CN111394042B - PU adhesive for soft mirror leather and preparation method thereof - Google Patents
PU adhesive for soft mirror leather and preparation method thereof Download PDFInfo
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- CN111394042B CN111394042B CN202010240544.0A CN202010240544A CN111394042B CN 111394042 B CN111394042 B CN 111394042B CN 202010240544 A CN202010240544 A CN 202010240544A CN 111394042 B CN111394042 B CN 111394042B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
- C09J175/06—Polyurethanes from polyesters
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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
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
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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
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/4236—Polycondensates having carboxylic or carbonic ester groups in the main chain containing only aliphatic groups
- C08G18/4238—Polycondensates having carboxylic or carbonic ester groups in the main chain containing only aliphatic groups derived from dicarboxylic acids and dialcohols
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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
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
- C08G18/7614—Polyisocyanates or polyisothiocyanates cyclic aromatic containing only one aromatic ring
- C08G18/7628—Polyisocyanates or polyisothiocyanates cyclic aromatic containing only one aromatic ring containing at least one isocyanate or isothiocyanate group linked to the aromatic ring by means of an aliphatic group
- C08G18/7642—Polyisocyanates or polyisothiocyanates cyclic aromatic containing only one aromatic ring containing at least one isocyanate or isothiocyanate group linked to the aromatic ring by means of an aliphatic group containing at least two isocyanate or isothiocyanate groups linked to the aromatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate groups, e.g. xylylene diisocyanate or homologues substituted on the aromatic ring
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Synthetic Leather, Interior Materials Or Flexible Sheet Materials (AREA)
- Polyurethanes Or Polyureas (AREA)
Abstract
The scheme relates to a PU adhesive for soft lens leather and a preparation method thereof, and the preparation method comprises the following steps: adding polyester polyol and isocyanate into a reaction bottle, stirring and reacting for 2 hours at 70-80 ℃, adding a dihydric alcohol chain extender and an organic solvent to seal the end of the polyester polyol and the isocyanate, and continuously stirring for 1 hour to package the polyester polyol and the isocyanate to obtain a main agent with the solid content of 60%; adding another organic solvent, isocyanate and a trifunctional chain extender into another reaction bottle, reacting for 2 hours at 70-80 ℃, cooling and discharging to obtain a curing agent with the NCO content of 10% and the solid content of 80%; and mixing the main agent and the curing agent in proportion, and adding an organic solvent for dilution until the PU adhesive for the soft mirror leather with the solid content of 40% is obtained. The PU adhesive for soft lens leather is resistant to permeation of organic silicon and a plasticizer, and does not have a matte surface when used for the soft lens leather; the product has high peel strength, good hydrolysis resistance and mildew resistance and soft hand feeling; has the advantages of simple preparation process, convenient operation and the like.
Description
Technical Field
The invention relates to the field of PU adhesives, and particularly relates to a PU adhesive for soft mirror leather and a preparation method thereof.
Background
The improvement of living standard promotes the rapid upgrade of consumption level of people, and especially, the handbag used by women has different styles and is frequently updated. In recent years, PU handbags for mirror leather are gradually raised, and the impression of the old plate of the leather-like style of the leather-like PU synthetic leather of the prior art is changed. In contrast to conventional leather and PU leather handbags, the PU bag for mirror leather exhibits a good reflective property "glittering" under sunlight, and its surface is extremely flat, thus exhibiting the mirror style called "mirror leather". The PU leather of the common wet method type needs to be subjected to graining treatment, and the surface of the PU leather is uneven and refracted by image light, so that the PU leather does not have the effect of a mirror. Mirror-style handbags can be classified into the following types according to differences in hand feel: such as rebound type, branding color-changing type, hard type, soft and elastic type, Q-sense type, soft type and meat sense type.
When preparing polyurethane synthetic leather (PU leather), the foaming purpose is mainly achieved by utilizing the microphase separation between PU molecular chains, if the needed hand feeling of the PU leather can not be obtained by only pure PU resin, a certain amount of auxiliary agents are required to be added into the resin for regulation, and the commonly used auxiliary agents are as follows: organosilicon, modified polyether, plasticizer, diatomite, kaolin and the like. PU leather made of pure PU resin generally has hard hand feeling, and the resin is preferably used for hard mirror surface leather with rebound resilience and branding color change. Meanwhile, because the PU resin is pure, the situation that the auxiliary agent is separated out to the surface of the dry-process fabric in the wet-process bass process to cause the surface of the mirror leather to fog is not needed to be worried about. The reason for the fogging of the mirror surface also includes the fogging caused by the precipitation of the organic solvent remained in the PU adhesive into the dry-process fabric. The soft elastic type, Q-feeling type, soft type and meat-feeling type PU mirror leather cannot achieve the hand feeling by pure PU resin, and the hand feeling cannot be achieved by pure PU resin, the hand feeling cannot be adjusted by a certain amount of auxiliary agents, and the most common method is to add organic silicon and a plasticizer into wet resin to prepare the wet base with the hand feeling. However, the compatibility between the resin and the additives is poor easily due to the addition of the organic silicon or the plasticizer in the wet-process PU resin, and the additives easily enter the dry-process surface layer through the PU adhesive after the dry-process veneering is completed, so that the surface of the PU leather is fogged. If the common PU leather is subjected to graining, the fogging of the leather surface does not affect the performance and the selling price, but the graining of the mirror leather is not needed, and if the leather is fogged, the refraction of light rays is directly affected, so the selling price grade of the mirror leather is directly reduced. Therefore, in order to prevent fogging, the PU adhesive used for soft mirror leather must have both dry-bonding (ensuring that organic solvent in the adhesive is completely volatilized when wet-bonding is performed) and performance of preventing the auxiliary agent from being precipitated.
Few PU adhesives sold on the market are suitable for dry sticking, can resist the penetration of organic silicon and plasticizer, and simultaneously keeps higher peel strength and soft hand feeling. How to prepare the PU adhesive suitable for the soft lens leather is always a research hotspot in recent years.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the PU adhesive for the soft mirror leather and the preparation method thereof, so that the prepared adhesive is suitable for dry sticking and is resistant to penetration of organic silicon and plasticizer.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a preparation method of a PU adhesive for soft lens leather comprises the following steps:
1) adding polyester polyol and isocyanate into a reaction bottle, stirring and reacting for 2 hours at 70-80 ℃, then adding a dihydric alcohol chain extender and an organic solvent to seal the end of the polyester polyol and the isocyanate, and continuously stirring for 1 hour to package the polyester polyol and the isocyanate to obtain a main agent with the solid content of 60%;
2) adding another organic solvent, isocyanate and a trifunctional chain extender into another reaction bottle, reacting for 2 hours at 70-80 ℃, cooling and discharging to obtain a curing agent with the NCO content of 10% and the solid content of 80%;
3) and mixing the main agent and the curing agent in proportion, and adding an organic solvent for dilution until the PU adhesive for the soft mirror leather with the solid content of 40% is obtained.
Preferably, in the preparation method, the polyester polyol is at least one selected from the group consisting of poly (methyl propylene adipate) glycol, poly (methyl propylene sebacate) glycol, poly (neopentyl glycol adipate) glycol, and poly (neopentyl glycol sebacate) glycol.
Preferably, in the preparation method, the isocyanate in step 1) and step 2) is m-xylylene isocyanate.
Preferably, in the preparation method, the glycol chain extender in the step 1) is methyl propylene glycol.
Preferably, in the preparation method, the trifunctional chain extender in the step 2) is one selected from glycerol, trimethylolpropane, diethylenetriamine and triethanolamine.
Preferably, the preparation method, wherein the organic solvent in step 1) and the other organic solvent in step 2) are selected from any two of dimethyl carbonate, butanone, acetone, cyclohexanone, and N, N-Dimethylformamide (DMF).
The PU adhesive for the soft mirror leather prepared by the preparation method.
The technical difficulty of the invention is that the PU adhesive has low crystallinity and high-strength stripping, and the prepared PU adhesive is suitable for dry sticking and can resist the penetration of organic silicon and plasticizer. Researches show that the crystallization performance of the PU resin can be reduced due to the steric hindrance effect of the polyester polyol containing the side methyl and the chain extender, and the PU adhesive is endowed with the advantages of dry adhesion and soft hand feeling. Meanwhile, the side methyl structure plays a role of a long arm in PU resin, can prevent organic silicon and a plasticizer existing in wet base fabric from permeating into the surface of dry-process fabric, and has good hydrolysis resistance, heat resistance and mould resistance. But the common peeling strength of the PU resin with poor crystallization performance is low, but the invention adopts a two-component mode to replace a common single component, and the curing agent uses a trifunctional chain extender which can form a cross-linked network structure with an auxiliary agent, thereby overcoming the defect of low peeling of the low-crystallinity PU adhesive. The PU adhesive prepared by the invention is applied to soft mirror leather, has the characteristics of high peeling, hydrolysis resistance and mould resistance, and has no fogging condition on the surface after being placed in the air for half a year. Therefore, the PU adhesive has the characteristics of simple process, convenience in operation, low raw material cost and high product added value, and is particularly suitable for preparing soft elastic, Q-feeling, soft and meat-feeling high-grade PU mirror leather.
The polyester polyols used in the invention all have a side methyl structure, and long-chain polyols have side methyl groups, so that the side methyl structure is similar to that of an arm, the plasticizer in PU resin can be effectively prevented from exuding to cause fogging on the surface of soft lens leather, and a PU adhesive prepared from the polyester polyols containing the side methyl groups can also play a role of a long arm in the aspects of hydrolysis resistance, mildew resistance, thermal oxidation resistance, solvent resistance and the like. The structure of the side methyl has larger steric hindrance, and can effectively reduce the crystallization property of the PU resin, thereby reducing the softening point of the PU resin and enabling the PU resin to be suitable for dry pasting. The fogging of the mirror leather is related to the organic solvent remained in the PU adhesive, and is also related to the precipitation of the organic silicon and the plasticizer existing in the wet base.
The isocyanate in the invention is XDI (m-xylylene isocyanate); XDI has a single benzene ring structure, avoids the high crystallization performance of MDI (diphenylmethane diisocyanate) symmetrical double benzene ring structure, and inserts a-CH between isocyanate group and benzene ring in XDI2Effectively avoids resonance between benzene rings and isocyanate and prevents rolling structure under the condition of ultraviolet irradiation. And XDI has higher reaction activity, and the use of a catalyst can be avoided in the system. Most of catalysts used in the current market are organic metal, the aging rate of PU leather is easy to accelerate due to residual metal ions, and the XDI used in the invention can effectively avoid the condition.
The glycol chain extender used in the invention is methyl propylene glycol; because the methyl propylene glycol has an asymmetric structure, the PU adhesive prepared from the methyl propylene glycol has lower crystallization property and lower viscosity, and is convenient for the gluing treatment in the use process of leather factories. Meanwhile, the methyl propylene glycol has long arms, and the steric hindrance effect of the methyl propylene glycol can better endow the PU adhesive with the performances of solvent resistance, hydrolysis resistance, mildew resistance, aging delay and the like.
The trifunctional chain extender used in the present invention includes, but is not limited to, any one of glycerin, trimethylolpropane, diethylenetriamine, or triethanolamine. In the invention, because a large amount of polyester polyol with lateral methyl and a chain extender are used, the prepared PU adhesive has poor crystallinity and low softening point, and the prepared PU leather has poor peel strength. Therefore, the PU adhesive has a two-component PU adhesive structure, and the curing agent contains the trifunctional chain extender, so that a space net structure can be formed with the main agent, and the initial adhesion and the peel strength of the PU adhesive are enhanced conveniently.
According to the invention, different organic solvents are used in a matched manner, so that the solvents in the PU adhesive are volatilized in a gradient manner, the bonded material is better infiltrated, and the leveling problem (pits appear on the surface of the adhesive) caused by the concentrated volatilization of the solvents at a certain moment under a high-temperature condition is avoided, and the attractiveness and physical properties of the PU leather finished product are influenced.
The invention has the beneficial effects that: compared with the traditional PU adhesive, the PU adhesive for soft lens leather prepared by the invention has the following advantages: 1) the paint is resistant to permeation of organic silicon and a plasticizer, and does not have a matte surface when being used for soft mirror leather; 2) the prepared PU adhesive has higher peel strength, better hydrolysis resistance and mildew resistance and softer hand feeling; 3) the invention has the advantages of simple preparation process, convenient operation and the like; 4) wide application range and wide market.
Detailed Description
The technical solutions of the present invention are described clearly and completely below, and it is obvious that the described embodiments are some, not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In addition, the technical features involved in the different embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
First, preparation process
Firstly, weighing a certain amount of polyester polyol in a reaction bottle, distilling at 110 ℃ under reduced pressure to remove water to below 300ppm, and then adding an antioxidant and phosphoric acid to fully and uniformly stir. And adding isocyanate into a reaction bottle, uniformly stirring to react for 2 hours at 70-80 ℃, adding a dihydric alcohol chain extender and an organic solvent to seal the end of the isocyanate, and continuously stirring for 1 hour to package, wherein the component is a main agent part and the solid content is 60%. And adding an organic solvent into the other reaction bottle, adding isocyanate and a trifunctional chain extender, reacting for 2 hours at 70-80 ℃, cooling and discharging to prepare the curing agent with the NCO content of 10% and the solid content of 80%. When in use, the main agent and the curing agent are mixed according to a certain proportion, and then the organic solvent is added for dilution until the PU adhesive with the solid content of 40% is obtained.
Example 1: 300g of poly (methyl propylene glycol adipate) glycol is weighed in a reaction bottle, the water is removed to be below 300ppm by reduced pressure distillation at the temperature of 110 ℃, and simultaneously 0.2g of antioxidant BHT and 0.003g of phosphoric acid are added and fully stirred uniformly. And adding 71g of isocyanate (XDI) into a reaction bottle, uniformly stirring the mixture to react for 2 hours at the temperature of 70-80 ℃, adding 20.3g of methyl propylene glycol chain extender and an organic solvent N, N-dimethylformamide into the mixture to seal the end of the mixture, continuously stirring the mixture for 1 hour, and then packaging the mixture, wherein the main agent part is obtained, and the solid content is 60%. And adding an organic solvent butanone into another reaction bottle, then adding 110g of XDI and 17g of glycerol, reacting for 2 hours at the temperature of 70-80 ℃, cooling and discharging to prepare the curing agent with the NCO content of 10% and the solid content of 80%.
Example 2: 300g of poly sebacic acid methyl propylene glycol ester is weighed in a reaction bottle, reduced pressure distillation is carried out at the temperature of 110 ℃ to remove the water to be below 300ppm, and simultaneously 0.2g of antioxidant BHT and 0.003g of phosphoric acid are added and fully stirred uniformly. And adding 71g of isocyanate (XDI) into a reaction bottle, uniformly stirring the mixture to react for 2 hours at the temperature of 70-80 ℃, adding 20.3g of methyl propylene glycol chain extender and an organic solvent N, N-dimethylformamide into the mixture to seal the end of the mixture, continuously stirring the mixture for 1 hour, and then packaging the mixture, wherein the main agent part is obtained, and the solid content is 60%. And adding an organic solvent dimethyl carbonate into another reaction bottle, then adding 110g of XDI and 25g of trimethylolpropane, reacting for 2h at 70-80 ℃, adding the organic solvent, cooling and discharging to prepare the curing agent with the NCO content of 10% and the solid content of 80%.
Example 3: 300g of poly neopentyl glycol adipate diol is weighed into a reaction bottle, the water is removed to be below 300ppm by reduced pressure distillation at the temperature of 110 ℃, and simultaneously 0.2g of antioxidant BHT and 0.003g of phosphoric acid are added and fully stirred uniformly. And adding 71g of isocyanate (XDI) into a reaction bottle, uniformly stirring the mixture to react for 2 hours at the temperature of 70-80 ℃, adding 20.3g of methyl propylene glycol chain extender and an organic solvent N, N-dimethylformamide into the mixture to seal the end of the mixture, continuously stirring the mixture for 1 hour, and then packaging the mixture, wherein the main agent part is obtained, and the solid content is 60%. And adding an organic solvent acetone into another reaction bottle, then adding 110g of XDI and 19g of diethylenetriamine, reacting for 2h at 70-80 ℃, adding the organic solvent, cooling and discharging to prepare the curing agent with the NCO content of 10% and the solid content of 80%.
Example 4: weighing 300g of neopentyl glycol sebacate diol into a reaction bottle, distilling at 110 ℃ under reduced pressure to remove water to below 300ppm, adding 0.2g of antioxidant BHT and 0.003g of phosphoric acid, and fully and uniformly stirring. And adding 71g of isocyanate (XDI) into a reaction bottle, uniformly stirring the mixture to react for 2 hours at the temperature of 70-80 ℃, adding 20.3g of methyl propylene glycol chain extender and an organic solvent N, N-dimethylformamide into the mixture to seal the end of the mixture, continuously stirring the mixture for 1 hour, and then packaging the mixture, wherein the main agent part is obtained, and the solid content is 60%. And adding an organic solvent cyclohexanone into another reaction bottle, then adding 110g of XDI and 28g of triethanolamine, reacting for 2h at 70-80 ℃, adding the organic solvent, cooling and discharging, and preparing the curing agent with the NCO content of 10% and the solid content of 80%.
II, conclusion
Under the same conditions, preparing a PU adhesive from the main agent and the curing agent prepared in the embodiments according to a ratio of 100:7, adding an organic solvent DMF (dimethyl formamide) for dilution and stirring uniformly to enable the solid content of the PU adhesive to be 40%, coating the PU adhesive on the surface of a dry-method fabric, placing the dry-method fabric in a drying oven at 110 ℃ for 3min to remove the organic solvent, and then using wet-method Bass to overlay the soft mirror leather. And peeling off the dried soft lens leather from the release paper to obtain the soft lens leather. The fogging condition, peel strength, mold resistance and hydrolysis resistance of the surfaces of the soft lens leathers prepared in the 4 examples were compared to perform comprehensive evaluation, and the obtained experimental results are shown in table one.
Comprehensive physical property comparison of PU adhesive for surface-soft mirror leather
From the table one, it can be seen that the PU adhesive prepared in example 1 exhibits the best physical properties when used in soft lens leather. The PU adhesive obtained in the embodiment 1 has a wider market prospect than other adhesives.
While embodiments of the invention have been disclosed above, it is not limited to the applications listed in the description and the embodiments, which are fully applicable in all kinds of fields of application of the invention, and further modifications may readily be effected by those skilled in the art, so that the invention is not limited to the specific details without departing from the general concept defined by the claims and the scope of equivalents.
Claims (4)
1. A preparation method of a PU adhesive for soft lens leather is characterized by comprising the following steps:
1) adding polyester polyol and isocyanate into a reaction bottle, stirring and reacting for 2 hours at 70-80 ℃, then adding a glycol chain extender methyl propylene glycol and an organic solvent to seal the end of the polyester polyol and the isocyanate, and continuously stirring for 1 hour to package the polyester polyol and the isocyanate to obtain a main agent with the solid content of 60%;
2) adding another organic solvent, isocyanate and a trifunctional chain extender into another reaction bottle, reacting for 2 hours at 70-80 ℃, cooling and discharging to obtain a curing agent with the NCO content of 10% and the solid content of 80%;
3) mixing a main agent and a curing agent in proportion, and adding an organic solvent for dilution until the PU adhesive for soft mirror leather with the solid content of 40% is obtained; wherein the polyester polyol is selected from the group consisting of poly (methyl propylene adipate) glycol and poly (methyl propylene sebacate) glycol; the trifunctional chain extender is glycerol or trimethylolpropane.
2. The method according to claim 1, wherein the isocyanate in step 1) and step 2) is m-xylylene isocyanate.
3. The method according to claim 1, wherein the organic solvent in step 1) and the other organic solvent in step 2) are selected from any two of dimethyl carbonate, methyl ethyl ketone, acetone, cyclohexanone, and N, N-dimethylformamide.
4. A PU adhesive for soft lens leather prepared by the preparation method according to any one of claims 1 to 3.
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| CN202010240544.0A CN111394042B (en) | 2020-03-31 | 2020-03-31 | PU adhesive for soft mirror leather and preparation method thereof |
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| CN202010240544.0A CN111394042B (en) | 2020-03-31 | 2020-03-31 | PU adhesive for soft mirror leather and preparation method thereof |
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| CN111394042B true CN111394042B (en) | 2021-12-28 |
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| CN101463242B (en) * | 2009-01-22 | 2012-05-09 | 嘉兴禾欣化学工业有限公司 | Double-component environment protection type polyurethane adhesive for PVC thin film dry type composition and preparation method thereof |
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