 weight part crystalline substance, to be scattered in 50-100 weight part 60-100 DEG C of concentration be in the formic acid solution of 81-88wt.%, supersound process 5-30 minute; The preferred 83-87wt.% of concentration of formic acid solution; After supersound process, described condition can fully disperse biomass nano brilliant;
3rd step, then by the mixing of two kinds of solution, stir 10-60 minute.Above-mentioned mixing solutions limit is toppled over, limit stir join in the aqueous solution of 120-200 part ethanol, suction filtration; The aqueous solution of preferred 140-180 part ethanol;
4th step, the product continuation washing, the suction filtration in 60-100 DEG C of distilled water that will obtain after suction filtration, so repeat 2-5 time, in 80-120 DEG C of dry 3-24 hour, thus obtains brilliant reinforced nylon matrix material (powder) of biomass nano.
Present invention also offers the brilliant reinforced nylon matrix material of a kind of biomass nano, it is characterized in that: comprise nylon, biomass nano is brilliant, the weight part ratio of described biomass nano crystalline substance and described nylon is between 1-10: 15-20; The weight part ratio of the preferred described biomass nano crystalline substance of the present embodiment and described nylon is between 5-10: 15-20.
A preparation method for the brilliant reinforced nylon composite master batch of biomass nano, comprises the following steps:
The first step, to prepare the brilliant reinforced nylon matrix material of biomass nano according to above-mentioned steps;
Second step, above-mentioned biomass nano brilliant reinforced nylon matrix material 40-60 part, nylon 50-250 part, oxidation inhibitor 0.5-1.5 part to be mixed, through twin screw extruder melt blending, extruding pelletization, processing parameter: melt temperature is 190-220 DEG C, screw speed is 50rap/min, thus obtained nylon reinforced nylon 6 or nylon66 fiber composite master batch.Described oxidation inhibitor can be any one in antioxidant 1010, antioxidant 1076, antioxidant CA, oxidation inhibitor 164, anti-oxidant DLTP; Preferred antioxidant 1010.
The brilliant reinforced nylon composite master batch of a kind of biomass nano, is characterized in that: comprise biomass nano brilliant reinforced nylon matrix material 40-50 part, nylon 50-250 part, oxidation inhibitor 0.5-1.5 part melt blending extrude; In the brilliant reinforced nylon matrix material of described biomass nano, the weight part ratio of biomass nano crystalline substance and nylon is between 1-10: 15-20; In the brilliant reinforced nylon matrix material of the preferred described biomass nano of the present embodiment, the weight part ratio of biomass nano crystalline substance and nylon is between 5-10: 15-20.The biomass nano that above-mentioned feature limits brilliant reinforced nylon composite master batch good mechanical performance, thermally-stabilised good, high strength, high-modulus, good stability of the dimension, have market popularization value.
Embodiment 1
20 parts of nylon 6 are dissolved in the formic acid solution of 100 weight parts, 100 DEG C of 81wt.%, nanocrystalline for the chitin of 5 parts (Fig. 1 is its transmission electron microscope figure) are scattered in the formic acid solution of 50 parts of 100 DEG C of 81wt.%, supersound process 10 minutes.Then by two kinds of solution mixing, stir 30 minutes.Above-mentioned mixing solutions solution limit is toppled over, limit stir join in the aqueous solution of 120 parts of ethanol, suction filtration.The product obtained after suction filtration is continued washing, suction filtration in 100 DEG C of distilled water, so repeats 3 times, in 120 DEG C of dryings 24 hours, thus obtain nylon 6/ chitin nano-grained composite powder (Fig. 2 is its transmission electron microscope figure).Above-mentioned nylon 6/ chitin nano-grained composite powder 50 parts, nylon 650 parts, antioxidant 1010 0.5 part are mixed, through twin screw extruder melt blending, extruding pelletization, processing parameter: melt temperature is 190 DEG C, screw speed is 50rap/min, thus the obtained nanocrystalline reinforced nylon 6 composite master batch of chitin.
Embodiment 2
17 parts of nylon66 fiber are dissolved in the formic acid solution of 76 weight parts, 78 DEG C of 85wt.%, are scattered in the formic acid solution of 74 parts of 80 DEG C of 85wt.% by nanocrystalline for the chitin of 8 parts, supersound process 18 minutes.Then by two kinds of solution mixing, stir 10 minutes.Above-mentioned mixing solutions solution limit is toppled over, limit stir join in the aqueous solution of 160 parts of ethanol, suction filtration.The product obtained after suction filtration is continued washing, suction filtration in 80 DEG C of distilled water, so repeats 2 times, in 100 DEG C of dryings 12 hours, thus obtain nylon 6/ chitin nano-grained composite powder.Above-mentioned nylon 6/ chitin nano-grained composite powder 40 parts, nylon66 fiber 150 parts, antioxidant 1010 1.0 parts are mixed, through twin screw extruder melt blending, extruding pelletization, processing parameter: melt temperature is 205 DEG C, screw speed is 40rap/min, thus the obtained nanocrystalline reinforced PA66 composite master batch of chitin.
Embodiment 3
15 parts of nylon 6 are dissolved in the formic acid solution of 50 weight parts, 60 DEG C of 88wt.%, are scattered in the formic acid solution of 100 parts of 60 DEG C of 88wt.% by nanocrystalline for the chitin of 10 parts, supersound process 30 minutes.Then by two kinds of solution mixing, stir 60 minutes.Above-mentioned mixing solutions solution limit is toppled over, limit stir join in the aqueous solution of 200 parts of ethanol, suction filtration.The product obtained after suction filtration is continued washing, suction filtration in 60 DEG C of distilled water, so repeats 5 times, in 80 DEG C of dryings 3 hours, thus obtain nylon 6/ chitin nano-grained composite powder.Above-mentioned nylon 6/ chitin nano-grained composite powder 60 parts, nylon 6250 parts, antioxidant 1010 1.5 parts are mixed, through twin screw extruder melt blending, extruding pelletization, processing parameter: melt temperature is 220 DEG C, screw speed is 60rap/min, thus the obtained nanocrystalline reinforced nylon 6 composite master batch of chitin.
Embodiment 4
20 parts of nylon 6 are dissolved in the formic acid solution of 100 weight parts, 100 DEG C of 81wt.%, the Cellulose nanocrystal of 1 part are scattered in the formic acid solution of 50 parts of 100 DEG C of 81wt.%, supersound process 10 minutes.Then by two kinds of solution mixing, stir 30 minutes.Above-mentioned mixing solutions solution limit is toppled over, limit stir join in the aqueous solution of 120 parts of ethanol, suction filtration.The product obtained after suction filtration is continued washing, suction filtration in 100 DEG C of distilled water, so repeats 3 times, in 120 DEG C of dryings 24 hours, thus obtain nylon 6/ Cellulose nanocrystal composite powder.Above-mentioned nylon 6/ Cellulose nanocrystal composite powder 50 parts, nylon 650 parts, antioxidant 1010 0.5 part are mixed, through twin screw extruder melt blending, extruding pelletization, processing parameter: melt temperature is 190 DEG C, screw speed is 50rap/min, thus obtained Cellulose nanocrystal reinforced nylon 6 composite master batch.
Embodiment 5
15 parts of nylon 6 are dissolved in the formic acid solution of 50 weight parts, 60 DEG C of 83wt.%, the bacteria cellulose of 10 parts are scattered in the formic acid solution of 100 parts of 60 DEG C of 83wt.%, supersound process 30 minutes.Then by two kinds of solution mixing, stir 60 minutes.Above-mentioned mixing solutions solution limit is toppled over, limit stir join in the aqueous solution of 140 parts of ethanol, suction filtration.The product obtained after suction filtration is continued washing, suction filtration in 60 DEG C of distilled water, so repeats 5 times, in 80 DEG C of dryings 3 hours, thus obtain nylon 6/ bacteria cellulose composite powder.Above-mentioned nylon 6/ bacteria cellulose composite powder 60 parts, nylon 6250 parts, antioxidant 1010 1.5 parts are mixed, through twin screw extruder melt blending, extruding pelletization, processing parameter: melt temperature is 220 DEG C, screw speed is 60rap/min, thus obtained bacteria cellulose reinforced nylon 6 composite master batch.
Embodiment 6
17 parts of nylon66 fiber are dissolved in the formic acid solution of 76 weight parts, 78 DEG C of 87wt.%, are scattered in the formic acid solution of 74 parts of 80 DEG C of 87wt.% by nanocrystalline for the chitin of 8 parts, supersound process 18 minutes.Then by two kinds of solution mixing, stir 10 minutes.Above-mentioned mixing solutions solution limit is toppled over, limit stir join in the aqueous solution of 180 parts of ethanol, suction filtration.The product obtained after suction filtration is continued washing, suction filtration in 80 DEG C of distilled water, so repeats 2 times, in 100 DEG C of dryings 12 hours, thus obtain nylon 6/ Cellulose nanocrystal composite powder.Above-mentioned nylon 6/ Cellulose nanocrystal composite powder 40 parts, nylon66 fiber 150 parts, antioxidant 1010 1.0 parts are mixed, through twin screw extruder melt blending, extruding pelletization, processing parameter: melt temperature is 205 DEG C, screw speed is 40rap/min, thus obtained Cellulose nanocrystal reinforced PA66 composite master batch.
The present invention adds a kind of strong polar nano fiber (Fig. 1) in nylon material, interaction of hydrogen bond is formed by nanofiber and nylon matrix, the interfacial interaction of nanofiber and nylon matrix can be significantly improved, not only can improve the mechanical property of nylon matrix, its thermostability can also be improved.Biomass nano crystalline substance is a kind of novel polysaccharide nano-crystalline, there is following advantage in actual use: (1) biomass nano crystalline substance is a kind of natural synthesis polymer, extensively be present in animal, plant, microbe, the wide material sources of material, cheap, renewable; (2) have lower density, compared with conventional inorganic fillers, density and the polymeric matrix of biomass nano crystalline substance are close, excessively can not increase the proportion (Fig. 2) of material after filling; (3) have stronger rigidity speciality, demonstrate very high strength and modulus, the modulus as Cellulose nanocrystal can reach 145GPa; (5) the brilliant rich surface hydroxyl of biomass nano, amino, kharophen Deng Qiang polarity group, can produce very strong interaction with the nylon molecules chain of strong polarity, significantly improve mechanical property and the dimensional stability of nylon matrix.
Finally should be noted that; above embodiment is only in order to illustrate technical scheme of the present invention; but not limiting the scope of the invention; although done to explain to the present invention with reference to preferred embodiment; those of ordinary skill in the art is to be understood that; can modify to technical scheme of the present invention or equivalent replacement, and not depart from essence and the scope of technical solution of the present invention.
Claims (10)
1. a preparation method for the brilliant reinforced nylon matrix material of biomass nano, is characterized in that comprising the following steps:
The first step, 15-20 weight part nylon is dissolved in 50-100 weight part, temperature is in the formic acid solution of 60 DEG C-100 DEG C;
Second step, the biomass nano of 1-10 weight part crystalline substance is scattered in 50-100 weight part, temperature is in the formic acid solution of 60 DEG C-100 DEG C, supersound process 5-30 minute;
3rd step, the two kinds of solution the first step and second step prepared are mixed to get mixing solutions, stir 10-60 minute; Described mixing solutions is joined in the aqueous solution of 120-200 parts by weight of ethanol, suction filtration;
4th step, the product continuation washing, the suction filtration in 60 DEG C of-100 DEG C of distilled water that will obtain after suction filtration, in 80 DEG C of-120 DEG C of dry 3-24 hour, thus obtain the brilliant reinforced nylon matrix material of biomass nano.
2. the preparation method of the brilliant reinforced nylon matrix material of a kind of biomass nano according to claim 1, is characterized in that: described nylon is nylon 6 or nylon66 fiber.
3. the preparation method of the brilliant reinforced nylon matrix material of a kind of biomass nano according to claim 1, is characterized in that: the mass percent of described formic acid solution is 81%-88%.
4. the preparation method of the brilliant reinforced nylon matrix material of a kind of biomass nano according to claim 1,2 or 3, is characterized in that: in the 3rd step, the blending means of solution is that limit is toppled over, limit is stirred.
5. the preparation method of the brilliant reinforced nylon matrix material of a kind of biomass nano according to claim 1,2 or 3, it is characterized in that: described biomass nano crystalline substance is for fibrous biomass nano is brilliant, bacteria cellulose, and described fibrous biomass nano crystalline substance is that Cellulose nanocrystal or chitin are nanocrystalline; Described Cellulose nanocrystal is by acid hydrolyzation or mechanical phonograph recorder separation preparation; Described chitin is nanocrystalline to be prepared by acid hydrolyzation.
6. the brilliant reinforced nylon matrix material of biomass nano, it is characterized in that: comprise nylon, biomass nano is brilliant, the weight part ratio of described biomass nano crystalline substance and described nylon is between 1-10: 15-20.
7. a preparation method for the brilliant reinforced nylon composite master batch of biomass nano, is characterized in that comprising the following steps:
The first step, prepare the brilliant reinforced nylon matrix material of biomass nano according to the arbitrary described method of claim 1-5;
Second step, biomass nano brilliant reinforced nylon matrix material 40-60 part prepared by the first step, nylon 50-250 part, the mixing of oxidation inhibitor 0.5-1.5 part, through two/single screw extrusion machine melt blending, extrude, obtained nylon enhancement type composite master batch, processing parameter is: melt temperature is 190 DEG C-220 DEG C, and screw speed is 40-60 rev/min.
8. the preparation method of the brilliant reinforced nylon composite master batch of a kind of biomass nano according to claim 7, is characterized in that: described oxidation inhibitor is any one in antioxidant 1010, antioxidant 1076, antioxidant CA, oxidation inhibitor 164 or anti-oxidant DLTP.
9. the brilliant reinforced nylon composite master batch of biomass nano, is characterized in that: comprise biomass nano brilliant reinforced nylon matrix material 40-60 part, nylon 50-250 part, oxidation inhibitor 0.5-1.5 part melt blending is extruded; In the brilliant reinforced nylon matrix material of described biomass nano, the weight part ratio of biomass nano crystalline substance and nylon is between 1-10: 15-20.
10. the brilliant reinforced nylon composite master batch of a kind of biomass nano according to claim 9, is characterized in that: comprise biomass nano brilliant reinforced nylon matrix material 45-55 part, nylon 100-200 part, oxidation inhibitor 0.5-1.5 part melt blending is extruded; In the brilliant reinforced nylon matrix material of described biomass nano, the weight part ratio of biomass nano crystalline substance and nylon is between 5-10: 15-20.
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| CN109736672A (en) * | 2018-12-29 | 2019-05-10 | 商秋(上海)新材料科技有限公司 | A kind of ultra-silent energy-saving slab bridge window |
| CN115894987A (en) * | 2022-11-22 | 2023-04-04 | 湖北洋田塑料制品有限公司 | Preparation method of nano-cellulose whisker reinforced nylon composite material |
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