A kind of n-si series nano hydrogel flame retardant and its preparation and application

A nano-hydrogel and reaction technology, which is applied in the direction of flame-retardant fibers, textiles, papermaking, fiber treatment, etc., can solve the problems of reducing the mechanical and mechanical properties of the matrix material, adding a large amount of flame retardants, and poor durability. High efficiency, strong stability, and achieve the effect of isolated flame retardant

Active Publication Date: 2021-01-05
DONGHUA UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the advantage of the preparation of this kind of flame-retardant regenerated fiber is that the process is short, and the disadvantage is that in order to achieve a better flame-retardant effect, the amount of flame retardant added is relatively large, generally around 10% to 30%. The mechanical and mechanical properties of the base material are poor, and the cost is high

Method used

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  • A kind of n-si series nano hydrogel flame retardant and its preparation and application
  • A kind of n-si series nano hydrogel flame retardant and its preparation and application
  • A kind of n-si series nano hydrogel flame retardant and its preparation and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] (1) Weigh 4.53g of 0.025mol tyrosine and 3.00g of 0.025mol trimethylolethane and dissolve them in 500mL of toluene, put 0.125mol (23.75g) of p-toluenesulfonic acid into amino protection, and react in the single layer glass The reaction was carried out in a kettle, stirred mechanically, heated to 120°C in an oil bath, and reacted for 20 hours. The reactant was first dissolved with isopropanol, then precipitated at low temperature, and vacuum-dried at 50°C for 12 hours. The obtained intermediate product (II) was white powder.

[0046] (2) Weigh 2.48 g of 0.01 mol of 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane, dissolve it in 15 mL of tetrahydrofuran, and weigh 0.07 mol of triethylamine 7.08g, all were put into a three-necked flask; 3.14g of 0.03mol methacryloyl chloride was weighed, put into a 50mL constant-pressure separating funnel, and slowly added dropwise to the three-necked flask within 1 hour, stirred magnetically, and cooled to -20°C, reacted for 18 hours...

Embodiment 2

[0052] (1) Weigh 4.13g of 0.025mol phenylalanine and 3.00g of 0.025mol trimethylolethane and dissolve them in 500mL of tetrahydrofuran, the reaction temperature is 70°C, and the other reaction conditions are the same as in Example I to obtain the intermediate product (II) It is milky white powder.

[0053] (2) Weigh 0.01mol 1,3-bis(3-aminopropyl)-1,1,3,3-tetramethyldisiloxane 2.48g, 0.07mol triethylamine 7.08g, 0.03mol methacrylic Acid chloride 3.14g was dissolved in 20mL of dichloromethane, and the other reaction conditions were the same as in Example I to obtain the intermediate product (III) as a yellow oily substance.

[0054] (3) Weigh 2.52 g of 0.0025 mol intermediate product (II) and 3.24 g of 0.01 mol intermediate product (III), and control the speed at 1000 rpm. Other conditions are the same as those in Example 1 to obtain a white flame-retardant nanogel with a particle size of about 600 nm. . Infrared spectrum data of gel: 2950~3050cm -1 (-CH 3 ),1725~1700cm -1 ...

Embodiment 3

[0059] (1) Weigh 12.38 g of 0.075 mol of phenylalanine and 3.03 g of 0.025 mol of tris hydroxymethylaminomethane and dissolve them in 500 mL of tetrahydrofuran. The other reaction conditions are the same as in Example 1, and the intermediate product (II) is obtained as a white powder.

[0060] (2) Weigh 3.25 g of 0.0025 mol product (II), 12.96 g of intermediate product (III) prepared in 0.04 mol example II, 2.03 g of 0.02 mol triethylamine, add a three-necked flask; dropwise add sodium hydroxide with a pH of 9 The solution obtains an alkaline environment with a pH of 8, the rotational speed is controlled at 1500 rpm, and other conditions are the same as in Example 1, and a white flame-retardant nanogel with a particle size of about 400 nm is obtained. Infrared spectrum data: 2950~3050cm -1 (-CH 3 ),1725~1700cm -1 (C=O), 1100~1270cm -1 (C-O-C),1050cm -1 (Si-O-Si), 830cm -1 (Si-CH 3 ).

[0061] The flame retardant nano gel is fully mixed with the regenerated cellulose sol...

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Abstract

The invention relates to an N-Si serial nano hydrogel and preparation and an application thereof. The N-Si serial nano hydrogel is as shown in a general formula I. The preparation comprises the step of carrying out a reaction on a polyamino compound II containing one or more benzene rings and a primary amine or secondary amine-containing silicone-containing compound, the end group of which is carbon-carbon double bonds to obtain the hydrogel. Permanent flame retardance can be achieved by means of grafting, layer-layer self-assembling and the like according to a stable nanoscale shape of a flame retardant. The nanoscale flame retardant is relatively small in damage to mechanical properties of matrix fibers while achieving efficient flame retardance under the circumstance of grafting or adding in a certain amount, and the process cost can be lowered effectively.

Description

technical field [0001] The invention belongs to the field of flame retardants and their preparation and application, in particular to an N-Si series nano hydrogel flame retardant and its preparation and application. Background technique [0002] Cellulose products are used in multiple fields due to their excellent properties such as renewability, wide sources, and variability, such as textiles and clothing, biomedical, aerospace and other fields. Cellulose is an extremely flammable polymer material (decomposition temperature: 210 ° C ~ 230 ° C, limiting oxygen index value: 18%). During the combustion process, the flame spreads quickly, the calorific value is high, and the amount of smoke is large. It can easily ignite other materials, which can start and spread a fire. This feature limits the in-depth application of cellulose products in more fields. Therefore, the academic community has launched a lot of research on flame-retardant cellulose. [0003] Flame retardants are...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/02D06M15/61
CPCC08G73/0246D06M15/61D06M2200/30
Inventor 吴德群李娜明景李发学王学利俞建勇杨占平曹建华陈昀于涛
Owner DONGHUA UNIV
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