CN112062925A - Leather surface waterproof material and preparation method thereof - Google Patents
Leather surface waterproof material and preparation method thereof Download PDFInfo
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- CN112062925A CN112062925A CN202010932619.1A CN202010932619A CN112062925A CN 112062925 A CN112062925 A CN 112062925A CN 202010932619 A CN202010932619 A CN 202010932619A CN 112062925 A CN112062925 A CN 112062925A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6633—Compounds of group C08G18/42
- C08G18/6659—Compounds of group C08G18/42 with compounds of group C08G18/34
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
- C08G18/3203—Polyhydroxy compounds
- C08G18/3206—Polyhydroxy compounds aliphatic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/34—Carboxylic acids; Esters thereof with monohydroxyl compounds
- C08G18/348—Hydroxycarboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/4202—Two or more polyesters of different physical or chemical nature
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6633—Compounds of group C08G18/42
- C08G18/6637—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/664—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203
- C08G18/6644—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203 having at least three hydroxy groups
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
- C09D175/06—Polyurethanes from polyesters
-
- C—CHEMISTRY; METALLURGY
- C14—SKINS; HIDES; PELTS; LEATHER
- C14C—CHEMICAL TREATMENT OF HIDES, SKINS OR LEATHER, e.g. TANNING, IMPREGNATING, FINISHING; APPARATUS THEREFOR; COMPOSITIONS FOR TANNING
- C14C11/00—Surface finishing of leather
- C14C11/003—Surface finishing of leather using macromolecular compounds
- C14C11/006—Surface finishing of leather using macromolecular compounds using polymeric products of isocyanates (or isothiocyanates) with compounds having active hydrogen
Abstract
The invention discloses a leather surface waterproof material and a preparation method thereof, wherein the leather surface waterproof material comprises the following raw materials in parts by weight: 1350-1400 parts of polyester diol, 700-720 parts of micro-branched polyester polyol, 7.5-8.0 parts of dibutyltin dilaurate, 695-710 parts of toluene diisocyanate, 165-170 parts of diethyl acetal, 130-135 parts of dimethylolpropionic acid, 150-160 parts of trimethylolpropane, 80-11400 parts of acetone and 98-102 parts of triethylamine. The waterproof material for the leather surface has the advantages that the waterproof performance is good, the waterproof effect is lasting, the abrasion of a coating is not easily caused, the attractiveness and the use of leather are kept, meanwhile, fluorine is not contained in the waterproof material for the leather surface, and the defects that artificial leather is not easily degraded due to the waterproof material containing fluorine, the artificial leather is not environment-friendly, harmful gas is easily released even when the artificial leather is worn on the body, and the human health is damaged can be effectively overcome.
Description
Technical Field
The invention relates to the technical field of leather manufacturing, in particular to a leather surface waterproof material and a preparation method thereof.
Background
With the improvement of living standard and the change of living style of people, consumers put forward higher requirements on the performance of leather products, so that the leather is required to have the traditional characteristics of fullness, softness, comfortable wearing and the like, and the leather is also required to have more service performances such as good sanitary performance, water resistance, oil resistance and the like. In Europe and America, the waterproof leather without coating or with light coating is fashionable, is suitable for shoe upper leather, automobile seat cushion leather, high-grade sofa leather, photochromic leather, suede leather, frosted leather and the like for outdoor sports, and has higher requirements on waterproofness. In order to meet the requirements and development of domestic and foreign markets, the development of high-quality waterproof leather is a very significant matter. Good waterproof materials are essential to produce high-grade waterproof leather.
Leather has a long history of water repellent treatment. As early as 1400 years ago, albott Brenda, irish, was driving from the local coast to finland with a boat made of leather tanned with lanolin fatted, oak bark. In the early 20 th century, in the 50 s, germans began to study the effect of water repellent treatments on leather properties. Leather, which had waterproof properties at the time, was mainly used for the production of military shoes, safety shoes, hiking boots and the like. In order to overcome the strong water absorption of zirconium tanned bottom leather in the early 60 s of the last century, strong filling and high-grade fatty acid soap treatment are adopted, and good waterproofness is achieved. In the early 80 s, soft leather products with waterproof function, especially leather garments and leather gloves, were popular in the international market. The market demand for waterproof leather has increased rapidly over the 90 s, fashion consumer leather continues to be a popular trend, consumers demand very comfortable and fashionable products, and leather with waterproof and antifouling properties has been very suitable for this demand.
However, the waterproof leather currently used has the following problems:
1. the fluorine-containing waterproof material is used in a large amount, so that the artificial leather is not easy to degrade and is not environment-friendly, and even the artificial leather is easy to release harmful gas when being worn on the body, thereby damaging the health of the human body;
2. the leather which does not use the fluorine-containing waterproof material has poor waterproof effect, tensile strength, tearing strength, wear resistance and other mechanical properties, and has poor appearance, texture and other comprehensive properties. Therefore, we improve the above and propose a leather surface waterproof material.
Disclosure of Invention
In order to solve the technical problems, the invention provides the following technical scheme:
the invention relates to a leather surface waterproof material which comprises the following raw materials in parts by weight:
1350-1400 parts of polyester diol, 700-720 parts of micro-branched polyester polyol, 7.5-8.0 parts of dibutyltin dilaurate, 695-710 parts of toluene diisocyanate, 165-170 parts of diethyl acetal, 130-135 parts of dimethylolpropionic acid, 150-160 parts of trimethylolpropane, 80-11400 parts of acetone and 98-102 parts of triethylamine.
In a preferred embodiment of the present invention, the hydroxyl value of the polyester diol is 62.1mg KOH/g, and the hydroxyl value of the slightly branched polyester polyol is 60.4mg KOH/g.
A preparation method of a leather surface waterproof material comprises the following steps:
the method comprises the following steps: under the protection of dry gas, adding polyester diol and micro-branched polyester polyol into a reaction kettle according to the weight part ratio, heating to 120 ℃, reacting for 1h, adding dibutyltin dilaurate and toluene diisocyanate, and reacting for 2-4 h to obtain a polyurethane prepolymer;
step two: adding diglycol into the prepared polyurethane prepolymer, reacting for 3-3.5 h at 80 ℃, cooling to 60 ℃, adding a solution consisting of dimethylolpropionic acid and acetone, reacting for 1h at 60 ℃, and adding acetone for dilution;
step three: and (3) adding a solution consisting of trimethylolpropane, acetone and triethylamine into the solution prepared in the step two, uniformly mixing, adding water, carrying out high-speed shearing emulsification, finally heating to 70 ℃, vacuumizing, carrying out reduced pressure distillation to remove all the residual acetone, cooling to 40 ℃, filtering and discharging.
As a preferred embodiment of the present invention, the step-one drying gas may be one of nitrogen gas and carbon dioxide gas.
As a preferred technical scheme of the invention, 3900-4000 parts by weight and 6500-6600 parts by weight of acetone are respectively added in the second step twice before and after.
As a preferable technical scheme of the invention, the weight part of acetone added in the third step is 780-800 parts.
The invention has the beneficial effects that: the waterproof material for the leather surface has the advantages that the waterproof performance is good, the waterproof effect is lasting, the abrasion of a coating is not easily caused, the attractiveness and the use of leather are kept, meanwhile, fluorine is not contained in the waterproof material for the leather surface, and the defects that artificial leather is not easily degraded due to the waterproof material containing fluorine, the artificial leather is not environment-friendly, harmful gas is easily released even when the artificial leather is worn on the body, and the human health is damaged can be effectively overcome.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a flow chart of a process for preparing the leather surface waterproof material.
Detailed Description
The preferred embodiments of the present invention will be described in conjunction with the accompanying drawings, and it will be understood that they are described herein for the purpose of illustration and explanation and not limitation.
The first embodiment is as follows:
the leather surface waterproof material comprises the following raw materials in parts by weight: 1350 parts of polyester diol, 700 parts of micro-branched polyester polyol, 7.5 parts of dibutyltin dilaurate, 695 parts of toluene diisocyanate, 165 parts of diethylene glycol, 130 parts of dimethylolpropionic acid, 150 parts of trimethylolpropane, 11180 parts of acetone and 98 parts of triethylamine.
Wherein the hydroxyl value of the polyester glycol is 62.1mg KOH/g, and the hydroxyl value of the slightly-branched polyester polyol is 60.4mg KOH/g.
A preparation method of a leather surface waterproof material comprises the following steps:
the method comprises the following steps: under the protection of dry gas, adding polyester diol and micro-branched polyester polyol into a reaction kettle according to the weight part ratio, heating to 120 ℃, reacting for 1h, adding dibutyltin dilaurate and toluene diisocyanate, and reacting for 2-4 h to obtain a polyurethane prepolymer;
step two: adding diglycol into the prepared polyurethane prepolymer, reacting for 3-3.5 h at 80 ℃, cooling to 60 ℃, adding a solution consisting of dimethylolpropionic acid and acetone, reacting for 1h at 60 ℃, and adding acetone for dilution;
step three: and (3) adding a solution consisting of trimethylolpropane, acetone and triethylamine into the solution prepared in the step two, uniformly mixing, adding water, carrying out high-speed shearing emulsification, finally heating to 70 ℃, vacuumizing, carrying out reduced pressure distillation to remove all the residual acetone, cooling to 40 ℃, filtering and discharging.
Wherein, the drying gas of the first step may be one of nitrogen gas and carbon dioxide gas.
Wherein, the weight parts of the acetone added in the second step and the acetone added in the second step are 3900 parts and 6500 parts respectively.
Wherein, the weight part of acetone added in the third step is 780 parts.
Example two:
the leather surface waterproof material comprises the following raw materials in parts by weight: 1360 parts of polyester glycol, 710 parts of micro-branched polyester polyol, 7.7 parts of dibutyltin dilaurate, 698 parts of toluene diisocyanate, 162 parts of diethylene glycol, 132 parts of dimethylolpropionic acid, 155 parts of trimethylolpropane, 11290 parts of acetone and 99 parts of triethylamine.
Wherein the hydroxyl value of the polyester glycol is 62.1mg KOH/g, and the hydroxyl value of the slightly-branched polyester polyol is 60.4mg KOH/g.
A preparation method of a leather surface waterproof material comprises the following steps:
the method comprises the following steps: under the protection of dry gas, adding polyester diol and micro-branched polyester polyol into a reaction kettle according to the weight part ratio, heating to 120 ℃, reacting for 1h, adding dibutyltin dilaurate and toluene diisocyanate, and reacting for 2-4 h to obtain a polyurethane prepolymer;
step two: adding diglycol into the prepared polyurethane prepolymer, reacting for 3-3.5 h at 80 ℃, cooling to 60 ℃, adding a solution consisting of dimethylolpropionic acid and acetone, reacting for 1h at 60 ℃, and adding acetone for dilution;
step three: and (3) adding a solution consisting of trimethylolpropane, acetone and triethylamine into the solution prepared in the step two, uniformly mixing, adding water, carrying out high-speed shearing emulsification, finally heating to 70 ℃, vacuumizing, carrying out reduced pressure distillation to remove all the residual acetone, cooling to 40 ℃, filtering and discharging.
Wherein, the drying gas of the first step may be one of nitrogen gas and carbon dioxide gas.
Wherein, the weight parts of the acetone added in the second step and the acetone added in the second step are 3950 parts and 6550 parts respectively.
Wherein the weight part of acetone added in the third step is 790 parts.
Example three:
the leather surface waterproof material comprises the following raw materials in parts by weight: 1380 part of polyester diol, 715 parts of micro-branched polyester polyol, 7.8 parts of dibutyltin dilaurate, 705 parts of toluene diisocyanate, 168 parts of diethylene glycol, 134 parts of dimethylolpropionic acid, 157 parts of trimethylolpropane, 11345 parts of acetone and 100 parts of triethylamine.
Wherein the hydroxyl value of the polyester glycol is 62.1mg KOH/g, and the hydroxyl value of the slightly-branched polyester polyol is 60.4mg KOH/g.
A preparation method of a leather surface waterproof material comprises the following steps:
the method comprises the following steps: under the protection of dry gas, adding polyester diol and micro-branched polyester polyol into a reaction kettle according to the weight part ratio, heating to 120 ℃, reacting for 1h, adding dibutyltin dilaurate and toluene diisocyanate, and reacting for 2-4 h to obtain a polyurethane prepolymer;
step two: adding diglycol into the prepared polyurethane prepolymer, reacting for 3-3.5 h at 80 ℃, cooling to 60 ℃, adding a solution consisting of dimethylolpropionic acid and acetone, reacting for 1h at 60 ℃, and adding acetone for dilution;
step three: and (3) adding a solution consisting of trimethylolpropane, acetone and triethylamine into the solution prepared in the step two, uniformly mixing, adding water, carrying out high-speed shearing emulsification, finally heating to 70 ℃, vacuumizing, carrying out reduced pressure distillation to remove all the residual acetone, cooling to 40 ℃, filtering and discharging.
Wherein, the drying gas of the first step may be one of nitrogen gas and carbon dioxide gas.
Wherein, the weight parts of the acetone added in the second step and the acetone added in the second step are 3975 parts and 6575 parts respectively.
Wherein, the weight part of acetone added in the third step is 795 parts.
Example four: the leather surface waterproof material comprises the following raw materials in parts by weight: 1400 parts of polyester diol, 720 parts of micro-branched polyester polyol, 8.0 parts of dibutyltin dilaurate, 710 parts of toluene diisocyanate, 170 parts of diethylene glycol, 135 parts of dimethylolpropionic acid, 160 parts of trimethylolpropane, 11400 parts of acetone and 102 parts of triethylamine.
Wherein the hydroxyl value of the polyester glycol is 62.1mg KOH/g, and the hydroxyl value of the slightly-branched polyester polyol is 60.4mg KOH/g.
A preparation method of a leather surface waterproof material comprises the following steps:
the method comprises the following steps: under the protection of dry gas, adding polyester diol and micro-branched polyester polyol into a reaction kettle according to the weight part ratio, heating to 120 ℃, reacting for 1h, adding dibutyltin dilaurate and toluene diisocyanate, and reacting for 2-4 h to obtain a polyurethane prepolymer;
step two: adding diglycol into the prepared polyurethane prepolymer, reacting for 3-3.5 h at 80 ℃, cooling to 60 ℃, adding a solution consisting of dimethylolpropionic acid and acetone, reacting for 1h at 60 ℃, and adding acetone for dilution;
step three: and (3) adding a solution consisting of trimethylolpropane, acetone and triethylamine into the solution prepared in the step two, uniformly mixing, adding water, carrying out high-speed shearing emulsification, finally heating to 70 ℃, vacuumizing, carrying out reduced pressure distillation to remove all the residual acetone, cooling to 40 ℃, filtering and discharging.
Wherein, the drying gas of the first step may be one of nitrogen gas and carbon dioxide gas.
Wherein, the weight parts of acetone added in the second step are 4000 parts and 6600 parts respectively.
Wherein the weight part of the acetone added in the third step is 800 parts.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. The leather surface waterproof material is characterized by comprising the following raw materials in parts by weight:
1350-1400 parts of polyester diol, 700-720 parts of micro-branched polyester polyol, 7.5-8.0 parts of dibutyltin dilaurate, 695-710 parts of toluene diisocyanate, 165-170 parts of diethyl acetal, 130-135 parts of dimethylolpropionic acid, 150-160 parts of trimethylolpropane, 80-11400 parts of acetone and 98-102 parts of triethylamine.
2. The leather surface waterproofing material according to claim 1, wherein the hydroxyl value of the polyester glycol is 62.1mg KOH/g, and the hydroxyl value of the slightly branched polyester polyol is 60.4mg KOH/g.
3. The preparation method of the leather surface waterproof material according to claim 1, characterized by comprising the following steps:
the method comprises the following steps: under the protection of dry gas, adding polyester diol and micro-branched polyester polyol into a reaction kettle according to the weight part ratio, heating to 120 ℃, reacting for 1h, adding dibutyltin dilaurate and toluene diisocyanate, and reacting for 2-4 h to obtain a polyurethane prepolymer;
step two: adding diglycol into the prepared polyurethane prepolymer, reacting for 3-3.5 h at 80 ℃, cooling to 60 ℃, adding a solution consisting of dimethylolpropionic acid and acetone, reacting for 1h at 60 ℃, and adding acetone for dilution;
step three: and (3) adding a solution consisting of trimethylolpropane, acetone and triethylamine into the solution prepared in the step two, uniformly mixing, adding water, carrying out high-speed shearing emulsification, finally heating to 70 ℃, vacuumizing, carrying out reduced pressure distillation to remove all the residual acetone, cooling to 40 ℃, filtering and discharging.
4. The method for preparing the leather surface waterproofing material according to claim 3, wherein the step-one drying gas may be one of nitrogen gas and carbon dioxide gas.
5. The method for preparing the leather surface waterproof material as claimed in claim 3, wherein the acetone is added twice before and after the step two in parts by weight of 3900-4000 parts and 6500-6600 parts respectively.
6. The preparation method of the leather surface waterproof material according to claim 3, wherein the weight part of acetone added in the third step is 780-800 parts.
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102702466A (en) * | 2012-06-20 | 2012-10-03 | 温州市宏得利树脂有限公司 | Preparation method of aqueous polyurethane emulsion for synthetic leather |
US20160208432A1 (en) * | 2013-09-06 | 2016-07-21 | Dic Corporation | Urethane resin composition, leather-like sheet, and method for producing the leather-like sheet |
CN106928829A (en) * | 2017-03-08 | 2017-07-07 | 江苏元盛化工有限公司 | A kind of Aqueous Polyurethane Leather Finishing Agent preparation method |
CN108822675A (en) * | 2018-06-06 | 2018-11-16 | 山东莱福特皮革制品有限公司 | A kind of leather aqueous coating agent, preparation method and roll coating process |
-
2020
- 2020-09-08 CN CN202010932619.1A patent/CN112062925A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102702466A (en) * | 2012-06-20 | 2012-10-03 | 温州市宏得利树脂有限公司 | Preparation method of aqueous polyurethane emulsion for synthetic leather |
US20160208432A1 (en) * | 2013-09-06 | 2016-07-21 | Dic Corporation | Urethane resin composition, leather-like sheet, and method for producing the leather-like sheet |
CN106928829A (en) * | 2017-03-08 | 2017-07-07 | 江苏元盛化工有限公司 | A kind of Aqueous Polyurethane Leather Finishing Agent preparation method |
CN108822675A (en) * | 2018-06-06 | 2018-11-16 | 山东莱福特皮革制品有限公司 | A kind of leather aqueous coating agent, preparation method and roll coating process |
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Title |
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Application publication date: 20201211 |