CN115322285A - Permeable acrylic resin applied to leather effect layer and preparation method thereof - Google Patents
Permeable acrylic resin applied to leather effect layer and preparation method thereof Download PDFInfo
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- CN115322285A CN115322285A CN202210955022.8A CN202210955022A CN115322285A CN 115322285 A CN115322285 A CN 115322285A CN 202210955022 A CN202210955022 A CN 202210955022A CN 115322285 A CN115322285 A CN 115322285A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1802—C2-(meth)acrylate, e.g. ethyl (meth)acrylate
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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
- 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
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09D133/24—Homopolymers or copolymers of amides or imides
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
- Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Treatment And Processing Of Natural Fur Or Leather (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Synthetic Leather, Interior Materials Or Flexible Sheet Materials (AREA)
Abstract
The invention relates to a permeable acrylic resin applied to a leather effect layer and a preparation method thereof. The preparation method comprises the following steps: adding an emulsifier and a monomer into deionized water for mixing, and uniformly stirring to obtain a pre-emulsion; mixing and stirring an emulsifier and deionized water to obtain an emulsifier solution; adding 10% of pre-emulsion and initiator into an emulsifier solution for reaction, dropwise adding the rest pre-emulsion and initiator during the reaction, and obtaining first reaction liquid after the reaction is finished; respectively dropwise adding an oxidant solution and a reducing agent solution into the first reaction solution to obtain a second reaction solution; and cooling the second reaction solution, adding an ammonia water solution to adjust the pH value of the system, filtering and discharging. The preparation method introduces the urea heterocyclic monomer into the polymer structure to endow the coating film with high glossiness; and N-hydroxyethyl acrylamide is introduced to enable the N-hydroxyethyl acrylamide to have self-crosslinking reaction with carboxyl, so that the uniform fusion among molecules is facilitated, and better transparency and transparency can be obtained.
Description
Technical Field
The invention belongs to the field of leather treatment agents, and particularly relates to a permeable acrylic resin applied to a leather effect layer and a preparation method thereof.
Background
At present, leather products on the market are various, such as leather sofas, leather seats, leather bags and the like, and the leather surfaces of the leather products need to be subjected to a finishing procedure at the later processing stage so as to form various colors, various glosses and various appearances with different styles.
However, the transparent resin on the market at present has the problem that the softness, the gloss and the transparent feeling cannot be considered at the same time, and harmful gas can be generated in the preparation process.
Therefore, the technical scheme of the invention is provided.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a permeable acrylic resin applied to a leather effect layer and a preparation method thereof. According to the preparation method of the permeable acrylic resin applied to the leather effect layer, the urea heterocyclic monomer is introduced into the polymer structure to endow the coating film with high glossiness; n-hydroxyethyl acrylamide is introduced to enable the N-hydroxyethyl acrylamide to perform self-crosslinking reaction with carboxyl, so that uniform fusion among molecules is facilitated, and better transparency and permeability can be obtained; meanwhile, the ethyl acrylate and the ethyl methacrylate are respectively soft monomers and medium-hard monomers and are used for adjusting the hardness of the resin film; acrylic acid is a water-soluble monomer, and can improve the stability and adhesive force of the emulsion; and compared with the N-hydroxymethyl acrylamide used in the traditional preparation process, the formaldehyde release can be effectively reduced.
The scheme of the invention is to provide a preparation method of a permeable acrylic resin applied to a leather effect layer, which comprises the following steps:
(1) Adding an emulsifier and a monomer into deionized water for mixing, and uniformly stirring to obtain a pre-emulsion; wherein the monomer comprises ethyl acrylate, ethyl methacrylate, acrylic acid, N-hydroxyethyl acrylamide and a functional monomer; the functional monomer is one of ethylene urea ethoxy methacrylate or methacrylamide ethyl ethylene urea;
(2) Mixing and stirring an emulsifier and deionized water to obtain an emulsifier solution;
(3) Adding 10% of pre-emulsion and initiator into an emulsifier solution for reaction, dropwise adding the rest pre-emulsion and initiator during the reaction, and obtaining first reaction liquid after the reaction is finished;
(4) Respectively dropwise adding an oxidant solution and a reducing agent solution into the first reaction solution to obtain a second reaction solution;
(5) And cooling the second reaction solution, adding an ammonia water solution to adjust the pH value of the system, and then filtering and discharging.
Preferably, in the step (1), the weight ratio of the ethyl acrylate, the ethyl methacrylate, the acrylic acid, the functional monomer and the N-hydroxyethyl acrylamide is (70-90); the emulsifier accounts for 0.5-1.0 wt% of the total amount of the monomers; the weight ratio of the deionized water to the total amount of the monomers is 1.
Preferably, the emulsifier is a branched alkyl alcohol polyoxyethylene ether phosphate monoester.
Preferably, in the step (2), mixing and stirring are carried out at the temperature of 78-80 ℃; the emulsifier accounts for 1.0-2.0 wt% of the total amount of the monomers.
Preferably, in the step (3), the initiator is ammonium persulfate; in the stage where 10% of the pre-emulsion and initiator are added to the emulsifier solution (this stage is called "first stage", the same applies hereinafter), initiator is 0.3 to 1.0wt.% of the total amount of monomers; in the stage of dropwise addition of the remaining pre-emulsion and initiator (this stage is referred to as "second stage", the same applies hereinafter), the initiator is 0.1 to 0.5wt.% of the total amount of monomers; the reaction temperature is 84-86 ℃.
Preferably, the reaction liquid a obtained after the reaction in the step (3) is kept at 86-88 ℃ for 1h, and then is cooled to 70 ℃.
Preferably, in the step (4), the oxidizing agent is tert-butyl hydroperoxide, and the tert-butyl hydroperoxide accounts for 0.4 to 1.0wt.% of the total amount of the monomers; the reducing agent is ascorbic acid, and the ascorbic acid accounts for 0.2-0.5 wt% of the total amount of the monomers; the weight ratio of the oxidizing agent to the reducing agent is 2.
Preferably, in step (4), the dropwise addition is completed within 1h, and the temperature is maintained for 30min.
Preferably, in the step (5), the temperature is reduced to below 40 ℃, the pH of the system is adjusted to 7.5-8.5, and the solid content of the discharged system is 25-35 wt.%.
Based on the same technical concept, the invention also provides a transparent acrylic resin applied to the leather effect layer, which is prepared by the preparation method.
The beneficial effects of the invention are as follows:
according to the preparation method of the transparent acrylic resin applied to the leather effect layer, the urea heterocyclic monomer is introduced into the polymer structure, so that the high glossiness of the coating film can be endowed; n-hydroxyethyl acrylamide is introduced to enable the N-hydroxyethyl acrylamide to perform self-crosslinking reaction with carboxyl, so that uniform fusion among molecules is facilitated, and better transparency and permeability can be obtained; meanwhile, the ethyl acrylate and the ethyl methacrylate are respectively soft monomers and medium-hard monomers and are used for adjusting the hardness of the resin film; acrylic acid is a water-soluble monomer, and can improve the stability and the adhesive force of the emulsion; and compared with the N-hydroxymethyl acrylamide used in the traditional preparation process, the formaldehyde release can be effectively reduced.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It should be apparent that the described embodiments are only some embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The embodiment provides a preparation method of a transparent acrylic resin applied to a leather effect layer, which comprises the following steps:
(1) Adding deionized water, a branched chain alkyl alcohol polyoxyethylene ether phosphate monoester emulsifier, ethyl acrylate, ethyl methacrylate, acrylic acid, ethylene urea ethoxy methacrylate and N-hydroxyethyl acrylamide into a pre-emulsification tank, mixing, and stirring uniformly to obtain a pre-emulsion;
(2) Adding deionized water and a branched chain alkyl alcohol polyoxyethylene ether phosphate monoester emulsifier into a reaction kettle at 78 ℃, and mixing and stirring to obtain an emulsifier solution;
(3) Adding 10% of pre-emulsion and ammonium persulfate initiator solution into a reaction kettle, flushing the system to 85 ℃, dropwise adding the rest of pre-emulsion and ammonium sulfate initiator solution in 2 hours when the temperature tends to fall back, maintaining the temperature at 84 ℃ during dropwise adding, heating to 86 ℃ after the reaction is finished, keeping the temperature for 1 hour, and cooling to 70 ℃ to obtain first reaction liquid;
(4) Respectively dropwise adding a tert-butyl hydroperoxide solution and an ascorbic acid reducing agent solution into the first reaction solution for 1h, and completely dropwise adding the solution and keeping the temperature for 30min to obtain a second reaction solution;
(5) And cooling the second reaction liquid to 40 ℃, adding a 20% ammonia water solution to adjust the pH of the system to 7.5, filtering, and discharging to obtain the permeable acrylic resin emulsion with the solid content of 25 wt.%.
Wherein the raw materials are as shown in table 1.
Table 1 amounts of the respective raw material components in example 1
Note: the amount of deionized water in the step (2) and the concentrations of the emulsifier, the initiator, the oxidant and the reducing agent solution can be adjusted as required, and finally, the solid content of the final emulsion of the system is ensured to be 25 wt.%.
Example 2
The embodiment provides a preparation method of a transparent acrylic resin applied to a leather effect layer, which comprises the following steps:
(1) Adding deionized water, a branched chain alkyl alcohol polyoxyethylene ether phosphate monoester emulsifier, ethyl acrylate, ethyl methacrylate, acrylic acid, methacrylamide ethyl ethylene urea and N-hydroxyethyl acrylamide into a pre-emulsification tank, mixing, and stirring uniformly to obtain a pre-emulsion;
(2) Adding deionized water and a branched chain alkyl alcohol polyoxyethylene ether phosphate monoester emulsifier into a reaction kettle at the temperature of 80 ℃, and mixing and stirring to obtain an emulsifier solution;
(3) Adding 10% of pre-emulsion and ammonium persulfate initiator solution into a reaction kettle, flushing the system to 86 ℃, dropwise adding the rest of pre-emulsion and ammonium sulfate initiator solution within 2 hours when the temperature has a falling trend, maintaining the temperature at 85 ℃ during dropwise adding, heating to 88 ℃ after the reaction is finished, preserving the temperature for 1 hour, and cooling to 70 ℃ to obtain first reaction liquid;
(4) Dropwise adding a tert-butyl hydroperoxide solution and an ascorbic acid reducing agent solution into the first reaction liquid respectively, completely dropwise adding the tert-butyl hydroperoxide solution and the ascorbic acid reducing agent solution for 1 hour, and keeping the temperature for 30min to obtain a second reaction liquid;
(5) And cooling the second reaction liquid to 38 ℃, adding a 20% ammonia water solution to adjust the pH of the system to 8.5, filtering, and discharging to obtain the permeable acrylic resin emulsion with the solid content of 35wt.%.
The formula of the raw materials is shown in table 2.
Table 2 amounts of raw material components used in example 2
Note: the amount of deionized water in the step (2) and the concentrations of the emulsifier, the initiator, the oxidant and the reducing agent solution can be adjusted as required, and finally the solid content of the final emulsion of the system is ensured to be 35wt.%.
Example 3
The embodiment provides a preparation method of a permeable acrylic resin applied to a leather effect layer, which comprises the following steps:
(1) Adding deionized water, a branched chain alkyl alcohol polyoxyethylene ether phosphate monoester emulsifier, ethyl acrylate, ethyl methacrylate, acrylic acid, methacrylamide ethyl ethylene urea and N-hydroxyethyl acrylamide into a pre-emulsification tank, mixing, and stirring uniformly to obtain a pre-emulsion;
(2) Adding deionized water and a branched chain alkyl alcohol polyoxyethylene ether phosphate monoester emulsifier into a reaction kettle at 79 ℃ for mixing and stirring to obtain an emulsifier solution;
(3) Adding 10% of pre-emulsion and ammonium persulfate initiator solution into a reaction kettle, flushing the system to 86 ℃, dropwise adding the rest of pre-emulsion and ammonium sulfate initiator solution in 2 hours when the temperature tends to fall back, maintaining the temperature at 85 ℃ during dropwise adding, heating to 88 ℃ after the reaction is finished, keeping the temperature for 1 hour, and cooling to 70 ℃ to obtain first reaction liquid;
(4) Respectively dropwise adding a tert-butyl hydroperoxide solution and an ascorbic acid reducing agent solution into the first reaction solution for 1h, and completely dropwise adding the solution and keeping the temperature for 30min to obtain a second reaction solution;
(5) And cooling the second reaction liquid to 35 ℃, adding a 20% ammonia water solution to adjust the pH of the system to 8.0, filtering, and discharging to obtain the permeable acrylic resin emulsion with the solid content of 30 wt.%.
The formulation of the raw materials is shown in table 3.
Table 3 amounts of the respective raw material components in example 3
Note: the amount of deionized water in the step (2) and the concentrations of the emulsifier, the initiator, the oxidant and the reducing agent solution can be adjusted as required, and finally the solid content of the final emulsion of the system is ensured to be 30 wt.%.
Test examples
And sequentially carrying out bottom sealing and bottom slurry treatment on the treated buffed cowhide sofa leather blank, spraying isolation and surface slurry, and finally carrying out effect layer coating, wherein the formula of the effect layer is shown in table 4.
TABLE 4 Effect layer formulation
| Starting materials | Dosage of |
| Transparent pigment paste | 35g |
| Acrylic resin to be tested | 150g |
| DOWELLIURU2305 | 130g |
| DOWELLERCASEIN5835 | 40g |
| DOWELLERWAX5050 | 50g |
| Water (W) | 100g |
The acrylic resins to be tested are the permeable acrylic resin obtained in example 3 and the commercially available permeable resins of the same type, and the detection results of the effect layer are shown in table 5.
TABLE 5 test results
| Item | Commercially available same type transparent resin | Transparent acrylic resin obtained in example 3 |
| Softness degree | 4.0 | 4.5 |
| 60 degree gloss | 2.3 | 2.8 |
| Sense of permeability | 3.5 | 4.5 |
Wherein, softness and transparency are divided into 5 grades, and the higher the grade is, the better the softness is, the better the transparency is.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (10)
1. A preparation method of a permeable acrylic resin applied to a leather effect layer is characterized by comprising the following steps:
(1) Adding an emulsifier and a monomer into deionized water for mixing, and uniformly stirring to obtain a pre-emulsion; wherein the monomer comprises ethyl acrylate, ethyl methacrylate, acrylic acid, N-hydroxyethyl acrylamide and a functional monomer; the functional monomer is one of ethylene urea ethoxy methacrylate or methacrylamide ethyl ethylene urea;
(2) Mixing and stirring an emulsifier and deionized water to obtain an emulsifier solution;
(3) Adding 10% of pre-emulsion and initiator into an emulsifier solution for reaction, dropwise adding the rest pre-emulsion and initiator during the reaction, and obtaining first reaction liquid after the reaction is finished;
(4) Respectively dropwise adding an oxidant solution and a reducing agent solution into the first reaction solution to obtain a second reaction solution;
(5) And cooling the second reaction solution, adding an ammonia water solution to adjust the pH value of the system, filtering and discharging.
2. The preparation method of the permeable acrylic resin applied to the leather effect layer according to claim 1, wherein in the step (1), the weight ratio of the ethyl acrylate, the ethyl methacrylate, the acrylic acid, the functional monomer and the N-hydroxyethyl acrylamide is 70-90; the emulsifier accounts for 0.5 to 1.0wt.% of the total amount of the monomers; the weight ratio of the deionized water to the total amount of the monomers is 1.
3. The method for preparing the transparent acrylic resin applied to the leather effect layer according to claim 1, wherein the emulsifier is a branched alkyl alcohol polyoxyethylene ether phosphate monoester.
4. The method for preparing the transparent acrylic resin applied to the leather effect layer according to the claim 1, wherein in the step (2), the mixture is stirred at 78-80 ℃; the emulsifier accounts for 1.0-2.0 wt% of the total amount of the monomers.
5. The method for preparing the transparent acrylic resin applied to the leather effect layer according to claim 1, wherein in the step (3), the initiator is ammonium persulfate; in the stage of adding 10% of pre-emulsion and initiator into the emulsifier solution, the initiator accounts for 0.3-1.0 wt% of the total amount of the monomers; in the stage of dripping the rest pre-emulsion and the initiator, the initiator accounts for 0.1 to 0.5 weight percent of the total amount of the monomers; the reaction temperature is 84-86 ℃.
6. The preparation method of the transparent acrylic resin applied to the leather effect layer as claimed in claim 1, wherein the reaction solution a obtained after the reaction in the step (3) is kept at 86-88 ℃ for 1h and then cooled to 70 ℃.
7. The method for preparing the transparent acrylic resin applied to the leather effect layer as claimed in claim 1, wherein in the step (4), the oxidant is tert-butyl hydroperoxide, and the tert-butyl hydroperoxide accounts for 0.4-1.0 wt.% of the total amount of the monomers; the reducing agent is ascorbic acid, and the ascorbic acid accounts for 0.2-0.5 wt% of the total amount of the monomers; the weight ratio of the oxidizing agent to the reducing agent is 2.
8. The method for preparing the transparent acrylic resin applied to the leather effect layer according to claim 1, wherein in the step (4), the dripping is completed within 1h and the temperature is kept for 30min.
9. The preparation method of the transparent acrylic resin applied to the leather effect layer as claimed in claim 1, wherein in the step (5), the temperature is reduced to be below 40 ℃, the pH of the system is adjusted to be 7.5-8.5, and the solid content of the discharged system is 25-35 wt.%.
10. The transparent acrylic resin applied to the leather effect layer obtained by the preparation method of any one of claims 1 to 9.
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| CN111454402A (en) * | 2020-06-02 | 2020-07-28 | 上海金狮化工有限公司 | Acrylate emulsion leather finishing agent and preparation method thereof |
| CN114133481A (en) * | 2021-10-28 | 2022-03-04 | 上海金狮化工有限公司 | Acrylic coating resin and preparation method and application thereof |
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2022
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Patent Citations (8)
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| CN101831230A (en) * | 2010-04-09 | 2010-09-15 | 陕西科技大学 | Method for preparing polyacrylate/nano-SiO2 compound coating agent by using reactive emulsifier |
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