CN111636200A - Terylene FDY oiling agent and preparation method thereof - Google Patents
Terylene FDY oiling agent and preparation method thereof Download PDFInfo
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- CN111636200A CN111636200A CN202010393181.4A CN202010393181A CN111636200A CN 111636200 A CN111636200 A CN 111636200A CN 202010393181 A CN202010393181 A CN 202010393181A CN 111636200 A CN111636200 A CN 111636200A
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Abstract
The invention discloses a terylene FDY oil agent and a preparation method thereof, relating to the field of terylene spinning oil agents and comprising the following components in percentage by weight: 14-33% of base oil, 24-38% of smoothing agent, 7-11% of bundling agent, 7-11% of emulsifier, 5-7% of antistatic agent, 1-3% of penetrating agent and the balance of additive; according to the invention, through selection and proportioning of monomers, the prepared FDY oiling agent has good comprehensive performances of smoothness, bundling, static resistance, permeability, heat resistance, sizing and uniform coating, has good spinnability, greatly reduces abnormal broken filaments, broken ends, white powder, tension fluctuation and winding phenomena, and can obviously improve the high-quality product rate under the same spinning process conditions. In the subsequent printing and dyeing, the phenomena of difficult dyeing and uneven dyeing are reduced, and the M rate of fiber dyeing is improved.
Description
Technical Field
The invention relates to the field of polyester spinning oil, in particular to a polyester FDY oil and a preparation method thereof.
Background
The polyester FDY oiling agent is an essential auxiliary agent in the spinning process of a polyester spinning and stretching one-step method, and can ensure that fibers have good performances of smoothness, bundling, static resistance and the like, so that spinning can be smoothly carried out, and spun filaments meet the requirements of subsequent processing. However, most domestic terylene FDY oil agents still depend on import at present, although the domestic oil agents have certain progress, the quality of the FDY oil agents still has certain difference compared with the imported oil agents, the FDY oil agents generally easily cause abnormal spinning phenomena such as broken filaments, broken ends, white powder, tension fluctuation, winding and the like in spinning application, and the FDY oil agents are easily difficult to dye, uneven in dyeing and the like in later dyeing, so that the quality of fibers is seriously reduced.
For example, a chinese patent publication discloses "a middle strength heavy denier polyester FDY yarn and a method for producing the same", publication No. CN102443861A, which discloses a middle strength heavy denier polyester FDY yarn and a method for producing the same, the polyester FDY yarn being prepared by the following method: according to the direct spinning FDY process route, PET melt is extruded from a spinneret orifice of an oval spinneret plate for spinning, then is cooled and solidified into filaments through side air blowing in sequence, and then is oiled by an oil tanker, heated and drawn by two pairs of hot rollers for shaping, and is added with a main network to be wound into an FDY spinning cake.
Disclosure of Invention
The invention provides a terylene FDY oil agent and a preparation method thereof, aiming at overcoming the problems that the prior oil agent has poor quality, commonly leads to abnormal spinning phenomena such as broken filaments, broken ends, white powder, tension fluctuation, winding and the like in spinning application, is easy to cause the phenomena of difficult dyeing, uneven dyeing and the like in subsequent dyeing, seriously reduces the quality of fibers and the like.
In order to achieve the purpose, the invention adopts the following technical scheme:
the terylene FDY oiling agent comprises the following components in percentage by weight: 14-33% of base oil, 24-38% of smoothing agent, 7-11% of bundling agent, 7-11% of emulsifier, 5-7% of antistatic agent, 1-3% of penetrating agent and the balance of additive.
The prior FDY oiling agent is easy to cause abnormal spinning phenomena such as broken filaments, broken ends, white powder, tension fluctuation, winding and the like in spinning application, and is easy to cause the phenomena of difficult dyeing, uneven dyeing and the like in the subsequent dyeing, because the prior FDY oiling agent cannot achieve balanced proportioning in the aspects of smoothness, bundling, antistatic property, permeation, heat resistance, sizing and uniform performance, the invention prepares the terylene FDY oiling agent with good comprehensive performances of smoothness, bundling, antistatic property, permeation, heat resistance, sizing and uniform adhesion by specific selection of various functional components and strict limitation of the proportioning.
Preferably, the base oil comprises one or more of isooctyl stearate, isooctyl oleate, diisooctyl sebacate, trimethylolpropane oleate, pentaerythritol oleate and technical white oil; the smoothing agent comprises one or more of oleic acid polyethylene glycol 600 diester, lauric acid polyethylene glycol 400 diester and C12-C14 fatty alcohol block polyoxyethylene polyoxypropylene ether, wherein PO/EO of the C12-C14 fatty alcohol block polyoxyethylene polyoxypropylene ether is 1.7-5.7, and the molecular weight is 600-1200.
Preferably, the bundling agent comprises one or more of oleic acid polyethylene glycol 400 diester, ricinoleic acid polyoxyethylene ester, isomeric tridecanol polyoxyethylene ether, and C4-C12 fatty alcohol random polyoxyethylene polyoxypropylene ether; the average addition number of polyoxyethylene in the polyoxyethylene ricinoleate is 20; the average addition number of polyoxyethylene in the isomeric tridecanol polyoxyethylene ether is 3-12; the C4-C12 fatty alcohol random polyoxyethylene polyoxypropylene ether has EO/PO of 1-2.3 and molecular weight of 1150-1600.
Preferably, the emulsifier comprises one or more of sorbitan polyoxyethylene ether stearate, oleic acid polyoxyethylene ester and lauric acid polyoxyethylene ester; the average addition number of polyoxyethylene in the sorbitan polyoxyethylene ether stearate is 80; the average addition number of polyoxyethylene in the polyoxyethylene oleate is 3; the average addition number of polyoxyethylene in the polyoxyethylene oleate is 5; the average addition number of polyoxyethylene in the polyoxyethylene laurate is 9.
Preferably, the antistatic agent comprises one or more of C12-C14 fatty alcohol polyoxyethylene ether phosphate potassium salt and C12-C14 fatty alcohol polyoxyethylene ether sulfate sodium/potassium salt; the average addition number of polyoxyethylene in the C12-C14 fatty alcohol polyoxyethylene ether phosphate potassium salt is 3; the average addition number of polyoxyethylene in the C12-C14 fatty alcohol polyoxyethylene ether sodium sulfate/potassium salt is 3.
Preferably, the penetrant comprises C12-C14 fatty alcohol block polyoxyethylene polyoxypropylene ether, EO/PO 1-1.4, molecular weight 950-.
Preferably, the additives comprise bacteriostatic agents, surface tension reducers, oil film enhancers, antifoaming agents and stabilizers; the bacteriostatic agent is an acetophenone compound; the surface tension reducing agent is polyether modified silicone oil; the oil film reinforcing agent is polyoxypropylene stearate, and the average addition number of polyoxyethylene is 5; the defoaming agent is glycerol random polyoxyethylene polyoxypropylene ether, the EO/PO of the glycerol random polyoxyethylene polyoxypropylene ether is 0.5-1.3, and the molecular weight of the glycerol random polyoxyethylene polyoxypropylene ether is 2700-3300; the stabilizer is one of cetyl alcohol or oleic acid.
In order to solve various problems of FDY oil in spinning application, the invention also specifically selects various components and additives in oil preparation.
The problems of yarn breakage and yarn breakage during spinning are often caused by insufficient smoothness or permeability of the finish. In terms of smoothness, the selected monomers mainly comprise three categories of synthetic fatty acid ester, industrial white oil and polyether substances (the synthetic fatty acid ester and the industrial white oil are classified as base oil and the polyether substances are classified as smoothing agents), the smoothness performance of the monomers is comprehensively evaluated through measuring the viscosity and the fluidity of the monomers and the dynamic and static friction coefficients after fibers are oiled, and the smoothing agent monomers are screened or adjusted to solve the problem of insufficient smoothness of the existing oil agent. In terms of permeability, a monomer with lower surface tension is selected as a penetrant, such as C12-C14 fatty alcohol block polyoxyethylene polyoxypropylene ether (EO/PO is 1-1.4, molecular weight is 950-1500) which is a special polyether, and polyether modified silicone oil is added in the additive to be used as a surface tension reducer to reduce the surface tension of the oil agent.
The white powder problem in spinning is often caused by insufficient smoothness and permeability of the finish and insufficient oil film strength of the finish to the fiber, and insufficient finish bundling property affects the white powder, and among these, the white powder problem is often caused by insufficient oil film strength. For the problem of insufficient oil film strength, the invention selects monomers with high oil film strength during formulation design, for example, synthetic fatty acid ester with high oil film strength is preferred for base oil, fatty acid polyoxyethylene ester with high oil film strength is preferred for other components (smoothing agent, bundling agent and emulsifier), and oil film enhancer polyoxypropylene stearate is added into the additive to enhance the oil film strength. For the oil agent bundling property, which is an index for evaluating the cohesion capability during fiber tow processing, the general oil agent has good smoothness, poor bundling property, good oil agent bundling property and poor smoothness, in order to give consideration to both good smoothness and bundling property of the oil agent, the invention measures the monomer viscosity, the fluidity and the dynamic and static friction coefficients after the fiber is oiled, and when designing the oil agent formula, oleic acid polyethylene glycol 400 diester, ricinoleic acid polyoxyethylene ester, isotridecanol polyoxyethylene ether and C4-C12 fatty alcohol random polyoxyethylene polyoxypropylene ether are selected as the bundling agent.
For the problem of tension fluctuation of the filaments during spinning, the coking phenomenon of an oiling roller is serious due to poor heat resistance of an oiling agent, so that the tension fluctuation of the fibers is obvious in the spinning process. In addition, when oiling, the oil agent is prepared into emulsion for use, and because spinning is carried out at high temperature, the concentration of the oil agent in the emulsion is continuously increased along with continuous heating and water evaporation of the emulsion, and the viscosity of the emulsion is changed therewith. When the viscosity-temperature viscosity-concentration characteristic of the oil is not ideal, namely, the problem of tension fluctuation can be caused when the viscosity of the emulsion fluctuates greatly along with the temperature or the concentration of the oil during spinning. In the invention, the oil agent monomer with better heat resistance is preferably selected in the design of the oil agent formula, wherein the base oil is selected from synthetic fatty acid ester with high boiling point and large latent heat of vaporization and industrial white oil with high flash point. For the problem that the viscosity-temperature viscosity-concentration characteristic of the oil agent is not ideal, the viscosity mutation phenomenon of the oil agent is avoided, monomers with high thermal decomposition temperature, such as a smoothing agent, a bundling agent and an emulsifier, are selected, and more polyether substances (fatty acid polyoxyethylene ester) or polyether substances containing ester bonds are selected, so that the molecular weight distribution of the polyether substances is widened, and the compatibility among the components of the oil agent and the overall stability of the oil agent are improved.
The winding problem of the yarn during spinning is often due to insufficient bundling property and antistatic property of the finish. For antistatic property, the anionic surfactant with polyether structure is adopted, and the invention selects polyether phosphate ester salt and polyether sulfate ester salt, which not only have oleophylic hydrocarbon group, but also have hydrophilic strong polar group, and have strong moisture absorption and conductivity, and simultaneously can keep better antistatic property under various humidity conditions.
The problem of difficult dyeing during dyeing is often solved by the whiting problem during spinning because the spun silk is much whiting. In addition, the dyeing difficulty can be caused due to insufficient sizing property of the oil agent, and the weight percentage of the industrial white oil added into the base oil is 8-17%, so that the sizing property of the oil agent is ensured.
The problem of uneven dyeing during dyeing is often caused by severe foaming or insufficient uniformity of finish during use. For the severe foaming of the oil agent in use, the invention adds the defoaming agent into the additive. The invention adds penetrant and polyoxyethylene laurate for the lack of oil agent uniformity, wherein the polyoxyethylene laurate has good smoothness and bundling property and excellent level dyeing property.
In the oil agent, the base oil, the smoothing agent, the bundling agent, the antistatic agent and the penetrating agent are difficult to form uniform and stable oil agent or emulsion due to obvious difference of hydrophilic-lipophilic balance value (HLB value). Therefore, after the monomer types and contents of the components are determined, the components and contents of the emulsifier need to be reasonably designed, so that the prepared oil agent and oil agent emulsion are uniform and stable, and the particle size of the emulsion is small. The oil agent is used by being prepared into emulsion, so the final oil agent needs to be prepared into partial hydrophily, and the HLB value of the oil agent is 12-18. In addition, stabilizing agents of oleic acid and hexadecanol are added into the additive, so that the oil agent is uniformly dispersed for a long time and is not layered. Meanwhile, the surface tension value of the oil emulsion which is prepared into a certain concentration (generally 15-18%) is also reasonable, and the surface tension value of the oil emulsion after the formula design is 20-40dyn/cm (a test value at room temperature and under standard atmospheric pressure), and the oil emulsion has better performance in various aspects during application.
Preferably, the additive of the oil agent further comprises an anti-yellowing agent, the amount of the anti-yellowing agent is 0.1-2 wt% of the total amount of the oil agent, the molecular weight of the anti-yellowing agent is 1000-1500, and the anti-yellowing agent has the following general molecular structure:
wherein x is the mole number of the oxyethylene group, and R is acyl.
The spun polyester filament yarns are processed into cloth in a textile mill, and then dyed in a printing and dyeing mill, so that a certain circulation period exists, and if the circulation period is too long, the spun polyester filament yarns are easy to turn yellow and affect subsequent processing. After the fabric is yellowed, the fabric needs to be whitened again through certain process treatment before dyeing, and after the fabric is bleached by a substance with strong oxidizing property, the fiber material is oxidized, so that the strength of the fiber is reduced, and the total light reflectivity of the fabric is reduced and the brightness of the fiber is reduced due to the fact that the whiteness is improved through a bluing process. In order to further solve the yellowing problem before processing of the polyester filament yarn and save the bleaching process, so that the fiber has better strength and performance, 0.1-2 wt% of an anti-yellowing agent is added in the preparation of the polyester FDY oiling agent, the general formula of the molecular structure of the anti-yellowing agent is shown as the above formula, the main body of the anti-yellowing agent is thioester, and when the anti-yellowing agent is used, the anti-yellowing agent can effectively decompose hydroperoxide in a system and convert the hydroperoxide into a stable product, so that the system is free of color change, non-toxic and non-colored, and is suitable for the fiber; because the terylene FDY oil agent is prepared into emulsion for use, the anti-yellowing agent in the prior art is usually insoluble in water, and the use of the non-soluble anti-yellowing agent can cause the particle size of the oil agent emulsion to be increased, the emulsion to be dispersed unevenly and even the phenomena of layering and turbidity, therefore, when the anti-yellowing agent is synthesized, a polyoxyethylene chain segment is introduced, and the introduction of the hydrophilic polyoxyethylene chain segment improves the compatibility of the anti-yellowing agent and a water phase and the overall stability of the oil agent emulsion, and on the basis, the anti-yellowing agent can better exert the anti-yellowing performance in the oil agent; in addition, the anti-yellowing agent also has excellent thermal stability and smoothness of polyether substances containing ester bonds, and has the advantages of high oil film strength, low surface tension, high wetting speed, low foaming capacity and high defoaming speed, wherein, the thermal stability endowed by the polyether structure containing ester bonds can meet the requirement of anti-yellowing of oil solution and fiber at a high temperature for a long time, meanwhile, the diester-terminated polyether structure endows excellent smoothness and high oil film strength, the ester bond-containing polyether structure endows low surface tension and high wetting speed, which are beneficial to rapid and uniform oiling, the ester bond-containing polyether structure endows low foaming capacity and high defoaming speed which are consistent with the performance requirements of the oil agent, meanwhile, due to the ester bond, the oiling agent is easier to combine with the polyester fiber containing a large amount of ester bonds, and the anti-yellowing agent is stably attached to the surface of the fiber for a long time after oiling.
Preferably, the preparation method of the anti-yellowing agent comprises the following steps: carrying out condensation reaction on methyl acrylate and hydrogen sulfide at 65-70 ℃ under the catalysis of sodium acetate at 1-3bar to prepare an intermediate product dimethyl thiodipropionate; then, carrying out ester exchange reaction on the intermediate product dimethyl thiodipropionate and polyethylene glycol monolaurate at the temperature of 120 ℃ and 135 ℃ under normal pressure and under the catalysis of sulfuric acid to prepare the anti-yellowing agent; wherein, the mol ratio of the methyl acrylate to the hydrogen sulfide is 2-2.1:1, and the dosage of the sodium acetate is 10-20mol percent of the methyl acrylate; the molar ratio of dimethyl thiodipropionate to polyethylene glycol monolaurate is 1: 2-2.1; the dosage of the sulfuric acid is 5-10 mol% of dimethyl thiodipropionate.
When the anti-yellowing agent is prepared, firstly, methyl acrylate and vulcanization can be subjected to condensation reaction under the catalysis of sodium acetate to prepare a dimethyl thiodipropionate intermediate, then the dimethyl thiodipropionate intermediate is subjected to ester exchange reaction with polyethylene glycol monolaurate under the catalysis of acid, and during the reaction, methanol molecules are continuously removed to prepare the anti-yellowing agent.
A preparation method of a terylene FDY oil agent comprises the following preparation steps:
(1) proportionally adding the emulsifier, the bundling agent, the antistatic agent and the penetrant into a reaction kettle, and stirring at the stirring speed of 500-600r/min at the temperature of 40-70 ℃ for 0.5-1 h;
(2) and (3) putting the base oil and the smoothing agent into the reaction kettle, continuously stirring for 45-60min, then putting the additive, stirring uniformly, naturally cooling and filtering to obtain the terylene FDY oiling agent.
Therefore, the invention has the following beneficial effects:
(1) according to the invention, through selection and proportioning of monomers, the prepared FDY oiling agent has good comprehensive performances of smoothness, bundling, static resistance, permeability, heat resistance, sizing and uniform coating, has good spinnability, greatly reduces abnormal broken filaments, broken ends, white powder, tension fluctuation and winding phenomena, and can obviously improve the high-quality product rate under the same spinning process conditions. In the subsequent printing and dyeing, the phenomena of difficult dyeing and uneven dyeing are reduced, and the M rate of fiber dyeing is improved;
(2) the anti-yellowing agent suitable for being used in the oil agent is prepared, so that the FDY oil agent has excellent anti-yellowing capability, the yellowing phenomenon of fiber products in long-term circulation is reduced, and the investment on a whitening process before dyeing is reduced or even the whitening process before dyeing is omitted.
Detailed Description
The invention will now be further described with reference to specific embodiments in which the numbers in brackets for the components are the average addition number of polyoxyethylene.
General example: the terylene FDY oiling agent comprises the following components in percentage by weight: 14-33% of base oil, 24-38% of smoothing agent, 7-11% of bundling agent, 7-11% of emulsifier, 5-7% of antistatic agent, 1-3% of penetrating agent and the balance of additive;
the preparation method of the terylene FDY oiling agent comprises the following preparation steps:
(1) proportionally adding the emulsifier, the bundling agent, the antistatic agent and the penetrant into a reaction kettle, and stirring at the stirring speed of 500-600r/min at the temperature of 40-70 ℃ for 0.5-1 h;
(2) adding the base oil and the smoothing agent into a reaction kettle, continuously stirring for 45-60min, then adding the additive, stirring uniformly, naturally cooling and filtering to obtain a terylene FDY oiling agent;
the additive of the oil agent also comprises an anti-yellowing agent, the dosage of the anti-yellowing agent is 0.1-2 wt% of the total amount of the oil agent, and the molecular weight of the anti-yellowing agent is 1000-1500; the preparation method of the anti-yellowing agent comprises the following steps: carrying out condensation reaction on methyl acrylate and hydrogen sulfide at 65-70 ℃ under the catalysis of sodium acetate at 1-3bar to prepare an intermediate product dimethyl thiodipropionate; then, carrying out ester exchange reaction on the intermediate product dimethyl thiodipropionate and polyethylene glycol monolaurate at the temperature of 120 ℃ and 135 ℃ under normal pressure and under the catalysis of sulfuric acid to prepare the anti-yellowing agent; wherein, the mol ratio of the methyl acrylate to the hydrogen sulfide is 2-2.1:1, and the dosage of the sodium acetate is 10-20mol percent of the methyl acrylate; the molar ratio of dimethyl thiodipropionate to polyethylene glycol monolaurate is 1: 2-2.1; the dosage of the sulfuric acid is 5-10 mol% of dimethyl thiodipropionate;
example 1: the terylene FDY oiling agent comprises the following components in percentage by weight:
31% of base oil, 19% of trimethylolpropane oleate and 12% of industrial white oil;
35% of smoothing agent, wherein 25% of oleic acid polyethylene glycol 600 diester and 10% of C12-C14 fatty alcohol block polyoxyethylene polyoxypropylene ether;
11% of a bundling agent, wherein 8% of oleic acid polyethylene glycol 400 diester and 3% of isomeric tridecanol polyoxyethylene (6) ether;
11% of emulsifier, wherein 5% of sorbitan polyoxyethylene (80) ether stearate and 6% of polyoxyethylene (9) laurate;
7% of antistatic agent, wherein the content of C12-C14 fatty alcohol polyoxyethylene (3) ether phosphate potassium salt is 7%;
3% of penetrating agent, namely 3% of C12-C14 fatty alcohol block polyoxyethylene polyoxypropylene ether;
1.5 percent of additive, wherein the content of p-hydroxyacetophenone is 0.1 percent, the content of polyether modified silicone oil is 0.1 percent, the content of stearic acid polyoxypropylene (5) ester is 0.5 percent, the content of glycerol random polyoxyethylene polyoxypropylene ether is 0.6 percent, and the content of hexadecanol is 0.2 percent;
the preparation method of the terylene FDY oiling agent comprises the following preparation steps:
(1) proportionally adding the emulsifier, the bundling agent, the antistatic agent and the penetrant into a reaction kettle, and stirring at the stirring speed of 500r/min for 1h at the temperature of 60 ℃;
(2) and (3) putting the base oil and the smoothing agent into the reaction kettle, continuously stirring for 50min, then putting the additive, stirring uniformly, naturally cooling and filtering to obtain the polyester FDY oiling agent.
Example 2: the terylene FDY oiling agent comprises the following components in percentage by weight:
30% of base oil, 10% of isooctyl stearate, 10% of trimethylolpropane oleate and 10% of industrial white oil;
38% of smoothing agent, wherein 20% of lauric acid polyethylene glycol 400 diester and C12-C1418% of fatty alcohol block polyoxyethylene polyoxypropylene ether;
11% of bundling agent, wherein 7% of ricinoleic acid polyoxyethylene (20) ester and C4-C12Fatty alcohol random polyoxyethylene polyoxypropylene ether 4%;
10% of emulsifier, wherein the sorbitan polyoxyethylene (80) ether stearate is 3%, the oleic acid polyoxyethylene (3) ester is 3%, and the lauric acid polyoxyethylene (9) ester is 4%;
antistatic agent 7%, wherein C12-C14Fatty alcohol polyoxyethylene (3) ether phosphate potassium salt 3%, C12-C144% of fatty alcohol polyoxyethylene (3) ether sulfate sodium salt;
penetrant 2%, i.e. C12-C142% of fatty alcohol block polyoxyethylene polyoxypropylene ether;
1 percent of additive, wherein 0.1 percent of p-hydroxyacetophenone, 0.1 percent of polyether modified silicone oil, 0.3 percent of stearic acid polyoxypropylene (5) ester, 0.3 percent of glycerol random polyoxyethylene polyoxypropylene ether and 0.2 percent of hexadecanol;
the preparation method of the terylene FDY oiling agent comprises the following preparation steps:
(1) proportionally adding the emulsifier, the bundling agent, the antistatic agent and the penetrant into a reaction kettle, and stirring at the stirring speed of 600r/min for 0.5h at 70 ℃;
(2) and (3) putting the base oil and the smoothing agent into the reaction kettle, continuously stirring for 55min, then putting the additive, stirring uniformly, naturally cooling and filtering to obtain the polyester FDY oiling agent.
Example 3: the terylene FDY oiling agent comprises the following components in percentage by weight:
33% of base oil, wherein the content of isooctyl stearate is 10%, the content of isooctyl oleate is 3%, the content of trimethylolpropane oleate is 10%, and the content of industrial white oil is 10%;
36% of smoothing agent, wherein 14% of oleic acid polyethylene glycol 600 diester, 8% of lauric acid polyethylene glycol 400 diester, and 14% of C12-C14 fatty alcohol block polyoxyethylene polyoxypropylene ether;
10% of bundling agent, wherein 4% of oleic acid polyethylene glycol 400 diester, 3% of ricinoleic acid polyoxyethylene (20) ester and 3% of C4-C12 fatty alcohol random polyoxyethylene polyoxypropylene ether;
10% of emulsifier, wherein the sorbitan polyoxyethylene (80) ether stearate is 3%, the oleic acid polyoxyethylene (5) ester is 4%, and the lauric acid polyoxyethylene (9) ester is 3%;
6 percent of antistatic agent, wherein the content of C12-C14 fatty alcohol polyoxyethylene (3) ether phosphate potassium salt is 3 percent, and the content of C12-C14 fatty alcohol polyoxyethylene (3) ether sulfate sodium salt is 3 percent;
2% of penetrating agent, namely 2% of C12-C14 fatty alcohol block polyoxyethylene polyoxypropylene ether;
1.5 percent of additive, wherein the content of p-hydroxyacetophenone is 0.1 percent, the content of polyether modified silicone oil is 0.1 percent, the content of stearic acid polyoxypropylene (5) ester is 0.5 percent, the content of glycerol random polyoxyethylene polyoxypropylene ether is 0.6 percent, and the content of oleic acid is 0.2 percent;
the preparation method of the terylene FDY oiling agent comprises the following preparation steps:
(1) proportionally adding the emulsifier, the bundling agent, the antistatic agent and the penetrant into a reaction kettle, and stirring at the stirring speed of 650r/min for 0.7h at 40 ℃;
(2) and (3) putting the base oil and the smoothing agent into the reaction kettle, continuously stirring for 45min, then putting the additive, stirring uniformly, naturally cooling and filtering to obtain the polyester FDY oiling agent.
Example 4: the terylene FDY oiling agent comprises the following components in percentage by weight:
31% of base oil, 19% of trimethylolpropane oleate and 12% of industrial white oil;
35% of smoothing agent, wherein 25% of oleic acid polyethylene glycol 600 diester and 10% of C12-C14 fatty alcohol block polyoxyethylene polyoxypropylene ether;
11% of a bundling agent, wherein 8% of oleic acid polyethylene glycol 400 diester and 3% of isomeric tridecanol polyoxyethylene (6) ether;
11% of emulsifier, wherein 5% of sorbitan polyoxyethylene (80) ether stearate and 6% of polyoxyethylene (9) laurate;
7% of antistatic agent, wherein the content of C12-C14 fatty alcohol polyoxyethylene (3) ether phosphate potassium salt is 7%;
3% of penetrating agent, namely 3% of C12-C14 fatty alcohol block polyoxyethylene polyoxypropylene ether;
2 percent of additive, wherein the invention is specially made 0.5 percent of anti-yellowing agent, 0.1 percent of p-hydroxyacetophenone, 0.1 percent of polyether modified silicone oil, 0.5 percent of stearic acid polyoxypropylene (5) ester, 0.6 percent of glycerol random polyoxyethylene polyoxypropylene ether and 0.2 percent of hexadecanol;
the preparation method of the anti-yellowing agent comprises the following steps: carrying out condensation reaction on methyl acrylate and hydrogen sulfide at 70 ℃ under the catalysis of sodium acetate at 3bar to prepare an intermediate product dimethyl thiodipropionate; then, carrying out ester exchange reaction on the intermediate product dimethyl thiodipropionate and polyethylene glycol monolaurate at 135 ℃ under normal pressure and the catalysis of sulfuric acid to prepare the anti-yellowing agent; wherein, the mol ratio of the methyl acrylate to the hydrogen sulfide is 2.1:1, and the dosage of the sodium acetate is 18mol percent of the methyl acrylate; the molar ratio of dimethyl thiodipropionate to polyethylene glycol monolaurate is 1: 2.1; the dosage of the sulfuric acid is 9mol percent of dimethyl thiodipropionate.
The preparation method of the terylene FDY oiling agent comprises the following preparation steps:
(1) proportionally adding the emulsifier, the bundling agent, the antistatic agent and the penetrant into a reaction kettle, and stirring at the stirring speed of 500r/min for 1h at the temperature of 60 ℃;
(2) and (3) putting the base oil and the smoothing agent into the reaction kettle, continuously stirring for 50min, then putting the additive, stirring uniformly, naturally cooling and filtering to obtain the polyester FDY oiling agent.
Example 5: the terylene FDY oiling agent comprises the following components in percentage by weight:
30% of base oil, 10% of isooctyl stearate, 10% of trimethylolpropane oleate and 10% of industrial white oil;
38% of smoothing agent, wherein 20% of lauric acid polyethylene glycol 400 diester and C12-C1418% of fatty alcohol block polyoxyethylene polyoxypropylene ether;
11% of bundling agent, wherein 7% of ricinoleic acid polyoxyethylene (20) ester and C4-C12Fatty alcohol random polyoxyethylene polyoxypropylene ether 4%;
10% of emulsifier, wherein the sorbitan polyoxyethylene (80) ether stearate is 3%, the oleic acid polyoxyethylene (3) ester is 3%, and the lauric acid polyoxyethylene (9) ester is 4%;
antistatic agent 7%, wherein C12-C14Fatty alcohol polyoxyethylene (3) ether phosphate potassium salt 3%, C12-C144% of fatty alcohol polyoxyethylene (3) ether sulfate sodium salt;
penetrant 2%, i.e. C12-C142% of fatty alcohol block polyoxyethylene polyoxypropylene ether;
2 percent of additive, wherein the anti-yellowing agent is 1 percent, the p-hydroxyacetophenone is 0.1 percent, the polyether modified silicone oil is 0.1 percent, the stearic acid polyoxypropylene (5) ester is 0.3 percent, the glycerol random polyoxyethylene polyoxypropylene ether is 0.3 percent, and the hexadecanol is 0.2 percent;
the preparation method of the anti-yellowing agent comprises the following steps: carrying out condensation reaction on methyl acrylate and hydrogen sulfide at 65 ℃ under the catalysis of sodium acetate at 1bar to prepare an intermediate product dimethyl thiodipropionate; then, carrying out ester exchange reaction on the intermediate product dimethyl thiodipropionate and polyethylene glycol monolaurate under the catalysis of sulfuric acid at 120 ℃ and normal pressure to prepare the anti-yellowing agent; wherein, the mol ratio of the methyl acrylate to the hydrogen sulfide is 2:1, and the using amount of the sodium acetate is 10mol percent of the methyl acrylate; the molar ratio of dimethyl thiodipropionate to polyethylene glycol monolaurate is 1: 2; the dosage of the sulfuric acid is 5mol percent of dimethyl thiodipropionate.
The preparation method of the terylene FDY oiling agent comprises the following preparation steps:
(1) proportionally adding the emulsifier, the bundling agent, the antistatic agent and the penetrant into a reaction kettle, and stirring at the stirring speed of 600r/min for 0.5h at 70 ℃;
(2) and (3) putting the base oil and the smoothing agent into the reaction kettle, continuously stirring for 55min, then putting the additive, stirring uniformly, naturally cooling and filtering to obtain the polyester FDY oiling agent.
Example 6: the terylene FDY oiling agent comprises the following components in percentage by weight:
33% of base oil, wherein the content of isooctyl stearate is 10%, the content of isooctyl oleate is 3%, the content of trimethylolpropane oleate is 10%, and the content of industrial white oil is 10%;
36% of smoothing agent, wherein 14% of oleic acid polyethylene glycol 600 diester, 8% of lauric acid polyethylene glycol 400 diester, and 14% of C12-C14 fatty alcohol block polyoxyethylene polyoxypropylene ether;
10% of bundling agent, wherein 4% of oleic acid polyethylene glycol 400 diester, 3% of ricinoleic acid polyoxyethylene (20) ester and 3% of C4-C12 fatty alcohol random polyoxyethylene polyoxypropylene ether;
10% of emulsifier, wherein the sorbitan polyoxyethylene (80) ether stearate is 3%, the oleic acid polyoxyethylene (5) ester is 4%, and the lauric acid polyoxyethylene (9) ester is 3%;
6 percent of antistatic agent, wherein the content of C12-C14 fatty alcohol polyoxyethylene (3) ether phosphate potassium salt is 3 percent, and the content of C12-C14 fatty alcohol polyoxyethylene (3) ether sulfate sodium salt is 3 percent;
2% of penetrating agent, namely 2% of C12-C14 fatty alcohol block polyoxyethylene polyoxypropylene ether;
3 percent of additive, wherein the anti-yellowing agent specially prepared in the invention is 1.5 percent, 0.1 percent of p-hydroxyacetophenone, 0.1 percent of polyether modified silicone oil, 0.5 percent of stearic acid polyoxypropylene (5) ester, 0.6 percent of glycerol random polyoxyethylene polyoxypropylene ether and 0.2 percent of oleic acid;
the preparation method of the anti-yellowing agent comprises the following steps: carrying out condensation reaction on methyl acrylate and hydrogen sulfide at 70 ℃ under 2bar under the catalysis of sodium acetate to prepare an intermediate product dimethyl thiodipropionate; then, carrying out ester exchange reaction on the intermediate product dimethyl thiodipropionate and polyethylene glycol monolaurate at 125 ℃ under normal pressure and the catalysis of sulfuric acid to prepare the anti-yellowing agent; wherein the molar ratio of the methyl acrylate to the hydrogen sulfide is 2.1:1, and the using amount of the sodium acetate is 15mol percent of the methyl acrylate; the molar ratio of dimethyl thiodipropionate to polyethylene glycol monolaurate is 1: 2; the dosage of the sulfuric acid is 7mol percent of dimethyl thiodipropionate.
The preparation method of the terylene FDY oiling agent comprises the following preparation steps:
(1) proportionally adding the emulsifier, the bundling agent, the antistatic agent and the penetrant into a reaction kettle, and stirring at the stirring speed of 650r/min for 0.7h at 40 ℃;
(2) and (3) putting the base oil and the smoothing agent into the reaction kettle, continuously stirring for 45min, then putting the additive, stirring uniformly, naturally cooling and filtering to obtain the polyester FDY oiling agent.
The appearance of the terylene FDY oiling agent prepared by the invention is light yellow transparent liquid (at 25 ℃), the pH value is 6.9 +/-0.9, and 15% oiling agent emulsion is stable and does not delaminate and change within 72 hours at 25 ℃.
The oil solutions of examples 1-6 were compared with commercially available Wujiang Yangliang Dacron FDY oil solution D2002, and the data of the basic performance index test are shown in the following table.
From the data, compared with the commercially available Wujiang Yanglan polyester FDY oiling agent D2002, the polyester FDY oiling agent prepared by the invention has better basic performance, and after the anti-yellowing agent is added (examples 4-6), the polyester FDY oiling agent prepared by the invention also has better anti-yellowing capability.
Spinning tests were carried out on the oil prepared in the example of the invention and FDY oil D2002 of Wujiang Yanglan polyester sold in the market, and the results are shown in the following table, wherein the appearance and whiteness are obtained by observing and measuring fibers subjected to oiling treatment by different oils after being stored in the same environment for the same time (25 ℃, 20% RH and 30 days).
The above table shows that the polyester FDY oil agent prepared by the method has excellent spinnability, is not easy to cause abnormal phenomena such as broken filaments, broken ends, white powder, tension fluctuation, winding and the like in the spinning process of fibers, and obviously improves the rate of qualified spinning products; in the subsequent printing and dyeing, the M rate of fiber dyeing is obviously improved, the phenomena of difficult dyeing, uneven dyeing and the like are not easy to appear, and the fiber treated by adding the oil agent (examples 4-6) of the special antioxidant disclosed by the invention has no yellowing on the surface after being stored for 30 days, and is little in whiteness reduction and basically unchanged.
The raw materials and equipment used in the invention are common raw materials and equipment in the field if not specified; the methods used in the present invention are conventional in the art unless otherwise specified.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and all simple modifications, alterations and equivalents of the above embodiments according to the technical spirit of the present invention are still within the protection scope of the technical solution of the present invention.
Claims (10)
1. The terylene FDY oiling agent is characterized by comprising the following components in percentage by weight: 14-33% of base oil, 24-38% of smoothing agent, 7-11% of bundling agent, 7-11% of emulsifier, 5-7% of antistatic agent, 1-3% of penetrating agent and the balance of additive.
2. The polyester FDY finish of claim 1 wherein the base oil comprises one or more of isooctyl stearate, isooctyl oleate, diisooctyl sebacate, trimethylolpropane oleate, pentaerythritol oleate, and technical white oils; the smoothing agent comprises one or more of oleic acid polyethylene glycol 600 diester, lauric acid polyethylene glycol 400 diester and C12-C14 fatty alcohol block polyoxyethylene polyoxypropylene ether, wherein PO/EO of the C12-C14 fatty alcohol block polyoxyethylene polyoxypropylene ether is 1.7-5.7, and the molecular weight is 600-1200.
3. The terylene FDY oil agent according to claim 1, wherein the bundling agent comprises one or more of oleic acid polyethylene glycol 400 diester, ricinoleic acid polyoxyethylene ester, isomeric tridecanol polyoxyethylene ether, C4-C12 fatty alcohol random polyoxyethylene polyoxypropylene ether; the average addition number of polyoxyethylene in the polyoxyethylene ricinoleate is 20; the average addition number of polyoxyethylene in the isomeric tridecanol polyoxyethylene ether is 3-12; the C4-C12 fatty alcohol random polyoxyethylene polyoxypropylene ether has EO/PO of 1-2.3 and molecular weight of 1150-1600.
4. The terylene FDY oiling agent of claim 1, wherein the emulsifier comprises one or more of sorbitan polyoxyethylene ether stearate, oleic acid polyoxyethylene ester and lauric acid polyoxyethylene ester; the average addition number of polyoxyethylene in the sorbitan polyoxyethylene ether stearate is 80; the average addition number of polyoxyethylene in the polyoxyethylene oleate is 3; the average addition number of polyoxyethylene in the polyoxyethylene oleate is 5; the average addition number of polyoxyethylene in the polyoxyethylene laurate is 9.
5. The terylene FDY oil agent according to claim 1, wherein the antistatic agent comprises one or more of C12-C14 fatty alcohol polyoxyethylene ether phosphate potassium salt, C12-C14 fatty alcohol polyoxyethylene ether sulfate sodium/potassium salt; the average addition number of polyoxyethylene in the C12-C14 fatty alcohol polyoxyethylene ether phosphate potassium salt is 3; the average addition number of polyoxyethylene in the C12-C14 fatty alcohol polyoxyethylene ether sodium sulfate/potassium salt is 3.
6. The terylene FDY oiling agent as defined in claim 1, wherein the penetrating agent comprises C12-C14 fatty alcohol block polyoxyethylene polyoxypropylene ether, EO/PO of which is 1-1.4, and the molecular weight is 950-1500.
7. The polyester FDY oiling agent according to claim 1, wherein the additives comprise bacteriostatic agent, surface tension reducer, oil film enhancer, defoaming agent and stabilizer; the bacteriostatic agent is an acetophenone compound; the surface tension reducing agent is polyether modified silicone oil; the oil film reinforcing agent is polyoxypropylene stearate, and the average addition number of polyoxyethylene is 5; the defoaming agent is glycerol random polyoxyethylene polyoxypropylene ether, the EO/PO of the glycerol random polyoxyethylene polyoxypropylene ether is 0.5-1.3, and the molecular weight of the glycerol random polyoxyethylene polyoxypropylene ether is 2700-3300; the stabilizer is one of cetyl alcohol or oleic acid.
8. The polyester FDY oiling agent as defined in claim 1, wherein the additive of the oiling agent further comprises an anti-yellowing agent, the amount of the anti-yellowing agent is 0.1-2 wt% of the total amount of the oiling agent, the molecular weight of the anti-yellowing agent is 1000-1500, and the anti-yellowing agent has the following general molecular structure:
wherein x is the mole number of the oxyethylene group, and R is acyl.
9. The polyester FDY oiling agent as defined in claim 8, wherein the preparation method of the anti-yellowing agent comprises the following steps: carrying out condensation reaction on methyl acrylate and hydrogen sulfide at 65-70 ℃ under the catalysis of sodium acetate at 1-3bar to prepare an intermediate product dimethyl thiodipropionate; then, carrying out ester exchange reaction on the intermediate product dimethyl thiodipropionate and polyethylene glycol monolaurate at the temperature of 120 ℃ and 135 ℃ under normal pressure and under the catalysis of sulfuric acid to prepare the anti-yellowing agent; wherein, the mol ratio of the methyl acrylate to the hydrogen sulfide is 2-2.1:1, and the dosage of the sodium acetate is 10-20mol percent of the methyl acrylate; the molar ratio of dimethyl thiodipropionate to polyethylene glycol monolaurate is 1: 2-2.1; the dosage of the sulfuric acid is 5-10 mol% of dimethyl thiodipropionate.
10. The preparation method of the terylene FDY oiling agent according to any one of claims 1 to 9, which is characterized by comprising the following preparation steps:
(1) proportionally adding the emulsifier, the bundling agent, the antistatic agent and the penetrant into a reaction kettle, and stirring at the stirring speed of 500-600r/min at the temperature of 40-70 ℃ for 0.5-1 h;
(2) and (3) putting the base oil and the smoothing agent into the reaction kettle, continuously stirring for 45-60min, then putting the additive, uniformly stirring, naturally cooling and filtering to obtain the polyester FDY oiling agent.
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