CN114755257B - Method and equipment for testing electron irradiation carcass ply pre-crosslinking by using differential scanning calorimeter - Google Patents
Method and equipment for testing electron irradiation carcass ply pre-crosslinking by using differential scanning calorimeter Download PDFInfo
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- CN114755257B CN114755257B CN202210422188.3A CN202210422188A CN114755257B CN 114755257 B CN114755257 B CN 114755257B CN 202210422188 A CN202210422188 A CN 202210422188A CN 114755257 B CN114755257 B CN 114755257B
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- electron irradiation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/02—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering
- G01N25/12—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering of critical point; of other phase change
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C35/00—Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
- B29C35/002—Component parts, details or accessories; Auxiliary operations
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C35/00—Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
- B29C35/02—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould
- B29C35/08—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould by wave energy or particle radiation
- B29C35/0866—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould by wave energy or particle radiation using particle radiation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K17/00—Measuring quantity of heat
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/20—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C35/00—Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
- B29C35/02—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould
- B29C35/08—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould by wave energy or particle radiation
- B29C35/0866—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould by wave energy or particle radiation using particle radiation
- B29C2035/0877—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould by wave energy or particle radiation using particle radiation using electron radiation, e.g. beta-rays
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
- B29L2030/00—Pneumatic or solid tyres or parts thereof
- B29L2030/002—Treads
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
Abstract
The application belongs to the technical field of tire production control, and particularly relates to a method and equipment for testing electron irradiation carcass ply pre-crosslinking by using a differential scanning calorimeter. A method of testing electron-irradiated carcass ply pre-crosslinking using a differential scanning calorimeter, the method comprising the steps of: 1) Sampling the rubber materials on the front side and the back side of the carcass ply after the rubber coating, and distinguishing the rubber materials on the front side and the back side; 2) Respectively analyzing the sizing materials on the front side and the back side by a differential scanning calorimeter; 3) And comparing the glass transition temperature results of the rubber materials at the positive side and the negative side, and judging that the carcass ply is subjected to electron irradiation when the difference value of the glass transition temperatures of the rubber materials at the positive side and the negative side is 1.0-3.5 ℃. The method has the advantages of simplified testing process, standardized operation flow, digitalized result and simplified electron irradiation mechanism. By the design of the invention, the simplicity and convenience of a testing method are obviously improved, and whether the carcass ply is successfully subjected to electron irradiation pre-crosslinking and mechanism hierarchical analysis are timely known.
Description
Technical Field
The application belongs to the technical field of tire production control, and particularly relates to a method and equipment for testing electron irradiation carcass ply pre-crosslinking by using a differential scanning calorimeter.
Background
The automotive industry is rapidly developing worldwide, and automobile tires are an important component of vehicles, and the quality and performance of the tires directly affect the performance of the vehicles. The radial tire carcass ply is a carcass layer composed of rubber-covered tyre cord fabric and is a stressed framework layer of the tire. Radial tires are classified according to carcass framework materials, and the carcass is a steel wire, called all-steel tire, and is generally used for commercial heavy duty tires; the carcass is a fibrous semi-steel tire, commonly used for passenger tires.
The passenger car tires in the current market have poor operability and large rolling resistance, and a carcass ply with higher fatigue resistance and strength is urgently needed to meet the requirements of semi-steel radial car tires. The carcass ply of the semisteel radial car tire in the market at present is subjected to electron irradiation in a delayed time, and the glue stock is subjected to pre-crosslinking treatment to improve the adhesion between the ply and the inner liner, so that higher fatigue resistance and strength are obtained.
The Chinese patent application (publication No. CN109291339A, publication No. 20190201) of the applicant discloses a method for changing the performance of a rubberized fabric by electron irradiation, comprising the steps of: the fiber curtain cloth enters an electron irradiation area of a double-window electron irradiation device, wherein parameters of the double-window electron irradiation device are voltage 500KV and dose 40KGY, and irradiation dose fluctuation is less than 5%. The stability of the electron irradiation parameters directly influences the quality of the tire fiber curtain cloth, and the tire fiber curtain cloth needs to be marked for the abnormal irradiation dose of the tire fiber curtain cloth generated by special reasons according to the Chinese patent application (publication number: CN111376509A, application publication date: 20200707) filed by the applicant, thereby being beneficial to the subsequent isolation treatment of the abnormal tire fiber curtain cloth.
In the prior application (application publication number: CN114235607A, application publication date: 2022.03.25), an evaluation method for pre-crosslinking of a tire cord fabric is invented, the elastic modulus and the viscous modulus obtained by strain scanning of a rubber processing analyzer are plotted against strain change, a curve can not only reflect the magnitude of the modulus, but also intuitively distinguish the elastic modulus and the viscous modulus of the tire cord fabric, and the pre-crosslinking rate of the tire cord fabric after electron irradiation is deduced according to the curve area. The invention directly provides a calculation method for detecting the pre-crosslinking degree of the carcass ply, however, the method has the following defects: (1) The method is suitable for laboratory detection and analysis, but is not suitable for engineering field technicians to judge whether the carcass ply is successfully crosslinked; (2) the test method requires further optimization.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a method for testing electron irradiation carcass ply pre-crosslinking by using a differential scanning calorimeter, which has the advantages of simplified testing process, standardized operation flow, digitalized result and simplified electron irradiation mechanism. By the design of the invention, the simplicity and convenience of a testing method are obviously improved, and whether the carcass ply is successfully subjected to electron irradiation pre-crosslinking and mechanism hierarchical analysis are timely known.
In order to achieve the above object. The invention adopts the following technical scheme:
a method of testing electron-irradiated carcass ply pre-crosslinking using a differential scanning calorimeter, the method comprising the steps of:
1) Sampling the rubber materials on the front side and the back side of the carcass ply after the rubber coating, and distinguishing the rubber materials on the front side and the back side;
2) Respectively analyzing the sizing materials on the front side and the back side by a differential scanning calorimeter;
3) And comparing the glass transition temperature results of the rubber materials at the positive side and the negative side, and judging that the carcass ply is subjected to electron irradiation when the difference value of the glass transition temperatures of the rubber materials at the positive side and the negative side is 1.0-3.5 ℃.
Preferably, the usage parameters of the differential scanning calorimeter analysis include: detecting the temperature to be between 120 ℃ below zero and 20 ℃ and the temperature fluctuation range to +/-0.2 ℃; the temperature rise rate is 5 ℃/min.
Preferably, the glass transition temperature difference of the positive and negative side sizing materials is 1.5-3.0 ℃.
Preferably, the rubber material in the carcass ply comprises natural rubber, and the weight average molecular weight Mw needs to satisfy the range: 120 ten thousand < Mw < 270 ten thousand; the natural rubber is used in 80-100 parts by weight based on 100 parts by weight of rubber in the sizing material.
The invention further discloses a method for controlling the pre-crosslinking of the carcass ply by using the differential scanning calorimeter, which comprises the steps of collecting the glass transition temperatures of the rubber materials at the front side and the back side by using the differential scanning calorimeter, comparing the glass transition temperature results of the rubber materials at the front side and the back side, and judging that the carcass ply is successfully pre-crosslinked by using the carcass ply subjected to the electron irradiation when the glass transition temperature difference of the rubber materials at the front side and the back side is 1.0-3.5 ℃; and beyond the range of 1.0-3.5 ℃ of the glass transition temperature difference, regulating the work of the tire cord calendering site electron irradiation tube by outputting numerical values.
The invention further discloses equipment for controlling the pre-crosslinking of the carcass ply by using the differential scanning calorimeter, the equipment comprises the differential scanning calorimeter and a control system, the control system collects data of the differential scanning calorimeter, and the data of the differential scanning calorimeter are compared through the glass transition temperature results of the rubber materials at the front side and the back side, and the difference of the glass transition temperatures of the rubber materials at the front side and the back side is 1.0-3.5 ℃, so that the carcass ply is judged to be successfully pre-crosslinked by the electron irradiation; and beyond the range of 1.0-3.5 ℃ of the glass transition temperature difference, regulating the work of the tire cord calendering site electron irradiation tube by outputting numerical values.
Further, the invention also discloses a computer device, comprising a memory, a processor and a computer program stored on the memory, wherein the processor executes the computer program to realize the following method: collecting glass transition temperatures of the positive and negative side sizing materials, comparing the glass transition temperature results of the positive and negative side sizing materials, and judging that the carcass ply is successfully pre-crosslinked after electron irradiation if the difference value of the glass transition temperatures of the positive and negative side sizing materials is 1.0-3.5 ℃; and beyond the range of 1.0-3.5 ℃ of the glass transition temperature difference, regulating the work of the tire cord calendering site electron irradiation tube by outputting numerical values.
Further, the present invention also discloses a computer readable storage medium having stored thereon a computer program or instructions which when executed by a processor, performs the following method: collecting glass transition temperatures of the positive and negative side sizing materials, comparing the glass transition temperature results of the positive and negative side sizing materials, and judging that the carcass ply is successfully pre-crosslinked after electron irradiation if the difference value of the glass transition temperatures of the positive and negative side sizing materials is 1.0-3.5 ℃; and beyond the range of 1.0-3.5 ℃ of the glass transition temperature difference, regulating the work of the tire cord calendering site electron irradiation tube by outputting numerical values.
Further, the invention also discloses a computer program product comprising a computer program or instructions which, when executed by a processor, implement the method of: collecting glass transition temperatures of the positive and negative side sizing materials, comparing the glass transition temperature results of the positive and negative side sizing materials, and judging that the carcass ply is successfully pre-crosslinked after electron irradiation if the difference value of the glass transition temperatures of the positive and negative side sizing materials is 1.0-3.5 ℃; and beyond the range of 1.0-3.5 ℃ of the glass transition temperature difference, regulating the work of the tire cord calendering site electron irradiation tube by outputting numerical values.
By adopting the technical scheme, the invention uses the differential scanning calorimeter to characterize the glass transition temperature of the carcass ply compound subjected to electron irradiation after glue coating and the glass transition temperature of the carcass ply compound not subjected to electron irradiation after glue coating, so that whether the electron irradiation and the electron irradiation mechanism can be obviously distinguished. The method has the advantages of simplified testing process, standardized operation flow, digitalized result and simplified electron irradiation mechanism. By the design of the invention, the simplicity and convenience of a testing method are obviously improved, and whether the carcass ply is successfully subjected to electron irradiation pre-crosslinking and mechanism hierarchical analysis are timely known.
Drawings
FIG. 1 is a schematic view of an electron irradiated curtain, wherein the front side of the curtain is the side of the curtain subjected to electron irradiation, and the back side of the curtain is the side not subjected to electron irradiation.
FIG. 2 is a graph showing the glass transition temperature results for electron irradiated cord compounds and non-electron irradiated cord compounds.
Detailed Description
The technical scheme in the embodiment of the invention is checked and fully described in combination with the embodiment of the invention, and the invention is further explained. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. Given the embodiments of the present invention, all other embodiments that would be obvious to one of ordinary skill in the art without making any inventive effort are within the scope of the present invention.
The rubber material in the carcass ply of the invention contains natural rubber, and the weight average molecular weight Mw needs to satisfy the range: 120 ten thousand < Mw < 270 ten thousand; the natural rubber is used in 80-100 parts by weight based on 100 parts by weight of rubber in the sizing material.
The invention provides a method for analyzing the pre-crosslinking of a carcass ply compound by using a differential scanning calorimeter, which comprises the following steps: and (3) the coated carcass ply is not required to be treated in any chemical or physical mode, and the samples of the sizing materials on the front side and the back side of the carcass ply after the coating are respectively subjected to differential scanning calorimeter analysis.
The sizing material sampling method comprises the following steps: the carcass ply after the coating is sampled for the sizing material on the front side and the back side (the area is 1 cm) 2 ) Distinguishing the sizing materials on the front side and the back side, namely an electron irradiation side and a non-electron irradiation side; the carcass ply which is not irradiated by electrons after the glue coating is not distinguished.
Parameters used for analysis by the differential scanning calorimeter of the present invention include: detecting the temperature to be between 120 ℃ below zero and 20 ℃ and the temperature fluctuation range to +/-0.2 ℃; the temperature rise rate is 5 ℃/min.
Comparative examples and examples 1 to 5 are shown in tables 1 and 2 below.
TABLE 1 differentiation of the glass transition temperatures of examples 1-5
TABLE 2 differentiation of glass transition temperatures for comparative examples 1-2
Tables 1 and 2 show the glass transition temperature test results of different carcass ply compound formulations for electron irradiated and non-electron irradiated ply compounds of different specifications. In the embodiment, the glass transition temperatures have obvious numerical value difference, the glass transition temperature of the electron irradiation curtain cloth rubber material is obviously higher than that of the non-electron irradiation curtain cloth rubber material, and the electron irradiation generates slight crosslinking on the surface of the rubber material to influence the movement of the minimum unit of the rubber macromolecular chain, thereby influencing the glass transition temperature of the rubber macromolecular chain. The trend of the glass transition temperature characterization result is equivalent to that of a comparative example, and the Mooney result of the sizing material subjected to the electron irradiation and the non-electron irradiation has obvious positive significance for the electron irradiation management and control and research and development technicians in the calendaring site to know the electron irradiation mechanism.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art. The generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (9)
1. A method for testing electron-irradiated carcass ply pre-crosslinking using a differential scanning calorimeter, comprising the steps of:
1) Sampling the sizing materials on the front side and the back side of the carcass cord after the coating, and distinguishing an electron irradiation side from a non-electron irradiation side;
2) Respectively carrying out differential scanning calorimeter analysis on the electron irradiation side and the non-electron irradiation side;
3) Comparing the glass transition temperature results of the electron irradiation side and the non-electron irradiation side, and judging that the carcass ply is successfully pre-crosslinked after the electron irradiation when the difference of the glass transition temperatures of the electron irradiation side and the non-electron irradiation side is 1.0-3.5 ℃.
2. A method of testing electron-irradiated carcass ply pre-crosslinking using a differential scanning calorimeter as defined in claim 1, wherein the parameters of use analyzed by the differential scanning calorimeter comprise: detecting the temperature to be between 120 ℃ below zero and 20 ℃ and the temperature fluctuation range to +/-0.2 ℃; the temperature rise rate is 5 ℃/min.
3. A method of testing pre-cross-linking of electron irradiated carcass ply using a differential scanning calorimeter as claimed in claim 1, wherein the difference in glass transition temperature between the electron irradiated side and the non-electron irradiated side is 1.5-3.0 ℃.
4. A method according to any one of claims 1-3, wherein the size comprises natural rubber and the weight average molecular weight Mw is in the range of: 120 ten thousand < Mw < 270 ten thousand; the natural rubber is used in 80-100 parts by weight based on 100 parts by weight of rubber in the sizing material.
5. A method for controlling electron irradiation carcass ply pre-crosslinking by using a differential scanning calorimeter is characterized in that the method collects the glass transition temperatures of an electron irradiation side and a non-electron irradiation side by using the differential scanning calorimeter, and compares the glass transition temperature results of the electron irradiation side and the non-electron irradiation side, and judges that the carcass ply is successfully pre-crosslinked by the electron irradiation when the difference value of the glass transition temperatures of the electron irradiation side and the non-electron irradiation side is 1.0-3.5 ℃; and beyond the range of 1.0-3.5 ℃ of the glass transition temperature difference, regulating the work of the tire cord calendering site electron irradiation tube by outputting numerical values.
6. The equipment is characterized by comprising a differential scanning calorimeter and a control system, wherein the control system collects data of the differential scanning calorimeter, and compares the glass transition temperature results of an electron irradiation side and a non-electron irradiation side, and judges that the carcass ply is successfully pre-crosslinked after the electron irradiation if the glass transition temperature difference of the electron irradiation side and the non-electron irradiation side is 1.0-3.5 ℃; and beyond the range of 1.0-3.5 ℃ of the glass transition temperature difference, regulating the work of the tire cord calendering site electron irradiation tube by outputting numerical values.
7. A computer device comprising a memory, a processor and a computer program stored on the memory, wherein the processor executes the computer program to perform the method of: collecting the glass transition temperatures of an electron irradiation side and a non-electron irradiation side, comparing the glass transition temperature results of the electron irradiation side and the non-electron irradiation side, and judging that the carcass ply is successfully pre-crosslinked after the electron irradiation if the difference value of the glass transition temperatures of the electron irradiation side and the non-electron irradiation side is 1.0-3.5 ℃; and beyond the range of 1.0-3.5 ℃ of the glass transition temperature difference, regulating the work of the tire cord calendering site electron irradiation tube by outputting numerical values.
8. A computer readable storage medium having stored thereon a computer program or instructions, which when executed by a processor, performs the method of: collecting the glass transition temperatures of an electron irradiation side and a non-electron irradiation side, comparing the glass transition temperature results of the electron irradiation side and the non-electron irradiation side, and judging that the carcass ply is successfully pre-crosslinked after the electron irradiation if the difference value of the glass transition temperatures of the electron irradiation side and the non-electron irradiation side is 1.0-3.5 ℃; and beyond the range of 1.0-3.5 ℃ of the glass transition temperature difference, regulating the work of the tire cord calendering site electron irradiation tube by outputting numerical values.
9. A computer program product comprising a computer program or instructions which, when executed by a processor, performs the method of: collecting the glass transition temperatures of an electron irradiation side and a non-electron irradiation side, comparing the glass transition temperature results of the electron irradiation side and the non-electron irradiation side, and judging that the carcass ply is successfully pre-crosslinked after the electron irradiation if the difference value of the glass transition temperatures of the electron irradiation side and the non-electron irradiation side is 1.0-3.5 ℃; and beyond the range of 1.0-3.5 ℃ of the glass transition temperature difference, regulating the work of the tire cord calendering site electron irradiation tube by outputting numerical values.
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