High-modulus low-shrinkage industrial yarn chemical fiber oiling agent and preparation method thereof

Abstract

The invention discloses a high-modulus low-shrinkage industrial yarn chemical fiber oiling agent which is prepared from the following raw materials in percentage by mass: 50-70% of a mixture of vegetable oil and synthetic ester, 15-45% of a polyoxyethylene ether type surfactant, 5-15% of an ethylene oxide-propylene oxide copolymer and 5-10% of an anionic surfactant aqueous solution. The mass ratio of the vegetable oil to the synthetic ester is (1: 1)-(1: 4). By adding the random polyether and the block polyether, the heat resistance of the oiling agent is improved, the shearing resistance of an oil film is enhanced, and the oiling agent can adapt to a high-temperature and high-rotating-speed production process. The industrial yarn prepared by the oiling agent is good in wettability, can be uniformly spread on the surface of fiber by adopting an emulsion oiling mode, reduces friction, reduces yarn damage and generation of white powder, and is less in blue smoke emission and low in yarn breaking frequency in the use process, and the prepared fiber is small in thermal shrinkage rate and high in elastic modulus.

Description

Technical Field

[0001] The invention belongs to the field of functional polyester industrial yarn production, relates to a high modulus low shrinkage industrial yarn chemical fiber oil agent and a preparation method thereof, and specifically relates to an oil agent used in the spinning process of high modulus low shrinkage polyester industrial yarn and a preparation method thereof. Background Art

[0002] High modulus low shrinkage polyester industrial yarn is a kind of industrial fiber. High modulus low shrinkage means high modulus and low shrinkage. It has excellent properties such as high breaking strength, high elastic modulus, low elongation, and good impact resistance. It is widely used in rubber skeleton substrates, such as automotive radial tire cord fabrics, high-grade geogrids, and V-belt hard wire ropes. Tires made of high modulus low shrinkage polyester industrial yarn have the advantages of fatigue resistance, small deformation, and aging resistance. It has gradually replaced standard polyester industrial yarn. In addition, with the development of basic industries and the application of high-tech, low-shrinkage industrial yarns have become a new development direction. The application fields of high modulus low shrinkage polyester industrial yarns are becoming more and more extensive, and its demand is also further increasing.

[0003] In order to obtain high modulus and low shrinkage industrial yarn, most of them optimize the production process. For example, patent CN 102797054 A improves the cooling process, adjusts the temperature of the nascent fiber during the spinning process, ensures the stability of the solidification point of the nascent fiber, achieves the purpose of reducing the orientation and crystallization of the nascent fiber, and obtains high-quality high modulus and low shrinkage fiber; patent CN 109735942 A modifies polyester by heptanediol with tert-butyl side groups, reduces the effect of activation on the mechanical properties of polyester fiber, and the heat treatment temperature and high overfeed rate cooperate with each other to improve the integrity of fiber crystallization and reduce shrinkage during application. At present, the development and optimization of functional high modulus and low shrinkage oil agents are relatively few. Among them, patent CN 102912640 A discloses a crude oil polyester industrial oil agent, which can be used for high modulus and low shrinkage chemical fiber production, but fluorinated surfactants are added, and the raw materials are not environmentally friendly and safe. Summary of the invention

[0005] The purpose of the present invention is to provide a high modulus and low shrinkage industrial spinning oil, which is compounded with a smoothing agent, a sizing agent, an antistatic agent and an emulsifier to prepare a high modulus and low shrinkage chemical fiber oil with high temperature resistance and friction resistance, and the raw materials of the oil are safe and environmentally friendly. The oil has good wettability and can be evenly spread on the fiber surface by emulsion oiling, thereby reducing friction, reducing the damage to the filaments and the generation of white powder; adding random and block polyethers improves the heat resistance, enhances the shear resistance of the oil film, and can adapt to the production process of high temperature and high speed; used for spinning, the prepared fiber has high modulus and low shrinkage.

[0006] In order to achieve the above object, the present invention adopts the following technical solutions:

[0007] A new type of high modulus and low shrinkage industrial fiber oil is made of the following raw materials in percentage by mass:

[0008] Mixture of vegetable oil and synthetic ester 50-70%

[0009] Polyoxyethylene ether surfactant 15~45%

[0010] Ethylene oxide propylene oxide copolymer 5~15%

[0011] Anionic surfactant aqueous solution 5-10%;

[0012] The mass ratio of the vegetable oil to the synthetic ester is 1:1 to 1:4.

[0013] Preferably, the novel high modulus low shrinkage industrial silk chemical fiber oil is made of the following raw materials in percentage by mass:

[0014] Mixture of vegetable oil and synthetic ester 50-70%

[0015] Polyoxyethylene ether surfactant 15-30%

[0016] Ethylene oxide propylene oxide copolymer 8~15%

[0017] Anionic surfactant aqueous solution 5-10%.

[0018] The vegetable oil is one of palm oil and peanut oil or a mixture of two of them; the synthetic ester is a mixture of one or more of trimethylolpropane trioctanoate, lauryl oleate and glycerol trioleate.

[0019] The polyoxyethylene ether type surfactant is a mixture of two or three of fatty alcohol polyoxyethylene ether, fatty acid polyoxyethylene ether and fatty amine polyoxyethylene ether.

[0020] Preferably, the polyoxyethylene ether type surfactant is a mixture of fatty alcohol polyoxyethylene ether and fatty amine polyoxyethylene ether in a mass ratio of 2:1 to 1:2, or a mixture of fatty alcohol polyoxyethylene ether and fatty acid polyoxyethylene ether in a mass ratio of 1:1 to 1:3, or a mixture of fatty alcohol polyoxyethylene ether, fatty acid polyoxyethylene ether and fatty amine polyoxyethylene ether in a mass ratio of 1:1:1 to 2:1:2.

[0021] The fatty alcohol polyoxyethylene ether is a polyoxyethylene ether prepared by condensing fatty alcohol as an initiator with a molar ratio of the initiator to ethylene oxide (EO) of 1:5 to 1:10.

[0022] Specifically, the fatty alcohol polyoxyethylene ether is fatty alcohol polyoxyethylene ether MOA-2, fatty alcohol polyoxyethylene ether MOA-3, and fatty alcohol polyoxyethylene ether MOA-5.

[0023] The fatty acid polyoxyethylene ether is a polyoxyethylene ether prepared by condensing fatty acid as an initiator with a molar ratio of the initiator to ethylene oxide (EO) of 1:5 to 1:10.

[0024] Specifically, the fatty acid polyoxyethylene ether is fatty acid coconut oil polyether CE-10.

[0025] The fatty amine polyoxyethylene ether is a polyoxyethylene ether prepared by condensing fatty amine as an initiator according to a molar ratio of the initiator to ethylene oxide (EO) of 1:5 to 1:10.

[0026] Specifically, the fatty amine polyoxyethylene ether is octadecylamine polyoxyethylene ether AC1802 or octadecylamine polyoxyethylene ether AC1805.

[0027] The ethylene oxide propylene oxide copolymer is a mixture of block polyether and random polyether in a mass ratio of 1:1 to 2:1.

[0028] The block polyether is C 4 -C 12 The monobasic saturated acid is used as the initiator, and the block polyether with a molecular weight of 1000-1500 is obtained by polymerization according to the molar ratio of EO (ethylene oxide) to PO (propylene oxide) of 2:1-3:1.

[0029] The C 4 -C 12 The monobasic saturated acid is selected from caprylic acid, lauric acid and the like.

[0030] The block polyether is prepared by the following method: according to the molecular weight of the block polyether, the relative molecular weight of the initiator, and the molar ratio of EO (ethylene oxide) to PO (propylene oxide), the relative molecular weight of the initiator, the mass of ethylene oxide and propylene oxide are calculated; the measured initiator is put into a reaction kettle, and then a catalytic amount of NaOH aqueous solution is added, the temperature is increased and vacuum is drawn, dehydration is carried out at 100-120 DEG C, and then the air in the reaction kettle is replaced with nitrogen, and the pressure is continuously reduced, and ethylene oxide is introduced at 140 DEG C to start condensation reaction, and the reaction temperature is maintained at 140-160 DEG C and the vacuum degree is maintained at 0.2-0.3Mpa; propylene oxide is introduced to start condensation reaction, and the reaction temperature is maintained at 140-160 DEG C and the vacuum degree is maintained at 0.2-0.3Mpa; after the reaction is completed, the feed liquid is cooled, glacial acetic acid is used to neutralize the feed liquid until the acid ester is 0.4-0.5mgKOH / g, and then an appropriate amount of hydrogen peroxide is used for decolorization, and finally dehydration is carried out for 5 hours, cooling, and discharging.

[0031] Specifically, the block polyether can be lauric acid block polyether (molecular weight 1500, EO:PO=2:1), lauric acid block polyether (molecular weight 1500, EO:PO=3:1), caprylic acid block polyether (molecular weight 1500, EO:PO=2:1).

[0032] In some specific embodiments of the present invention, lauric acid block polyether (molecular weight 1500, EO:PO = 2:1) is prepared by the following method: 200g of lauric acid, 792g of ethylene oxide, 522g of propylene oxide are weighed, and 7.6g of NaOH is dissolved in an appropriate amount of water (the mass of NaOH is 0.5% of the total mass of the raw materials); lauric acid is put into a reaction kettle, and then an aqueous NaOH solution is added, the temperature is increased and vacuum is drawn, and dehydration is carried out at 100-120° C., and then the air in the reaction kettle is replaced with nitrogen, and the pressure is continued. At 140° C., ethylene oxide is introduced to start a condensation reaction, and the reaction temperature is maintained at 140-160° C. and the vacuum degree is maintained at 0.2-0.3Mpa; after the ethylene oxide is consumed, propylene oxide is introduced to start a condensation reaction, and the reaction temperature is maintained at 140-160° C. and the vacuum degree is maintained at 0.2-0.3Mpa until the propylene oxide is consumed; after the reaction is completed, the feed liquid is cooled, and glacial acetic acid is used to neutralize the feed liquid until the acid ester is 0.4-0.5mgKOH / g, and then 1% hydrogen peroxide is used for decolorization, and finally dehydration is carried out for 5h, cooling, and discharging.

[0033] In some specific embodiments of the present invention, lauric acid block polyether (molecular weight 1500, EO:PO=3:1) can be prepared by referring to the preparation method of lauric acid block polyether (molecular weight 1500, EO:PO=2:1), and only the amounts of EO and PO are adjusted.

[0034] In some specific embodiments of the present invention, caprylic acid block polyether (molecular weight 1500, EO:PO=2:1) ​​can be prepared by referring to the preparation method of lauric acid block polyether (molecular weight 1500, EO:PO=2:1), and only the amounts of caprylic acid, EO and PO are adjusted.

[0035] The random polyether is an ether compound with a molecular weight of 2500 to 3000 generated by ring-opening addition reaction of ethylene oxide, propylene oxide and the initiator under the action of a catalyst, with polyol or isomeric alcohol as the initiator, and the molar ratio of EO (ethylene oxide) to PO (propylene oxide) is 2:1 to 5:1.

[0036] The polyol is propylene glycol; the isomeric alcohols are isomeric tridecanol and isomeric octadecyl alcohol.

[0037] The random polyether is prepared by the following method: the relative molecular weight of the initiator, the mass of ethylene oxide and propylene oxide are calculated according to the molecular weight of the random polyether, the relative molecular weight of the initiator, and the molar ratio of EO (ethylene oxide) and PO (propylene oxide); the measured initiator is put into a reaction kettle, a catalytic amount of NaOH aqueous solution is added, the temperature is increased and vacuum is drawn, dehydration is carried out at 100-120 DEG C, the air in the reaction kettle is replaced with nitrogen, the pressure is continuously reduced, a mixture of ethylene oxide and propylene oxide mixed in proportion is introduced at 140 DEG C to start condensation reaction, the reaction temperature is maintained at 140-160 DEG C, and the vacuum degree is maintained at 0.2-0.3Mpa; after the reaction is completed, the feed liquid is cooled, glacial acetic acid is used to neutralize the feed liquid until the acid ester is 0.4-0.5mgKOH / g, an appropriate amount of hydrogen peroxide is used for decolorization, and finally dehydration is carried out for 5 hours, cooling and discharging.

[0038] Specifically, the random polyether can be propylene glycol random polyether (molecular weight 2500, EO:PO=2:1), isomeric tridecanol random polyether (molecular weight 2500, EO:PO=3:1), isomeric octadecyl alcohol random polyether (molecular weight 2500, EO:PO=2:1).

[0039] In some specific embodiments of the present invention, propylene glycol random polyether (molecular weight 2500, EO:PO = 2:1) is prepared by the following method: weigh 76g propylene glycol, 1478g ethylene oxide, 974g propylene oxide, and 12.6g NaOH is dissolved in an appropriate amount of water (the mass of NaOH is 0.5% of the total mass of the raw materials); propylene oxide and propylene oxide are mixed uniformly; propylene glycol is put into a reaction kettle, and then a NaOH aqueous solution is added, the temperature is increased and vacuum is drawn, dehydration is carried out at 100-120°C, and then the air in the reaction kettle is replaced with nitrogen, and the pressure is continued to be reduced, and a mixture of ethylene oxide and propylene oxide is introduced at 140°C to start a condensation reaction, and the reaction temperature is maintained at 140-160°C and the vacuum degree is maintained at 0.2-0.3Mpa. After the ethylene oxide and propylene oxide are consumed, the reaction is completed, and the feed liquid is cooled, and glacial acetic acid is used to neutralize the feed liquid until the acid ester is 0.4-0.5mgKOH / g, and then 1% hydrogen peroxide is used for decolorization, and finally dehydration is carried out for 5h, cooling, and discharging.

[0040] In some specific embodiments of the present invention, isotridecyl alcohol random polyether (molecular weight 2500, EO:PO=3:1) can be prepared by referring to the preparation method of propylene glycol random polyether (molecular weight 2500, EO:PO=2:1), and only the amounts of isotridecyl alcohol, EO and PO are adjusted.

[0041] In some specific embodiments of the present invention, isomeric octadecyl alcohol random polyether (molecular weight 2500, EO:PO=2:1) ​​can be prepared by referring to the preparation method of propylene glycol random polyether (molecular weight 2500, EO:PO=2:1), and only the amounts of isomeric tridecanol, EO and PO are adjusted.

[0042] The anionic surfactant aqueous solution is prepared by mixing anionic surfactant and water in a mass ratio of 1:1.5 to 1:5.

[0043] The anionic surfactant is a mixture of one or more of sodium alkyl sulfonate, castor oil phosphate, and fatty alcohol ether phosphate.

[0044] The alkyl sodium sulfonate is sodium dodecyl sulfonate or sodium secondary alkyl sulfonate.

[0045] The fatty alcohol polyoxyethylene ether potassium phosphate.

[0046] Preferably, when the anionic surfactant contains sodium alkyl sulfonate, the mass percentage of the sodium alkyl sulfonate does not exceed 2%.

[0047] More preferably, when the anionic surfactant contains sodium alkyl sulfonate, the mass percentage of the sodium alkyl sulfonate does not exceed 1%.

[0048] Another object of the present invention is to provide a method for preparing the high modulus low shrinkage industrial silk chemical fiber oil, comprising: weighing each component, stirring the vegetable oil and synthetic ester mixture, ethylene oxide ether type surfactant, and ethylene oxide propylene oxide copolymer at a temperature of 30 to 60°C, the stirring time is 60 to 120 minutes, the stirring speed is 500 to 1000 r / min, after stirring evenly, adding an anionic surfactant aqueous solution, stirring at a temperature of 15 to 45°C, the stirring time is 60 to 120 minutes, the stirring speed is 500 to 1000 r / min, and after the stirring is completed, filtering to obtain the oil.

[0049] As a further preferred embodiment of the method for preparing the high modulus low shrinkage industrial silk chemical fiber oil of the present invention, it further comprises: canning the oil.

[0050] Beneficial effects of the present invention:

[0051] 1. The raw materials selected for the industrial silk chemical fiber oil of the present invention are green and environmentally friendly, the preparation process of the oil is simple, the product is safe and stable, and the preparation cost is low.

[0052] 2. The present invention improves the heat resistance of industrial silk chemical fiber oil and enhances the shear resistance of the oil film by adding random polyether and block polyether, and can adapt to high-temperature and high-speed production processes.

[0053] 3. The industrial silk chemical fiber oil agent of the present invention has good wettability for preparing industrial silk. It adopts the emulsion oiling method and can be evenly spread on the fiber surface, thereby reducing friction, reducing silk damage and the generation of white powder. The industrial silk chemical fiber oil agent of the present invention is a functional oil agent and is used for continuous production. During use, it emits less blue smoke and has a low frequency of broken silk. The prepared fiber has a small thermal shrinkage rate and a high elastic modulus, which can meet market demand. DETAILED DESCRIPTION

[0054] The present invention is further described below in conjunction with specific examples to facilitate understanding of the present invention, but the present invention is not limited thereto.

[0055] Example 1

[0056] The industrial silk chemical fiber oil in this embodiment is made of the following raw materials in parts by weight:

[0057] Weigh 60 parts by mass of a mixture of vegetable oil and synthetic ester (15 parts by mass of palm oil, 45 parts by mass of triolein), 25 parts by mass of a polyoxyethylene ether type surfactant (10 parts by mass of fatty alcohol polyoxyethylene ether MOA-5, 15 parts by mass of octadecylamine polyoxyethylene ether AC1805), 8 parts by mass of an ethylene oxide propylene oxide copolymer (4 parts by mass of lauric acid block polyether (molecular weight 1500, EO:PO=2:1), 4 parts by mass of propylene glycol random polyether (molecular weight 2500, EO:PO=2:1)), and 7 parts by mass of anionic surfactant aqueous solution (2 parts by mass of sodium dodecyl sulfate, 5 parts by mass of water).

[0058] Mix the mixture of vegetable oil and synthetic ester, polyoxyethylene ether surfactant and ethylene oxide propylene oxide copolymer, and stir at 45°C for 30 minutes; after stirring evenly, add anionic surfactant aqueous solution and stir at 30°C for 45 minutes to obtain a clear and transparent oil-in-water system, filter, prepare oil agent, and seal.

[0059] Example 2

[0060] Weigh 50 parts by mass of a mixture of vegetable oil and synthetic ester (15 parts by mass of peanut oil, 20 parts by mass of trimethylolpropane tricaprylate, 15 parts by mass of glycerol trioleate), 30 parts by mass of polyoxyethylene ether type surfactant (10 parts by mass of fatty acid coconut oil polyether CE-10, 10 parts by mass of octadecylamine polyoxyethylene ether AC1805, 10 parts by mass of fatty alcohol polyoxyethylene ether MOA-3), 15 parts by mass of ethylene oxide propylene oxide copolymer (10 parts by mass of lauric acid block polyether (molecular weight 1500, EO:PO=2:1), 5 parts by mass of isomeric tridecanol random polyether (molecular weight 2500, EO:PO=3:1)), 5 parts by mass of anionic surfactant aqueous solution (2 parts by mass of sodium secondary alkyl sulfonate SAS-60, 3 parts by mass of water); prepare industrial silk chemical fiber oil according to the preparation method of Example 1.

[0061] Example 3

[0062] Weigh 65 parts by mass of a mixture of vegetable oil and synthetic ester (13 parts by mass of palm oil, 52 parts by mass of triolein), 15 parts by mass of polyoxyethylene ether type surfactant (10 parts by mass of fatty alcohol polyoxyethylene ether MOA-2, 5 parts by mass of octadecylamine polyoxyethylene ether AC1802), 10 parts by mass of ethylene oxide propylene oxide copolymer (5 parts by mass of octanoic acid block polyether (molecular weight 1500, EO:PO=2:1), 5 parts by mass of propylene glycol random polyether (molecular weight 2500, EO:PO=2:1)), and 10 parts by mass of anionic surfactant aqueous solution (3 parts by mass of fatty alcohol polyoxyethylene ether potassium phosphate MOA-3PK, 7 parts by mass of water); prepare industrial silk chemical fiber oil according to the preparation method of Example 1.

[0063] Example 4

[0064] Weigh 55 parts by mass of a mixture of vegetable oil and synthetic ester (20 parts by mass of peanut oil, 35 parts by mass of lauryl oleate), 20 parts by mass of polyoxyethylene ether type surfactant (10 parts by mass of fatty alcohol polyoxyethylene ether MOA-5, 10 parts by mass of coconut oil oxyethylene ether CE-10), 15 parts by mass of ethylene oxide propylene oxide copolymer (10 parts by mass of lauric acid block polyether (molecular weight 1500, EO:PO=3:1), 5 parts by mass of isomeric octadecyl alcohol random polyether (molecular weight 2500, EO:PO=2:1)), and 10 parts by mass of anionic surfactant aqueous solution (4 parts by mass of sodium dodecyl sulfate, 6 parts by mass of water); prepare industrial silk chemical fiber oil according to the preparation method of Example 1.

[0065] Example 5

[0066] Weigh 70 parts by mass of a mixture of vegetable oil and synthetic ester (14 parts by mass of palm oil, 28 parts by mass of glycerol trioleate, 28 parts by mass of lauryl oleate), 15 parts by mass of polyoxyethylene ether type surfactant (5 parts by mass of fatty alcohol polyoxyethylene ether MOA-3, 10 parts by mass of octadecylamine polyoxyethylene ether AC1802), 10 parts by mass of ethylene oxide propylene oxide copolymer (5 parts by mass of octanoic acid block polyether (molecular weight 1500, EO:PO=2:1), 5 parts by mass of isomeric tridecanol random polyether (molecular weight 2500, EO:PO=3:1)), and 5 parts by mass of anionic surfactant aqueous solution (1 part by mass of sodium secondary alkyl sulfonate SAS-60, 4 parts by mass of water); prepare an industrial silk chemical fiber oil according to the preparation method of Example 1.

[0067] Comparative Example 1

[0068] Weigh 50 parts by mass of vegetable oil (20 parts by mass of palm oil, 30 parts by mass of peanut oil), 30 parts by mass of polyoxyethylene ether type surfactant (10 parts by mass of fatty acid coconut oil polyether CE-10, 10 parts by mass of octadecylamine polyoxyethylene ether AC1805, 10 parts by mass of fatty alcohol polyoxyethylene ether MOA-3), 8 parts by mass of lauric acid block polyether (molecular weight 1500, EO:PO=3:1), 7 parts by mass of anionic surfactant aqueous solution (2 parts by mass of sodium dodecyl sulfate, 5 parts by mass of water); prepare industrial silk chemical fiber oil according to the preparation method of Example 1.

[0069] Comparative Example 2

[0070] Weigh 65 parts by mass of synthetic ester (30 parts by mass of lauryl oleate, 25 parts by mass of trimethylolpropane tricaprylate), 15 parts by mass of polyoxyethylene ether type surfactant (10 parts by mass of fatty alcohol polyoxyethylene ether MOA-2, 5 parts by mass of octadecylamine polyoxyethylene ether AC1802), 10 parts by mass of isomeric octadecyl alcohol random polyether (molecular weight 2500, EO:PO=2:1), and 10 parts by mass of anionic surfactant aqueous solution (3 parts by mass of fatty alcohol polyoxyethylene ether potassium phosphate MOA-3PK, 7 parts by mass of water); prepare industrial silk chemical fiber oil according to the preparation method of Example 1.

[0071] Comparative Example 3

[0072] Weigh 50 parts by mass of vegetable oil (peanut oil), 30 parts by mass of polyoxyethylene ether type surfactant (10 parts by mass of fatty acid coconut oil polyether CE-10, 10 parts by mass of octadecylamine polyoxyethylene ether AC1805, 10 parts by mass of fatty alcohol polyoxyethylene ether MOA-3), 15 parts by mass of ethylene oxide propylene oxide copolymer (10 parts by mass of lauric acid block polyether (molecular weight 1500, EO:PO=2:1), 5 parts by mass of isomeric tridecyl alcohol random polyether (molecular weight 2500, EO:PO=3:1)), and 5 parts by mass of anionic surfactant aqueous solution (2 parts by mass of sodium secondary alkyl sulfonate SAS-60, 3 parts by mass of water); prepare industrial silk chemical fiber oil according to the preparation method of Example 1.

[0073] Comparative Example 4

[0074] Weigh 50 parts by mass of a mixture of vegetable oil and synthetic ester (10 parts by mass of peanut oil, 20 parts by mass of trimethylolpropane trioctanoate, 10 parts by mass of glycerol trioleate), 30 parts by mass of polyoxyethylene ether type surfactant (10 parts by mass of fatty acid coconut oil polyether CE-10, 10 parts by mass of octadecylamine polyoxyethylene ether AC1805, 10 parts by mass of fatty alcohol polyoxyethylene ether MOA-3), 15 parts by mass of lauric acid block polyether (molecular weight 1500, EO:PO=2:1), and 5 parts by mass of anionic surfactant aqueous solution (2 parts by mass of sodium secondary alkyl sulfonate SAS-60, 3 parts of water); prepare industrial silk chemical fiber oil according to the preparation method of Example 1.

[0075] The oils prepared in the examples and comparative examples were investigated, and the test method was as follows:

[0076] Smoke test: Weigh 15g of sample and place it in a quartz beaker. Heat the beaker on an electric stove to 250℃ and observe the amount of smoke emitted by the oil.

[0077] Coking test: measure a drop of sample on a steel test piece, place the steel test piece in a 250℃ oven for 5 minutes, take it out, cool it, and observe the coking of the sample on the steel test piece.

[0078] High modulus and low shrinkage: The breaking strength and constant load elongation (load is 4.0 cN / dtex) were measured using the British In-stron 4464 tensile tester; the dry heat shrinkage was measured using the Testerita MKV dry heat shrinkage tester at a temperature of 180°C and a time of 1 min.

[0079] Tests on broken yarn frequency and hairiness rate: The spinning machine experiment (production of high modulus low shrinkage industrial yarn) was carried out under spinning process conditions (stretching temperature 250°C, stretching speed 4300m / s, oiling by nozzle, oiling rate 0.75%), and the hairiness rate and broken yarn frequency of the fiber were observed and recorded.

[0080] 1. Oil performance evaluation

[0081]

[0082] It can be seen from the experimental results that the smoke generation of the oils prepared in the five embodiments is good, and the coking degree is light. This is because most of the components in the oils are resistant to high temperatures, especially the random polyether has excellent high temperature resistance, and can be completely decomposed by heating for a long time, with less residue, which can improve the white powder loss caused by friction and avoid the formation of cokes by heating to affect the quality of the silk; the industrial silk prepared by the five embodiments is tested, and the fiber has a large breaking strength, and the fixed load elongation and heat drying shrinkage are low, indicating that it has high strength and high dimensional stability. The coking degree of the oils prepared in Examples 1, 2, and 4 is relatively high, because the addition amount of sodium alkyl sulfonate is high, and brittle cokes are easily formed after heating, but the coking degree meets the industry requirements; the hairiness rate is low, because the presence of continuous EO and PO in the block polyether is conducive to the formation of hydrogen bonds, which enhances the cohesion of the silk bundle and the shear resistance of the oil film; the low frequency of broken silk is due to the good smoothness of the oil, the coke formed by heating, and the small residue, which reduces friction.

[0083] In Comparative Example 1, only vegetable oil is used as the oil agent. Vegetable oil has good lubricity but is not resistant to high temperatures. It is easily oxidized to form a colloid and forms a brittle solid coke when heated. In addition, only block polyether is added. The heat resistance of block polyether is not as good as that of random polyether. Therefore, the smoke emission is large and the coking degree is high, which leads to a high frequency of broken wires and a high hairiness rate.

[0084] In comparative example 2, only synthetic ester is used as the oil agent. Synthetic ester is resistant to high temperature but has poor lubricity. Random polyether has good heat resistance and is easy to decompose, but cannot enhance the yarn bundle cohesion and oil film shearing property. Therefore, the smoke emission is small but the hairiness rate is high and the frequency of broken yarns is high.

[0085] Compared with the oil in Comparative Example 2, only peanut oil was added to the oil in Comparative Example 3, and only block polyether was added to the oil in Comparative Example 4. The smoke emission of the oil in Comparative Example 3 is large, which is due to the fact that no high-temperature resistant synthetic ester was added and the heat resistance of the vegetable oil was poor. The high coking degree of the oil in Comparative Example 3 is due to the fact that the vegetable oil is easily oxidized to form a colloid that cokes when heated; the high coking degree of the oil in Comparative Example 4 is due to the fact that no random polyether with good heat resistance was added; Comparative Example 4 is slightly better than Comparative Example 3 because the heat resistance of the block polyether is lower than that of the random polyether, but higher than that of the vegetable oil. The large coking degree of the oil in Comparative Example 3 leads to a high hairiness rate and a high frequency of broken wires; the large coking degree of Comparative Example 4 leads to a high frequency of broken wires, but because a large amount of block polyether was added, the hairiness rate was partially reduced.

[0086] In addition, it should be noted that the specific parameters, names, etc. of the specific embodiments described in this patent book may be different: any equivalent or simple changes made based on the concept and principle of the patent of the present invention are included in the protection scope of the patent of the present invention: technicians in the technical field to which the present invention belongs can make various modifications or supplements to the specific embodiments described or replace them in a similar manner, as long as they do not deviate from the scope defined in the claims of the present invention, they should all fall within the protection scope of the present invention.

Claims

1. A high modulus low shrinkage industrial silk chemical fiber oil, characterized in that: Made of the following raw materials in percentage by mass: Mixture of vegetable oil and synthetic ester 50-70% Polyoxyethylene ether surfactant 15~45% Ethylene oxide propylene oxide copolymer 5~15% Anionic surfactant aqueous solution 5-10%; The mass ratio of the vegetable oil to the synthetic ester is 1:1 to 1:

4.

2. The high modulus low shrinkage industrial silk chemical fiber oil according to claim 1, characterized in that: The vegetable oil is one of palm oil and peanut oil or a mixture of two of them; the synthetic ester is a mixture of one or more of trimethylolpropane trioctanoate, lauryl oleate and glycerol trioleate.

3. The high modulus low shrinkage industrial yarn chemical fiber oil according to claim 1, characterized in that: The polyoxyethylene ether type surfactant is a mixture of two or three of fatty alcohol polyoxyethylene ether, fatty acid polyoxyethylene ether and fatty amine polyoxyethylene ether.

4. The high modulus low shrinkage industrial silk chemical fiber oil according to claim 1 or 2, characterized in that: The polyoxyethylene ether type surfactant is a mixture of fatty alcohol polyoxyethylene ether and fatty amine polyoxyethylene ether in a mass ratio of 2:1 to 1:2, or a mixture of fatty alcohol polyoxyethylene ether and fatty acid polyoxyethylene ether in a mass ratio of 1:1 to 1:3, or a mixture of fatty alcohol polyoxyethylene ether, fatty acid polyoxyethylene ether and fatty amine polyoxyethylene ether in a mass ratio of 1:1:1 to 2:1:

2.

5. The high modulus low shrinkage industrial yarn chemical fiber oil according to claim 1, characterized in that: The ethylene oxide propylene oxide copolymer is a mixture of block polyether and random polyether in a mass ratio of 1:1 to 2:

1.

6. The high modulus low shrinkage industrial fiber oil according to claim 5, characterized in that: The block polyether is C4-C 12 A block polyether with a molecular weight of 1000 to 1500 is obtained by polymerization with a monobasic saturated acid as an initiator and a molar ratio of EO to PO of 2:1 to 3:1; The random polyether is an ether compound with a molecular weight of 2500-3000, which is prepared by using polyol or isomeric alcohol as initiator and the molar ratio of EO to PO is 2:1-5:1; the polyol is propylene glycol; the isomeric alcohol is isomeric tridecanol and isomeric octadecyl alcohol.

7. The high modulus low shrinkage industrial fiber oil according to claim 1, characterized in that: The anionic surfactant aqueous solution is prepared by mixing anionic surfactant and water in a mass ratio of 1:1.5 to 1:5; the anionic surfactant is a mixture of one or more of sodium alkyl sulfonate, castor oil phosphate, and fatty alcohol ether phosphate.

8. The high modulus low shrinkage industrial fiber oil according to claim 7, characterized in that: The sodium alkyl sulfonate is sodium dodecyl sulfonate or sodium secondary alkyl sulfonate; the potassium phosphate of fatty alcohol polyoxyethylene ether is described.

9. The high modulus low shrinkage industrial fiber oil according to claim 1 or 7, characterized in that: When the anionic surfactant contains sodium alkyl sulfonate, the mass percentage of the sodium alkyl sulfonate is not more than 2%.

10. A method for preparing the high modulus low shrinkage industrial silk chemical fiber oil according to claim 1, characterized in that: The method comprises the following steps: weighing each component, stirring the vegetable oil with a synthetic ester mixture, an ethylene oxide ether type surfactant and an ethylene oxide propylene oxide copolymer at a temperature of 30 to 60°C for 60 to 120 minutes and a stirring speed of 500 to 1000 r / min, and after stirring evenly, adding an anionic surfactant aqueous solution, stirring at a temperature of 15 to 45°C for 60 to 120 minutes and a stirring speed of 500 to 1000 r / min, and filtering after the stirring to obtain an oil agent.

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