CN115679702A - Yellowing-resistant flying-weaving treating agent and preparation method thereof - Google Patents
Yellowing-resistant flying-weaving treating agent and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a yellowing-resistant flying-weaving treating agent and a preparation method thereof, and belongs to the technical field of treating agents for shoes. 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, terminating and adjusting the solid content. The yellowing-resistant fly-weaving treating agent prepared by the invention is particularly suitable for fly-weaving fabrics. The polymer obtained by blending and crosslinking of the invention has small molecular weight, is easy to diffuse to the surface of the flyaway fabric and permeate into the concave holes, and is easy to form a crosslinking structure with the surface of the flyaway fabric due to higher reaction activity, thereby improving the bonding force. The HDI of pure aliphatic is used as a reaction raw material, so that the condition that the aromatic isocyanate has a benzene ring structure and is subjected to cross-linking structure fracture in light, heat and oxygen environments to cause mechanical property reduction and degradation to generate a chromophoric group is avoided.
Description
Technical Field
The invention belongs to the technical field of shoe treating agents, and particularly relates to a yellowing-resistant fly-weaving treating agent and a preparation method thereof.
Background
The flyknitted fabric (Flyknit) is a novel lightweight technology, is mainly used for processing the vamp of the overall sneaker, and has the following advantages:
1) Has rich texture change. The fly-woven fabric is different from the traditional vamp material in that abundant texture effect design can be performed by means of the diversity of yarns and the change of the texture structure.
2) Has good elasticity and extensibility. The elongation percentage of the fly-woven material is greatly higher than that of the traditional leather material, the elasticity difference of all angles is not large, the upper surface formed by weaving can well wrap the foot, and the wearing comfort experience is improved. The properties and combination forms of the yarns, the shapes and sizes of the loops, the weave structures of the fabrics and the like are key factors influencing the elasticity and the ductility of the fly-knitted fabric.
3) The manufacturing of the fly-woven fabric with higher technological content is integrally formed after computer programming input and automatic machine weaving, so that the manufacturing process of the traditional shoes and boots is changed.
Although the fly-woven fabric is developed rapidly, the products and the technology of the related shoe treatment agent are quite deficient and basically in a blank state.
Disclosure of Invention
The invention provides a yellowing-resistant flying-weaving treating agent and a preparation method thereof, and fills the market blank in the aspect of flying-weaving treating agents.
The invention aims to provide a yellowing-resistant flying weaving treating agent which comprises the following components in parts by mass:
particularly, the polyester polyol is polyester diol with a hydroxyl value of 34-40mgKOH/g, an acid value of less than or equal to 0.30mgKOH/g, water content of less than or equal to 0.03%, a molecular weight of 3000 +/-500 and chroma of less than or equal to 30.
Specifically, the epoxy resin is a transparent semisolid, and has an epoxy equivalent of 454-555g/Eq and an epoxy value of 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 dibutyltin 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) Putting butanone, polyester polyol and epoxy resin into a reaction kettle, and mixing and dissolving to obtain a mixture A;
(2) Heating the reaction kettle, adding HDI and a catalyst into the kettle, stirring the HDI and the catalyst with the mixture A, detecting that the red light spectrum is not changed any more, and stopping the reaction 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 the viscosity of the mixture C; and when the solid content and the viscosity are out of the product requirement range, adding ethyl acetate into the mixture C and uniformly mixing until the solid content and the viscosity of the mixture C meet the standard, thus obtaining the yellowing-resistant flying-weaving treating agent.
Particularly, in the step (1), stirring is carried out when the mixture is dissolved, and the stirring speed is more than or equal to 400rpm; the temperature is more than or equal to 50 ℃, and the dissolving time is more than or equal to 2h.
Particularly, in the step (2), the temperature of the reaction kettle is increased to be more than or equal to 80 ℃, and the stirring 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 2h.
In particular, in the step (4), the mixture C has a solid content of 15-20% and a viscosity of 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 treating 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 flyaway fabric and permeate into the concave holes, and is easy to form a crosslinking structure with the surface of the flyaway fabric due to higher reaction activity, thereby improving the bonding force.
The HDI of pure aliphatic series is used as a reaction raw material, so that the condition that the aromatic isocyanate has a benzene ring structure and is subjected to cross-linking structure fracture in light, heat and oxygen environments to cause mechanical property reduction and degradation to generate chromophoric groups is avoided.
Detailed Description
For a better understanding of the present invention, the present invention is further described in conjunction with the following specific examples, wherein the terminology used in the examples is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
In the invention:
HDI refers to hexamethylene diisocyanate;
example one
A preparation method of a yellowing-resistant flying-weaving treating agent comprises the following steps:
(1) Weighing the corresponding raw materials according to the following mass parts for later use;
wherein the polyester polyol is polyester diol with hydroxyl value of 34-40mgKOH/g, acid value less than 0.30mgKOH/g, water less than 0.03%, molecular weight of 3000+500 and chroma less than 30; the epoxy resin is transparent semisolid, the epoxy equivalent is 454-555g/Eq, and the epoxy value is 0.18-0.22Eq/mg; the terminator is 1, 3-butanediol; the catalyst is dibutyltin dilaurate;
(2) Putting butanone, polyester polyol and epoxy resin into a reaction kettle, and mixing and dissolving to obtain a mixture A;
stirring is carried out when the materials are mixed and dissolved, and the stirring speed is 400rpm; the temperature is 50 ℃, and the dissolving time is 2h.
(3) Heating the reaction kettle to 80 ℃, adding HDI and a catalyst into the kettle, stirring the HDI and the catalyst with the mixture A at 60rpm, detecting that the red light spectrum is not changed any more, and stopping the reaction to obtain a mixture B;
(4) Adding a terminator into the mixture B, and stirring and reacting for 10min at the rotating speed of more than or equal to 60rpm; stopping heating, adding ethyl acetate, and stirring at the residual temperature to react to obtain a mixture C;
the rotation speed of the residual temperature stirring is 200rpm, and the time is 2h.
(5) Measuring the solid content and the viscosity of the mixture C; and when the solid content and the viscosity are out of the range required by 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 standard, thus obtaining the yellowing-resistant fly-weaving treating agent.
In said step (5), the mixture C has a solids content of 15% and a viscosity of 1812CPS/25 ℃.
Example two
A preparation method of a yellowing-resistant flying-weaving treating agent comprises the following steps:
(1) Weighing the corresponding raw materials according to the following mass parts for later use;
wherein the polyester polyol is polyester diol with hydroxyl value of 34-40mgKOH/g, acid value less than 0.30mgKOH/g, water less than 0.03%, molecular weight of 3000+500 and chroma less than 30; the epoxy resin is transparent semisolid, the epoxy equivalent is 454-555g/Eq, and the epoxy value is 0.18-0.22Eq/mg; the terminating agent is 1, 4-butanediol; the catalyst is stannous octoate;
(2) Putting butanone, polyester polyol and epoxy resin into a reaction kettle, and mixing and dissolving to obtain a mixture A;
stirring is carried out when the materials are mixed and dissolved, and the stirring speed is 400rpm; the temperature is 50 ℃, and the dissolving time is 2h.
(3) Heating the reaction kettle to 80 ℃, adding HDI and a catalyst into the kettle, stirring the HDI and the catalyst with the mixture A at 60rpm, detecting that the red light spectrum is not changed any more, and stopping the reaction to obtain a mixture B;
(4) Adding a terminator into the mixture B, and stirring and reacting for 10min at the rotating speed of more than or equal to 60rpm; stopping heating, adding ethyl acetate, and stirring at the residual temperature to react to obtain a mixture C;
the rotation speed of the residual temperature stirring is 200rpm, and the time is 2h.
(5) Measuring the solid content and the viscosity of the mixture C; and when the solid content and the viscosity are out of the range required by 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 standard, thus obtaining the yellowing-resistant fly-weaving treating agent.
In the step (5), the mixture C has a solid content of 20% and a viscosity of 2400CPS/25 ℃.
EXAMPLE III
A preparation method of a yellowing-resistant flying-weaving treating agent comprises the following steps:
(1) Weighing corresponding raw materials according to the following mass parts for later use;
wherein the polyester polyol is polyester diol with a hydroxyl value of 34-40mgKOH/g, an acid value of less than 0.30mgKOH/g, water content of less than 0.03%, a molecular weight of 3000+500 and chroma of less than 30; the epoxy resin is transparent semisolid, the epoxy equivalent is 454-555g/Eq, and the epoxy value is 0.18-0.22Eq/mg; the terminating agent is ethylene glycol; the catalyst is dibutyltin dilaurate;
(2) Putting butanone, polyester polyol and epoxy resin into a reaction kettle, and mixing and dissolving to obtain a mixture A;
stirring is carried out when the materials are mixed and dissolved, and the stirring speed is 400rpm; the temperature is 50 ℃, and the dissolving time is 2h.
(3) Heating the reaction kettle to 80 ℃, adding HDI and a catalyst into the kettle, stirring the HDI and the catalyst with the mixture A at 60rpm, detecting that the red light spectrum is not changed any more, and stopping the reaction to obtain a mixture B;
(4) Adding a terminator into the mixture B, and stirring and reacting for 10min at the rotating speed of more than or equal to 60rpm; stopping heating, adding ethyl acetate, and stirring at the residual temperature to react to obtain a mixture C;
the rotation speed of the residual temperature stirring is 200rpm, and the time is 2h.
(5) Measuring the solid content and the viscosity of the mixture C; and when the solid content and the viscosity are out of the product requirement range, adding ethyl acetate into the mixture C and uniformly mixing until the solid content and the viscosity of the mixture C meet the standard, thus obtaining the yellowing-resistant flying-weaving treating agent.
In the step (5), the mixture C has a solids content of 18% and a viscosity of 2231CPS/25 ℃.
Example four
A preparation method of a yellowing-resistant flying-weaving treating agent comprises the following steps:
(1) Weighing the corresponding raw materials according to the following mass parts for later use;
wherein the polyester polyol is polyester diol with a hydroxyl value of 34-40mgKOH/g, an acid value of less than 0.30mgKOH/g, water content of less than 0.03%, a molecular weight of 3000+500 and chroma of less than 30; the epoxy resin is transparent semisolid, the epoxy equivalent is 454-555g/Eq, and the epoxy value is 0.18-0.22Eq/mg; the terminating agent is 1, 6-hexanediol; the catalyst is dibutyltin dilaurate;
(2) Putting butanone, polyester polyol and epoxy resin into a reaction kettle, and mixing and dissolving to obtain a mixture A;
stirring is carried out when the materials are mixed and dissolved, and the stirring speed is 400rpm; the temperature is 50 ℃, and the dissolving time is 2h.
(3) Heating the reaction kettle to 80 ℃, adding HDI and a catalyst into the kettle, stirring the HDI and the catalyst with the mixture A at 60rpm, detecting that the red light spectrum is not changed any more, and stopping the reaction to obtain a mixture B;
(4) Adding a terminator into the mixture B, and stirring and reacting for 10min at the rotating speed of more than or equal to 60rpm; stopping heating, adding ethyl acetate, and stirring at the residual temperature to react to obtain a mixture C;
the rotation speed of the residual temperature stirring is 200rpm, and the time is 2h.
(5) Measuring the solid content and the viscosity of the mixture C; and when the solid content and the viscosity are out of the product requirement range, adding ethyl acetate into the mixture C and uniformly mixing until the solid content and the viscosity of the mixture C meet the standard, thus obtaining the yellowing-resistant flying-weaving treating agent.
In said step (5), the mixture C has a solids content of 20% and a viscosity of 2400CPS/25 ℃.
EXAMPLE five
A preparation method of a yellowing-resistant flying-weaving treating agent comprises the following steps:
(1) Weighing corresponding raw materials according to the following mass parts for later use;
wherein the polyester polyol is polyester diol with hydroxyl value of 34-40mgKOH/g, acid value less than 0.30mgKOH/g, water less than 0.03%, molecular weight of 3000+500 and chroma less than 30; the epoxy resin is transparent semisolid, the epoxy equivalent is 454-555g/Eq, and the epoxy value is 0.18-0.22Eq/mg; the terminator is 1, 3-butanediol; the catalyst is dibutyltin dilaurate;
(2) Putting butanone, polyester polyol and epoxy resin into a reaction kettle, and mixing and dissolving to obtain a mixture A;
stirring is carried out when the materials are mixed and dissolved, and the stirring speed is 400rpm; the temperature is 50 ℃, and the dissolving time is 2h.
(3) Heating the reaction kettle to 80 ℃, adding HDI and a catalyst into the kettle, stirring the HDI and the catalyst with the mixture A at 60rpm, detecting that the red light spectrum is not changed any more, and stopping the reaction 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 at the residual temperature to react to obtain a mixture C;
the rotation speed of the residual temperature stirring is 200rpm, and the time is 2h.
(5) Measuring the solid content and the viscosity of the mixture C; and when the solid content and the viscosity are out of the product requirement range, adding ethyl acetate into the mixture C and uniformly mixing until the solid content and the viscosity of the mixture C meet the standard, thus obtaining the yellowing-resistant flying-weaving treating agent.
In the step (5), the mixture C has a solid content of 20% and a viscosity of 2400CPS/25 ℃.
The performance tests performed on the finished products of the previous examples one to five are shown in table 1 below, wherein:
initial tack, peel strength, and shear strength were tested according to the records of GB-19340-2014 adhesive for shoes and bags.
The standard test piece is placed in a yellowing resistance tester under the test condition of 50 ℃ for 48 hours, the yellowing degree is observed, and the yellowing grade is represented by 1-4 from poor to excellent.
TABLE 1
As can be seen from table 1, as the ratio of polyester polyol to epoxy resin increases, the obtained product has better treatment effect on the woven fabric, but the ratio is not completely linearly related; the effect is best when the ratio is 2.5 and starts to diminish when the ratio is 2.5.
The above detailed description is specific to one possible embodiment of the present invention, and the embodiment is not intended to limit the scope of the present invention, and all equivalent implementations or modifications without departing from the scope of the present invention should be included in the technical scope of the present invention.
Claims (10)
1. The yellowing-resistant flying weaving treating agent is characterized by comprising the following components in parts by mass:
2. the yellowing-resistant fly-weaving finishing agent as claimed in claim 1, wherein the polyester polyol is polyester diol having a hydroxyl value of 34 to 40mgKOH/g, an acid value of 0.30mgKOH/g or less, a water content of 0.03% or less, a molecular weight of 3000 ± 500, and a color of 30 or less.
3. The yellowing-resistant fly-weaving treatment agent according to claim 1, wherein the epoxy resin is a transparent semisolid having an epoxy equivalent of 454 to 555g/Eq and an epoxy value of 0.18 to 0.22Eq/mg.
4. The yellowing-resistant fly-weaving agent according to claim 1, wherein the terminator is at least one of 1, 3-butanediol, 1, 4-butanediol, ethylene glycol, and 1, 6-hexanediol.
5. The yellowing-resistant texturing agent according to claim 1, wherein the catalyst is at least one of dibutyltin dilaurate and stannous octoate.
6. A process for preparing a yellowing-resistant fly-weaving treatment agent according to any one of claims 1 to 5, comprising the steps of:
(1) Putting butanone, polyester polyol and epoxy resin into a reaction kettle, and mixing and dissolving to obtain a mixture A;
(2) Heating the reaction kettle, adding HDI and a catalyst into the kettle, stirring the HDI and the catalyst with the mixture A, detecting that the red light spectrum is not changed any more, and stopping the reaction 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 the viscosity of the mixture C; and when the solid content and the viscosity are out of the range required by 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 standard, thus obtaining the yellowing-resistant fly-weaving treating agent.
7. The method for preparing the yellowing-resistant flying fabric treating agent according to claim 6, wherein in the step (1), stirring is performed when the components are mixed and dissolved, and the stirring speed is not less than 400rpm; the temperature is more than or equal to 50 ℃, and the dissolving time is more than or equal to 2h.
8. The preparation method of the yellowing-resistant flying fabric treating agent according to claim 6, wherein in the step (2), the temperature of the reaction kettle is raised to be more than or equal to 80 ℃, and the stirring speed is more than or equal to 60rpm.
9. The preparation method of the yellowing-resistant flying fabric treating agent according to claim 6, wherein in the step (3), the stirring time is not less than 10min after the terminator is added, and the rotating speed is not less than 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 2h.
10. The method for preparing the yellowing-resistant flying weaving treating agent according to claim 6, wherein in the step (4), the solid content of the mixture C is 15-20%, and the viscosity is 1800-2400CPS/25 ℃.
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