A kind of blocked isocyanate and polyurethane cooperate with anti-crease finishing method to cotton fabric
Technical field
The invention belongs to cotton fabrics to cooperate with anti-crease finishing method field, in particular to a kind of blocked isocyanate and polyurethane
Anti-crease finishing method is cooperateed with to cotton fabric.
Background technique
Cotton fiber is since the advantages that its excellent snugness of fit, hygroscopicity, is used widely, but in use process
It middle cotton fabric the shortcomings that there are easy wrinkle, needs to carry out anti-crease finishing to it.The main reason for cotton fabric wrinkles be cotton fiber without
Hydroxyl in setting zone on strand can slide under external force, form hydrogen bond in new position and hinder strand
It is returned to original state.Currently, most widely used is N- methylol amide class crosslinking agent, but after the arrangement of this kind of crosslinking agent
There is Form aldehyde release in cotton fabric, endanger human health.Later, polybasic carboxylic acid class crosslinking agent became research hotspot,
BTCA is considered as the crosslinking agent of most potential substitution 2D resin, but there are cotton fabrics after high production cost, arrangement by BTCA
The problems such as strength damage is big.Unsaturated polybasic carboxylic acid such as itaconic acid, maleic acid etc. are also used for cotton fabric crease-shedding arrangement, but whole
After reason there is yellowing in fabric, and anti-wrinkle effect is bad.Blocked polyurethane is environmentally friendly, efficient, cheap because having many advantages, such as,
The industries such as textile, leather finish are used widely, and also can be used as anti-crease finishing of the crosslinking agent for cotton fabric.End-sealed type is poly-
Deblocking reaction occurs under the conditions ofs high temperature etc. for urethane, the high isocyanate groups of reactivity is released, with hydroxyl in cotton fiber
Crosslinking, to assign cotton fiber excellent wrinkle resistance.
Cotton fabric crease-shedding, which arranges, at present is mainly arranged using one-step method, i.e. second dipping and rolling, is baked, is dried, washing.One-step method
Post-finishing agent is arranged in cotton fabric internal crosslinking, or is deposited on surface, crosslinking film forming, so that cotton fabric crease-shedding performance is improved,
But one-step method arrange after crease recovery properties of woven fabrics not enough and fabric strength decline is obvious, and the total dosage of finishing agent compares
Height, and method for sorting of the present invention can reduce the total dosage of finishing agent while improving creasy recovery angle.
Summary of the invention
Cotton fabric is cooperateed with technical problem to be solved by the invention is to provide a kind of blocked isocyanate and polyurethane and is resisted
Wrinkle method for sorting, to overcome fabric after the total dosage height of finishing agent and arrangement that cotton fabric crease-shedding arrangement needs in the prior art to roll over
Low and strongly decline the defect of the recovery that wrinkles.
The present invention uses two step finishing techniques, is first arranged using small molecule crosslinking agent, is formed and is handed over inside cotton fiber
Connection, is then arranged using aqueous polyurethane, and polyurethane can deposit in fiber surface or fabric tissue gap, and inside is handed over
Connection deposits both film forming synergistic effect so that crease recovery properties of woven fabrics further increases with surface.It can be whole in cotton fabric crease-shedding
Polyurethane with synergy is selected during reason, is reduced the total dosage of finishing agent, is with a wide range of applications.
Of the invention a kind of blocked isocyanate and polyurethane are to Cotton Fabric method, comprising:
(1) cotton fabric is immersed in blocked isocyanate finishing fluid, second dipping and rolling, drying bakes, the cotton arranged is knitted
Object;Wherein, the concentration of contained blocked isocyanate is 30g/L~100g/L in finishing fluid, and contained chain extender concentration is 4.5g/L
~15.0g/L;Second dipping and rolling liquid carrying rate is 70%~85%;
(2) cotton fabric arranged in step (1) to be immersed in aqueous polyurethane finishing fluid, second dipping and rolling, drying bakes,
Washing, drying, the cotton fabric after obtaining blocked isocyanate and polyurethane arrangement;Wherein, aqueous polyurethane concentration in finishing fluid
For 30g/L~100g/L;Second dipping and rolling liquid carrying rate is 70%~85%.
Blocked isocyanate is the sodium hydrogensulfite end-cap product of isocyanates, blocked isocyanate in the step (1)
The preparation method comprises the following steps: by isocyanates instill aqueous solution of sodium bisulfite in, be stirred to react at 25~40 DEG C to get.
The isocyanates is hexamethylene diisocyanate HDI, isophorone diisocyanate IPDI, 2,4- toluene two
One of isocyanates TDI.
Chain extender is diethanol amine in the step (1).
The process conditions dried in the step (1) are as follows: it is dried on heat setting machine, drying temperature is 50 DEG C~70 DEG C,
Drying time is 2min~4min.
Baking temperature is 100 DEG C~140 DEG C in the step (1), and baking the time is 120s~300s.
Aqueous polyurethane is that (the safe new material of the big China of Anhui peace is limited for AH-1618E type aqueous polyurethane in the step (2)
Company), Adwel-1315 anion-type water-thinned polyurethane (Yantai Wanhua chemistry limited liability company), Adwel-1629 aliphatic
Aqueous polyurethane (Yantai Wanhua chemistry limited liability company),(Cohan wound polymer China has 990R/ Cohan wound TPU
Limit company), Dispercoll U54 polyurethane (Cohan create polymer in Co., Ltd), the poly- ammonia of BAYPRET® polyether-type
One of ester (Dutch Tuo Na chemical company).
The process conditions dried in the step (2) are as follows: it is dried on heat setting machine, drying temperature is 60 DEG C~80 DEG C,
Drying time is 3min~5min.
Baking temperature is 110 DEG C~150 DEG C in the step (2), and baking the time is 120s~300s.
The present invention carries out small molecule blocked isocyanate and two step of high-molecular aqueous polyurethane, due to the hole of cotton fiber
Diameter in 50nm hereinafter, small molecule blocked isocyanate can be uniformly distributed between the micropore of cotton fiber and fento, it is baked
Cheng Zhongneng reacts with cellulose macromolecule and chain extender simultaneously, to hinder the sliding of cotton fiber or strand, improves
The wrinkle resistance of cotton fabric;Then the anti-crease finishing for carrying out high-molecular aqueous polyurethane, makes it in cotton fiber surface filming,
The tension failure strength of fibrous elasticity and fabric can be further enhanced.
Beneficial effect
(1) present invention is simple, at low cost, does not increase energy consumption, is convenient for industrialized production, and is with a wide range of applications and city
Field prospect.
(2) present invention selects finishing agent with synergy during cotton fabric crease-shedding arranges, and can reduce finishing agent
Total dosage.
(3) wash-and-wear fabrics that the present invention is prepared have good crease resistant finishing and strength retention, the fabric
In not less than 200 ° of the creasy recovery angle (non-finishing of cotton textiles creasy recovery angle is 120 °) after standard is washed, tearing brute force is protected
Rate is stayed to be greater than 75%, whiteness with higher.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, those skilled in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Range.
Main agents: cyanate is hexamethylene diisocyanate HDI, isophorone diisocyanate IPDI, 2,4- first
Phenylene diisocyanate TDI (AR, Shanghai Aladdin biochemical technology limited liability company), sodium hydrogensulfite (AR, Chinese medicines group chemistry
Reagent Co., Ltd), AH-1618E type aqueous polyurethane (Anhui Anda-Huatai New Material Co., Ltd.), Adwel-1315 yin from
Subtype aqueous polyurethane (Yantai Wanhua chemistry limited liability company), Adwel-1629 water-based aliphaic polyurethane (Yantai Wanhua
Chemical limited liability company),TPU (Co., Ltd in polymer is created in Cohan), Dispercoll are created in 990R/ Cohan
(Holland, which opens up, receives chemical public affairs for U54 polyurethane (Cohan wound polymer in Co., Ltd), BAYPRET® polyether polyurethane
Department).
It arranges obtained fabric and is cut into sample in thermostatic constant wet chamber's (21 ± 1 DEG C of humidity of temperature after a standard is washed
It is 65 ± 2%) it balances at least 4 hours and is tested.Indices test is carried out to finish fabric, specific as follows:
The measurement of creasy recovery angle is according to AATCC66-2008 " crease recovery of fabrics: replying horn cupping " standard test wrinkle
Recovery angle (WRA).
According to ASTM D1424-1996, " impact pendulnm method measures tearing for fabric for the measurement of fabric tear strength retention
Strongly " standard test tearing brute force.Tearing brute force retention rate TSR are as follows:
TSR=T/T0× 100%
In formula: T0For the tearing brute force of non-finish fabric, unit cN;T is the fabric tear strength after arranging, and unit is
cN。
The measurement of whiteness is according to AATCC110-2005 " whiteness of textile " standard test.
Standard washing is completed according to AATCC Test Method 124-2001.
Embodiment 1
(1) 29.7g NaHSO is weighed3It is dissolved in 88mL deionized water, magnetic agitation makes it completely dissolved, then thereto
33mL ethyl alcohol is added, is warming up to 25 DEG C, measures 20.1mL HDI and is dissolved in 17.6g ethyl acetate solution and is slowly added dropwise into NaHSO3
In aqueous solution, 1h is added dropwise, at interval of 20min measurement reaction system in isocyanate content and ending ratio, when in system not
Stop reaction when containing free isocyanate, rotary evaporation to reaction solution a large amount of white solids occurs, filters out white solid, put
Enter drying 24 hours in 45 DEG C of vacuum ovens, obtains sealing end HDI drying solid powder, product ending ratio 91%.
(2) cotton fabric is first padded into sealing end HDI finishing fluid (sealing end HDI mass concentration 55g/L, diethanol amine mass concentration
8.1g/L), second dipping and rolling (pick-up rate 80%), preliminary drying (70 DEG C, 3min), bakes (130 DEG C, 5min).
(3) cotton fabric after arranging in step (2) is padded into polyurethane finishing fluid (AH-1618E type aqueous polyurethane matter again
Measure concentration 35g/L), second dipping and rolling (pick-up rate 80%), preliminary drying (70 DEG C, 5min) bakes (140 DEG C, 4min), standard washing,
Drying.WRA=207 ° of creasy recovery angle is measured after once washing, tearing brute force retention rate TSR=76.0%, whiteness WI=
77.9。
Embodiment 2
(1) 14.5g NaHSO is weighed3It is dissolved in 72.5mL deionized water, magnetic agitation makes it completely dissolved, then to it
Middle addition 15mL ethyl alcohol, is warming up to 30 DEG C, measure 13.6mL IPDI be dissolved in 3.6g ethyl acetate solution and be slowly added dropwise into
NaHSO3In aqueous solution, 1h is added dropwise, and at interval of isocyanate content and ending ratio in 20min measurement reaction system, works as body
Stop reaction when not containing free isocyanate in system, rotary evaporation to reaction solution a large amount of white solids occurs, filters out white
Solid is put into drying 24 hours in 45 DEG C of vacuum ovens, obtains sealing end IPDI drying solid powder, product ending ratio 92%.
(2) cotton fabric is first padded into sealing end IPDI finishing fluid and (blocks IPDI mass concentration 45g/L, diethanol amine quality is dense
Spend 5.6g/L), second dipping and rolling (pick-up rate 75%), preliminary drying (70 DEG C, 4min) bakes (130 DEG C, 4min).
(3) cotton fabric after arranging in step (2) is padded into polyurethane finishing fluid (the poly- ammonia of BAYPRET® polyether-type again
Ester mass concentration 35g/L), second dipping and rolling (pick-up rate 80%), preliminary drying (70 DEG C, 5min) bakes (140 DEG C, 4min), standard water
It washes.WRA=204 ° of creasy recovery angle is measured after once washing, tearing brute force retention rate TSR=77.5%, whiteness WI=
78.0。
Embodiment 3
(1) 28.62g NaHSO is weighed3It is dissolved in 88mL deionized water, adds 31mL ethyl alcohol, measure 20.8mL TDI
It is dissolved in 17.6g ethyl acetate solution and is slowly added dropwise into NaHSO3In aqueous solution, 30 DEG C of reactions are warming up to, when not containing in system
Stop reaction when free isocyanate, rotary evaporation to reaction solution a large amount of white solids occurs, filters out white solid, be put into 45
It is 24 hours dry in DEG C vacuum oven, obtain sealing end TDI drying solid powder, product ending ratio 90.1%.
(2) cotton fabric is first padded into sealing end TDI finishing fluid (sealing end TDI mass concentration 40g/L, diethanol amine mass concentration
5.0g/L), second dipping and rolling (pick-up rate 75%), preliminary drying (70 DEG C, 3min), bakes (130 DEG C, 4min).
(3) cotton fabric after arranging in step (2) is padded into polyurethane finishing fluid (Dispercoll U54 polyurethane matter again
Measure concentration 50g/L): second dipping and rolling (aqueous polyurethane, pick-up rate 80%), preliminary drying (70 DEG C, 5min), bake (140 DEG C,
3.5min), standard is washed.WRA=202 ° of creasy recovery angle is measured after once washing, tearing brute force retention rate TSR=
79.5%, whiteness WI=78.9.
Embodiment 4
(1) 10.1g NaHSO is weighed3It is dissolved in 32mL deionized water, adds 12mL ethyl alcohol, it is molten to measure 6.1mL HDI
In 4.9g ethyl acetate solution and it is slowly added dropwise into NaHSO3In aqueous solution, 30 DEG C of reactions are warming up to, are measured at interval of 20min anti-
Isocyanate content and ending ratio in system are answered, stops reaction when not containing free isocyanate in system, rotary evaporation is extremely
There are a large amount of white solids in reaction solution, filters out white solid, is put into drying 24 hours in 45 DEG C of vacuum ovens, is blocked
HDI drying solid powder, product ending ratio 90.8%.
(2) cotton fabric is first padded into sealing end HDI finishing fluid (sealing end HDI mass concentration 50g/L, diethanol amine mass concentration
6.3g/L), second dipping and rolling (pick-up rate 80%), preliminary drying (70 DEG C, 3min), bakes (130 DEG C, 4min).
(3) cotton fabric after arranging in step (2) padded into polyurethane finishing fluid again (Adwel-1315 is anion-type water-thinned
Polyurethane mass concentration 45g/L), second dipping and rolling (pick-up rate 80%), preliminary drying (70 DEG C, 5min) bakes (140 DEG C, 4min), mark
Quasi- washing.WRA=210 ° of creasy recovery angle is measured after once washing, tearing brute force retention rate TSR=75.1%, whiteness WI
=77.2.
Comparative example 1
(1) 29.7g NaHSO is weighed3It is dissolved in 88mL deionized water, magnetic agitation makes it completely dissolved, then thereto
33mL ethyl alcohol is added, is warming up to 25 DEG C, measures 20.1mL HDI and is dissolved in 17.6g ethyl acetate solution and is slowly added dropwise into NaHSO3
In aqueous solution, 1h is added dropwise, at interval of 20min measurement reaction system in isocyanate content and ending ratio, when in system not
Stop reaction when containing free isocyanate, rotary evaporation to reaction solution a large amount of white solids occurs, filters out white solid, put
Enter drying 24 hours in 45 DEG C of vacuum ovens, obtains sealing end HDI drying solid powder, product ending ratio 91%.
(2) cotton fabric is padded into sealing end HDI finishing fluid (sealing end HDI mass concentration 95g/L, diethanol amine mass concentration
15g/L), second dipping and rolling (pick-up rate 80%), preliminary drying (70 DEG C, 3min), bakes (130 DEG C, 5min), standard washing.By one
WRA=190 ° of creasy recovery angle is measured after secondary washing, tearing brute force retention rate TSR=70.1%, whiteness WI=73.9.
Comparative example 2
Cotton fabric is padded into polyurethane finishing fluid (AH-1618E type aqueous polyurethane mass concentration 100g/L), second dipping and rolling
(pick-up rate 80%), preliminary drying (70 DEG C, 5min), bakes (140 DEG C, 4min), standard washing, drying.It is surveyed after once washing
WRA=191 ° of creasy recovery angle is obtained, tearing brute force retention rate TSR=72.5%, whiteness WI=70.9.
Comparative example 3
Cotton fabric is padded into polyurethane finishing fluid (Dispercoll U54 polyurethane mass concentration 100g/L), second dipping and rolling
(pick-up rate 80%), preliminary drying (70 DEG C, 5min), bakes (140 DEG C, 4min), standard washing, drying.It is surveyed after once washing
WRA=196 ° of creasy recovery angle is obtained, tearing brute force retention rate TSR=72.3%, whiteness WI=71.9.
For comparative example 4 it can be concluded that the total dosage of finishing agent of the present invention is 90g/L, wrinkle recovery angle of woven fabrics using viscoelasticity theory is 202 °, is torn
Broken strength retention is 79.5%;And the existing total dosage of finishing technique is 100g/L, wrinkle recovery angle of woven fabrics using viscoelasticity theory is 196 °, is torn
Strength retention is 72.3%.Method for sorting of the present invention has the synergistic effect of internal crosslinking and surface filming so that reagent is always used
Amount reduces, while crease resistant finishing also increases.