Disclosure of Invention
The technical problems to be solved by the invention are as follows: aiming at the problems that winding and broken ends occur due to poor antistatic performance of the existing spinning oil and the fabric is easy to yellow due to easy oxidation of the oil agent, the antioxidant antistatic spinning oil is provided.
In order to solve the technical problems, the invention adopts the following technical scheme:
an antioxidant antistatic spinning oil comprises the following components of 100-150 parts of a spinning oil base material, 1-3 parts of polyoxyethylene laurate, 1-3 parts of polyethylene glycol oleate, 5-15 parts of an antistatic active agent, 3-9 parts of a spinning oil smoothing active agent and 2-5 parts of an oil antioxidant active agent;
the preparation method of the antistatic active agent comprises the following steps: taking phosphorus oxychloride according to a mass ratio of 3-6: 1-5: 10-20, adding propyl trichlorosilane and an alcohol additive, stirring and mixing at 40-50 ℃ to obtain a mixture a, and mixing the mixture a according to a mass ratio of 3-7: 10-20, adding diethylene glycol dimethyl ether, stirring and mixing at 100-110 ℃, cooling to room temperature to obtain a cooling material, and taking the cooling material according to a mass ratio of 2-5: 10-15, adding absolute ethyl alcohol, standing, distilling the precipitate under reduced pressure, and drying to obtain the antistatic active agent.
The preparation method of the alcohol additive comprises the following steps: taking active raw materials according to a mass ratio of 2-6: 5-8: adding 50-70 parts of n-decyl glycidyl ether and deionized water, adding a catalyst accounting for 5-10% of the mass of the active raw materials, stirring and mixing, introducing hydrogen for reaction, keeping the reaction at the temperature of 150-200 ℃ under 8MPa for 4-7 hours, cooling to room temperature, filtering, and taking the filtrate to obtain the alcohol additive.
The active raw materials are as follows: mixing one or more of sorbitol, fructose, mannitol, galacto-oligosaccharide, maltose and lactose at any mass ratio.
The preparation method of the catalyst comprises the following steps: according to the mass parts, 10-15 parts of cerium nitrate, 3-7 parts of cobalt nitrate, 5-9 parts of gallium nitrate and 80-100 parts of deionized water are stirred and mixed at 40-50 ℃ to obtain a mixture, and the mixture is taken according to the mass ratio of 20-50: and 3-5, adding tartaric acid, heating to 70-80 ℃, stirring and mixing, adding ethylene glycol accounting for 20-30% of the weight of the tartaric acid, stirring and mixing at 80-90 ℃, performing suction filtration, drying suction filtration residues, calcining at 600-700 ℃, and cooling to room temperature to obtain the catalyst.
The preparation method of the spinning oil smoothing active agent comprises the following steps: taking an initial active agent according to the mass ratio of 5-9: 1-4, adding pyridine, introducing nitrogen for dehydration for 20-30 min to obtain a dehydrate, and taking propylene oxide according to a mass ratio of 3-7: 2-5, adding butylene oxide, adding dehydrate accounting for 2-9% of the mass of propylene oxide, introducing nitrogen for protection, heating to 120-130 ℃, preserving heat, cooling to room temperature to obtain a cooling object a, and taking the cooling object a according to the mass ratio of 40-50: and 2-5, adding oxalic acid, mixing, decoloring by using active carbon, filtering, and taking the filtrate to obtain the spinning oil smoothing activator.
The starting active agents are: mixing 5-10 parts of myristamine, 3-7 parts of lauric acid, 1-4 parts of octyldodecanol, 20-40 parts of propylene glycol and 1-3 parts of nonyl phenol according to parts by weight.
The preparation method of the oil antioxidant active agent comprises the following steps: according to the mass parts, 20-30 parts of nuclear molecule active agent, 5-8 parts of triethylamine, 1-4 parts of 4-dimethylpyridine and 40-60 parts of N, N-dimethylformamide are stirred and mixed at 20-25 ℃ to obtain a stirring mixture, and the stirring mixture is taken according to the mass ratio of 40-50: 5-9, adding an antioxidant raw material, stirring and mixing at 0-4 ℃, stirring and mixing at 20-25 ℃, and distilling under reduced pressure to obtain the antioxidant active agent of the oil.
The preparation method of the nuclear molecule active agent comprises the following steps: taking 1, 4-butanediamine according to a mass ratio of 2-5: 10-20 adding methanol, then adding methyl acrylate accounting for 20-30% of the mass of the methanol, stirring and mixing at 20-25 ℃, carrying out reduced pressure distillation to obtain a reduced pressure distillate, and taking the reduced pressure distillate according to the mass ratio of 2-6: and (3) adding methanol into the mixture 10-15, adding 1, 4-butanediamine with the mass 2-4 times that of the methanol, stirring and mixing the mixture at the temperature of 20-25 ℃, and distilling the mixture under reduced pressure to obtain the nuclear molecule active agent.
The preparation method of the antioxidant raw material comprises the following steps: taking beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid according to a mass ratio of 2-5: adding 10-20 parts of N, N-dimethylformamide, stirring and mixing at 30-40 ℃, adding 10-15% by mass of benzoyl chloride of the N, N-dimethylformamide, introducing nitrogen for protection, stirring and mixing at 30-40 ℃, and distilling under reduced pressure to obtain the antioxidant raw material.
The spinning oil base material comprises: according to the mass parts, 5-10 parts of mineral oil, 1-3 parts of amino silicone oil, 2-5 parts of castor oil and 5-10 parts of chemical fiber oil are mixed to obtain the oil.
Compared with other methods, the method has the beneficial technical effects that:
(1) the antistatic active agent prepared by the invention takes an alcohol additive as a main raw material, mainly uses acid complex gallium which is carried out by cerium nitrate, cobalt nitrate, gallium nitrate and the like as an active component to absorb CO molecules in a non-dissociative way, has the functions of CO insertion and C-C chain growth, ensures that cobalt ions and gallium ions in a crystal lattice structure of perovskite can be uniformly dispersed at the atomic level in the catalytic process, has better catalytic activity, carries out catalytic hydrogenation on fructose, mannitol, galacto-oligosaccharide and the like to improve alcohol conversion, takes the polyhydroxy compound as the raw material to introduce polyhydroxy compound, and adds n-decyl glycidyl ether to carry out dissociation of the alcohol active agent to obtain alcohol anions under the alkali catalytic condition to attack an epoxy compound to carry out ring opening to generate an alcohol ether compound, on the one hand, introduces double flame-retardant elements of silicon and phosphorus into spinning oil to form flame-retardant protection on the surface of fibers after the spinning oil is oiled, on the other hand, phosphorus trichloride and an alcohol ether compound are subjected to phosphorylation reaction, and oxygen anions in the obtained product have good hygroscopicity and hydrophilicity, so that charges generated on the surface of the fiber can be better dissipated, and the antistatic effect is improved;
(2) the spinning oil smoothing activator prepared by the invention takes myristamine, lauric acid and the like as the raw materials of the initiator, propylene oxide, butylene oxide and the like are added for reaction, the propylene oxide chain link is introduced to improve the heat resistance of the spinning oil, the initiator with short carbon chain is introduced to reduce the decomposition residue of the spinning oil, so that the coking phenomenon on the spinning surface is greatly reduced, thereby improving the phenomena of broken filaments and broken filaments of the fiber, on the other hand, introducing the starting agent raw material with larger viscosity, so that the steric hindrance between molecules of the smoothing active agent is reduced, the mutual entanglement between flexible macromolecular chains is increased, the cohesive force and the wear resistance of an oil film formed when the spinning oil is used are improved by improving the viscosity of the spinning oil, the spinning oil is well adhered to fibers, and the surface tension when the spinning oil is spread is reduced by chain link arrangement of a polyether molecular chain, so that the spinning oil is tightly arranged to form a continuous oil film for spinning protection;
(3) the antioxidant raw material prepared by the invention is prepared by taking beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid as a raw material, adding benzoyl chloride for acyl chlorination reaction, adding a nuclear molecule formed by 1, 4-butanediamine and methyl acrylate as a skeleton structure of a grafted antioxidant active agent, and carrying out amidation condensation reaction on an obtained acyl chloride product and a terminal amino group of the skeleton, on one hand, hindered phenol and tertiary amine active groups with free radical scavenging function are introduced into spinning oil to play a long-acting protection on the antioxidant performance of an oil base, on the other hand, the introduced amido bond has better polarity and stability, the antioxidant active agent is connected to keep antioxidant stability in the heating process of the spinning oil, and the antioxidant is uniformly dispersed in the oil agent by using a branched chain structure of the skeleton structure, improving the performance of the spinning oil.
Detailed Description
The preparation method of the catalyst comprises the following steps: taking 10-15 parts of cerium nitrate, 3-7 parts of cobalt nitrate, 5-9 parts of gallium nitrate and 80-100 parts of deionized water by weight, stirring and mixing at 40-50 ℃ for 20-40 min to obtain a mixture, and taking the mixture according to the mass ratio of 20-50: 3-5, adding tartaric acid, heating to 70-80 ℃, stirring and mixing for 30-60 min, adding ethylene glycol with the mass of 20-30% of that of the tartaric acid, stirring and mixing for 3-6 h at 80-90 ℃, performing suction filtration, drying suction filtration residues, calcining for 3-5 h at 600-700 ℃, and cooling to room temperature to obtain the catalyst.
The active raw materials are as follows: mixing one or more of sorbitol, fructose, mannitol, galacto-oligosaccharide, maltose and lactose at any mass ratio.
The preparation method of the alcohol additive comprises the following steps: taking active raw materials according to a mass ratio of 2-6: 5-8: adding 50-70 parts of n-decyl glycidyl ether and deionized water, adding a catalyst accounting for 5-10% of the mass of the active raw material, stirring and mixing at 800r/min for 20-40 min, introducing hydrogen for reaction, keeping at 150-200 ℃ for 4-7 h under 8MPa, cooling to room temperature, filtering, and taking the filtrate to obtain the alcohol additive.
The preparation method of the antistatic active agent comprises the following steps: taking phosphorus oxychloride according to a mass ratio of 3-6: 1-5: 10-20, adding propyl trichlorosilane and an alcohol additive, stirring and mixing at 40-50 ℃ for 1-3 hours to obtain a mixture a, and mixing the mixture a according to a mass ratio of 3-7: 10-20, adding diethylene glycol dimethyl ether, stirring and mixing at 100-110 ℃ for 3-5 h, cooling to room temperature to obtain a cooling material, and taking the cooling material according to a mass ratio of 2-5: 10-15, adding absolute ethyl alcohol, standing for 30-50 min, distilling the precipitate under reduced pressure, and drying to obtain the antistatic active agent.
The starting active agents were: mixing 5-10 parts of myristamine, 3-7 parts of lauric acid, 1-4 parts of octyldodecanol, 20-40 parts of propylene glycol and 1-3 parts of nonyl phenol according to parts by weight.
The preparation method of the spinning oil smoothing active agent comprises the following steps: taking an initial active agent according to the mass ratio of 5-9: 1-4, adding pyridine, introducing nitrogen for dehydration for 20-30 min to obtain a dehydrate, and taking propylene oxide according to a mass ratio of 3-7: 2-5, adding butylene oxide, adding dehydrate accounting for 2-9% of the mass of propylene oxide, introducing nitrogen for protection, heating to 120-130 ℃, preserving heat for 20-30 min, cooling to room temperature to obtain a cooling object a, and taking the cooling object a according to the mass ratio of 40-50: and 2-5, adding oxalic acid, mixing, decoloring by using active carbon, filtering, and taking the filtrate to obtain the spinning oil smoothing activator.
The preparation method of the nuclear molecule active agent comprises the following steps: taking 1, 4-butanediamine according to a mass ratio of 2-5: 10-20 adding methanol, then adding methyl acrylate accounting for 20-30% of the mass of the methanol, stirring and mixing at 20-25 ℃ for 18-24 h, carrying out reduced pressure distillation to obtain a reduced pressure distillate, and taking the reduced pressure distillate according to the mass ratio of 2-6: and (2) adding methanol into the mixture 10-15, adding 1, 4-butanediamine with the mass 2-4 times that of the methanol, stirring and mixing the mixture at the temperature of 20-25 ℃ for 20-24 hours, and distilling the mixture under reduced pressure to obtain the nuclear molecule active agent.
The preparation method of the antioxidant raw material comprises the following steps: taking beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid according to a mass ratio of 2-5: adding N, N-dimethylformamide into the mixture 10-20, stirring and mixing the mixture at the temperature of 30-40 ℃ for 20-40 min, adding benzoyl chloride accounting for 10-15% of the mass of the N, N-dimethylformamide, introducing nitrogen for protection, stirring and mixing the mixture at the temperature of 30-40 ℃ for 3-7 h, and distilling the mixture under reduced pressure to obtain the antioxidant raw material.
The preparation method of the oil antioxidant active agent comprises the following steps: according to the mass parts, 20-30 parts of nuclear molecule active agent, 5-8 parts of triethylamine, 1-4 parts of 4-lutidine and 40-60 parts of N, N-dimethylformamide are stirred and mixed for 40-50 min at 20-25 ℃ to obtain a stirred mixture, and the stirred mixture is taken according to the mass ratio of 40-50: 5-9, adding an antioxidant raw material, stirring and mixing at 0-4 ℃ for 30-50 min, stirring and mixing at 20-25 ℃ for 10-12 h, and distilling under reduced pressure to obtain the antioxidant active agent of the oil.
The spinning oil base material comprises: according to the mass parts, 5-10 parts of mineral oil, 1-3 parts of amino silicone oil, 2-5 parts of castor oil and 5-10 parts of chemical fiber oil are mixed to obtain the oil.
The antioxidant antistatic spinning oil comprises, by mass, 100-150 parts of a spinning oil base material, 1-3 parts of polyoxyethylene laurate, 1-3 parts of polyethylene glycol oleate, 5-15 parts of an antistatic active agent, 3-9 parts of a spinning oil smoothing active agent and 2-5 parts of an oil antioxidant active agent.
The preparation method of the catalyst comprises the following steps: taking 10 parts of cerium nitrate, 3 parts of cobalt nitrate, 5 parts of gallium nitrate and 80 parts of deionized water, stirring and mixing at 40 ℃ for 20min to obtain a mixture, and taking the mixture according to a mass ratio of 20: 3, adding tartaric acid, heating to 70 ℃, stirring and mixing for 30min, adding ethylene glycol accounting for 20% of the weight of the tartaric acid, stirring and mixing for 3h at 80 ℃, performing suction filtration, drying suction filtration residues, calcining for 3h at 600 ℃, and cooling to room temperature to obtain the catalyst.
The active raw materials are as follows: mixing sorbitol and fructose according to any mass ratio to obtain the product.
The preparation method of the alcohol additive comprises the following steps: taking active raw materials according to the mass ratio of 2: 5: adding n-decyl glycidyl ether and deionized water into 50, adding a catalyst with the mass of 5% of that of the active raw material, stirring and mixing at 800r/min for 20min, introducing hydrogen for reaction, keeping at 150 ℃ under 8MPa for 4h, cooling to room temperature, filtering, and taking the filtrate to obtain the alcohol additive.
The preparation method of the antistatic active agent comprises the following steps: taking phosphorus oxychloride according to a mass ratio of 3: 1: 10, adding propyl trichlorosilane and an alcohol additive, stirring and mixing for 1h at 40 ℃ to obtain a mixture a, and mixing the mixture a according to a mass ratio of 3: 10, adding diethylene glycol dimethyl ether, stirring and mixing for 3 hours at 100 ℃, cooling to room temperature to obtain a cooling material, and taking the cooling material according to a mass ratio of 2: 10 adding absolute ethyl alcohol, standing for 30min, taking the precipitate, distilling under reduced pressure, and drying to obtain the antistatic active agent.
The starting active agents were: mixing 5 parts of myristamine, 3 parts of lauric acid, 1 part of octyldodecanol, 20 parts of propylene glycol and 1 part of nonyl phenol according to parts by weight to obtain the composition.
The preparation method of the spinning oil smoothing active agent comprises the following steps: taking an initial active agent according to the mass ratio of 5: 1, adding pyridine, introducing nitrogen for dehydration for 20min to obtain a dehydrate, and taking propylene oxide according to a mass ratio of 3: 2, adding butylene oxide, adding dehydrate accounting for 2% of the mass of propylene oxide, introducing nitrogen for protection, heating to 120 ℃, preserving the heat for 20min, cooling to room temperature to obtain a cooling object a, and taking the cooling object a according to a mass ratio of 40: 2, adding oxalic acid, mixing, decoloring by active carbon, filtering, and taking the filtrate to obtain the spinning oil smoothing active agent.
The preparation method of the nuclear molecule active agent comprises the following steps: taking 1, 4-butanediamine according to a mass ratio of 2: 10, adding methanol, adding methyl acrylate accounting for 20% of the mass of the methanol, stirring and mixing for 18 hours at 20 ℃, carrying out reduced pressure distillation to obtain a reduced pressure distillate, and taking the reduced pressure distillate according to the mass ratio of 2: 10 adding methanol, adding 1, 4-butanediamine 2 times of the mass of the methanol, stirring and mixing for 20 hours at the temperature of 20 ℃, and distilling under reduced pressure to obtain the nuclear molecule active agent.
The preparation method of the antioxidant raw material comprises the following steps: taking beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid according to the mass ratio of 2: 10 adding N, N-dimethylformamide, stirring and mixing for 20min at 30 ℃, adding 10 mass percent of benzoyl chloride of the N, N-dimethylformamide, introducing nitrogen for protection, stirring and mixing for 3h at 30 ℃, and distilling under reduced pressure to obtain the antioxidant raw material.
The preparation method of the oil antioxidant active agent comprises the following steps: according to the mass parts, 20 parts of nuclear molecule active agent, 5 parts of triethylamine, 1 part of 4-dimethylpyridine and 40 parts of N, N-dimethylformamide are stirred and mixed for 40min at 20 ℃ to obtain a stirred mixture, and the stirred mixture is taken according to the mass ratio of 40: 5 adding antioxidant raw materials, stirring and mixing at 0 deg.C for 30min, stirring and mixing at 20 deg.C for 10 hr, and distilling under reduced pressure to obtain antioxidant active agent.
The spinning oil base material comprises: according to the mass parts, 5 parts of mineral oil, 1 part of amino silicone oil, 2 parts of castor oil and 5 parts of chemical fiber oil are mixed to obtain the oil.
The antioxidant antistatic spinning oil comprises, by mass, 100 parts of a spinning oil base material, 1 part of polyoxyethylene laurate, 1 part of polyethylene glycol oleate, 5 parts of an antistatic active agent, 3 parts of a spinning oil smoothing active agent and 2 parts of an oil antioxidant active agent.
The preparation method of the catalyst comprises the following steps: taking 12 parts of cerium nitrate, 5 parts of cobalt nitrate, 7 parts of gallium nitrate and 90 parts of deionized water in parts by mass, stirring and mixing at 45 ℃ for 30min to obtain a mixture, and taking the mixture according to a mass ratio of 35: 4, adding tartaric acid, heating to 75 ℃, stirring and mixing for 45min, adding ethylene glycol accounting for 25% of the weight of the tartaric acid, stirring and mixing for 5h at 85 ℃, performing suction filtration, drying suction filtration residues, calcining for 4h at 650 ℃, and cooling to room temperature to obtain the catalyst.
The active raw materials are as follows: mixing mannitol and galacto-oligosaccharide at any mass ratio.
The preparation method of the alcohol additive comprises the following steps: taking active raw materials according to a mass ratio of 4: 6: 60 adding n-decyl glycidyl ether and deionized water, adding a catalyst accounting for 8% of the mass of the active raw material, stirring and mixing at 800r/min for 30min, introducing hydrogen for reaction, keeping at 175 ℃ under 8MPa for 5h, cooling to room temperature, filtering, and taking the filtrate to obtain the alcohol additive.
The preparation method of the antistatic active agent comprises the following steps: taking phosphorus oxychloride according to a mass ratio of 5: 3: 15, adding propyl trichlorosilane and an alcohol additive, stirring and mixing for 2 hours at 45 ℃ to obtain a mixture a, and mixing the mixture a according to a mass ratio of 5: adding diethylene glycol dimethyl ether 15, stirring and mixing at 105 ℃ for 4 hours, cooling to room temperature to obtain a cooling material, and taking the cooling material according to a mass ratio of 4: 12 adding absolute ethyl alcohol, standing for 40min, distilling the precipitate under reduced pressure, and drying to obtain the antistatic active agent.
The starting active agents were: according to the mass parts, 8 parts of myristamine, 5 parts of lauric acid, 3 parts of octyldodecanol, 30 parts of propylene glycol and 2 parts of nonyl phenol are mixed to obtain the composition.
The preparation method of the spinning oil smoothing active agent comprises the following steps: taking an initial active agent according to the mass ratio of 7: 3, adding pyridine, introducing nitrogen for dehydration for 25min to obtain a dehydrate, and taking propylene oxide according to a mass ratio of 5: 3, adding butylene oxide, adding dehydrate accounting for 5% of the mass of propylene oxide, introducing nitrogen for protection, heating to 125 ℃, preserving the heat for 25min, cooling to room temperature to obtain a cooling object a, and taking the cooling object a according to a mass ratio of 45: 3, adding oxalic acid, mixing, decoloring by active carbon, filtering, and taking the filtrate to obtain the spinning oil smoothing active agent.
The preparation method of the nuclear molecule active agent comprises the following steps: taking 1, 4-butanediamine according to a mass ratio of 4: 15, adding methanol, adding methyl acrylate accounting for 25% of the mass of the methanol, stirring and mixing for 21 hours at 22 ℃, carrying out reduced pressure distillation to obtain a reduced pressure distillate, and taking the reduced pressure distillate according to a mass ratio of 4: 12 adding methanol, adding 1, 4-butanediamine with the mass of 3 times of that of the methanol, stirring and mixing for 22 hours at the temperature of 22 ℃, and distilling under reduced pressure to obtain the nuclear molecule active agent.
The preparation method of the antioxidant raw material comprises the following steps: taking beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid according to a mass ratio of 4: 15 adding N, N-dimethylformamide, stirring and mixing at 35 ℃ for 30min, adding benzoyl chloride accounting for 12% of the mass of the N, N-dimethylformamide, introducing nitrogen for protection, stirring and mixing at 35 ℃ for 5h, and distilling under reduced pressure to obtain the antioxidant raw material.
The preparation method of the oil antioxidant active agent comprises the following steps: according to the mass parts, 25 parts of nuclear molecule active agent, 6 parts of triethylamine, 3 parts of 4-dimethylpyridine and 50 parts of N, N-dimethylformamide are stirred and mixed for 45min at 23 ℃ to obtain a stirred mixture, and the stirred mixture is taken according to the mass ratio of 45: 7 adding antioxidant raw materials, stirring and mixing at 2 deg.C for 40min, stirring and mixing at 23 deg.C for 11h, and distilling under reduced pressure to obtain antioxidant active agent.
The spinning oil base material comprises: according to the mass portion, 7 portions of mineral oil, 2 portions of amino silicone oil, 4 portions of castor oil and 8 portions of chemical fiber oil are mixed to obtain the product.
An antioxidant antistatic spinning oil comprises, by mass, 125 parts of a spinning oil base material, 2 parts of polyoxyethylene laurate, 2 parts of polyethylene glycol oleate, 10 parts of an antistatic active agent, 6 parts of a spinning oil smoothing active agent and 4 parts of an oil antioxidant active agent.
The preparation method of the catalyst comprises the following steps: taking 15 parts of cerium nitrate, 7 parts of cobalt nitrate, 9 parts of gallium nitrate and 100 parts of deionized water in parts by mass, stirring and mixing at 50 ℃ for 40min to obtain a mixture, and taking the mixture according to a mass ratio of 50: and 5, adding tartaric acid, heating to 80 ℃, stirring and mixing for 60min, adding ethylene glycol accounting for 30% of the weight of the tartaric acid, stirring and mixing for 6h at 90 ℃, performing suction filtration, drying suction filtration residues, calcining for 5h at 700 ℃, and cooling to room temperature to obtain the catalyst.
The active raw materials are as follows: mixing maltose and lactose at any mass ratio.
The preparation method of the alcohol additive comprises the following steps: taking active raw materials according to the mass ratio of 6: 8: adding 70 n-decyl glycidyl ether and deionized water, adding 10% of catalyst by mass of active raw material, stirring and mixing at 800r/min for 40min, introducing hydrogen gas for reaction, keeping at 200 ℃ under 8MPa for 7h, cooling to room temperature, filtering, and collecting filtrate to obtain the alcohol additive.
The preparation method of the antistatic active agent comprises the following steps: taking phosphorus oxychloride according to a mass ratio of 6: 5: 20, adding propyl trichlorosilane and an alcohol additive, stirring and mixing for 3 hours at 50 ℃ to obtain a mixture a, and mixing the mixture a according to a mass ratio of 7: 20 adding diethylene glycol dimethyl ether, stirring and mixing for 5 hours at 110 ℃, cooling to room temperature to obtain a cooling material, and taking the cooling material according to the mass ratio of 5: 15 adding absolute ethyl alcohol, standing for 50min, taking the precipitate, distilling under reduced pressure, and drying to obtain the antistatic active agent.
The starting active agents were: according to the mass parts, 10 parts of myristamine, 7 parts of lauric acid, 4 parts of octyldodecanol, 40 parts of propylene glycol and 3 parts of nonyl phenol are mixed to obtain the composition.
The preparation method of the spinning oil smoothing active agent comprises the following steps: taking an initial active agent according to the mass ratio of 9: 4, adding pyridine, introducing nitrogen for dehydration for 30min to obtain a dehydrate, and taking propylene oxide according to a mass ratio of 7: and 5, adding butylene oxide, adding dehydrate accounting for 9% of the mass of propylene oxide, introducing nitrogen for protection, heating to 130 ℃, preserving the heat for 30min, cooling to room temperature to obtain a cooling object a, and taking the cooling object a according to the mass ratio of 50: and 5, adding oxalic acid, mixing, decoloring by using active carbon, filtering, and taking filtrate to obtain the spinning oil smoothing active agent.
The preparation method of the nuclear molecule active agent comprises the following steps: taking 1, 4-butanediamine according to a mass ratio of 5: 20, adding methanol, adding methyl acrylate accounting for 30% of the mass of the methanol, stirring and mixing for 24 hours at 25 ℃, carrying out reduced pressure distillation to obtain a reduced pressure distillate, and taking the reduced pressure distillate according to the mass ratio of 6: adding methanol 15, adding 1, 4-butanediamine 4 times of methanol, stirring and mixing at 25 deg.C for 24 hr, and distilling under reduced pressure to obtain nuclear molecule active agent.
The preparation method of the antioxidant raw material comprises the following steps: taking beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid according to the mass ratio of 5: 20 adding N, N-dimethylformamide, stirring and mixing at 40 deg.C for 40min, adding benzoyl chloride 15% of the mass of N, N-dimethylformamide, introducing nitrogen for protection, stirring and mixing at 40 deg.C for 7h, and distilling under reduced pressure to obtain antioxidant raw material.
The preparation method of the oil antioxidant active agent comprises the following steps: according to the mass parts, 30 parts of nuclear molecule active agent, 8 parts of triethylamine, 4 parts of 4-dimethylpyridine and 60 parts of N, N-dimethylformamide are stirred and mixed for 50min at 25 ℃ to obtain a stirred mixture, and the stirred mixture is taken according to the mass ratio of 50: 9 adding antioxidant raw materials, stirring and mixing at 4 deg.C for 50min, stirring and mixing at 25 deg.C for 12 hr, and distilling under reduced pressure to obtain antioxidant active agent.
The spinning oil base material comprises: according to the mass parts, 10 parts of mineral oil, 3 parts of amino silicone oil, 5 parts of castor oil and 10 parts of chemical fiber oil are mixed to obtain the oil.
An antioxidant antistatic spinning oil comprises, by mass, 150 parts of a spinning oil base material, 3 parts of polyoxyethylene laurate, 3 parts of polyethylene glycol oleate, 15 parts of an antistatic active agent, 9 parts of a spinning oil smoothing active agent and 5 parts of an oil antioxidant active agent.
Comparative example 1: essentially the same procedure as in example 1 was followed, except that the antistatic active agent was absent.
Comparative example 2: essentially the same procedure as in example 1 except that spin oil smoothing actives were absent.
Comparative example 3: essentially the same procedure as in example 1, except that the oil antioxidant active was absent.
Comparative example 4: an antioxidant antistatic spinning oil produced by a certain company in Nanjing.
The antioxidant antistatic spinning oils obtained in the examples and comparative examples were tested according to GB/T14342-1993, and the test results are shown in Table 1:
table 1:
test items
|
Example 1
|
Example 2
|
Example 3
|
Comparative example 1
|
Comparative example 2
|
Comparative example 3
|
Comparative example 4
|
Surface static electricity (kv)
|
0.07
|
0.08
|
0.12
|
0.10
|
0.18
|
0.20
|
0.28
|
Oil application Rate (%)
|
1.20
|
1.15
|
1.19
|
1.02
|
1.07
|
1.12
|
0.89
|
Breaking strength (g)
|
53.1
|
52.5
|
51.6
|
52.9
|
51.9
|
52.3
|
48.6
|
Oxidation resistance
|
Is preferably used
|
Is preferably used
|
Is preferably used
|
Is preferably used
|
In general
|
In general
|
Is poor |
In conclusion, the antioxidant antistatic spinning oil obtained by the invention has good antistatic property and uniform oiling, has better effect compared with a commercially available product, and is worthy of great popularization.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, but rather as the subject matter of the invention is to be construed in all aspects and as broadly as possible, and all changes, equivalents and modifications that fall within the true spirit and scope of the invention are therefore intended to be embraced therein.