CN102899918A - Method for producing wet-process waterborne polyurethane synthetic leather coating base - Google Patents
Method for producing wet-process waterborne polyurethane synthetic leather coating base Download PDFInfo
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- CN102899918A CN102899918A CN2012103901195A CN201210390119A CN102899918A CN 102899918 A CN102899918 A CN 102899918A CN 2012103901195 A CN2012103901195 A CN 2012103901195A CN 201210390119 A CN201210390119 A CN 201210390119A CN 102899918 A CN102899918 A CN 102899918A
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Abstract
The invention relates to a method for producing a wet-process waterborne polyurethane synthetic leather coating base. The method comprises the following steps of: coating slurry on non-woven cloth by using a scraper of a blade coating machine in the coating amount of 80 to 380 g/m<2>; mixing 5 to 15 mass parts of demulsifier, 0.5 to 3 mass parts of cross-linking agent, 1 to 5 mass parts of 10 percent acid solution and 80 to 90 mass parts of water uniformly to obtain solidification liquid; allowing the non-woven cloth containing the coating slurry to pass through the solidification liquid; and washing the non-woven cloth, wringing and drying to obtain the wet-process waterborne polyurethane synthetic leather coating base. By the method, the problems of the pollution of a solvent of dimethylformamide and unsafety of products caused by dimethylformamide residues in the production of a solvent type wet-process polyurethane coating base can be solved; and the product has high physical and mechanical properties, water-vapor permeability and handfeel characteristics.
Description
Technical field
The present invention relates to the Synthetic Leather technical field, particularly a kind of production method of aqueous polyurethane synthetic leather wet-process coating bass.
Background technology
Synthetic leather is institutional framework and the serviceability of simulation natural leather, and can be used as the composite of natural leather substitute.Usually with nonwoven fabric simulation lamina reticularis, with microvoid polyurethane coating simulation grain layer, resulting synthetic leather positive and negative are all quite similar with leather, and have certain gas permeability,, be widely used in and make footwear, boots, case and bag and ball etc. more near natural leather than ordinary people fabricate-leather.
Show according to the national statistics office data: (the new criteria for classifying: annual sales revenue 2000 ten thousand above enterprises) 495,2,410,000 tons of output increase by 9.57% to the above enterprise of artificial leather synthetic leather scale in 2011; 925.35 hundred million yuan of total industrial output values increase by 29.55%; 69.85 hundred million yuan of profits taxes increase by 32.12%; 47.86 hundred million yuan of total profits increase by 36.15%.All in all, in the situation of large economic environment recovery, China's Synthetic Leather shows rapid growth momentum.
Bass utilizes aqueous polyurethane synthetic leather wet-process coating bass at synthetic leather industry middle finger semi-finished product, by the processing technology of follow-up routine, can produce all kinds of synthetic leather products.
At present, solvent type production method is mainly adopted in the production of Synthetic Leather wet-process coating bass, and its typical process flow is as follows: non-weaving cloth → blade coating → solidify → wash → water squeezing → drying → coating bass.This production technology adopts solvent borne polyurethane, pigment and dimethyl formamide (MDF) for the coating paste that main component forms, and at first is to utilize doctor knife coater to be coated on the non-weaving cloth, then enters DMF and H
2O is in the solidification liquid of main component composition, because solvent borne polyurethane and H
2O incompatible and DMF and H
2The unconfined of O dissolves each other, so that solvent borne polyurethane/DMF system is because H
2The existence of O, DMF and H
2Move towards phase double replacement between the O, so that DMF is by H
2O extracts, and is final so that solvent borne polyurethane forms micro porous coating, thereby obtains solvent borne polyurethane wet-process coating bass.This production method can produce two great problems, and the first has adopted DMF to make solvent, and process can cause the solvent contamination of DMF; It two is H
2O is the DMF in the replacement solvent type polyurethane completely, can cause that the DMF of product is residual, finally causes the product safety problem.
According to the production method of above-mentioned solvent borne polyurethane synthetic leather wet-process coating bass, production process exists serious MDF problem of environmental pollution, is a non-clean production process, and human body is had larger harm.The residual product safety problem that causes that occurs easily DMF in the resulting Synthetic Leather.
Summary of the invention
The production method that the purpose of this invention is to provide a kind of aqueous polyurethane synthetic leather wet-process coating bass, with solve the DMF pollution problem that produces in the production of present solvent borne polyurethane synthetic leather wet-process coating bass and synthetic leather produce in the residual product safety problem that causes of product DMF.
For achieving the above object, the technical solution used in the present invention is:
Step 1, at first, be that 30% aqueous polyurethane, 5～10 parts of solid contents are that 25% aqueous pigment cream and 1～10 part of solid content are that 20% aqueous gelatin solution mixes by mass fraction with 70～85 parts of solid contents, namely get coating paste through vacuumizing and defoaming, filtered through gauze;
Then, by doctor knife coater coating paste is coated in the non-weaving cloth surface, the coating weight of coating paste is 80～380g/m
2
Step 2, at first is that 10% acid solution and 80～90 parts of water mix and make demulsifier dissolve to get solidification liquid fully by mass fraction with 5～15 parts of demulsifiers, 0.5～3 part of crosslinking agent, 1～5 part of mass fraction;
Then, the non-weaving cloth of the coating slurry of step 1 by solidification liquid, is formed porous polyurethane coating;
Step 3, the non-weaving cloth washing with step 2, water squeezing and the dry aqueous polyurethane synthetic leather wet-process coating bass that gets.
It is the anion-type water-thinned polyurethane of carboxylate radical or sulfonate radical that described aqueous polyurethane adopts hydrophilic radical.
The water stain that described aqueous pigment cream adopts natural leather or synthetic leather suitability for industrialized production to use.
Described demulsifier is water-soluble magnesium salt, water-soluble Ca salt or water-soluble zinc salt.
Water-soluble magnesium salt is one or both in magnesium chloride, the magnesium nitrate; Water-soluble Ca salt is one or both in calcium chloride, the calcium nitrate; Water-soluble zinc salt is the mixture of one or more arbitrary proportions in zinc sulfate, zinc chloride, the zinc acetate.
Described crosslinking agent is the mixture of one or more arbitrary proportions in aziridine, carbodiimides, trimethylol melamine, the hexa methoxy methylene tri poly cyanamid.
Described acid solution is the mixture of one or more arbitrary proportions in formic acid, acetic acid, propionic acid, sulfuric acid, the hydrochloric acid.
The coating paste temperature that is coated in the step 1 on the non-weaving cloth is 20～50 ℃, and the solidification liquid temperature that non-weaving cloth passes through in the step 2 is 20～80 ℃; The pH that is washed to aqueous polyurethane synthetic leather wet-process coating bass in the step 3 is 6～7.
With respect to prior art, the present invention has following beneficial effect: use polyurethane coating slurry has replaced solvent borne polyurethane and DMF(dimethyl formamide) coating paste that forms, the solidification liquid that the solidification liquid that forms with demulsifier, crosslinking agent, acid solution and water has replaced DMF and water to form, also just eliminate use and the pollution problem of DMF, also eliminated the product safety problem that causes because DMF is residual in the solvent borne polyurethane synthetic leather wet method bass simultaneously.The production environment of a safety can be provided, be of value to the healthy of workman; Resulting aqueous polyurethane synthetic leather wet-process coating bass is compared with solvent borne polyurethane synthetic leather wet-process coating bass, coating has the microcellular structure of very similar connection, and aqueous polyurethane synthetic leather wet-process coating bass has better physical and mechanical properties, gas permeability, water vapor permeability, moisture absorption hydrofuge and feel characteristic.
The specific embodiment
The present invention is described in further detail below by the specific embodiment, but the present invention has more than and is limited to these examples.
Embodiment 1:
Step 1, at first, be that 30% hydrophilic radical is that the anion-type water-thinned polyurethane of carboxylate radical, 6 parts of solid contents are that the water stain that uses of 25% natural leather suitability for industrialized production and 2 parts of solid contents are that 20% aqueous gelatin solution mixes by mass fraction with 70 parts of solid contents, namely get coating paste through vacuumizing and defoaming, filtered through gauze;
Then, be that 20 ℃ coating paste is coated in the non-weaving cloth surface by doctor knife coater with temperature, the coating weight of coating paste is 200g/m
2
Step 2, at first is that 10% formic acid and 80 parts of water mix and make demulsifier dissolve to get solidification liquid fully by mass fraction with 5 parts of demulsifier magnesium chlorides, 0.5 part of crosslinking agent aziridine, 1 part of mass fraction;
Then, be 40 ℃ of solidification liquids with the non-weaving cloth of the coating slurry of step 1 by temperature, form porous polyurethane coating;
Step 3, with the non-weaving cloth of step 2 be washed to that pH is 6, water squeezing and dry aqueous polyurethane synthetic leather wet-process coating bass.
Embodiment 2:
Step 1, at first, be that 30% hydrophilic radical is that the anion-type water-thinned polyurethane of sulfonate radical, 8 parts of solid contents are that the water stain that uses of 25% synthetic leather suitability for industrialized production and 7 parts of solid contents are that 20% aqueous gelatin solution mixes by mass fraction with 80 parts of solid contents, namely get coating paste through vacuumizing and defoaming, filtered through gauze;
Then, be that 40 ℃ coating paste is coated in the non-weaving cloth surface by doctor knife coater with temperature, the coating weight of coating paste is 160g/m
2
Step 2, at first is that 10% acetic acid and 90 parts of water mix and make demulsifier dissolve to get solidification liquid fully by mass fraction with the mixture of 15 parts of demulsifier magnesium chlorides and magnesium nitrate, 2.5 parts of crosslinking agent carbodiimides, 5 parts of mass fractions;
Then, be 60 ℃ of solidification liquids with the non-weaving cloth of the coating slurry of step 1 by temperature, form porous polyurethane coating;
Step 3, with the non-weaving cloth of step 2 be washed to that pH is 7, water squeezing and dry aqueous polyurethane synthetic leather wet-process coating bass.
Embodiment 3:
Step 1, at first, be that 30% hydrophilic radical is that the anion-type water-thinned polyurethane of carboxylate radical, 5 parts of solid contents are that the water stain that uses of 25% natural leather suitability for industrialized production and 1 part of solid content are that 20% aqueous gelatin solution mixes by mass fraction with 72 parts of solid contents, namely get coating paste through vacuumizing and defoaming, filtered through gauze;
Then, be that 50 ℃ coating paste is coated in the non-weaving cloth surface by doctor knife coater with temperature, the coating weight of coating paste is 300g/m
2
Step 2, at first is that 10% propionic acid and 83 parts of water mix and make demulsifier dissolve to get solidification liquid fully by mass fraction with 8 parts of demulsifier calcium chloride, 1 part of crosslinking agent trimethylol melamine, 2 parts of mass fractions;
Then, be 80 ℃ of solidification liquids with the non-weaving cloth of the coating slurry of step 1 by temperature, form porous polyurethane coating;
Step 3, with the non-weaving cloth of step 2 be washed to that pH is 6.5, water squeezing and dry aqueous polyurethane synthetic leather wet-process coating bass.
Embodiment 4:
Step 1, at first, be that 30% hydrophilic radical is that the anion-type water-thinned polyurethane of sulfonate radical, 7 parts of solid contents are that the water stain that uses of 25% synthetic leather suitability for industrialized production and 5 parts of solid contents are that 20% aqueous gelatin solution mixes by mass fraction with 75 parts of solid contents, namely get coating paste through vacuumizing and defoaming, filtered through gauze;
Then, be that 35 ℃ coating paste is coated in the non-weaving cloth surface by doctor knife coater with temperature, the coating weight of coating paste is 80g/m
2
Step 2, at first is that 10% sulfuric acid and 85 parts of water mix and make demulsifier dissolve to get solidification liquid fully by mass fraction with the mixture of 10 parts of demulsifier calcium chloride and calcium nitrate, 2 parts of crosslinking agent hexa methoxy methylene tri poly cyanamids, 4 parts of mass fractions;
Then, be 20 ℃ of solidification liquids with the non-weaving cloth of the coating slurry of step 1 by temperature, form porous polyurethane coating;
Step 3, with the non-weaving cloth of step 2 be washed to that pH is 6.8, water squeezing and dry aqueous polyurethane synthetic leather wet-process coating bass.
Embodiment 5:
Step 1, at first, be that 30% hydrophilic radical is that the anion-type water-thinned polyurethane of carboxylate radical, 10 parts of solid contents are that the water stain that uses of 25% natural leather suitability for industrialized production and 10 parts of solid contents are that 20% aqueous gelatin solution mixes by mass fraction with 85 parts of solid contents, namely get coating paste through vacuumizing and defoaming, filtered through gauze;
Then, be that 45 ℃ coating paste is coated in the non-weaving cloth surface by doctor knife coater with temperature, the coating weight of coating paste is 140g/m
2
Step 2, at first is that 10% hydrochloric acid and 88 parts of water mix and make demulsifier dissolve to get solidification liquid fully by mass fraction with the mixture of 12 parts of demulsifier zinc sulfate, 3 parts of crosslinking agent aziridine and carbodiimides, 5 parts of mass fractions;
Then, be 50 ℃ of solidification liquids with the non-weaving cloth of the coating slurry of step 1 by temperature, form porous polyurethane coating;
Step 3, with the non-weaving cloth of step 2 be washed to that pH is 6.3, water squeezing and dry aqueous polyurethane synthetic leather wet-process coating bass.
Embodiment 6:
Step 1, at first, be that 30% hydrophilic radical is that the anion-type water-thinned polyurethane of sulfonate radical, 9 parts of solid contents are that the water stain that uses of 25% synthetic leather suitability for industrialized production and 8 parts of solid contents are that 20% aqueous gelatin solution mixes by mass fraction with 83 parts of solid contents, namely get coating paste through vacuumizing and defoaming, filtered through gauze;
Then, be that 30 ℃ coating paste is coated in the non-weaving cloth surface by doctor knife coater with temperature, the coating weight of coating paste is 380g/m
2
Step 2, at first is that the mixture of 10% formic acid and hydrochloric acid and 86 parts of water mix and make demulsifier dissolve to get solidification liquid fully by mass fraction with the mixture of the mixture of 13 parts of demulsifier zinc sulfate, zinc chloride and zinc acetates, 1.5 parts of crosslinking agent trimethylol melamines and hexa methoxy methylene tri poly cyanamid, 3 parts of mass fractions;
Then, be 70 ℃ of solidification liquids with the non-weaving cloth of the coating slurry of step 1 by temperature, form porous polyurethane coating;
Step 3, with the non-weaving cloth of step 2 be washed to that pH is 6.5, water squeezing and dry aqueous polyurethane synthetic leather wet-process coating bass.
The non-weaving cloth that the present invention adopts is called again nonwoven fabric, can be various non-weaving cloths.
Key technology of the present invention and principle have following some:
One, the bright anion-type water-thinned polyurethane that utilizes of this law has replaced solvent borne polyurethane, can not use any solvent in the production process, can solve the DMF pollution problem that produces in the present solvent borne polyurethane synthetic leather wet-process coating bass production fully; Its two, the aqueous polyurethane synthetic leather wet-process coating bass that the present invention produces does not contain MDF in the product, can solve fully in the present solvent borne polyurethane synthetic leather wet-process coating bass because the residual safety problem that causes of DMF; Its three owing to do not use DMF, compare with the production of solvent borne polyurethane synthetic leather wet-process coating bass, save the DMF removal process, whole energy-saving production technology consumption reduction; Its four, can not use any solvent in the whole production process, the production environment of a safety can be provided, be of value to the healthy of workman; They are five years old, resulting aqueous polyurethane synthetic leather wet-process coating bass is compared with solvent borne polyurethane synthetic leather wet-process coating bass, coating has the microcellular structure of very similar connection, and aqueous polyurethane synthetic leather wet-process coating bass has better physical and mechanical properties, gas permeability, water vapor permeability, moisture absorption hydrofuge and feel characteristic.
The aqueous gelatin solution that adopts can play multiple effect, and one can play good thickening power, makes coating paste reach the viscosity requirement of coating; Its two, can increase the thixotropy of coating paste, prevent the infiltration non-weaving cloth that coating paste is too much; Its three, can play and help freezing action, coating paste is entered after the solidification liquid, solidify with speed faster on the surface, thereby prevent that slurry is dispersed in the solidification liquid; Its four, gelatin can form three-dimensional net structure under the effect of crosslinking agent, thereby improves the physical and mechanical properties of coating; Its five, gelatin is a kind of protide material, can improve flatness and the smooth feeling of coating.
After the non-weaving cloth of coating slurry immerses solidification liquid, one, the hydrogen ion (H that acid solution provides
+), with the hydrophilic radical carboxylate radical (COO in the anion-type water-thinned polyurethane
-) and sulfonate radical (SO
3 -) be converted into carboxylate radical (COOH) and sulfonate radical (SO
3H), because-COOH or-SO
3The hydrophily of H is far smaller than-COO
-With-SO
3 -So the stability of anion-type water-thinned polyurethane in the aqueous solution has decline; Its two, the CATION of demulsifier, i.e. divalence magnesium ion (Mg
2+), divalent calcium ion (Ca
2+), divalent zinc ion (Zn
2+) can be further sealing-COO
-With-SO
3 -, the stable utmost point of anion-type water-thinned polyurethane in the aqueous solution reduced; Its three, crosslinking agent can and anion-type water-thinned polyurethane produce crosslinked action, the stability of reduction anionic soluble polyurethane in the aqueous solution.Under above-mentioned triple role, the anion aqueous polyurethane breakdown of emulsion solidifies, and forms the polyurethane coating with microcellular structure.
The aqueous gelatin solution that adopts can play multiple effect, and one can play good thickening power, makes coating paste reach the viscosity requirement of coating; Its two, can increase the thixotropy of coating paste, prevent the infiltration non-weaving cloth that coating paste is too much; Its three, can play and help freezing action, coating paste is entered after the solidification liquid, solidify with speed faster on the surface, thereby prevent that slurry is dispersed in the solidification liquid; Its four, gelatin can form three-dimensional net structure under the effect of crosslinking agent, thereby improves the physical and mechanical properties of coating; Its five, gelatin is a kind of protide material, can improve flatness and the smooth feeling of coating.
Crosslinking agent has crosslinked ability to aqueous polyurethane, and aqueous polyurethane is thoroughly solidified, and improves the mechanical property of polyurethane gel coating.
Acid solution can be regulated the pH of solidification liquid, and hydrogen ion (H is provided
+).
Resulting aqueous polyurethane synthetic leather wet-process coating bass is compared with solvent borne polyurethane synthetic leather wet-process coating bass, coating has the microcellular structure of very similar connection, and aqueous polyurethane synthetic leather wet-process coating bass has better physical and mechanical properties, gas permeability, water vapor permeability, moisture absorption hydrofuge and feel characteristic, sees also shown in the table 1.
The key property contrast of two kinds of Synthetic Leather wet-process coatings of table 1 bass
Annotate: the A sample is solvent borne polyurethane synthetic leather wet-process coating bass; The B sample is aqueous polyurethane synthetic leather wet-process coating bass; A sample and B sample adopt same non-weaving cloth as base cloth.
Claims (8)
1. the production method of an aqueous polyurethane synthetic leather wet-process coating bass is characterized in that: may further comprise the steps:
Step 1, at first, be that 30% aqueous polyurethane, 5～10 parts of solid contents are that 25% aqueous pigment cream and 1～10 part of solid content are that 20% aqueous gelatin solution mixes by mass fraction with 70～85 parts of solid contents, namely get coating paste through vacuumizing and defoaming, filtered through gauze;
Then, by doctor knife coater coating paste is coated in the non-weaving cloth surface, the coating weight of coating paste is 80～380g/m
2
Step 2, at first is that 10% acid solution and 80～90 parts of water mix and make demulsifier dissolve to get solidification liquid fully by mass fraction with 5～15 parts of demulsifiers, 0.5～3 part of crosslinking agent, 1～5 part of mass fraction;
Then, the non-weaving cloth of the coating slurry of step 1 by solidification liquid, is formed porous polyurethane coating;
Step 3, the non-weaving cloth washing with step 2, water squeezing and the dry aqueous polyurethane synthetic leather wet-process coating bass that gets.
2. the production method of a kind of aqueous polyurethane synthetic leather wet-process coating bass according to claim 1 is characterized in that: it is the anion-type water-thinned polyurethane of carboxylate radical or sulfonate radical that described aqueous polyurethane adopts hydrophilic radical.
3. the production method of a kind of aqueous polyurethane synthetic leather wet-process coating bass according to claim 1 is characterized in that: the water stain that described aqueous pigment cream adopts natural leather or synthetic leather suitability for industrialized production to use.
4. the production method of a kind of aqueous polyurethane synthetic leather wet-process coating bass according to claim 1, it is characterized in that: described demulsifier is water-soluble magnesium salt, water-soluble Ca salt or water-soluble zinc salt.
5. the production method of a kind of aqueous polyurethane synthetic leather wet-process coating bass according to claim 4, it is characterized in that: water-soluble magnesium salt is one or both in magnesium chloride, the magnesium nitrate; Water-soluble Ca salt is one or both in calcium chloride, the calcium nitrate; Water-soluble zinc salt is the mixture of one or more arbitrary proportions in zinc sulfate, zinc chloride, the zinc acetate.
6. the production method of a kind of aqueous polyurethane synthetic leather wet-process coating bass according to claim 1, it is characterized in that: described crosslinking agent is the mixture of one or more arbitrary proportions in aziridine, carbodiimides, trimethylol melamine, the hexa methoxy methylene tri poly cyanamid.
7. the production method of a kind of aqueous polyurethane synthetic leather wet-process coating bass according to claim 1, it is characterized in that: described acid solution is the mixture of one or more arbitrary proportions in formic acid, acetic acid, propionic acid, sulfuric acid, the hydrochloric acid.
8. the production method of a kind of aqueous polyurethane synthetic leather wet-process coating bass according to claim 1, it is characterized in that: the coating paste temperature that is coated in the step 1 on the non-weaving cloth is 20～50 ℃, and the solidification liquid temperature that non-weaving cloth passes through in the step 2 is 20～80 ℃; The pH that is washed to aqueous polyurethane synthetic leather wet-process coating bass in the step 3 is 6～7.
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| CN103981729A (en) * | 2014-05-07 | 2014-08-13 | 安安(中国)有限公司 | Aqueous polyurethane making method used for superfine fiber synthetic leather production |
| CN104250939A (en) * | 2013-06-28 | 2014-12-31 | 桐乡市高桥皮革有限责任公司 | Method for re-fixing color of leather finished product |
| CN106917298A (en) * | 2017-04-21 | 2017-07-04 | 齐鲁工业大学 | A kind of preparation method of high color fastness dyeing-free superfine fiber chemical leather bass |
| CN108586692A (en) * | 2018-01-23 | 2018-09-28 | 陕西科技大学 | A kind of use for synthetic leather can polish the preparation method and application of aqueous polyurethane |
| CN109680507A (en) * | 2018-07-23 | 2019-04-26 | 北华航天工业学院 | The preparation method of the new application and aqueous ecological synthetic leather wet process bass of lanthanum acetate and cerous acetate |
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| CN106917298A (en) * | 2017-04-21 | 2017-07-04 | 齐鲁工业大学 | A kind of preparation method of high color fastness dyeing-free superfine fiber chemical leather bass |
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| CN111041844A (en) * | 2019-12-24 | 2020-04-21 | 兰州科天水性高分子材料有限公司 | Anti-siphon shoe leather base and preparation method thereof |
| CN111286991A (en) * | 2020-03-19 | 2020-06-16 | 合肥科天水性科技有限责任公司 | Air filter medium and preparation method thereof |
| CN115961480A (en) * | 2022-12-27 | 2023-04-14 | 福建极利新材料科技有限公司 | Preparation method of waterborne polyurethane figured fiber bass |
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