Synthetic fiber treating agent as well as preparation method and application thereof

Abstract

The invention discloses a synthetic fiber treating agent as well as a preparation method and application thereof, and belongs to the technical field of fiber treating agents. The synthetic fiber treating agent provided by the invention is prepared from the following raw materials in percentage by mass: 3 to 8 percent of antistatic agent, 5 to 10 percent of cationic surfactant, 15 to 25 percent of high-temperature lubricating ester, 10 to 15 percent of nonionic emulsifier, 0.1 to 0.5 percent of antioxidant and the balance of water, the antistatic agent comprises organic phosphonate. According to the invention, the organic phosphonate and the cationic surfactant are compounded and synergistically form ion pairs, so that the static dissipation efficiency is enhanced, the antistatic durability and stability of the synthetic fiber treating agent are improved, and the treating agent can be applied to a high-speed spinning process of synthetic fibers such as polyester or chinlon.

Description

Technical Field

[0001] The present invention relates to the technical field of fiber treatment agents, in particular to a synthetic fiber treatment agent and a preparation method and application thereof. Background Art

[0002] During the production of synthetic fibers, high-speed friction between the fibers and processing equipment can easily lead to static electricity accumulation, resulting in fiber entanglement and increased breakage rates. At the same time, static electricity can absorb dust and thus affect fiber cleanliness. To address these problems, a treatment agent with good surface adhesion stability is needed for synthetic fibers. Traditional treatment agents often use substances such as quaternary ammonium salts and phosphate esters as surfactants, which are prone to thermal decomposition in high-temperature spinning processes, producing volatile substances that pollute the environment, or forming white powder deposition on the surface of the hot roller, thereby reducing the heat transfer efficiency of the equipment. Patent application publication number CN 116837495 A discloses a polyester industrial yarn oil agent, which uses neopentyl polyol isostearate and Gemini surfactant compound. Although it can reduce white powder deposition, its antistatic component relies on sulfonate-type anionic surfactants, and its antistatic performance is limited.

[0003] Organic phosphonate treatment agents contain both hydrophobic alkyl chains and electrophilic phosphonic acid groups in their molecules, and exhibit thermal stability. However, in actual applications, they lack compatibility with other components in the fiber treatment agent, which easily leads to oil stratification and makes it difficult to meet the requirements of excellent antistatic properties during high-speed spinning.

[0004] Therefore, how to provide a synthetic fiber treatment agent with both stability and antistatic properties is an urgent problem to be solved in this field. Summary of the Invention

[0005] In response to the above-mentioned problems in the prior art, the applicant of the present invention provides a synthetic fiber treatment agent and its preparation method and application. The synthetic fiber treatment agent provided by the present invention is a compound of an organic phosphonate and a cationic surfactant, and has excellent antistatic properties and good stability.

[0006] The technical solutions of the present invention are as follows:

[0007] The first aspect of the present invention provides a synthetic fiber treatment agent comprising the following raw materials in percentage by weight: 3-8% antistatic agent, 5-10% cationic surfactant, 15-25% high-temperature lubricating ester, 10-15% nonionic emulsifier, 0.1-0.5% antioxidant, and the balance being water;

[0008] The antistatic agent includes an organic phosphonate.

[0009] Preferably, the organic phosphonate is potassium octylphosphonate monoethyl ester, and the chemical structural formula of potassium octylphosphonate monoethyl ester is as follows:

[0010]

[0011] Preferably, the cationic surfactant is octadecyldimethylhydroxyethylammonium chloride.

[0012] Preferably, the high-temperature lubricating ester is pentaerythritol fatty acid ester, preferably, the high-temperature lubricating ester is pentaerythritol tetraoleate.

[0013] Preferably, the nonionic emulsifier is polyoxyethylene monooleate.

[0014] Preferably, the antioxidant is dilauryl thiodipropionate.

[0015] The second aspect of the present invention is to protect a method for preparing the synthetic fiber treating agent of the first aspect, comprising the following steps, in percentage by mass:

[0016] S1, mixing the antistatic agent, the cationic surfactant, and the nonionic emulsifier at temperature T1 to form a pre-emulsified phase;

[0017] S2, adding the high-temperature lubricating ester and the antioxidant to the pre-emulsified phase, heating to temperature T2, and stirring until a homogeneous phase is obtained;

[0018] S3. Add water to the homogeneous phase, perform high-speed homogenization and emulsification, and then cool to temperature T3 to obtain a synthetic fiber treating agent.

[0019] Preferably, in step S1, the temperature T1 is 50-60°C, and the mixing time is 20-40 minutes;

[0020] In step S2, the temperature T2 is 70-80°C.

[0021] Preferably, in step S3, the temperature T3 is not higher than 40°C;

[0022] And / or, the high-speed homogenization emulsification rate is 5000-8000 rpm, and the time is 15-25 min.

[0023] The third aspect of the present invention protects the use of the synthetic fiber treatment agent described in the first aspect, and / or the synthetic fiber treatment agent prepared by the preparation method described in the second aspect in a synthetic fiber high-speed spinning process.

[0024] The beneficial technical effects of the present invention are:

[0025] (1) In the synthetic fiber treatment agent provided by the present invention, the organic phosphonate can form a conductive layer on the surface of the synthetic fiber, neutralize static electricity through ion migration, and the positively charged groups in the cationic surfactant can be bound to the fiber surface through electrostatic adsorption, thereby reducing the surface resistance of the fiber. In addition, the organic phosphonate and the cationic surfactant can synergistically form ion pairs, thereby improving the stability of the treatment agent and further enhancing the static dissipation efficiency, thereby improving the antistatic durability of the synthetic fiber treatment agent.

[0026] (2) Compared with most existing cationic surfactants and anionic surfactants, which produce precipitation when compounded and make the synthetic fiber treatment agent lose its effect, the anionic organic phosphonate selected in the present invention is compounded with a cationic surfactant and, after high-speed homogenization, can form a stable emulsion-like liquid treatment agent for treating synthetic fibers. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] Figure 1 This is an infrared spectrum of potassium monoethyl octylphosphonate prepared in Example 1 of the present invention.

[0028] Figure 2 This is the mass spectrum of potassium monoethyl octylphosphonate prepared in Example 1 of the present invention. DETAILED DESCRIPTION

[0029] The present invention will be described in detail below with reference to the embodiments and accompanying drawings.

[0030] In certain embodiments, the synthetic fiber treatment agent provided by the present invention selects potassium monoethyl octylphosphonate as an antistatic agent and selects octadecyl dimethyl hydroxyethyl ammonium chloride as a cationic surfactant. Wherein, potassium monoethyl octylphosphonate has good thermal stability, can form a conductive layer on the fiber surface, and neutralizes static electricity by ion migration. Octadecyl dimethyl hydroxyethyl ammonium chloride has a lipophilic chain structure, and the positively charged quaternary ammonium group firmly binds to the fiber surface by electrostatic adsorption, reducing surface resistance. In addition, potassium monoethyl octylphosphonate can form an ion pair with octadecyl dimethyl hydroxyethyl ammonium chloride, improves the stability of the treatment agent, also enhances static dissipation efficiency, and then improves the antistatic persistence of the treatment agent.

[0031] In some embodiments, the high temperature lubricating ester is a pentaerythritol fatty acid ester. Preferably, the carbon chain length of the fatty acid is C 16 -C 18 Among them, the tetrahydroxy structure can form a dense ester film, which is resistant to high temperature oxidation, so that the treating agent can remain stable in the high-temperature high-speed spinning process of synthetic fibers. 16 -C 18 The long carbon chain fatty acids have weak softness, which can provide low friction coefficient and reduce the wear of spinning machinery. 16 -C18 The price of long-chain fatty acids is relatively stable and low-cost, which is conducive to the industrial production and application of treatment agents. In addition, the ester group has good compatibility with the polar groups of fibers (such as the ester group of polyester), which can enhance film adhesion.

[0032] In some embodiments, the nonionic emulsifier is polyoxyethylene monooleate, specifically PEG400MO, and the ethylene oxide addition number is 8-12.

[0033] In some embodiments, the synthetic fiber treating agent is an emulsion liquid.

[0034] In some embodiments, when the synthetic fiber treating agent is used in a synthetic fiber high-speed spinning process, it is applied to the fiber surface by dipping or spraying.

[0035] Example 1

[0036] A synthetic fiber treating agent comprises the following raw materials in percentage by weight: 3% potassium monoethyl octylphosphonate, 10% octadecyldimethylhydroxyethylammonium chloride, 25% pentaerythritol fatty acid ester, 10% polyoxyethylene monooleate PEG400MO, 0.5% dilauryl thiodipropionate, and 51.5% deionized water.

[0037] Wherein, the potassium monoethyl octylphosphonate is prepared by the following method:

[0038] (1) 0.2 mol of 1-bromooctane and 0.2 mol of triethyl phosphite were mixed uniformly and transported into the microreactor at a constant flow rate of 87 μL / min using a horizontal flow pump. The mixed raw materials were reacted in an oil bath at 180°C for 3 h under the control of the flow rate of 87 μL / min.

[0039] (2) After the reaction was completed, the temperature was lowered to 120°C and distilled under reduced pressure for 8 hours to obtain 0.196 mol of the intermediate product diethyl octylphosphonate.

[0040] (3) 0.1 mol of diethyl octylphosphonate was added to a three-necked flask, and 20.57 g of a 30% KOH aqueous solution was added dropwise at 120° C. under magnetic stirring. The ester was then hydrolyzed at 120° C. for 6 h. After the reaction was completed, potassium monoethyl octylphosphonate was obtained.

[0041] The intermediate product diethyl octylphosphonate (a) and the product potassium monoethyl octylphosphonate (b) in the above preparation process were tested by Fourier transform infrared spectrometer. The results are as follows: Figure 1 As shown. Figure 1 It can be seen that in the two spectral lines, 2840-2960cm -1 The stretching vibration peaks of CH2 and CH3 are at 1350-1470cm -1The peaks are the bending vibration peaks of CH2 and CH3. Figure 1 In spectral line a, 1245cm -1 The peak of P=O stretching vibration is 1022cm -1 The peak is the stretching vibration peak of POC. Figure 1 Spectral line b, 3000-3600cm -1 The stretching vibration peak of OH is at 1170 cm -1 The peak of P=O stretching vibration is 1043 cm -1 The peak at 1646cm is the stretching vibration peak of POC. -1 The peak at 37° is the O=P-OH stretching vibration peak, which proves that potassium monoethyl octylphosphonate has been synthesized.

[0042] Take the above-prepared potassium monoethyl octylphosphonate and perform mass spectrometry detection. The results are as follows: Figure 2 As shown. Figure 2 The results show that M is potassium monoethyl octylphosphonate (260.35 g / mol); m / z = 261 is [M+1H + ] mass spectrum peak; m / z=223 is the fragment structure [M-1K - ]; m / z=195 is a fragment structure [M-1K - -1C2H4]; the mass spectrum peak at m / z = 251 is the intermediate diethyl octylphosphonate, proving the synthesis of potassium monoethyl octylphosphonate.

[0043] A method for preparing a synthetic fiber treating agent comprises the following steps, in percentage by mass:

[0044] S1. Mix the formulated amounts of potassium monoethyl octylphosphonate, octadecyldimethylhydroxyethylammonium chloride, and polyoxyethylene monooleate PEG400MO at 55° C. for 30 minutes to form a pre-emulsified phase.

[0045] S2. Add the formulated amount of pentaerythritol tetraoleate and dilauryl thiodipropionate to the pre-emulsified phase, raise the temperature to 75° C., and stir until the phase becomes homogeneous.

[0046] S3. Slowly add the formulated amount of deionized water to the homogeneous phase, and emulsify for 20 minutes in a high-speed homogenizer at an emulsification rate of 6500 rpm. After the emulsification is completed, cool the mixture to below 40° C. and discharge the mixture to obtain a synthetic fiber treating agent, which is a light yellow emulsion-like liquid.

[0047] Example 2

[0048] A synthetic fiber treating agent comprises the following raw materials in percentage by weight: 5% potassium monoethyl octylphosphonate, 5% octadecyldimethylhydroxyethylammonium chloride, 20% pentaerythritol fatty acid ester, 12% polyoxyethylene monooleate PEG400MO, 0.3% dilauryl thiodipropionate, and 57.7% deionized water.

[0049] The preparation method of the potassium monoethyl octylphosphonate is the same as that in Example 1.

[0050] A method for preparing a synthetic fiber treating agent is basically the same as that of Example 1, except that the raw material components described in this example are used.

[0051] Example 3

[0052] A synthetic fiber treating agent comprises the following raw materials in percentage by weight: 8% potassium monoethyl octylphosphonate, 8% octadecyldimethylhydroxyethyl ammonium chloride, 15% pentaerythritol fatty acid ester, 15% polyoxyethylene monooleate PEG400MO, 0.1% dilauryl thiodipropionate, and 53.9% deionized water.

[0053] A method for preparing potassium monoethyl octylphosphonate is the same as that in Example 1.

[0054] A preparation method of a synthetic fiber treating agent is the same as that of Example 1.

[0055] Example 4

[0056] A synthetic fiber treating agent comprises the following raw materials in percentage by weight: 8% potassium monoethyl octylphosphonate, 5% octadecyldimethylhydroxyethylammonium chloride, 20% pentaerythritol fatty acid ester, 12% polyoxyethylene monooleate PEG400MO, 0.3% dilauryl thiodipropionate, and 54.7% deionized water.

[0057] A method for preparing potassium monoethyl octylphosphonate is the same as that in Example 1.

[0058] A preparation method of a synthetic fiber treating agent is the same as that of Example 1.

[0059] Comparative Example 1

[0060] A synthetic fiber treating agent comprises the following raw materials in percentage by mass: 20% of pentaerythritol fatty acid ester, 15% of polyoxyethylene monooleate PEG400MO, 0.3% of dilauryl thiodipropionate, and 64.7% of deionized water.

[0061] A method for preparing a synthetic fiber treating agent comprises the following steps, in percentage by mass:

[0062] S1. Add the formulated amount of polyoxyethylene monooleate PEG400MO at 55°C to form a pre-emulsified phase.

[0063] S2. Add the formulated amount of pentaerythritol tetraoleate and dilauryl thiodipropionate to the pre-emulsified phase, raise the temperature to 75° C., and stir until the phase becomes homogeneous.

[0064] S3. Slowly add the formulated amount of deionized water to the homogeneous phase, and emulsify the phase in a high-speed homogenizer at a controlled emulsification rate of 6500 rpm. After emulsification, cool the phase to below 40° C. and discharge the phase to obtain a synthetic fiber treating agent.

[0065] Comparative Example 2

[0066] A synthetic fiber treating agent comprises the following raw materials in percentage by mass: 8% potassium monoethyl octylphosphonate, 20% pentaerythritol fatty acid ester, 12% polyoxyethylene monooleate PEG400MO, 0.3% dilauryl thiodipropionate, and 59.7% deionized water.

[0067] A method for preparing potassium monoethyl octylphosphonate is the same as that in Example 1.

[0068] A method for preparing a synthetic fiber treating agent comprises the following steps, in percentage by mass:

[0069] S1. Mix the formulated amounts of potassium monoethyl octylphosphonate and polyoxyethylene monooleate PEG400MO at 55° C. to form a pre-emulsified phase.

[0070] S2. Add the formulated amount of pentaerythritol tetraoleate and dilauryl thiodipropionate to the pre-emulsified phase, raise the temperature to 75° C., and stir until the phase becomes homogeneous.

[0071] S3. Slowly add the formulated amount of deionized water to the homogeneous phase, and emulsify the phase in a high-speed homogenizer at a controlled emulsification rate of 6500 rpm. After emulsification, cool the phase to below 40° C. and discharge the phase to obtain a synthetic fiber treating agent.

[0072] Comparative Example 3

[0073] A synthetic fiber treating agent comprises the following raw materials in percentage by mass: 8% of octadecyldimethylhydroxyethylammonium chloride, 20% of pentaerythritol fatty acid ester, 12% of polyoxyethylene monooleate PEG400MO, 0.3% of dilauryl thiodipropionate, and 59.7% of deionized water.

[0074] A method for preparing a synthetic fiber treating agent comprises the following steps, in percentage by mass:

[0075] S1. Mix the formulated amounts of octadecyldimethylhydroxyethylammonium chloride and polyoxyethylene monooleate PEG400MO at 55° C. to form a pre-emulsified phase.

[0076] S2. Add the formulated amount of pentaerythritol tetraoleate and dilauryl thiodipropionate to the pre-emulsified phase, raise the temperature to 75° C., and stir until the phase becomes homogeneous.

[0077] S3. Slowly add the formulated amount of deionized water to the homogeneous phase, and emulsify the phase in a high-speed homogenizer at a controlled emulsification rate of 6500 rpm. After emulsification, cool the phase to below 40° C. and discharge the phase to obtain a synthetic fiber treating agent.

[0078] Comparative Example 4

[0079] A synthetic fiber treating agent comprises the following raw materials in percentage by weight: 8% potassium monoethyl octylphosphonate, 5% octadecyltrimethylammonium chloride, 20% pentaerythritol fatty acid ester, 12% polyoxyethylene monooleate PEG400MO, 0.3% dilauryl thiodipropionate, and 54.7% deionized water.

[0080] A method for preparing potassium monoethyl octylphosphonate is the same as that in Example 1.

[0081] A synthetic fiber treatment agent was prepared according to the preparation method in Example 1. In step S1, potassium monoethyl octylphosphonate, octadecyltrimethylammonium chloride, and polyoxyethylene monooleate PEG400MO were mixed at 55° C. to form a precipitate, which was then separated into layers.

[0082] Test Case

[0083] (1) Antistatic performance test

[0084] The electrostatic properties of polyester fabric were evaluated using a fabric induction electrostatic meter. The synthetic fiber treatment agents prepared in the above examples and comparative examples 1-3 were added to deionized water to prepare 100 mL of a 0.1 wt% solution. 45×45 mm polyester specimens were immersed in each of these solutions for 12 hours, dried at 40°C for 30 minutes, and then equilibrated in an environment of 20±2°C and 35±5% humidity for 12 hours. Before testing, the specimens were secured to the instrument's turntable, zeroed, and then the high-voltage electric field was activated. After the rotating specimens completed electrostatic induction, the steady-state electrostatic voltage and half-life values ​​were recorded. Each experiment was repeated three times and the average value was calculated. The test results are shown in Table 1.

[0085] Table 1: Antistatic test results of the treatment agents of Examples 1-4 and Comparative Examples 1-3

[0086] sample Electrostatic voltage (V) Static voltage half-life (s) Example 1 924.33 1.46 Example 2 1462.67 1.76 Example 3 1590.67 1.64 Example 4 1532.67 1.72 Comparative Example 1 4662.33 3.55 Comparative Example 2 1942.71 2.09 Comparative Example 3 2306.36 2.28

[0087] The results of electrostatic voltage and electrostatic voltage half-life can reflect the quality of the antistatic performance of the treatment agent. The lower the value, the stronger the antistatic performance of the treatment agent.

[0088] The formula of the treating agent prepared in Comparative Example 1 does not contain organic phosphonate and cationic surfactant. Compared with the fabric treated with the treating agent prepared in Comparative Example 1, the electrostatic voltage of the fabric treated with the treating agent prepared in Example 1 is reduced by 80%, and the electrostatic voltage half-life is reduced by 60%.

[0089] No cationic surfactant was added to the formula of the treating agent prepared in Comparative Example 2, and no organic phosphonate was added to the formula of the treating agent prepared in Comparative Example 3. Compared with the fabrics treated with the treating agents prepared in Comparative Examples 2 and 3, the fabrics treated with the treating agents prepared in Examples 1-4 of the present invention had lower electrostatic voltage and electrostatic voltage half-life, wherein the electrostatic voltage of the fabric was 924.33~1590.67V, and the electrostatic voltage half-life was 1.46~1.76s.

[0090] When the treating agent was prepared according to the formula in Comparative Example 4, precipitation and stratification occurred, and the antistatic effect was lost.

[0091] (2) Stability test

[0092] The synthetic fiber treatment agents prepared in Examples 1-4 and Comparative Examples 1-3 were placed in an oven at 48°C for 48 hours. The results were as follows: the treatment agents prepared in Examples 1-4 remained stable, while the treatment agents prepared in Comparative Examples 1-3 were unstable and easily precipitated and separated.

[0093] In summary, the present invention selects an organic phosphonate as an antistatic agent and octadecyldimethylhydroxyethylammonium chloride as a cationic surfactant, and compounding the two, and high-speed homogenization and emulsification are performed to obtain a synthetic fiber treating agent in the form of an emulsion. The treating agent has excellent antistatic properties and stability and can be applied to the high-speed spinning process of synthetic fibers such as polyester or nylon.

[0094] The above description is merely a preferred embodiment of the present invention, and the present invention is not limited to the above embodiment. It is understood that other improvements and variations directly derived or imagined by those skilled in the art without departing from the spirit and concept of the present invention should be considered to be included in the scope of protection of the present invention.

Claims

1. A synthetic fiber treating agent, characterized in that The raw materials include the following percentage by weight: 3-8% antistatic agent, 5-10% cationic surfactant, 15-25% high-temperature lubricating ester, 10-15% nonionic emulsifier, 0.1-0.5% antioxidant, and the balance is water; The antistatic agent includes an organic phosphonate.

2. The synthetic fiber treating agent according to claim 1, characterized in that The organic phosphonate is potassium octylphosphonate monoethyl ester, and the chemical structural formula of potassium octylphosphonate monoethyl ester is as follows:

3. The synthetic fiber treating agent according to claim 1, characterized in that The cationic surfactant is octadecyl dimethyl hydroxyethyl ammonium chloride.

4. The synthetic fiber treating agent according to claim 1, characterized in that The high-temperature lubricating ester is pentaerythritol fatty acid ester, and preferably, the high-temperature lubricating ester is pentaerythritol tetraoleate.

5. The synthetic fiber treating agent according to claim 1, characterized in that The nonionic emulsifier is polyoxyethylene monooleate.

6. The synthetic fiber treating agent according to claim 1, characterized in that The antioxidant is dilauryl thiodipropionate.

7. A method for preparing the synthetic fiber treating agent according to any one of claims 1 to 6, characterized in that: The process comprises the following steps, in percentage by mass: S1, mixing the antistatic agent, the cationic surfactant, and the nonionic emulsifier at temperature T1 to form a pre-emulsified phase; S2, adding the high-temperature lubricating ester and the antioxidant to the pre-emulsified phase, heating to temperature T2, and stirring until a homogeneous phase is obtained; S3. Add water to the homogeneous phase, perform high-speed homogenization and emulsification, and then cool to temperature T3 to obtain a synthetic fiber treating agent.

8. The preparation method according to claim 7, characterized in that In step S1, the temperature T1 is 50-60°C, and the mixing time is 20-40 minutes; In step S2, the temperature T2 is 70-80°C.

9. The preparation method according to claim 7, characterized in that In step S3, the temperature T3 is not higher than 40°C; And / or, the high-speed homogenization emulsification rate is 5000-8000 rpm, and the time is 15-25 min.

10. Use of the synthetic fiber treating agent according to any one of claims 1 to 6, and / or the synthetic fiber treating agent prepared by the preparation method according to any one of claims 7 to 9, in a synthetic fiber high-speed spinning process.

Images