CN116289201A - A kind of intumescent flame retardant flame-retardant polyester/cotton blended fabric and preparation method thereof - Google Patents

Abstract

The invention relates to a polyester/cotton blended fabric which is flame-retardant by an intumescent flame retardant and a preparation method thereof. The surface of the polyester/cotton blended fabric which is flame-retardant by an intumescent flame retardant has a network flame-retardant film, and the network flame-retardant The /cotton blended fabric is bridged by covalent bonds; the network flame retardant film is formed by connecting the intumescent flame retardant on the surface of the polyester/cotton blended fabric through the action of the crosslinking agent; the structural formula of the intumescent flame retardant is

The preparation method is as follows: dissolving intumescent flame retardant, tris (epoxypropyl) isocyanurate, sodium thiosulfate and dicyandiamide in a mixture of water and acetone, and adjusting the pH value of the solution to 6 with ammonia water ~7 to obtain a flame retardant finishing solution, immerse the polyester/cotton blended fabric in the flame retardant finishing solution, and process the polyester/cotton blended fabric by padding-drying-baking to obtain an intumescent flame retardant flame-retardant polyester /Cotton blend fabric. The flame retardant polyester/cotton blended fabric of the invention has excellent flame retardant effect and good flame retardant durability.

Description

A kind of intumescent flame retardant flame-retardant polyester/cotton blended fabric and preparation method thereof

technical field

The invention belongs to the technical field of flame-retardant modification of polyester/cotton blended fabrics, and relates to a polyester/cotton blended fabric flame-retardant with an intumescent flame retardant and a preparation method thereof.

Background technique

With the development of society, people's living standards are constantly improving, and people's awareness of safety protection is gradually increasing. The social demand for textile materials with flame-retardant and protective functions is expanding day by day. Polyester/cotton blended fabrics have the characteristics of crispness, smoothness, quick drying, and durability. They have a large number of applications in civil and industrial fields such as indoor and vehicle interiors, protective clothing, etc. However, there is a special "candle wick effect" in the combustion process of polyester/cotton blended fabrics, and its flame retardancy is different from that of polyester and cotton fabrics, resulting in poor flame retardancy of polyester/cotton blended fabrics, which is difficult to meet the stringent Flame retardant standard requirements. Therefore, the flame retardant modification of polyester/cotton blended fabric is helpful to improve its safety protection performance and expand its application field.

Intumescent flame retardant is a flame retardant and system based on phosphorus and nitrogen. Compared with traditional halogen flame retardants, it has the characteristics of low smoke, non-toxic, high efficiency, and anti-melt drop. It has become an important development direction of flame retardant material science. . Chinese invention patent CN106436285A discloses the preparation and application of an intumescent flame retardant system doped with silica sol. The acid source, carbon source and gas source are mixed to form an intumescent flame retardant system, and then doped with silica sol. It is used to improve the flame retardancy of polyester, cotton or polyester-cotton blended fabrics. However, the composition of the intumescent flame retardant system is complex, and the intumescent flame retardant coating cannot form a strong chemical bond with the polyester/cotton blended fabric, resulting in poor durability of the flame retardant polyester/cotton blended fabric.

Chinese invention patent CN104846639A discloses a method for flame-retardant finishing of cotton fabrics with a reactive intumescent flame retardant. Poor performance, using a mixed system of ethanol and water as a solvent, the reactive intumescent flame retardant is more likely to chemically react with the hydroxyl group of ethanol, thereby losing its activity, resulting in poor durability of the finished cotton fabric.

Literature (Phosphorus/Nitrogen Flame Retardants on Polyester/Cotton Blended Fabric Flame Retardant Finishing [J]. Textile Journal, 2022, 43(6): 94-99, 106) Synthesized phytic acid ammonium salt by using phytic acid and urea, and rolled- The baking-baking process is used for formaldehyde-free flame-retardant finishing of polyester/cotton blended fabrics. Ammonium phytate can produce covalent bond crosslinks with cotton fibers under the catalysis of dicyandiamide. However, during the high-temperature baking process, the ammonium phosphate group The group is easy to decompose to form phosphate and ammonia, which leads to the inability to construct the phosphorus/nitrogen synergistic flame retardant effect, the flame retardant efficiency of the flame retardant is reduced, the washing resistance of the finished polyester/cotton blended fabric is poor, and the flame retardant effect is lost after washing .

Therefore, it is necessary to develop an intumescent flame retardant that integrates an acid source, a carbon source, and a gas source, and graft the intumescent flame retardant on a polyester/cotton blended fabric through a covalent bond to provide an efficient and durable flame retardant. combustion function.

Contents of the invention

The purpose of the present invention is to solve the above-mentioned problems in the prior art, and to provide a polyester/cotton blended fabric flame-retardant with an intumescent flame retardant and a preparation method thereof. The present invention synthesizes an intumescent flame retardant, which contains an acid source, a gas source and a carbon source at the same time, and the combination of the three can effectively construct an intumescent flame retardant to solve the problem of nitrogen loss during high-temperature baking , has high flame retardant properties; the intumescent flame retardant forms a flame retardant network structure on the surface of polyester/cotton blended fabrics under the action of three (glycidyl) isocyanurate crosslinking agents, through multiple A covalent cross-link is deposited on the surface of the polyester/cotton blended fabric to achieve a durable flame retardant effect.

In order to achieve the above object, the technical scheme adopted in the present invention is as follows:

An intumescent flame retardant flame-retardant polyester/cotton blended fabric has a network flame-retardant film on the surface of the intumescent flame-retardant flame-retardant polyester/cotton blended fabric, and the network flame-retardant film and the polyester/cotton blended fabric are covalently Bonds are bridged to produce stable bonds with polyester/cotton blended fabrics, thus endowing polyester/cotton blended fabrics with efficient and durable flame-retardant functions;

The network flame retardant film is formed by connecting the intumescent flame retardant on the surface of the polyester/cotton blended fabric through the crosslinking agent tris(glycidyl)isocyanurate;

The structural formula of intumescent flame retardant is

As a preferred technical solution:

A kind of intumescent flame retardant flame-retardant polyester/cotton blended fabric as mentioned above, the flame-retardant performance of the intumescent flame retardant flame-retardant polyester/cotton blended fabric is: limiting oxygen index (LOI) is 29.8%～33.5% , the damage length is 11.9-8.3cm, no droplet is produced, the maximum heat release rate is 121.3-139.2W/g (the LOI of unmodified polyester/cotton blended fabric is 17.3%, the damage length is 30cm, and the maximum heat release rate is 213.5W/g); after 30 times of washing, the damaged length is not higher than 14.6cm, indicating that the modified polyester/cotton blended fabric has an efficient and durable flame retardant function.

The present invention also provides a method for preparing polyester/cotton blended fabrics flame-retardant by intumescent flame retardants as described above. The polyester/cotton blended fabrics are immersed in a flame-retardant finishing solution, and the fabric is treated by padding-drying-baking. Polyester/cotton blended fabric is processed to obtain intumescent flame retardant flame-retardant polyester/cotton blended fabric;

The flame retardant finishing solution is to dissolve the intumescent flame retardant, tri(epoxypropyl) isocyanurate, sodium thiosulfate and dicyandiamide in the mixture of water and acetone, and adjust the pH value of the solution to 6-7, under this pH condition, the phosphate group is transformed into an ammonium phosphate group, which is helpful for covalent bond crosslinking with cotton fiber.

As a preferred technical solution:

A kind of preparation method of polyester/cotton blended fabric which is flame-retardant by intumescent flame retardant as mentioned above, the concentration of intumescent flame retardant in the flame-retardant finishing liquid is 100～200g/L, and the increase of the dosage of flame retardant is helpful It is used to improve the flame retardant performance of polyester/cotton blended fabrics, but the content of flame retardants on polyester/cotton blended fabrics will reach saturation, and too much will be wasted.

The preparation method of the polyester/cotton blended fabric of a kind of intumescent flame retardant flame-retardant as mentioned above, three (epoxypropyl) isocyanurates serve as network crosslinking agent, three (epoxypropyl) isocyanates The three epoxy groups of uric acid ester can cross-link with the phosphate and hydroxyl groups of the intumescent flame retardant, so that the intumescent flame retardant is connected to each other on the surface of the polyester/cotton blended fabric to form a network structure; the three (epoxy Propyl) isocyanurate can also react with the hydroxyl group on the surface of the fabric, as a crosslinking agent between the flame retardant and the polyester/cotton blended fabric, and the flame retardant network coating is grafted on the polyester/cotton blended fabric through covalent bonds. Cotton blend fabric surface, which provides efficient and durable flame retardant function. The molar ratio of tris (glycidyl) isocyanurate to intumescent flame retardant is 2 to 3:1, increasing the amount of tris (glycidyl) isocyanurate is helpful for the formation of network structure And the grafting of flame retardant on the fabric, but it is wasteful if it is too high; acetone is the solvent of tri(epoxypropyl) isocyanurate, and acetone accounts for 20% to 30% of the total volume of water and acetone; Sodium thiosulfate is used as a catalyst to promote the reaction of the epoxy group of three (epoxypropyl) isocyanurate and the hydroxyl group of cotton fiber and intumescent flame retardant. The quality of sodium thiosulfate is three (epoxypropylene) base) 3-5% of isocyanurate; under the catalysis of dicyandiamide, the ammonium phosphate group of the intumescent flame retardant can undergo esterification and cross-linking reaction with the hydroxyl group of cotton fiber, and the quality of dicyandiamide is the expansion 5-7% of the type flame retardant.

The above-mentioned preparation method of polyester/cotton blended fabric with intumescent flame retardant flame retardant, the process parameters of padding-drying-baking are: 100% to 110% overfill rate; 70% to 80°C prebaking temperature, The pre-baking time is 2-4 minutes; the baking temperature is 160-170°C, and the baking time is 5-8 minutes. The higher the excess rate, the higher the liquid carrying capacity of the polyester/cotton blended fabric, which helps to improve the flame retardant performance, but the flame retardant content on the fabric is too high, which will be saturated, resulting in waste; the increase of the baking temperature will help It is used to promote the reaction between tris(glycidyl)isocyanurate and intumescent flame retardants and polyester/cotton blended fabrics, but if it is too high, it will be wasteful and will easily cause damage to the physical properties of the fabric.

A method for preparing polyester/cotton blended fabrics flame-retardant by intumescent flame retardants as described above, wherein the polyester/cotton blended fabrics are 35/65, 40/60 or 45/55 polyester/cotton blended fabrics.

A method for preparing an intumescent flame retardant flame-retardant polyester/cotton blended fabric as described above, the preparation method of the intumescent flame retardant is: heating tris(glycidyl)isocyanurate to 140- After 150°C, add pentaerythritol to react for 3-4 hours (140-150°C is higher than the melting point of tris(epoxypropyl)isocyanurate, and tris(epoxypropyl)isocyanurate is liquid at this temperature State, contribute to the progress of the reaction; the reaction time is 3 to 4 hours, the rise of the reaction temperature and the extension of the time are conducive to the progress of the synthesis reaction, but if it is too high, it will be a waste), then add phosphoric acid and Continue to react for 3 to 4 hours (the rise of the reaction temperature and the extension of the time will help the synthesis reaction, but if it is too high, it will be a waste), and the intumescent flame retardant is obtained after drying and purification.

A method for preparing polyester/cotton blended fabrics that are flame-retardant with an intumescent flame retardant as described above, the molar ratio of tris(epoxypropyl)isocyanurate and pentaerythritol is 2 to 2.2:1, and two moles of three The epoxy group of (epoxypropyl) isocyanurate and the two hydroxyl groups of pentaerythritol undergo epoxy ring-opening addition reaction; the molar ratio of phosphoric acid and three (epoxypropyl) isocyanurate is 2 ～2.3:1, the remaining two epoxy groups of tris(glycidyl)isocyanurate and the phosphate group can undergo epoxy ring-opening addition reaction, a slight excess of phosphoric acid helps to improve the reaction efficiency, but too much High is wasted.

As mentioned above, the preparation method of polyester/cotton blended fabric with intumescent flame retardant flame retardant, after the reaction, the product is first vacuum-dried to remove moisture, and then purified by methanol and toluene. The yield of intumescent flame retardant 75-79%.

Principle of the present invention is as follows:

The present invention synthesizes an intumescent flame retardant, which contains an acid source, a gas source and a carbon source at the same time, and the combination of the three can effectively construct an intumescent flame retardant, which can solve the problem of nitrogen loss during high-temperature baking The problem is that it has high flame retardant properties. Tris (glycidyl) isocyanurate contains three epoxy groups, which can be used as a network cross-linking agent to produce a cross-linking reaction with the phosphate and hydroxyl groups of the intumescent flame retardant during the baking process, so that The intumescent flame retardant is connected to each other on the surface of the polyester/cotton blended fabric to form a network film structure; tri(epoxypropyl)isocyanurate can also react with the hydroxyl group of the cotton fiber, as a flame retardant and polyester/cotton blended fabric The crosslinking agent between the flame retardants grafts the flame retardant network structure on the surface of the polyester/cotton blended fabric through covalent bonds; in addition, the ammonium phosphate root of the intumescent flame retardant is combined with the cotton fiber under the action of dicyandiamide catalyst and high temperature The hydroxyl group undergoes an esterification reaction. Therefore, the present invention provides a highly efficient and durable flame retardant function by building a network structure on the surface of the fabric and fixing it on the surface of the polyester/cotton blended fabric through various crosslinking methods.

Beneficial effect:

(1) The preparation method of the polyester/cotton blended fabric of a kind of intumescent flame retardant flame-retardant of the present invention, phosphorus-containing flame-retardant group, nitrogen-containing heterocyclic ring, polyol group are combined by covalent bond, synthesis contains three The flame retardant with one group will not lose nitrogen due to baking; the phosphate radical in the intumescent flame retardant acts as an acid source, the nitrogen-containing heterocycle acts as a gas source, and the polyol acts as a carbon source. The combination of the three It can effectively construct intumescent flame retardant; during the combustion process, the intumescent flame retardant helps to form intumescent charcoal on the surface of polyester/cotton blended fabrics, which has the effect of isolating heat, oxygen and flammable gases, and has excellent Flame retardant properties;

(2) The preparation method of the polyester/cotton blended fabric of a kind of intumescent flame retardant flame-retardant of the present invention, by constructing network structure on the fabric surface, and be fixed on the polyester/cotton blended fabric surface by various cross-linking ways, thereby Provide efficient and durable flame retardant function;

(3) An intumescent flame retardant flame-retardant polyester/cotton blended fabric of the present invention has excellent flame-retardant effect and good flame-retardant durability.

Description of drawings

Fig. 1 is the ¹³ C nuclear magnetic resonance spectrum of the intumescent flame retardant in embodiment 1;

Figure 2 is a schematic diagram of the crosslinking mechanism of intumescent flame retardants on polyester/cotton blended fabrics, where IFR stands for intumescent flame retardants and Fabric stands for polyester/cotton blended fabrics.

Detailed ways

The present invention will be further described below in combination with specific embodiments. It should be understood that these examples 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 teachings of the present invention, those skilled in the art can make various changes or modifications to the present invention, and these equivalent forms also fall within the scope defined by the appended claims of the present application.

According to AATCC 61-2006 "Accelerated Test of Household and Commercial Washing Color Fastness", the present invention washes polyester/cotton blended fabrics flame-retardant by intumescent flame retardants.

The test method that the present invention adopts is as follows:

(1) Limiting oxygen index: determined according to the standard of GB/T 5454-1997 "Oxygen index method for textile combustion performance experiment";

(2) Damage length: measured according to GB/T 5455-2014 "Determination of smoldering and afterburning time of damage length in vertical direction of textile combustion performance";

(3) Maximum heat release rate: Tested with reference to ASTM D7309-21a.

Example 1

A kind of preparation method of the polyester/cotton blended fabric that intumescent flame retardant fire-retardant is specifically as follows:

(1) According to the molar ratio of tris (epoxypropyl) isocyanurate and pentaerythritol is 2:1, after heating tris (epoxypropyl) isocyanurate to 140°C, add pentaerythritol to react for 4 hours, then Add phosphoric acid according to the molar ratio of phosphoric acid and tris(glycidyl)isocyanurate as 2:1, and continue to react at 110°C for 3h. Carry out purification, make intumescent flame retardant, the productive rate of intumescent flame retardant is 75%, and its structural formula is

(2) According to the molar ratio of tris (epoxypropyl) isocyanurate and intumescent flame retardant is 2.3:1, the quality of sodium thiosulfate is tris (epoxypropyl) isocyanurate 3%, the quality of dicyandiamide is the ratio of 6% of intumescent flame retardant, the intumescent flame retardant that step (1) obtains, three (epoxypropyl) isocyanurate, sodium thiosulfate Dicyandiamide is dissolved in the mixed solution of water and acetone (acetone accounts for 25% of the total volume of water and acetone), and ammonia water is used to adjust the pH value of the solution to 6 to obtain a flame-retardant finishing solution. In the flame-retardant finishing solution, the intumescent flame retardant The concentration is 100g/L;

(3) Immerse the 35/65 polyester/cotton blended fabric in the flame-retardant finishing solution obtained in step (2) (the cross-linking mechanism is shown in Figure 2), and the polyester/cotton blended fabric is processed by padding-drying-baking. The fabric is processed, and the excess rate is controlled to be 100%, the pre-baking temperature is 80°C, the pre-baking time is 2min, the baking temperature is 170°C, and the baking time is 5min, and the intumescent flame retardant flame-retardant polyester/ Cotton blend fabric.

The prepared intumescent flame retardant flame-retardant polyester/cotton blended fabric has a network flame-retardant film on the surface, and the network flame-retardant film is made of intumescent flame retardant connected by three (glycidyl) isocyanurate on the polyester It is formed on the surface of the polyester/cotton blended fabric, and the network flame-retardant film and the polyester/cotton blended fabric are bridged by covalent bonds;

The flame retardant properties of polyester/cotton blended fabrics flame-retardant by intumescent flame retardants are: the limiting oxygen index is 29.8%, the damaged length is 11.9cm, no molten droplets are produced, and the maximum heat release rate is 139.2W/g; after 30 times The damaged length after washing was 14.6 cm.

The ¹³ C NMR spectrum of the intumescent flame retardant is shown in Fig. 1 . As can be seen from Figure 1, the chemical shift at 150.6ppm is caused by the carbon atom of the C=O structure on the nitrogen heterocycle, and the chemical shift at 59.2 and 46.2ppm is caused by the carbon atom and central carbon of the pentaerythritol C-OH structure The chemical shifts at 45.7 and 45.2ppm are caused by the carbon atoms of the CN structure connected to the epoxy group; the chemical shifts at 67.0ppm and 63.9ppm are caused by the epoxy group in the structure of the intumescent flame retardant The COP generated after the reaction is caused by the carbon atoms of the C-OH structure, indicating that the epoxy group reacted with the phosphate group. The chemical shifts at 74.8 and 69.7ppm are caused by the ring-opening carbon atom of the epoxy group and the pentaerythritol carbon atom in the CO structure after the reaction of the epoxy group and the pentaerythritol hydroxyl group, respectively. The above results indicate the successful synthesis of intumescent flame retardants.

Comparative example 1

A method for preparing an intumescent flame retardant flame-retardant polyester/cotton blended fabric is basically the same as in the examples, except that the flame retardant solution in step (2) is the intumescent flame retardant obtained in step (1). agent, sodium thiosulfate and dicyandiamide are dissolved in a mixture of water and acetone (acetone accounts for 25% of the total volume of water and acetone), and ammonia water is used to adjust the pH value of the solution to 6, while the intumescent flame retardant, The consumption proportion relationship between sodium thiosulfate and dicyandiamide, the proportion relationship between water and acetone and the concentration of flame retardant solution are all the same as in Example 1. The flame retardant properties of the polyester/cotton blended fabric obtained by the intumescent flame retardant flame retardant are as follows: the limiting oxygen index is 29.3%, the damaged length is 12.1 cm, no droplet is produced, and the maximum heat release rate is 142.3 W/g ; After 5 times of washing, the damaged length is 30cm.

Comparing Example 1 with Comparative Example 1, it can be seen that the flame-retardant performance of the flame-retardant polyester/cotton blended fabric prepared in Comparative Example 1 is slightly lower than that of the flame-retardant polyester/cotton blended fabric prepared in Example 1, while for The washing resistance of the flame-retardant polyester/cotton blended fabric prepared in Example 1 is obviously poor, because the intumescent flame retardant in Comparative Example 1 is simply deposited on the polyester/cotton blended fabric and cannot form a covalent bond with the fabric. Combination, and the surface of polyester/cotton blended fabrics cannot be combined to form a network flame retardant film, and the intumescent flame retardant is easily washed off during the washing process, thus losing the flame retardant effect.

Example 2

A kind of preparation method of the polyester/cotton blended fabric that intumescent flame retardant fire-retardant is specifically as follows:

(1) According to the molar ratio of tris (epoxypropyl) isocyanurate and pentaerythritol is 2.1:1, after heating tris (epoxypropyl) isocyanurate to 145°C, add pentaerythritol to react for 3 hours, then Add phosphoric acid according to the molar ratio of phosphoric acid and tris(epoxypropyl)isocyanurate as 2.1:1, and continue to react at 115°C for 3h. Carry out purification, make intumescent flame retardant, the productive rate of intumescent flame retardant is 76%, and its structural formula is

(2) According to the molar ratio of tris (glycidyl) isocyanurate and intumescent flame retardant is 3:1, the quality of sodium thiosulfate is tris (glycidyl) isocyanurate 3.5%, the quality of dicyandiamide is the ratio of 7% of intumescent flame retardant, the intumescent flame retardant that step (1) obtains, three (epoxypropyl) isocyanurate, sodium thiosulfate and dicyandiamide are dissolved in the mixed solution of water and acetone (acetone accounts for 30% of the total volume of water and acetone), and ammonia water is used to adjust the pH value of the solution to 6.2 to obtain a flame-retardant finishing solution, and the intumescent flame retardant in the flame-retardant finishing solution The concentration is 200g/L;

(3) Immerse the 40/60 polyester/cotton blended fabric in the flame-retardant finishing solution obtained in step (2), and process the polyester/cotton blended fabric by padding-drying-baking to control the excess rate of 110 %, the pre-drying temperature is 78°C, the pre-drying time is 3min, the curing temperature is 160°C, and the curing time is 8min, and the intumescent flame retardant flame-retardant polyester/cotton blended fabric is obtained.

The prepared intumescent flame retardant flame-retardant polyester/cotton blended fabric has a network flame-retardant film on the surface, and the network flame-retardant film is made of intumescent flame retardant connected by three (glycidyl) isocyanurate on the polyester It is formed on the surface of the polyester/cotton blended fabric, and the network flame-retardant film and the polyester/cotton blended fabric are bridged by covalent bonds;

The flame retardant properties of polyester/cotton blended fabrics flame-retardant by intumescent flame retardants are: the limiting oxygen index is 33.5%, the damaged length is 8.3cm, no molten droplets are produced, and the maximum heat release rate is 121.3W/g; after 30 times The damaged length after washing was 12.5 cm.

Example 3

A kind of preparation method of the polyester/cotton blended fabric that intumescent flame retardant fire-retardant is specifically as follows:

(1) According to the molar ratio of tris(epoxypropyl)isocyanurate and pentaerythritol is 2.1:1, heat tris(epoxypropyl)isocyanurate to 150°C and then add pentaerythritol to react for 3.5h, Then add phosphoric acid according to the molar ratio of phosphoric acid and three (glycidyl) isocyanurate is 2.2:1, and continue to react 4h at 105 ℃, after the reaction finishes, the product first removes moisture by vacuum drying, and then adopts methanol and Toluene is purified to obtain an intumescent flame retardant, and the yield of the intumescent flame retardant is 76%, and its structural formula is

(2) According to the molar ratio of tris (glycidyl) isocyanurate and intumescent flame retardant is 2:1, the quality of sodium thiosulfate is tris (glycidyl) isocyanurate 4%, the quality of dicyandiamide is the ratio of 5% of intumescent flame retardant, the intumescent flame retardant that step (1) obtains, three (epoxypropyl) isocyanurate, sodium thiosulfate and dicyandiamide are dissolved in the mixed solution of water and acetone (acetone accounts for 20% of the total volume of water and acetone), and ammonia water is used to adjust the pH value of the solution to 6.5 to obtain a flame-retardant finishing solution, and the intumescent flame retardant in the flame-retardant finishing solution The concentration is 120g/L;

(3) Immerse the 45/55 polyester/cotton blended fabric in the flame-retardant finishing solution obtained in step (2), and process the polyester/cotton blended fabric by padding-drying-baking to control the excess rate of 105 %, the pre-drying temperature is 76 ° C, the pre-drying time is 4 min, the curing temperature is 165 ° C, and the curing time is 6 min, and the intumescent flame retardant flame-retardant polyester/cotton blended fabric is obtained.

The prepared intumescent flame retardant flame-retardant polyester/cotton blended fabric has a network flame-retardant film on the surface, and the network flame-retardant film is made of intumescent flame retardant connected by three (glycidyl) isocyanurate on the polyester It is formed on the surface of the polyester/cotton blended fabric, and the network flame-retardant film and the polyester/cotton blended fabric are bridged by covalent bonds;

The flame retardant properties of polyester/cotton blended fabrics flame-retardant by intumescent flame retardants are: the limiting oxygen index is 30.5%, the damage length is 11.1cm, no droplet is produced, and the maximum heat release rate is 133W/g; after 30 times of washing The post-damage length was 14cm.

Example 4

A kind of preparation method of the polyester/cotton blended fabric that intumescent flame retardant fire-retardant is specifically as follows:

(1) According to the molar ratio of tris(epoxypropyl)isocyanurate and pentaerythritol is 2.2:1, heat tris(epoxypropyl)isocyanurate to 145°C and then add pentaerythritol to react for 3.5h, Then add phosphoric acid according to the molar ratio of phosphoric acid and three (glycidyl) isocyanurate is 2.2:1, and continue to react 4h at 108 ℃, after the reaction finishes, the product first removes moisture by vacuum drying, and then adopts methanol and Toluene is purified to obtain an intumescent flame retardant, and the yield of the intumescent flame retardant is 76%, and its structural formula is

(2) According to the molar ratio of tris (epoxypropyl) isocyanurate and intumescent flame retardant is 2.8:1, the quality of sodium thiosulfate is tris (epoxypropyl) isocyanurate 4.5%, the quality of dicyandiamide is the ratio of 5.5% of intumescent flame retardant, the intumescent flame retardant that step (1) obtains, three (epoxypropyl) isocyanurate, sodium thiosulfate and dicyandiamide are dissolved in the mixed solution of water and acetone (acetone accounts for 22% of the total volume of water and acetone), and ammonia water is used to adjust the pH value of the solution to 6.8 to obtain a flame-retardant finishing solution. In the flame-retardant finishing solution, the intumescent flame retardant The concentration is 180g/L;

(3) Immerse the 35/65 polyester/cotton blended fabric in the flame-retardant finishing solution obtained in step (2), and process the polyester/cotton blended fabric by padding-drying-baking to control the excess rate of 105 %, the pre-drying temperature is 75°C, the pre-drying time is 4min, the curing temperature is 168°C, and the curing time is 7min, and the intumescent flame retardant flame-retardant polyester/cotton blended fabric is obtained.

The prepared intumescent flame retardant flame-retardant polyester/cotton blended fabric has a network flame-retardant film on the surface, and the network flame-retardant film is made of intumescent flame retardant connected by three (glycidyl) isocyanurate on the polyester It is formed on the surface of the polyester/cotton blended fabric, and the network flame-retardant film and the polyester/cotton blended fabric are bridged by covalent bonds;

The flame retardant properties of polyester/cotton blended fabrics flame-retardant by intumescent flame retardants are: the limiting oxygen index is 32.8%, the damaged length is 8.9cm, no molten droplets are produced, and the maximum heat release rate is 124.1W/g; after 30 times The damaged length after washing was 12.8 cm.

Example 5

A kind of preparation method of the polyester/cotton blended fabric that intumescent flame retardant fire-retardant is specifically as follows:

(1) According to the molar ratio of tris (epoxypropyl) isocyanurate and pentaerythritol is 2.2:1, after heating tris (epoxypropyl) isocyanurate to 145°C, add pentaerythritol to react for 4 hours, then Add phosphoric acid according to the molar ratio of phosphoric acid and tris(glycidyl)isocyanurate as 2.3:1, and continue to react at 110°C for 3.5h. Toluene is purified to obtain an intumescent flame retardant, and the yield of the intumescent flame retardant is 79%, and its structural formula is

(2) According to the molar ratio of tris (epoxypropyl) isocyanurate and intumescent flame retardant is 2.6:1, the quality of sodium thiosulfate is tris (epoxypropyl) isocyanurate 4.8%, the quality of dicyandiamide is the ratio of 6% of intumescent flame retardant, the intumescent flame retardant that step (1) obtains, three (glycidyl) isocyanurate, sodium thiosulfate and dicyandiamide are dissolved in the mixed solution of water and acetone (acetone accounts for 25% of the total volume of water and acetone), and ammonia water is used to adjust the pH value of the solution to 6.6 to obtain a flame-retardant finishing solution. In the flame-retardant finishing solution, the intumescent flame retardant The concentration is 150g/L;

(3) Immerse the 40/60 polyester/cotton blended fabric in the flame-retardant finishing solution obtained in step (2), and process the polyester/cotton blended fabric by padding-drying-baking to control the excess rate of 108 %, the pre-drying temperature is 72 ° C, the pre-drying time is 2 min, the curing temperature is 165 ° C, and the curing time is 6 min, and the intumescent flame retardant flame-retardant polyester/cotton blended fabric is obtained.

The prepared intumescent flame retardant flame-retardant polyester/cotton blended fabric has a network flame-retardant film on the surface, and the network flame-retardant film is made of intumescent flame retardant connected by three (glycidyl) isocyanurate on the polyester It is formed on the surface of the polyester/cotton blended fabric, and the network flame-retardant film and the polyester/cotton blended fabric are bridged by covalent bonds;

The flame retardant properties of polyester/cotton blended fabrics flame-retardant by intumescent flame retardants are: the limiting oxygen index is 31.4%, the damage length is 10.5cm, there is no droplet generation, and the maximum heat release rate is 128.3W/g; after 30 times The damaged length after washing was 13.2 cm.

Example 6

A kind of preparation method of the polyester/cotton blended fabric that intumescent flame retardant fire-retardant is specifically as follows:

(1) According to the molar ratio of tris (epoxypropyl) isocyanurate and pentaerythritol is 2.2:1, after heating tris (epoxypropyl) isocyanurate to 145°C, add pentaerythritol to react for 3 hours, then Add phosphoric acid according to the molar ratio of phosphoric acid and tris(epoxypropyl)isocyanurate as 2.3:1, and continue to react at 112°C for 3.5h. Toluene is purified to obtain an intumescent flame retardant, and the yield of the intumescent flame retardant is 78%, and its structural formula is

(2) According to the molar ratio of tris (epoxypropyl) isocyanurate and intumescent flame retardant is 2.5:1, the quality of sodium thiosulfate is tris (epoxypropyl) isocyanurate 5%, the quality of dicyandiamide is the ratio of 6.5% of intumescent flame retardant, the intumescent flame retardant that step (1) obtains, three (glycidyl) isocyanurate, sodium thiosulfate and dicyandiamide are dissolved in the mixed solution of water and acetone (acetone accounts for 28% of the total volume of water and acetone), and ammonia water is used to adjust the pH value of the solution to 7 to obtain a flame-retardant finishing solution. In the flame-retardant finishing solution, the intumescent flame retardant The concentration is 160g/L;

(3) Immerse the 45/55 polyester/cotton blended fabric in the flame-retardant finishing solution obtained in step (2), and process the polyester/cotton blended fabric by padding-drying-baking to control the excess rate of 102 %, the pre-drying temperature is 70 ° C, the pre-drying time is 3 min, the curing temperature is 162 ° C, and the curing time is 6 min, and the intumescent flame retardant flame-retardant polyester/cotton blended fabric is obtained.

The prepared intumescent flame retardant flame-retardant polyester/cotton blended fabric has a network flame-retardant film on the surface, and the network flame-retardant film is made of intumescent flame retardant connected by three (glycidyl) isocyanurate on the polyester It is formed on the surface of the polyester/cotton blended fabric, and the network flame-retardant film and the polyester/cotton blended fabric are bridged by covalent bonds;

The flame retardant properties of polyester/cotton blended fabrics flame-retardant by intumescent flame retardants are: the limiting oxygen index is 31.9%, the damaged length is 9.9cm, no molten droplets are produced, and the maximum heat release rate is 126.8W/g; after 30 times The damaged length after washing was 13.1 cm.

Claims (10)

1. A polyester/cotton blended fabric that is flame-retardant by an intumescent flame retardant, characterized in that: the surface of the polyester/cotton blended fabric that is flame-retardant by an intumescent flame retardant has a network flame-retardant film, and the network flame-retardant film and the polyester/cotton blended fabric Cotton blend fabrics are bridged by covalent bonds; The network flame retardant film is formed by connecting the intumescent flame retardant on the surface of the polyester/cotton blended fabric through tris(epoxypropyl)isocyanurate; The structural formula of intumescent flame retardant is

2. a kind of intumescent flame retardant flame-retardant polyester/cotton blended fabric according to claim 1 is characterized in that the flame-retardant performance of the intumescent flame retardant flame-retardant polyester/cotton blended fabric is: limiting oxygen The index is 29.8%-33.5%, the damage length is 11.9-8.3cm, no droplet occurs, and the maximum heat release rate is 121.3-139.2W/g; after 30 times of washing, the damage length is not higher than 14.6cm. 3. The preparation method of a kind of intumescent flame retardant flame-retardant polyester/cotton blended fabric as claimed in claim 1 or 2, characterized in that: the polyester/cotton blended fabric is immersed in the flame-retardant finishing solution, -Bake-bake the polyester/cotton blended fabric to process the polyester/cotton blended fabric with intumescent flame retardant; The flame retardant finishing solution is to dissolve the intumescent flame retardant, tri(epoxypropyl) isocyanurate, sodium thiosulfate and dicyandiamide in the mixture of water and acetone, and adjust the pH value of the solution to 6 ~ 7 get. 4. The preparation method of an intumescent flame retardant flame-retardant polyester/cotton blended fabric according to claim 3, wherein the concentration of the intumescent flame retardant in the flame-retardant finishing solution is 100 to 200 g/L . 5. the preparation method of the polyester/cotton blended fabric of a kind of intumescent flame retardant flame retardant according to claim 4 is characterized in that, three (epoxypropyl) isocyanurate and intumescent flame retardant The molar ratio is 2 to 3:1; acetone accounts for 20% to 30% of the total volume of water and acetone; the quality of sodium thiosulfate is 3 to 5% of tris (epoxypropyl) isocyanurate; bis The mass of cyanamide is 5-7% of that of the intumescent flame retardant. 6. the preparation method of the polyester/cotton blended fabric of a kind of intumescent flame retardant flame-retardant according to claim 5, is characterized in that, The process parameters of padding-baking-baking are: excess rolling rate 100-110%; pre-baking temperature 70-80°C, pre-baking time 2-4 minutes; The baking temperature is 160-170°C, and the baking time is 5-8 minutes. 7. the preparation method of the polyester/cotton blended fabric of a kind of intumescent flame retardant flame-retardant according to claim 6, is characterized in that, the polyester/cotton blended fabric is 35/65, 40/60 or 45/55 Poly/cotton blend fabric. 8. the preparation method of a kind of intumescent flame retardant flame-retardant polyester/cotton blended fabric according to claim 3, is characterized in that, the preparation method of intumescent flame retardant is: three (epoxypropyl) Heat the isocyanurate to 140-150°C, add pentaerythritol to react for 3-4 hours, then add phosphoric acid and continue to react at 105-115°C for 3-4 hours, dry and purify to obtain intumescent flame retardant. 9. the preparation method of the polyester/cotton blended fabric of a kind of intumescent flame retardant flame retardant according to claim 8 is characterized in that, the mol ratio of three (epoxypropyl) isocyanurate and pentaerythritol is 2～2.2:1; the molar ratio of phosphoric acid and tris(epoxypropyl)isocyanurate is 2～2.3:1. 10 . The method for preparing an intumescent flame retardant flame-retardant polyester/cotton blended fabric according to claim 8 , wherein the yield of the intumescent flame retardant is 75-79%. 11 .

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