Quaternary phosphonium salt polymer special for polyester water-based slurry and preparation method of quaternary phosphonium salt polymer

Abstract

The preparation method comprises the following steps: adding a soluble polyester hot melt adhesive into trioxymethylene and trichloromethane, stirring and dissolving, then adding trimethylchlorosilane, placing in an ice-water bath, stirring, then adding a tin tetrachloride-trichloromethane solution, stirring for 0.5 h, then adding a sodium hydroxide solution, stirring for 0.5 h, adding a sodium hydroxide solution, stirring for 0.5 h, adding a sodium hydroxide solution, stirring for 0.5 h, and cooling to room temperature to obtain the quaternary phosphonium salt polymer special for the terylene water-based slurry. And heating to 30-50 DEG C, continuously reacting for 1-2 hours, finally adding a small amount of methanol / water mixed solution, and carrying out vacuum concentration and room-temperature vacuum drying for 24 hours to obtain the chloromethylated soluble polyester hot melt adhesive. The preparation method comprises the following steps: dissolving a chloromethylated soluble polyester hot melt adhesive and a phenylphosphine compound in a first solvent, reacting at 50-100 DEG C for 8-12 hours, precipitating with diethyl ether, and carrying out vacuum drying for 12 hours to obtain quaternary phosphonium salt polymer slurry; compared with the traditional slurry, the quaternary phosphonium salt polymer slurry obtained by the invention has the advantages of excellent bonding force, wear resistance and the like, and can be applied to polyester fiber sizing.

Description

Technical Field

[0001] The present invention relates to the field of polyester slurry, in particular to a quaternary phosphonium salt polymer dedicated to polyester aqueous slurry and a preparation method thereof Background Art

[0002] The main uses of polyester fabrics include clothing fabrics, home decoration and outdoor products. Polyester fabrics are very suitable for making clothing fabrics, such as coats, shirts, pants, etc., due to their excellent wrinkle resistance and shape retention. However, during the weaving process of polyester textiles, the warp yarns are subjected to multiple stretching, bending and friction, which can easily cause fiber splitting and fluffing, and in severe cases, breakage. Sizing can form a layer of sizing on the fiber surface to protect the fiber from damage and prevent pilling. The main function of sizing is to make the fibers cohesive, enhance the bonding force between fibers, prevent the fibers from separating or sliding during the weaving process, and thus improve the stability and strength of the fabric.

[0003] Usually polyester cannot be dissolved in solvents, which makes modification difficult. However, low molecular weight soluble polyester hot melt adhesive can still be dissolved in organic solvents. In order to improve the water solubility of soluble polyester hot melt adhesive so that it can be used in polyester special slurry, the soluble polyester hot melt adhesive is chloromethylated to a certain extent and then reacted with phenylphosphine compounds to generate an aqueous polymer slurry with a quaternary phosphonium salt structure. This aqueous polymer slurry is easy to size polyester and has good adhesion, which improves the bonding force between polyesters and plays a good role in preventing pilling. And quaternary phosphonium salts have certain antibacterial ability, which can effectively reduce biological infection in the slurry pool.

[0004] The invention discloses a quaternary phosphonium salt polymer for polyester water-based slurry and a preparation method thereof. A soluble polyester hot melt adhesive is added to trioxymethylene and chloroform, stirred and dissolved, then trimethylsilyl chloride is added, placed in an ice-water bath and stirred, then a tin tetrachloride-chloroform solution is added, stirred for 0.5 hours, heated to 30-50°C and continued to react for 1-2 hours, and finally a small amount of methanol / water mixed solution is added, concentrated under reduced pressure, and vacuum dried at room temperature for 24 hours to obtain a chloromethylated soluble polyester hot melt adhesive; then the chloromethylated soluble polyester hot melt adhesive and a phenylphosphine compound are dissolved in a first solvent, reacted at 50-100°C for 8-12 hours, precipitated by ether, and vacuum dried for 12 hours to obtain a quaternary phosphonium salt polymer slurry. The water-based polymer slurry obtained by the invention has the advantages of excellent adhesion, wear resistance, etc. compared with traditional slurry. Summary of the invention

[0005] The purpose of the present invention is to provide a quaternary phosphonium salt polymer special for polyester aqueous slurry and a preparation method thereof.

[0006] In order to achieve the above objectives, the following technical solutions are provided: A quaternary phosphonium salt polymer for polyester aqueous slurry and a preparation method thereof comprises the following steps: (1) Add 0.001 mol of soluble polyester hot melt adhesive to 5-8 g of trioxymethylene and 100-200 mL of chloroform and stir to dissolve, then add 25-50 mL of trimethylsilyl chloride, place in an ice-water bath and stir, then add 50-80 mL of tin tetrachloride-chloroform solution, stir for 0.5 h, heat to 30-50 ° C and continue to react for 1-2 h, finally add a small amount of methanol / water mixed solution, concentrate under reduced pressure, and vacuum dry at room temperature for 24 h to obtain chloromethylated soluble polyester hot melt adhesive.

[0007] (2) The product of (1) and 0.001-0.01 mole of a phenylphosphine compound are dissolved in 10 mL of a first solvent, reacted at 50-100° C. for 8-12 h, precipitated with 100 mL of ether, and vacuum dried for 12 h to obtain a quaternary phosphonium salt polymer slurry.

[0008] Preferably, the quaternary phosphonium salt polymer dedicated to polyester aqueous slurry and the preparation method thereof are characterized in that the phenyl phosphine compound is triphenyl phosphine, ethyl diphenyl phosphine, diphenyl propyl phosphine, etc., but is not limited thereto.

[0009] Preferably, the quaternary phosphonium salt polymer dedicated to polyester aqueous slurry and the preparation method thereof are characterized in that the first solvent is N,N-dimethylformamide, N,N-dimethylacetamide, dimethyl sulfoxide, etc., but is not limited thereto.

[0010] The beneficial effect of the present invention is that the soluble polyester hot melt adhesive having high bonding strength, good heat resistance and cold resistance is chloromethylated and then reacted with a phenylphosphine compound to generate an aqueous polymer slurry with a quaternary phosphonium salt structure, which is easy to size polyester, improves the bonding force between polyesters, and plays a good role in preventing pilling. In addition, the quaternary phosphonium salt has a certain antibacterial ability and can effectively reduce the biological infection of the slurry pool. BRIEF DESCRIPTION OF THE DRAWINGS

[0011] Figure 1 A quaternary phosphonium salt polymer specially used for polyester aqueous slurry and a preparation method thereof. The hydrogen nuclear magnetic resonance spectrum of the product (1) in Example 1; Figure 2 This is a test table of the adhesion performance of Examples 1-6. Specific implementation methods The principle of the invention is that the soluble polyester hot melt adhesive is chloromethylated and reacted with a phenylphosphine compound to generate an aqueous polymer slurry with a quaternary phosphonium salt structure. The soluble polyester hot melt adhesive improves the bonding force between polyester fibers, and the quaternary phosphonium salt structure improves the water solubility, which has a good effect on preventing pilling of polyester fibers.

[0013] The present invention will be further described below with reference to the accompanying drawings and embodiments, and the purpose and effects of the present invention will become more apparent.

[0014] Embodiment 1: (1) Add 0.001 mol of soluble polyester hot melt adhesive to 5 g of trioxymethylene and 100 mL of chloroform and stir to dissolve. Then add 25 mL of trimethylsilyl chloride and stir in an ice-water bath. Then add 50 mL of tin tetrachloride-chloroform solution and stir for 0.5 h. Then heat to 30 °C and continue to react for 2 h. Finally, add a small amount of methanol / water mixed solution, concentrate under reduced pressure, and dry in vacuum at room temperature for 24 h to obtain chloromethylated soluble polyester hot melt adhesive.

[0015] (2) The product of (1) and 0.001 mol of triphenylphosphine were dissolved in 10 mL of N,N-dimethylformamide, reacted at 50° C. for 12 h, precipitated with 100 mL of ether and dried in vacuum for 12 h to obtain a quaternary phosphonium salt polymer slurry.

[0016] Embodiment 2: (1) 0.001 mol of soluble polyester hot melt adhesive was added to 8 g of trioxymethylene and 200 mL of chloroform and stirred to dissolve. Then, 50 mL of trimethylsilyl chloride was added and stirred in an ice-water bath. Then, 80 mL of tin tetrachloride-chloroform solution was added and stirred for 0.5 h. The mixture was heated to 50 °C and the reaction was continued for 1 h. Finally, a small amount of methanol / water mixed solution was added and the mixture was concentrated under reduced pressure and dried in vacuum at room temperature for 24 h to obtain chloromethylated soluble polyester hot melt adhesive.

[0017] (2) The product of (1) and 0.01 mol of ethyldiphenylphosphine were dissolved in 10 mL of N,N-dimethylacetamide, reacted at 100° C. for 8 h, precipitated with 100 mL of ether and dried in vacuum for 12 h to obtain a quaternary phosphonium salt polymer slurry.

[0018] Embodiment 3: (1) Add 0.001 mol of soluble polyester hot melt adhesive to 5 g of trioxymethylene and 100 mL of chloroform and stir to dissolve. Then add 25 mL of trimethylsilyl chloride and stir in an ice-water bath. Then add 50 mL of tin tetrachloride-chloroform solution and stir for 0.5 h. Then heat to 30 °C and continue to react for 2 h. Finally, add a small amount of methanol / water mixed solution, concentrate under reduced pressure, and dry in vacuum at room temperature for 24 h to obtain chloromethylated soluble polyester hot melt adhesive.

[0019] (2) The product of (1) and 0.001 mol of diphenylpropylphosphine were dissolved in 10 mL of dimethyl sulfoxide, reacted at 50° C. for 12 h, precipitated with 100 mL of ether and dried in vacuum for 12 h to obtain a quaternary phosphonium salt polymer slurry.

[0020] Embodiment 4: (1) 0.001 mol of soluble polyester hot melt adhesive was added to 8 g of trioxymethylene and 200 mL of chloroform and stirred to dissolve. Then, 50 mL of trimethylsilyl chloride was added and stirred in an ice-water bath. Then, 80 mL of tin tetrachloride-chloroform solution was added and stirred for 0.5 h. The mixture was heated to 50 °C and the reaction was continued for 1 h. Finally, a small amount of methanol / water mixed solution was added and the mixture was concentrated under reduced pressure and dried in vacuum at room temperature for 24 h to obtain chloromethylated soluble polyester hot melt adhesive.

[0021] (2) The product of (1) and 0.001 mol of triphenylphosphine were dissolved in 10 mL of N,N-dimethylformamide, reacted at 100° C. for 8 h, precipitated with 100 mL of ether and dried in vacuum for 12 h to obtain a quaternary phosphonium salt polymer slurry.

[0022] Embodiment 5: (1) Add 0.001 mol of soluble polyester hot melt adhesive to 8 g of trioxymethylene and 200 mL of chloroform and stir to dissolve. Then add 50 mL of trimethylsilyl chloride and stir in an ice-water bath. Then add 80 mL of tin tetrachloride-chloroform solution and stir for 0.5 h. Then heat to 30 °C and continue to react for 2 h. Finally, add a small amount of methanol / water mixed solution, concentrate under reduced pressure, and dry in vacuum at room temperature for 24 h to obtain chloromethylated soluble polyester hot melt adhesive.

[0023] (2) The product of (1) and 0.01 mol of ethyldiphenylphosphine were dissolved in 10 mL of N,N-dimethylacetamide, reacted at 50° C. for 12 h, precipitated with 100 mL of ether and dried in vacuum for 12 h to obtain a quaternary phosphonium salt polymer slurry.

[0024] Embodiment 6: (1) Add 0.001 mol of soluble polyester hot melt adhesive to 5 g of trioxymethylene and 100 mL of chloroform and stir to dissolve. Then add 25 mL of trimethylsilyl chloride and stir in an ice-water bath. Then add 50 mL of tin tetrachloride-chloroform solution and stir for 0.5 h. Then heat to 50 °C and continue to react for 1 h. Finally, add a small amount of methanol / water mixed solution, concentrate under reduced pressure, and dry in vacuum at room temperature for 24 h to obtain chloromethylated soluble polyester hot melt adhesive.

[0025] (2) The product of (1) and 0.001 mol of diphenylpropylphosphine were dissolved in 10 mL of dimethyl sulfoxide, reacted at 100° C. for 8 h, precipitated with 100 mL of ether and dried in vacuum for 12 h to obtain a quaternary phosphonium salt polymer slurry.

Claims

1. A quaternary phosphonium salt polymer for polyester aqueous slurry and a preparation method thereof, characterized in that: The following steps are involved: (1) Add 0.001 mole of soluble polyester hot melt adhesive to 5-8g of trioxymethylene and 100-200mL of chloroform, stir and dissolve, then add 25-50mL of trimethylsilyl chloride, place in an ice water bath and stir, then add 50-80mL of tin tetrachloride-chloroform solution, stir for 0.5h, heat to 30-50°C and continue to react for 1-2h, finally add a small amount of methanol / water mixed solution, concentrate under reduced pressure, and vacuum dry at room temperature for 24h to obtain chloromethylated soluble polyester hot melt adhesive; (2) The product of (1) and 0.001-0.01 mole of a phenylphosphine compound are dissolved in 10 mL of a first solvent, reacted at 50-100° C. for 8-12 h, precipitated with 100 mL of ether, and vacuum dried for 12 h to obtain a quaternary phosphonium salt polymer slurry.

2. A quaternary phosphonium salt polymer for polyester aqueous slurry and a preparation method thereof according to claim 1, characterized in that: The phenylphosphine compounds are triphenylphosphine, ethyldiphenylphosphine, diphenylpropylphosphine and the like.

3. A quaternary phosphonium salt polymer for polyester aqueous slurry and a preparation method thereof according to claim 1, characterized in that: The first solvent is N,N-dimethylformamide, N,N-dimethylacetamide, dimethyl sulfoxide, etc.

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