Flame retardant thermal insulation fabric

Abstract

The invention discloses a flame retardant warm-keeping fabric, which belongs to the technical field of functional fabrics. The fabric is blended and made of viscose fiber, modified polyester fiber and wool fiber, and the mass ratio of the three is 50:45-55:65-75; and the modified polyester fiber is polymerized by a modified monomer with a diol structure, terephthalic acid and ethylene glycol. The fabric of the invention is blended by viscose fiber, modified polyester fiber and cotton fiber. The viscose fiber has good hygroscopicity, is easy to dye, is not prone to static electricity, and has good spinnability. The cotton fiber has good air permeability and skin affinity and has a warm-keeping function. The modified polyester fiber not only has high strength, but also has a flame retardant property that is long-lasting, stable and excellent in effect. The obtained fabric is not only comfortable to wear, but also has a flame retardant function, and has extremely high application value in special fields.

Description

Technical Field

[0001] The invention belongs to the technical field of functional fabrics, and in particular relates to a flame retardant and thermal insulation fabric. Background Art

[0002] With the improvement of people's living standards and the development of the textile industry, many clothing fabrics with special functions have emerged. The development of functional clothing fabrics is based on raw materials, giving them new properties to meet people's fashion needs for nature, comfort, beauty, and health. Common functions include moisture absorption and quick drying, anti-ultraviolet, antibacterial, antistatic, anti-radiation, flame retardant, and warmth. When functional fabrics are used as fire suits, special work clothes, high-temperature filter materials, and used in special fields such as safety protection, environmental protection, chemical industry, and aerospace, the fabrics are required to have good flame retardancy. If the flame retardant performance of the fabric is not good, it is easy to cause harm to the wearer's body, and this fabric cannot have a long-term development prospect.

[0003] In the prior art, the fabric is often treated with a post-finishing technique to roll the fabric to obtain flame retardant properties. However, this flame retardant effect easily disappears after washing and rubbing. Moreover, the fabric produced by this method has the defects of high cost, heavy weight, poor warmth retention, etc. Summary of the invention

[0004] The purpose of the present invention is to overcome the defects of the prior art and provide a flame retardant and warm-keeping fabric.

[0005] The purpose of the present invention can be achieved through the following technical solutions:

[0006] A flame retardant thermal insulation fabric is made by blending viscose fiber, modified polyester fiber and wool fiber, and the mass ratio of the three is 50:45-55:65-75.

[0007] Furthermore, the modified polyester fiber is prepared by the following steps:

[0008] S1. Allylamine and THF (tetrahydrofuran) are placed in a three-necked flask, the temperature of which is maintained at 26-28°C, and the mixture is stirred and mixed evenly; 2-chloroethanol, sodium carbonate and THF are mixed and then slowly dripped into the three-necked flask using a constant pressure dropping funnel, stirring while adding, and stirring and reacting at 26-28°C for 3h after the addition is completed. After the reaction is completed, most of the THF is removed by rotary evaporation, distilled water is added and mixed, and then extracted with ethyl acetate for multiple times, and the organic phase is washed with a saturated NaCl aqueous solution for multiple times and then with anhydrous Na 2 SO 4 Dry, filter, and finally distill under reduced pressure to remove ethyl acetate to obtain intermediate 1; the dosage ratio of allylamine, 2-chloroethanol and sodium carbonate is 6g:8g:10.5g;

[0009] Under the action of sodium carbonate, the -NH 2 A nucleophilic substitution reaction occurs with the -Cl on the 2-chloroethanol molecule. By controlling the molar ratio of the two to be close to 1:1 and a slight excess of allylamine, a substitution reaction occurs. The process is shown below to obtain intermediate 1:

[0010]

[0011] S2, dimethyl phosphite, CCl 4 and tetrahydrofuran were added to a three-necked flask with a stirring device in sequence, the flask was transferred to an ice bath and stirred, triethylamine and the ethyl acetate solution of intermediate 1 were added dropwise to the flask at the same time, after the addition was completed, the three-necked flask was transferred to room temperature and stirred for 10 hours, after the reaction was completed, the filtrate was filtered, and the filtrate was rotary evaporated (to remove tetrahydrofuran, ethyl acetate and CCl 4 ), to obtain intermediate 2; dimethyl phosphite, CCl 4 , tetrahydrofuran, triethylamine, and intermediate 1 are used in a ratio of 11 g:15.4 g:20 mL:10.1 g:10.1 g;

[0012] The -NH- contained in intermediate 1 undergoes an Atherton-Todd reaction with dimethyl phosphite, and the reaction process is shown below to obtain intermediate 2:

[0013]

[0014] S3, tetramethyldisiloxane is placed in a three-necked flask, a platinum catalyst is added, stirred and heated, and after the temperature rises to 75°C, the toluene solution of intermediate 2 is slowly dripped into the system, and the reaction is continued at this temperature for 2h. After the reaction is completed, the catalyst is filtered out, and the reaction solution is evaporated to remove the solvent (toluene) to obtain a modified monomer; the mass ratio of tetramethyldisiloxane to intermediate 2 is 6.7g:20.9g; the amount of platinum catalyst added is 10μg / g of the total mass of the reaction raw materials (tetramethyldisiloxane and intermediate 2);

[0015] Under the action of platinum catalyst, tetramethyldisiloxane and the unsaturated carbon-carbon double bond on the intermediate 2 molecule undergo a hydrosilylation reaction to obtain a modified monomer, the two ends of which are alcohol -OH. The reaction process is as follows:

[0016]

[0017] S4, adding terephthalic acid, ethylene glycol, modified monomer, titanium catalyst and triphenyl phosphate (stabilizer) into a polymerization kettle, after nitrogen replacement, carrying out esterification reaction at 0.25MPa, after the esterification is completed (the water output reaches the theoretical value), gradually raising the temperature in the kettle to 280°C, reducing the vacuum degree of the system to below 100Pa, carrying out polycondensation reaction, discharging and pelletizing to obtain modified polyester; the mass ratio of terephthalic acid, ethylene glycol and modified monomer is 33g:9-11g:23-28g; the amount of titanium catalyst and triphenyl phosphate used is 0.2% and 0.1% of the mass of terephthalic acid, respectively;

[0018] The modified monomer has -OH at both ends of the molecule, which is a diol structure. It is used to replace part of ethylene glycol as a raw material for polyester synthesis, and Si-O-Si segments and N-containing groups are introduced on the main chain of the synthesized modified polyester fiber, and phosphate groups are introduced on the side chain. It should be noted that the Si-O-Si segment on the main chain can not only improve the high temperature resistance of the modified polyester, but also the introduction of Si enables the material to quickly generate a Si-C layer in the event of a fire, which plays a role in isolating oxygen and preventing heat transfer, and can also prevent molten dripping and secondary combustion. When the N-containing group burns, it can produce NO and NO 2 、N 2 It consumes oxygen and dilutes the combustible gas, and N is directly connected to a phosphate group, which forms a strong dehydrating agent, polymetaphosphoric acid, during the thermal decomposition process, so that the polyester polymer is rapidly dehydrated and carbonized during the thermal degradation process, and a carbon layer is formed on the surface of the polyester, which has a flame retardant effect; therefore, a synergistic flame retardant effect of Si-PN is formed, giving the modified polyester excellent flame retardant properties; it should be noted that the flame retardant synergistic components are distributed on the main chain and side chain of the molecule, and will not migrate or seep out, nor will they be significantly reduced due to washing, friction and increased wearing times.

[0019] S5. Mixing the PET slices and the modified polyester in a mass ratio of 70:18-22, and preparing the modified polyester fiber by melt spinning.

[0020] Beneficial effects of the present invention:

[0021] The fabric of the present invention is blended by viscose fiber, modified polyester fiber and cotton fiber. The viscose fiber has good hygroscopicity, is easy to dye, is not prone to static electricity and has good spinnability. The cotton fiber has good air permeability and skin affinity and has a warm-keeping function. The modified polyester fiber has not only high strength but also long-lasting, stable and excellent flame-retardant properties. The obtained fabric is not only comfortable to wear but also has a flame-retardant function and has extremely high application value in special fields. DETAILED DESCRIPTION

[0022] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0023] Example 1

[0024] Preparation of modified polyester fiber:

[0025] S1. 6 g of allylamine and 80 mL of THF were placed in a three-necked flask, the temperature was maintained at 26°C, and the mixture was stirred and mixed evenly; 8 g of 2-chloroethanol, 10.5 g of sodium carbonate and 40 mL of THF were mixed and then slowly dripped into the three-necked flask using a constant pressure dropping funnel, and stirred while adding. After the addition was completed, stirring and reacting at 26°C for 3 h. After the reaction was completed, most of the THF was removed by rotary evaporation, distilled water was added and mixed, and then extracted with ethyl acetate for multiple times. The organic phase was washed with a saturated NaCl aqueous solution for multiple times and then washed with anhydrous Na 2 SO 4 Dry, filter, and finally distill under reduced pressure to remove ethyl acetate to obtain intermediate 1;

[0026] S2, 11g dimethyl phosphite, 15.4g CCl 4 and 20 mL of tetrahydrofuran were added to a three-necked flask with a stirring device in sequence, the flask was transferred to an ice bath and stirred, 10.1 g of triethylamine and 40 mL of ethyl acetate solution containing 10.1 g of intermediate 1 were added dropwise to the flask at the same time, after the addition was completed, the three-necked flask was transferred to room temperature and stirred for 10 h, after the reaction was completed, the filtrate was filtered, and the filtrate was rotary evaporated (to remove tetrahydrofuran, ethyl acetate and CCl 4 ), to obtain intermediate 2;

[0027] S3, 6.7g of tetramethyldisiloxane was placed in a three-necked flask, 276μg of platinum catalyst was added, stirred and heated, and after the temperature rose to 75°C, 20.9g of toluene solution of intermediate 2 was slowly dripped into the system, and the reaction was continued at this temperature for 2h. After the reaction was completed, the catalyst was filtered out, and the reaction solution was evaporated to remove the solvent (toluene) to obtain a modified monomer;

[0028] S4, 33g of terephthalic acid, 11g of ethylene glycol, 23g of modified monomer, 0.066g of titanium catalyst and 0.033g of triphenyl phosphate (stabilizer) were added to a polymerization kettle, and after nitrogen replacement, esterification reaction was carried out at 0.25MPa. After the esterification was completed (the water output reached the theoretical value), the temperature in the kettle was gradually raised to 280°C, and the vacuum degree of the system was reduced to below 100Pa, and a polycondensation reaction was carried out. After discharging and pelletizing, a modified polyester was obtained;

[0029] S5. After mixing 70 g of PET chips and 18 g of modified polyester, the modified polyester fibers were prepared by melt spinning.

[0030] Example 2

[0031] Preparation of modified polyester fiber:

[0032] S1. Place 12 g of allylamine and 160 mL of THF in a three-necked flask, keep the temperature at 28°C, and stir to mix evenly; mix 16 g of 2-chloroethanol, 21 g of sodium carbonate and 80 mL of THF, and then slowly drip into the three-necked flask using a constant pressure dropping funnel, stirring while adding, and continue to stir and react at 28°C for 3 hours after the addition is completed. After the reaction is completed, remove most of the THF by rotary evaporation, add distilled water and mix, then extract with ethyl acetate several times, wash the organic phase with a saturated NaCl aqueous solution several times, and then with anhydrous Na 2 SO 4 Dry, filter, and finally remove ethyl acetate by distillation under reduced pressure to obtain intermediate 1;

[0033] S2, 22g of dimethyl phosphite, 30.8g of CCl 4 and 40 mL of tetrahydrofuran were added to a three-necked flask with a stirring device in sequence, the flask was transferred to an ice bath and stirred, 20.2 g of triethylamine and 80 mL of ethyl acetate solution containing 20.2 g of intermediate 1 were added dropwise into the flask at the same time, after the addition was completed, the three-necked flask was transferred to room temperature and stirred for 10 h, after the reaction was completed, the filtrate was filtered, and the filtrate was rotary evaporated (to remove tetrahydrofuran, ethyl acetate and CCl 4 ), to obtain intermediate 2;

[0034] S3, 13.4g of tetramethyldisiloxane was placed in a three-necked flask, 552μg of platinum catalyst was added, stirred and heated, and after the temperature rose to 75°C, 41.8g of toluene solution of intermediate 2 was slowly dripped into the system, and the reaction was continued at this temperature for 2h. After the reaction was completed, the catalyst was filtered out, and the reaction solution was evaporated to remove the solvent (toluene) to obtain a modified monomer;

[0035] S4, 66g of terephthalic acid, 18g of ethylene glycol, 56g of modified monomer, 0.132g of titanium catalyst and 0.066g of triphenyl phosphate (stabilizer) were added to a polymerization kettle, and after nitrogen replacement, esterification reaction was carried out at 0.25MPa. After the esterification was completed (the water output reached the theoretical value), the temperature in the kettle was gradually raised to 280°C, and the vacuum degree of the system was reduced to below 100Pa, and a polycondensation reaction was carried out. After discharging and pelletizing, a modified polyester was obtained;

[0036] S5. After mixing 140 g of PET chips and 44 g of modified polyester, the modified polyester fibers were prepared by melt spinning.

[0037] Example 3

[0038] Preparation of fabrics:

[0039] 500g of viscose fiber, 450g of modified polyester fiber obtained in Example 1, and 650g of wool fiber were subjected to drawing, roving and spun yarn to obtain fine yarn, and then the fine yarn was respectively wound on the warp beam and reel of a shuttle loom, and then the warp yarn on the warp beam and the weft yarn on the reel were interwoven with each other by the shuttle on the shuttle loom to obtain fabric.

[0040] Example 4

[0041] Preparation of fabrics:

[0042] 500g of viscose fiber, 500g of modified polyester fiber obtained in Example 1, and 700g of wool fiber were subjected to drawing, roving and spun yarn to obtain fine yarn, and then the fine yarn was respectively wound on the warp beam and reel of a shuttle loom, and then the warp yarn on the warp beam and the weft yarn on the reel were interwoven with each other by the shuttle on the shuttle loom to obtain a fabric.

[0043] Example 5

[0044] Preparation of fabrics:

[0045] 500g of viscose fiber, 550g of modified polyester fiber obtained in Example 2, and 750g of wool fiber were subjected to drawing, roving and spun yarn to obtain fine yarn, and then the fine yarn was respectively wound on the warp beam and reel of a shuttle loom, and then the warp yarn on the warp beam and the weft yarn on the reel were interwoven with each other by the shuttle on the shuttle loom to obtain fabric.

[0046] Comparative Example

[0047] The fabric is obtained by replacing the modified polyester fiber in Example 3 with ordinary polyester fiber and keeping the other raw materials and preparation process unchanged.

[0048] The fabrics obtained in Examples 3-5 and the comparative example were cut into test samples and subjected to the following performance tests:

[0049] Thermal insulation performance: According to the national standard GB / T 11048-2008 "Determination of thermal resistance and moisture resistance of textiles under steady-state conditions of biological comfort", thermal resistance tester is used for thermal resistance test;

[0050] Flame retardant properties: The limiting oxygen index is obtained according to GB / T 5454-1997 Textile Combustion Performance Oxygen Index Method;

[0051] The measured results are shown in the following table:

[0052] Example 3 Example 4 Example 5 Comparative Example <![CDATA[Thermal resistance / mK·m 2 ·W -1 > 34.4 35.1 35.9 32.0 LOI / % 38.2 38.5 38.8 26.8

[0053] It can be seen from the data in the above table that the fabric obtained by the present invention has good warmth retention, and through the incorporation of modified polyester fiber, the fabric has excellent flame retardant properties.

[0054] In the description of the specification, the description with reference to the terms "one embodiment", "example", "specific example", etc. means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representation of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in any one or more embodiments or examples in a suitable manner.

[0055] The above contents are merely examples and explanations of the present invention. Those skilled in the art may make various modifications or additions to the specific embodiments described or replace them in a similar manner. As long as they do not deviate from the invention or exceed the scope defined by the claims, they shall all fall within the protection scope of the present invention.

Claims

1. A flame retardant thermal insulation fabric, made by blending viscose fiber, modified polyester fiber and wool fiber, characterized in that: The modified polyester fiber is prepared by the following steps: S1. Allylamine and THF are placed in a three-necked flask, the temperature of which is maintained at 26-28°C, and stirred to mix evenly; 2-chloroethanol, sodium carbonate and THF are mixed evenly, and then slowly dripped into the three-necked flask using a constant pressure dropping funnel, stirring while adding, and after the addition is completed, stirring and reacting at 26-28°C for 3 hours. After the reaction is completed, intermediate 1 is obtained; S2, dimethyl phosphite, CCl4 and tetrahydrofuran are added to a three-necked flask with a stirring device in sequence, the flask is transferred to an ice bath and stirred, triethylamine and the ethyl acetate solution of intermediate 1 are added dropwise to the flask at the same time, after the addition is completed, the three-necked flask is transferred to room temperature and stirred for 10 hours, after the reaction is completed, the filtrate is filtered, and the filtrate is evaporated to obtain intermediate 2; S3, tetramethyldisiloxane is placed in a three-necked flask, a platinum catalyst is added, the mixture is stirred and heated, and after the temperature rises to 75°C, the toluene solution of the intermediate 2 is slowly dripped into the system, and the reaction is continued at this temperature for 2 hours. After the reaction is completed, the catalyst is filtered out, and the reaction solution is evaporated to remove the solvent to obtain a modified monomer; S4, adding terephthalic acid, ethylene glycol, modified monomer, titanium catalyst and triphenyl phosphate into a polymerization kettle, after nitrogen replacement, carrying out esterification reaction at 0.25 MPa, after the esterification, gradually raising the temperature in the kettle to 280°C, reducing the vacuum degree of the system to below 100 Pa, carrying out polycondensation reaction, discharging and pelletizing to obtain modified polyester; S5. After mixing the PET chips and the modified polyester, the modified polyester fibers are prepared by melt spinning.

2. The flame retardant thermal insulation fabric according to claim 1, characterized in that: The mass ratio of viscose fiber, modified polyester fiber and wool fiber is 50:45-55:65-75.

3. The flame retardant thermal insulation fabric according to claim 1, characterized in that: Purification process in step S1: remove most of THF by rotary evaporation, add distilled water to mix, then extract with ethyl acetate multiple times, wash the organic phase with saturated NaCl aqueous solution multiple times, dry with anhydrous Na2SO4, filter, and finally remove ethyl acetate by vacuum distillation.

4. The flame retardant thermal insulation fabric according to claim 1, characterized in that: In step S1, the usage ratio of allylamine, 2-chloroethanol and sodium carbonate is 6g:8g:10.5g.

5. The flame retardant thermal insulation fabric according to claim 1, characterized in that: In step S2, the ratio of the amount of dimethyl phosphite, CCl4, tetrahydrofuran, triethylamine and intermediate 1 is 11 g:15.4 g:20 mL:10.1 g:10.1 g.

6. The flame retardant thermal insulation fabric according to claim 1, characterized in that: The mass ratio of tetramethyldisiloxane to intermediate 2 in step S3 is 6.7 g:20.9 g.

7. The flame retardant thermal insulation fabric according to claim 1, characterized in that: In step S4, the mass ratio of terephthalic acid, ethylene glycol and modified monomer is 33g:9-11g:23-28g; the amount of titanium catalyst and triphenyl phosphate used is 0.2% and 0.1% of the mass of terephthalic acid, respectively.

8. The flame retardant thermal insulation fabric according to claim 1, characterized in that: In step S5, the PET chips and the modified polyester are mixed in a mass ratio of 70:18-22.

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