Fabric flame retardant and preparation method thereof

By using fabric flame retardant prepared by specific comonomers, the problem of hard feel and formaldehyde exceeding the standard in the prior art is solved, and soft feel, good flame retardant effect and environmentally friendly storage stability are achieved.

CN119593210APending Publication Date: 2025-03-11SHANGHAI YAYUN TECHNOLOGY CO LTD

Patent Information

Application Number
CN202411846200.9
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-12-16
Publication Date
2025-03-11

AI Technical Summary

Technical Problem

After finishing, existing fabric flame retardants cause the fabric to feel hard when they are finished, and there are problems such as excessive formaldehyde, high phosphorus content and hydrogen chloride gas, which affects the environment and human health.

Method used

Using alkenyl aminotriazine, polyalkenyl siloxane, alkenylsulfonyl propylene diacetamide and allyl polyoxyethylene ether comonomer, a phosphorus-free, halogen-free, formaldehyde-free flame retardant is prepared through polymerization to enhance the feel of the fabric and achieve synergistic flame retardant.

Benefits of technology

The finished fabric feels soft and smooth, the flame retardant effect reaches level B1, the storage stability is good, there is no precipitation or stickiness, and the color is uniform, safe and environmentally friendly.

✦ Generated by Eureka AI based on patent content.

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Patent Text Reader

Abstract

The invention relates to a fabric flame retardant and a preparation method thereof. The fabric flame retardant is obtained by polymerizing a monomer composition, and the total weight of the monomer composition is 100%. Comprising the following components in percentage by weight: 15 to 30 percent of alkenyl amino triazine comonomer, 5 to 20 percent of polyalkenyl siloxane comonomer, 5 to 15 percent of alkenyl sulfonyl propylidene diacetamide comonomer, 2 to 10 percent of allyl polyoxyethylene ether comonomer and 40 to 65 percent of deionized water. The flame-retardant effect of the fabric finished by the flame retardant can reach B1 level, the fabric is soft and smooth in hand feeling, the fabric surface is not separated out and is not sticky in the storage process, and the color yield is uniform. And the flame retardant is phosphorus-free, halogen-free, formaldehyde-free, safe and environment-friendly.
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Description

Technical Field

[0001] The invention relates to the field of textile auxiliaries, in particular to the field of fabric flame retardants, and particularly to a fabric flame retardant with good hand feel and a preparation method thereof. Background Art

[0002] Textiles are widely used in various fields such as clothing, medical care, chemicals, construction, aerospace, etc., and people's demand for textiles is increasing day by day. However, textiles are mostly flammable or combustible materials, which pose a great fire hazard. The application of flame-retardant textiles can greatly reduce fire accidents caused by textiles. At present, there are generally two processing methods for producing flame-retardant textiles on the market. One is to mix flame retardants into spinning solution to directly prepare flame-retardant fibers. This processing method is only applicable to synthetic fiber textiles; the other is flame-retardant finishing method, which uses flame retardants to flame-retardant finish fabrics. This processing method is applicable to both natural fiber textiles such as cotton fibers and synthetic fiber textiles. The flame-retardant finishing method has a wider range of applications and is more flexible, and the finishing process is simple and efficient, but there are also problems such as poor compatibility between fabrics and flame retardants, which leads to hardness of the fabric after finishing and precipitation of flame retardants during storage.

[0003] Currently, the most commonly used flame retardant finishing method with little effect on the feel of fabrics is the Proban method, which was created by Aubrey-Wilson Ltd. in the UK. Fabrics finished with this method have good flame retardant effect, and the feel and strength of the treated fabrics remain excellent. However, the formaldehyde content on cotton textiles after finishing seriously exceeds the standard, which seriously endangers the environment and human health.

[0004] In order to solve this type of formaldehyde problem, researchers in this field have also conducted corresponding research. For example, the Chinese patent application number 200810123174.1, "A flame retardant for cellulose fiber fabrics and its synthesis method", synthesized a flame retardant containing three elements: phosphorus, nitrogen, and silicon. The flame retardant can improve the feel of cellulose fiber fabrics, and there is no free formaldehyde on the surface of the fabric after finishing. However, the preparation process of the flame retardant is relatively cumbersome, and the preparation process is accompanied by the generation of harmful hydrogen chloride gas. In addition, the flame retardant contains phosphorus, which has potential hazards to human health and the environment.

[0005] Therefore, it is of great practical significance to develop an environmentally friendly flame retardant that is phosphorus-free, halogen-free, and formaldehyde-free and can improve the feel of fabrics after finishing. Summary of the invention

[0006] In order to solve the existing problems, the present invention provides a flame retardant that can improve the feel of fabrics after finishing. The flame retardant uses alkenylaminotriazine comonomer as the main flame retardant monomer to provide nitrogen flame retardant elements; uses polyalkenylsiloxane comonomer to improve the feel, and the silicon element has a synergistic flame retardant effect; uses alkenylsulfonylpropylenediethylamide comonomer to provide sulfur and nitrogen elements to achieve synergistic flame retardancy; uses allyl polyoxyethylene ether comonomer to improve the hydrophilicity of the flame retardant, and the allyl polyoxyethylene ether comonomer itself has good emulsification, and the reaction system does not need to add an additional emulsifier. The flame retardant effect of the fabric finished with the flame retardant of the present invention can reach B1 level according to the standard "GB / T 17591-2006 Flame Retardant Fabrics". The finished fabric has a soft and smooth feel, good storage stability, no precipitation on the fabric surface during storage, no stickiness, and uniform color. In addition, the flame retardant is phosphorus-free, halogen-free, formaldehyde-free, safe and environmentally friendly.

[0007] One aspect of the present invention is to provide a flame retardant obtained by polymerizing a monomer composition, wherein the monomer composition, based on a total weight of 100%, comprises the following components:

[0008]

[0009] Another aspect of the present invention is to provide a method for preparing the above-mentioned fabric flame retardant, which comprises the following steps:

[0010] 1) Adding comonomer and deionized water into a reactor and mixing them evenly, heating to 50-60° C. and shearing for 30-60 minutes to obtain a pre-emulsion;

[0011] 2) Take 1 / 3 of the pre-emulsion in step 1), add 1 / 3 of the initiator solution, heat to 78-85°C to initiate emulsion polymerization, keep warm for 10-30 minutes, then simultaneously drop the remaining pre-emulsion and initiator solution, and keep warm for 3-5 hours;

[0012] 3) Cooling the material in step 2) to room temperature and discharging the material to obtain a fabric flame retardant. DETAILED DESCRIPTION

[0013] In one embodiment of the present invention, a fabric flame retardant is provided, which is obtained by polymerizing a monomer composition, wherein the monomer composition, based on a total weight of 100%, comprises the following components:

[0014]

[0015] In a preferred embodiment, a fabric flame retardant is provided, which is obtained by polymerizing a monomer composition, wherein the monomer composition, based on a total weight of 100%, comprises the following components:

[0016]

[0017] In a preferred embodiment, the alkenylaminotriazine comonomer is one of 2-vinyl-4,6-diamino-1,3,5-triazine and 2,4-diallyloxy-6-amino-1,3,5-triazine.

[0018] In a preferred embodiment, the polyalkenylsiloxane comonomer is one of tetrakis(dimethylvinylsiloxy)silane and 2,4,6-trivinyl-2,4,6-trimethylcyclotrisiloxane.

[0019] In a preferred embodiment, the alkenylsulfonylpropylene diacetamide comonomer is N,N'-1,3-propylene di[2-(vinylsulfonyl)]acetamide.

[0020] In a preferred embodiment, the number average molecular weight of the allyl polyoxyethylene ether comonomer is 2000-3000.

[0021] In a preferred embodiment, a method for preparing a fabric flame retardant is provided, characterized in that:

[0022] 1) Adding comonomer and deionized water into a reactor and mixing them evenly, heating to 50-60° C. and shearing for 30-60 minutes to obtain a pre-emulsion;

[0023] 2) Take 1 / 3 of the pre-emulsion in step 1), add 1 / 3 of the initiator solution, heat to 78-85°C to initiate emulsion polymerization, keep warm for 10-30 minutes, then simultaneously drop the remaining pre-emulsion and initiator solution, and keep warm for 3-5 hours;

[0024] 3) Cooling the material in step 2) to room temperature and discharging the material to obtain a fabric flame retardant.

[0025] In a preferred embodiment, the initiator is ammonium persulfate or potassium persulfate.

[0026] Example

[0027] The present invention will be further described below in conjunction with specific embodiments. It should be understood that these embodiments are only used to illustrate the present invention and are not intended to limit the scope of the present invention. In addition, it should be understood that after reading the content taught by the present invention, those skilled in the art can make various changes or modifications to the present invention, and these equivalent forms fall within the scope limited by the appended claims of the application equally.

[0028] In each embodiment, all raw materials and fabrics are commercially available. Among them, 2-vinyl-4,6-diamino-1,3,5-triazine was purchased from Shanghai Yuanye Biotechnology Co., Ltd., 2,4-diallyloxy-6-amino-1,3,5-triazine was purchased from Shanghai Mairui Biochemical Technology Co., Ltd., tetrakis(dimethylvinylsiloxy)silane and 2,4,6-trivinyl-2,4,6-trimethylcyclotrisiloxane were purchased from the official website of MacLean Reagent, and N,N'-1,3-propylenebis[2-(vinylsulfonyl)]acetamide was purchased from Shanghai Xingui Biotechnology Co., Ltd.

[0029] The commercially available flame retardant sample used in the experiment was an N-series phosphorus-free flame retardant produced by a Zhejiang company.

[0030] In the experiment, a conventional high-speed shear mixer used in the laboratory in the art was used to prepare the emulsion by shearing.

[0031] The performance measurement and application effect in each embodiment are measured and evaluated according to the following methods:

[0032] 1. Application technology of textiles:

[0033] Sample: cotton poplin, polyester knitted fabric (commercially available)

[0034] Formula: Flame retardant 350g / L

[0035] Flame retardant finishing process: Padding (padding rate 75-90%) → drying (180℃×120s)

[0036] 2. Fabric performance determination:

[0037] Fabric combustion performance test: Determined in accordance with GB / T5455-1997 Textile combustion performance test vertical combustion method;

[0038] Flame retardant fabric performance evaluation: refer to GB / T 17591-2006 Flame Retardant Fabric standard, B1 flame retardant standard is: afterburning time ≤ 5s, smoldering time ≤ 5s, damaged length ≤ 150mm;

[0039] Hand feel evaluation: The hand feel of the original fabric is scored as 1 point, and the hand feel evaluation results of 5 people are combined (1-5 points, 1 point is the worst, 5 points is the best);

[0040] Storage stability: After the finished fabric is stored at room temperature for 6 months, check whether there is precipitation or stickiness on the fabric surface, and whether the color of the fabric surface is uniform.

[0041] Example 1

[0042] In a four-necked flask equipped with a stirrer and a thermometer, 24 g of 2-vinyl-4,6-diamino-1,3,5-triazine, 12 g of tetrakis(dimethylvinylsiloxy)silane, 6 g of N,N'-1,3-propylenebis[2-(vinylsulfonyl)]acetamide, 7.5 g of allyl polyoxyethylene ether (APEG2400) and 60 g of deionized water were added. The temperature was raised to 55°C and high-speed shearing was performed for 45 min to obtain a pre-emulsion.

[0043] Take 36.5g of the pre-emulsion and heat it to 80°C, add 3.3g of ammonium persulfate aqueous solution (mass fraction 5%), keep warm for 20min, then add the remaining 73g of the pre-emulsion and 6.7g of ammonium persulfate aqueous solution (mass fraction 5%) at the same time, keep warm for 3h after the addition is completed, and collect the material after the temperature drops to room temperature to obtain a fabric flame retardant for standby use.

[0044] Example 2

[0045] In a four-necked flask equipped with a stirrer and a thermometer, 20 g of 2,4-diallyloxy-6-amino-1,3,5-triazine, 14 g of 2,4,6-trivinyl-2,4,6-trimethylcyclotrisiloxane, 6 g of N,N'-1,3-propylenebis[2-(vinylsulfonyl)]acetamide, 7.5 g of allyl polyoxyethylene ether (APEG2400) and 52 g of deionized water were added. The temperature was raised to 58°C and high-speed shearing was performed for 50 min to obtain a pre-emulsion.

[0046] Take 33.2g of the pre-emulsion and heat it to 85°C, add 3g of ammonium persulfate aqueous solution (mass fraction 5%) dropwise, keep warm for 20min, then add the remaining 66.3g of the pre-emulsion and 6g of ammonium persulfate aqueous solution (mass fraction 5%) at the same time, keep warm for 4h after the addition is completed, collect the material after the temperature drops to room temperature, and obtain a fabric flame retardant for standby use.

[0047] Example 3

[0048] In a four-necked flask equipped with a stirrer and a thermometer, 22 g of 2,4-diallyloxy-6-amino-1,3,5-triazine, 12 g of tetrakis(dimethylvinylsiloxy)silane, 9 g of N,N'-1,3-propylenebis[2-(vinylsulfonyl)]acetamide, 8 g of allyl polyoxyethylene ether (APEG2160) and 58 g of deionized water were added. The temperature was raised to 55°C and high-speed shearing was performed for 45 min to obtain a pre-emulsion.

[0049] Take 36.3g of pre-emulsion and heat it to 85°C, add 3.3g of ammonium persulfate aqueous solution (mass fraction 5%), keep warm for 30min, then add the remaining 72.7g of pre-emulsion and 6.7g of potassium persulfate aqueous solution (mass fraction 5%) at the same time, keep warm for 3h after the addition, and collect the material after the temperature drops to room temperature to obtain a fabric flame retardant for standby use.

[0050] The comparison of the application effect of each embodiment and the commercially available flame retardant for fabrics with good hand feel and the storage stability of the finished fabrics are shown in Table 1 and Table 2.

[0051] Table 1 Application effect on cotton and polyester fabrics

[0052] Table 2 Storage stability of cotton and polyester fabrics after finishing

[0053]

[0054] It can be seen from Table 1 and Table 2 that when the dosage is 350 g / L, the flame retardant effect of the flame retardant prepared by the present invention is slightly better than the commercial flame retardant and can reach B1 level. The fabric treated with the flame retardant prepared by the present invention has a soft and smooth feel, and the feel is significantly better than the commercial sample. The treated fabric is stored at room temperature for 6 months, and there is no precipitation on the fabric surface, it is dry and non-sticky, the color is uniform, and it has good storage stability.

[0055] Although the present invention has been disclosed as above by way of embodiments, it is not intended to limit the protection scope of the present invention. Any changes and modifications made by any technician familiar with the technology without departing from the concept and scope of the present invention should fall within the protection scope of the present invention.

Claims

1. A fabric flame retardant, characterized in that: It is obtained by polymerizing a monomer composition, wherein the monomer composition, with the total weight being 100%, comprises the following components:

2. The flame retardant for fabrics according to claim 1, characterized in that: It is obtained by polymerizing a monomer composition, wherein the monomer composition, with the total weight being 100%, comprises the following components:

3. The flame retardant for fabrics according to claim 1, characterized in that: The alkenylaminotriazine comonomer is 2-vinyl-4,6-diamino-1,3,5-triazine or 2,4-diallyloxy-6-amino-1,3,5-triazine.

4. The flame retardant for fabrics according to claim 1, characterized in that: The polyalkenylsiloxane comonomer is tetrakis(dimethylvinylsiloxy)silane or 2,4,6-trivinyl-2,4,6-trimethylcyclotrisiloxane.

5. The flame retardant for fabrics according to claim 1, characterized in that: The alkenylsulfonylpropylene diacetamide comonomer is N,N'-1,3-propylene di[2-(vinylsulfonyl)]acetamide.

6. The flame retardant for fabrics according to claim 1, characterized in that: The number average molecular weight of the allyl polyoxyethylene ether comonomer is 2000-3000.

7. The method for preparing the flame retardant for fabrics according to any one of claims 1 to 6, comprising the following steps: 1) Adding comonomer and deionized water into a reactor and mixing them evenly, heating to 50-60° C. and shearing for 30-60 minutes to obtain a pre-emulsion; 2) Take 1 / 3 of the pre-emulsion in step 1), add 1 / 3 of the initiator solution, heat to 78-85°C to initiate emulsion polymerization, keep warm for 10-30 minutes, then simultaneously drop the remaining pre-emulsion and initiator solution, and keep warm for 3-5 hours; 3) Cooling the material in step 2) to room temperature and discharging the material to obtain a fabric flame retardant.

8. The method for preparing a fabric flame retardant according to claim 7, wherein the initiator is ammonium persulfate or potassium persulfate.

9. The method for preparing a fabric flame retardant according to claim 7, wherein the mass fraction of the initiator is 5%.

Citation Information

Patent Citations

  • Combustion inhibitor for cellulose base fiber fabric and its synthesis method

    CN101307565A

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