Preparation method of phosphorus-nitrogen-silicon-based flame-retardant polyester-cotton blended fabric

Abstract

The invention discloses a preparation method of a phosphorus-nitrogen-silicon-based flame-retardant polyester-cotton blended fabric, which comprises the following steps: synthesizing an acrylate-based cationic monomer containing phosphorus and nitrogen components and an acrylate-based cationic monomer containing silicon and nitrogen components; and adding an initiator, a penetrant and the like into the prepared aqueous solution, and carrying out flame-retardant treatment on the polyester-cotton blended fabric to obtain the phosphorus-nitrogen-silicon-based flame-retardant polyester-cotton blended fabric. The flame-retardant monomer prepared by the invention is fixed on the surface of the polyester-cotton fabric through dipping deposition and in-situ polymerization, so that the fabric has a durable flame-retardant effect and has a very good practical value.

Description

Technical Field

[0001] The present invention relates to a flame retardant process technology for polyester-cotton blended fabrics, belonging to the technical field of textile functional finishing. Background Art

[0002] Polyester-cotton blended fabrics combine the excellent properties of polyester and cotton, such as breathable comfort, dimensional stability, smoothness and stiffness, easy washing and quick drying, etc., and have very wide applications in aspects such as clothing and furniture decoration. However, compared with pure polyester fabrics or cotton fabrics, polyester-cotton fabrics will form a special "scaffold effect" during the combustion process, resulting in more intense combustion, thus bringing greater fire safety hazards. Although the flame retardant treatment technologies for polyester fabrics and cotton fabrics have been relatively mature, due to their special structure and combustion process, polyester-cotton blended fabrics have higher requirements for flame retardant technologies. Therefore, it is urgent to develop more novel and efficient flame retardant technologies for polyester-cotton fabrics. Summary of the Invention

[0003] The purpose of the present invention is to provide a preparation method for a phosphorus-nitrogen-silicon-based flame retardant polyester-cotton blended fabric, so that the polyester-cotton blended fabric has a durable flame retardant effect.

[0004] In order to achieve the above-mentioned invention purpose, the present invention provides the following technical solutions:

[0005] A preparation method for a phosphorus-nitrogen-silicon-based flame retardant polyester-cotton blended fabric, comprising the following steps:

[0006] Weigh a certain amount of flame retardant monomer A, flame retardant monomer B, initiator, penetrant and water to prepare a flame retardant finishing solution;

[0007] The polyester-cotton fabric is impregnated in the flame retardant finishing solution for 10 - 30 min;

[0008] Transfer the fabric to pre-dry at 60 - 90 °C for 10 - 30 min, and then cure at 140 - 170 °C for 1 - 5 min, thereby obtaining a phosphorus-nitrogen-silicon-based flame retardant polyester-cotton blended fabric;

[0009] The flame retardant finishing solution contains 300 - 500 g / L of flame retardant monomer A, 100 - 300 g / L of flame retardant monomer B, 1 wt% of initiator (1 wt% of the total amount of flame retardant monomer A and flame retardant monomer B), 5 - 10 g / L of penetrant, and the balance is water.

[0010] The described flame retardant monomer A is prepared as follows: Using phosphorus oxychloride as the raw material, after dissolving it in chloroform, the reaction temperature is maintained at 35°C. Neopentyl glycol is slowly added and the reaction is maintained for 4 hours. Then, the temperature is raised to 45°C and stirred for 1 hour, and then further raised to 60°C and stirred for 1 hour. After the above reaction is completed, the obtained solution is placed in a rotary evaporator to remove the solvent, thereby obtaining the intermediate 2-oxo-2-chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane. The purified intermediate product and dimethylaminoethyl methacrylate are dissolved in N,N-dimethylformamide. After introducing nitrogen, the reaction is carried out at 80°C for 24 hours under the action of potassium iodide and an inhibitor (1,4-benzenediol). After the reaction is completed, the solution is filtered and purified. Then, it is placed in a rotary evaporator again to remove the solvent, and the phosphazene-based acrylate flame retardant monomer A is obtained.

[0011] The structural formula of the flame retardant monomer A is:

[0012]

[0013] Preferably, in the preparation method of the flame retardant monomer A, the molar ratio of phosphorus oxychloride, neopentyl glycol, dimethylaminoethyl methacrylate, and potassium iodide is 1.3:1.3:1:1.3.

[0014] Preferably, in the preparation method of the flame retardant monomer A, the dosage of the inhibitor 1,4-benzenediol is 1 wt% of the monomer dosage.

[0015] The described flame retardant monomer B is prepared as follows: Weigh a certain mass of γ-chloropropyltriethoxysilane and dimethylaminoethyl methacrylate. After adding N,N-dimethylformamide and fully dissolving them, nitrogen is introduced, and the reaction is carried out at 80°C for 24 hours under the action of potassium iodide and an inhibitor (1,4-benzenediol). After the reaction is completed, the solution is filtered and purified. Then, it is placed in a rotary evaporator to remove the solvent, and the silicon-nitrogen-based acrylate flame retardant monomer B is obtained.

[0016] The structural formula of the flame retardant monomer B is:

[0017]

[0018] Preferably, in the preparation method of the flame retardant monomer B, the molar ratio of γ-chloropropyltriethoxysilane, dimethylaminoethyl methacrylate, and potassium iodide is 1.3:1:1.3.

[0019] Preferably, in the preparation method of the flame retardant monomer B, the dosage of the inhibitor 1,4-benzenediol is 1 wt% of the monomer dosage.

[0020] Preferably, the initiator is at least one of potassium persulfate and azodiisobutyramidine hydrochloride.

[0021] Preferably, the penetrant in step (3) is at least one of penetrant JFC and Peregal O.

[0022] The present invention provides a phosphorus-nitrogen-silicon-based flame-retardant polyester-cotton blended fabric prepared by the preparation method described in the above technical solution, including the synthesis of acrylate-based cationic flame-retardant monomers and the flame-retardant finishing of polyester-cotton blended flame-retardant fabrics.

[0023] The preparation method of the phosphorus-nitrogen-silicon-based flame-retardant polyester-cotton blended fabric of the present invention impregnates and rolls a polyester-cotton blended fabric with a flame-retardant finishing solution of a phosphorus-nitrogen-silicon-based flame-retardant monomer containing a C═C bond, and reacts and fixes on the fabric surface through high temperature, endowing the fabric with good flame-retardant effect; the flame-retardant finishing solution realizes the fixation on the surface of the polyester-cotton fabric through the methods of impregnation deposition and in-situ polymerization, so that the fabric obtains a durable flame-retardant effect and has good practical value. Description of the drawings:

[0024] Figure 1 It is the infrared spectrum of flame-retardant monomer A.

[0025] Figure 2 It is the infrared spectrum of flame-retardant monomer B. Detailed implementation manners

[0026] The present invention will be further described below through examples. The examples are only used to explain the present invention, but do not constitute any limitation to the claims of the present invention.

[0027] The flame-retardant monomers A and B in the following examples are prepared by the following steps respectively.

[0028] Using phosphorus oxychloride (26 mmol) as a raw material, dissolving it in chloroform (100 mL), keeping the reaction temperature at 35 °C, slowly adding neopentyl glycol (26 mmol) and reacting for 4 h, then heating to 45 °C and stirring for 1 h, and then heating to 60 °C and stirring for 1 h. After the above reaction is completed, the obtained solution is placed in a rotary evaporator to evaporate the solvent, thereby obtaining the intermediate 2-oxo-2-chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane. The purified intermediate product and dimethylaminoethyl methacrylate (20 mmol) are dissolved in N,N-dimethylformamide, and after introducing nitrogen, the reaction is carried out at 80 °C for 24 h under the action of potassium iodide (26 mmol) and 1,4-benzenediol. After the reaction is completed, the solution is filtered and purified. Then it is placed in a rotary evaporator again to evaporate the solvent to obtain the phosphorus-nitrogen-based acrylate flame-retardant monomer A, and its synthesis process is as follows.

[0029]

[0030] Weigh 26 mmol of γ-chloropropyltriethoxysilane and 20 mmol of dimethylaminoethyl methacrylate. After adding them to N,N-dimethylformamide (100 mL) and fully dissolving, pass nitrogen gas, and then react at 80 °C for 24 h under the action of potassium iodide (26 mmol) and 1,4-benzenediol. After the reaction, filter the solution by suction and purify it. Then place it in a rotary evaporator to remove the solvent to obtain the silicon-nitrogen-based acrylate flame retardant monomer B. The synthesis process is as follows.

[0031]

[0032] Example 1

[0033] A preparation method of a phosphorus-nitrogen-silicon-based flame retardant polyester-cotton blended fabric, comprising the following steps:

[0034] Weigh a certain amount of water, flame retardant monomer A, flame retardant monomer B, potassium persulfate and penetrant JFC to prepare a flame retardant finishing solution. Among them, the concentration of flame retardant monomer A is 300 g / L, the concentration of flame retardant monomer B is 200 g / L, the concentration of penetrant JFC is 5 g / L, and potassium persulfate is 1 wt% (1 wt% of the total amount of flame retardant monomer A and flame retardant monomer B);

[0035] Immerse the polyester-cotton fabric in the finishing solution for 30 min;

[0036] Transfer it to pre-bake at 60 °C for 30 min, and then bake at 170 °C for 1 min to obtain the phosphorus-nitrogen-silicon-based flame retardant polyester-cotton blended fabric.

[0037] Example 2

[0038] A preparation method of a phosphorus-nitrogen-silicon-based flame retardant polyester-cotton blended fabric, comprising the following steps:

[0039] Weigh a certain amount of water, flame retardant monomer A, flame retardant monomer B, potassium persulfate and penetrant JFC to prepare a flame retardant finishing solution. Among them, the concentration of flame retardant monomer A is 300 g / L, the concentration of flame retardant monomer B is 200 g / L, and the concentration of penetrant JFC is 8 g / L;

[0040] Immerse the polyester-cotton fabric in the finishing solution for 30 min;

[0041] Transfer it to pre-bake at 60 °C for 30 min, and then bake at 170 °C for 2 min to obtain the phosphorus-nitrogen-silicon-based flame retardant polyester-cotton blended fabric.

[0042] Example 3

[0043] A preparation method of a phosphorus-nitrogen-silicon-based flame retardant polyester-cotton blended fabric, comprising the following steps:

[0044] Weigh a certain amount of water, flame retardant monomer A, flame retardant monomer B, potassium persulfate and Peregal O to prepare a flame retardant finishing solution. Among them, the concentration of flame retardant monomer A is 400 g / L, the concentration of flame retardant monomer B is 100 g / L, and the concentration of Peregal O is 8 g / L;

[0045] Immerse the polyester-cotton fabric in the finishing solution for 20 min;

[0046] Transfer it to pre-bake at 80 °C for 20 min and then cure at 160 °C for 3 min to obtain a phosphorus-nitrogen-silicon-based flame retardant polyester-cotton blended fabric.

[0047] Example 4

[0048] A preparation method of a phosphorus-nitrogen-silicon-based flame retardant polyester-cotton blended fabric includes the following steps:

[0049] Weigh a certain amount of water, flame retardant monomer A, flame retardant monomer B, 2,2'-azobis(2-methylpropionamidine) dihydrochloride and penetrant JFC to prepare a flame retardant finishing solution. Among them, the concentration of flame retardant monomer A is 400 g / L, the concentration of flame retardant monomer B is 200 g / L, and the concentration of penetrant JFC is 5 g / L;

[0050] Immerse the polyester-cotton fabric in the finishing solution for 20 min;

[0051] Transfer it to pre-bake at 80 °C for 20 min and then cure at 160 °C for 3 min to obtain a phosphorus-nitrogen-silicon-based flame retardant polyester-cotton blended fabric.

[0052] Example 5

[0053] A preparation method of a phosphorus-nitrogen-silicon-based flame retardant polyester-cotton blended fabric includes the following steps:

[0054] Weigh a certain amount of water, flame retardant monomer A, flame retardant monomer B, 2,2'-azobis(2-methylpropionamidine) dihydrochloride and Peregal O to prepare a flame retardant finishing solution. Among them, the concentration of flame retardant monomer A is 500 g / L, the concentration of flame retardant monomer B is 300 g / L, and the concentration of Peregal O is 10 g / L;

[0055] Immerse the polyester-cotton fabric in the finishing solution for 10 min;

[0056] Transfer it to pre-bake at 90 °C for 10 min and then cure at 140 °C for 5 min to obtain a phosphorus-nitrogen-silicon-based flame retardant polyester-cotton blended fabric.

[0057] Test the flame retardant performance of the polyester-cotton blended fabric in the examples according to GB / T 5455-1997 "Textiles - Burning performance - Vertical test method", and the results are shown in the following table.

[0058] Table 1 Flame retardant performance of the polyester-cotton blended fabric in the examples

[0059] Length of damaged carbon / mm Afterflame time / s Smoldering time / s Example 1 146 1.9 0 Example 2 124 0.7 0 Example 3 97 0 0 Example 4 85 0 0 Example 5 63 0 0

[0060] As can be seen from the test data in Table 1, for the method of preparing the flame-retardant polyester-cotton blended fabric according to the embodiments, the phosphorus-nitrogen-silicon-based flame-retardant monomer of the present invention is used for the flame-retardant finishing of the polyester-cotton blended fabric, which can endow the fabric with good and durable flame-retardant effects and has good practical application prospects.

[0061] The above are only the preferred embodiments of the present invention. It should be pointed out that for those of ordinary skill in the art, without departing from the principle of the present invention, several improvements and refinements can still be made, and these improvements and refinements should also be regarded as the protection scope of the present invention.

Claims

1. A preparation method of a phosphorus, nitrogen and silicon-based flame-retardant polyester-cotton blended fabric, comprising the following steps: Weigh a certain amount of flame-retardant monomer A, flame-retardant monomer B, initiator, penetrant and water to prepare a flame-retardant finishing solution; Immerse the polyester-cotton fabric in the flame-retardant finishing solution for 10 - 30 min; Transfer the fabric to pre-bake at 60 - 90 °C for 10 - 30 min, and then cure at 140 - 170 °C for 1 - 5 min to obtain the phosphorus, nitrogen and silicon-based flame-retardant polyester-cotton blended fabric; The structural formula of flame-retardant monomer A is: The structural formula of flame-retardant monomer B is: The flame-retardant finishing solution contains 300 - 500 g / L of flame-retardant monomer A, 100 - 300 g / L of flame-retardant monomer B, 1 wt% of initiator (1 wt% of the total amount of flame-retardant monomer A and flame-retardant monomer B), 5 - 10 g / L of penetrant, and the balance is water.

2. The preparation method of a phosphorus, nitrogen and silicon-based flame retardant polyester-cotton blended fabric according to claim 1, characterized in that: For the said flame-retardant monomer A, the preparation method is: Using phosphorus oxychloride as the raw material, dissolve it in chloroform, keep the reaction temperature at 35 °C, slowly add neopentyl glycol and keep the reaction for 4 h, then raise the temperature to 45 °C and stir for 1 h, and then raise the temperature to 60 °C and stir for 1 h; After the above reaction is completed, place the obtained solution in a rotary evaporator to evaporate the solvent, thus obtaining the intermediate 2-oxo-2-chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane; Dissolve the purified intermediate product and dimethylaminoethyl methacrylate in N,N-dimethylformamide, introduce nitrogen, and react at 80 °C for 24 h under the action of potassium iodide and the inhibitor 1,4-benzenediol; After the reaction is completed, filter the solution and carry out purification treatment; Then place it in a rotary evaporator again to evaporate the solvent to obtain the phosphorus and nitrogen-based acrylate flame-retardant monomer A.

3. The preparation method of a phosphorus-nitrogen-silicon-based flame-retardant polyester-cotton blended fabric according to claim 2, characterized in that: In the preparation method of flame-retardant monomer A, the molar ratio of phosphorus oxychloride, neopentyl glycol, dimethylaminoethyl methacrylate and potassium iodide is 1.3:1.3:1:1.

3.

4. The preparation method of a phosphorus, nitrogen and silicon-based flame retardant polyester-cotton blended fabric according to claim 2, characterized in that: In the preparation method of the said flame-retardant monomer A, the dosage of the inhibitor 1,4-benzenediol is 1 wt% of the monomer dosage.

5. The preparation method of a phosphorus, nitrogen and silicon-based flame retardant polyester-cotton blended fabric according to claim 1, characterized in that: For the said flame-retardant monomer B, the preparation method is: Weigh a certain mass of γ-chloropropyltriethoxysilane and dimethylaminoethyl methacrylate, add N,N-dimethylformamide and dissolve it fully, introduce nitrogen, and react at 80 °C for 24 h under the action of potassium iodide and the inhibitor 1,4-benzenediol; After the reaction is completed, filter the solution and carry out purification treatment; Then place it in a rotary evaporator to evaporate the solvent to obtain the silicon and nitrogen-based acrylate flame-retardant monomer B.

6. The preparation method of a phosphorus, nitrogen and silicon-based flame retardant polyester-cotton blended fabric according to claim 5, characterized in that: In the preparation method of flame-retardant monomer B, the molar ratio of γ-chloropropyltriethoxysilane, dimethylaminoethyl methacrylate and potassium iodide is 1.3:1:1.

3.

7. The preparation method of a phosphorus-nitrogen-silicon-based flame-retardant polyester-cotton blended fabric according to claim 5, characterized in that: In the preparation method of flame-retardant monomer B, the dosage of the inhibitor 1,4-benzenediol is 1 wt% of the monomer dosage.

8. The preparation method of a phosphorus-nitrogen-silicon-based flame-retardant polyester-cotton blended fabric according to claim 1, wherein: The said initiator is at least one of potassium persulfate and azobisisobutyramidine hydrochloride.

9. The preparation method of a phosphorus, nitrogen and silicon-based flame retardant polyester-cotton blended fabric according to claim 1, characterized in that: The penetrant is at least one of penetrant JFC and Peregal O.

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