CN109880504A - A kind of leather separation layer finishing agent and preparation method thereof and leather - Google Patents
A kind of leather separation layer finishing agent and preparation method thereof and leather Download PDFInfo
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Abstract
The invention discloses a kind of leather separation layer finishing agent and preparation method thereof and leathers, the preparation method of the leather separation layer finishing agent includes: that 10~25 parts of isocyanates, 10~20 parts of dihydric alcohols and 1~3 part of hydrophilic chain extender are reacted 1~4h at 70~90 DEG C, 0~5 part of organic solvent is added, then 40~50 DEG C are cooled to, continuously add 1~3 part of organic base and 150~200 parts of water, after being uniformly dispersed, it is subsequently added into 1~2.5 part of amine chain extender chain extension, it is stirred to react 1~2h, obtains the aqueous polyurethane in end group containing amino；40~70 parts of aqueous polyurethanes are taken, 30~60 parts of aqueous epoxy resins are added, are stirred to react 3~5h.In leather separation layer finishing agent preparation process of the present invention can not solubilizer, or need to only add minimal amount of organic solvent, when spraying nonirritant taste, it not can cause environmental pollution, and the finishing agent is applied in leather separation layer, there is good wet scratch to scrape performance and weight from plate, and not haftplatte.
Description
Technical field
The present invention relates to leather manufacture technical fields, in particular to a kind of leather separation layer finishing agent and its preparation
Method and leather.
Background technique
In current tanning technology, before leather falls soft or embossing procedure, it is necessary to spray separation layer finishing agent, use
To prevent leather from being declined after the contaminants such as greasy dirt, dust with the followability of the pulp layer resin of later process when falling soft,
Lead to upper layer resin wear when leather meets water, seriously affects the quality and appearance of leather.Spraying separation layer finishing agent can also be with
Sticky finiss during leather high temperature is embossed is prevented, haftplatte phenomenon occurs, influences the normal operating of later process, and can shadow
Ring the quality of leather.Used leather separation layer finishing agent is nearly all nitrocotton lotion currently on the market, and nitrocotton is
White powder, it is not soluble in water, therefore contain a large amount of organic solvents in nitrocotton lotion, the dosage of organic solvent is more than nitrocotton cream
The 45% of liquid gross mass makes nitrocotton lotion have strong pungent smell, causes VOC content higher (> 450g/L), and
And so a large amount of organic solvent is evaporate into air, brings detrimental effect to operator and working environment, it also can be to certainly
Right environment causes seriously to pollute, and does not meet the requirement of present environmental protection.
Summary of the invention
In view of this, a kind of leather separation layer finishing agent provided by the invention and preparation method thereof and leather, better gram
The above-mentioned problems of the prior art and defect are taken, the embodiment of the present invention is by preparing the aqueous poly- ammonia in end group containing amino
Then ester is modified the leather separation layer finishing agent that the aqueous polyurethane obtains using aqueous epoxy resins, can in the preparation process
Not solubilizer, or need to only add minimal amount of organic solvent, epoxy resin modified aqueous poly- ammonia finishing agent can be obtained, it is both non-stimulated
Nature and flavor road, not can cause environmental pollution, and the finishing agent is applied in leather separation layer, not only there is good moisture-resistant to scratch
It scrapes performance, and there is good weight from plate performance, not haftplatte when weight.
A kind of leather separation layer finishing agent, comprising the following steps:
10~25 parts of isocyanates, 10~20 parts of dihydric alcohols and 1~3 part of hydrophilic chain extender are reacted 1 at 70~90 DEG C
~4h is added 0~5 part of organic solvent, is then cooled to 40~50 DEG C, continuously adds 1~3 part of organic base and 150~200 parts
Water after being uniformly dispersed, is subsequently added into 1~2.5 part of amine chain extender chain extension, is stirred to react 1~2h, obtain containing amino in end group
Aqueous polyurethane；
The aqueous polyurethane for taking 40~70 parts of steps (1) to prepare is added 30~60 parts of aqueous epoxy resins, is stirred to react 3
~5h.
Further, the aqueous epoxy resins are by by 100~300 parts of epoxy resin, 10~30 parts of emulsifiers and 700
~900 parts of water are mixed with to obtain.
Further, the epoxy resin is one of E-55, E-51 and E-44 or a variety of；The emulsifier be it is non-from
Sub- emulsifier or anion emulsifier.
Further, the emulsifier is nonionic emulsifier.
Further, the isocyanates is isophorone diisocyanate, dicyclohexyl methyl hydride diisocyanate and first
One of phenylene diisocyanate is a variety of.
Further, the dihydric alcohol is polycaprolactone diols, polyhexamethylene adipate glycol, polycarbonate binary
One of alcohol, polyether Glycols and polytetrahydrofuran ether glycol are a variety of.
Further, the hydrophilic chain extender is 2,2- dihydromethyl propionic acid, 2,2- dimethylolpropionic acid and N- methyl two
One of ethanol amine；The organic base is the one or more of triethylamine, triethanolamine and diethyl ethylene diamine.
Further, the amine chain extender is a kind of or more in hydrazine hydrate, ethylenediamine, diethylenetriamine and polyethers triamine
Kind；The organic solvent is one in dimethylformamide, ethyl pyrrolidone, glycol dimethyl ether and dimethyl ether
Kind is a variety of.
The embodiment of the invention also provides a kind of leather separation layer finishing agent, the leather separation layer finishing agent is by above-mentioned
The preparation method of leather separation layer finishing agent is prepared.
The embodiment of the invention also provides a kind of leather, the leather isolation covered with paint, lacquer, colour wash, etc. including upper leather separation layer finishing agent
Layer.
Compared with prior art, a kind of leather separation layer finishing agent of the embodiment of the present invention and preparation method thereof and leather
Beneficial effect includes:
By preparing the aqueous polyurethane in end group containing amino, then using the modified aqueous poly- ammonia of aqueous epoxy resins
The leather separation layer finishing agent that ester obtains, in the preparation process can not solubilizer, or need to only add minimal amount of organic solvent
Epoxy resin modified aqueous poly- ammonia finishing agent is obtained, both nonirritant taste, not can cause environmental pollution, and the finishing agent
Applied in leather separation layer, not only there is good wet scratch to scrape performance, but also there is good weight from plate, when weight not
Haftplatte.
To enable the above objects, features and advantages of the present invention to be clearer and more comprehensible, preferred embodiment is cited below particularly, makees detailed
It is described as follows.
Specific embodiment
To facilitate the understanding of the present invention, it elaborates below with reference to the mode of embodiment to technical solution of the present invention,
In the following description, numerous specific details are set forth in order to facilitate a full understanding of the present invention.
But the invention can be embodied in many other ways as described herein, those skilled in the art can be with
Similar improvement is done without violating the connotation of the present invention, therefore the present invention is not limited to the specific embodiments disclosed below.
Unless otherwise defined, all technologies used herein and scientific term have and the common skill of fields of the present invention
The normally understood identical meaning of art personnel.When there is a conflict, the definition in this specification shall prevail.
Term as used herein:
Term "comprising" used herein, " comprising ", " having ", " containing " or its any other deformation, it is intended that covering
Non-exclusionism includes.For example, composition, step, method, product or device comprising listed elements are not necessarily limited to those and want
Element, but may include not expressly listed other elements or such composition, step, method, product or device it is intrinsic
Element.
Conjunction " by ... form " exclude any element that do not point out, step or component.If in claim,
This phrase will make claim closed, so that it is not included the material in addition to the material of those descriptions, but relative
Except customary impurities.When phrase " by ... form " be rather than immediately following theme in the clause that appears in claim main body after
When, only it is limited to element described in the clause；Other elements be not excluded the claim as a whole it
Outside.
Equivalent, concentration or other values or parameter are excellent with range, preferred scope or a series of upper limit preferred values and lower limit
When the Range Representation that choosing value limits, this should be understood as specifically disclosing by any range limit or preferred value and any range
Any pairing of lower limit or preferred value is formed by all ranges, regardless of whether the range separately discloses.For example, when open
When range " 1~5 ", described range should be interpreted as including range " 1~4 ", " 1~3 ", " 1~2 ", " 1~2 and 4~
5 ", " 1~3 and 5 " etc..When numberical range is described herein, unless otherwise stated, otherwise the range is intended to include its end
Value and all integers and score in the range.
"and/or" is used to indicate that one of illustrated situation or both may to occur, for example, A and/or B includes (A
And B) and (A or B).
A kind of leather separation layer finishing agent, comprising the following steps:
(1) 10~25 parts of isocyanates, 10~20 parts of dihydric alcohols and 1~3 part of hydrophilic chain extender is anti-at 70~90 DEG C
1~4h is answered, 0~5 part of organic solvent is added, is then cooled to 40~50 DEG C, continuously adds 1~3 part of organic base and 150~200
Part water, after being uniformly dispersed, is subsequently added into 1~2.5 part of amine chain extender chain extension, is stirred to react 1~2h, obtain containing ammonia in end group
The aqueous polyurethane of base.
The specific enumerable dosage of above-mentioned isocyanates is 10 parts, 12 parts, 15 parts, 18 parts, 20 parts, 23 parts or 25 parts etc.；
The specific enumerable dosage of dihydric alcohol is 10 parts, 12 parts, 15 parts, 18 parts or 20 parts etc.；The dosage of hydrophilic chain extender can specifically arrange
Lift is 1 part, 1.5 parts, 2 parts, 2.5 parts or 3 parts etc.；The specific enumerable dosage of organic solvent is 0 part, 1 part, 2 parts, 3 parts, 4 parts
Or 5 parts etc.；The specific enumerable dosage of organic base is 1 part, 1.5 parts, 2 parts, 2.5 parts or 3 parts etc.；The dosage of water is specific enumerable
It is 150 parts, 160 parts, 170 parts, 180 parts, 190 parts or 200 parts etc.；It is 1 part that the dosage of amine chain extender chain extension is specific enumerable,
1.2 parts, 1.5 parts, 1.8 parts, 2 parts, 2.3 parts or 2.5 parts etc..
Preferably, the isocyanates is isophorone diisocyanate, dicyclohexyl methyl hydride diisocyanate and toluene
One of diisocyanate is a variety of.
Preferably, the dihydric alcohol is polycaprolactone diols, polyhexamethylene adipate glycol, polycarbonate binary
One of alcohol, polyether Glycols and polytetrahydrofuran ether glycol are a variety of.
Preferably, the hydrophilic chain extender is 2,2- dihydromethyl propionic acid, 2,2- dimethylolpropionic acid and N- methyl diethyl
One of hydramine；More preferably, the hydrophilic chain extender uses 2,2- dihydromethyl propionic acid.
Preferably, the organic base is the one or more of triethylamine, triethanolamine and diethyl ethylene diamine.
Preferably, the amine chain extender is a kind of or more in hydrazine hydrate, ethylenediamine, diethylenetriamine and polyethers triamine
Kind；More preferably, the amine chain extender uses hydrazine hydrate.
Preferably, the organic solvent is dimethylformamide, ethyl pyrrolidone, glycol dimethyl ether and dipropylene glycol
One of dimethyl ether is a variety of.
(2) aqueous polyurethane for taking 40~70 parts of such as 40 parts, 50 parts, 60 parts or 70 parts steps (1) preparations, is added 30~60
Part such as 30 parts, 40 parts, 50 parts or 60 parts aqueous epoxy resins, are stirred to react 3~5h.
Preferably, the aqueous epoxy resins by by 100~300 parts of epoxy resin, 10~30 parts of emulsifiers and 700~
900 parts of water are mixed with to obtain.
The specific enumerable dosage of above-mentioned epoxy resin is 100 parts, 150 parts, 200 parts, 250 parts or 300 parts etc.；Emulsifier
Dosage it is specific enumerable be 10 parts, 15 parts, 20 parts, 35 parts or 30 parts etc.；The specific enumerable dosage of water is 700 parts, 750
Part, 800 parts, 850 parts or 900 parts etc..
Preferably, the epoxy resin is one of E-55, E-51 and E-44 or a variety of；The emulsifier is nonionic
Emulsifier or anion emulsifier.
Above-mentioned nonionic emulsifier can be enumerated as Tween 80, Brij92, Aceonon 300 MO, polyoxy second
Alkene fatty alcohol or polyoxyethylene oxypropylene stearate etc..Anion emulsifier can be enumerated as neopelex, butyl
Sodium naphthalene sulfonate or sldium lauryl sulfate etc..
Preferably, the emulsifier is nonionic emulsifier, and nonionic emulsifier is more negative to the emulsifying effectiveness of epoxy resin
Ionic emulsifying agent is more preferable to the emulsifying effectiveness of epoxy resin, and the aqueous epoxy resins obtained after emulsifying are for the poly- ammonia of modified water-soluble
The moisture-resistant that the leather separation layer finishing agent that ester obtains is applied to leather separation layer scratches that scrape performance and weight more preferable from plate performance.
The embodiment of the invention also provides a kind of leather separation layer finishing agent, the leather separation layer finishing agent is by above-mentioned
The preparation method of leather separation layer finishing agent is prepared.
The embodiment of the invention also provides a kind of leather, the leather isolation covered with paint, lacquer, colour wash, etc. including upper leather separation layer finishing agent
Layer.
Above-mentioned water is preferably deionized water, naturally it is also possible to for distilled water, pure water or ultrapure water etc..
Above by the aqueous polyurethane prepared in end group containing amino, it is aqueous that this then is modified using aqueous epoxy resins
The leather separation layer finishing agent that polyurethane obtains, in the preparation process can not solubilizer, or need to only add minimal amount of organic solvent,
Epoxy resin modified aqueous poly- ammonia finishing agent can be obtained, both nonirritant taste, not can cause environmental pollution, and the painting
It adorns agent to be applied in leather separation layer, not only there is good moisture-resistant to scratch and scrape performance, but also there is good weight from plate performance,
Not haftplatte when weight.To facilitate the understanding of the present invention, below with reference to embodiment to further illustrate the technical scheme of the present invention.Shen
It asks someone to state, the present invention is illustrated by the following examples detailed process equipment and process flow of the invention, but the present invention is simultaneously
It is not limited to following detailed process equipments and process flow, that is, does not mean that the present invention should rely on above-mentioned detailed process equipment and work
Skill process could be implemented.It should be clear to those skilled in the art, any improvement in the present invention, to product of the present invention
The equivalence replacement of each raw material and addition, the selection of concrete mode of auxiliary element etc., all fall within protection scope of the present invention and public affairs
Within the scope of opening.
Embodiment 1
(1) aqueous polyurethane is prepared: by 10 parts of isophorone diisocyanate, 10 parts of polycaprolactone diols (molecular weight
For 2000) and 1 part of 2,2- dihydromethyl propionic acid be added in reaction kettle, be warming up to after being uniformly mixed at 70 DEG C and react 4h,
Then 40 DEG C are cooled to, 1 part of triethanolamine is continuously added and is neutralized, add 150 parts of water, after being uniformly dispersed, be subsequently added into 1
Part hydrazine hydrate, is stirred to react 1h, obtains the aqueous polyurethane in end group containing amino.
(2) aqueous epoxy resins are prepared: 10 parts of Tween 80s being added in 700 parts of water and are stirred evenly, mixed liquor are obtained, by this
Mixed liquor is added in 100 parts of epoxy resin E-44s, and high speed dispersion is uniform, obtains aqueous epoxy resins.
(3) prepare leather separation layer finishing agent: 30 parts of steps (2) are added in the aqueous polyurethane for taking 40 parts of steps (1) to prepare
The aqueous epoxy resins of preparation, are stirred to react 3h at room temperature, obtain leather separation layer finishing agent.
Embodiment 2
(3) it prepares aqueous polyurethane: 15 parts of dicyclohexyl methyl hydride diisocyanates, 12 parts of polycaprolactone diolss (is divided
Son amount is warming up at 80 DEG C anti-2000) to be added in reaction kettle with 1.5 parts of 2,2- dimethylolpropionic acids after being uniformly mixed
3h is answered, is then cooled to 45 DEG C, 1.5 parts of triethylamines is continuously added and is neutralized, add 160 parts of water, after being uniformly dispersed, then
1.2 parts of diethylenetriamines are added, are stirred to react 1.5h, obtain the aqueous polyurethane in end group containing amino.
(4) aqueous epoxy resins are prepared: 15 parts of Tween 80s being added in 750 parts of water and are stirred evenly, mixed liquor are obtained, by this
Mixed liquor is added in 150 parts of epoxy resin E-44s, and high speed dispersion is uniform, obtains aqueous epoxy resins.
(3) prepare leather separation layer finishing agent: 40 parts of steps (2) are added in the aqueous polyurethane for taking 50 parts of steps (1) to prepare
The aqueous epoxy resins of preparation, are stirred to react 3.5h at room temperature, obtain leather separation layer finishing agent.
Embodiment 3
(5) aqueous polyurethane is prepared: by 20 parts of isophorone diisocyanate, 15 parts of polycaprolactone diols (molecular weight
2000) to be added in reaction kettle with 2 parts of 2,2- dihydromethyl propionic acids, it is warming up at 80 DEG C and reacts after being uniformly mixed
Then 2.5h is cooled to 45 DEG C, continuously add 2 parts of triethanolamines and neutralized, add 170 parts of water, after being uniformly dispersed, then
1.8 parts of hydrazine hydrates are added, are stirred to react 1.5h, obtain the aqueous polyurethane in end group containing amino.
(6) aqueous epoxy resins are prepared: 20 parts of Tween 80s being added in 800 parts of water and are stirred evenly, mixed liquor are obtained, by this
Mixed liquor is added in 200 parts of epoxy resin E-44s, and high speed dispersion is uniform, obtains aqueous epoxy resins.
(3) prepare leather separation layer finishing agent: 50 parts of steps (2) are added in the aqueous polyurethane for taking 60 parts of steps (1) to prepare
The aqueous epoxy resins of preparation, are stirred to react 4h at room temperature, obtain leather separation layer finishing agent.
Embodiment 4
(7) prepare aqueous polyurethane: by 23 parts of toluene di-isocyanate(TDI)s, 18 parts of polycaprolactone diolss, (molecular weight is
2000) it is added in reaction kettle with 2.5 parts of N methyldiethanol amines, is warming up to after being uniformly mixed at 90 DEG C and reacts 1.5h,
1 part of dimethylformamide is added, is then cooled to 50 DEG C, continuously adds 2.5 parts of diethyl ethylene diamines and is neutralized, added
180 parts of water after being uniformly dispersed, are subsequently added into 2.5 parts of polyethers triamines, are stirred to react 2h, obtain in end group containing the aqueous of amino
Polyurethane.
(8) aqueous epoxy resins are prepared: 25 parts of Tween 80s being added in 850 parts of water and are stirred evenly, mixed liquor are obtained, by this
Mixed liquor is added in 250 parts of epoxy resin E-44s, and high speed dispersion is uniform, obtains aqueous epoxy resins.
(3) prepare leather separation layer finishing agent: 50 parts of step (2) systems are added in the aqueous polyurethane for taking 50 steps (1) to prepare
Standby aqueous epoxy resins, are stirred to react 4.5h at room temperature, obtain leather separation layer finishing agent.
Embodiment 5
(9) aqueous polyurethane is prepared: by 25 parts of isophorone diisocyanate, 20 parts of polycaprolactone diols (molecular weight
For 2000) and 3 parts of 2,2- dihydromethyl propionic acids be added in reaction kettle, be warming up to after being uniformly mixed at 90 DEG C and react 1h,
5 parts of dimethylformamides are added, are then cooled to 50 DEG C, continuously adds 3 parts of triethanolamines and is neutralized, add 200 parts of water,
After being uniformly dispersed, 2.5 parts of hydrazine hydrates are subsequently added into, 1.5h is stirred to react, obtains the aqueous polyurethane in end group containing amino.
(10) aqueous epoxy resins are prepared: 30 parts of Tween 80s being added in 900 parts of water and are stirred evenly, mixed liquor is obtained, it will
The mixed liquor is added in 300 parts of epoxy resin E-44s, and high speed dispersion is uniform, obtains aqueous epoxy resins.
(3) prepare leather separation layer finishing agent: 60 parts of step (2) systems are added in the aqueous polyurethane for taking 70 steps (1) to prepare
Standby aqueous epoxy resins, are stirred to react 5h at room temperature, obtain leather separation layer finishing agent.
The leather separation layer finishing agent of Examples 1 to 5 preparation is applied in leather separation layer, and the nitre with conventional commercial
Change cotton lotion to carry out moisture-resistant and scratch scraping performance and weight and being detected from plate performance, as a result as shown in table 1 below.
Table 1
It can be obtained by upper table 1, leather separation layer finishing agent prepared by the embodiment of the present invention 1~5 is applied to leather separation layer,
Its moisture-resistant, which is scratched, to be scraped performance and weight and is significantly better than that the moisture-resistant of nitrocotton lotion of conventional commercial is scratched and scrapes performance and again from plate performance
It presses from plate performance；And the embodiment of the present invention 1~5 prepare the spraying of leather separation layer finishing agent when almost free from extraneous odour.
The above is only a preferred embodiment of the present invention, is not intended to restrict the invention, for those skilled in the art
For member, inventive formulation and preparation process can have various modifications and variations.All within the spirits and principles of the present invention, institute
Any modification, equivalent substitution, improvement and etc. of work, should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of leather separation layer finishing agent, it is characterised in that: include:
10~25 parts of isocyanates, 10~20 parts of dihydric alcohols and 1~3 part of hydrophilic chain extender are reacted into 1~4h at 70~90 DEG C,
0~5 part of organic solvent is added, is then cooled to 40~50 DEG C, continuously adds 1~3 part of organic base and 150~200 parts of water, disperses
After uniformly, it is subsequently added into 1~2.5 part of amine chain extender chain extension, is stirred to react 1~2h, is obtained in end group containing the aqueous of amino
Polyurethane；
40~70 parts of aqueous polyurethanes are taken, 30~60 parts of aqueous epoxy resins are added, are stirred to react 3~5h.
2. the preparation method of leather separation layer finishing agent according to claim 1, it is characterised in that: the water-base epoxy tree
Rouge by 100~300 parts of epoxy resin, 10~30 parts of emulsifiers and 700~900 parts of water by being mixed with to obtain.
3. the preparation method of leather separation layer finishing agent according to claim 2, it is characterised in that: the epoxy resin is
One of E-55, E-51 and E-44 or a variety of；The emulsifier is nonionic emulsifier or anion emulsifier.
4. the preparation method of leather separation layer finishing agent according to claim 3, it is characterised in that: the emulsifier is non-
Ionic emulsifying agent.
5. the preparation method of leather separation layer finishing agent according to claim 1, it is characterised in that: the isocyanates is
One of isophorone diisocyanate, dicyclohexyl methyl hydride diisocyanate and toluene di-isocyanate(TDI) are a variety of.
6. the preparation method of leather separation layer finishing agent according to claim 1, it is characterised in that: the dihydric alcohol is poly-
Caprolactone dihydric alcohol, polyhexamethylene adipate glycol, polycarbonate glycol, polyether Glycols and polytetrahydrofuran ether glycol
One of or it is a variety of.
7. the preparation method of leather separation layer finishing agent according to claim 1, it is characterised in that: the hydrophilic chain extender
For one of 2,2- dihydromethyl propionic acid, 2,2- dimethylolpropionic acid and N methyldiethanol amine；The organic base is three second
Amine, triethanolamine and diethyl ethylene diamine it is one or more.
8. the preparation method of leather separation layer finishing agent according to claim 1, it is characterised in that: the amine chain extender
It is one or more in hydrazine hydrate, ethylenediamine, diethylenetriamine and polyethers triamine；The organic solvent be dimethylformamide,
One of ethyl pyrrolidone, glycol dimethyl ether and dimethyl ether are a variety of.
9. a kind of leather separation layer finishing agent, it is characterised in that: the leather separation layer finishing agent is any by claim 1~8
The preparation method of leather separation layer finishing agent described in is prepared.
10. a kind of leather, it is characterised in that: the leather isolation covered with paint, lacquer, colour wash, etc. including leather separation layer finishing agent as claimed in claim 9
Layer.
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| CN110951040B (en) * | 2019-12-06 | 2022-04-12 | 嘉兴学院 | Cationic waterborne polyurethane leather color fixing agent and preparation method thereof |
| 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 |
| CN114181592A (en) * | 2021-12-30 | 2022-03-15 | 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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