CN111996611A - Antistatic agent and preparation method thereof - Google Patents
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- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/198—Graphene oxide
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
- D01F1/103—Agents inhibiting growth of microorganisms
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
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- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/224—Esters of carboxylic acids; Esters of carbonic acid
- D06M13/2243—Mono-, di-, or triglycerides
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
- D06M13/46—Compounds containing quaternary nitrogen atoms
- D06M13/463—Compounds containing quaternary nitrogen atoms derived from monoamines
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/32—Polyesters
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Abstract
The invention discloses an antistatic agent and a preparation method thereof. The preparation method of the antistatic agent comprises the following steps: (1) modifying graphene oxide: dispersing 2-5g of graphene oxide in 0.5-1.2L of water, and performing ultrasonic dispersion for 1-3h to obtain graphene oxide hydrosol; adding 0.3-1g of modifier into the graphene oxide hydrosol, and stirring for 10-40 min; filtering, washing with water, and vacuum drying at 20-70 deg.C for 5-12h to obtain modified graphene oxide; (2) chemical reduction: dissolving 2-5g of reducing agent in 0.5-1.2L of water, adding 1-2g of the modified graphene oxide, and stirring in a water bath at 70-110 ℃ for 1-3 h; filtering, washing with water, and vacuum drying at 40-80 deg.C for 8-15 hr. According to the invention, the modified graphene oxide composite material is used as an antistatic agent, so that the antistatic performance is improved, and the antibacterial effect is improved; and the cationic quaternary ammonium salt modifier is added, so that the antibacterial performance of the antibacterial agent is further improved.
Description
Technical Field
The invention relates to an antistatic agent and a preparation method thereof.
Background
The textile material is an electrical insulator material, particularly synthetic fibers such as terylene, acrylic fibers, polyvinyl chloride fibers and the like, and has poor moisture absorption performance and high specific resistance. Thus, during the textile processing, the intimate contact and friction between fibers or fibers and the machine parts, as well as the mutual contact and friction of the processed textiles, can cause the transfer of electrical charge and the generation of static electricity.
The presence of static electricity, on the one hand, affects the quality of the product and the wearability of the fabric, and on the other hand, discharges to produce sparks, causing fire and serious consequences. The use of antistatic fabrics is particularly important in special environments and workplaces, such as the electronic industry, the medical and health industry, and flammable and explosive places such as gas stations and mines. At present, adding a surfactant to the surface of a formed fiber to obtain an antistatic fabric is the most conventional and simplest method, but the antistatic effect gradually decreases as the number of washing times increases. Therefore, the development of the antistatic fabric with strong and durable antistatic performance has profound significance.
Disclosure of Invention
The antistatic agent is added into the high polymer in a molten state, and then the high polymer is spun into fibers, so that the antistatic fabric obtained by processing generally has better antistatic durability. The carbon-based material has the advantages of small density, stable structure, low price and the like, and has the potential of being used as an antistatic agent. The surface of the graphene oxide material contains oxygen-containing functional groups such as hydroxyl, carboxyl and the like, so that the graphene oxide material has good modifiable performance, can be combined with various materials in a covalent or non-covalent manner, and can be further stripped by adding a modifying material; after the reduction treatment is carried out on the graphene oxide, the oxygen-containing functional group on the surface of the graphene oxide is reduced, and the original sp of the graphene material2The hybrid structure and the delocalized pi-bond structure formed by the carbon atoms of the hybrid structure are repaired, and the conductivity of the hybrid structure can be obviously improved. After the graphene oxide is reduced, the possibility of reoxidation still exists in the subsequent processing process, so that if an antioxidant mechanism can be simultaneously established in the graphene reduction and oxidation process, a new idea for preparing a durable antistatic performance material is possible.
Based on the research background and thought, the technical scheme adopted by the invention is as follows:
a method for preparing an antistatic agent, comprising the steps of:
(1) modifying graphene oxide: dispersing 2-5g of graphene oxide in 0.5-1.2L of water, and performing ultrasonic dispersion for 1-3h to obtain graphene oxide hydrosol; adding 0.3-1g of modifier into the graphene oxide hydrosol, and stirring for 10-40 min; filtering, washing with water, and vacuum drying at 20-70 deg.C for 5-12h to obtain modified graphene oxide;
(2) chemical reduction: dissolving 2-5g of reducing agent in 0.5-1.2L of water, adding 1-2g of the modified graphene oxide, and stirring in a water bath at 70-110 ℃ for 1-3 h; filtering, washing with water, and vacuum drying at 40-80 deg.C for 8-15 hr.
The modifier is one or two of glyceryl monostearate and octadecyl dimethyl benzyl ammonium chloride.
Preferably, the modifier is glyceryl monostearate and octadecyl dimethyl benzyl ammonium chloride in a weight ratio of (1-3): (1-3) mixing.
The reducing agent is any one of tea polyphenol, vitamin C, sodium citrate and sodium borohydride.
An antistatic agent prepared by any one of the above methods.
The invention has the beneficial effects that:
(1) the novel antistatic agent is prepared by adopting a method of modifying graphene oxide and combining chemical reduction. On one hand, the selected modifier has an antistatic property, and the addition of the modifier can effectively increase the sheet peeling degree of the graphene oxide and can also increase the compatibility of the antistatic agent and a fiber matrix; on the other hand, after the modified graphene oxide is chemically reduced, the oxygen-containing functional groups on the surface of the modified graphene oxide are reduced, and sp of the graphene material is reduced2The hybrid structure and the delocalized pi bond formed by the carbon atoms of the hybrid structure are repaired, and the conductivity is improved; in addition, sodium citrate is used as a reducing agent, so that oxygen-containing functional groups can be reduced, and the sodium citrate can be combined with a selected cationic modifier through electrostatic action to protect reduced graphene oxide and prevent the reduced graphene oxide from being oxidized again in subsequent processing steps;
(2) according to the invention, the modified graphene oxide composite material is used as the antistatic agent, so that the antistatic performance of the fabric is improved, and meanwhile, the antibacterial effect of the fabric is improved; and by adding the cationic quaternary ammonium salt modifier, the antibacterial performance of the fabric is further improved.
Detailed Description
The graphene oxide has the purity of 99.0 wt%, the single-layer rate of 99.0% and the transverse dimension of 0.5-10 μm, and is purchased from Shanghai carbon source Hui Gu New Material science and technology company Limited.
Sodium citrate, CAS No.: 68-04-2, available from Standard science and technology, Inc. of Tianjin.
Tea polyphenols, purchased from Shanghai koji chemical Co., Ltd.
Octadecyl dimethyl benzyl ammonium chloride, CAS number: 122-19-0, available from Shanghai Xuejie chemical Co., Ltd.
Glyceryl monostearate, CAS number 123-94-4, available from Bailingwei technologies, Inc., Beijing.
An HH model digital display constant temperature water bath kettle, which is purchased from Youzhou national instruments manufacturing Co.
The YK300ST ultrasonic cleaning machine is purchased from Shanghai Yingke automatic cleaning equipment Co.
Model DZF-6020 vacuum drying oven, available from Shanghai Kol instruments, Inc.
Model CR22GII high speed centrifuge available from Hitachi, Japan.
CM type high speed mixer available from Shanghai Kenck mechanical Equipment, Inc.
Model KTE-36 twin screw granulator, available from Nanjing Kerke.
The ZY type melt spinning machine is available from Sichuan research science and technology Co.
Model LD128 sectional warper, purchased from longde machinofacture, sunward, japan.
An IR-408 type loom available from Qingdao-Liu eight machines, Inc.
Example 1
A method for preparing an antistatic agent, comprising the steps of:
dispersing 2g of graphene oxide in 1L of deionized water, and performing ultrasonic dispersion for 1h under the conditions that the ultrasonic frequency is 40kHz and the power is 450W to obtain graphene oxide hydrosol; adding 0.5g of modifier into the graphene oxide hydrosol, and stirring for 20 min; and after filtering and washing, carrying out vacuum drying for 10 hours at 50 ℃ to obtain the modified graphene oxide.
The modifier is octadecyl dimethyl benzyl ammonium chloride.
Example 2
Essentially the same as example 1, with the only difference that:
the modifier is glyceryl monostearate.
Example 3
Essentially the same as example 1, with the only difference that:
the modifier is formed by mixing glyceryl monostearate and octadecyl dimethyl benzyl ammonium chloride according to the weight ratio of 1: 1.
Example 4
A method for preparing an antistatic agent, comprising the steps of:
(1) dispersing 2g of graphene oxide in 1L of deionized water, and performing ultrasonic dispersion for 1h under the conditions that the ultrasonic frequency is 40kHz and the power is 450W to obtain graphene oxide hydrosol; adding 0.5g of modifier into the graphene oxide hydrosol, and stirring for 20 min; filtering, washing with water, and vacuum-drying at 50 ℃ for 10h to obtain modified graphene oxide;
(2) dissolving 3g of reducing agent in 1L of deionized water, adding 2g of modified graphene oxide, and stirring in a water bath at 90 ℃ for 2 hours; after filtration and water washing, vacuum drying is carried out for 12h at 65 ℃.
The modifier is octadecyl dimethyl benzyl ammonium chloride.
The reducing agent is sodium citrate.
Example 5
Essentially the same as example 4, with the only difference that:
the modifier is glyceryl monostearate.
Example 6
Essentially the same as example 4, with the only difference that:
the modifier is formed by mixing glyceryl monostearate and octadecyl dimethyl benzyl ammonium chloride according to the weight ratio of 1: 1.
Example 7
Essentially the same as example 4, with the only difference that:
the reducing agent is tea polyphenol.
Comparative example 1
An antistatic agent adopts graphene oxide.
Comparative example 2
A method for preparing an antistatic agent, comprising the steps of:
dissolving 3g of reducing agent in 1L of deionized water, adding 2g of graphene oxide, and stirring in a water bath at 90 ℃ for 2 hours; after filtration and water washing, vacuum drying is carried out for 12h at 65 ℃.
The reducing agent is sodium citrate.
Comparative example 3
A method for preparing an antistatic agent, comprising the steps of:
(1) dissolving 3g of reducing agent in 1L of deionized water, adding 2g of graphene oxide, and stirring in a water bath at 90 ℃ for 2 hours; filtering, washing with water, and vacuum-drying at 65 ℃ for 12h to obtain reduced graphene oxide;
(2) dispersing the reduced graphene oxide in 1L of deionized water, and performing ultrasonic-assisted dispersion for 1h under the conditions that the ultrasonic frequency is 40kHz and the power is 450W to obtain reduced graphene oxide hydrosol; adding 0.5g of modifier into the reduced graphene oxide hydrosol, and stirring for 20 min; after filtration and washing with water, the mixture was dried under vacuum at 50 ℃ for 10 hours.
The modifier is octadecyl dimethyl benzyl ammonium chloride.
The reducing agent is sodium citrate.
Test example 1: antistatic Property test of antistatic agent
And 6.1 and 6.2 in the former reference standard GB/T16801 and 2013 fabric conditioner antistatic performance determination.
Preparation of test pieces
Test piece washing treatment
The polyester fabric used for the test was cut to remove a 10 cm-wide fabric edge, and a 500mm × 500mm test fabric piece was cut.
Dissolving soap flakes with deionized water to prepare a soap solution with the concentration of 1g/L in terms of dry sodium soap, and the temperature is 40 ℃.
2L of a soap solution at 40 ℃ was added to the rinser, 20 pieces of 500mm by 500mm test cloth were put in, and the rinse was performed for 15min with a lid. The rotation washing mode is clockwise 5 circles, anticlockwise 5 circles, rotation for 3min, stop for 2min, rotation rate is kept at 20r/min, and the above steps are repeated. And (5) discarding the wastewater after the time is up, and quickly rotating to dewater for 30S.
Adding 2L of 40 ℃ deionized water into the rinser, stirring and rinsing for 3min, rotating for 5 circles clockwise and 5 circles anticlockwise, discarding the wastewater after the time is up, and quickly rotating for dewatering for 30S. Rinse 3 times as such.
Drying of test pieces
The washed shackles are clamped by plastic shackles, the two corner hangers are clamped by plastic clips, and the shackles are dried for 3 hours at room temperature. Air drying, taking down, placing on filter paper, covering with filter paper, placing into enamel plate, drying in oven at 45 deg.C for 4 hr, taking out, placing in hygrostat, and storing for use.
Test pieces were treated with conditioner test solutions
Weighing the antistatic agent into 1000mL beakers, adding deionized water to prepare 850mL of solution with the antistatic agent sample concentration of 30.0g/L, and respectively placing the solution in 4 400mL beakers, wherein 200mL of sample solution is used for parallel test in each beaker.
For each sample, 4 test pieces of 500 mm. times.500 mm were taken, and each piece was immersed in 4 200mL of the sample solution at room temperature for 10min and turned over with a glass rod from time to time. Taking out the soaked test piece, clamping two corners by a plastic clamp, hanging and drying for 3h, and then putting into a 45 ℃ oven for drying for 4 h.
And (4) carrying out an antistatic performance test on the dried test piece.
And (3) measuring the charge surface density according to the national standard GB/T12703.2-2009 part 2 of textile static testing method: charge areal density.
Table 1: antistatic performance meter of antistatic agent
| Areal density of charge (uc/m)2) | |
| Antistatic agent prepared in example 1 | 4.71 |
| Antistatic agent prepared in example 2 | 4.75 |
| Antistatic agent prepared in example 3 | 3.94 |
| Antistatic agent prepared in example 4 | 1.71 |
| Antistatic agent prepared in example 5 | 2.28 |
| Antistatic agent prepared in example 6 | 1.24 |
| Antistatic agent prepared in example 7 | 2.03 |
| Antistatic agent prepared in comparative example 1 | 6.04 |
| Antistatic agent prepared in comparative example 2 | 4.95 |
| Antistatic agent prepared in comparative example 3 | 3.58 |
Comparing examples 1 to 3 with comparative example 1, it can be seen that the antistatic performance of the fabric with the modified graphene oxide as the antistatic agent is significantly improved compared with that of the graphene oxide. The reason may be that the surface of graphene oxide contains a large number of functional groups, such as carboxyl, hydroxyl, epoxy, etc., which gives it good modifiability; the selected modifier has antistatic performance, and can generate non-covalent action with graphene oxide to promote the exfoliation of the graphene oxide and increase the compatibility of the antistatic agent and a fiber matrix.
Comparing examples 4-6 with examples 1-3, it can be seen that the antistatic performance of the fabric is obviously improved after the modified graphene oxide is subjected to reduction treatment, and the reason should be that: a large number of oxygen-containing functional groups exist on the surface of the modified graphene oxide, and the original sp of the graphene is reduced2The delocalized pi bond formed by hybridized carbon atoms is recovered, which is beneficial to the improvement of electron transmission and electric conductivity.
Comparing example 4 with comparative example 3, it can be seen that when graphene oxide is reduced first and then modified, the antistatic performance of the fabric is not as good as that of the fabric modified first and then reduced, which may be due to the fact that the surface of graphene oxide contains a large amount of oxygen-containing functional groups, such a structure is easier to combine with a modifier, and the synergistic effect is more obvious.
Firstly, octadecyl dimethyl benzyl ammonium chloride is adopted to modify graphene oxide, and then sodium citrate is adopted to reduce the graphene oxide, so that the antistatic fabric obtained has better antistatic durability, and the reason may be that: when sodium citrate is selected as a reducing agent and octadecyl dimethyl benzyl ammonium chloride is selected as a modifying agent, after the oxygen-containing functional groups on the surface of the graphene oxide are reduced by the sodium citrate, the residual sodium citrate can be combined with cationic octadecyl dimethyl benzyl ammonium chloride due to the action of electrostatic force, and further, the phenomenon that the reduced graphene oxide is re-oxidized in the subsequent processing steps is avoided. The glyceryl monostearate belongs to a nonionic modifier, and does not generate electrostatic interaction with sodium citrate; and when the tea polyphenol is used as a reducing agent, the tea polyphenol is difficult to generate electrostatic interaction with cationic octadecyl dimethyl benzyl ammonium chloride.
And (4) carrying out antibacterial performance test on the dried test piece.
And (3) carrying out an antibacterial performance test according to the national standard GB/T20944.3-2008, and testing strains: escherichia coli (ATCC 25922).
Table 2: bactericidal rate test results table
| Escherichia coli% | |
| Example 1 | 94.0 |
| Example 2 | 78.5 |
| Example 6 | 94.9 |
| Comparative example 1 | 74.2 |
| Comparative example 4 | 43.7 |
According to the table 2, the addition of the graphene and the cationic quaternary ammonium salt has a positive effect on the improvement of the antibacterial performance of the fabric. The reason why the graphene material has antibacterial performance may be that: the graphene can generate strong dispersion interaction with phospholipid molecules on bacterial cell membranes, so that the phospholipid molecules on the cell membranes can be directly extracted in a large scale to kill bacteria; the sterilization mechanism of the cationic quaternary ammonium salt is as follows: the positive ions can adsorb negatively charged bacteria through electrostatic force, hydrogen bond force, hydrophobic interaction with protein molecules and the like, and gather on cell walls to generate a chamber barrier effect, so that the bacteria are inhibited in growth and die.
The foregoing detailed description of the preferred embodiments of the invention has been presented. It should be understood that numerous modifications and variations could be devised by those skilled in the art in light of the present teachings without departing from the inventive concepts. Therefore, the technical solutions available to those skilled in the art through logic analysis, reasoning and limited experiments based on the prior art according to the concept of the present invention should be within the scope of protection defined by the claims.
Claims (4)
1. A preparation method of an antistatic agent is characterized by comprising the following steps: the method comprises the following steps:
(1) modifying graphene oxide: dispersing 2-5g of graphene oxide in 0.5-1.2L of water, and performing ultrasonic dispersion for 1-3h to obtain graphene oxide hydrosol; adding 0.3-1g of modifier into the graphene oxide hydrosol, and stirring for 10-40 min; filtering, washing with water, and vacuum drying at 20-70 deg.C for 5-12h to obtain modified graphene oxide;
(2) chemical reduction: dissolving 2-5g of reducing agent in 0.5-1.2L of water, adding 1-2g of the modified graphene oxide, and stirring in a water bath at 70-110 ℃ for 1-3 h; filtering, washing with water, and vacuum drying at 40-80 deg.C for 8-15 hr.
2. The process for the preparation of antistatic agents according to claim 1, characterized in that: the modifier is one or two of glyceryl monostearate and octadecyl dimethyl benzyl ammonium chloride.
3. The process for the preparation of antistatic agents according to claim 1, characterized in that: the reducing agent is any one of tea polyphenol, vitamin C, sodium citrate and sodium borohydride.
4. An antistatic agent, characterized in that it is prepared by the process of any one of claims 1 to 3.
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| CN111485312A (en) * | 2020-04-28 | 2020-08-04 | 安徽宏祥丝绸织造有限公司 | Preparation method of anti-static silk fabric |
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