CN110129917A - A kind of antibacterial starch base melt spinning resin and its application - Google Patents
A kind of antibacterial starch base melt spinning resin and its application Download PDFInfo
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- CN110129917A CN110129917A CN201910368090.2A CN201910368090A CN110129917A CN 110129917 A CN110129917 A CN 110129917A CN 201910368090 A CN201910368090 A CN 201910368090A CN 110129917 A CN110129917 A CN 110129917A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/10—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained by reactions only involving carbon-to-carbon unsaturated bonds as constituent
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/18—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from other substances
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Artificial Filaments (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The present invention relates to a kind of antibacterial starch base melt spinning resin and its application, each ingredient and parts by weight are as follows: 15-65 parts of starch, 35-85 parts of PVA, 20-45 parts of plasticiser, 1.0-2.5 parts of decomposing inhibitor, 0.5-5 parts of fluorine carbon activity agent, 1.0-10 parts of processing aid, 0.1-5 parts of graphene dispersing solution.The present invention is modified starch-based resin system, graphene dispersing solution is added, it is dispersed in starch-based resin with making graphene uniform, effectively improve its initial pyrolyzation temperature, improve melt index, inhibit small molecule plasticizers migration, the starch base melt spinning resin of acquisition has good anti-microbial property, antibacterial starch-based fiber is prepared by melt spinning method with it, contain finely dispersed nano-graphene in the antibacterial starch-based fiber of acquisition, it can be combined well with starch-based resin, to assign starch-based fiber good antibiotic property.
Description
Technical field
The invention belongs to polymeric material fields, and in particular to a kind of antibacterial starch base melt spinning resin and its application.
Background technique
In recent years, with the improvement of people's environmental awareness, solving because of white pollution caused by after common plastics package waste,
It is extremely urgent to research and develop biodegradable packaging material.Circular regeneration of the starch plastics due to its fully bio-degradable and raw material
Property receives significant attention, if it is possible to realize that its melt spinning process, application range will greatly be extended.It is related at present to form sediment
The compound system of powder base resin and starch and PVA carries out melt spinning and has not been reported.
PVA (polyvinyl alcohol) due to good biological degradability, it is current solve because of plastic product it is discarded after caused by
White pollution in terms of have broad application prospects.But compared with other macromolecule resin materials, since PVA resin can not be into
Row melt spinning, so significantly limiting its application range.
Chinese patent CN102776597 is related to a kind of high strength high modulus polyvinyl alcohol fiber and its melt spinning method, can be with
Melting extrusion, but PVA powder makees plasticizer with water, adds polyalcohol, substantially still falls within solwution method spinning, only made with water
For solvent, and produce because of the low boiling point of water and unstable.Currently, being referred in the prior art using polyalcohol and oligomer
It is modified, but with a large amount of water as solvent, and it is not described the origin of polyalcohol and oligomer, it can not judge that its is practical
Property.
Starch-based resin and fiber are also brought be easy by harmful bacteria in actual use due to natural biological degradability
The problem of pollution, so starch-based resin of the research and development with antibiotic property has greatly realistic meaning.
Summary of the invention
The purpose of the present invention is to provide a kind of antibacterial starch base melt spinning resin and its applications, by starch/PVA
System is modified, and widens its fusing point and decomposition point distance, improves its melt index, makes its initial pyrolyzation temperature >=265 DEG C,
Melt index reaches 5-40g/10min (test condition: 210 DEG C, 5.0Kg), assigns starch-based resin and the good antibacterial of fiber
Property.
In order to achieve the above object, the invention provides the following technical scheme:
A kind of antibacterial starch base melt spinning resin, each ingredient and parts by weight are as follows: 15-65 parts of starch, PVA 35-85
Part, 20-45 parts of plasticiser, 1.0-2.5 parts of decomposing inhibitor, 0.5-5 parts of fluorine carbon activity agent, 1.0-10 parts of processing aid, graphite
0.1-5 parts of alkene dispersion liquid.
Wherein, the plasticiser is compound system comprising by propylene oxide, polyglycereol or PEG100-20000, season penta
Tetrol, 1-4 butanediol, diethylene glycol (DEG), in trimethylolpropane three kinds or more and deionized water addition reaction product, the addition is anti-
Product is answered to be compounded with glycerol, polyglycereol or PEG100-20000；Wherein, addition reaction temperature is 60~85 DEG C, when reaction
Between be 1.5-6 hours, addition reaction product is no less than 10 parts when compounding.
Further, the starch in cornstarch, tapioca, potato starch and modified starch at least one
Kind, fineness >=300 mesh of starch, wherein modified starch is acetate starch, oxidized starch or acetylated starch.
Further, the alcoholysis degree 85%-100% of the PVA, degree of polymerization 500-3000, average molecular weight 65000-
85000, volatile matter≤5%, sodium acetate≤2.8, ash content≤1.0, pH value 6.5-7.0, partial size 80-500 mesh.
Also, the PVA that the PVA is 500-800 by the degree of polymerization is compounded with the PVA that the degree of polymerization is 1200-2000, the two
Weight ratio be the degree of polymerization be 500-800 PVA: the degree of polymerization be 1200-2000 PVA=1:2-2.5.
Preferably, the decomposing inhibitor is selected from 1- butyl -3- methyl miaow Cuo tetrafluoroborate, 1- vinyl -3- ethyl
Miaow Cuo borate, 1- ethoxy -3- methyl miaow Cuo tetrafluoroborate, 1- butyl -3- methyl miaow Cuo villaumite, 1- vinyl 3- ethyl
Miaow Cuo smelling salts, dodecyl sulfobetaine, graphene, graphene oxide and rutile/anatase TiO2In at least one
Kind.
Further, 1- butyl -3- methyl miaow Cuo tetrafluoroborate in the decomposing inhibitor: 1- butyl -3- methyl miaow Cuo
Villaumite=1-2:1, weight ratio, the compounding of the two can effectively improve initial pyrolyzation temperature, while can also be effectively
Reduce the water imbibition of PVA.
Also, the fluorine carbon activity agent in Du Pont FSO-100, Du Pont FS-31 and Noah's ark chemistry AC-702 at least one
Kind.
Further, the processing aid be lubricant, antioxidant, flow improver additive and heat stabilizer at least two kinds with
On.
Also, the heat stabilizer is zinc stearate, calcium stearate, magnesium stearate or methyl methacrylate；The antioxygen
Agent is antioxidant 1010, irgasfos 168, antioxidant 300, antioxidant 330, a variety of mixtures in TNP；The lubricant or stream
Dynamic promotor is selected from least one of oleamide, erucyl amide, stearic amide.
Further, the preparation method of the graphene dispersing solution is the silane coupling agent hydrating solution for taking 0.5-3%, will
Graphene powder, which is added, carries out ultrasonic wave dispersion, obtains the graphene dispersing solution of graphene content 5-15%, wherein the graphite
The size of alkene powder is long and wide less than 200 microns, and thickness is less than 10 nanometers.
Antibacterial starch base melt spinning resin of the present invention is used to prepare non-woven fabrics.
The present invention passes through the mutual synergistic effect of the above plasticiser, decomposing inhibitor and graphene, can be effectively
Starch-based resin initial pyrolyzation temperature is improved, melt index is improved, the small molecule solvent (decomposing inhibitor) of introducing can seep
It is thoroughly intermolecular to PVA, its Van der Waals force is destroyed, spin-drawing rate is improved.
In plasticiser of the invention, using addition low molecular weight glycerol and high molecular weight polyglycereol (polyglycereol 10/9/8/7/
6/5/4//3) or PEG (PEG100-20000 etc.) is compounded, to reduce appearance effects caused by small molecule plasticizers migration.
In antibacterial starch base melt spinning resin of the present invention, compounded using high polymerization degree with the PVA of low polymerization degree, effectively
Improve melt-processed mobility；Graphene is added in formula, realizes starch base tree using the natural bacteriostatic of graphene
The antibiotic property of rouge and fiber improves the initial pyrolyzation temperature and fiber of starch-based resin provide antibiotic property while
Intensity.
Compared with prior art, the invention has the following beneficial effects:
The present invention successfully realizes that the fusion plastification of starch-based resin squeezes out by adding PVA system to be modified starch,
Melt index reaches 5-40g/10min (test condition: 210 DEG C, 5.0Kg), temperature of initial decomposition >=265 DEG C, processing temperature 120
℃-240℃；With completely biodegradable, degradability will not be influenced because of modified generation crosslinking due to.
Antibacterial starch-based fiber is prepared by melt spinning method using antibacterial starch base melt spinning resin of the invention,
Contain finely dispersed nano-graphene in the antibacterial starch-based fiber of acquisition, can be combined well with starch-based resin, thus
The good antibiotic property of starch-based fiber is assigned, solvent or coagulating bath are not used, the energy, and three-waste free discharge is saved, there is work
Skill is simple, and equipment investment is few, and occupied area is small, the advantage of low production cost.
Specific embodiment
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1
By 10 parts of pentaerythrite, 15 parts of 1,4-butanediol, 10 parts of diethylene glycol (DEG), PEG2000/5 parts, 25 parts of deionized water, point
It is not added in reaction kettle and stirs evenly, be added dropwise with 30 parts of propylene oxide, and 0.02 part of phosphoric acid catalyst is added and carries out addition
Reaction, revolving speed are 80~100 revs/min, and mixing time is 100~120 minutes, and temperature is 60~85 DEG C, obtain addition reaction
Product one.
By 20 parts of 400 mesh cornstarch, 10 parts of PVA0599,30 parts of PVA1299, one 20 parts of addition reaction product, the third three
5 parts of alcohol, 5 parts of polyglycereol, 5 parts of deionized water, 2.0 parts of tetrafluoroborate of methyl miaow Cuo of 1- butyl -3-, dodecyl sulfobetaines
1.0 parts of alkali, anatase titanium dioxide TiO22.0 parts, 0.45 part of zinc stearate, 1.0 parts of oleamide, Du Pont FSO-100/1.5 parts, antioxygen
1010/0.4 part of agent, antioxidant 300/0.5 part, SiO20.2 part, 0.5 part of graphene dispersing solution, mixed at high speed is put into respectively
It in machine, heats while stirring, plasticising is given under 40 DEG C -120 DEG C/40min state, place 24 hours, then put into pelletizer and make
Grain, obtains starch base melt spinning resin.
Graphene powder is added and carries out ultrasonic wave dispersion, obtains graphene and contain by the silane coupling agent hydrating solution for taking 1%
The graphene dispersing solution of amount 10%, wherein the size of the graphene powder is long and wide less than 200 microns, and thickness is less than 10
Nanometer.
Examination spinning, 120 DEG C of melt processing temperature-are carried out on single unit spinning machine with obtained starch base melt spinning resin
240 DEG C, spinneret extruded velocity 0.5-1.0m/min, 3-6 times of drafting multiple, the results are shown in Table 1.
Embodiment 2
By 25 parts of an acetoglyceride, two 25 parts of acetoglycerides, 15 parts of glycerine, gather sweet by 20 parts of triacetyl glycerine
15 parts of oil, which is separately added into reaction kettle, to stir evenly, and 0.02 part of phosphoric acid catalyst is added and carries out addition reaction, revolving speed is 80~100
Rev/min, mixing time is 100~120 minutes, and temperature is 60~85 DEG C, obtains addition reaction product two.
By 20 parts of 450 mesh tapioca, 20 parts of PVA0899 20 parts of .PVA1799,2 25 parts of addition reaction product, the third three
5 parts of alcohol, polyethylene glycol-800/5 part, 5 parts of deionized water, 1- butyl -3- methyl miaow Cuo villaumite, 1.5 parts, dodecyl sulfo group sweet tea
1.0 parts of dish alkali, 0.05 part of smelling salts of ethyl miaow Cuo of 1- vinyl 3-, anatase titanium dioxide TiO22.0 parts, 0.45 part of zinc stearate, resolve acyl
1.5 parts of amine, 1.5 parts of Du Pont FS-31,0.6 part of antioxidant 1010,0.3 part of antioxidant 300, SiO20.5 part, graphene dispersion
It 1.0 parts of liquid, puts into high-speed mixer, heats while stirring respectively, give plasticising under 40 DEG C -120 DEG C/40min state, put
It sets 24 hours, then puts into pelletizer and be granulated, obtain starch base melt spinning resin.
Examination spinning is carried out on single unit spinning machine with the resin, 120 DEG C -240 DEG C of melt processing temperature, spinneret extruded velocity
0.5-1.0m/min, 3-6 times of drafting multiple, the results are shown in Table 1.
Embodiment 3
By 30 parts of 600 mesh potato starch, 15 parts of PVA0599,15 parts of PVA2099, the addition reaction product of embodiment 2
2 30 parts, 5 parts of glycerine, 5 parts of polyethylene glycol 2000,5 parts of deionized water, 1- butyl -3- methyl miaow Cuo tetrafluoroborate 1.5
Part, 1.5 parts of villaumite of methyl miaow Cuo of 1- butyl -3-, 1.0 parts of dodecyl sulfobetaine, anatase titanium dioxide TiO22.0 parts, 1- ethylene
0.1 part of smelling salts of ethyl miaow Cuo of base 3-, 0.45 part of zinc stearate, 1.0 parts of oleamide, 1.5 parts of Du Pont FSO-100, antioxidant
1010 0.6 parts, 0.3 part of antioxidant 300, SiO20.5 part, 3.0 parts of graphene dispersing solution, high-speed mixer is put into respectively
In, it heats while stirring, plasticising is given under 40 DEG C -120 DEG C/40min state, place 24 hours, then put into pelletizer and be granulated,
Obtain starch base melt spinning resin.
Examination spinning is carried out on single unit spinning machine with the resin, 120 DEG C -240 DEG C of melt processing temperature, spinneret extruded velocity
0.5-1.0m/min, 3-6 times of drafting multiple, the results are shown in Table 1.
Embodiment 4
By 20 parts of 800 mesh cornstarch, 10 parts of PVA0588,30 parts of PVA2088, the addition reaction product one of embodiment 1
30 parts, 5 parts of glycerine, 5 parts of Macrogol 6000,1.5 parts of tetrafluoroborate of methyl miaow Cuo of 1- butyl -3-, 1- butyl -3- first
1.5 parts of villaumite of base miaow Cuo, 1.5 parts of dodecyl sulfobetaine, 0.1 part of smelling salts of ethyl miaow Cuo of 1- vinyl 3-, anatase titanium dioxide
TiO22.0 parts, 0.45 part of zinc stearate, 1.0 parts of oleamide, Du Pont FSO-100/1.5 parts, antioxidant 1010/0.6 part resists
300 0.3 parts of oxygen agent, SiO20.5 part, 5.0 parts of graphene dispersing solution, put into high-speed mixer respectively, while stirring plus
Heat gives plasticising under 40 DEG C -120 DEG C/40min state, places 24 hours, then put into pelletizer and be granulated, and it is molten to obtain starch base
Melt spinning resin.
Examination spinning is carried out on single unit spinning machine with the resin, 120 DEG C -240 DEG C of melt processing temperature, spinneret extruded velocity
0.5-1.0m/min, 3-6 times of drafting multiple, the results are shown in Table 1, wherein anti-microbial property test is according to national standard GB/T
20944.3-2008 is carried out, and is tested to the bacteriostasis rates of Escherichia coli (8099), 210 DEG C of melt index test condition, 5.0Kg.
Table 1
Claims (10)
1. a kind of antibacterial starch base melt spinning resin, each ingredient and parts by weight are as follows: 15-65 parts of starch, PVA35-85 parts, modeling
20-45 parts of agent, 1.0-2.5 parts of decomposing inhibitor, 0.5-5 parts of fluorine carbon activity agent, 1.0-10 parts of processing aid, graphene dispersion
0.1-5 parts of liquid；
Wherein, the plasticiser be compound system comprising by propylene oxide, polyglycereol or PEG100-20000, pentaerythrite,
1-4 butanediol, diethylene glycol (DEG), in trimethylolpropane three kinds or more and deionized water addition reaction product, which produces
Object is compounded with glycerol, polyglycereol or PEG100-20000；Wherein, addition reaction temperature is 60~85 DEG C, and the reaction time is
1.5-6 hours, addition reaction product was no less than 10 parts when compounding.
2. antibacterial starch base melt spinning resin according to claim 1, which is characterized in that the starch forms sediment selected from corn
At least one of powder, tapioca, potato starch and modified starch, wherein the fineness of starch >=300 mesh, the modification
Starch is acetate starch, oxidized starch or acetylated starch.
3. antibacterial starch base melt spinning resin according to claim 1, which is characterized in that the alcoholysis degree 85%- of the PVA
100%, degree of polymerization 500-3000, average molecular weight 65000-85000, volatile matter≤5%, sodium acetate≤2.8, ash content≤1.0,
PH value 6.5-7.0, partial size 80-500 mesh.
4. antibacterial starch base melt spinning resin according to claim 1 or claim 2, which is characterized in that the PVA is by the degree of polymerization
The PVA of 500-800 is compounded with the PVA that the degree of polymerization is 1200-3000, and the weight ratio of the two is that the degree of polymerization is 500-800's
PVA: the degree of polymerization is the PVA=1:2-2.5 of 1200-3000.
5. antibacterial starch base melt spinning resin according to claim 1, which is characterized in that the fluorine carbon activity agent is selected from Du
At least one of nation FSO-100, Du Pont FS-31 and Noah's ark chemistry AC-702.
6. antibacterial starch base melt spinning resin according to claim 1, which is characterized in that the decomposing inhibitor is selected from 1-
Butyl -3- methyl miaow Cuo tetrafluoroborate, 1- vinyl -3- ethyl miaow Cuo borate, 1- ethoxy -3- methyl miaow Cuo tetrafluoro boron
Hydrochlorate, 1- butyl -3- methyl miaow Cuo villaumite, 1- vinyl 3- ethyl miaow Cuo smelling salts, dodecyl sulfobetaine, graphene,
Graphene oxide and rutile-type or anatase titanium dioxide TiO2At least one of.
7. antibacterial starch base melt spinning resin according to claim 1, which is characterized in that the processing aid is lubrication
At least two or more in agent, antioxidant, flow improver additive and heat stabilizer.
8. antibacterial starch base melt spinning resin according to claim 7, which is characterized in that the lubricant or flowing promote
Agent is selected from least one of oleamide, erucyl amide, stearic amide；The heat stabilizer is selected from zinc stearate, tristearin
At least one of sour calcium, magnesium stearate and methyl methacrylate；The antioxidant is antioxidant 1010, irgasfos 168, resists
Oxygen agent 300, antioxidant 330, a variety of mixtures in TNP.
9. antibacterial starch base melt spinning resin according to claim 1, which is characterized in that the system of the graphene dispersing solution
Preparation Method is the silane coupling agent hydrating solution for taking 0.5-3%, and graphene powder is added and carries out ultrasonic wave dispersion, obtains stone
The graphene dispersing solution of black alkene content 5-15%, wherein the size of the graphene powder is long and wide less than 200 microns, thickness
Degree is less than 10 nanometers.
10. antibacterial starch base melt spinning resin is preparing the application in non-woven fabrics as described in claim any one of 1-9.
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| CN110863264A (en) * | 2019-10-13 | 2020-03-06 | 浙江理工大学 | Preparation method of degradable superfine fiber based tea packaging material |
| CN112358655A (en) * | 2020-11-09 | 2021-02-12 | 绍兴兆丽新材料科技有限公司 | Environment-friendly medicine packaging material and preparation method thereof |
| CN112457535A (en) * | 2020-11-30 | 2021-03-09 | 绍兴兆丽新材料科技有限公司 | Environment-friendly spicy cabbage packaging bag and preparation method thereof |
| CN115141432A (en) * | 2022-07-11 | 2022-10-04 | 浙江科技学院 | Antibacterial starch and preparation method thereof |
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| CN115141432B (en) * | 2022-07-11 | 2023-06-30 | 浙江科技学院 | Antibacterial starch and preparation method thereof |
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Application publication date: 20190816 |