CN110437461A - A kind of oxygen bleaching one-bath finishing technique of anion-modified hyperbranched silicone - Google Patents
A kind of oxygen bleaching one-bath finishing technique of anion-modified hyperbranched silicone Download PDFInfo
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- CN110437461A CN110437461A CN201910708834.0A CN201910708834A CN110437461A CN 110437461 A CN110437461 A CN 110437461A CN 201910708834 A CN201910708834 A CN 201910708834A CN 110437461 A CN110437461 A CN 110437461A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
- C08G83/002—Dendritic macromolecules
- C08G83/005—Hyperbranched macromolecules
- C08G83/006—After treatment of hyperbranched macromolecules
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06L—DRY-CLEANING, WASHING OR BLEACHING FIBRES, FILAMENTS, THREADS, YARNS, FABRICS, FEATHERS OR MADE-UP FIBROUS GOODS; BLEACHING LEATHER OR FURS
- D06L1/00—Dry-cleaning or washing fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods
- D06L1/12—Dry-cleaning or washing fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods using aqueous solvents
- D06L1/14—De-sizing
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06L—DRY-CLEANING, WASHING OR BLEACHING FIBRES, FILAMENTS, THREADS, YARNS, FABRICS, FEATHERS OR MADE-UP FIBROUS GOODS; BLEACHING LEATHER OR FURS
- D06L4/00—Bleaching fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods; Bleaching leather or furs
- D06L4/10—Bleaching fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods; Bleaching leather or furs using agents which develop oxygen
- D06L4/12—Bleaching fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods; Bleaching leather or furs using agents which develop oxygen combined with specific additives
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06L—DRY-CLEANING, WASHING OR BLEACHING FIBRES, FILAMENTS, THREADS, YARNS, FABRICS, FEATHERS OR MADE-UP FIBROUS GOODS; BLEACHING LEATHER OR FURS
- D06L4/00—Bleaching fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods; Bleaching leather or furs
- D06L4/10—Bleaching fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods; Bleaching leather or furs using agents which develop oxygen
- D06L4/13—Bleaching fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods; Bleaching leather or furs using agents which develop oxygen using inorganic agents
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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
- D06M11/32—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 oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—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 oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/38—Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic System
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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
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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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
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2387/00—Characterised by the use of unspecified macromolecular compounds, obtained otherwise than by polymerisation reactions only involving unsaturated carbon-to-carbon bonds
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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
- 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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- 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
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/50—Modified hand or grip properties; Softening compositions
Abstract
The invention discloses a kind of oxygen bleaching one-bath finishing techniques of anion-modified hyperbranched silicone, and self-emulsifying, anion-modified hyperbranched silicone softening agent and the oxygen bleaching of synthesis, anion-modified hyperbranched silicone including anion-modified hyperbranched silicone are the same as bath.Anion-modified hyperbranched silicone is added in bleaching in the present invention, observes the stability for the treatment of fluid and the whiteness of fabric, pliability, capillary effect, ultimate strength and H by the variation of the amount of addition organosilicon2O2The variation of resolution ratio.To which the influence of anion-modified hyperbranched silicone is added in fabric oxygen bleaching for analysis.
Description
Technical field
The invention belongs to fabric bleaching fields, and in particular to a kind of oxygen bleaching of anion-modified hyperbranched silicone is whole with bathing
Science and engineering skill.
Background technique
Cotton fiber has natural flexibility due to containing oily wax, but by desizing, kiering, bleaching, etc. after techniques,
Due to the place to go of oily wax and the damage of fiber, cotton fabric can become coarse, therefore usually need to be added in afterfinish soft
Soft dose of progress soft treatment.And anion-modified hyperbranched silicone softening agent is added in bleaching process can be in fabric bleaching
During obtain soft effect simultaneously.Process flow is shortened in this measure, reduces the energy consumption in production and worker
Labor intensity.
Hyperbranched silicone has the good performance that dissaving structure and silicone-based polymers have.With big
The features such as molecular structure, melting viscosity is low, polyfunctional group, easily prepared.These features make to have in dyeing wide
Application prospect.Hyperbranched silicone contains a large amount of end moieties, can by its end group carry out functional modification, thus
Functional form polymer is prepared, then fabric is handled again.That is we can be a large amount of by introducing in fabric surface
Functional groups, come reach assign the specific function of fabric requirement.
Anion-modified hyperbranched silicone be it is carried out on the basis of synthesis of super branched organosilicon it is anion-modified
To synthesize a kind of novel finishing agent.It is with high reactivity excellent that this novel finishing agent is not only provided with hyperbranched silicone
Point, it also achieves the functionalization of hyperbranched silicone softening agent.Experiment shows that anion-modified organic silicone finishing agent is one
Kind can be in the finishing agent used in dye bath.It can avoid fabric from being worn so that generating folding in textile dyeing
Wrinkle, scratch etc. defects and influence fabric property.It can also impart to the effect of soft fabric as softening agent.What this project was inquired into
It is then influence of the anion-modified hyperbranched silicone in fabric oxygen bleaching with bath.
For at present, the development and application of Hyperbranched Organo-silicon Polymer have been achieved with some no small achievements.Over-expense has
The development of organosilicon polymer also causes more and more to pay close attention to synthesis.At home, the Wang Zhong of Dalian University of Technology is just equal uses
The hyperbranched polyol polyester of one-step synthesis method fluoroalkyl sealing end；Wang Shengjie et al. design has synthesized two kinds of A2 monomers and has passed through
A2-B2Or A2-B3Monomer, which has synthesized method, thinks new hyperbranched organosilicon polymer.
At abroad, since soft comfortable of the people to clothing is more demanding, so the consumption market of softening agent is more wide.
Compared to the country, hyperbranched silicone softening agent is more early in development abroad and research.Although domestic study starting evening to this,
The domestic research to hyperbranched silicone macromolecular was also just in accelerated development in recent years.
Hyperbranched silicone is added in cotton fabric oxygen bleaching by the present invention can assign fabric softness.Come from process flow
It says, general fabrics bleaching is to separate with soft finish.And addition hyperbranched silicone softening agent can be in fabric in oxygen bleaching
Soft effect is obtained while bleaching.This measure shortens process flow, reduces the energy loss in textile finishing processes.In
When factory process, the labor intensity of worker can be reduced, improves production efficiency.
Summary of the invention
Goal of the invention: in order to solve the deficiencies in the prior art, the present invention provides a kind of anion-modified hyperbranched organic
The oxygen bleaching one-bath finishing technique of silicon.
Technical solution: a kind of synthesis technology of anion-modified hyperbranched silicone includes the following steps:
The four-hole boiling flask of thermometer, reflux condensate device, drying is formed into a reaction unit, then in dry four-hole boiling flask
Then middle addition hyperbranched silicone and isopropanol start that sodium chloroacetate solution is added dropwise, control the dropwise addition of temperature and sodium chloroacetate
Speed carries out graft reaction, synthetic anionic modified ultra-branching organosilicon.
A kind of synthesis technology preparation of anion-modified hyperbranched silicone according to it is anion-modified hyperbranched
The self-emulsifying technique of organosilicon, includes the following steps:
By electric mixer, four-hole boiling flask, constant pressure funnel be connected composition one easy emulsifier unit, then by yin from
The ratio of sub- modified ultra-branching organosilicon and distilled water is 3:7, and distilled water is first poured into four mouthfuls of beakers, then will be anion-modified
Hyperbranched silicone pours into constant pressure funnel, opens electric mixer, and the switch of constant pressure funnel is unscrewed, anion is made
Modified ultra-branching organosilicon slowly instills four-hole boiling flask, drips off beginning timing to anion-modified hyperbranched silicone, stirring
40min completes the self-emulsifying of anion-modified hyperbranched silicone.
A kind of synthesis technology preparation of anion-modified hyperbranched silicone according to it is anion-modified hyperbranched
Organosilicon and oxygen bleaching one-bath finishing technique, the process flow of the soft softening one-bath of oxygen bleaching are as follows: fabric → enzyme desizing → alkaline scouring → oxygen bleaching
Soft softening one-bath；Concrete operations therein are as follows:
A. enzyme desizing:
Process flow is as follows: enzyme desizing prescription is first added, is warming up to 55-60 DEG C, fabric is then added and is handled, the time is handled
For 60min, then cool down, cold water is washed, and hot water wash is dried；
Enzyme desizing prescription is as follows: desizing enzyme 3.0-5.0g/L；NaCl 5.0g/L；JFC 1.0g/L；Bath raio is 20:1；Treatment fluid
After preparing by bath raio, need to be added suitable CH3COONa adjusts pH=6-7；
B. alkaline scouring:
Process flow is as follows: alkaline scouring prescription and fabric being added at 50 DEG C, is warming up to 100 DEG C, is handled, the processing time is
Then 120min cools down, hot water wash, cold water is washed；
Alkaline scouring prescription is as follows: NaOH 30.0g/L；Refining agent 4.0g/L；Bleeding agent 2.0g/L；Bath raio 20:1；
After fabric kiering, need to be detected with phenolphthalein solution until cloth cover does not redden (not aobvious alkalinity), knitting after being detected with phenolphthalein
Object is answered squezzing, is dried for standby；
C. the soft softening one-bath of oxygen bleaching:
Process flow is as follows: the fabric of bleaching process prescription and wetting being added at 50 DEG C, is warming up to 100 DEG C, is handled, locates
The reason time is 60min, is then cooled down, bleaching post-processing；
Bleaching process prescription is as follows: 30%H2O2 5.0g/L；Hydrogen peroxide bleaching stabilizer 1.0g/L；Anion-modified hyperbranched silicone 0-
10.0%(o.w.f)；Appropriate 1%NaOH；Bath raio is 20:1；After treatment fluid is prepared by bath raio, needs to be added suitable NaOH and adjust
pH=10-11；
It cleans after matched solution and bleaching during this and must all use distilled water；It to be stirred in due course in bleaching, supplement is steamed
Distilled water is to maintain bath raio.It should also be noted that fabric cannot be made to leak out liquid level for a long time in this process；Fabric bleaching is complete, takes out,
Wash with distilled water until not reddened with phenolphthalein solution detection fabric surface.
The utility model has the advantages that anion-modified hyperbranched silicone is added in bleaching in the present invention, by the amount that organosilicon is added
Variation to observe the stability for the treatment of fluid and the whiteness of fabric, pliability, capillary effect, ultimate strength and H2O2The change of resolution ratio
Change.To which the influence of anion-modified hyperbranched silicone is added in fabric oxygen bleaching for analysis.
The present invention is inquired by the way that anion-modified hyperbranched silicone is added in the technique of fabric oxygen bleaching as softening agent
The influence when finishing agent is to fabric bleaching, the conclusion that obtains are as follows:
(1) influence to the soft softening one-bath of oxygen bleaching: anion-modified hyperbranched silicone, which is added, will not be such that bleaching liquid is layered, but
It is the increase with its concentration, bleaching liquid will appear muddy phenomenon.
(2) influence to textile finishing performance: when finishing agent concentration is 10%o.w.f, fabric can obtain optimal soft
Softness；When finishing agent concentration is 4%o.w.f, fabric whiteness is best.Hereafter with the increase of finishing agent concentration, whiteness decline.
When finishing agent concentration is 6%o.w.f, wetting property of the fabric is most strong.But it when finishing agent concentration is greater than this concentration, knits
Object wetability, which declines capillary effect, to be reduced；When finishing agent concentration is 4%o.w.f, the maximum intensity of fiber, the breaking strength of fabric is most
Greatly.After this, as finishing agent concentration increases, fabric breaking strength is gradually reduced；To H2O2The influence of resolution ratio: AMHTPOS
H can be alleviated to a certain extent2O2Decomposition, the whiteness of fabric can be improved.
(3) anion-modified organosilicon is added in fabric bleaching can make fabric obtain soft effect, shorten work
Skill process.
Detailed description of the invention
Influence schematic diagram of the finishing agent concentration to whiteness in Fig. 1 present invention；
Influence schematic diagram of the finishing agent concentration to bending stiffness and pliability in Fig. 2 present invention；
Influence schematic diagram of the finishing agent concentration to capillary effect in Fig. 3 present invention；
Influence schematic diagram of the finishing agent concentration to ultimate strength in Fig. 4 present invention；
Fig. 5 Central Plains treatment fluid of the present invention and addition 4%o.w.f finishing agent H2O2Resolution ratio constitutional diagram；
Original cloth and the anion-modified hyperbranched silicone sample cloth infrared spectroscopy constitutional diagram of 10%o.w.f in Fig. 6 present invention.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, so that the technology of this field
Personnel can better understand advantages and features of the invention, to make apparent boundary to protection scope of the present invention
It is fixed.Embodiment described in the invention is only a part of the embodiment of the present invention, instead of all the embodiments, based on the present invention
In embodiment, those of ordinary skill in the art's every other implementation obtained without making creative work
Example, shall fall within the protection scope of the present invention.
Embodiment
1. a kind of oxygen bleaching one-bath finishing technique of anion-modified hyperbranched silicone
1.1 synthetic anionic modified ultra-branching organosilicons
The four-hole boiling flask of thermometer, reflux condensate device, drying is formed into a reaction unit, then in dry four-hole boiling flask
Then middle addition hyperbranched silicone (referred to as HTPOS) and isopropanol start that sodium chloroacetate solution is added dropwise, control temperature and chlorine
The rate of addition of sodium acetate carries out graft reaction, synthetic anionic modified ultra-branching organosilicon.
The anion-modified hyperbranched silicone (Anion modified hyper branched silicone) of synthesis
Referred to as AMHTPOS.
The self-emulsifying of 1.2 synthetic anionic modified ultra-branching organosilicons
The advantages of AMHTPOS first is that do not have to be added emulsifier can realize self-emulsifying.
Self-emulsifying step are as follows: electric mixer, four-hole boiling flask, constant pressure funnel are connected and form an easy cream
Makeup is set, and is then 3:7 in the ratio of anion-modified hyperbranched silicone and distilled water, distilled water is first poured into four mouthfuls of burnings
Then anion-modified hyperbranched silicone is poured into constant pressure funnel by cup, electric mixer is opened, constant pressure funnel
Switch unscrewing, so that anion-modified hyperbranched silicone is slowly instilled four-hole boiling flask, to anion-modified hyperbranched organic
The complete beginning timing of silica drop stirs 40min, completes the self-emulsifying of anion-modified hyperbranched silicone.
1.3 anion-modified hyperbranched silicone softening agents and oxygen bleaching are the same as bath
A kind of synthesis technology preparation of anion-modified hyperbranched silicone according to it is anion-modified hyperbranched organic
Silicon and oxygen bleaching one-bath finishing technique, the process flow of the soft softening one-bath of oxygen bleaching are as follows: fabric → enzyme desizing → alkaline scouring → oxygen bleaching is soft
With bath；Concrete operations therein are as follows:
A. enzyme desizing:
Process flow is as follows: enzyme desizing prescription is first added, is warming up to 55-60 DEG C, fabric is then added and is handled, the time is handled
For 60min, then cool down, cold water is washed, and hot water wash is dried；
Enzyme desizing prescription is as follows: desizing enzyme 3.0-5.0g/L；NaCl 5.0g/L；JFC 1.0g/L；Bath raio is 20:1；Treatment fluid
After preparing by bath raio, need to be added suitable CH3COONa adjusts pH=6-7；
B. alkaline scouring:
Process flow is as follows: alkaline scouring prescription and fabric being added at 50 DEG C, is warming up to 100 DEG C, is handled, the processing time is
Then 120min cools down, hot water wash, cold water is washed；
Alkaline scouring prescription is as follows: NaOH 30.0g/L；Refining agent 4.0g/L；Bleeding agent 2.0g/L；Bath raio 20:1；
After fabric kiering, need to be detected with phenolphthalein solution until cloth cover does not redden (not aobvious alkalinity), knitting after being detected with phenolphthalein
Object is answered squezzing, is dried for standby；
C. the soft softening one-bath of oxygen bleaching:
Process flow is as follows: the fabric of bleaching process prescription and wetting being added at 50 DEG C, is warming up to 100 DEG C, is handled, locates
The reason time is 60min, is then cooled down, bleaching post-processing；
Bleaching process prescription is as follows: 30%H2O2 5.0g/L；Hydrogen peroxide bleaching stabilizer 1.0g/L；Anion-modified hyperbranched silicone 0-
10.0%(o.w.f)；Appropriate 1%NaOH；Bath raio is 20:1；After treatment fluid is prepared by bath raio, needs to be added suitable NaOH and adjust
pH=10-11；
It bleaches soft softening one-bath experiment and is divided into 6 groups, wherein one group is added without AMHTPOS, remaining five groups are separately added into 2.0%
The softening agent of o.w.f, 4.0%o.w.f, 6.0%o.w.f, 8.0%o.w.f, 10.0%o.w.f.
It cleans after matched solution and bleaching during this and must all use distilled water；It to stir, mend in due course in bleaching
Distilled water is filled to maintain bath raio.It should also be noted that fabric cannot be made to leak out liquid level for a long time in this process；Fabric bleaching is complete, takes
Out, wash with distilled water until not reddened with phenolphthalein solution detection fabric surface.
2. performance and test
2.1 oxygen bleaching softnesses are tested with bath performance
Unsorted dose for the treatment of fluid and the treatment fluid that various concentration finishing agent is added are stood for 24 hours, observe whether its solution is deposited
Phenomena such as being layered.
2.2 whiteness
The present invention is using the intellectual digital whiteness instrument test fabric whiteness of WSB-3A.Fabric to be tested is folded 4 layers, after folding
Fabric area cannot be less than the area of measurement window.Folded fabric is placed on whiteness test instrument and tests, and tests 3 times, takes
Average value.
2.3 flexibility
Test method:
(1) instrument test: the present invention uses the bending stiffness of FAST-2 style instrument test fabric.Fabric after arrangement is cut into
The sample specification of 5cm × 13cm, in the smooth measurement plane for being placed on style instrument, fabric leading portion and indicator light will be spaced 1cm's
Distance.Then pressure plare, which is covered fabric, slowly pushes pressure plare to move forward, when sample fabric is in cantilever-shaped and is bent downwardly
When with 45 ° of contact of incline plane, the sample length that sample fabric stretches out level table, this length, that is, bending length L are at this moment recorded.Bending
Rigidity Calculation formula are as follows: B=9.18 × 10-8WL3(cNcm2/ cm).Wherein the B in formula is bending stiffness (cNcm2/ cm), W
For sample mass area ratio (g/cm2), L is bending length cm.
(2) artificial grading: using 5 people grading method.Cloth specimen order after arrangement is upset into discharge.5 classmates are touched with hand
Then every piece of cloth specimen experiences its softness.Best pliability is 5 grades, and untrimmed fabric is 1 grade.
2.4 capillary effect
Test method: cloth specimen is clipped on glass bar with clip, then glass bar is fixed on iron stand.Away from sample lower section
One centimeters draw the starting point that a line rises as liquid along broadwise.Start to count when the liquid wetting in ceramic whiteware disk is to graduation mark
When.The height that liquid level rises along cloth cover is recorded after 30min.Three groups of numbers are taken, average height is calculated.
2.5 ultimate strength
Test method: YG065H electronic fabric strength tester test fabric ultimate strength is used.By fabric sample be cut into 30cm ×
5.5cm.It is noted that being along through to cutting cloth specimen.Open strength tester display switch and computer.Collet is adjusted by uplink, downlink
Between spacing.Select strength test software parallel machine on computer.It places cloth specimen and stretches until cloth specimen is broken, then record is disconnected
Split strength.
2.6 infrared spectroscopy
Test method: this project is knitted using the Fourier infrared spectrograph of model FTIR-7600 to by AMHTPOS processing
Object carries out qualitative analysis.
2.7 H2O2Resolution ratio
Test method: KMnO4 Titration.
Titration principle are as follows: 2KMnO4+5H2O2+3H2SO4=2MnSO4+K2SO4+5O2+8H2O
The treatment fluid that 5mLAM is 4%o.w.f is pipetted with pipette, is placed in the conical flask of 250mL, is added 10mL6mol/L's
H2SO4, with 0.1 mol/LKMnO after shaking up4Titrate HTPOS.It is terminal that solution, which is dropped to colour-fast within blush and 30s,.
Write down consumption KMnO4Volume, parallel drop are averaged three times.
Calculation method: H2O2Concentration=；
H2O2Resolution ratio=。
3 results and discussion
The dosage of 3.1 AMHTPOS is to oxygen bleaching with the influence of bath
After the treatment fluid placement for 24 hours of AMHTPOS is added, treatment fluid is observed.It was found that treatment fluid is not layered.But as HMTPOS is dense
The increase of degree, treatment fluid is in muddy shape, and has floating floccule in liquid.And the treatment fluid of softening agent is not added, then it presents clear
Clear shape has no that floating is cotton-shaped in liquid.This explanation, AMHTPOS, which is added, in bleaching will not destroy treatment fluid stability.Analyze it
Reason may be that dendroid is presented in the structure of silicon modified organic polymer, be not completely soluble in water.So when it is stirred so
After standing afterwards, a part being not completely soluble in water is just floated in treatment fluid with cotton-shaped.
AMHTPOS can't change the process conditions of bleaching as a kind of soft additive.So determining 30%H2O2It is dense
Degree is 5.0g/L, and the concentration of hydrogen peroxide bleaching stabilizer is 1.0g/L, and temperature is 100 DEG C, time 60min, and bath raio is the bleaching work of 20:1
Under the conditions of skill, when investigating dosage difference, the dosage of AMHTPOS is inquired into fabric bending stiffness, whiteness, capillary effect, ultimate strength
It influences.As a result such as table 1.
Influence of the different finishing agent concentration of table 1 to the soft softening one-bath of oxygen bleaching
The influence of 3.2 pairs of whiteness
In 30%H2O2Concentration is 5.0g/L, and hydrogen peroxide bleaching stabilizer concentration is 1.0g/L, osmotic agent concentration 1.0g/L, time 1h,
Temperature is 100 DEG C, and under conditions of bath raio is 20:1, influence result such as Fig. 1 finishing agent of the finishing agent of various concentration to whiteness is dense
Spend the influence schematic diagram to whiteness.
We can be clearly seen that from Fig. 1, when the concentration of anion-modified hyperbranched silicone increases, fabric
Whiteness also becomes larger.But after its concentration increases to 4%o.w.f, fabric whiteness, which is affected by, to be gradually reduced.Analysis
Its reason may be when the concentration of finishing agent gradually increases, and contained amino also gradually increases.In anion-modified organosilicon
Side chain on contain primary amino group and secondary amino group, altogether there are three reactive hydrogen atom on the two amino, these three active hydrogens easily occur
It aoxidizes and forms chromophore, this diamine structure has the synergistic effect for accelerating its oxidation, and fabric is made to be easy yellowing.So working as
When the concentration of anion-modified hyperbranched silicone is greater than 4%o.w.f, the whiteness of fabric can because increasing for amino content and by
To influence.Therefore in production application, it should find one between finishing agent amino content and fabric yellowing degree and most preferably put down
Weighing apparatus point.
The influence of 3.3 pairs of pliabilitys
In 30%H2O2Concentration is 5.0g/L, and hydrogen peroxide bleaching stabilizer concentration is 1.0g/L, osmotic agent concentration 1.0g/L, time 1h,
Temperature is 100 DEG C, under conditions of bath raio is 20:1, influence result of the finishing agent of various concentration to pliability such as Fig. 2 finishing agent
Influence schematic diagram of the concentration to bending stiffness and pliability.
As shown in Figure 2 when the dosage of anion-modified hyperbranched silicone increases from 0 ~ 10%o.w.f, the bending of fabric
Rigidity is gradually reduced, that is to say, that the pliability of fabric is gradually increased.The structure of this and anion-modified hyperbranched silicone has
It closes.Because of hyperbranched silicone (HTPOS-NH2) structure be dendroid, and be the characteristics of dendritic structure with mobility and
Film forming.This feature can make softening agent come in the drawout of fabric surface more evenly.And silicone softening agent is attached to and knits
When object surface, it can form the macromolecule membrane of one layer of reticular structure between fiber.It thus can be to avoid fabric and yarn
Directly contacting between line, between fiber and fiber, can also reduce its coefficient of friction.It is special in external force that fiber is allowed in this way
Opposite slide to generate smoothing effect can occur in the case where small.So easily deformation occurs and generates soft hand for fabric
Sense.Therefore, know that, when the concentration of anion-modified hyperbranched silicone is gradually increased, the feel of fabric is better by Fig. 2, that is
Soft result of the fabric is also better.
The influence of 3.4 pairs of capillary effects
In 30%H2O2Concentration is 5.0g/L, and hydrogen peroxide bleaching stabilizer concentration is 1.0g/L, osmotic agent concentration 1.0g/L, time 1h,
Temperature is 100 DEG C, and under conditions of bath raio is 20:1, influence result such as Fig. 3 finishing agent of the finishing agent of various concentration to capillary effect is dense
Spend the influence schematic diagram to capillary effect.
The data of Fig. 3 show, when the concentration of anion-modified hyperbranched silicone is 6%o.w.f, the hair of fabric at this time
Imitate best, the wetability of fabric is best.When the concentration of finishing agent is more than 6%o.w.f, the wettability of fabric is gradually decreased, hair
Effect is reduced.Due to containing more hydrophilic radical in finishing agent, so fabric hydrophilic increases in the enhancing of finishing agent dosage
By force, the wetted performance enhancement of fiber, water absorption of fabrics enhancing, capillary effect increase.It, may when finishing agent concentration is more than 6%o.w.f
It is because finishing agent excessively affects the removal of cotton fiber surface wax, so that water absorption of fabrics reduces, capillary effect is reduced.
The influence of 3.5 pairs of ultimate strengths
In 30%H2O2Concentration is 5.0g/L, and hydrogen peroxide bleaching stabilizer concentration is 1.0g/L, osmotic agent concentration 1.0g/L, time 1h,
Temperature is 100 DEG C, and under conditions of bath raio is 20:1, the influence result such as Fig. 4 of the finishing agent of various concentration to ultimate strength is arranged
Influence schematic diagram of the agent concentration to ultimate strength.
As the fracture mechanism of cotton fabric it is found that the fracture of fiber must be as caused by molecule chain break.It is negative when being added
When ion modification hyperbranched silicone, the covalent bond in basic structural unit and finishing agent between fiber can generate covalent friendship
Connection.Therefore the case where limited space between each basic structural unit, mobility reduce, and fabric bears external force can be uneven,
The decline of fibre strength is caused, so that fabric breaking strength declines.By being learnt in table, when the concentration of finishing agent reaches 4%o.w.f
When, the breaking strength of fabric is optimal at this time.When to analyze its reason may be that AMHTPOS is arranged to fabric surface at this time, shape
At one layer of dendroid film, play the role of certain strength protection to fabric in fabric tension.When more than 4%o.w.f, fabric
Breaking strength can decline, it may be possible to since excessive finishing agent makes the limitation of activity between each basic unit of fiber, move
Dynamic space reduces.So fiber is when stretching, the pulling force by very little is just broken.So, it is contemplated that the fracture of fabric
Intensity, the dosage of finishing agent is no more than 4%o.w.f.
3.6 couples of H2O2The influence of resolution ratio
In 30%H2O2Concentration is 5.0g/L, and hydrogen peroxide bleaching stabilizer concentration is 1.0g/L, under conditions of osmotic agent concentration is 1.0g/L,
Wherein 4%o.w.f is added in one group for the treatment of fluid, and two groups for the treatment of fluids are placed 0.5,1.0,1.5,2.0,2.5, survey its H respectively2O2Point
Solution rate, as a result such as Fig. 5 original treatment fluid and addition 4%o.w.f finishing agent H2O2Resolution ratio constitutional diagram.
As shown in Figure 5, in H2O2Concentration under the same conditions, with the variation of time, H in original cloth and sample cloth2O2Point
Solution rate is gradually increased.This is because H in treatment fluid2O2It is gradually decomposing, decomposition principle are as follows: H2O2 → H++HO2 -.Same
The resolution ratio of time, the resolution ratio ratio 4%o.w.f sample cloth of original cloth are much bigger.Analyze addition when its reason may be oxygen bleaching
AMHTPOS forms one layer of dendroid film in fabric surface, and the H of attachment on the fabric is effectively protected2O2.Make its resolution ratio
It reduces.Between 0 ~ 0.5 h, it can be seen that either original cloth or sample cloth H2O2Resolution ratio accelerate.Analysis is likely to be
The NaOH and H played regulatory role in treatment fluid2O2Reaction, accelerates H2O2Decomposition.So the resolution ratio of time period is accelerated.
3.7 infrared spectrum analysis
Infrared light is carried out to the original cloth without soft treatment and the sample cloth that the anion-modified hyperbranched silicone of 10%o.w.f is added
Spectrum analysis, as a result such as Fig. 6 original cloth and the anion-modified hyperbranched silicone sample cloth infrared spectroscopy constitutional diagram of 10%o.w.f.By Fig. 6
As can be seen that the difference between the infrared absorption spectrum of two kinds of cloth specimens is as follows: at 1000-1050cm-1, ether (C-O-C's) stretches
Intensity, position and the shape difference of contracting vibration absorption peak；At 3250-3400cm-1, inspection information can where there is-OH suctions
Peak is received, there is-OH on cotton fiber.Due to not using pressed disc method, but its infrared spectrogram directly is surveyed with fabric, so not
Detect-NH2Stretching vibration absworption peak.
The present invention is inquired by the way that anion-modified hyperbranched silicone is added in the technique of fabric oxygen bleaching as softening agent
The influence when finishing agent is to fabric bleaching, the conclusion that obtains are as follows:
(1) influence to the soft softening one-bath of oxygen bleaching: anion-modified hyperbranched silicone, which is added, will not be such that bleaching liquid is layered, but
It is the increase with its concentration, bleaching liquid will appear muddy phenomenon.
(2) influence to textile finishing performance: when finishing agent concentration is 10%o.w.f, fabric can obtain optimal soft
Softness；When finishing agent concentration is 4%o.w.f, fabric whiteness is best.Hereafter with the increase of finishing agent concentration, whiteness decline.
When finishing agent concentration is 6%o.w.f, wetting property of the fabric is most strong.But it when finishing agent concentration is greater than this concentration, knits
Object wetability, which declines capillary effect, to be reduced；When finishing agent concentration is 4%o.w.f, the maximum intensity of fiber, the breaking strength of fabric is most
Greatly.After this, as finishing agent concentration increases, fabric breaking strength is gradually reduced；To H2O2The influence of resolution ratio: AMHTPOS
H can be alleviated to a certain extent2O2Decomposition, the whiteness of fabric can be improved.
(3) anion-modified organosilicon is added in fabric bleaching can make fabric obtain soft effect, shorten work
Skill process.
Claims (3)
1. a kind of synthesis technology of anion-modified hyperbranched silicone, characterized by the following steps:
The four-hole boiling flask of thermometer, reflux condensate device, drying is formed into a reaction unit, then in dry four-hole boiling flask
Then middle addition hyperbranched silicone and isopropanol start that sodium chloroacetate solution is added dropwise, control the dropwise addition of temperature and sodium chloroacetate
Speed carries out graft reaction, synthetic anionic modified ultra-branching organosilicon.
2. a kind of synthesis technology preparation of anion-modified hyperbranched silicone according to claim 1 is anion-modified
The self-emulsifying technique of hyperbranched silicone, characterized by the following steps:
By electric mixer, four-hole boiling flask, constant pressure funnel be connected composition one easy emulsifier unit, then by yin from
The ratio of sub- modified ultra-branching organosilicon and distilled water is 3:7, and distilled water is first poured into four mouthfuls of beakers, then will be anion-modified
Hyperbranched silicone pours into constant pressure funnel, opens electric mixer, and the switch of constant pressure funnel is unscrewed, anion is made
Modified ultra-branching organosilicon slowly instills four-hole boiling flask, drips off beginning timing to anion-modified hyperbranched silicone, stirring
40min completes the self-emulsifying of anion-modified hyperbranched silicone.
3. a kind of synthesis technology preparation of anion-modified hyperbranched silicone according to claim 1 is anion-modified
Hyperbranched silicone and oxygen bleaching one-bath finishing technique, it is characterised in that: the process flow of the soft softening one-bath of oxygen bleaching are as follows: fabric → enzyme moves back
Slurry → soft the softening one-bath of alkaline scouring → oxygen bleaching；Concrete operations therein are as follows:
A. enzyme desizing:
Process flow is as follows: enzyme desizing prescription is first added, is warming up to 55-60 DEG C, fabric is then added and is handled, the time is handled
For 60min, then cool down, cold water is washed, and hot water wash is dried；
Enzyme desizing prescription is as follows: desizing enzyme 3.0-5.0g/L；NaCl 5.0g/L；JFC 1.0g/L；Bath raio is 20:1；Treatment fluid
After preparing by bath raio, need to be added suitable CH3COONa adjusts pH=6-7；
B. alkaline scouring:
Process flow is as follows: alkaline scouring prescription and fabric being added at 50 DEG C, is warming up to 100 DEG C, is handled, the processing time is
Then 120min cools down, hot water wash, cold water is washed；
Alkaline scouring prescription is as follows: NaOH 30.0g/L；Refining agent 4.0g/L；Bleeding agent 2.0g/L；Bath raio 20:1；
After fabric kiering, need to be detected with phenolphthalein solution until cloth cover does not redden (not aobvious alkalinity), knitting after being detected with phenolphthalein
Object is answered squezzing, is dried for standby；
C. the soft softening one-bath of oxygen bleaching:
Process flow is as follows: the fabric of bleaching process prescription and wetting being added at 50 DEG C, is warming up to 100 DEG C, is handled, locates
The reason time is 60min, is then cooled down, bleaching post-processing；
Bleaching process prescription is as follows: 30%H2O2 5.0g/L；Hydrogen peroxide bleaching stabilizer 1.0g/L；Anion-modified hyperbranched silicone 0-
10.0%(o.w.f)；Appropriate 1%NaOH；Bath raio is 20:1；After treatment fluid is prepared by bath raio, needs to be added suitable NaOH and adjust
pH=10-11；
It cleans after matched solution and bleaching during this and must all use distilled water；It to be stirred in due course in bleaching, supplement is steamed
Distilled water is to maintain bath raio；
It should also be noted that fabric cannot be made to leak out liquid level for a long time in this process；Fabric bleaching is complete, takes out, wash with distilled water
Until not reddened with phenolphthalein solution detection fabric surface.
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| CN104650364A (en) * | 2015-02-05 | 2015-05-27 | 南通斯恩特纺织科技有限公司 | Preparation method of hyper-branched polyether amide block silicone |
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