CN108867030B - Antistatic agent for cotton fabric - Google Patents

Antistatic agent for cotton fabric Download PDF

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CN108867030B
CN108867030B CN201810817253.6A CN201810817253A CN108867030B CN 108867030 B CN108867030 B CN 108867030B CN 201810817253 A CN201810817253 A CN 201810817253A CN 108867030 B CN108867030 B CN 108867030B
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graphene oxide
antistatic agent
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sodium azide
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CN108867030A (en
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黄勇
艾旭盛
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Shanghai Weidye Technology Co.,Ltd.
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Shanghai Yunji Chemical New Material Co ltd
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating 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
    • D06M11/73Treating 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
    • D06M11/74Treating 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
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating 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
    • D06M11/07Treating 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 halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
    • D06M11/11Treating 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 halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with halogen acids or salts thereof
    • D06M11/13Ammonium halides or halides of elements of Groups 1 or 11 of the Periodic Table
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating 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
    • D06M11/32Treating 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 oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36Treating 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 oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/44Oxides or hydroxides of elements of Groups 2 or 12 of the Periodic Table; Zincates; Cadmates
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02Natural fibres, other than mineral fibres
    • D06M2101/04Vegetal fibres
    • D06M2101/06Vegetal fibres cellulosic

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The invention discloses a preparation method of a cotton fabric antistatic agent, and belongs to the technical field of textile materials. Adding 5-10 parts of graphene oxide and 2-3 parts of sodium azide reagent into 10-20 parts of water, stirring for 0.5-1 h, filtering, washing and drying to obtain sodium azide modified graphene oxide; adding 5-10 parts of sodium azide modified graphene oxide and 5-10 parts of sodium periodate powder into 10-20 parts of water, stirring for 0.5-1 h, filtering, washing and drying to obtain modified graphene oxide; mixing 5-10 parts of modified graphene oxide, 5-10 parts of zinc oxide solution and 20-30 parts of water, adjusting the pH to 8.0 by using urea solution, and carrying out hydrothermal reaction for 1-2 hours to obtain a mixed solution; and adding 1-2 parts of dilute hydrochloric acid solution into the mixed solution, and stirring for 0.5-1 h to obtain the cotton fabric antistatic agent. The invention further improves the washing fastness and durability of the antistatic agent.

Description

Antistatic agent for cotton fabric
Technical Field
The invention discloses an antistatic agent for cotton fabrics, belonging to the technical field of textile materials.
Background
The fabric is easy to generate static electricity due to friction and induction in production, processing and use. The charge build-up phenomenon is more pronounced in synthetic fiber products where moisture regain is generally lower. The electrification phenomenon of the textile material in production can cause the phenomena of fiber winding or blockage of machine parts, semi-products or yarn hair and broken ends, unclear warp opening, uneven fabric folding and the like during weaving, and the smooth production is influenced; when the textile is used, the accumulation of electrostatic charges easily causes dust adhesion, and the clothing entangles limbs to generate the uncomfortable adhesion feeling; and can cause the pH value of blood to rise, the calcium content in the blood to decrease, the calcium content in urine to increase, the blood sugar to rise and the vitamin C to fall. The high static voltage may cause electric shock to a human body and cause damage to electronic components, even resulting in fire and explosion.
The antistatic agent is a general term for a substance used for suppressing the generation of static electricity on the surface of a material having excellent electrical insulating properties such as a synthetic resin or the like or for eliminating the accumulated static electricity. They play a role in the production, processing and use processes of synthetic fibers, and are particularly significant in preventing static electricity from generating and accumulating and overcoming the phenomenon that the fibers rub against each other to generate charges. The antistatic agent mainly refers to metal powder, inorganic substances such as carbon and the like, polysiloxane compounds, surfactants and the like. External antistatic agents are currently most used. It is used for surface spraying, dipping and coating in the production, processing and other processes of synthetic fiber. External antistatic agents are anionic, cationic, nonionic and amphoteric surfactants. The anionic antistatic agent has high heat stability, and is used mainly in the production and processing of synthetic fiber. It mainly comprises higher alcohol acid ester (salt), aliphatic sulfonate and higher acid phosphate. As the cation part of the counter ion, in addition to metal ions such as sodium and potassium, alkylol amine such as triethanolamine is used.
External antistatic agents are mostly surfactants, and they are poor in washing resistance and durability, and antistatic properties are substantially lost after processing.
Disclosure of Invention
The invention mainly solves the technical problems that: the invention aims to solve the problem that the washing fastness and durability of the conventional external antistatic agent cannot be further improved, and discloses a cotton fabric antistatic agent.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
(1) adding 1-2 parts of graphene oxide and 6-8 parts of sodium azide into 10-20 parts of water by mass, stirring for 0.5-1 h, filtering, washing and drying to obtain sodium azide modified graphene oxide;
(2) adding 5-10 parts of sodium azide modified graphene oxide and 5-10 parts of sodium periodate powder into 10-20 parts of water by mass, mixing and stirring for 0.5-1 h, filtering, washing and drying to obtain modified graphene oxide;
(3) mixing 5-10 parts of modified graphene oxide, 5-10 parts of zinc chloride solution and 20-30 parts of water according to mass fraction, adjusting the pH to 8.0 by using urea solution, and carrying out hydrothermal reaction for 1-2 hours to obtain a mixed solution;
(4) and mixing 1-2 parts of dilute hydrochloric acid solution and 5-10 parts of mixed solution by mass fraction, and stirring for 0.5-1 h to obtain the antistatic agent.
The sodium azide reagent in the step (1) is a dimethylformamide solution of sodium azide with the mass fraction of 40-41%.
And (3) the zinc oxide solution is a zinc chloride solution with the mass fraction of 20-30%.
And (3) the urea solution is 15-20% by mass.
The hydrothermal reaction in the step (3) is carried out for 1-2 h at the temperature of 140-180 ℃ and the pressure of 1.2-3.2 MPa.
And (4) the dilute hydrochloric acid solution in the step (4) is a dilute hydrochloric acid solution with the mass fraction of 5-10%.
The invention has the beneficial effects that:
(1) according to the invention, a sodium azide reagent is added into an antistatic agent, the sodium azide is a good nucleophilic reagent, and can carry out ring-opening addition and hydroxyl esterification on an epoxy group on added graphene oxide to carry out covalent bond connection on the graphene oxide, amino groups are generated after azide substitution, the amino groups are protonated under an acidic condition to have positive charges, and the same charges repel each other, so that the amino groups are favorably dispersed, meanwhile, cotton fabrics have negative charges, and the graphene oxide can be well attached to cotton fabrics due to the mutual attraction of the positive charges and the negative charges, so that the durability of the antistatic agent is enhanced;
(2) according to the invention, graphene oxide is added into the antistatic agent, the graphene oxide is stripped into single-layer or few-layer graphene through ultrasonic treatment, the graphene oxide is dispersed in the solution, zinc ions in the solution are adsorbed, and in the subsequent hydrothermal reaction process, the zinc ions are converted into nano zinc oxide and successfully embedded into a graphene oxide lamellar structure, so that the structure is stable and compact, the loss of the zinc oxide in the use process can be effectively avoided, and the antistatic effect of the product can be effectively maintained for a long time.
Detailed Description
Mixing and stirring 1-2 parts of graphene oxide, 6-8 parts of sodium azide reagent and 10-20 parts of water for 0.5-1 h, pouring the mixture into a No. 2 three-neck flask, carrying out ultrasonic dispersion for 45-60 min under the condition that the ultrasonic frequency is 45-60 kHz, moving the No. 2 flask into a digital display speed measurement constant-temperature magnetic stirrer, carrying out constant-temperature stirring reaction for 2-3 h under the conditions that the temperature is 65-75 ℃ and the rotating speed is 400-600 r/min, filtering to obtain a No. 2 filter cake, washing the obtained No. 2 filter cake with dimethylformamide for 3-5 times, and carrying out vacuum drying to obtain sodium azide modified graphene oxide; adding 5-10 parts of sodium azide modified graphene oxide and 5-10 parts of sodium periodate powder into 10-20 parts of water, mixing and stirring for 0.5-1 h, filtering, washing, and then drying in vacuum to obtain modified graphene oxide; mixing 5-10 parts of modified graphene oxide, 5-10 parts of zinc oxide solution and 20-30 parts of water, adjusting the pH to 8.0 by using urea solution, adding the mixed solution with the adjusted pH into a hydro-thermal synthesis reaction kettle, heating to 140-180 ℃, pressurizing to 1.2-3.2 MPa, and reacting for 1-2 hours to obtain a mixed solution; and adding 1-2 parts of dilute hydrochloric acid solution into the mixed solution, and stirring for 0.5-1 h to obtain the antistatic agent. The sodium azide reagent is 40-41% by mass. The zinc oxide solution is 20-30% by mass. The urea solution is 35-45% by mass. The dilute hydrochloric acid solution is 5-10% by mass.
Example 1
Mixing and stirring 1 part of graphene oxide, 6 parts of sodium azide reagent and 10 parts of water for 0.5h, pouring the mixture into a No. 2 three-neck flask, ultrasonically dispersing the mixture for 45min under the ultrasonic frequency of 45kHz, moving the No. 2 flask into a digital display speed measurement constant-temperature magnetic stirrer, stirring the mixture for reaction for 2h under the conditions of temperature of 65 ℃ and rotating speed of 400r/min at constant temperature, filtering to obtain a No. 2 filter cake, washing the obtained No. 2 filter cake with dimethylformamide for 3 times, and then drying the filter cake in vacuum to obtain sodium azide modified graphene oxide; adding 5 parts of sodium azide modified graphene oxide and 5 parts of sodium periodate powder into 10 parts of water, mixing and stirring for 0.5h, filtering, washing, and then drying in vacuum to obtain modified graphene oxide; mixing 5 parts of modified graphene oxide, 5 parts of zinc oxide solution and 20 parts of water, adjusting the pH to 8.0 by using urea solution, adding the mixed solution with the adjusted pH into a hydro-thermal synthesis reaction kettle, heating to 140 ℃, pressurizing to 1.2MPa, and reacting for 1 hour to obtain a mixed solution; and adding 1 part of dilute hydrochloric acid solution into the mixed solution, and stirring for 0.5h to obtain the antistatic agent. The sodium azide reagent is a sodium azide reagent with the mass fraction of 40%. The zinc oxide solution is 20% by mass. The urea solution is 35% by mass. The dilute hydrochloric acid solution is 5% in mass fraction.
Example 2
Mixing and stirring 1 part of graphene oxide, 6 parts of sodium azide reagent and 10 parts of water for 0.5h, pouring the mixture into a No. 2 three-neck flask, ultrasonically dispersing the mixture for 45min under the ultrasonic frequency of 45kHz, moving the No. 2 flask into a digital display speed measurement constant-temperature magnetic stirrer, stirring the mixture for reaction for 2h under the conditions of temperature of 65 ℃ and rotating speed of 400r/min at constant temperature, filtering to obtain a No. 2 filter cake, washing the obtained No. 2 filter cake with dimethylformamide for 3 times, and then drying the filter cake in vacuum to obtain sodium azide modified graphene oxide; adding 5 parts of sodium azide modified graphene oxide and 5 parts of sodium periodate powder into 10 parts of water, mixing and stirring for 0.5h, filtering, washing, and then drying in vacuum to obtain modified graphene oxide; mixing 5 parts of modified graphene oxide and 20 parts of water, adjusting the pH value to 8.0 by using a urea solution, adding the mixed solution with the adjusted pH value into a hydro-thermal synthesis reaction kettle, heating to 140 ℃, pressurizing to 1.2MPa, and reacting for 1 hour to obtain a mixed solution; and adding 1 part of dilute hydrochloric acid solution into the mixed solution, and stirring for 0.5h to obtain the antistatic agent. The sodium azide reagent is a sodium azide reagent with the mass fraction of 40%. The urea solution is 35% by mass. The dilute hydrochloric acid solution is 5% in mass fraction.
Example 3
Mixing and stirring 1 part of graphene oxide, 6 parts of sodium azide reagent and 10 parts of water for 0.5h, pouring the mixture into a No. 2 three-neck flask, ultrasonically dispersing the mixture for 45min under the ultrasonic frequency of 45kHz, moving the No. 2 flask into a digital display speed measurement constant-temperature magnetic stirrer, stirring the mixture for reaction for 2h under the conditions of temperature of 65 ℃ and rotating speed of 400r/min at constant temperature, filtering to obtain a No. 2 filter cake, washing the obtained No. 2 filter cake with dimethylformamide for 3 times, and then drying the filter cake in vacuum to obtain sodium azide modified graphene oxide; adding 5 parts of sodium azide modified graphene oxide and 5 parts of sodium periodate powder into 10 parts of water, mixing and stirring for 0.5h, filtering, washing, and then drying in vacuum to obtain modified graphene oxide; mixing 5 parts of modified graphene oxide, 5 parts of zinc oxide solution and 20 parts of water, adjusting the pH to 8.0 by using urea solution, adding the mixed solution with the adjusted pH into a hydro-thermal synthesis reaction kettle, heating to 140 ℃, pressurizing to 1.2MPa, and reacting for 1 hour to obtain the antistatic agent. The sodium azide reagent is a sodium azide reagent with the mass fraction of 40%. The zinc oxide solution is 20% by mass. The urea solution is 35% by mass.
Comparative example: antistatic agent produced by Dongguan company
The products obtained in examples 1 to 3 and comparative products were tested for their performance by the following specific test methods:
the specific detection results are shown in the following table 1:
table 1: antistatic agent performance test meter
Figure 306393DEST_PATH_IMAGE001
From the above table data, one can see: the antistatic agent prepared by the invention has better washing resistance and durability.

Claims (6)

1. A preparation method of a cotton fabric antistatic agent is characterized by comprising the following specific preparation steps:
(1) adding 1-2 parts by weight of graphene oxide and 6-8 parts by weight of sodium azide into 10-20 parts by weight of water, stirring for 0.5-1 h, filtering, washing and drying to obtain sodium azide modified graphene oxide;
(2) adding 5-10 parts by weight of sodium azide modified graphene oxide and 5-10 parts by weight of sodium periodate powder into 10-20 parts by weight of water, mixing and stirring for 0.5-1 h, filtering, washing and drying to obtain modified graphene oxide;
(3) mixing 5-10 parts by weight of modified graphene oxide, 5-10 parts by weight of zinc chloride solution and 20-30 parts by weight of water, adjusting the pH to 8.0 by using urea solution, and performing hydrothermal reaction to obtain a mixed solution;
(4) and mixing 1-2 parts of dilute hydrochloric acid solution and 5-10 parts of mixed solution in parts by weight, and stirring for 0.5-1 h to obtain the antistatic agent.
2. The method for preparing the antistatic agent for the cotton fabrics, according to claim 1, is characterized in that the sodium azide in the step (1) is a dimethylformamide solution of the sodium azide with the mass fraction of 40-41%.
3. The method for preparing the cotton fabric antistatic agent according to claim 1, wherein the zinc chloride solution in the step (3) is 20-30% by mass.
4. The method for preparing the cotton fabric antistatic agent according to claim 1, wherein the urea solution in the step (3) is a urea solution with a mass fraction of 15-20%.
5. The method for preparing the antistatic agent for the cotton fabrics according to claim 1, wherein the hydrothermal reaction in the step (3) is carried out for 1-2 h at 140-180 ℃ and 1.2-3.2 MPa.
6. The method for preparing the antistatic agent for the cotton fabric according to claim 1, wherein the dilute hydrochloric acid solution in the step (4) is a dilute hydrochloric acid solution with a mass fraction of 5-10%.
CN201810817253.6A 2018-07-24 2018-07-24 Antistatic agent for cotton fabric Active CN108867030B (en)

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CN111996611B (en) * 2020-09-03 2022-11-22 湖北尚助化学有限公司 Antistatic agent and preparation method thereof
CN116084190A (en) * 2022-12-29 2023-05-09 江苏华达新材料科技有限公司 Antistatic dyeing auxiliary agent and preparation method and application thereof

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CN105085835B (en) * 2014-05-14 2018-01-16 泰山玻璃纤维有限公司 A kind of graphene modified polyvinyl acetate class film forming agent preparation method
CN104370284A (en) * 2014-10-24 2015-02-25 国网山西省电力公司晋城供电公司 Preparation method of controllable high-substitution hydroxyl functionalized graphene
CN105088793A (en) * 2015-08-25 2015-11-25 无锡市长安曙光手套厂 Non-woven fabric, and preparation method and application thereof
CN106892425A (en) * 2017-04-27 2017-06-27 山东金城石墨烯科技有限公司 A kind of preparation method of nitration Graphene
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