CN104805521B - Preparation method of polyester fiber with antibacterial function - Google Patents
Preparation method of polyester fiber with antibacterial function Download PDFInfo
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- CN104805521B CN104805521B CN201510085957.5A CN201510085957A CN104805521B CN 104805521 B CN104805521 B CN 104805521B CN 201510085957 A CN201510085957 A CN 201510085957A CN 104805521 B CN104805521 B CN 104805521B
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Abstract
The invention provides a preparation method of polyester fiber with an antibacterial function. The preparation method specifically comprises steps as follows: (1) preparation of isocyanate-modified negative-ion powder: 100 parts of negative-ion powder are added to a container and stirred and heated to the temperature of 120 DEG C for 30-60 min, then 1-5 parts of isocyanate are added while high-speed stirring, the mixture reacts continuously at the temperature of 100-120 DEG C for 30-60 min, and the isocyanate-modified negative-ion powder is obtained for use; (2) preparation of the polyester fiber: 100 parts of PTA, 40-60 parts of ethylene glycol and 0.2-2 parts of a compound titanium catalyst are added to an esterification kettle and evenly stirred, the mixture firstly reacts at the esterification temperature of 200-230 DEG C for 30-60 min and is continuously heated to the temperature of 250-260 DEG C for a reaction for 30-60 min, then 1-5 parts of the isocyanate-modified negative-ion powder are added, the mixture reacts at the vacuum degree of 30-100 Pa for 4-5 h until the acid value is smaller than 0.5 mgKOH/g, polyester resin is obtained, and the polyester fiber is obtained through spinning. The polyester fiber has the permanent antibacterial function.
Description
Technical field
The invention belongs to textile field is and in particular to a kind of preparation method of the polyester fiber with antibacterial functions.
Background technology
Polyethylene terephthalate (pet, hereinafter referred to as polyester) and products thereof since the advent of the world, because it has
The favor of multiple good characteristics, extremely people.Over nearly 10 years, because polyester is all very fast in the development of fiber and non-fibre field,
Demand expanding day, therefore, worldwide, the production of polyester of especially Asia develops rapidly, and also promotes simultaneously
With the growth driving polyester vertical industry, polyester is made to become the big kind of one of synthetic material.
The polyester fiber of industrial mass production is made with polyethylene terephthalate, China's trade name
Terylene.Terylene have excellent crease resistance, elasticity and dimensional stability, fast light wear-resisting, not mould do not eat into, can pure weaving make,
Therefore can be widely used in spinning with the natural fibers such as cotton, hair, silk, fiber crops and other chemical fibres with arbitrary proportion blended union
Weaver's industry, is the important source material manufacturing the fabrics such as clothes, bedding, interior decoration, carpet.But terylene and natural fiber simultaneously
Compare and exist the shortcoming that moisture content is low, poor air permeability, easily stains, easily send different after especially absorbing the perspiration that human body is discharged
Taste, breed bacteria, are considered as a kind of material of non-health environmental protection for a long time always.With scientific and technical development and people
Growth in the living standard, is modified to the polyester textile fiber being worn, so as to have antibacterial and deodouring effect, lifting its fabric
Comfortableness and feature, become textile material development an important topic.
The fabric on the market at present with antibacterial and deodouring function is mainly realized by adsorbing addition type antibacterial
, such as patent 201110261719.7 reports a kind of processing method of permanent seal cooling antibacterial and deodouring fabric, the method be by
Nanometer grade inorganic antibacterial agent is added in high polymer powder with 3%-30% weight ratio, and mix homogeneously is formed by screw rod granulating technique
Antibacterial matrices.Antibacterial matrices are mixed with high polymer with the ratio of 0.3%-10%, spinning, after spinning and weaving formed fabric,
Again through antibacterial Final finishing, using the fabric of the method processing of this invention, there is strong excellent of good anti-bacterial effect, persistency
Point.Patent 201110325322.x reports a kind of polyethylene terephthalate antibacterial composite material and its preparation work
Skill, this composite is made up of the component of following parts by weight: 62～72 parts of polyethylene terephthalate, natural organic anti-
15～25 parts of microbial inoculum, 5～15 parts of inorganic antiseptic, 1～3 part of lubricant, 0.5～1.5 part of antioxidant.This invention also includes described
The preparation technology of polyethylene terephthalate antibacterial composite material, the polyethylene terephthalate antibacterial of this invention
Property composite, good anti-bacterial effect, it is easy to processing, low cost of manufacture, can be used for making mineral water bottle, beer bottle and fruit drink
Bottle etc.；Preparation process is simple, is suitable to industrialized production.The common feature of above patent is that antibacterial is added directly into polyester tree
In fat.
In recent years, anion powder is paid close attention to by people as a kind of new inorganic material with specific function, ion
Composition in powder body be characterized with boracic aluminum, sodium, ferrum, the silicate material of lithium circulus, there is pyroelectricity and piezoelectricity
Property, affected the anion that can discharge by environment, and combined to form negative oxygen ion with the oxygen molecule of in the air, it is had very
High activity, has very strong redox, can destroy the cell membrane of antibacterial or the activity of cellular plasm organized enzyme, thus
Reach the purpose of antibiotic and sterilizing.Meanwhile, the substantial amounts of cyclic metabolism for human body for the presence of anion, anti-ageing of scientific investigations showed that
Always, prevention disease has great positive role.Therefore, anion powder is increasing as healthy, efficient additive
It is applied in textile fabric.As patent cn200910054876.3, " a kind of anion technology prepares all-cotton functional home textile fiber face
Material method and its application in home textile product ", patent cn200910054874.4 " a kind of preparing silk by anion technology
Method and its application in home textile product " etc..The same with the first two patent, anion powder is simply filled in polymer by them
In, the As time goes on increase with washing times, can gradually weaken and finally lose its antibacterial and deodouring function.Only will bear
Ion powder organically combines in fiber molecule chain, the textile fabric forever with antibacterial and deodouring function could be obtained, among these
Key technology be how anion powder to be organically introduced in polyester molecule chain.
Due to the hydrophilic on anion breeze surface, it is poor with the compatibility being polymerized macromole to cause it, so needing to add
Enter surface modifier and carry out modified negative-ion breeze, to improve the compatibility of anion breeze and polyester fiber so as to can be smooth
The molecular structure being attached to polyester fiber in.In similar patent cn200710190594.7, rainbow is contained in Wujiang City, Jiangsu Province
Group Co., Ltd discloses " weaving of negative-ion fiber ", be just anion powder, coupling agent, dispersant by formula ratio with
Polyester fiber body mixes, and obtains the modified dacron fabric of anion by twin-screw extrusion, stretching, then spinning, wherein
Coupling agent used is silane coupler, that is, so-called surface modifier.This patent passes through surface modifier to anion
Breeze is modified reaching the purpose improving anion breeze and the polyester compatibility, but anion breeze is also simply by intermolecular
Active force is combined with polymer macromolecule, is not introduced in strand, easily comes off from polymer surfaces, and can be certain
The mechanical property of material is affected on degree.
In order to anion breeze and polyester molecule are formed organic whole it is ensured that when filling anion breeze polyester fine
The mechanical property of dimension keeps constant, and we utilize the hydroxyl on anion breeze surface, are allowed to react with isocyanates, thus being formed
The isocyano of anion breeze molecular end, in grafting, the anion powder of isocyano can be used as chain extender and end-capping reagent
Participate in the synthetic reaction of polyester, thus anion breeze is organically combined in polyester fiber strand, and improve poly- further
The elasticity of ester fiber.
Content of the invention
It is an object of the invention to provide a kind of polyester fiber preparation method containing anion breeze, the technical side of the present invention
The technical scheme that case is taken is as follows:
1st, the preparation of isocyanate-modified anion powder
Add 100 parts of anion powder in a reservoir, stirring is warming up to 120 DEG C of maintenance 30-60min, after in high-speed stirred
The isocyanates of lower addition 1-5 part, obtain final product isocyanate-modified bearing at a temperature of 100-120 DEG C after continuing reaction 30-60min
Ion powder, standby.
2nd, the preparation of polyester fiber
100 parts of the ethylene glycol of pta, 40-60 part, the compound Titanium series catalyst of 0.2-2 part is added in reaction kettle of the esterification,
First at 200-230 DEG C of esterification temperature, react 30-60min after stirring, be continuously heating to 250-260 DEG C of pressure reaction 30-
60min, the isocyanate-modified anion powder being subsequently adding 1-5 part reacts 4-5h under vacuum 30-100pa, until acid
Value obtains polyester resin less than 0.5mgkoh/g, then obtains polyester fiber through spinning.
Compound Titanium series catalyst of the present invention is the titanium/Si oxide copolymer of hydrolysis, wherein ti/si atom
Than for 9: 1.
Isocyanates of the present invention are methyl diphenylene diisocyanate (mdi), XDI
(xdi), PPDI (ppdi), naphthalene -1,5- diisocyanate (ndi) one or more.
Present invention has the advantage that
Anion powder is organically combined in polyester molecule chain, makes product have permanent antibacterial functions, process letter
Single, economically feasible, wide market.
Specific embodiment
The following is several specific embodiments of the present invention, further illustrate the present invention, but the present invention is not limited only to this.
Embodiment 1
1st, the preparation of the modified anion powder of methyl diphenylene diisocyanate (mdi)
Add 100 parts of anion powder in a reservoir, stirring is warming up to 120 DEG C of maintenance 30min, after under high velocity agitation plus
Enter 1 part of methyl diphenylene diisocyanate (mdi), after continuing reaction 30min at a temperature of 100 DEG C, obtain final product diphenyl methane two
The modified anion powder of isocyanates (mdi), standby.
2nd, the preparation of polyester fiber
The pta of 100 parts of addition, 40 parts of ethylene glycol, the titanium/Si oxide of 0.2 part of hydrolysis in reaction kettle of the esterification
Copolymer (ti/si atomic ratio be 9: 1), first reacts 30min at 200 DEG C of esterification temperature after stirring, is continuously heating to 250
DEG C reaction 30min, is subsequently adding the modified anion powder of 1 part of methyl diphenylene diisocyanate (mdi) in vacuum 30pa
Lower reaction 4h, until acid number obtains polyester resin less than 0.5mgkoh/g, then obtains polyester fiber through spinning.
Embodiment 2
1st, the preparation of the modified anion powder of XDI (xdi)
Add 100 parts of anion powder in a reservoir, stirring is warming up to 120 DEG C of maintenance 50min, after under high velocity agitation plus
Enter 3 parts of XDI (xdi), after continuing reaction 50min at a temperature of 110 DEG C, obtain final product phenylenedimethylidyne two
The modified anion powder of isocyanates (xdi), standby.
2nd, the preparation of polyester fiber
In reaction kettle of the esterification add 100 parts pta, 50 parts of ethylene glycol, 1 part of hydrolysis titanium/Si oxide common
Polymers (ti/si atomic ratio be 9: 1), first reacts 50min at 220 DEG C of esterification temperature after stirring, is continuously heating to 250
DEG C reaction 50min, is subsequently adding the modified anion powder of 3 parts of XDI (xdi) in vacuum 70pa
Lower reaction 4h, until acid number obtains polyester resin less than 0.5mgkoh/g, then obtains polyester fiber through spinning.
Embodiment 3
1st, the preparation of the modified anion powder of PPDI (ppdi)
Add 100 parts of anion powder in a reservoir, stirring is warming up to 120 DEG C of maintenance 60min, after under high velocity agitation plus
Enter 5 parts of PPDI (ppdi), after continuing reaction 60min at a temperature of 120 DEG C, obtain final product PPDI
(ppdi) the modified anion powder of i, standby.
2nd, the preparation of polyester fiber
In reaction kettle of the esterification add 100 parts pta, 60 parts of ethylene glycol, 2 parts of hydrolysis titanium/Si oxide common
Polymers (ti/si atomic ratio be 9: 1), first reacts 60min at 230 DEG C of esterification temperature after stirring, is continuously heating to 260
DEG C reaction 60min, is subsequently adding the modified anion powder of 5 parts of PPDI (ppdi) anti-under vacuum 100pa
Answer 5h, until acid number obtains polyester resin less than 0.5mgkoh/g, then obtain polyester fiber through spinning.
Claims (3)
1. a kind of preparation method of the polyester fiber with antibacterial functions is it is characterised in that the present invention's comprises the concrete steps that: (1) is different
The preparation of cyanate modified anion powder, adds 100 parts of anion powder in a reservoir, and stirring is warming up to 120 DEG C of maintenance 30-
60min, after add the isocyanates of 1-5 part under high velocity agitation, continue at a temperature of 100-120 DEG C after reaction 30-60min i.e.
Isocyanate-modified anion powder, standby, the preparation of (2) polyester fiber, add in reaction kettle of the esterification 100 parts pta,
The ethylene glycol of 40-60 part, the compound Titanium series catalyst of 0.2-2 part, first react after stirring at 200-230 DEG C of esterification temperature
30-60min, is continuously heating to 250-260 DEG C of reaction 30-60min, is subsequently adding the isocyanate-modified anion of 1-5 part
Powder reacts 4-5h under vacuum 30-100pa, until acid number obtains polyester resin less than 0.5mgkoh/g, then obtains polyester through spinning
Fiber.
2. a kind of preparation method of the polyester fiber with antibacterial functions according to claim 1 is it is characterised in that described
Compound Titanium series catalyst be hydrolysis titanium/Si oxide copolymer, wherein ti/si atomic ratio be 9: 1.
3. a kind of preparation method of the polyester fiber with antibacterial functions according to claim 1 is it is characterised in that described
Isocyanates be methyl diphenylene diisocyanate (mdi), XDI (xdi), to benzene two Carbimide.
Ester (ppdi), naphthalene -1,5- diisocyanate (ndi) one or more.
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| CN201510085957.5A CN104805521B (en) | 2015-02-23 | 2015-02-23 | Preparation method of polyester fiber with antibacterial function |
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| CN105524260B (en) * | 2015-12-01 | 2017-12-22 | 东华大学 | The method that situ aggregation method prepares the anti-biotic material based on cupric oxide/cuprous oxide |
| CN115594855A (en) * | 2021-06-28 | 2023-01-13 | 中国石油化工股份有限公司（Cn） | Photochromic polyester, polyester fiber and preparation method |
| CN114990888A (en) * | 2022-06-10 | 2022-09-02 | 王应剑 | Easily-cleaned antibacterial negative ion mattress and preparation method thereof |
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| JP2013053244A (en) * | 2011-09-05 | 2013-03-21 | Unitika Ltd | Polyamide resin composition, and molding made by molding the same |
| CN104098759B (en) * | 2013-04-12 | 2017-06-27 | 中国石油化工股份有限公司 | Preparation method for manufacturing mould lower shrinkage type industrial yarn polyester high |
| CN103772673A (en) * | 2013-06-13 | 2014-05-07 | 淄博晓光化工材料有限公司 | Method for synthesizing PET polyester chips by using titanium catalyst |
| CN103755932B (en) * | 2013-12-21 | 2016-03-09 | 安徽神剑新材料股份有限公司 | A kind of preparation method of crystallized polyurethane resin and the application on powder coating thereof |
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| CN104264268A (en) * | 2014-09-18 | 2015-01-07 | 海安县华荣化纤有限公司 | Anti-neutron radiation polyester fiber preparation method |
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