CN111455687B - Impregnation processing technology of water-based microfiber synthetic leather - Google Patents
Impregnation processing technology of water-based microfiber synthetic leather Download PDFInfo
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- CN111455687B CN111455687B CN202010296472.1A CN202010296472A CN111455687B CN 111455687 B CN111455687 B CN 111455687B CN 202010296472 A CN202010296472 A CN 202010296472A CN 111455687 B CN111455687 B CN 111455687B
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/12—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins
- D06N3/14—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins with polyurethanes
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0002—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate
- D06N3/0004—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate using ultra-fine two-component fibres, e.g. island/sea, or ultra-fine one component fibres (< 1 denier)
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0002—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate
- D06N3/0011—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate using non-woven fabrics
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0056—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the compounding ingredients of the macro-molecular coating
- D06N3/0063—Inorganic compounding ingredients, e.g. metals, carbon fibres, Na2CO3, metal layers; Post-treatment with inorganic compounds
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/007—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by mechanical or physical treatments
- D06N3/0077—Embossing; Pressing of the surface; Tumbling and crumbling; Cracking; Cooling; Heating, e.g. mirror finish
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0086—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the application technique
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N2211/00—Specially adapted uses
- D06N2211/12—Decorative or sun protection articles
- D06N2211/28—Artificial leather
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
- Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear
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Abstract
The invention discloses an impregnation processing technology of water-based microfiber synthetic leather. The control of the migration of the aqueous polyurethane resin to two sides in the drying process, namely the control of the distribution of the polyurethane resin is crucial to the processing of the aqueous microfiber, but the existing process technology has certain defects. The invention adopts low-concentration univalent electrolyte solution as coagulant aid, and the low-concentration univalent electrolyte solution is matched with waterborne polyurethane resin to form impregnated resin slurry. The resin-impregnated slurry has the characteristics of low viscosity at room temperature, good fluidity and wettability and capability of fully permeating into the microfiber non-woven fabric, but the resin-impregnated slurry has the characteristic of thermal gelation, the temperature is increased, the viscosity of the slurry is rapidly increased to gel, the resin can be solidified at a corresponding position before water is not volatilized, the purpose of fixing the resin before complete drying is achieved, and the migration phenomenon which is difficult to avoid during ordinary hot air drying is effectively prevented.
Description
Technical Field
The invention belongs to the field of microfiber synthetic leather, and particularly relates to an impregnation processing technology of water-based microfiber synthetic leather.
Background
In recent years, as the environmental protection pressure is increasingly severe, some backward genuine leather productivity is gradually eliminated, and the genuine leather market has some atrophy, so that a certain market space is reserved for synthetic leather, wherein especially for microfiber synthetic leather, the microfiber synthetic leather is taken as third-generation artificial leather, and the structure, the performance and the sanitary performance of the microfiber synthetic leather are closer to those of genuine leather; is a good substitute product for genuine leather, and is increasingly accepted by high-end consumer markets in recent years.
However, the conventional microfiber processing adopts oleoresin and wet solidification process, wherein the oleoresin uses DMF as solvent, and then the solvent DMF in the oleoresin is replaced by water in the wet solidification stage to fix the oleoresin. The wet solidification process has the advantages that the microfiber resin is fixed in position in microfiber leather and then dried, and a plurality of holes are left during the replacement of water and DMF during solidification, so that the microfiber leather can be endowed with soft and comfortable hand feeling. The traditional oily microfiber has the defects that DMF must be used as a solvent, the DMF waste water amount is large, the recovery cost is high, the environmental protection risk is high, and the traditional oily microfiber is also a bottleneck for restricting the development of the traditional oily microfiber industry. Wherein, the water-based microfiber is an important direction for environmental protection transformation and upgrading in the microfiber industry. The water-based microfiber is also a hotspot of research in the recent industry, the water-based microfiber solves the problem of environmental protection because the water is used as a solvent to avoid the use of DMF, but simultaneously the wet solidification process can not be adopted any more, and the existing advantages of the wet solidification process can not be inherited, so the retention of the characteristics of the oily process is also a hotspot of research on the water-based microfiber process. Among them, the most prominent is the process of cell retention and solidification. Chinese patent CN110685159A production method for aqueous microfiber synthesis discloses a preparation process of aqueous microfiber, which adopts aqueous polyurethane resin and aqueous acrylic resin to blend as impregnation slurry, and utilizes the hydrolysis of sodium hydroxide on acrylic ester in an alkali weight reduction environment to simultaneously reduce acrylic ester resin in the resin and sea components in sea-island fibers to obtain a base material containing foam pores. Chinese patent CN110607694A, a waterborne microfiber non-woven fabric capable of replacing genuine leather, also discloses a method for preparing foam holes in waterborne microfiber resin: adding a polymer particle which can be dissolved in toluene into the impregnated resin, and dissolving the polymer particle to obtain the cell by utilizing the toluene decrement process.
In addition, it is known in the industry that moisture volatilizes from the middle to the two side surfaces during the drying process after the impregnation with the aqueous resin, and the volatilization of the moisture causes migration of the resin, thereby affecting the distribution state of the resin and affecting the hand feeling.
The oily wet solidification process does not have the defect, and a plurality of proposals are made for solving the problem. In the patent CN102382278B of asahi-chuan chemistry, a water-based polyurethane resin, a preparation method and applications thereof, a wet solidification process is disclosed, in which an aqueous solution of an inorganic ionic compound is used as a water-based solidification solution, and the characteristic that the water-based polyurethane resin is easy to break emulsion when meeting strong electrolyte is utilized to simulate oiliness. In addition, the invention patent of Lanzhou Ketian CN108823679A discloses a wet-process microfiber preparation method, which is also a stepwise process of dipping and salt solidification in a salt solidification tank to simulate an oily wet process. The stepwise solidification process can indeed achieve the effect similar to wet solidification and also effectively avoid migration, but requires the addition of a solidification tank and the production of a corresponding large amount of waste water. In addition, patent CN109134819A "preparation of aqueous polyurethane resin for impregnation of fixed island microfiber synthetic leather" by boston discloses an amphoteric aqueous polyurethane resin, wherein the resin structure contains both anionic and cationic groups, and can be cured and molded without being completely dried, which is also a solution to migration.
Further, Japanese patent CN200880116175.1 discloses a method for producing an artificial leather using a water-based urethane resin composition for artificial leather, a method for producing an artificial leather, and an artificial leather, wherein a water-based urethane resin having a heat-sensitive coagulation effect is prepared by using a nonionic surfactant as an emulsifier by utilizing the property that polyoxyethylene ether has a cloud point at a high temperature, and the heat-sensitivity of the water-based urethane resin is utilized to prevent the migration of the resin to the surface. However, the production process of the nonionic surfactant externally emulsified waterborne polyurethane resin is difficult to control, the particle size of the obtained emulsion is large, the stability is poor, and the nonionic surfactant seriously influences the water resistance and high temperature resistance of the resin.
Chinese patent application No. CN101994263B, patent No. CN101994263B, discloses a method for producing a leather material, in which a fiber base material is impregnated with a mixed solution containing a carboxylic acid and/or carboxylic ester urethane resin, an ammonium salt of an inorganic acid, and water, and then dried to obtain a leather material. However, the inorganic acid ammonium salt and the sodium hydroxide used for alkali deweighting can generate chemical reaction to produce sodium sulfate and ammonia gas, so the method can only be suitable for the leather manufacturing process without deweighting and can not be suitable for the production of the microfiber synthetic leather.
In addition, some thickening agents are adopted to improve the viscosity of the slurry to prevent migration in the drying process, but the adoption of the thickening agents and the improvement of the viscosity inevitably affect the slurry permeation to a certain degree, and especially for a high-gram-weight dense woven base material, the balance of permeation and migration control through the thickening agents is difficult to achieve. The invention discloses waterborne polyurethane microfiber synthetic leather and a preparation method thereof, and discloses a microfiber leather preparation method disclosed in patent No. CN107956134A, which refers to a method of microwave drying, wherein microwave heating is rapid, and microwave is expected to be beneficial to controlling resin migration, but microwave equipment is high in cost and difficult to use as common drying equipment.
From the above, it can be seen that controlling the migration of the aqueous polyurethane resin to both sides in the drying process, i.e. controlling the distribution of the polyurethane resin, is important for the processing of the aqueous microfiber, but the existing process technologies all have certain disadvantages.
Disclosure of Invention
The technical problem to be solved by the present invention is to overcome the defects of the prior art, and to provide a method for processing aqueous microfiber synthetic leather for preventing migration of impregnated resin, wherein a low-concentration monovalent electrolyte solution is used as a coagulant aid, and is matched with an aqueous polyurethane resin to form an impregnated resin slurry, the impregnated resin slurry has a thermal gelation property, the temperature is increased, the viscosity of the slurry is rapidly increased to form gel, the resin can be solidified at a corresponding position before moisture is not volatilized, the purpose of fixing the resin before complete drying is achieved, the migration phenomenon which is difficult to avoid during ordinary hot air drying is effectively prevented, and the method is applicable to a wider range.
Therefore, the invention adopts the following technical scheme: an impregnation processing technology of water-based microfiber synthetic leather comprises the following steps:
1) dissolving the univalent electrolyte with deionized water, and preparing a univalent electrolyte solution with the mass concentration of 0.5-2% as a coagulant aid;
2) according to the mass ratio of the waterborne polyurethane resin to the coagulant aid of 100: uniformly mixing the waterborne polyurethane resin and the coagulant aid in a ratio of 15-100 to obtain waterborne polyurethane resin slurry;
3) carrying out a padding process on the superfine fiber non-woven fabric and the aqueous polyurethane resin slurry to obtain a padded superfine fiber non-woven fabric;
4) and pre-solidifying the padded superfine fiber non-woven fabric through a low-medium temperature hot air oven, and drying the padded superfine fiber non-woven fabric through a high-temperature oven to obtain the impregnated superfine fiber non-woven fabric.
The obtained microfiber-impregnated non-woven fabric is treated by the processes of ordinary weight reduction, dyeing, reduction cleaning, after finishing and the like to obtain microfiber leather.
In the industry, the migration phenomenon in the impregnation and drying process of the water-based microfiber synthetic leather is known in the industry, generally, a commonly adopted countermeasure in the industry is to adopt a thickening agent to improve the viscosity of slurry so as to prevent the migration in the drying process, but the adoption of the thickening agent and the improvement of the viscosity inevitably influence the permeation of the slurry to a certain extent, and especially for a high-gram-weight dense woven base material, the balance of the permeation and the migration is difficult to control through the thickening agent. In addition, there is also reported an aqueous pseudo-wet salt coagulation process, in which an aqueous resin is impregnated and then passed through a salt coagulation tank, and a divalent electrolyte salt is usually selected, but the coagulation effect is also achieved, but the generation of waste water in the salt coagulation tank is increased.
The impregnation resin slurry (namely, the aqueous polyurethane resin slurry) has the characteristics of low viscosity at room temperature, good fluidity and wettability and can fully permeate into the microfiber nonwoven fabric, but the impregnation resin slurry has the characteristic of thermal gelation, the temperature is increased, the viscosity of the slurry is rapidly increased to gel, the resin can be solidified at a corresponding position before the moisture is not volatilized, the purpose of fixing the resin before complete drying is achieved, and the migration phenomenon which is difficult to avoid during ordinary hot air drying can be fully prevented.
Further, in step 1), the monovalent electrolyte is one or more of sodium chloride, potassium chloride, sodium sulfate, potassium sulfate, sodium phosphate and potassium phosphate.
Further, in the step 2), the aqueous polyurethane resin is an electrolyte-sensitive aqueous emulsion.
Furthermore, the aqueous polyurethane resin is preferably a carboxylic acid type aqueous polyurethane resin, and the carboxylic acid type hydrophilic monomer accounts for 2.0-2.6% of the total resin.
Further, in the step 3), the padding process is a multi-padding and multi-rolling process.
Further, in step 3), the padding process is at least a 3-padding 3-rolling process.
Further, in the step 3), the padding process controls the weight ratio of the dry weight gain of the polyurethane resin to the weight of the base fabric to be 0.2-0.4: 1, preferably 0.25 to 0.35: 1.
further, in the step 4), the pre-solidification process comprises a gradient heating step of 3-5min × 50-60 ℃ and 2-5min × 75-85 ℃.
Further, in the step 4), the drying process comprises a gradient heating step of 3-5min × 100-120 ℃ and 1-3min × 140-150 ℃.
Further, the drying in step 4) may be performed by a simple oven, but is not limited to oven drying, and more efficient drying methods such as microwave drying and infrared drying may also be used.
The invention has the following beneficial effects:
according to the thermal gelation scheme provided by the invention, the electrolyte liquid is added into the impregnation slurry, the gelation behavior is triggered by temperature, and the adopted electrolyte coagulant aid has low concentration and small dosage, so that the wastewater amount is small. Meanwhile, the impregnation slurry does not contain a thickening agent, the penetration and wetting performance of the impregnation slurry is not affected, meanwhile, a pre-gelling process is adopted, the resin is solidified before water is not volatilized at a lower temperature, and migration is effectively avoided. Therefore, the invention is a more economical and convenient aqueous microfiber impregnation processing technology, and is particularly suitable for processing thick and dense microfiber leather.
Drawings
FIG. 1 is a graph of migration of a product obtained in example 1 of the present invention by SEM observation;
FIG. 2 is a graph of migration of a product obtained in example 2 of the present invention by SEM observation;
FIG. 3 is a graph of migration of the product obtained in example 3 of the present invention by SEM observation;
FIG. 4 is a graph of migration of a product obtained in example 4 of the present invention by SEM observation;
FIG. 5 is a graph of migration of the product obtained in example 5 of the present invention by SEM observation;
FIG. 6 is a graph of migration of a product obtained in example 6 of the present invention by SEM observation;
FIG. 7 is a graph of migration of the product obtained in example 7 of the present invention by SEM observation;
FIG. 8 is a graph showing migration of a product obtained in comparative example 1 of the present invention by SEM observation;
FIG. 9 is a graph showing migration observed by SEM of a product obtained in comparative example 2 of the present invention.
FIG. 10 is a graph showing migration of a product obtained in comparative example 3 of the present invention by SEM observation.
Detailed Description
The present invention is illustrated by the following specific examples, which include but are not limited to these examples.
Example 1
The unit gram weight of the PET/COPET type island-fixed non-woven fabric is 350g/m 2 And cutting the non-woven base cloth with the weight of 10g for later use. 0.4g of NaCl, 40g of deionized water is used for fully dissolving to obtain a 1% NaCl aqueous solution, and 100g of 35% solid content waterborne polyurethane is addedResin TF-3906 (hydrophilic group content: 2.6%) was mixed well and added to the immersion bath. Immersing 10g of non-woven fabric into an immersion tank, adopting a 3-immersion 3-rolling process, scraping resin on the surface of the non-woven fabric, controlling the liquid carrying rate to be 118% -122%, obtaining a wet pulp non-woven fabric, placing the wet pulp non-woven fabric into a setting machine, presetting according to a gradient temperature rise program of 60 ℃ 3min → 85 ℃ 2min, sending the wet pulp non-woven fabric into a high-temperature setting machine after presetting, completely drying according to a gradient temperature rise program of 100 ℃ 3min → 150 ℃ 1min, and obtaining the impregnated superfine fiber non-woven fabric. The superfine fiber leather can be obtained after the obtained superfine fiber impregnated non-woven fabric is treated by the processes of conventional weight reduction, dyeing, reduction cleaning, after finishing and the like.
Example 2
PA/COPET type island-fixed non-woven fabric with unit gram weight of 300g/m 2 And cutting the non-woven base cloth with the weight of 10g for later use. 1.5g of KCl, fully dissolved by 75g of deionized water to obtain a 2% KCl aqueous solution, added into 100g of aqueous polyurethane resin TF-678 (hydrophilic group content is 2.1%) with solid content of 35%, uniformly mixed and added into an immersion tank. Soaking 10g of prepared non-woven fabric into a soaking tank, adopting a 4-soaking 4-rolling process, scraping resin on the surface of the non-woven fabric, controlling the liquid carrying rate to be 123% -127% to obtain a wet pulp non-woven fabric, placing the wet pulp non-woven fabric into a setting machine, presetting according to a gradient temperature rise program of 60 ℃ 2min → 80 ℃ 3min, sending the wet pulp non-woven fabric into a high-temperature setting machine after presetting, completely drying according to a gradient temperature rise program of 100 ℃ 2min → 140 ℃ 2min, and obtaining the impregnated superfine fiber non-woven fabric. The superfine fiber leather can be obtained after the obtained superfine fiber impregnated non-woven fabric is treated by the processes of conventional weight reduction, dyeing, reduction cleaning, after finishing and the like.
Example 3
PA/COPET type island-fixed non-woven fabric with unit gram weight of 200g/m 2 And cutting the non-woven base cloth with the weight of 10g for later use. 0.24gNa 2 SO 4 And dissolved sufficiently in 16g of deionized water to obtain 1.5% Na 2 SO 4 Adding the aqueous solution into 100g of aqueous polyurethane resin TF-678 with solid content of 35%, uniformly mixing, and adding into an immersion tank. Soaking 10g of non-woven fabric into a soaking tank, scraping resin on the surface of the non-woven fabric by adopting a 3-soaking and 3-rolling process, controlling the liquid carrying rate to be 81-85 percent, and obtaining the wet pulp non-woven fabricAnd placing the fabric in a setting machine, presetting according to a gradient temperature increasing program of 50 ℃ for 3min → 75 ℃ for 2min, sending the preset fabric into a high-temperature setting machine, completely drying according to a gradient temperature increasing program of 100 ℃ for 3min → 150 ℃ for 1min, and obtaining the impregnated superfine fiber non-woven fabric. The superfine fiber leather can be obtained after the obtained superfine fiber impregnated non-woven fabric is treated by the processes of conventional weight reduction, dyeing, reduction cleaning, after finishing and the like.
Example 4
PA/COPET type island-fixed non-woven fabric with unit gram weight of 200g/m 2 And cutting a non-woven base fabric with the weight of 10g for later use. 1.25g K 2 SO 4 Dissolved sufficiently in 50g of deionized water to give 2.5% K 2 SO 4 Adding the aqueous solution into 100g of aqueous polyurethane resin TF-678 with solid content of 35%, uniformly mixing, and adding into an immersion tank. Immersing 10g of non-woven fabric into an impregnation tank, adopting a 3-immersion 3-rolling process, scraping resin on the surface of the non-woven fabric, controlling the liquid carrying rate to be 85% -90%, obtaining a wet pulp non-woven fabric, placing the wet pulp non-woven fabric into a setting machine, presetting according to a gradient temperature rise program of 50 ℃ for 5min → 75 ℃ for 5min, sending the wet pulp non-woven fabric into a high-temperature setting machine after presetting, completely drying according to a gradient temperature rise program of 100 ℃ for 5min → 140 ℃ for 3min, and obtaining the impregnated superfine fiber non-woven fabric. The superfine fiber leather can be obtained after the obtained superfine fiber impregnated non-woven fabric is treated by the processes of conventional weight reduction, dyeing, reduction cleaning, after finishing and the like.
Example 5
The unit gram weight of the PET/COPET type figured-island non-woven fabric is 350g/m 2 And cutting the non-woven base cloth with the weight of 10g for later use. 0.5gNa 3 PO 4 Fully dissolved by 100g of deionized water to obtain 0.5 percent of Na 3 PO 4 Adding the aqueous solution into 100g of aqueous polyurethane resin TF-3906 with the solid content of 35%, uniformly mixing, and then adding into an immersion tank. Immersing 10g of non-woven fabric into an immersion tank, adopting a 3-immersion 3-rolling process, scraping resin on the surface of the non-woven fabric, controlling the liquid carrying rate to be 168% -172%, obtaining a wet pulp non-woven fabric, placing the wet pulp non-woven fabric into a setting machine, presetting according to a gradient temperature-rising program of 60 ℃ for 3min → 80 ℃ for 4min, sending the wet pulp non-woven fabric into a high-temperature setting machine after presetting, completely drying according to a gradient temperature-rising program of 120 ℃ for 5min → 150 ℃ for 3min, and obtaining the immersion liquidSoaking the superfine fiber non-woven fabric. The superfine fiber leather can be obtained after the obtained superfine fiber impregnated non-woven fabric is treated by the processes of conventional weight reduction, dyeing, reduction cleaning, after finishing and the like.
Example 6
The unit gram weight of the PET/COPET type island-fixed non-woven fabric is 280g/m 2 And cutting the non-woven base cloth with the weight of 10g for later use. 0.1g K 3 PO 4 Dissolved sufficiently in 20g of deionized water to give 0.5% K 3 PO 4 Adding the aqueous solution into 100g of aqueous polyurethane resin TF-3906 with the solid content of 35%, uniformly mixing, and then adding into an immersion tank. Immersing 10g of non-woven fabric into an immersion tank, adopting a 3-immersion 3-rolling process, scraping resin on the surface of the non-woven fabric, controlling the liquid carrying rate to be 135% -140%, obtaining wet pulp non-woven fabric, placing the wet pulp non-woven fabric into a setting machine, presetting according to a gradient temperature rise program of 55 ℃ 4min → 80 ℃ 3min, sending the wet pulp non-woven fabric into a high-temperature setting machine after presetting, completely drying according to a gradient temperature rise program of 110 ℃ 3min → 140 ℃ 3min, and obtaining the impregnated superfine fiber non-woven fabric. The obtained superfine fiber impregnated non-woven fabric can be treated by the processes of conventional weight reduction, dyeing, reduction cleaning, after finishing and the like to obtain superfine fiber leather.
Example 7
The unit gram weight of the PET/COPET type island-fixed non-woven fabric is 350g/m 2 And cutting the non-woven base cloth with the weight of 10g for later use. 1.5g NaCl, 100g deionized water is fully dissolved to obtain 1.5% NaCl aqueous solution, 100g 50% solid content aqueous polyurethane resin Impranil 1068 is added, mixed evenly and added into the soaking tank. Immersing 10g of non-woven fabric into an impregnation tank, adopting a 3-dipping 3-rolling process, scraping resin on the surface of the non-woven fabric, controlling the liquid carrying rate to be 118% -122%, obtaining a wet pulp non-woven fabric, placing the wet pulp non-woven fabric into a setting machine, presetting according to a gradient temperature-rising program of 60 ℃ 3min → 85 ℃ 2min, sending the wet pulp non-woven fabric into a high-temperature setting machine after presetting, completely drying according to a gradient temperature-rising program of 100 ℃ 3min → 150 ℃ 1min, and obtaining the impregnated superfine fiber non-woven fabric. The superfine fiber leather can be obtained after the obtained superfine fiber impregnated non-woven fabric is treated by the processes of conventional weight reduction, dyeing, reduction cleaning, after finishing and the like.
Comparative example 1
PETCOPET type island-fixed nonwoven fabric with unit gram weight of 350g/m 2 And cutting the non-woven base cloth with the weight of 10g for later use. 40g of deionized water is added into 100g of 35% solid content aqueous polyurethane resin TF-3906, and the mixture is added into a soaking tank after being uniformly mixed. Immersing 10g of non-woven fabric into an impregnation tank, adopting a 3-dipping 3-rolling process, scraping resin on the surface of the non-woven fabric, controlling the liquid carrying rate to be 118% -122%, obtaining a wet pulp non-woven fabric, placing the wet pulp non-woven fabric into a setting machine, presetting according to a gradient temperature-rising program of 60 ℃ 3min → 85 ℃ 2min, sending the wet pulp non-woven fabric into a high-temperature setting machine after presetting, completely drying according to a gradient temperature-rising program of 100 ℃ 3min → 150 ℃ 1min, and obtaining the impregnated superfine fiber non-woven fabric. The superfine fiber leather can be obtained after the obtained superfine fiber impregnated non-woven fabric is treated by the processes of conventional weight reduction, dyeing, reduction cleaning, after finishing and the like.
Comparative example 2
The unit gram weight of the PA/COPET type figured island non-woven fabric is 300g/m 2 And cutting the non-woven base cloth with the weight of 10g for later use. 75g of deionized water is added into 100g of aqueous polyurethane resin TF-678 with the solid content of 35 percent, and the mixture is added into a soaking tank after being uniformly mixed. Soaking 10g of prepared non-woven fabric into a soaking tank, adopting a 4-soaking 4-rolling process, scraping resin on the surface of the non-woven fabric, controlling the liquid carrying rate to be 123% -127% to obtain a wet pulp non-woven fabric, placing the wet pulp non-woven fabric into a setting machine, presetting according to a gradient temperature rise program of 60 ℃ 2min → 80 ℃ 3min, sending the wet pulp non-woven fabric into a high-temperature setting machine after presetting, completely drying according to a gradient temperature rise program of 100 ℃ 2min → 140 ℃ 2min, and obtaining the impregnated superfine fiber non-woven fabric. The superfine fiber leather can be obtained after the obtained superfine fiber impregnated non-woven fabric is treated by the processes of conventional weight reduction, dyeing, reduction cleaning, after finishing and the like.
Comparative example 3
The unit gram weight of the PET/COPET type island-fixed non-woven fabric is 350g/m 2 And cutting the non-woven base cloth with the weight of 10g for later use. 100g of deionized water is added into 100g of 50% solid content waterborne polyurethane resin Impranil 1068, and the mixture is added into a soaking tank after being uniformly mixed. After 10g of non-woven fabric is immersed in an immersion tank, a 3-immersion 3-rolling process is adopted, resin on the surface of the non-woven fabric is scraped off, the liquid carrying rate is controlled to be 118% -122%, a wet pulp non-woven fabric is obtained, and the wet pulp non-woven fabric is placed in a setting machinePre-shaping according to a gradient temperature increasing program of 60 ℃ 3min → 85 ℃ 2min, sending the pre-shaped material into a high-temperature shaping machine after pre-shaping, and completely drying according to a gradient temperature increasing program of 100 ℃ 3min → 150 ℃ 1min to obtain the impregnated superfine fiber non-woven fabric. The superfine fiber leather can be obtained after the obtained superfine fiber impregnated non-woven fabric is treated by the processes of conventional weight reduction, dyeing, reduction cleaning, after finishing and the like.
And (3) observing the migration condition:
the microfiber leather sample prepared in the embodiment is sampled, and SEM photograph results of migration conditions of the sample bottle are shown in the figure by adopting SEM.
Statistics of migration observations
| Example numbering | Migration situation | Comparative example no | Migration situation |
| 1 | Is not obvious | 1 | Is obvious |
| 2 | Is not obvious | 2 | Is obvious |
| 3 | Is not obvious | ||
| 4 | Is not obvious | ||
| 5 | Is not obvious | ||
| 6 | Is not obvious | ||
| 7 | Slight swimming movement | 3 | Is obvious |
From the comparison results, the low-concentration electrolyte thermally-induced coagulation aiding scheme provided by the invention can effectively avoid the occurrence of migration, and meanwhile, the nonuniform wetting and penetration caused by the low viscosity of the working solution is fully avoided. In addition, as can be seen from example 7 and comparative example 3, the low-concentration electrolyte thermal-assisted coagulation scheme provided by the invention is effective for most of microfiber-impregnated emulsions, but the specific effect has a certain correlation with the electrolyte resistance level of the corresponding emulsion, and the migration prevention effect of the low-concentration electrolyte thermal-assisted coagulation provided by the invention is correspondingly reduced for the emulsion with better electrolyte resistance.
Claims (7)
1. An impregnation processing technology of water-based microfiber synthetic leather is characterized by comprising the following steps:
1) dissolving the univalent electrolyte with deionized water, and preparing a univalent electrolyte solution with the mass concentration of 0.5-2% as a coagulant aid;
2) according to the mass ratio of the waterborne polyurethane resin to the coagulant aid of 100: uniformly mixing the waterborne polyurethane resin and the coagulant aid in a ratio of 15-100 to obtain waterborne polyurethane resin slurry;
3) carrying out a padding process on the superfine fiber non-woven fabric and the aqueous polyurethane resin slurry to obtain a padded superfine fiber non-woven fabric;
4) the padding superfine fiber non-woven fabric is pre-solidified by a low-medium temperature hot air oven and is dried by a high-temperature oven to obtain the impregnated superfine fiber non-woven fabric;
in the step 1), the monovalent electrolyte is one or a mixture of more of sodium chloride, potassium chloride, sodium sulfate, potassium sulfate, sodium phosphate and potassium phosphate;
in the step 2), the aqueous polyurethane resin is an electrolyte sensitive aqueous emulsion, a carboxylic acid type aqueous polyurethane resin is selected, and the carboxylic acid type hydrophilic monomer accounts for 2.0-2.6% of the total amount of the resin.
2. The impregnation processing process for the aqueous microfiber synthetic leather according to claim 1, wherein in step 3), the padding process is a multi-impregnation and multi-rolling process.
3. The impregnation processing process of the waterborne microfiber synthetic leather according to claim 2, wherein in step 3), the padding process is at least a 3-in-3 process.
4. The impregnation processing process of the water-based microfiber synthetic leather according to claim 1, wherein in step 3), the padding process controls the ratio of the dry weight gain of the polyurethane resin to the weight of the base fabric to be 0.2-0.4: 1.
5. the impregnation processing process of the water-based microfiber synthetic leather according to claim 4, wherein in step 3), the padding process controls the ratio of the dry weight gain of the polyurethane resin to the weight of the base fabric to be 0.25 to 0.35: 1.
6. the impregnation processing process of the waterborne microfiber synthetic leather according to claim 1, wherein in step 4), the pre-coagulation process comprises a gradient temperature rise step of 60 ℃ for 3-5min and 80 ℃ for 2-5 min.
7. The impregnation processing process of the waterborne microfiber synthetic leather according to claim 1, wherein in step 4), the drying process comprises a gradient temperature rise step of 5min 100 ℃ and 3-5min 150 ℃.
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| CN105178055A (en) * | 2015-10-15 | 2015-12-23 | 四川大学 | Water-saving superfine fiber synthetic leather base cloth impregnation method based on cationic water-based polyurethane |
| CN106192449A (en) * | 2016-08-17 | 2016-12-07 | 福建鑫发无纺布有限责任公司 | A kind of full aqueous, environmental protective superfine fiber leather manufacture method |
| CN106868880A (en) * | 2017-04-10 | 2017-06-20 | 合肥科天水性科技有限责任公司 | A kind of aqueous polyurethane imitates woven fabric and its manufacture method |
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