CN115161796A - High-wear-resistance impact-resistance polyamide cord fabric - Google Patents
High-wear-resistance impact-resistance polyamide cord fabric Download PDFInfo
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- CN115161796A CN115161796A CN202210781842.XA CN202210781842A CN115161796A CN 115161796 A CN115161796 A CN 115161796A CN 202210781842 A CN202210781842 A CN 202210781842A CN 115161796 A CN115161796 A CN 115161796A
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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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/90—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyamides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05C—APPARATUS FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05C3/00—Apparatus in which the work is brought into contact with a bulk quantity of liquid or other fluent material
- B05C3/02—Apparatus in which the work is brought into contact with a bulk quantity of liquid or other fluent material the work being immersed in the liquid or other fluent material
- B05C3/12—Apparatus in which the work is brought into contact with a bulk quantity of liquid or other fluent material the work being immersed in the liquid or other fluent material for treating work of indefinite length
- B05C3/125—Apparatus in which the work is brought into contact with a bulk quantity of liquid or other fluent material the work being immersed in the liquid or other fluent material for treating work of indefinite length the work being a web, band, strip or the like
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/02—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by baking
- B05D3/0254—After-treatment
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/04—Formation of amino groups in compounds containing carboxyl groups
- C07C227/06—Formation of amino groups in compounds containing carboxyl groups by addition or substitution reactions, without increasing the number of carbon atoms in the carbon skeleton of the acid
- C07C227/08—Formation of amino groups in compounds containing carboxyl groups by addition or substitution reactions, without increasing the number of carbon atoms in the carbon skeleton of the acid by reaction of ammonia or amines with acids containing functional groups
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/03—Preparation of carboxylic acid esters by reacting an ester group with a hydroxy group
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/30—Preparation of carboxylic acid esters by modifying the acid moiety of the ester, such modification not being an introduction of an ester group
- C07C67/307—Preparation of carboxylic acid esters by modifying the acid moiety of the ester, such modification not being an introduction of an ester group by introduction of halogen; by substitution of halogen atoms by other halogen atoms
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/30—Preparation of carboxylic acid esters by modifying the acid moiety of the ester, such modification not being an introduction of an ester group
- C07C67/333—Preparation of carboxylic acid esters by modifying the acid moiety of the ester, such modification not being an introduction of an ester group by isomerisation; by change of size of the carbon skeleton
- C07C67/343—Preparation of carboxylic acid esters by modifying the acid moiety of the ester, such modification not being an introduction of an ester group by isomerisation; by change of size of the carbon skeleton by increase in the number of carbon atoms
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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
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- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G3/00—Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
- D02G3/44—Yarns or threads characterised by the purpose for which they are designed
- D02G3/48—Tyre cords
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06C—FINISHING, DRESSING, TENTERING OR STRETCHING TEXTILE FABRICS
- D06C3/00—Stretching, tentering or spreading textile fabrics; Producing elasticity in textile fabrics
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06C—FINISHING, DRESSING, TENTERING OR STRETCHING TEXTILE FABRICS
- D06C7/00—Heating or cooling textile fabrics
- D06C7/02—Setting
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Abstract
The invention relates to the field of cord fabrics, and aims to solve the problems that the existing cord fabrics are poor in mechanical property and poor in wear resistance and impact resistance when being bonded with rubber to form tires, and particularly relates to high-wear-resistance impact-resistance nylon cord fabrics; the wear-resistant impact-resistant additive and the silicon nitride are added into the nylon 6 slices for blending, so that the mechanical property of the modified nylon yarn prepared from the nylon 6 can be obviously improved, the nylon cord fabric with excellent mechanical property is prepared, and the nylon cord fabric can bear huge pressure, impact load and strong vibration when applied to a tire framework, so that the wear resistance and impact resistance of the tire are improved, and the service life of the tire is prolonged.
Description
Technical Field
The invention relates to the field of cord fabrics, in particular to high-wear-resistance impact-resistance nylon cord fabric.
Background
With the continuous development of the automobile industry and the tire industry and the improvement of the living quality requirements of people, the requirements on the comprehensive performance of the tire are higher and higher, and particularly, the requirements on comfort, oil saving, environmental protection and the like when the tire is used are higher, so that the higher requirements are provided for the framework material of the tire. The cord fabric is used as a framework of various rubber products such as tires and the like, and can bear huge pressure, impact load and strong vibration, so the cord fabric is an important material affecting the performance and the service life of the tires.
However, the existing cord fabric has poor mechanical properties, and the tire made by bonding the cord fabric with rubber still has the problem of poor wear resistance and impact resistance, and how to improve the problem that the existing cord fabric has poor mechanical properties is the key of the invention, so a high wear resistance and impact resistance nylon cord fabric is urgently needed to solve the problems.
Disclosure of Invention
In order to overcome the technical problems, the invention aims to provide nylon cord fabric with high wear resistance and impact resistance: the method comprises the steps of uniformly mixing nylon 6 slices, a wear-resistant impact-resistant additive, silicon nitride and a coupling agent to obtain a mixture, putting the mixture into an extruder to be melted and extruded, spinning to obtain modified nylon yarns, stranding and twisting the modified nylon yarns on a straight twisting machine to obtain cord threads, weaving and forming the cord threads, dipping, drying, stretching and shaping, and rolling into a fabric roll to obtain the high-wear-resistant impact-resistant nylon cord fabric.
The purpose of the invention can be realized by the following technical scheme:
the nylon cord fabric with high wear resistance and impact resistance is prepared by the following steps:
the method comprises the following steps: weighing 50-60 parts of chinlon 6 slices, 5-15 parts of wear-resistant and impact-resistant additive, 3-12 parts of silicon nitride and 1-3 parts of coupling agent according to parts by weight for later use; the coupling agent is a silane coupling agent KH-560;
step two: uniformly mixing nylon 6 slices, a wear-resistant and impact-resistant additive, silicon nitride and a coupling agent to obtain a mixture;
step three: putting the mixture into an extruder for melt extrusion, and spinning to obtain modified nylon yarns;
step four: carrying out plying and twisting on the modified nylon yarn on a direct twisting machine to obtain a cord;
step five: and (3) knitting the cord thread for forming, and then rolling the cord thread into a cloth roll after dipping, drying, stretching and shaping treatment to obtain the high-wear-resistance impact-resistance nylon cord fabric.
As a further scheme of the invention: the wear-resistant and impact-resistant additive is prepared by the following steps:
a1: adding isophthalic acid and absolute ethyl alcohol into a three-neck flask provided with a stirrer, a thermometer and a constant-pressure dropping funnel, stirring for 15-20min under the conditions that the temperature is 30-35 ℃ and the stirring speed is 300-400r/min, then dropwise adding acetyl chloride while stirring, controlling the dropwise adding speed to be 1-2 drops/s, continuously stirring and reacting for 3-5h after the dropwise adding is finished, carrying out vacuum filtration on a reaction product after the reaction is finished, washing a filter cake for 2-3 times by using absolute methyl alcohol, then placing the filter cake into a vacuum drying box, and drying for 3-5h under the condition that the temperature is 55-65 ℃ to obtain an intermediate 1;
the reaction principle is as follows:
a2: adding the intermediate 1, deionized water, concentrated sulfuric acid and anhydrous methanol into a three-neck flask provided with a stirrer, a thermometer and a constant-pressure dropping funnel, stirring for 20-30min under the conditions that the temperature is-5-0 ℃ and the stirring speed is 300-400r/min, then dropwise adding the mixed solution while stirring, controlling the dropwise adding speed to be 1-2 drops/s, continuously stirring and reacting for 1-1.5h under the condition that the temperature is increased to 25-30 ℃ after the dropwise adding is finished, adding potassium carbonate powder into a reaction product after the reaction is finished to adjust the pH to be 6-7, then carrying out vacuum filtration, washing the filtrate for 2-3 times by using ethyl acetate, then extracting for 2-3 times by using trichloromethane, drying the extract by using anhydrous sodium sulfate, then filtering, and carrying out rotary evaporation on the filtrate to remove the solvent to obtain an intermediate 2;
the reaction principle is as follows:
a3: adding the intermediate 2 and anhydrous methanol into a three-neck flask provided with a stirrer, a thermometer, a gas-guide tube and a constant-pressure dropping funnel, introducing nitrogen for protection, adding octafluoropentanol dropwise while stirring under the conditions that the temperature is-5-0 ℃ and the stirring speed is 300-400r/min, controlling the dropwise adding speed to be 1-2 drops/s, continuously stirring and reacting for 20-30min after the dropwise adding is finished, then continuously stirring and reacting for 10-15h under the condition of heating to 25-30 ℃, removing the solvent by rotary evaporation of a reaction product after the reaction is finished, then placing the reaction product in a vacuum drying box, and drying for 8-10h under the condition of the temperature of 40-45 ℃ to obtain an intermediate 3;
the reaction principle is as follows:
a4: adding the intermediate 3 and hydrobromic acid solution into a four-neck flask provided with a stirrer, a thermometer, a reflux condenser tube and a constant-pressure dropping funnel, dropwise adding acetic anhydride while stirring at the stirring speed of 300-400r/min at the temperature of 25-30 ℃, controlling the dropwise adding speed to be 1-2 drops/s, heating to reflux while stirring after dropwise adding is finished, controlling the heating speed to be 2-3 ℃/min, then continuously stirring for reaction for 10-15h, evaporating and concentrating a reaction product to half of the original volume after the reaction is finished, then adjusting the pH to be 8-9 by using a saturated sodium carbonate solution, precipitating and precipitating a precipitate, then carrying out vacuum filtration, placing a filter cake into a vacuum drying oven, and drying for 6-8h at the temperature of 60-65 ℃ to obtain an intermediate 4;
the reaction principle is as follows:
a5: adding the intermediate 4 and anhydrous acetonitrile into a three-neck flask provided with a stirrer and a thermometer, stirring for 20-30min at the temperature of 25-30 ℃ and at the stirring speed of 300-400r/min, then adding p-phenylenediamine and anhydrous sodium carbonate, continuing stirring for reaction for 3-5h at the temperature of 85-90 ℃, after the reaction is finished, carrying out rotary evaporation on a reaction product to remove the solvent, then adding the reaction product into the mixed solution, standing for layering, washing the organic phase with saturated saline solution for 2-3 times, then drying with anhydrous magnesium sulfate, carrying out vacuum filtration, carrying out rotary evaporation on the filtrate to remove the solvent, and thus obtaining the wear-resistant impact-resistant additive.
The reaction principle is as follows:
as a further scheme of the invention: the dosage ratio of the isophthalic acid, the absolute ethyl alcohol and the acetyl chloride in the step A1 is 0.1mol:80-100mL:0.2mol.
As a further scheme of the invention: the using ratio of the intermediate 1, the deionized water, the concentrated sulfuric acid, the anhydrous methanol and the mixed solution in the step A2 is 10mmol:8.5mL:3.5mL:15mL of: 18g, wherein the mass fraction of the concentrated sulfuric acid is 98%, and the mixed solution is 30% of hydrogen peroxide and 20% of ferrous sulfate solution according to a mass ratio of 1:0.6 of the mixture.
As a further scheme of the invention: the dosage ratio of the intermediate 2, the anhydrous methanol and the octafluoropentanol in the step A3 is 0.1mol:100-120mL:0.2mol.
As a further scheme of the invention: the dosage ratio of the intermediate 3, the hydrobromic acid solution and the acetic anhydride in the step A4 is 10mmol:30-40mL:35-45mL, and the mass fraction of the hydrobromic acid solution is 40%.
As a further scheme of the invention: the dosage ratio of the intermediate 4, the anhydrous acetonitrile, the p-phenylenediamine and the anhydrous sodium carbonate in the step A5 is 20mmol:40-50mL:10mmol:10mmol, wherein the mixed solution is prepared by mixing ethyl acetate and deionized water according to a volume ratio of 2-3:1, and (b) a mixed solution.
The invention has the beneficial effects that:
the high-wear-resistance impact-resistance nylon cord fabric is prepared by uniformly mixing nylon 6 slices, a wear-resistance impact-resistance additive, silicon nitride and a coupling agent to obtain a mixture, putting the mixture into an extruder for melt extrusion, spinning to obtain modified nylon silk threads, stranding and twisting the modified nylon silk threads on a straight twisting machine to obtain cord threads, weaving the cord threads for molding, dipping, drying, stretching and shaping, and rolling into a fabric roll to obtain the high-wear-resistance impact-resistance nylon cord fabric; the wear-resistant impact-resistant additive and the silicon nitride are added into the nylon 6 slices for blending, so that the mechanical property of the modified nylon yarn prepared from the nylon 6 can be obviously improved, the nylon cord fabric with excellent mechanical property is prepared, and the nylon cord fabric can bear huge pressure, impact load and strong vibration when applied to a tire framework, so that the wear resistance and impact resistance of the tire are improved, and the service life of the tire is prolonged.
Firstly, isophthalic acid reacts with acetyl chloride to generate ester groups, an intermediate 1 is obtained, then alcoholic hydroxyl groups are introduced to a benzene ring of the intermediate 1 to obtain an intermediate 2, then the ester groups on the intermediate 2 and the hydroxyl groups on octafluoropentanol undergo an ester exchange reaction, so that a large number of C-F bonds are introduced to the intermediate 2 to obtain an intermediate 3, then the alcoholic hydroxyl groups on the intermediate 3 are substituted by hydrobromic acid, bromine atoms are introduced to obtain an intermediate 4, then the bromine atoms on the intermediate 4 and the amino groups on p-phenylenediamine undergo a nucleophilic substitution reaction, so that the intermediate 4 is connected to two ends of the p-phenylenediamine to obtain the wear-resistant and impact-resistant additive; the molecular structure of the wear-resistant impact-resistant additive contains a large number of benzene rings and C-F bonds, the benzene rings and the C-F bonds are high in stability and difficult to destroy, so that the nylon cord fabric is endowed with good mechanical properties, then silicon nitride is added, the silicon nitride is excellent in mechanical properties, and is added into nylon 6 as a filler to modify the nylon 6, so that the mechanical properties of the nylon cord fabric are further improved, and finally the high-wear-resistant impact-resistant nylon cord fabric is prepared.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the embodiment is a preparation method of a wear-resistant and impact-resistant additive, which comprises the following steps:
a1: adding 0.1mol of isophthalic acid and 80mL of absolute ethyl alcohol into a three-neck flask provided with a stirrer, a thermometer and a constant-pressure dropping funnel, stirring for 15min under the conditions that the temperature is 30 ℃ and the stirring rate is 300r/min, then dropwise adding 0.2mol of acetyl chloride while stirring, controlling the dropwise adding rate to be 1 drop/s, continuing stirring and reacting for 3h after the dropwise adding is finished, carrying out vacuum filtration on a reaction product after the reaction is finished, washing a filter cake for 2 times by using absolute methyl alcohol, then placing the filter cake into a vacuum drying oven, and drying for 3h under the condition that the temperature is 55 ℃ to obtain an intermediate 1;
a2: adding 10mmol of intermediate 1, 8.5mL of deionized water, 3.5mL of 98 mass percent concentrated sulfuric acid and 15mL of anhydrous methanol into a three-neck flask provided with a stirrer, a thermometer and a constant-pressure dropping funnel, stirring for 20min under the conditions that the temperature is-5 ℃ and the stirring speed is 300r/min, and then dropwise adding 18g of 30 mass percent hydrogen peroxide and 20 mass percent ferrous sulfate solution while stirring according to the mass ratio of 1:0.6, controlling the dropping rate to be 1 drop/s, heating to 25 ℃ after the dropping is finished, continuing stirring for reaction for 1h, adding potassium carbonate powder into a reaction product after the reaction is finished, adjusting the pH to be 6, then carrying out vacuum filtration, washing the filtrate for 2 times by using ethyl acetate, then extracting for 2 times by using trichloromethane, drying the extract by using anhydrous sodium sulfate, then filtering, and carrying out rotary evaporation on the filtrate to remove the solvent to obtain an intermediate 2;
a3: adding 0.1mol of intermediate 2 and 100mL of anhydrous methanol into a three-neck flask provided with a stirrer, a thermometer, a gas-guide tube and a constant-pressure dropping funnel, introducing nitrogen for protection, dropwise adding 0.2mol of octafluoropentanol while stirring at the temperature of-5 ℃ and the stirring speed of 300r/min, controlling the dropwise adding speed to be 1 drop/s, continuously stirring and reacting for 20min after the dropwise adding is finished, then continuously stirring and reacting for 10h under the condition of heating to 25 ℃, removing the solvent by rotary evaporation of a reaction product after the reaction is finished, then placing the reaction product in a vacuum drying oven, and drying for 8h under the condition of the temperature of 40 ℃ to obtain an intermediate 3;
a4: adding 10mmol of intermediate 3 and 30mL of hydrobromic acid solution with the mass fraction of 40% into a four-neck flask provided with a stirrer, a thermometer, a reflux condenser tube and a constant-pressure dropping funnel, dropwise adding 35mL of acetic anhydride while stirring at the stirring speed of 300r/min at the temperature of 25 ℃, controlling the dropwise adding rate to be 1 drop/s, heating to reflux while stirring after dropwise adding is finished, controlling the heating rate to be 2 ℃/min, continuing stirring for reaction for 10 hours, evaporating and concentrating a reaction product to be half of the original volume after the reaction is finished, adjusting the pH to be 8 by using a saturated sodium carbonate solution, precipitating and precipitating precipitates, then carrying out vacuum filtration, placing a filter cake into a vacuum drying box, and drying for 6 hours at the temperature of 60 ℃ to obtain an intermediate 4;
a5: adding 20mmol of intermediate 4 and 40mL of anhydrous acetonitrile into a three-neck flask provided with a stirrer and a thermometer, stirring for 20min at the temperature of 25 ℃ and the stirring speed of 300r/min, then adding 10mmol of p-phenylenediamine and 10mmol of anhydrous sodium carbonate, continuing stirring and reacting for 3h at the temperature of 85 ℃, removing the solvent by rotary evaporation of the reaction product after the reaction is finished, and then adding ethyl acetate and deionized water according to the volume ratio of 2:1, standing for layering, washing the organic phase with saturated saline solution for 2 times, drying with anhydrous magnesium sulfate, carrying out vacuum filtration, and carrying out rotary evaporation on the filtrate to remove the solvent, thereby obtaining the wear-resistant and impact-resistant additive.
Example 2:
this embodiment is a method for preparing a wear-resistant and impact-resistant additive, comprising the following steps:
a1: adding 0.1mol of isophthalic acid and 100mL of absolute ethyl alcohol into a three-neck flask provided with a stirrer, a thermometer and a constant-pressure dropping funnel, stirring for 20min under the conditions that the temperature is 35 ℃ and the stirring speed is 400r/min, then dropwise adding 0.2mol of acetyl chloride while stirring, controlling the dropwise adding speed to be 2 drops/s, continuing stirring and reacting for 5h after the dropwise adding is finished, carrying out vacuum filtration on a reaction product after the reaction is finished, washing a filter cake for 3 times by using absolute methyl alcohol, then placing the filter cake into a vacuum drying box, and drying for 5h under the condition that the temperature is 65 ℃ to obtain an intermediate 1;
a2: adding 10mmol of intermediate 1, 8.5mL of deionized water, 3.5mL of 98% concentrated sulfuric acid and 15mL of anhydrous methanol into a three-neck flask provided with a stirrer, a thermometer and a constant-pressure dropping funnel, stirring for 30min at the temperature of 0 ℃ and the stirring speed of 400r/min, and then dropwise adding 18g of 30% hydrogen peroxide and 20% ferrous sulfate solution according to the mass ratio of 1:0.6, controlling the dropping rate to be 2 drops/s, heating to 30 ℃ after the dropping is finished, continuing stirring for reacting for 1.5 hours, adding potassium carbonate powder into a reaction product after the reaction is finished, adjusting the pH to 7, then carrying out vacuum filtration, washing the filtrate for 3 times by using ethyl acetate, then extracting for 3 times by using trichloromethane, drying the extract by using anhydrous sodium sulfate, then filtering, and carrying out rotary evaporation on the filtrate to remove the solvent to obtain an intermediate 2;
a3: adding 0.1mol of intermediate 2 and 120mL of anhydrous methanol into a three-neck flask provided with a stirrer, a thermometer, a gas-guide tube and a constant-pressure dropping funnel, introducing nitrogen for protection, dropwise adding 0.2mol of octafluoropentanol while stirring at the temperature of 0 ℃ and the stirring speed of 400r/min, controlling the dropwise adding speed to be 2 drops/s, continuously stirring and reacting for 30min after the dropwise adding is finished, then continuously stirring and reacting for 15h under the condition of heating to 30 ℃, removing the solvent by rotary evaporation of a reaction product after the reaction is finished, then placing the reaction product in a vacuum drying oven, and drying for 10h under the condition of the temperature of 45 ℃ to obtain an intermediate 3;
a4: adding 10mmol of intermediate 3 and 40mL of hydrobromic acid solution with the mass fraction of 40% into a four-neck flask provided with a stirrer, a thermometer, a reflux condenser tube and a constant-pressure dropping funnel, dropwise adding 45mL of acetic anhydride while stirring at the stirring speed of 400r/min at the temperature of 30 ℃, controlling the dropwise adding speed to be 2 drops/s, heating to reflux while stirring after dropwise adding is finished, controlling the heating speed to be 3 ℃/min, continuing stirring for reaction for 15 hours, evaporating and concentrating a reaction product to be half of the original volume after the reaction is finished, adjusting the pH to be 9 by using a saturated sodium carbonate solution, precipitating and precipitating precipitates, then carrying out vacuum suction filtration, placing a filter cake into a vacuum drying box, and drying for 8 hours at the temperature of 65 ℃ to obtain an intermediate 4;
a5: adding 20mmol of intermediate 4 and 50mL of anhydrous acetonitrile into a three-neck flask provided with a stirrer and a thermometer, stirring for 30min at the temperature of 30 ℃ and the stirring speed of 400r/min, then adding 10mmol of p-phenylenediamine and 10mmol of anhydrous sodium carbonate, continuing stirring and reacting for 5h at the temperature of 90 ℃, removing the solvent by rotary evaporation of the reaction product after the reaction is finished, and then adding ethyl acetate and deionized water according to the volume ratio of 3:1, standing and layering, washing the organic phase with saturated saline solution for 3 times, drying with anhydrous magnesium sulfate, carrying out vacuum filtration, and carrying out rotary evaporation on the filtrate to remove the solvent to obtain the wear-resistant and impact-resistant additive.
Example 3:
the embodiment is high-wear-resistant impact-resistant nylon cord fabric which is prepared by the following steps:
the method comprises the following steps: weighing 50 parts of chinlon 6 slices, 5 parts of wear-resistant and impact-resistant additive from example 1, 3 parts of silicon nitride and 1 part of coupling agent in parts by weight for later use; the coupling agent is a silane coupling agent KH-560;
step two: uniformly mixing nylon 6 slices, a wear-resistant and impact-resistant additive, silicon nitride and a coupling agent to obtain a mixture;
step three: putting the mixture into an extruder for melt extrusion, and spinning to obtain modified nylon yarns;
step four: carrying out plying and twisting on the modified nylon yarn on a direct twisting machine to obtain a cord;
step five: and (3) knitting and molding the cord thread, and then rolling into a fabric roll after gum dipping, drying, stretching and shaping treatment to obtain the high-wear-resistance impact-resistance nylon cord fabric.
Example 4:
the embodiment is high-wear-resistant impact-resistant nylon cord fabric which is prepared by the following steps:
the method comprises the following steps: weighing 60 parts of nylon 6 slices, 15 parts of wear-resistant and impact-resistant additive from example 2, 12 parts of silicon nitride and 3 parts of coupling agent according to parts by weight for later use; the coupling agent is a silane coupling agent KH-560;
step two: uniformly mixing chinlon 6 slices, a wear-resistant and impact-resistant additive, silicon nitride and a coupling agent to obtain a mixture;
step three: putting the mixture into an extruder for melt extrusion, and spinning to obtain modified nylon yarns;
step four: carrying out plying and twisting on the modified nylon yarn on a direct twisting machine to obtain a cord;
step five: and (3) knitting the cord thread for forming, and then rolling the cord thread into a cloth roll after dipping, drying, stretching and shaping treatment to obtain the high-wear-resistance impact-resistance nylon cord fabric.
Comparative example 1:
comparative example 1 differs from example 4 in that the wear-resistant impact-resistant additive and silicon nitride are not added.
Comparative example 2:
comparative example 2 differs from example 4 in that no abrasion and impact resistant additive is added.
Comparative example 3:
comparative example 3 differs from example 4 in that no silicon nitride is added.
The performances of the nylon cord fabrics with high wear resistance and impact resistance in the examples 3-4 and the comparative examples 1-3 are detected, and the detection results are shown in the following table:
referring to the data in the table, it can be known from the comparison between example 4 and comparative examples 1 to 3 that the mechanical properties of the nylon cord fabric with high wear resistance and impact resistance can be obviously improved by adding the wear resistance and impact resistance additive and the silicon nitride, so that the wear resistance and impact resistance of the tire can be improved.
In the description herein, references to the description of "one embodiment," "an example," "a specific example," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only, and it will be appreciated by those skilled in the art that various modifications, additions and substitutions can be made to the embodiments described without departing from the scope of the invention as defined in the appended claims.
Claims (7)
1. The high-wear-resistance impact-resistance nylon cord fabric is characterized by being prepared by the following steps:
the method comprises the following steps: weighing 50-60 parts of chinlon 6 slices, 5-15 parts of wear-resistant and impact-resistant additive, 3-12 parts of silicon nitride and 1-3 parts of coupling agent according to parts by weight for later use; the coupling agent is a silane coupling agent KH-560;
step two: uniformly mixing nylon 6 slices, a wear-resistant and impact-resistant additive, silicon nitride and a coupling agent to obtain a mixture;
step three: putting the mixture into an extruder for melt extrusion, and spinning to obtain modified nylon yarns;
step four: carrying out plying and twisting on the modified nylon yarn on a direct twisting machine to obtain a cord;
step five: and (3) knitting and molding the cord thread, and then rolling into a fabric roll after gum dipping, drying, stretching and shaping treatment to obtain the high-wear-resistance impact-resistance nylon cord fabric.
2. The nylon cord fabric with high wear resistance and impact resistance as claimed in claim 1, wherein the wear-resistant and impact-resistant additive is prepared by the following steps:
a1: adding isophthalic acid and absolute ethyl alcohol into a three-neck flask, stirring, dropwise adding acetyl chloride while stirring, continuing stirring for reaction after dropwise adding, performing vacuum filtration on a reaction product after the reaction is finished, and washing and drying a filter cake to obtain an intermediate 1;
a2: adding the intermediate 1, deionized water, concentrated sulfuric acid and anhydrous methanol into a three-neck flask, stirring, dropwise adding the mixed solution while stirring, heating after dropwise adding, continuously stirring for reaction, adjusting the pH value of a reaction product after the reaction is finished, performing vacuum filtration, washing and extracting filtrate, drying, filtering and performing rotary evaporation on the extract to obtain an intermediate 2;
a3: adding the intermediate 2 and anhydrous methanol into a three-neck flask, dropwise adding octafluoropentanol while stirring, continuously stirring for reaction after dropwise adding is finished, and performing rotary evaporation on a reaction product after the reaction is finished, and then drying to obtain an intermediate 3;
a4: adding the intermediate 3 and hydrobromic acid solution into a four-neck flask, dropwise adding acetic anhydride while stirring, stirring and heating to reflux after dropwise addition is finished, then continuously stirring for reaction, evaporating and concentrating a reaction product after the reaction is finished, then adjusting pH, precipitating a precipitate, then performing vacuum filtration, and drying a filter cake to obtain an intermediate 4;
a5: adding the intermediate 4 and anhydrous acetonitrile into a three-neck flask, stirring, adding p-phenylenediamine and anhydrous sodium carbonate, heating, continuously stirring for reaction, carrying out rotary evaporation on a reaction product after the reaction is finished, adding the reaction product into a mixed solution, standing for layering, washing and drying an organic phase, carrying out vacuum filtration, and carrying out rotary evaporation on a filtrate to obtain the wear-resistant and impact-resistant additive.
3. The nylon cord fabric with high wear resistance and impact resistance according to claim 2, wherein the usage ratio of the isophthalic acid, the absolute ethyl alcohol and the acetyl chloride in the step A1 is 0.1mol:80-100mL:0.2mol.
4. The nylon cord fabric with high wear resistance and impact resistance according to claim 2, wherein the intermediate 1, deionized water, concentrated sulfuric acid, anhydrous methanol and the mixed solution in the step A2 are used in a ratio of 10mmol:8.5mL:3.5mL:15mL of: 18g, the mass fraction of the concentrated sulfuric acid is 98%, and the mixed solution is 30% of hydrogen peroxide and 20% of ferrous sulfate solution according to the mass ratio of 1:0.6 of the mixture.
5. The nylon cord fabric with high wear resistance and impact resistance according to claim 2, wherein the amount ratio of the intermediate 2, the anhydrous methanol and the octafluoropentanol in the step A3 is 0.1mol:100-120mL:0.2mol.
6. The nylon cord fabric with high wear resistance and impact resistance according to claim 2, wherein the intermediate 3, the hydrobromic acid solution and the acetic anhydride in the step A4 are used in a ratio of 10mmol:30-40mL:35-45mL, and the mass fraction of the hydrobromic acid solution is 40%.
7. The nylon cord fabric with high wear resistance and impact resistance according to claim 2, wherein the amount ratio of the intermediate 4, anhydrous acetonitrile, p-phenylenediamine and anhydrous sodium carbonate in the step A5 is 20mmol:40-50mL:10mmol:10mmol, wherein the mixed solution is prepared by mixing ethyl acetate and deionized water according to a volume ratio of 2-3:1, and (b) a mixed solution.
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