CN109880504B - Leather isolation layer coating agent, preparation method thereof and leather - Google Patents
Leather isolation layer coating agent, preparation method thereof and leather Download PDFInfo
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Abstract
The invention discloses a leather isolation layer coating agent, a preparation method thereof and leather, wherein the preparation method of the leather isolation layer coating agent comprises the following steps: reacting 10-25 parts of isocyanate, 10-20 parts of dihydric alcohol and 1-3 parts of hydrophilic chain extender at 70-90 ℃ for 1-4 h, adding 0-5 parts of organic solvent, cooling to 40-50 ℃, continuously adding 1-3 parts of organic base and 150-200 parts of water, dispersing uniformly, then adding 1-2.5 parts of amine chain extender for chain extension, and stirring for reacting for 1-2 h to obtain the waterborne polyurethane containing amino in the terminal group; and (3) taking 40-70 parts of waterborne polyurethane, adding 30-60 parts of waterborne epoxy resin, and stirring for reacting for 3-5 hours. The leather isolating layer coating agent of the invention can be prepared without adding solvent or only adding a small amount of organic solvent, has no pungent taste during spraying, does not pollute the environment, is applied to the leather isolating layer, has good wet scratching performance and heavy pressing and board separating performance, and does not stick to the board.
Description
Technical Field
The invention relates to the technical field of leather manufacturing, in particular to a leather isolation layer finishing agent, a preparation method thereof and leather.
Background
In the prior leather-making technology, before the leather is flaked or embossed, an isolating layer coating agent is required to be sprayed to prevent the adhesion of the leather polluted by pollutants such as oil stain and dust during the flaking and the sizing resin of the subsequent process from being reduced, and the upper resin is separated when the leather is in water, thereby seriously affecting the quality and the appearance of the leather. The spraying of the isolating layer finishing agent can also prevent the coating from being sticky in the high-temperature embossing process of the leather, the plate sticking phenomenon from occurring, the normal operation of the subsequent process is influenced, and the quality of the leather can be influenced. At present, leather isolation layer coating agents used in the market are almost all nitrocotton emulsion, and nitrocotton is white powder and is insoluble in water, so that the nitrocotton emulsion contains a large amount of organic solvents, the using amount of the organic solvents exceeds 45% of the total mass of the nitrocotton emulsion, the nitrocotton emulsion has strong pungent smell, the VOC content is higher (more than 450g/L), and the large amount of organic solvents volatilize into the air, bring adverse effects on operators and working environment, cause serious pollution to the natural environment and do not meet the requirements of environmental protection at present.
Disclosure of Invention
In view of the above, the embodiment of the invention provides a leather isolating layer coating agent, a preparation method thereof and leather, which better overcome the problems and defects of the prior art, the leather isolating layer coating agent is prepared by preparing the waterborne polyurethane containing amino groups in the terminal groups, and then modifying the waterborne polyurethane by using the waterborne epoxy resin, a solvent is not added in the preparation process, or only a small amount of organic solvent is added, so that the epoxy resin modified waterborne polyurethane coating agent can be obtained, the non-irritating taste is realized, no pollution is caused to the environment, and the coating agent is applied to the leather isolating layer, so that the leather isolating layer coating agent not only has good wet scratch resistance, but also has good stress-release performance, and is not adhered to a plate during stress.
A leather barrier coating finish comprising the steps of:
reacting 10-25 parts of isocyanate, 10-20 parts of dihydric alcohol and 1-3 parts of hydrophilic chain extender at 70-90 ℃ for 1-4 h, adding 0-5 parts of organic solvent, cooling to 40-50 ℃, continuously adding 1-3 parts of organic base and 150-200 parts of water, dispersing uniformly, then adding 1-2.5 parts of amine chain extender for chain extension, and stirring for reacting for 1-2 h to obtain the waterborne polyurethane containing amino in the terminal group;
and (2) taking 40-70 parts of the waterborne polyurethane prepared in the step (1), adding 30-60 parts of waterborne epoxy resin, and stirring and reacting for 3-5 hours.
Further, the water-based epoxy resin is prepared by mixing 100-300 parts of epoxy resin, 10-30 parts of emulsifier and 700-900 parts of water.
Further, the epoxy resin is one or more of E-55, E-51 and E-44; the emulsifier is a nonionic emulsifier or an anionic emulsifier.
Further, the emulsifier is a nonionic emulsifier.
Further, the isocyanate is one or more of isophorone diisocyanate, dicyclohexylmethane diisocyanate and toluene diisocyanate.
Further, the dihydric alcohol is one or more of polycaprolactone dihydric alcohol, poly adipic acid hexanediol glycol, polycarbonate dihydric alcohol, polyether dihydric alcohol and polytetrahydrofuran ether glycol.
Further, the hydrophilic chain extender is one of 2, 2-dimethylolpropionic acid, 2-dimethylolbutyric acid and N-methyldiethanolamine; the organic base is one or more of triethylamine, triethanolamine and diethylethanolamine.
Further, the amine chain extender is one or more of hydrazine hydrate, ethylenediamine, diethylenetriamine and polyether triamine; the organic solvent is one or more of dimethylformamide, ethyl pyrrolidone, ethylene glycol dimethyl ether and dipropylene glycol dimethyl ether.
The embodiment of the invention also provides a leather isolating layer finishing agent, which is prepared by the preparation method of the leather isolating layer finishing agent.
The embodiment of the invention also provides leather which comprises the leather isolation layer coated by the leather isolation layer coating agent.
Compared with the prior art, the leather isolating layer finishing agent and the preparation method thereof and the leather have the beneficial effects that:
the leather isolating layer coating agent is prepared by preparing the waterborne polyurethane with amino in the end group and then modifying the waterborne polyurethane by the waterborne epoxy resin, a solvent is not added in the preparation process, or only a small amount of organic solvent is added, so that the epoxy resin modified waterborne polyurethane coating agent can be obtained, the irritation taste is avoided, the environment is not polluted, and the coating agent is applied to the leather isolating layer, so that the leather isolating layer coating agent has good wet scratching performance, good stress-free property and no adhesion to a board during stress.
In order to make the aforementioned and other objects, features and advantages of the invention more comprehensible, preferred embodiments accompanied with figures are described in detail below.
Detailed Description
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention.
This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein, but rather should be construed as broadly as the present invention is capable of modification in various respects, all without departing from the spirit and scope of the present invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In case of conflict, the present specification, including definitions, will control.
The terms as used herein:
the terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.
The conjunction "consisting of … …" excludes any unspecified elements, steps or components. If used in a claim, the phrase is intended to claim as closed, meaning that it does not contain materials other than those described, except for the conventional impurities associated therewith. When the phrase "consisting of … …" appears in a clause of the subject matter of the claims rather than immediately after the subject matter, it defines only the elements described in the clause; other elements are not excluded from the claims as a whole.
When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or as a range of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when the range "1 ~ 5" is disclosed, the ranges described should be construed to include the ranges "1 ~ 4", "1 ~ 3", "1 ~ 2 and 4 ~ 5", "1 ~ 3 and 5", and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.
"and/or" is used to indicate that one or both of the illustrated conditions may occur, e.g., a and/or B includes (a and B) and (a or B).
A leather barrier coating finish comprising the steps of:
(1) 10-25 parts of isocyanate, 10-20 parts of dihydric alcohol and 1-3 parts of hydrophilic chain extender react at 70-90 ℃ for 1-4 h, 0-5 parts of organic solvent is added, then the temperature is reduced to 40-50 ℃, 1-3 parts of organic base and 150-200 parts of water are continuously added, after uniform dispersion, 1-2.5 parts of amine chain extender is added for chain extension, and the mixture is stirred and reacts for 1-2 h to obtain the waterborne polyurethane containing amino in the end group.
The amount of the isocyanate to be used may be specifically 10 parts, 12 parts, 15 parts, 18 parts, 20 parts, 23 parts or 25 parts; the amount of the diol to be used may be specifically 10 parts, 12 parts, 15 parts, 18 parts or 20 parts, etc.; the amount of the hydrophilic chain extender to be used may specifically be 1 part, 1.5 parts, 2 parts, 2.5 parts or 3 parts; the amount of the organic solvent to be used may be specifically exemplified by 0 part, 1 part, 2 parts, 3 parts, 4 parts or 5 parts; the amount of the organic base to be used may be specifically 1 part, 1.5 parts, 2 parts, 2.5 parts or 3 parts; the amount of water to be used may be specifically exemplified by 150 parts, 160 parts, 170 parts, 180 parts, 190 parts or 200 parts; the amount of the amine chain extender to be used for chain extension may be specifically 1 part, 1.2 parts, 1.5 parts, 1.8 parts, 2 parts, 2.3 parts or 2.5 parts.
Preferably, the isocyanate is one or more of isophorone diisocyanate, dicyclohexylmethane diisocyanate, and toluene diisocyanate.
Preferably, the diol is one or more of polycaprolactone diol, polyhexamethylene adipate diol, polycarbonate diol, polyether diol and polytetrahydrofuran ether diol.
Preferably, the hydrophilic chain extender is one of 2, 2-dimethylolpropionic acid, 2-dimethylolbutyric acid and N-methyldiethanolamine; more preferably, the hydrophilic chain extender adopts 2, 2-dimethylolpropionic acid.
Preferably, the organic base is one or more of triethylamine, triethanolamine and diethylethanolamine.
Preferably, the amine chain extender is one or more of hydrazine hydrate, ethylenediamine, diethylenetriamine and polyether triamine; more preferably, the amine chain extender adopts hydrazine hydrate.
Preferably, the organic solvent is one or more of dimethylformamide, ethyl pyrrolidone, ethylene glycol dimethyl ether and dipropylene glycol dimethyl ether.
(2) And (2) taking 40-70 parts, such as 40 parts, 50 parts, 60 parts or 70 parts of the waterborne polyurethane prepared in the step (1), adding 30-60 parts, such as 30 parts, 40 parts, 50 parts or 60 parts of waterborne epoxy resin, and stirring and reacting for 3-5 hours.
Preferably, the waterborne epoxy resin is prepared by mixing 100-300 parts of epoxy resin, 10-30 parts of emulsifier and 700-900 parts of water.
The amount of the epoxy resin to be used may be specifically 100 parts, 150 parts, 200 parts, 250 parts or 300 parts; the amount of the emulsifier to be used may be specifically 10 parts, 15 parts, 20 parts, 35 parts or 30 parts; the amount of water to be used may be specifically 700 parts, 750 parts, 800 parts, 850 parts, 900 parts or the like.
Preferably, the epoxy resin is one or more of E-55, E-51 and E-44; the emulsifier is a nonionic emulsifier or an anionic emulsifier.
Examples of the nonionic emulsifier include tween 80, polyoxyethylene oleyl ether, polyoxyethylene monooleate, polyoxyethylene fatty alcohol, and polyoxyethylene oxypropylene stearate. Examples of the anionic emulsifier include sodium dodecylbenzenesulfonate, sodium butylnaphthalenesulfonate, and sodium laurylsulfate.
Preferably, the emulsifier is a nonionic emulsifier, the emulsifying effect of the nonionic emulsifier on the epoxy resin is better than that of the anionic emulsifier on the epoxy resin, and the emulsified waterborne epoxy resin is used for modifying the leather isolation layer finishing agent obtained from the waterborne polyurethane and has better wet scratching resistance and heavy-press separation plate performance when applied to the leather isolation layer.
The embodiment of the invention also provides a leather isolating layer finishing agent, which is prepared by the preparation method of the leather isolating layer finishing agent.
The embodiment of the invention also provides leather which comprises the leather isolation layer coated by the leather isolation layer coating agent.
The water is preferably deionized water, but may be distilled water, pure water, ultrapure water, or the like.
The leather isolating layer coating agent is prepared by preparing the waterborne polyurethane with amino in the end group and then modifying the waterborne polyurethane by the waterborne epoxy resin, a solvent is not added in the preparation process, or only a small amount of organic solvent is added, so that the waterborne polyurethane coating agent modified by the epoxy resin can be obtained, the non-irritating taste is realized, the environment is not polluted, and the coating agent is applied to the leather isolating layer, so that the leather isolating layer coating agent has good wet scratch resistance, good re-pressing and board separating performance and no adhesion during re-pressing. In order to facilitate understanding of the present invention, the following embodiments are provided to further illustrate the technical solutions of the present invention. The applicant states that the present invention is illustrated in detail by the following examples, but the present invention is not limited to the following detailed process equipment and process flow, which means that the present invention should not be implemented by relying on the detailed process equipment and process flow. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Example 1
(1) Preparing waterborne polyurethane: adding 10 parts of isophorone diisocyanate, 10 parts of polycaprolactone diol (molecular weight 2000) and 1 part of 2, 2-dimethylolpropionic acid into a reaction kettle, stirring and mixing uniformly, heating to 70 ℃ for reaction for 4 hours, then cooling to 40 ℃, continuously adding 1 part of triethanolamine for neutralization, adding 150 parts of water, dispersing uniformly, then adding 1 part of hydrazine hydrate, and stirring for reaction for 1 hour to obtain the waterborne polyurethane containing amino in the end group.
(2) Preparing a water-based epoxy resin: adding 10 parts of tween 80 into 700 parts of water, uniformly stirring to obtain a mixed solution, adding the mixed solution into 100 parts of epoxy resin E-44, and uniformly dispersing at a high speed to obtain the water-based epoxy resin.
(3) Preparing a leather isolating layer finishing agent: and (3) taking 40 parts of the waterborne polyurethane prepared in the step (1), adding 30 parts of the waterborne epoxy resin prepared in the step (2), and stirring and reacting at room temperature for 3 hours to obtain the leather isolation layer coating agent.
Example 2
(3) Preparing waterborne polyurethane: adding 15 parts of dicyclohexylmethane diisocyanate, 12 parts of polycaprolactone diol (molecular weight is 2000) and 1.5 parts of 2, 2-dimethylolbutyric acid into a reaction kettle, stirring and mixing uniformly, heating to 80 ℃ for reaction for 3 hours, cooling to 45 ℃, continuously adding 1.5 parts of triethylamine for neutralization, adding 160 parts of water, dispersing uniformly, adding 1.2 parts of diethylenetriamine, and stirring for reaction for 1.5 hours to obtain the waterborne polyurethane with the amino group in the terminal group.
(4) Preparing a water-based epoxy resin: adding 15 parts of tween 80 into 750 parts of water, uniformly stirring to obtain a mixed solution, adding the mixed solution into 150 parts of epoxy resin E-44, and uniformly dispersing at a high speed to obtain the water-based epoxy resin.
(3) Preparing a leather isolating layer finishing agent: and (3) taking 50 parts of the waterborne polyurethane prepared in the step (1), adding 40 parts of the waterborne epoxy resin prepared in the step (2), and stirring and reacting at room temperature for 3.5 hours to obtain the leather isolation layer coating agent.
Example 3
(5) Preparing waterborne polyurethane: adding 20 parts of isophorone diisocyanate, 15 parts of polycaprolactone diol (molecular weight is 2000) and 2 parts of 2, 2-dimethylolpropionic acid into a reaction kettle, stirring and mixing uniformly, heating to 80 ℃ for reaction for 2.5 hours, cooling to 45 ℃, continuously adding 2 parts of triethanolamine for neutralization, adding 170 parts of water, dispersing uniformly, adding 1.8 parts of hydrazine hydrate, and stirring for reaction for 1.5 hours to obtain the waterborne polyurethane containing amino in the terminal group.
(6) Preparing a water-based epoxy resin: adding 20 parts of tween 80 into 800 parts of water, uniformly stirring to obtain a mixed solution, adding the mixed solution into 200 parts of epoxy resin E-44, and uniformly dispersing at a high speed to obtain the water-based epoxy resin.
(3) Preparing a leather isolating layer finishing agent: and (3) taking 60 parts of the waterborne polyurethane prepared in the step (1), adding 50 parts of the waterborne epoxy resin prepared in the step (2), and stirring and reacting at room temperature for 4 hours to obtain the leather isolation layer coating agent.
Example 4
(7) Preparing waterborne polyurethane: adding 23 parts of toluene diisocyanate, 18 parts of polycaprolactone diol (molecular weight of 2000) and 2.5 parts of N-methyldiethanolamine into a reaction kettle, stirring and mixing uniformly, heating to 90 ℃, reacting for 1.5h, adding 1 part of dimethylformamide, then cooling to 50 ℃, continuously adding 2.5 parts of diethylethanolamine for neutralization, adding 180 parts of water, dispersing uniformly, then adding 2.5 parts of polyether triamine, stirring and reacting for 2h to obtain the waterborne polyurethane containing amino in the terminal group.
(8) Preparing a water-based epoxy resin: adding 25 parts of tween 80 into 850 parts of water, uniformly stirring to obtain a mixed solution, adding the mixed solution into 250 parts of epoxy resin E-44, and uniformly dispersing at a high speed to obtain the water-based epoxy resin.
(3) Preparing a leather isolating layer finishing agent: and (3) taking 50 parts of the waterborne polyurethane prepared in the step (1), adding 50 parts of the waterborne epoxy resin prepared in the step (2), and stirring and reacting at room temperature for 4.5 hours to obtain the leather isolation layer coating agent.
Example 5
(9) Preparing waterborne polyurethane: adding 25 parts of isophorone diisocyanate, 20 parts of polycaprolactone diol (molecular weight is 2000) and 3 parts of 2, 2-dimethylolpropionic acid into a reaction kettle, stirring and mixing uniformly, heating to 90 ℃ for reaction for 1 hour, adding 5 parts of dimethylformamide, cooling to 50 ℃, continuously adding 3 parts of triethanolamine for neutralization, adding 200 parts of water, dispersing uniformly, then adding 2.5 parts of hydrazine hydrate, stirring and reacting for 1.5 hours to obtain the waterborne polyurethane containing amino in the terminal group.
(10) Preparing a water-based epoxy resin: adding 30 parts of tween 80 into 900 parts of water, uniformly stirring to obtain a mixed solution, adding the mixed solution into 300 parts of epoxy resin E-44, and uniformly dispersing at a high speed to obtain the water-based epoxy resin.
(3) Preparing a leather isolating layer finishing agent: and (3) taking 70 parts of the waterborne polyurethane prepared in the step (1), adding 60 parts of the waterborne epoxy resin prepared in the step (2), and stirring and reacting at room temperature for 5 hours to obtain the leather isolation layer coating agent.
The leather isolation layer coating agent prepared in the examples 1 to 5 is applied to a leather isolation layer, and is detected to have the wet scratch resistance and the re-pressing and separating plate performance with the conventional commercially available nitrocellulose emulsion, and the results are shown in the following table 1.
TABLE 1
The above table 1 shows that the leather isolation layer finishing agent prepared in the embodiments 1-5 of the invention is applied to a leather isolation layer, and the wet scratch resistance and the heavy-pressing separation plate performance of the leather isolation layer finishing agent are obviously superior to those of the traditional commercially available nitrocotton emulsion; the leather isolating layer coating agents prepared in the embodiments 1 to 5 of the invention have almost no peculiar smell when being sprayed.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and it will be apparent to those skilled in the art that various modifications and variations can be made in the formulation and preparation process of the present 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 (10)
1. A preparation method of a leather isolation layer finishing agent is characterized by comprising the following steps: the method comprises the following steps:
reacting 10-25 parts of isocyanate, 10-20 parts of dihydric alcohol and 1-3 parts of hydrophilic chain extender at 70-90 ℃ for 1-4 h, adding 0-5 parts of organic solvent, cooling to 40-50 ℃, continuously adding 1-3 parts of organic base and 150-200 parts of water, dispersing uniformly, then adding 1-2.5 parts of amine chain extender for chain extension, and stirring for reacting for 1-2 h to obtain the waterborne polyurethane containing amino in the terminal group;
and (3) taking 40-70 parts of waterborne polyurethane, adding 30-60 parts of waterborne epoxy resin, and stirring for reacting for 3-5 hours.
2. The method for preparing a leather barrier coating finishing agent as claimed in claim 1, wherein: the water-based epoxy resin is prepared by mixing 100-300 parts of epoxy resin, 10-30 parts of emulsifier and 700-900 parts of water.
3. The method for preparing a leather barrier coating finishing agent as claimed in claim 2, wherein: the epoxy resin is one or more of E-55, E-51 and E-44; the emulsifier is a nonionic emulsifier or an anionic emulsifier.
4. The method for preparing a leather barrier coating finishing agent as claimed in claim 3, wherein: the emulsifier is a nonionic emulsifier.
5. The method for preparing a leather barrier coating finishing agent as claimed in claim 1, wherein: the isocyanate is one or more of isophorone diisocyanate, dicyclohexylmethane diisocyanate and toluene diisocyanate.
6. The method for preparing a leather barrier coating finishing agent as claimed in claim 1, wherein: the dihydric alcohol is one or more of polycaprolactone dihydric alcohol, poly adipic acid hexanediol ester diol, polycarbonate dihydric alcohol and polyether dihydric alcohol.
7. The method for preparing a leather barrier coating finishing agent as claimed in claim 1, wherein: the hydrophilic chain extender is one of 2, 2-dimethylolpropionic acid, 2-dimethylolbutyric acid and N-methyldiethanolamine; the organic base is one or more of triethylamine, triethanolamine and diethylethanolamine.
8. The method for preparing a leather barrier coating finishing agent as claimed in claim 1, wherein: the amine chain extender is one or more of hydrazine hydrate, ethylenediamine, diethylenetriamine and polyether triamine; the organic solvent is one or more of dimethylformamide, ethyl pyrrolidone, ethylene glycol dimethyl ether and dipropylene glycol dimethyl ether.
9. A leather isolating layer finishing agent is characterized in that: the leather isolation layer coating agent is prepared by the preparation method of the leather isolation layer coating agent as claimed in any one of claims 1 to 8.
10. Leather, characterized in that: a leather barrier layer comprising the leather barrier layer finish of claim 9.
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| CN111548717A (en) * | 2020-06-02 | 2020-08-18 | 四川达威科技股份有限公司 | Waterborne polyurethane artificial leather surface treatment agent and preparation method thereof |
| CN114181592B (en) * | 2021-12-30 | 2022-12-02 | 盛瑞(常州)特种材料有限公司 | Water-based leather finishing agent, application thereof and leather treatment method |
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| CN102605617B (en) * | 2012-01-19 | 2014-07-09 | 朗盛（常州）有限公司 | Leather isolating layer finishing agent, preparation method and application thereof in leather isolating layer |
| CN104211898B (en) * | 2014-08-13 | 2016-08-17 | 佛山市顺德区巴德富实业有限公司 | A kind of Amino End Group aqueous pu dispersions and preparation method thereof |
| CN104278530B (en) * | 2014-09-29 | 2016-03-30 | 惠州大亚湾达志精细化工有限公司 | A kind of polyurethane aqueous finishing agent of modification polytrimethylene carbonate for leather and preparation method thereof |
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