A method for treating polyester filter material to make it waterproof and oil-repellent and the filter material prepared

Abstract

The present invention provides a method for treating polyester filter material to make it water-resistant and oil-repellent and the filter material prepared. The treatment method comprises the steps of fully oscillating and padding the polyester fabric with a functional finishing agent; specifically, the functional finishing agent is obtained by grafting a fluorine-containing compound after forming a block polymer with phenyl acrylate and epoxy olefin; by structurally designing the functional finishing agent, the finished polyester filter cloth not only has excellent water-resistant and oil-repellent effects, but also maintains the flexibility of the original fabric, can be firmly fixed on the fabric surface, has strong water-washing resistance, and is suitable for more usage scenarios.

Description

Technical Field

[0001] The invention relates to the field of textile chemistry, and in particular to a method for treating a polyester filter material to make it waterproof and oil-repellent, and the prepared filter material. Background Art

[0002] Fabric finishing agents are chemical additives used to improve fabric properties. They are widely used in textile finishing processes to give fabrics special functional properties, such as waterproof, oil-proof, antifouling, antistatic and antibacterial. Among them, water-repellent and oil-repellent finishing agents are an important category, which aims to change the wetting properties of the fabric surface to make it hydrophobic and oil-repellent. This type of finishing agent is usually based on a chemical system of silicone, fluoride or polymer emulsion, and is combined with the fiber by coating or impregnation to form a hydrophobic and oil-repellent protective film. Silicone finishing agents are widely used for their excellent softness and breathability, while fluorinated finishing agents occupy the high-end market with their excellent hydrophobic and oil-repellent capabilities. However, with the increasingly stringent environmental regulations, the application of traditional fluorinated finishing agents has been restricted, prompting researchers to develop new environmentally friendly finishing agents and promote the green development of water-repellent and oil-repellent technology.

[0003] Although the technology of waterproof and oil-repellent filter cloth has developed rapidly, there are still some problems in practical application. First, the use of traditional fluorine-containing finishing agents may bring environmental and health risks. Perfluorinated compounds are persistent and bioaccumulative, and their decomposition products may pose a threat to the ecological environment and human health. Secondly, the durability of waterproof and oil-repellent filter cloth has also attracted much attention. After long-term use or repeated washing, the surface coating may fall off or fail, resulting in a significant decrease in function. In addition, the air permeability or flexibility of some high-performance filter cloths may be affected by the surface coating and cannot meet the comfort requirements of certain application scenarios. Future research directions should focus on developing environmentally friendly finishing agents, improving the durability of materials, and optimizing the balance between usage experience and protective performance, so as to provide technical support for the sustainable development of waterproof and oil-repellent filter cloth.

[0004] In summary, the market still lacks an environmentally friendly waterproof and oil-repellent filter material that can take into account both usage experience and protection. Summary of the invention

[0005] Purpose of the invention: The purpose of the present invention is to provide an environmentally friendly waterproof and oil-repellent filter material that can take into account both usage experience and protectiveness, has a soft feel and lasting waterproof and oil-repellent performance, and reduces threats to the ecological environment and human health; accordingly, a preparation method of the waterproof and oil-repellent filter material is provided.

[0006] The technical solution of the present invention:

[0007] In a first aspect, the present invention provides a method for treating polyester filter material to be waterproof and oil-repellent, comprising the steps of fully oscillating and padding the polyester fabric using a functional finishing agent;

[0008] The functional finishing agent is obtained by forming a block polymer with phenyl acrylate and epoxy olefin, and grafting a fluorine-containing compound; the fluorine-containing compound is selected from one or more combinations of 5,5-bis(trifluoromethyl)-6,6,7,7,8,8,8-heptafluorooctane-1-ol (CAS: 1980040-36-5) and 2,2,3,4,4,6,6,6-octafluoro-3,5,5-tri(trifluoromethyl)hexan-1-ol (CAS: 232267-34-4).

[0009] In some embodiments, the phenyl-containing acrylate is selected from one or more combinations of phenyl methacrylate, 2,3,5,6-tetrafluorophenyl methacrylate, and pentafluorophenyl methacrylate.

[0010] In some embodiments, the method for preparing the epoxy-containing olefin comprises the following steps:

[0011] The compound represented by Formula 1 is dissolved in a solvent, ethylene glycol and p-toluenesulfonic acid are added, and the reaction is carried out at 40-50° C. After the reaction is completed, the intermediate is separated by distillation; KH560 and the intermediate are added to the solvent, triethylamine is added, the temperature is increased and stirred under an inert gas for reaction, and after the reaction is completed, an HCl aqueous solution is used for hydrolysis, and after the hydrolysis is completed, the product is separated and purified by recrystallization, and the product is washed and dried to obtain an epoxy-containing olefin;

[0012] Formula 1.

[0013] In some embodiments, the molar ratio of KH560 to the compound of Formula 1 is 1:1-1.5, the reaction temperature of the heating and stirring reaction is 60-80° C., and the reaction time is 4-6 hours.

[0014] In some embodiments, the method for preparing the functional finishing agent comprises the following steps:

[0015] S1: adding phenyl acrylate, initiator and solvent into a reactor, introducing inert gas under stirring, heating and keeping the temperature to react, and obtaining a polymer;

[0016] S2: adding the polymer prepared in S1 to a reactor, and then adding epoxy-containing olefin, initiator and solvent, introducing inert gas and heating to react, and after the reaction, precipitating the obtained product with n-hexane and drying to obtain a functional finishing agent precursor;

[0017] S3: After mixing the functional finishing agent precursor, the fluorine-containing compound and the solvent, a catalyst is added, and the mixture is reacted under heating conditions for 6 to 12 hours to obtain the functional finishing agent.

[0018] In some embodiments, the initiator and solvent in S1 are not particularly limited. For example, the initiator can be selected from one or more combinations of free radical initiators such as benzoyl peroxide (BPO) and azobisisobutyronitrile (AIBN); the solvent can be selected from one or more combinations of toluene, ethyl acetate or DMF, etc., to facilitate control of reaction viscosity and heat dissipation.

[0019] In some embodiments, the added mass of the initiator in S1 is 0.5% to 2% of the added mass of the phenyl-containing acrylate.

[0020] In some embodiments, the mass ratio of the phenyl-containing acrylate to the epoxy-containing olefin is 5 to 3:1; preferably, the mass ratio of the phenyl-containing acrylate to the epoxy-containing olefin is 4:1. The amount of phenyl-containing acrylate and epoxy-containing olefin added affects the block structure of the synthetic polymer and has a great influence on the performance of the functional finishing agent.

[0021] In some embodiments, the temperature increase in steps S1 and S2 is to increase the temperature to 60-80° C., and the reaction time is 2-6 hours.

[0022] In some embodiments, the added mass ratio of the functional finishing agent precursor to the fluorine-containing compound is 2 to 3.5:1.

[0023] In some embodiments, the reaction temperature in step S3 is 60-80° C., and the reaction time is 4-6 hours.

[0024] In some embodiments, the step of using a functional finishing agent to fully oscillate and pad the polyester fabric specifically includes the following contents:

[0025] The functional finishing agent is diluted with isopropyl alcohol to obtain a finishing solution; the fabric is dipped into the finishing solution, and then pre-baked and baked in sequence to achieve a waterproof and oil-repellent treatment of the fabric.

[0026] In some embodiments, the mass content of the finishing agent in the finishing liquid is 20% to 70%.

[0027] In a second aspect, the present invention further provides a filter material obtained by the above-mentioned water-repellent and oil-repellent step.

[0028] Compared with the prior art, the present invention has the following beneficial effects:

[0029] 1. Through the structural design of the functional finishing agent, the finished polyester filter cloth not only has excellent water-repellent and oil-repellent effects, but also maintains the flexibility of the original fabric, is easy to degrade, reduces biological hazards, and is suitable for more usage scenarios.

[0030] 2. The structure of the epoxy-olefin-containing polymer monomer of the functional finishing agent is designed to have a long chain containing silicon-oxygen bonds, which can be firmly fixed on the surface of the fabric and have strong water-washing resistance; and fluorine-containing compounds are grafted onto the epoxy-olefin to regulate the fluorine chain segments to preferentially arrange the outermost layer, promote the accumulation of fluorine elements on the surface, and make the finishing agent have higher water and oil repellency.

[0031] 3. By regulating the content of the polymerized monomers of the functional finishing agent - phenyl acrylate and epoxy olefin, and forming a block structure, the shielding effect of the F atom is adjusted to make the overall surface tension extremely low, while improving the softness of the fabric. DETAILED DESCRIPTION

[0032] The technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all of the embodiments. Based on the embodiments in the present invention, all other embodiments obtained by ordinary technicians in the field without creative work are within the scope of protection of the present invention. Other raw materials and equipment of the present invention are all commonly available on the market, well known to those skilled in the art, and will not be described in detail.

[0033] Preparation of epoxy-containing olefins

[0034] 1 mol of the compound represented by formula 1 was dissolved in 20 mL of toluene, 1.2 mol of ethylene glycol and 0.05 mol of p-toluenesulfonic acid were added, and the mixture was stirred at 40°C for 2 h. After the reaction was completed, the intermediate was separated by distillation. 1 mol of KH560 and 1.2 mol of the intermediate were added to 50 mL of toluene, 0.05 mol of triethylamine was added, the mixture was heated to 70°C under a nitrogen atmosphere and stirred for 6 h. After the reaction was completed, the mixture was hydrolyzed with 50 mL of 1% HCl aqueous solution. After the hydrolysis was completed, the product was separated and purified by recrystallization, and the product was washed and dried to obtain an epoxy-containing olefin.

[0035] The synthesized epoxy-containing olefin powder was analyzed by infrared spectrum using Fourier transform infrared spectrometer and potassium bromide tablet. The infrared spectrum of the reaction product shows that:

[0036] At 915 cm -1 There is symmetrical stretching vibration of epoxy group at 1600 cm -1 There is a C=C stretching vibration peak at 3350cm -1 There is an OH stretching vibration peak at 1100 cm -1 There is COC stretching vibration, indicating that the hydroxyl and epoxy groups have successfully undergone ring-opening reaction; 3400cm -1 The presence of characteristic peaks of Si-OH indicates that the above steps have successfully prepared modified epoxy-containing olefins.

[0037] Example 1

[0038] S1: 30 g of phenyl methacrylate, 0.15 g of azobisisobutyronitrile and 50 mL of toluene were added to a reactor, nitrogen was introduced under stirring, the temperature was raised to 60° C. and the temperature was kept for 4 h to obtain a polymer;

[0039] S2: Add the polymer prepared in S1 and 10 g of epoxy-containing olefin (prepared as described above), 0.2 g of azobisisobutyronitrile and 100 mL of toluene into the reactor, introduce nitrogen and heat to 60° C. to react for 6 h. After the reaction, precipitate the obtained product with n-hexane and dry it to obtain a functional finishing agent precursor;

[0040] S3: After mixing 40 g of the prepared functional finishing agent precursor, 20 g of 5,5-bis(trifluoromethyl)-6,6,7,7,8,8,8-heptafluorooctane-1-ol and 150 mL of toluene, 0.3 g of triethylamine was added, and the mixture was reacted under heating conditions for 6 h. After the reaction was completed, functional finishing agent 1 was obtained by precipitation and drying.

[0041] Example 2

[0042] The method is basically the same as Example 1, except that the phenyl-containing acrylate used in step S1 is 2,3,5,6-tetrafluorophenyl methacrylate, and a functional finishing agent 2 is prepared.

[0043] Example 3

[0044] The method is basically the same as Example 1, except that the fluorine-containing compound used in step S3 is 2,2,3,4,4,6,6,6-octafluoro-3,5,5-tri(trifluoromethyl)hexan-1-ol, and a functional finishing agent 3 is prepared.

[0045] Example 4

[0046] The process is basically the same as Example 1, except that the amount of epoxy-containing olefin used in step S2 is 7.5 g, and a functional finishing agent 4 is prepared.

[0047] Example 5

[0048] Basically the same as Example 1, except that the amount of epoxy-containing olefin used in step S2 is 6 g, and a functional finishing agent 5 is prepared.

[0049] Comparative Example 1

[0050] 30 g of pentafluorophenyl methacrylate, 0.15 g of azobisisobutyronitrile and 50 mL of toluene were added into a reactor, nitrogen was introduced under stirring, the temperature was raised to 60° C. and the reaction was maintained at this temperature for 4 h to obtain finishing agent 6.

[0051] Comparative Example 2

[0052] S1: 30 g of pentafluorophenyl methacrylate, 0.15 g of azobisisobutyronitrile and 50 mL of toluene were added into a reactor, nitrogen was introduced under stirring, the temperature was raised to 60° C. and the temperature was kept for 4 h to obtain a polymer;

[0053] S2: Add the polymer prepared in S1 and 10 g of epoxy-containing olefin (prepared as described above), 0.2 g of azobisisobutyronitrile and 100 mL of toluene into the reactor, introduce nitrogen and heat to 60°C to react for 6 h. After the reaction, precipitate the product with n-hexane and dry it to obtain finishing agent 7.

[0054] Comparative Example 3

[0055] S1: 30 g of pentafluorophenyl methacrylate, 0.15 g of azobisisobutyronitrile and 50 mL of toluene were added into a reactor, nitrogen was introduced under stirring, the temperature was raised to 60° C. and the temperature was kept for 4 h to obtain a polymer;

[0056] S2: Add the polymer prepared in S1, 10 g of glycidyl methacrylate, 0.2 g of azobisisobutyronitrile and 100 mL of toluene into the reactor, introduce nitrogen, and heat to 60° C. to react for 6 h. After the reaction, precipitate the obtained product with n-hexane and dry it to obtain a finishing agent precursor;

[0057] S3: After mixing 40 g of the prepared functional finishing agent precursor, 20 g of 5,5-bis(trifluoromethyl)-6,6,7,7,8,8,8-heptafluorooctane-1-ol and 150 mL of toluene, 0.3 g of triethylamine was added, and the mixture was reacted under heating conditions for 6 h. After the reaction was completed, the finishing agent 8 was obtained by precipitation and drying.

[0058] Performance Tests of Experimental Examples and Comparative Examples

[0059] The above finishing agent was prepared into an isopropanol solution with a concentration of 30g / L, and the polyester fabric was immersed for 30min, and then subjected to two immersions and two rollings with a rolling rate of 80%, pre-baked at 80℃ for 3min, baked at 160℃ for 3min, washed with water, soaped, and washed with water to obtain the finished fabric, and the following tests were carried out. The performance evaluation method and test standards are as follows:

[0060] 1. Use DSA100 contact angle measuring device to measure the static contact angles (water contact angle and oil contact angle) of water and diiodomethane on the finished fabric respectively;

[0061] 2. 10 soft feel evaluators are required to give scores, and the evaluation level is divided into the following levels: 4-5 points for excellent overall feel, 2-3 points for average overall feel, and 0-1 points for poor overall feel. The softness evaluation result can be given by the score. The higher the comprehensive average score, the better the softness effect of the towel after the sample is washed;

[0062] 3. Referring to AATCC 135-2015 "Dimensional Stability of Fabrics after Home Laundering", wash the fabric in Test 1 20 times, dry the washed fabric and measure the water contact angle again.

[0063] The test results are shown in the following table.

[0064] Table 1 Test results

[0065]

[0066] From the above tests, it can be seen that the present invention greatly improves the waterproof and oil-repellent effect of the obtained finishing agent by designing and modifying the structure of the functional finishing agent, adopting a block structure and grafting fluorine compounds and silicone, and can be firmly fixed on the surface of the fabric, has strong water washability, and improves the softness of the fabric.

[0067] It can be seen from the comparison of the examples and comparative examples in the table that using the epoxy-containing olefin provided by the present invention to replace glycidyl methacrylate can help regulate the arrangement of fluorine segments, promote the accumulation of fluorine elements on the surface, and thus improve the waterproof and oil-repellent effect of the fabric.

[0068] At the same time, it can be concluded from the comparison between the embodiments that when the added mass ratio of phenyl acrylate and epoxy olefin is 4:1, the balance between the fabric feel and waterproof performance can be effectively balanced, which can not only meet the high waterproof and oil-proof effect, but also have an excellent overall feel.

[0069] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention rather than to limit the protection scope of the present invention. Although the present invention has been described in detail with reference to the best embodiments, the present invention is not limited to the embodiments disclosed above, but should cover various modifications and equivalent combinations based on the essence of the present invention.

Claims

1. A method for treating polyester filter material to make it waterproof and oil-repellent, comprising the steps of using a functional finishing agent to fully vibrate and pad the polyester fabric; It is characterized in that The functional finishing agent is obtained by forming a block polymer with phenyl acrylate and epoxy olefin, and grafting a fluorine-containing compound; the fluorine-containing compound is selected from one or more combinations of 5,5-bis(trifluoromethyl)-6,6,7,7,8,8,8-heptafluorooctane-1-ol and 2,2,3,4,4,6,6,6-octafluoro-3,5,5-tri(trifluoromethyl)hexan-1-ol; The preparation method of the epoxy-containing olefin comprises the following steps: The compound represented by Formula 1 is dissolved in a solvent, ethylene glycol and p-toluenesulfonic acid are added, and the reaction is carried out at 40-50° C. After the reaction is completed, the intermediate is separated by distillation; KH560 and the intermediate are added to the solvent, triethylamine is added, the temperature is increased and stirred under an inert gas for reaction, and after the reaction is completed, an HCl aqueous solution is used for hydrolysis, and after the hydrolysis is completed, the product is separated and purified by recrystallization, and the product is washed and dried to obtain an epoxy-containing olefin; Formula 1.

2. The processing method according to claim 1, characterized in that: The phenyl-containing acrylate is selected from one or more combinations of phenyl methacrylate, 2,3,5,6-tetrafluorophenyl methacrylate, and pentafluorophenyl methacrylate.

3. The processing method according to claim 1, characterized in that: The preparation method of the functional finishing agent comprises the following steps: S1: adding phenyl acrylate, initiator and solvent into a reactor, introducing inert gas under stirring, heating and keeping the temperature to react, and obtaining a polymer; S2: adding the polymer prepared in S1 to a reactor, and then adding epoxy-containing olefin, initiator and solvent, introducing inert gas and heating to react, and after the reaction, precipitating the obtained product with n-hexane and drying to obtain a functional finishing agent precursor; S3: After mixing the functional finishing agent precursor, the fluorine-containing compound and the solvent, a catalyst is added, and the mixture is reacted under heating conditions for 6 to 12 hours to obtain the functional finishing agent.

4. The processing method according to claim 3, characterized in that: The added mass ratio of the phenyl-containing acrylate to the epoxy-containing olefin is 5 to 3:

1.

5. The processing method according to claim 3, characterized in that: The heating in steps S1 and S2 means heating to 60-80° C. and the reaction time is 2-6 hours.

6. The processing method according to claim 3, characterized in that: The added mass ratio of the functional finishing agent precursor to the fluorine-containing compound is 2 to 3.5:

1.

7. The processing method according to claim 1, characterized in that: The step of using a functional finishing agent to fully oscillate and pad the polyester fabric comprises the following contents: The functional finishing agent is diluted with isopropyl alcohol to obtain a finishing solution; the fabric is dipped into the finishing solution, and then pre-baked and baked in sequence to achieve a waterproof and oil-repellent treatment of the fabric.

8. The processing method according to claim 7, characterized in that: The mass content of the finishing agent in the finishing liquid is 20% to 70%.

9. A filter material, characterized in that: The polyester filter material is prepared by the waterproof and oil-repellent treatment method of any one of claims 1 to 8.

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