CN115679702B - Yellowing-resistant fly-weaving treating agent and preparation method thereof - Google Patents
Yellowing-resistant fly-weaving treating agent and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a yellowing-resistant fly-weaving treating agent and a preparation method thereof, belonging to the technical field of shoe treating agents. The formula comprises polyester polyol, epoxy resin, HDI, a terminator, a catalyst, butanone and ethyl acetate. The preparation method comprises the following steps: mixing, reacting, stopping, and adjusting the solid content. The yellowing-resistant fly-weaving treatment agent prepared by the invention is particularly suitable for fly-weaving fabrics. The polymer obtained by blending and crosslinking has small molecular weight, is easy to diffuse to the surface of the fly-weaving cloth and permeate into the concave holes, and has higher reactivity, so that a crosslinking structure is easy to form with the fly-weaving surface, and the adhesive force is improved. The pure aliphatic HDI is used as a reaction raw material, so that the problem that the mechanical property is reduced and the aromatic isocyanate is degraded to generate a chromophore because the aromatic isocyanate has a benzene ring structure and a crosslinking structure is broken under the light, heat and oxygen environments is avoided.
Description
Technical Field
The invention belongs to the technical field of shoe treatment agents, and particularly relates to a yellowing-resistant fly-weaving treatment agent and a preparation method thereof.
Background
Fly-knitting (Flyknit) is a novel lightweight technology, is mainly used for processing the vamp of the whole sports shoe, and the fly-knitting fabric prepared by the fly-knitting technology has the following advantages:
1) Has rich texture change. The biggest difference between the fly-knitted fabric and the traditional shoemaking fabric is that the yarn diversity and the change of the tissue structure can be used for designing rich texture effects.
2) Has good elasticity and extensibility. The elongation rate of the fly-knitting material is greatly higher than that of the traditional leather material, the elasticity of each angle is not greatly different, the knitted upper can wrap the feet well, and the wearing comfort experience is improved. The properties and combination form of the yarns, the shape and size of the loops, the weave structure of the fabric and the like are key factors influencing the elasticity and the ductility of the fly fabric.
3) The manufacturing of the fly-knitting fabric with higher technological content is completed by computer programming input and automatic knitting by a machine, thus changing the manufacturing flow of the traditional shoes and boots.
Although fly-knitted fabrics are rapidly developed, the related shoe treatment products and techniques are quite deficient and are essentially blank.
Disclosure of Invention
The invention provides a yellowing-resistant fly-weaving treatment agent and a preparation method thereof, and fills the market blank in the aspect of fly-weaving treatment agent.
The invention provides a yellowing-resistant fly-weaving treatment agent, which comprises the following components in parts by mass:
in particular, the polyester polyol is polyester glycol with a hydroxyl value of 34-40mgKOH/g, an acid value of less than or equal to 0.30mgKOH/g, a water content of less than or equal to 0.03%, a molecular weight of 3000+/-500 and a chromaticity of less than or equal to 30.
In particular, the epoxy resin is transparent semi-solid, the epoxy equivalent weight is 454-555g/Eq, and the epoxy value is 0.18-0.22Eq/mg.
In particular, the terminator is at least one of 1, 3-butanediol, 1, 4-butanediol, ethylene glycol and 1, 6-hexanediol.
In particular, the catalyst is at least one of dibutyl tin dilaurate and stannous octoate.
The second object of the present invention is to provide a method for preparing the yellowing-resistant fly-weaving treatment agent, comprising the steps of:
(1) Butanone, polyester polyol and epoxy resin are put into a reaction kettle, and mixed and dissolved to obtain a mixture A;
(2) Heating a reaction kettle, adding HDI and a catalyst into the kettle, stirring with the mixture A, and stopping the reaction after detecting that the red light spectrum is not changed any more to obtain a mixture B;
(3) Adding a terminator into the mixture B, stirring for reaction, stopping heating, adding ethyl acetate, and stirring for reaction at the residual temperature to obtain a mixture C;
(4) Measuring the solid content and viscosity of the mixture C; and when the solid content and the viscosity are out of the required range of the product, adding ethyl acetate into the mixture C and uniformly mixing until the solid content and the viscosity of the mixture C meet the standards, thus obtaining the yellowing-resistant fly-weaving treatment agent.
Particularly, in the step (1), stirring is carried out during mixing and dissolving, wherein the stirring speed is more than or equal to 400rpm; the temperature is more than or equal to 50 ℃, and the dissolution time is more than or equal to 2 hours.
In particular, in the step (2), the temperature of the reaction kettle is increased to be more than or equal to 80 ℃, and the stirring rotating speed is more than or equal to 60rpm.
Particularly, in the step (3), the stirring time is more than or equal to 10min after the terminator is added, and the rotating speed is more than or equal to 60rpm; the rotation speed of the residual temperature stirring is more than or equal to 200rpm, and the time is more than or equal to 2 hours.
In particular, in said step (4), the solid content of mixture C is 15-20% and the viscosity is 1800-2400CPS/25 ℃.
The invention takes diisocyanate as a cross-linking agent, and simultaneously reacts with hydroxyl in polyester polyol and hydroxyl in epoxy resin to form a polyurethane structure through cross-linking.
Compared with the prior art, the invention has the beneficial effects that:
the yellowing-resistant fly-weaving treatment agent prepared by the invention is particularly suitable for fly-weaving fabrics. The polymer obtained by blending and crosslinking has small molecular weight, is easy to diffuse to the surface of the fly-weaving cloth and permeate into the concave holes, and has higher reactivity, so that a crosslinking structure is easy to form with the fly-weaving surface, and the adhesive force is improved.
The pure aliphatic HDI is used as a reaction raw material, so that the problem that the mechanical property is reduced and the aromatic isocyanate is degraded to generate a chromophore because the aromatic isocyanate has a benzene ring structure and a crosslinking structure is broken under the light, heat and oxygen environments is avoided.
Detailed Description
For a better understanding of the present invention, reference will now be made to the following description of specific examples, which are included in the terminology used to describe specific embodiments of the invention and are not intended to limit the scope of the invention.
In the invention, the following components are added:
HDI refers to hexamethylene diisocyanate;
example 1
A preparation method of a yellowing-resistant fly-weaving treatment agent comprises the following steps:
(1) Weighing corresponding raw materials according to the following mass fractions for standby;
wherein the polyester polyol is polyester glycol with a hydroxyl value of 34-40mgKOH/g, an acid value of less than 0.30mgKOH/g, a water content of less than 0.03%, a molecular weight of 3000+500 and a chromaticity of less than 30; the epoxy resin is transparent semisolid, the epoxy equivalent weight is 454-555g/Eq, and the epoxy value is 0.18-0.22Eq/mg; the terminator is 1, 3-butanediol; the catalyst is dibutyl tin dilaurate;
(2) Butanone, polyester polyol and epoxy resin are put into a reaction kettle, and mixed and dissolved to obtain a mixture A;
stirring is carried out during mixing and dissolving, and the stirring rotating speed is 400rpm; the temperature was 50℃and the dissolution time was 2h.
(3) Heating the reaction kettle to 80 ℃, adding HDI and a catalyst into the kettle, stirring the mixture with the mixture A at 60rpm, and stopping the reaction after detecting that the red light spectrum is not changed any more to obtain a mixture B;
(4) Adding a terminator into the mixture B, stirring and reacting for 10min, wherein the rotating speed is more than or equal to 60rpm; stopping heating, adding ethyl acetate, and stirring for reaction at the residual temperature to obtain a mixture C;
the rotational speed of the stirring at the residual temperature is 200rpm for 2 hours.
(5) Measuring the solid content and viscosity of the mixture C; and when the solid content and the viscosity are out of the required range of the product, adding ethyl acetate into the mixture C and uniformly mixing until the solid content and the viscosity of the mixture C meet the standards, thus obtaining the yellowing-resistant fly-weaving treatment agent.
In said step (5), the solid content of mixture C was 15% and the viscosity was 1812CPS/25 ℃.
Example two
A preparation method of a yellowing-resistant fly-weaving treatment agent comprises the following steps:
(1) Weighing corresponding raw materials according to the following mass fractions for standby;
wherein the polyester polyol is polyester glycol with a hydroxyl value of 34-40mgKOH/g, an acid value of less than 0.30mgKOH/g, a water content of less than 0.03%, a molecular weight of 3000+500 and a chromaticity of less than 30; the epoxy resin is transparent semisolid, the epoxy equivalent weight is 454-555g/Eq, and the epoxy value is 0.18-0.22Eq/mg; the terminator is 1, 4-butanediol; the catalyst is stannous octoate;
(2) Butanone, polyester polyol and epoxy resin are put into a reaction kettle, and mixed and dissolved to obtain a mixture A;
stirring is carried out during mixing and dissolving, and the stirring rotating speed is 400rpm; the temperature was 50℃and the dissolution time was 2h.
(3) Heating the reaction kettle to 80 ℃, adding HDI and a catalyst into the kettle, stirring the mixture with the mixture A at 60rpm, and stopping the reaction after detecting that the red light spectrum is not changed any more to obtain a mixture B;
(4) Adding a terminator into the mixture B, stirring and reacting for 10min, wherein the rotating speed is more than or equal to 60rpm; stopping heating, adding ethyl acetate, and stirring for reaction at the residual temperature to obtain a mixture C;
the rotational speed of the stirring at the residual temperature is 200rpm for 2 hours.
(5) Measuring the solid content and viscosity of the mixture C; and when the solid content and the viscosity are out of the required range of the product, adding ethyl acetate into the mixture C and uniformly mixing until the solid content and the viscosity of the mixture C meet the standards, thus obtaining the yellowing-resistant fly-weaving treatment agent.
In said step (5), the solid content of mixture C is 20% and the viscosity is 2400CPS/25 ℃.
Example III
A preparation method of a yellowing-resistant fly-weaving treatment agent comprises the following steps:
(1) Weighing corresponding raw materials according to the following mass fractions for standby;
wherein the polyester polyol is polyester glycol with a hydroxyl value of 34-40mgKOH/g, an acid value of less than 0.30mgKOH/g, a water content of less than 0.03%, a molecular weight of 3000+500 and a chromaticity of less than 30; the epoxy resin is transparent semisolid, the epoxy equivalent weight is 454-555g/Eq, and the epoxy value is 0.18-0.22Eq/mg; the terminator is glycol; the catalyst is dibutyl tin dilaurate;
(2) Butanone, polyester polyol and epoxy resin are put into a reaction kettle, and mixed and dissolved to obtain a mixture A;
stirring is carried out during mixing and dissolving, and the stirring rotating speed is 400rpm; the temperature was 50℃and the dissolution time was 2h.
(3) Heating the reaction kettle to 80 ℃, adding HDI and a catalyst into the kettle, stirring the mixture with the mixture A at 60rpm, and stopping the reaction after detecting that the red light spectrum is not changed any more to obtain a mixture B;
(4) Adding a terminator into the mixture B, stirring and reacting for 10min, wherein the rotating speed is more than or equal to 60rpm; stopping heating, adding ethyl acetate, and stirring for reaction at the residual temperature to obtain a mixture C;
the rotational speed of the stirring at the residual temperature is 200rpm for 2 hours.
(5) Measuring the solid content and viscosity of the mixture C; and when the solid content and the viscosity are out of the required range of the product, adding ethyl acetate into the mixture C and uniformly mixing until the solid content and the viscosity of the mixture C meet the standards, thus obtaining the yellowing-resistant fly-weaving treatment agent.
In said step (5), the solid content of mixture C was 18% and the viscosity was 2231CPS/25 ℃.
Example IV
A preparation method of a yellowing-resistant fly-weaving treatment agent comprises the following steps:
(1) Weighing corresponding raw materials according to the following mass fractions for standby;
wherein the polyester polyol is polyester glycol with a hydroxyl value of 34-40mgKOH/g, an acid value of less than 0.30mgKOH/g, a water content of less than 0.03%, a molecular weight of 3000+500 and a chromaticity of less than 30; the epoxy resin is transparent semisolid, the epoxy equivalent weight is 454-555g/Eq, and the epoxy value is 0.18-0.22Eq/mg; the terminator is 1, 6-hexanediol; the catalyst is dibutyl tin dilaurate;
(2) Butanone, polyester polyol and epoxy resin are put into a reaction kettle, and mixed and dissolved to obtain a mixture A;
stirring is carried out during mixing and dissolving, and the stirring rotating speed is 400rpm; the temperature was 50℃and the dissolution time was 2h.
(3) Heating the reaction kettle to 80 ℃, adding HDI and a catalyst into the kettle, stirring the mixture with the mixture A at 60rpm, and stopping the reaction after detecting that the red light spectrum is not changed any more to obtain a mixture B;
(4) Adding a terminator into the mixture B, stirring and reacting for 10min, wherein the rotating speed is more than or equal to 60rpm; stopping heating, adding ethyl acetate, and stirring for reaction at the residual temperature to obtain a mixture C;
the rotational speed of the stirring at the residual temperature is 200rpm for 2 hours.
(5) Measuring the solid content and viscosity of the mixture C; and when the solid content and the viscosity are out of the required range of the product, adding ethyl acetate into the mixture C and uniformly mixing until the solid content and the viscosity of the mixture C meet the standards, thus obtaining the yellowing-resistant fly-weaving treatment agent.
In said step (5), the solid content of mixture C is 20% and the viscosity is 2400CPS/25 ℃.
Example five
A preparation method of a yellowing-resistant fly-weaving treatment agent comprises the following steps:
(1) Weighing corresponding raw materials according to the following mass fractions for standby;
wherein the polyester polyol is polyester glycol with a hydroxyl value of 34-40mgKOH/g, an acid value of less than 0.30mgKOH/g, a water content of less than 0.03%, a molecular weight of 3000+500 and a chromaticity of less than 30; the epoxy resin is transparent semisolid, the epoxy equivalent weight is 454-555g/Eq, and the epoxy value is 0.18-0.22Eq/mg; the terminator is 1, 3-butanediol; the catalyst is dibutyl tin dilaurate;
(2) Butanone, polyester polyol and epoxy resin are put into a reaction kettle, and mixed and dissolved to obtain a mixture A;
stirring is carried out during mixing and dissolving, and the stirring rotating speed is 400rpm; the temperature was 50℃and the dissolution time was 2h.
(3) Heating the reaction kettle to 80 ℃, adding HDI and a catalyst into the kettle, stirring the mixture with the mixture A at 60rpm, and stopping the reaction after detecting that the red light spectrum is not changed any more to obtain a mixture B;
(4) Adding a terminator into the mixture B, stirring and reacting for 10min, wherein the rotating speed is more than or equal to 60rpm; stopping heating, adding ethyl acetate, and stirring for reaction at the residual temperature to obtain a mixture C;
the rotational speed of the stirring at the residual temperature is 200rpm for 2 hours.
(5) Measuring the solid content and viscosity of the mixture C; and when the solid content and the viscosity are out of the required range of the product, adding ethyl acetate into the mixture C and uniformly mixing until the solid content and the viscosity of the mixture C meet the standards, thus obtaining the yellowing-resistant fly-weaving treatment agent.
In said step (5), the solid content of mixture C is 20% and the viscosity is 2400CPS/25 ℃.
The performance test was performed on the finished products of the foregoing examples one to five, the results of which are shown in the following table 1, wherein:
the initial tackiness, peel strength and shear strength were measured according to the description of GB-19340-2014 adhesive for shoes and bags.
The standard test piece for testing yellowing resistance according to the description of GB-19340-2014 adhesive for shoes and bags is placed in a yellowing resistance tester, the testing condition is 50 ℃ for 48 hours, the yellowing degree is observed, and the yellowing grade is from 1-4 to excellent.
TABLE 1
As can be seen from table 1, as the ratio of polyester polyol to epoxy resin increases, the better the resulting product treats the fly web, but the ratio is not entirely linearly related; the effect is optimal when the ratio is 2.5, and the effect starts to decrease when the ratio is 2.5.
The foregoing detailed description is directed to one of the possible embodiments of the present invention, which is not intended to limit the scope of the invention, but is to be accorded the full scope of all such equivalents and modifications so as not to depart from the scope of the invention.
Claims (6)
1. The yellowing-resistant fly-weaving treating agent is characterized by comprising the following components in parts by mass:
polyester polyol 10-20
5-10 parts of epoxy resin
HDI 0.9-1.2
Terminating agent 0.04-0.06
Catalyst 0.01-0.03
Butanone 30-40
30-40 parts of ethyl acetate;
the polyester polyol is polyester glycol with a hydroxyl value of 34-40mgKOH/g, an acid value of less than or equal to 0.30mgKOH/g, a water content of less than or equal to 0.03%, a molecular weight of 3000+/-500 and a chromaticity of less than or equal to 30;
the epoxy resin is transparent semisolid, the epoxy equivalent weight is 454-555g/Eq, and the epoxy value is 0.18-0.22Eq/mg;
the terminator is at least one of 1, 3-butanediol, 1, 4-butanediol, ethylene glycol and 1, 6-hexanediol;
the catalyst is at least one of dibutyl tin dilaurate and stannous octoate.
2. The method for preparing the yellowing-resistant fly-weaving treatment agent according to claim 1, which is characterized by comprising the following steps:
(1) Butanone, polyester polyol and epoxy resin are put into a reaction kettle, and mixed and dissolved to obtain a mixture A;
(2) Heating a reaction kettle, adding HDI and a catalyst into the kettle, stirring with the mixture A, and stopping the reaction after detecting that the red light spectrum is not changed any more to obtain a mixture B;
(3) Adding a terminator into the mixture B, stirring for reaction, stopping heating, adding ethyl acetate, and stirring for reaction at the residual temperature to obtain a mixture C;
(4) Measuring the solid content and viscosity of the mixture C; and when the solid content and the viscosity are out of the required range of the product, adding ethyl acetate into the mixture C and uniformly mixing until the solid content and the viscosity of the mixture C meet the standards, thus obtaining the yellowing-resistant fly-weaving treatment agent.
3. The method for producing a yellowing-resistant fly-weaving agent according to claim 2, wherein in the step (1), stirring is performed during mixing and dissolution, and the stirring rotation speed is not less than 400rpm; the temperature is more than or equal to 50 ℃, and the dissolution time is more than or equal to 2 hours.
4. The method for preparing the yellowing-resistant fly-weaving treatment agent according to claim 2, wherein in the step (2), the temperature of the reaction kettle is raised to be more than or equal to 80 ℃ and the stirring rotation speed is more than or equal to 60rpm.
5. The method for preparing the yellowing-resistant fly-weaving treatment agent according to claim 2, wherein in the step (3), the stirring time after adding the terminator is more than or equal to 10min, and the rotating speed is more than or equal to 60rpm; the rotation speed of the residual temperature stirring is more than or equal to 200rpm, and the time is more than or equal to 2 hours.
6. The process for producing a yellowing-resistant fly-weaving agent according to claim 2, wherein in the step (4), the solid content of the mixture C is 15 to 20% and the viscosity is 1800 to 2400CPS/25 ℃.
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