CN112301747A - Crease-resistant finishing method for cotton fabric - Google Patents
Crease-resistant finishing method for cotton fabric Download PDFInfo
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- CN112301747A CN112301747A CN202011093497.8A CN202011093497A CN112301747A CN 112301747 A CN112301747 A CN 112301747A CN 202011093497 A CN202011093497 A CN 202011093497A CN 112301747 A CN112301747 A CN 112301747A
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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
- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
- D06M16/003—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic with enzymes or microorganisms
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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
- D06M11/68—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 phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof
- D06M11/70—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 phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof with oxides of phosphorus; with hypophosphorous, phosphorous or phosphoric acids or their salts
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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
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/184—Carboxylic acids; Anhydrides, halides or salts thereof
- D06M13/192—Polycarboxylic acids; Anhydrides, halides or salts thereof
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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
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
- D06M15/03—Polysaccharides or derivatives thereof
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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
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
- D06M15/03—Polysaccharides or derivatives thereof
- D06M15/05—Cellulose or derivatives thereof
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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
- D06M2200/20—Treatment influencing the crease behaviour, the wrinkle resistance, the crease recovery or the ironing ease
Abstract
The invention relates to the field of textile after-finishing, and discloses a crease-resistant finishing method for cotton fabrics, which comprises the following steps: 1) cotton fabric pretreatment: soaking cotton fabric in a complex enzyme solution for treatment, washing with clear water at normal temperature, and rolling with a padder, wherein the liquid carrying rate is controlled to be 90-110%; 2) dipping the pretreated cotton fabric into finishing liquor, and carrying out two-dipping and two-rolling to take out the cotton fabric; 3) pre-baking the cotton fabric obtained in the step 2), and baking to obtain the crease-resistant cotton fabric. The invention organically combines the compound enzyme pretreatment process with the anti-wrinkle finishing agent mainly comprising the modified microcrystalline cellulose-chitosan compound, and the pretreated cotton fabric can efficiently adsorb the modified microcrystalline cellulose-chitosan compound, so that the modified microcrystalline cellulose-chitosan compound can fully react with polycarboxylic acid, thereby providing excellent and lasting anti-wrinkle performance, reducing the damage to the mechanical strength of the cotton fabric and having good water washing resistance.
Description
Technical Field
The invention relates to the field of textile after-finishing, in particular to a crease-resistant finishing method for cotton fabrics.
Background
The cotton fabric has excellent wearability, soft hand feeling and comfortable wearing, and is widely loved by consumers. However, in the process of taking or washing, when the cotton fabric is acted by external force, cellulose molecular chains can slide relatively, the original hydrogen bond action system is damaged, and a new hydrogen bond system can be formed at a new position. After the external force is removed, a hydrogen bond system newly formed among cellulose molecular chains can prevent the fibers from returning to the original state, and if the hydrogen bond action of the new system is strong and the stability is good, the cotton fabric can form wrinkles. Cotton fabrics are very prone to creasing and therefore anti-crease finishing of cotton fabrics is required to improve wearability.
The traditional cotton fabric crease-resistant finishing agent mostly uses 2D resin non-ironing crease-resistant finishing technology. Most of the 2D resin is hydroxymethyl finishing agent, and although the anti-wrinkle performance is excellent, the 2D resin can release formaldehyde in the finishing and taking processes, thereby causing great harm to human bodies. Along with the enhancement of consciousness of people on health and environmental protection, the control of formaldehyde release amount of textiles in various countries is more and more strict, and the formaldehyde-free finishing agent becomes a necessary trend for crease-resistant finishing development. Polycarboxylic acids such as butanetetracarboxylic acid (BTCA), citric acid, polymaleic acid, etc. can undergo a coupling reaction with hydroxyl groups on cellulose, and have an excellent crease-resistant finishing effect, particularly the BTCA effect. However, the finishing liquor of the polycarboxylic acid has strong acidity, and can cause great damage to the mechanical strength of the fabric in the high-temperature baking finishing process. Therefore, there is a need for a new crease-resistant finishing agent which is safe to the human body and has low damage to cotton fabrics. In addition, the existing crease-resistant finishing process basically does not carry out pretreatment on cotton fabrics, and the cotton fabrics are usually directly subjected to padding high-temperature finishing, so that the use rate of the finishing agent is low, and the waste is serious.
Disclosure of Invention
In order to solve the technical problems, the invention provides a crease-resistant finishing method for cotton fabrics, which organically combines a compound enzyme pretreatment process with a crease-resistant finishing agent mainly comprising a modified microcrystalline cellulose-chitosan compound, and the pretreated cotton fabrics can efficiently adsorb the modified microcrystalline cellulose-chitosan compound, so that the modified microcrystalline cellulose-chitosan compound can fully react with polycarboxylic acid, provide excellent and lasting crease resistance, reduce the damage to the mechanical strength of the cotton fabrics and have good washing resistance.
The specific technical scheme of the invention is as follows: a crease-resistant finishing method for cotton fabrics comprises the following steps:
1) cotton fabric pretreatment: soaking cotton fabric in complex enzyme solution, washing with clear water at normal temperature, and rolling with a padder to control the liquid carrying rate to 90-110%.
2) And (3) soaking the pretreated cotton fabric in the finishing liquid for two times and rolling for two times, and taking out the cotton fabric.
3) Pre-baking the cotton fabric obtained in the step 2), and baking to obtain the crease-resistant cotton fabric.
The method has the advantages that the cotton fabric is pretreated in the compound enzyme solution, the possibly residual polysaccharide with poor water solubility is removed, the hydrophilicity of the cotton fabric is increased, the number of surface hydroxyl groups is increased, the negative charge performance is enhanced, the modified microcrystalline cellulose-chitosan polymer is enhanced through electrostatic interaction and hydrogen bond action, the high-efficiency adsorption and the good film forming performance are realized, the cross-linking effect between the finishing agent and the cotton fabric is greatly enhanced through polycarboxylic acid reaction, the anti-wrinkle effect is improved, and meanwhile, the strength of the cotton fabric is kept better.
Preferably, the compound enzyme solution contains cellulase with the mass concentration of 0.1-1% and pectinase with the mass concentration of 0.1-0.5%; the treatment temperature is 35-50 deg.C, pH is 4.5-7.0, bath ratio is 1: 10-1: 30, and the treatment time is 20-45 min.
Preferably, in the step 2), the bath ratio of the cotton fabric to the finishing liquid is 1: 10-1: 20; the liquid carrying rate of the cotton fabric after being taken out is 80-120%.
Preferably, in the step 3), the pre-drying temperature is 80-100 ℃ and the time is 3-5 min; the baking temperature is 150-180 ℃, and the baking time is 1-3 min.
Preferably, the finishing liquid comprises 50-80g/L of polycarboxylic acid, 15-30g/L of sodium hypophosphite and 5-10g/L of modified microcrystalline cellulose-chitosan compound, and the solvent is water.
The modified microcrystalline cellulose-chitosan compound contains a large amount of active groups such as hydroxyl, amino and the like, contains a certain cationic group, can be efficiently adsorbed on cotton fabrics, has large specific surface area and many surface active sites, and can form a film on the cotton fabrics. The polycarboxylic acid reacts with hydroxyl on cotton fibers and hydroxyl/amino on a modified microcrystalline cellulose-chitosan compound under the catalytic action of a catalyst sodium hypophosphite to form a net-shaped cross-linked structure, so that the structure among cellulose chains in the cotton fabric is fixed, the mechanical strength of the fabric can be improved while the crease-resistant effect is given to the fabric, the fabric has good water resistance, no formaldehyde is released in the whole finishing process, and the fabric is healthy and environment-friendly. Further preferably, the cotton fabric crease-resistant finishing agent composition comprises 60-70g/L of polycarboxylic acid, 20-30g/L of sodium hypophosphite and 5-10g/L of modified microcrystalline cellulose-chitosan complex, and the solvent is water.
Preferably, the preparation method of the modified microcrystalline cellulose-chitosan compound comprises the following steps:
a) uniformly mixing microcrystalline cellulose and concentrated sulfuric acid with the mass fraction of 55-65% in a mass ratio of 1: 15-1: 25, and carrying out ultrasonic reaction for 2-3h at 40-50 ℃, the ultrasonic frequency of 25-35kHz and the power of 200-;
b) adding quaternized chitosan with the mass of 25-50% of microcrystalline cellulose into the reaction liquid obtained in the step a), and continuously performing ultrasonic reaction for 10-30min at the temperature of 40-50 ℃, the ultrasonic frequency of 25-35kHz and the power of 200-;
c) centrifuging the reaction liquid obtained in the step b), collecting supernatant, putting the supernatant into a dialysis bag, and dialyzing with deionized water until the pH value is 6-7 to obtain the modified microcrystalline cellulose-chitosan compound solution.
The microcrystalline cellulose has the characteristics of large specific surface area and many surface active sites, and is further decomposed and partially sulfated by adopting concentrated sulfuric acid treatment, so that the dispersibility of the microcrystalline cellulose in an aqueous solution is enhanced; the quaternized chitosan is introduced at the end of the reaction, the reaction is continued, and the molecular chain of the chitosan is slightly sulfated, so that the modified microcrystalline cellulose and the chitosan molecule with the amphoteric group can form a stably dispersed compound through electrostatic interaction. The positive charge of the compound can enable the compound to be efficiently adsorbed on the surface of cotton fabric, and the macromolecular structure of the chitosan can promote the compound to form a film on the surface, so that sufficient sites are provided for further esterification, crosslinking and crease-resistant finishing of polycarboxylic acid, and the crease-resistant finishing effect is guaranteed. The reaction time of the quaternized chitosan is not suitable to be too long, otherwise, the stability is influenced by too strong electrostatic action due to too high sulfation degree of the chitosan; the addition amount is not too much, otherwise, the microcrystalline cellulose can be completely wrapped, and the reaction sites are reduced. The non-quaternized chitosan has obvious negative charge property after sulfation, not only has weak acting force with the modified microcrystalline cellulose, but also has weak adsorption capacity on fabrics. On the other hand, if the degree of quaternization of chitosan is too high, the electrostatic interaction is too strong, so that the water dispersibility of the complex may be deteriorated, and the complex may precipitate. Preferably, in step a), the microcrystalline cellulose has a size of 80 to 120 μm and a crystallinity of 70 to 80%.
Preferably, in step b), the quaternized chitosan is prepared from chitosan and 2, 3-epoxypropyltrimethylammonium chloride, the quaternization degree is 50-80%, and the molecular weight of the chitosan is 50000-100000.
If the quaternization degree is too low, the complex formed after the sulfation reaction of the polysaccharide presents negative charge property, the binding capacity of the complex with cotton fabrics is weakened, and if the quaternization degree is too high, the internal electrostatic interaction of the complex formed after the reaction is too strong, the water dispersibility is poor, and the complex is precipitated. The molecular weight of chitosan also has a great influence, if the molecular weight is too small, intermolecular entanglement is difficult to form, stability is influenced, and if the molecular weight is too large, the viscosity of the system is too large, and the flowability is too poor, so that use is influenced. Preferably, in step c), the centrifugation speed is 10000-.
Preferably, in step c), the dialysis bag has a molecular weight cut-off of 10000.
Preferably, the polycarboxylic acid is one or more of butanetetracarboxylic acid, citric acid and polymaleic acid.
More preferably, the polycarboxylic acid is butanetetracarboxylic acid.
Compared with the prior art, the invention has the beneficial effects that:
(1) according to the invention, the surface property of the cotton fabric is modified by adopting the pretreatment of the compound enzyme, so that the adsorption film forming effect of the cotton fabric and the modified microcrystalline cellulose-chitosan is greatly enhanced through electrostatic interaction and hydrogen bond interaction, and then the cotton fabric reacts with the polycarboxylic acid, so that the anti-wrinkle effect is further improved.
(2) The modified microcrystalline cellulose-chitosan compound and the polycarboxylic acid are compounded for use to carry out the synergistic crease-resistant finishing on the cotton fabric. The modified microcrystalline cellulose-chitosan compound contains a large amount of active groups such as hydroxyl, amino and the like, contains a certain cationic group, can be efficiently adsorbed on cotton fabrics, has large specific surface area and many surface active sites, can form a film on the cotton fabrics, and further forms a net-shaped cross-linked structure with cellulose fibers under the esterification of polycarboxylic acid, so that the mechanical strength of the fabrics can be improved while the fabrics are endowed with excellent and lasting anti-wrinkle effect, and the modified microcrystalline cellulose-chitosan compound has good water resistance, no formaldehyde release in the whole finishing process, and is healthy and environment-friendly.
Detailed Description
The present invention will be further described with reference to the following examples.
The fabrics used in the examples and comparative examples were 120g/m2The bleached cotton fabric has the wrinkle recovery angle of 125 degrees, the whiteness of 93.56 and the breaking strength of 653N. The crease recovery angle and breaking strength of the fabric were measured according to GB/T3819-1997 and GB/T3923.1-2013, respectively, and the water wash resistance was tested according to AATCC 61-2013.
Example 1
Preparing a modified microcrystalline cellulose-chitosan compound:
a) uniformly mixing microcrystalline cellulose (with the size of about 100 mu m and the crystallinity of about 72.6%) and concentrated sulfuric acid with the mass fraction of 60% according to the mass ratio of 1: 20, and carrying out ultrasonic reaction for 2 hours at the temperature of 45 ℃, the ultrasonic frequency of 30kHz and the power of 250W;
b) adding quaternized chitosan with the mass of 30 percent of microcrystalline cellulose (the quaternization degree is 60 percent, the molecular weight is 70,000) into the reaction liquid in the step a), and continuously carrying out ultrasonic reaction for 20min under the conditions of 45 ℃, the ultrasonic frequency is 30kHz and the power is 250W;
c) centrifuging the reaction solution obtained in the step b) at 15,000rpm, collecting supernatant, placing the supernatant into a dialysis bag (with the molecular weight cutoff of 10000), and dialyzing with deionized water until the pH value is 6-7 to obtain the modified microcrystalline cellulose-chitosan compound solution.
Preparation of crease-resistant finishing agent composition: 30g of butane tetracarboxylic acid and 10g of sodium hypophosphite are dissolved in 500ml of microcrystalline cellulose-chitosan complex aqueous solution with the concentration of 8 g/L. Wherein the butane tetracarboxylic acid is 60g/L, and the sodium hypophosphite is 20 g/L.
Crease-resistant finishing of cotton fabrics:
cotton fabric pretreatment: treating 25g of cotton fabric in 500ml of complex enzyme solution containing 0.5% cellulase and 0.3% pectinase at 40 ℃ and pH 5.5 for 30min, washing with warm water at normal temperature, and rolling with a padder to control the liquid carrying rate to 100%.
And (3) treating the pretreated cotton fabric in the finishing agent by adopting a two-dipping and two-rolling process, wherein the liquid carrying rate is 100%, then pre-baking the cotton fabric for 4min at 80 ℃, and baking the cotton fabric for 2min at 160 ℃ to obtain the crease-resistant cotton fabric.
Example 2
Preparing a modified microcrystalline cellulose-chitosan compound:
a) uniformly mixing microcrystalline cellulose (with the size of about 120 mu m and the crystallinity of about 74.8%) and concentrated sulfuric acid with the mass fraction of 65% in a mass ratio of 1: 15, and carrying out ultrasonic reaction for 3 hours at 40 ℃ and the ultrasonic frequency of 25kHz and the power of 300W;
b) adding quaternized chitosan with the mass of 25% of microcrystalline cellulose (the quaternization degree is 50%, the molecular weight is 100,000) into the reaction liquid obtained in the step a), and continuously carrying out ultrasonic reaction for 30min under the conditions of 40 ℃, the ultrasonic frequency is 25kHz and the power is 300W;
c) centrifuging the reaction solution obtained in the step b) at 10,000rpm, collecting supernatant, placing the supernatant into a dialysis bag (with the molecular weight cutoff of 10000), and dialyzing with deionized water until the pH value is 6-7 to obtain the modified microcrystalline cellulose-chitosan compound solution.
Preparation of crease-resistant finishing agent composition: 40g of butane tetracarboxylic acid and 15g of sodium hypophosphite are dissolved in 500ml of microcrystalline cellulose-chitosan composite solution with the concentration of 5g/L, wherein the butane tetracarboxylic acid is 80g/L, and the sodium hypophosphite is 30 g/L.
Crease-resistant finishing of cotton fabrics:
pretreating cotton fabrics; 50g of cotton fabric is put into 500ml of complex enzyme solution containing 1 percent of cellulase and 0.5 percent of pectinase by mass concentration, treated for 20min under the conditions of 35 ℃ and pH 4.5, washed by warm water at normal temperature, pressed by a padder and controlled at the liquid-carrying rate of 90 percent.
And (3) treating the pretreated cotton fabric in the finishing agent by adopting a two-dipping and two-rolling process, wherein the liquid carrying rate is 80%, then pre-baking the cotton fabric at 80 ℃ for 5min, and baking the cotton fabric at 180 ℃ for 1min to obtain the crease-resistant cotton fabric.
Example 3
Preparation of microcrystalline cellulose-chitosan complex:
a) uniformly mixing microcrystalline cellulose (with the size of about 80 mu m and the crystallinity of about 70.3%) and concentrated sulfuric acid with the mass fraction of 55% according to the mass ratio of 1: 25, and carrying out ultrasonic reaction for 2.5h under the conditions of 43 ℃, ultrasonic frequency of 35kHz and power of 200W;
b) adding quaternized chitosan with the mass of 50% of microcrystalline cellulose (the quaternization degree is 80%, the molecular weight is 50,000) into the reaction liquid obtained in the step a), and continuously carrying out ultrasonic reaction for 10min at the temperature of 43 ℃, the ultrasonic frequency of 35kHz and the power of 200W;
c) centrifuging the reaction solution in the step b) at 12,000rpm, collecting supernatant, placing the supernatant into a dialysis bag (with the molecular weight cut-off of 10000), and dialyzing with deionized water until the pH value is 6-7 to obtain the modified microcrystalline cellulose-chitosan compound solution.
Preparation of crease-resistant finishing agent composition: 25g of butane tetracarboxylic acid and 7.5g of sodium hypophosphite are dissolved in 500ml of microcrystalline cellulose-chitosan composite solution with the concentration of 10g/L, wherein the butane tetracarboxylic acid is 50g/L, and the sodium hypophosphite is 15 g/L.
Crease-resistant finishing of cotton fabrics:
pretreating cotton fabrics; treating 40g cotton fabric in 1200ml complex enzyme solution containing cellulase and 0.3% pectase at 50 deg.C and pH 6.0 for 45min, washing with warm water at room temperature, and rolling with a padder to control the liquid carrying rate at 110%.
And (3) treating the pretreated cotton fabric in the finishing agent by adopting a two-dipping and two-rolling process, wherein the liquid carrying rate is 120%, then pre-baking the cotton fabric at 100 ℃ for 3min, and baking the cotton fabric at 150 ℃ for 3min to obtain the crease-resistant cotton fabric.
Example 4
Preparing a modified microcrystalline cellulose-chitosan compound:
a) uniformly mixing microcrystalline cellulose (with the size of about 80 mu m and the crystallinity of about 72.6%) and concentrated sulfuric acid with the mass fraction of 60% according to the mass ratio of 1: 20, and carrying out ultrasonic reaction for 2 hours under the conditions of 50 ℃, ultrasonic frequency of 30kHz and power of 250W;
b) adding quaternized chitosan with the mass of 40% of microcrystalline cellulose (the quaternization degree is 70%, the molecular weight is 80,000) into the reaction liquid obtained in the step a), and continuously carrying out ultrasonic reaction for 15min under the conditions of 50 ℃, the ultrasonic frequency is 30kHz and the power is 250W;
c) centrifuging the reaction solution in the step b) at 12,000rpm, collecting supernatant, placing the supernatant into a dialysis bag (with the molecular weight cut-off of 10000), and dialyzing with deionized water until the pH value is 6-7 to obtain the modified microcrystalline cellulose-chitosan compound solution.
Preparation of crease-resistant finishing agent composition: 35g of butane tetracarboxylic acid and 15g of sodium hypophosphite are dissolved in 500ml of microcrystalline cellulose-chitosan composite solution with the concentration of 6g/L, wherein the butane tetracarboxylic acid is 70g/L, and the sodium hypophosphite is 30 g/L.
Crease-resistant finishing of cotton fabrics:
cotton fabric pretreatment: treating 25g of cotton fabric in 625ml of complex enzyme solution containing 0.5% cellulase and 0.1% pectinase at 50 deg.C and pH 7.0 for 30min, washing with warm water at room temperature, and rolling with a padder to control the liquid-carrying rate to 100%.
And (3) treating the pretreated cotton fabric in the finishing agent by adopting a two-dipping and two-rolling process, wherein the liquid carrying rate is 100%, then pre-baking the cotton fabric for 3min at 90 ℃, and then baking the cotton fabric for 2min at 160 ℃ to obtain the crease-resistant cotton fabric.
Comparative example 1 (Cotton fabric without pretreatment)
Preparing a modified microcrystalline cellulose-chitosan compound:
a) uniformly mixing microcrystalline cellulose (with the size of about 100 mu m and the crystallinity of about 72.6%) and concentrated sulfuric acid with the mass fraction of 60% according to the mass ratio of 1: 20, and carrying out ultrasonic reaction for 2 hours at the temperature of 45 ℃, the ultrasonic frequency of 30kHz and the power of 250W;
b) adding quaternized chitosan with the mass of 30 percent of microcrystalline cellulose (the quaternization degree is 60 percent, the molecular weight is 70,000) into the reaction liquid in the step a), and continuously carrying out ultrasonic reaction for 20min under the conditions of 45 ℃, the ultrasonic frequency is 30kHz and the power is 250W;
c) centrifuging the reaction solution obtained in the step b) at 15,000rpm, collecting supernatant, placing the supernatant into a dialysis bag (with the molecular weight cutoff of 10000), and dialyzing with deionized water until the pH value is 6-7 to obtain the modified microcrystalline cellulose-chitosan compound solution.
Preparation of crease-resistant finishing agent composition: 30g of butane tetracarboxylic acid and 10g of sodium hypophosphite are dissolved in 500ml of microcrystalline cellulose-chitosan complex aqueous solution with the concentration of 8 g/L. Wherein the butane tetracarboxylic acid is 60g/L, and the sodium hypophosphite is 20 g/L.
Crease-resistant finishing of cotton fabrics: (ii) a And (2) treating 25g of cotton fabric in the finishing agent by adopting a two-dipping and two-rolling process, wherein the liquid carrying rate is 100%, pre-drying at 80 ℃ for 4min, and then drying at 160 ℃ for 2min to obtain the crease-resistant cotton fabric.
Comparative example 2 (Cotton fabric without pretreatment)
Preparing a modified microcrystalline cellulose-chitosan compound:
a) uniformly mixing microcrystalline cellulose (with the size of about 120 mu m and the crystallinity of about 74.8%) and concentrated sulfuric acid with the mass fraction of 65% in a mass ratio of 1: 15, and carrying out ultrasonic reaction for 3 hours at 40 ℃ and the ultrasonic frequency of 25kHz and the power of 300W;
b) adding quaternized chitosan with the mass of 25% of microcrystalline cellulose (the quaternization degree is 50%, the molecular weight is 100,000) into the reaction liquid obtained in the step a), and continuously carrying out ultrasonic reaction for 30min under the conditions of 40 ℃, the ultrasonic frequency is 25kHz and the power is 300W;
c) centrifuging the reaction solution obtained in the step b) at 10,000rpm, collecting supernatant, placing the supernatant into a dialysis bag (with the molecular weight cutoff of 10000), and dialyzing with deionized water until the pH value is 6-7 to obtain the modified microcrystalline cellulose-chitosan compound solution.
Preparation of crease-resistant finishing agent composition: 40g of butane tetracarboxylic acid and 15g of sodium hypophosphite are dissolved in 500ml of microcrystalline cellulose-chitosan composite solution with the concentration of 5g/L, wherein the butane tetracarboxylic acid is 80g/L, and the sodium hypophosphite is 30 g/L.
Crease-resistant finishing of cotton fabrics: 50g of cotton fabric is treated in the finishing agent by adopting a two-dipping and two-rolling process, the liquid carrying rate is 80 percent, and then the cotton fabric is pre-dried for 5min at 80 ℃ and then is baked for 1min at 180 ℃ to obtain the crease-resistant cotton fabric.
Comparative example 3 (Cotton fabric without pretreatment)
Preparation of microcrystalline cellulose-chitosan complex:
a) uniformly mixing microcrystalline cellulose (with the size of about 80 mu m and the crystallinity of about 70.3%) and concentrated sulfuric acid with the mass fraction of 55% according to the mass ratio of 1: 25, and carrying out ultrasonic reaction for 2.5h under the conditions of 43 ℃, ultrasonic frequency of 35kHz and power of 200W;
b) adding quaternized chitosan with the mass of 50% of microcrystalline cellulose (the quaternization degree is 80%, the molecular weight is 50,000) into the reaction liquid obtained in the step a), and continuously carrying out ultrasonic reaction for 10min at the temperature of 43 ℃, the ultrasonic frequency of 35kHz and the power of 200W;
c) centrifuging the reaction solution in the step b) at 12,000rpm, collecting supernatant, placing the supernatant into a dialysis bag (with the molecular weight cut-off of 10000), and dialyzing with deionized water until the pH value is 6-7 to obtain the modified microcrystalline cellulose-chitosan compound solution.
Preparation of crease-resistant finishing agent composition: 25g of butane tetracarboxylic acid and 7.5g of sodium hypophosphite are dissolved in 500ml of microcrystalline cellulose-chitosan composite solution with the concentration of 10g/L, wherein the butane tetracarboxylic acid is 50g/L, and the sodium hypophosphite is 15 g/L.
Crease-resistant finishing of cotton fabrics: and (3) treating 40g of cotton fabric in the finishing agent by adopting a two-dipping and two-rolling process, wherein the liquid carrying rate is 120%, pre-drying at 100 ℃ for 3min, and then baking at 150 ℃ for 3min to obtain the crease-resistant cotton fabric.
Comparative example 4 (Cotton fabric without pretreatment)
Preparing a modified microcrystalline cellulose-chitosan compound:
a) uniformly mixing microcrystalline cellulose (with the size of about 80 mu m and the crystallinity of about 72.6%) and concentrated sulfuric acid with the mass fraction of 60% according to the mass ratio of 1: 20, and carrying out ultrasonic reaction for 2 hours under the conditions of 50 ℃, ultrasonic frequency of 30kHz and power of 250W;
b) adding quaternized chitosan with the mass of 40% of microcrystalline cellulose (the quaternization degree is 70%, the molecular weight is 80,000) into the reaction liquid obtained in the step a), and continuously carrying out ultrasonic reaction for 15min under the conditions of 50 ℃, the ultrasonic frequency is 30kHz and the power is 250W;
c) centrifuging the reaction solution in the step b) at 12,000rpm, collecting supernatant, placing the supernatant into a dialysis bag (with the molecular weight cut-off of 10000), and dialyzing with deionized water until the pH value is 6-7 to obtain the modified microcrystalline cellulose-chitosan compound solution.
Preparation of crease-resistant finishing agent composition: 35g of butane tetracarboxylic acid and 15g of sodium hypophosphite are dissolved in 500ml of microcrystalline cellulose-chitosan composite solution with the concentration of 6g/L, wherein the butane tetracarboxylic acid is 70g/L, and the sodium hypophosphite is 30 g/L.
Crease-resistant finishing of cotton fabrics: and (3) treating 25g of cotton fabric in the finishing agent by adopting a two-dipping and two-rolling process, wherein the liquid carrying rate is 100%, pre-drying at 90 ℃ for 3min, and then baking at 160 ℃ for 2min to obtain the crease-resistant cotton fabric.
Comparative example 5 (step b) reaction time too long)
Preparing a modified microcrystalline cellulose-chitosan compound:
a) uniformly mixing microcrystalline cellulose (with the size of about 100 mu m and the crystallinity of about 72.6%) and concentrated sulfuric acid with the mass fraction of 60% according to the mass ratio of 1: 20, and carrying out ultrasonic reaction for 2 hours at the temperature of 45 ℃, the ultrasonic frequency of 30kHz and the power of 250W;
b) adding quaternized chitosan with the mass of 30 percent of microcrystalline cellulose (the quaternization degree is 60 percent, the molecular weight is 70,000) into the reaction liquid in the step a), and continuously carrying out ultrasonic reaction under the conditions of 45 ℃, the ultrasonic frequency is 30kHz and the power is 250W2h；
c) Centrifuging the reaction solution obtained in the step b) at 15,000rpm, collecting supernatant, placing the supernatant into a dialysis bag (with the molecular weight cutoff of 10000), and dialyzing with deionized water until the pH value is 6-7 to obtain the modified microcrystalline cellulose-chitosan compound solution.
Preparation of crease-resistant finishing agent composition: 30g of butane tetracarboxylic acid and 10g of sodium hypophosphite are dissolved in 500ml of microcrystalline cellulose-chitosan compound solution with the concentration of 8g/L, wherein the butane tetracarboxylic acid is 60g/L, and the sodium hypophosphite is 20 g/L.
Crease-resistant finishing of cotton fabrics:
pretreating cotton fabrics; treating 25g of cotton fabric in 500ml of complex enzyme solution containing 0.5% cellulase and 0.3% pectinase at 40 ℃ and pH 5.5 for 30min, washing with warm water at normal temperature, and rolling with a padder to control the liquid carrying rate to 100%.
And (3) treating the pretreated cotton fabric in the finishing agent by adopting a two-dipping and two-rolling process, wherein the liquid carrying rate is 100%, then pre-baking the cotton fabric for 4min at 80 ℃, and then baking the cotton fabric for 2min at 160 ℃ to obtain the crease-resistant cotton fabric.
Comparative example 6 (Chitosan not quaternized)
Preparing a modified microcrystalline cellulose-chitosan compound:
a) uniformly mixing microcrystalline cellulose (with the size of about 100 mu m and the crystallinity of about 72.6%) and concentrated sulfuric acid with the mass fraction of 60% according to the mass ratio of 1: 20, and carrying out ultrasonic reaction for 2 hours at the temperature of 45 ℃, the ultrasonic frequency of 30kHz and the power of 250W;
b) adding chitosan (molecular weight is 70,000) with the mass being 30% of that of the microcrystalline cellulose into the reaction solution obtained in the step a), and continuously carrying out ultrasonic reaction for 20min under the conditions of 45 ℃, ultrasonic frequency of 30kHz and power of 250W;
c) centrifuging the reaction solution obtained in the step b) at 15,000rpm, collecting supernatant, placing the supernatant into a dialysis bag (with the molecular weight cutoff of 10000), and dialyzing with deionized water until the pH value is 6-7 to obtain the modified microcrystalline cellulose-chitosan compound solution.
Preparation of crease-resistant finishing agent composition: 30g of butane tetracarboxylic acid and 10g of sodium hypophosphite are dissolved in 500ml of microcrystalline cellulose-chitosan compound solution with the concentration of 8g/L, wherein the butane tetracarboxylic acid is 60g/L, and the sodium hypophosphite is 20 g/L.
Crease-resistant finishing of cotton fabrics: pretreating cotton fabrics; and (3) treating 25g of cotton fabric in the finishing agent by adopting a two-dipping and two-rolling process, wherein the liquid carrying rate is 100%, pre-drying at 80 ℃ for 4min, and then baking at 160 ℃ for 2min to obtain the crease-resistant cotton fabric.
Comparative example 7 (quaternization degree of quaternized chitosan is too high)
Preparing a modified microcrystalline cellulose-chitosan compound:
a) uniformly mixing microcrystalline cellulose (with the size of about 100 mu m and the crystallinity of about 72.6%) and concentrated sulfuric acid with the mass fraction of 60% according to the mass ratio of 1: 20, and carrying out ultrasonic reaction for 2 hours at the temperature of 45 ℃, the ultrasonic frequency of 30kHz and the power of 250W;
b) adding microcrystalline cellulose to the reaction solution of step a)30％Of (d) quaternized chitosan (degree of quaternization of100％Molecular weight of 70,000), and continuously carrying out ultrasonic reaction for 20min at 45 ℃, ultrasonic frequency of 30kHz and power of 250W;
c) centrifuging the reaction solution obtained in the step b) at 15,000rpm, collecting supernatant, placing the supernatant into a dialysis bag (with the molecular weight cutoff of 10000), and dialyzing with deionized water until the pH value is 6-7 to obtain the modified microcrystalline cellulose-chitosan compound solution.
Preparation of crease-resistant finishing agent composition: 30g of butane tetracarboxylic acid and 10g of sodium hypophosphite are dissolved in 500ml of microcrystalline cellulose-chitosan compound solution with the concentration of 8g/L, wherein the butane tetracarboxylic acid is 60g/L, and the sodium hypophosphite is 20 g/L.
Crease-resistant finishing of cotton fabrics:
cotton fabric pretreatment: treating 25g of cotton fabric in 500ml of complex enzyme solution containing 0.5% cellulase and 0.3% pectinase at 40 ℃ and pH 5.5 for 30min, washing with warm water at normal temperature, and rolling with a padder to control the liquid carrying rate to 100%.
And (3) treating the pretreated cotton fabric in the finishing agent by adopting a two-dipping and two-rolling process, wherein the liquid carrying rate is 100%, then pre-baking the cotton fabric for 4min at 80 ℃, and then baking the cotton fabric for 2min at 160 ℃ to obtain the crease-resistant cotton fabric.
Comparative example 8 (molecular weight of quaternized chitosan is too low)
Preparing a modified microcrystalline cellulose-chitosan compound:
a) uniformly mixing microcrystalline cellulose (with the size of about 100 mu m and the crystallinity of about 72.6%) and concentrated sulfuric acid with the mass fraction of 60% according to the mass ratio of 1: 20, and carrying out ultrasonic reaction for 2 hours at the temperature of 45 ℃, the ultrasonic frequency of 30kHz and the power of 250W;
b) adding microcrystalline cellulose to the reaction solution of step a)30％Of (d) quaternized chitosan (degree of quaternization of60％Molecular weight of 20,000), and continuously carrying out ultrasonic reaction for 20min at 45 ℃, ultrasonic frequency of 30kHz and power of 250W;
c) centrifuging the reaction solution obtained in the step b) at 15,000rpm, collecting supernatant, placing the supernatant into a dialysis bag (with the molecular weight cutoff of 10000), and dialyzing with deionized water until the pH value is 6-7 to obtain the modified microcrystalline cellulose-chitosan compound solution.
Preparation of crease-resistant finishing agent composition: 30g of butane tetracarboxylic acid and 10g of sodium hypophosphite are dissolved in 500ml of microcrystalline cellulose-chitosan compound solution with the concentration of 8g/L, wherein the butane tetracarboxylic acid is 60g/L, and the sodium hypophosphite is 20 g/L.
Crease-resistant finishing of cotton fabrics:
cotton fabric pretreatment: cotton fabric pretreatment: treating 25g of cotton fabric in 500ml of complex enzyme solution containing 0.5% cellulase and 0.3% pectinase at 40 ℃ and pH 5.5 for 30min, washing with warm water at normal temperature, and rolling with a padder to control the liquid carrying rate to 100%.
And (3) treating the pretreated cotton fabric in the finishing agent by adopting a two-dipping and two-rolling process, wherein the liquid carrying rate is 100%, then pre-baking the cotton fabric for 4min at 80 ℃, and then baking the cotton fabric for 2min at 160 ℃ to obtain the crease-resistant cotton fabric.
Performance characterization
TABLE 1 Properties of Cotton Fabric after crease-resistant finishing
TABLE 2 Water washing resistance of finished Cotton Fabric
As can be seen from tables 1-2, after the anti-crease finishing agent composition of each embodiment of the present invention is used to perform anti-crease finishing on cotton fabric according to the specific process of pre-treating with the complex enzyme and then finishing, the crease recovery angle of the cotton fabric is greatly improved, the strength retention rate is high, and the crease recovery angle can be maintained at 240 ° or above after multiple washing cycles. The crease-resistant finishing process and the finishing agent composition have good adaptability and more excellent and durable crease-resistant finishing effect. In contrast, the groups of comparative examples 1 to 4 have relatively poor crease-resistant finishing effects because the surface of the cotton fabric is not subjected to the pretreatment process, and the negative charge property and the number of hydroxyl groups of the cotton fabric are not as good as those of the cotton fabric subjected to pretreatment in the examples.
In addition, although the cotton fabrics in comparative examples 5 to 8 were also subjected to complex enzyme pretreatment, the properties thereof were limited because the specifications of the anti-crease finish composition did not fall within the preferable range. For example, in comparative example 5, because the reaction time of the quaternized chitosan is too long and the sulfation degree is too high, the formed complex is centrifuged to filter out a great amount of polysaccharide, so that the content of the quaternized chitosan in the complex is low, and the adsorption on cotton fabrics is low; in comparative example 6, chitosan was not quaternized and the interaction of the final composite with cotton fabric was weak; in the comparative example 7, the quaternization degree of the quaternized chitosan is too high, and a substance which possibly forms water dispersibility deviation is filtered out in a centrifugal stage, so that the final effect is influenced; the molecular weight of chitosan in comparative example 8 is low, resulting in low water dispersibility and poor stability of its complex with modified microcrystalline cellulose.
The raw materials and equipment used in the invention are common raw materials and equipment in the field if not specified; the methods used in the present invention are conventional in the art unless otherwise specified.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and all simple modifications, alterations and equivalents of the above embodiments according to the technical spirit of the present invention are still within the protection scope of the technical solution of the present invention.
Claims (10)
1. A crease-resistant finishing method for cotton fabrics is characterized by comprising the following steps:
1) cotton fabric pretreatment: soaking cotton fabric in a complex enzyme solution for treatment, washing with clear water at normal temperature, and rolling with a padder, wherein the liquid carrying rate is controlled to be 90-110%;
2) dipping the pretreated cotton fabric into finishing liquor, and carrying out two-dipping and two-rolling to take out the cotton fabric;
3) pre-baking the cotton fabric obtained in the step 2), and baking to obtain the crease-resistant cotton fabric.
2. The method as claimed in claim 1, wherein in the step 1), the compound enzyme solution contains cellulase with the mass concentration of 0.1-1% and pectinase with the mass concentration of 0.1-0.5%; the treatment temperature is 35-50 deg.C, pH is 4.5-7.0, bath ratio is 1: 10-1: 30, and the treatment time is 20-45 min.
3. The method of claim 1, wherein in step 2), the bath ratio between the cotton fabric and the finishing liquor is from 1: 10 to 1: 20; the liquid carrying rate of the cotton fabric after being taken out is 80-120%.
4. The method of claim 1, wherein in step 3), the pre-drying temperature is 80-100 ℃ and the time is 3-5 min; the baking temperature is 150-180 ℃, and the baking time is 1-3 min.
5. The method of claim 1, wherein the finishing liquor comprises 50-80g/L of polycarboxylic acid, 15-30g/L of sodium hypophosphite and 5-10g/L of modified microcrystalline cellulose-chitosan complex, and the solvent is water.
6. The method of claim 5, wherein the modified microcrystalline cellulose-chitosan complex is prepared by:
a) uniformly mixing microcrystalline cellulose and concentrated sulfuric acid with the mass fraction of 55-65% in a mass ratio of 1: 15-1: 25, and carrying out ultrasonic reaction for 2-3h at 40-50 ℃, the ultrasonic frequency of 25-35kHz and the power of 200-;
b) adding quaternized chitosan with the mass of 25-50% of microcrystalline cellulose into the reaction liquid obtained in the step a), and continuously performing ultrasonic reaction for 10-30min at the temperature of 40-50 ℃, the ultrasonic frequency of 25-35kHz and the power of 200-;
c) centrifuging the reaction liquid obtained in the step b), collecting supernatant, putting the supernatant into a dialysis bag, and dialyzing with deionized water until the pH value is 6-7 to obtain the modified microcrystalline cellulose-chitosan compound solution.
7. The method of claim 6, wherein in step a), the microcrystalline cellulose has a size of 80-120 μm and a crystallinity of 70-75%.
8. The method as claimed in claim 6, wherein in step b), the quaternized chitosan is prepared from chitosan and 2, 3-epoxypropyltrimethylammonium chloride, the degree of quaternization is 50-80%, and the molecular weight of chitosan is 50000-100000.
9. The method as claimed in claim 6, wherein in step c), the centrifugation speed is 10000-15000 rpm; the cut-off molecular weight of the dialysis bag is 10000.
10. The method of claim 5, wherein the polycarboxylic acid is one or more of butanetetracarboxylic acid, citric acid, and polymaleic acid.
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