Preparation method and application process of environment-friendly stiffening agent

By preparing an environmentally friendly stiffening agent containing a polyester resin skeleton and hydrophilic groups, the problems of formaldehyde release, yellowing, and white marks in stiffening agents for polyester were solved, achieving high adhesion and water dispersibility, and improving the stiffening effect and storage convenience of the fabric.

CN121064381APending Publication Date: 2025-12-05DUPLUS CHEM OF ZHANGJIAGANG CITY
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Patent Information

Application Number
CN202511343467.0
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-09-19
Publication Date
2025-12-05

AI Technical Summary

Technical Problem

Existing stiffening agents for polyester have problems such as formaldehyde release, odor, yellowing, white marks, and softening, and the stiffening effect on the treated fabric is not good.

Method used

An environmentally friendly stiffening agent is prepared by linking polycarboxylic acids and polyols with ester groups to form a polyester resin skeleton and adding hydrophilic groups. The preparation process includes pre-emulsion formation, mixed liquid drop reaction and pH adjustment. The application process includes padding, pre-drying and baking steps.

Benefits of technology

It achieves high adhesion performance, no formaldehyde release, good water dispersibility and simple finishing process, solves the defects of traditional stiffening agents, and improves the stiffness and storage convenience of fabrics.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention discloses a preparation method and an application process of an environment-friendly stiffening agent, the molecular chain of the environment-friendly stiffening agent is as follows: (X-O) r-W-(O-(CO-Z-CO-O-Y-O) p-X) q, W is a (q + r)-valent organic group, (CO-Z-CO-O-Y-O) is a polyester resin skeleton taking a polycarboxylic acid component Z and a polyol component Y as polymerization components, and the formula is shown in the description. And X represents a residue of a polyacid having two or more carboxyl groups or hydrogen. The environment-friendly stiffening agent has the beneficial effects that the environment-friendly stiffening agent in the technical scheme has relatively high adhesion to polyester, can be co-melted with the polyester under the action of heat, is free of formaldehyde release, and has a strong hydrophilic group sulfonic acid group, so that the environment-friendly stiffening agent in the technical scheme has good water dispersibility, is convenient to store and simple in finishing process, and is suitable for industrial production. The problems of formaldehyde, yellowing, white marks, odor and softening of a traditional stiffening agent are effectively solved.
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Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of stiffening agent preparation, in particular to a preparation method and application process of an environment-friendly stiffening agent. BACKGROUND

[0002] Hard finishing is a finishing method that high molecular substances are made into finishing liquid and then impregnated onto fabrics, and a film is formed on the surface of the fabrics after heat treatment, thereby giving the fabrics a stiff, thick and full hand feeling. It is widely used in the processing of textile products such as lining cloth and bag cloth. At present, the stiffening finishing agents for polyester on the market mainly include melamine resin and polyacrylate resin. The former has high stiffening degree and low cost, but has problems such as formaldehyde release and odor. The latter has no formaldehyde release problem and has advantages such as non-yellowing at high temperature, but the stiffening effect of the fabric after finishing is not as good as that of melamine resin, and it also lacks elasticity and thickness, and has the defects of cold brittleness and easy softening. SUMMARY

[0003] The purpose of the present application is to solve the above problems, and a preparation method and application process of an environment-friendly stiffening agent are designed.

[0004] To achieve the above purpose, the technical scheme of the present application is an environment-friendly stiffening agent, and the molecular chain of the environment-friendly stiffening agent is as follows: (X-O) r -W-(O-(CO-Z-CO-O-Y-O) p -X) q wherein W is an organic group with (q+r) valence, (CO-Z-CO-O-Y-O) is a polyester resin skeleton with polybasic acid component Z and polyol component Y as polymerization components, and X is a residue of a polybasic acid with two or more carboxyl groups or hydrogen.

[0005] As a further description of the technical scheme, in the molecular chain of the environment-friendly stiffening agent, the average value of p is 3 or more, the average value of q is 0-15, the average value of r is 0-15, and the value of (q+r) is 3-15.

[0006] As a further description of the technical scheme, in the polyester resin skeleton, the carboxyl groups (-COOH) of the polybasic acid and the hydroxyl groups (-OH) of the polyol are dehydrated and condensed, connected by ester groups (-COO-), forming a long chain with alternating repeating units, and the long chain contains benzene rings.

[0007] As a further description of the technical scheme, the long chain contains a hydrophilic group, which is one or more of sulfonate, carboxylate and hydroxylate.

[0008] As a further description of the technical scheme, the raw materials of the environment-friendly stiffening agent are as follows: vinyl acetate, acrylate monomer, functional monomer, emulsifier, initiator and deionized water.

[0009] As a further description of the technical solution, the acrylate monomer is n-butyl acrylate, the functional monomer is hydroxyethyl acrylate, the emulsifier is glycerol polyoxyethylene ether, and the initiator is potassium persulfate.

[0010] A preparation method of an environment-friendly stiffening agent, comprising the following steps: Step one: mix and stir the acrylate monomer and glycerol polyoxyethylene ether to form a pre-emulsion A; Step two: prepare a mixed solution B by mixing potassium sulfate and an additive; Step three: add the mixed solution A and the mixed solution B step by step and react under heating to obtain a polymer emulsion finally; Step four: after adjusting the pH, add a water-soluble resin or a starch paste solution, cool and discharge to complete the preparation of the stiffening agent.

[0011] An application process of an environment-friendly stiffening agent, comprising the following steps: Step A: prepare the prepared stiffening agent; Step B: padding operation; Step C: pre-drying operation; Step D: baking the fabric.

[0012] As a further description of the technical solution, in step B, the padding operation adopts double padding and double rolling, and the rolling rate is 120%; In step C, the pre-drying temperature is 100 DEG C, and the pre-drying time is 5 min; In step D, the baking temperature is 120 DEG C, and the baking time is 40 s.

[0013] The environment-friendly stiffening agent has high adhesion to polyester, can be co-melted with polyester under the action of heat, does not release formaldehyde, has a strong hydrophilic group of sulfonic acid group, has good water dispersibility, is convenient to store, has a simple finishing process, and effectively solves the problems of formaldehyde, yellowing, white marks, odor and softening of traditional stiffening agents. DETAILED DESCRIPTION

[0014] At present, the stiffening finishing agents for polyester on the market mainly include melamine resin and polyacrylate resin. The former has high stiffening degree and low cost, but has problems of formaldehyde release and odor; the latter has no formaldehyde release problem and has advantages of no yellowing at high temperature, but the stiffening effect of the fabric after finishing is not as good as that of melamine resin, and the fabric also lacks elasticity and thickness, and has defects of cold brittleness and easy softening.

[0015] The present application aims to provide an environmentally-friendly stiffening agent with simple preparation process and excellent effect, which has high adhesion and can be co-melted with polyester under the action of heat without releasing formaldehyde. The present application will be described in detail below, and the environmentally-friendly stiffening agent has the following molecular chain: (X-O) r -W-(O-(CO-Z-CO-O-Y-O) p -X) q wherein W is an organic group with (q+r) valence, (CO-Z-CO-O-Y-O) is a polyester resin skeleton with polybasic acid component Z and polyhydric alcohol component Y as polymerization components, and X is a residue of polybasic acid with two or more carboxyl groups or hydrogen.

[0016] In the polyester resin skeleton, the carboxyl groups (-COOH) of the polybasic acid and the hydroxyl groups (-OH) of the polyhydric alcohol are dehydrated and condensed to form a long chain with alternating repeating units through ester groups (-COO-), and the long chain contains benzene rings; the long chain contains a hydrophilic group, which is one or more of sulfonate, carboxylate and hydroxylate.

[0017] In the molecular chain of the environmentally-friendly stiffening agent, the average value of p is 3 or more, the average value of q is 0-15, the average value of r is 0-15, and the value of (q+r) is 3-15.

[0018] The raw materials of the environmentally-friendly stiffening agent will be described in detail below, which are as follows: vinyl acetate, acrylic ester monomer, functional monomer, emulsifier, initiator and deionized water.

[0019] The acrylic ester monomer is n-butyl acrylate, the functional monomer is hydroxyethyl acrylate, the emulsifier is glycerol polyoxyethylene ether, and the initiator is potassium persulfate.

[0020] The preparation method of the environmentally-friendly stiffening agent will be described in detail below, which includes the following steps: Step one: mix and stir the acrylic ester monomer and glycerol polyoxyethylene ether to form pre-emulsion A; Step two: mix potassium sulfate and additives to form mixed solution B; Step three: add mixed solution A and mixed solution B drop by drop and react under heating to obtain a polymer emulsion; Step four: after adjusting the pH, add water-soluble resin or starch paste solution, cool and discharge to complete the preparation of the stiffening agent.

[0021] The application process of the environmentally-friendly stiffening agent will be described in detail below, which includes the following steps: Step A: preparing the stiffening agent; Step B: padding operation; in the step B, the padding operation adopts two dip-two pad, and the pick-up rate is 120%; Step C: pre-drying operation; in the step C, the pre-drying temperature is 100℃, and the pre-drying time is 5min; Step D: baking the fabric, in the step D, the baking temperature is 120℃, and the baking time is 40s.

[0022] The following will be described in detail in combination with examples and comparative examples: Example One: Finishing process: Stiffening agent 5%, → padding (two dip-two pad, pick-up rate 120%) → pre-drying (100℃×5min) → baking (120℃×40s) Fabric: pure polyester fabric 21T×16T 200g / m 2 Example Two: Finishing process: Stiffening agent 6%, → padding (two dip-two pad, pick-up rate 120%) → pre-drying (100℃×5min) → baking (130℃×50s) Fabric: pure polyester fabric 21T×16T 200g / m 2 Example Three Finishing process: Stiffening agent 8%, → padding (two dip-two pad, pick-up rate 120%) → pre-drying (100℃×5min) → baking (140℃, 60s) Fabric: pure polyester fabric 21T×16T 200g / m 2 The results of the bending stiffness test, whiteness test, moisture absorption rate test, and white mark of the unfinishing, example one, example two, and example three are shown in Table 1: Table 1 Bending stiffness test method: the fabric stiffness is measured according to the standard GB / T 18318-2001 "Textiles-Determination of fabric bending length", and the stiffness of the fabric is expressed by the bending stiffness (mN·cm).

[0023] Whiteness test method: the whiteness of the fabric is tested according to the standard GB / T 8424.2-2001 "Textiles Color Fastness Test Instrumental Assessment Method for Relative Whiteness", and each sample is tested at least 3 times at different positions, and the average value is taken.

[0024] Moisture absorption rate test method: the weight of the finished cloth sample is recorded as W0, and the weight of the cloth sample is recorded as W1 after being smoothed for 72h in an environment with a temperature of 25℃ and a humidity of RH60%, and the moisture absorption rate is The test method of white mark: based on the use of rubbing fastness instrument, the instrument is designed and modified to simulate the fine mark produced by nail scratch, and has quantitative and directional scratching force. Take several pieces of two kinds of fabrics with the same size and clean surface without damage. Use clamping device to fix the fabric flat on the test instrument platform, so that the sample length direction is consistent with the movement direction of the rubbing head. Place a piece of sandpaper between the test instrument platform and the sample to help reduce the movement of the sample during rubbing. The running speed is one reciprocating rubbing cycle per second, a total of 10 rubbing cycles, and the K / S change before and after rubbing is tested on the Xrite-7800 computer color matching instrument.

[0025] The test method of odor: put the finished fabric into a sealed bag and place it in 60℃ for 1h.

[0026] Comparative Example 1: using melamine resin type finishing.

[0027] Comparative Example 2: using polyacrylate finishing.

[0028] The results of the bending stiffness test, whiteness test, moisture absorption rate test, and white mark test of the comparative examples are shown in Table 2. Table 2 According to the results of the examples and comparative examples, it can be seen that the stiffening agent of the present application can change the problems of yellowing, white mark, moisture absorption and softening, and odor of traditional stiffening agents.

[0029] The environment-friendly stiffening agent of the technical solution has high adhesion to polyester, can co-melt with polyester under the action of heat, and does not release formaldehyde. In addition, the environment-friendly stiffening agent of the technical solution has a strong hydrophilic group, i.e. sulfonic acid group, and therefore has good water dispersibility, convenient storage, simple finishing process, and effectively solves the problems of formaldehyde, yellowing, white mark, odor, and softening of traditional stiffening agents.

[0030] The above technical solution only embodies the preferred technical solution of the present application, and some changes made by those skilled in the art to some parts thereof also embody the principle of the present application and are within the protection scope of the present application.

Claims

1. An environmentally friendly stiffening agent, characterized in that, The molecular chain of the environmentally friendly stiffening agent is as follows: (XO) r -W-(O-(CO-Z-CO-OYO) p -X) q , where W is an organic group with a (q+r) valence, (CO-Z-CO-OYO) is a polyester resin skeleton with polycarboxylic acid component Z and polyol component Y as polymer components, and X is a residue of a polyacid with more than 2 carboxyl groups or hydrogen.

2. The environmentally friendly stiffening agent according to claim 1, characterized in that, In the molecular chain of the environmentally friendly stiffening agent, the average value of p is 3 or more, the average value of q is 0-15, the average value of r is 0-15, and the value of (q+r) is 3-15.

3. The environmentally friendly stiffening agent according to claim 1, characterized in that, In the polyester resin skeleton, the carboxyl group (-COOH) of the polycarboxylic acid and the hydroxyl group (-OH) of the polyol undergo dehydration condensation and are connected by ester groups (-COO-) to form a long chain of alternating repeating units, which contains benzene rings.

4. The environmentally friendly stiffening agent according to claim 3, characterized in that, The long chain contains hydrophilic groups, which are one or more of sulfonates, carboxylates, and hydroxyl salts.

5. The environmentally friendly stiffening agent according to claim 1, characterized in that, The raw materials of the environmentally friendly stiffening agent are as follows: vinyl acetate, acrylate monomers, functional monomers, emulsifiers, initiators, and deionized water.

6. The environmentally friendly stiffening agent according to claim 5, characterized in that, The acrylate monomer is n-butyl acrylate, the functional monomer is hydroxyethyl acrylate, the emulsifier is glycerol polyoxyethylene ether, and the initiator is potassium persulfate.

7. A method for preparing an environmentally friendly stiffening agent as described in any one of claims 1-6, characterized in that, Includes the following steps: Step 1: Mix acrylate monomers with glycerol polyoxyethylene ether to form preemulsion A; Step 2: Prepare a mixture B by mixing potassium sulfate and the auxiliary agent; Step 3: Add mixture A and mixture B dropwise in stages and heat to react, finally obtaining a polymer emulsion; Step 4: After adjusting the pH, add water-soluble resin or starch gelatinization solution, cool and discharge to complete the preparation of the stiffening agent.

8. An application process for an environmentally friendly stiffening agent as described in any one of claims 1-4, characterized in that, Includes the following steps: Step A: Prepare the stiffening agent; Step B: Rolling operation; Step C: Pre-baking operation; Step D: Baking the fabric.

9. The application process of an environmentally friendly stiffening agent according to claim 8, characterized in that, In step B, the immersion rolling operation adopts a two-dip, two-roll process with a roll residue of 120%. In step C, the pre-drying temperature is 100℃ and the pre-drying time is 5 minutes; In step D, the baking temperature is 120℃ and the baking time is 40s.